Accessory Publication
data_51023c 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H34 La2 N24 O20' 
_chemical_formula_weight          1184.51 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'La'  'La'  -0.2871   2.4523 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    8.8374(10) 
_cell_length_b                    22.301(3) 
_cell_length_c                    10.4039(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.787(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2049.5(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     294(2) 
_cell_measurement_reflns_used     5133 
_cell_measurement_theta_min       2.16 
_cell_measurement_theta_max       26.45 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     1.919 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1168 
_exptl_absorpt_coefficient_mu     2.161 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.588741 
_exptl_absorpt_correction_T_max   1.000000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       294(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_standards_decay_%         . 
_diffrn_reflns_number             11463 
_diffrn_reflns_av_R_equivalents   0.0410 
_diffrn_reflns_av_sigmaI/netI     0.0424 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -27 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          1.83 
_diffrn_reflns_theta_max          26.45 
_reflns_number_total              4194 
_reflns_number_gt                 3166 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0536P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     CONSTR 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4194 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0418 
_refine_ls_R_factor_gt            0.0269 
_refine_ls_wR_factor_ref          0.0662 
_refine_ls_wR_factor_gt           0.0609 
_refine_ls_goodness_of_fit_ref    1.082 
_refine_ls_restrained_S_all       1.082 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
La1 La 0.240539(17) 0.501487(7) 0.969575(16) 0.01577(7) Uani 1 1 d . . . 
O1 O 0.0773(2) 0.54019(11) 0.7842(2) 0.0313(6) Uani 1 1 d . . . 
O2 O -0.1725(2) 0.54822(10) 0.8148(2) 0.0269(5) Uani 1 1 d . . . 
O3 O 0.3276(2) 0.60617(9) 0.8771(2) 0.0257(5) Uani 1 1 d . . . 
O4 O 0.5267(2) 0.55524(9) 0.9479(2) 0.0212(5) Uani 1 1 d . . . 
O5 O 0.1829(2) 0.38740(9) 0.9212(2) 0.0285(5) Uani 1 1 d . . . 
O6 O -0.0230(2) 0.44191(9) 0.9412(2) 0.0227(5) Uani 1 1 d . . . 
O7 O 0.3335(2) 0.56803(10) 1.1548(2) 0.0284(5) Uani 1 1 d . . . 
H7A H 0.2756 0.5781 1.2154 0.034 Uiso 1 1 d R . . 
H7B H 0.4284 0.5690 1.1740 0.034 Uiso 1 1 d R . . 
O8 O 0.3676(2) 0.46888(11) 0.7618(2) 0.0311(5) Uani 1 1 d . . . 
H8A H 0.3449 0.4359 0.7246 0.037 Uiso 1 1 d R . . 
H8B H 0.4099 0.4953 0.7162 0.037 Uiso 1 1 d R . . 
N1 N 0.0549(3) 0.59500(13) 0.5502(3) 0.0313(7) Uani 1 1 d . . . 
N2 N 0.0578(4) 0.57827(17) 0.4272(3) 0.0507(9) Uani 1 1 d . . . 
N3 N 0.1879(4) 0.59456(17) 0.3863(3) 0.0530(10) Uani 1 1 d . . . 
N4 N 0.2714(3) 0.62091(18) 0.4803(3) 0.0527(10) Uani 1 1 d . . . 
N5 N 0.5013(3) 0.70137(11) 0.8026(3) 0.0259(6) Uani 1 1 d . . . 
N6 N 0.5552(5) 0.70836(17) 0.6852(3) 0.0612(11) Uani 1 1 d . . . 
N7 N 0.4699(6) 0.7482(2) 0.6291(4) 0.0863(15) Uani 1 1 d . . . 
N8 N 0.3630(5) 0.76798(18) 0.7083(5) 0.0784(14) Uani 1 1 d . . . 
N9 N 0.0237(3) 0.28675(12) 0.9935(3) 0.0293(7) Uani 1 1 d . . . 
N10 N -0.0013(5) 0.27371(17) 1.1161(4) 0.0661(11) Uani 1 1 d . . . 
N11 N 0.0920(5) 0.23092(17) 1.1477(4) 0.0652(11) Uani 1 1 d . . . 
N12 N 0.1778(4) 0.21625(13) 1.0488(3) 0.0444(8) Uani 1 1 d . . . 
C1 C -0.0540(3) 0.55465(14) 0.7525(3) 0.0222(7) Uani 1 1 d . . . 
C2 C -0.0808(4) 0.58448(19) 0.6229(4) 0.0396(10) Uani 1 1 d . . . 
H2A H -0.1495 0.5596 0.5716 0.048 Uiso 1 1 calc R . . 
H2B H -0.1306 0.6226 0.6363 0.048 Uiso 1 1 calc R . . 
C3 C 0.1857(4) 0.62000(19) 0.5812(4) 0.0485(11) Uani 1 1 d . . . 
H3 H 0.2134 0.6348 0.6622 0.058 Uiso 1 1 calc R . . 
C4 C 0.4648(3) 0.60271(13) 0.9041(3) 0.0178(6) Uani 1 1 d . . . 
C5 C 0.5664(3) 0.65679(13) 0.8891(3) 0.0257(7) Uani 1 1 d . . . 
H5A H 0.5855 0.6749 0.9728 0.031 Uiso 1 1 calc R . . 
H5B H 0.6628 0.6437 0.8568 0.031 Uiso 1 1 calc R . . 
C6 C 0.3847(5) 0.73768(18) 0.8148(4) 0.0519(12) Uani 1 1 d . . . 
H6 H 0.3271 0.7412 0.8877 0.062 Uiso 1 1 calc R . . 
C7 C 0.0439(3) 0.39201(13) 0.9307(3) 0.0196(7) Uani 1 1 d . . . 
C8 C -0.0539(4) 0.33606(14) 0.9294(4) 0.0324(8) Uani 1 1 d . . . 
H8C H -0.1475 0.3444 0.9722 0.039 Uiso 1 1 calc R . . 
H8D H -0.0790 0.3249 0.8412 0.039 Uiso 1 1 calc R . . 
C9 C 0.1344(4) 0.25182(15) 0.9559(4) 0.0360(9) Uani 1 1 d . . . 
H9 H 0.1754 0.2526 0.8747 0.043 Uiso 1 1 calc R . . 
O9 O 0.3992(3) 0.38004(11) 0.5781(3) 0.0473(7) Uani 1 1 d . . . 
H9A H 0.3348 0.3519 0.5871 0.057 Uiso 1 1 d R . . 
H9B H 0.4904 0.3688 0.5673 0.057 Uiso 1 1 d R . . 
O10 O 0.5547(3) 0.54482(15) 0.6477(3) 0.0683(10) Uani 1 1 d . . . 
H10A H 0.5774 0.5142 0.6073 0.082 Uiso 1 1 d R . . 
H10B H 0.6204 0.5622 0.6979 0.082 Uiso 1 1 d R . . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
La1 0.01120(10) 0.01679(10) 0.01942(11) 0.00246(8) 0.00205(7) 0.00091(7) 
O1 0.0165(12) 0.0487(15) 0.0288(14) 0.0143(12) -0.0005(10) -0.0026(11) 
O2 0.0207(12) 0.0354(13) 0.0252(13) 0.0103(10) 0.0076(9) 0.0014(10) 
O3 0.0171(11) 0.0262(12) 0.0338(14) 0.0077(10) -0.0009(9) 0.0004(10) 
O4 0.0202(11) 0.0188(11) 0.0247(12) 0.0052(10) 0.0030(9) 0.0031(9) 
O5 0.0145(11) 0.0222(12) 0.0491(16) -0.0048(11) 0.0027(10) -0.0010(9) 
O6 0.0172(11) 0.0197(12) 0.0311(13) -0.0024(10) -0.0017(9) 0.0034(9) 
O7 0.0174(11) 0.0421(14) 0.0259(13) -0.0063(11) 0.0039(9) -0.0006(10) 
O8 0.0333(13) 0.0319(13) 0.0286(14) -0.0054(11) 0.0075(10) -0.0067(11) 
N1 0.0243(15) 0.0514(19) 0.0185(15) 0.0100(14) 0.0036(12) -0.0006(14) 
N2 0.051(2) 0.071(2) 0.0303(19) -0.0051(18) 0.0091(16) -0.0183(19) 
N3 0.044(2) 0.079(3) 0.037(2) -0.0030(19) 0.0181(16) -0.0103(19) 
N4 0.0341(19) 0.089(3) 0.035(2) 0.012(2) 0.0072(15) -0.0171(19) 
N5 0.0317(16) 0.0195(14) 0.0266(16) 0.0063(12) 0.0031(13) -0.0042(12) 
N6 0.086(3) 0.060(2) 0.040(2) 0.0175(19) 0.021(2) -0.003(2) 
N7 0.122(4) 0.080(3) 0.056(3) 0.045(3) -0.012(3) -0.012(3) 
N8 0.078(3) 0.055(3) 0.100(4) 0.045(3) -0.025(3) 0.009(2) 
N9 0.0288(17) 0.0187(14) 0.0406(19) 0.0032(13) 0.0058(14) 0.0001(12) 
N10 0.084(3) 0.061(3) 0.055(3) 0.018(2) 0.034(2) 0.025(2) 
N11 0.091(3) 0.058(2) 0.048(2) 0.021(2) 0.019(2) 0.016(2) 
N12 0.054(2) 0.0305(17) 0.048(2) 0.0070(16) -0.0007(17) 0.0124(16) 
C1 0.0212(17) 0.0244(17) 0.0209(17) 0.0010(14) 0.0010(13) -0.0029(14) 
C2 0.0236(19) 0.062(3) 0.033(2) 0.024(2) 0.0071(16) 0.0051(18) 
C3 0.041(2) 0.077(3) 0.028(2) 0.003(2) 0.0000(18) -0.021(2) 
C4 0.0186(16) 0.0160(15) 0.0189(16) 0.0008(13) 0.0027(12) 0.0005(12) 
C5 0.0227(17) 0.0206(16) 0.0337(19) 0.0073(15) -0.0033(14) 0.0014(14) 
C6 0.047(3) 0.044(2) 0.064(3) 0.017(2) 0.003(2) 0.019(2) 
C7 0.0178(16) 0.0199(16) 0.0211(17) -0.0015(13) -0.0011(13) -0.0021(13) 
C8 0.0220(18) 0.0204(17) 0.055(2) -0.0005(16) -0.0012(16) 0.0019(14) 
C9 0.045(2) 0.0295(19) 0.034(2) -0.0023(17) 0.0086(18) 0.0091(17) 
O9 0.0401(15) 0.0416(16) 0.0603(19) -0.0122(14) 0.0031(13) -0.0077(13) 
O10 0.0474(18) 0.096(3) 0.061(2) 0.0252(19) -0.0019(15) -0.0253(18) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
La1 O6 2.503(2) 3_567 ? 
La1 O1 2.524(2) . ? 
La1 O4 2.5412(19) 3_667 ? 
La1 O7 2.548(2) . ? 
La1 O8 2.572(2) . ? 
La1 O2 2.589(2) 3_567 ? 
La1 O5 2.640(2) . ? 
La1 O3 2.649(2) . ? 
La1 O6 2.689(2) . ? 
La1 O4 2.814(2) . ? 
La1 C7 3.017(3) . ? 
La1 C4 3.094(3) . ? 
O1 C1 1.239(3) . ? 
O2 C1 1.258(3) . ? 
O2 La1 2.589(2) 3_567 ? 
O3 C4 1.238(3) . ? 
O4 C4 1.270(3) . ? 
O4 La1 2.5412(19) 3_667 ? 
O5 C7 1.239(3) . ? 
O6 C7 1.266(3) . ? 
O6 La1 2.503(2) 3_567 ? 
O7 H7A 0.8551 . ? 
O7 H7B 0.8559 . ? 
O8 H8A 0.8524 . ? 
O8 H8B 0.8499 . ? 
N1 C3 1.315(4) . ? 
N1 N2 1.334(4) . ? 
N1 C2 1.456(4) . ? 
N2 N3 1.291(4) . ? 
N3 N4 1.342(4) . ? 
N4 C3 1.314(5) . ? 
N5 C6 1.320(4) . ? 
N5 N6 1.334(4) . ? 
N5 C5 1.448(4) . ? 
N6 N7 1.292(5) . ? 
N7 N8 1.348(7) . ? 
N8 C6 1.307(5) . ? 
N9 C9 1.319(4) . ? 
N9 N10 1.334(4) . ? 
N9 C8 1.447(4) . ? 
N10 N11 1.296(5) . ? 
N11 N12 1.337(5) . ? 
N12 C9 1.300(4) . ? 
C1 C2 1.515(5) . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
C3 H3 0.9300 . ? 
C4 C5 1.515(4) . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.518(4) . ? 
C8 H8C 0.9700 . ? 
C8 H8D 0.9700 . ? 
C9 H9 0.9300 . ? 
O9 H9A 0.8544 . ? 
O9 H9B 0.8540 . ? 
O10 H10A 0.8291 . ? 
O10 H10B 0.8615 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O6 La1 O1 71.56(7) 3_567 . ? 
O6 La1 O4 138.50(7) 3_567 3_667 ? 
O1 La1 O4 149.94(7) . 3_667 ? 
O6 La1 O7 70.07(7) 3_567 . ? 
O1 La1 O7 122.80(7) . . ? 
O4 La1 O7 78.23(7) 3_667 . ? 
O6 La1 O8 144.59(7) 3_567 . ? 
O1 La1 O8 73.06(7) . . ? 
O4 La1 O8 76.88(7) 3_667 . ? 
O7 La1 O8 131.41(7) . . ? 
O6 La1 O2 72.11(7) 3_567 3_567 ? 
O1 La1 O2 131.73(7) . 3_567 ? 
O4 La1 O2 72.64(7) 3_667 3_567 ? 
O7 La1 O2 70.88(7) . 3_567 ? 
O8 La1 O2 136.57(7) . 3_567 ? 
O6 La1 O5 114.25(7) 3_567 . ? 
O1 La1 O5 94.68(7) . . ? 
O4 La1 O5 74.58(6) 3_667 . ? 
O7 La1 O5 139.58(7) . . ? 
O8 La1 O5 69.75(7) . . ? 
O2 La1 O5 72.78(7) 3_567 . ? 
O6 La1 O3 85.73(7) 3_567 . ? 
O1 La1 O3 65.58(7) . . ? 
O4 La1 O3 108.67(6) 3_667 . ? 
O7 La1 O3 70.77(7) . . ? 
O8 La1 O3 78.73(7) . . ? 
O2 La1 O3 140.35(7) 3_567 . ? 
O5 La1 O3 146.80(7) . . ? 
O6 La1 O6 67.49(8) 3_567 . ? 
O1 La1 O6 67.22(7) . . ? 
O4 La1 O6 118.70(7) 3_667 . ? 
O7 La1 O6 128.95(7) . . ? 
O8 La1 O6 99.63(7) . . ? 
O2 La1 O6 70.13(7) 3_567 . ? 
O5 La1 O6 48.83(6) . . ? 
O3 La1 O6 131.00(6) . . ? 
O6 La1 O4 121.17(7) 3_567 . ? 
O1 La1 O4 106.67(6) . . ? 
O4 La1 O4 61.25(7) 3_667 . ? 
O7 La1 O4 62.79(7) . . ? 
O8 La1 O4 68.67(7) . . ? 
O2 La1 O4 119.02(6) 3_567 . ? 
O5 La1 O4 124.32(6) . . ? 
O3 La1 O4 47.42(6) . . ? 
O6 La1 O4 168.22(7) . . ? 
O6 La1 C7 90.68(8) 3_567 . ? 
O1 La1 C7 82.03(8) . . ? 
O4 La1 C7 95.69(7) 3_667 . ? 
O7 La1 C7 138.05(8) . . ? 
O8 La1 C7 85.59(8) . . ? 
O2 La1 C7 67.75(8) 3_567 . ? 
O5 La1 C7 24.15(7) . . ? 
O3 La1 C7 146.87(7) . . ? 
O6 La1 C7 24.80(7) . . ? 
O4 La1 C7 148.15(7) . . ? 
O6 La1 C4 102.62(7) 3_567 . ? 
O1 La1 C4 86.38(7) . . ? 
O4 La1 C4 85.43(7) 3_667 . ? 
O7 La1 C4 63.12(7) . . ? 
O8 La1 C4 73.84(8) . . ? 
O2 La1 C4 132.13(7) 3_567 . ? 
O5 La1 C4 141.47(7) . . ? 
O3 La1 C4 23.27(6) . . ? 
O6 La1 C4 153.46(7) . . ? 
O4 La1 C4 24.24(6) . . ? 
C7 La1 C4 158.63(8) . . ? 
C1 O1 La1 143.2(2) . . ? 
C1 O2 La1 135.7(2) . 3_567 ? 
C4 O3 La1 98.99(18) . . ? 
C4 O4 La1 150.64(19) . 3_667 ? 
C4 O4 La1 90.32(16) . . ? 
La1 O4 La1 118.75(7) 3_667 . ? 
C7 O5 La1 95.20(18) . . ? 
C7 O6 La1 147.26(19) . 3_567 ? 
C7 O6 La1 92.22(16) . . ? 
La1 O6 La1 112.51(8) 3_567 . ? 
La1 O7 H7A 121.7 . . ? 
La1 O7 H7B 118.8 . . ? 
H7A O7 H7B 115.1 . . ? 
La1 O8 H8A 121.5 . . ? 
La1 O8 H8B 119.0 . . ? 
H8A O8 H8B 116.4 . . ? 
C3 N1 N2 108.1(3) . . ? 
C3 N1 C2 132.3(3) . . ? 
N2 N1 C2 119.6(3) . . ? 
N3 N2 N1 106.4(3) . . ? 
N2 N3 N4 111.0(3) . . ? 
C3 N4 N3 105.0(3) . . ? 
C6 N5 N6 108.6(3) . . ? 
C6 N5 C5 131.1(3) . . ? 
N6 N5 C5 120.2(3) . . ? 
N7 N6 N5 105.9(4) . . ? 
N6 N7 N8 111.1(4) . . ? 
C6 N8 N7 105.2(4) . . ? 
C9 N9 N10 107.5(3) . . ? 
C9 N9 C8 131.1(3) . . ? 
N10 N9 C8 121.1(3) . . ? 
N11 N10 N9 106.3(3) . . ? 
N10 N11 N12 110.9(3) . . ? 
C9 N12 N11 105.1(3) . . ? 
O1 C1 O2 128.4(3) . . ? 
O1 C1 C2 118.1(3) . . ? 
O2 C1 C2 113.5(3) . . ? 
N1 C2 C1 115.1(3) . . ? 
N1 C2 H2A 108.5 . . ? 
C1 C2 H2A 108.5 . . ? 
N1 C2 H2B 108.5 . . ? 
C1 C2 H2B 108.5 . . ? 
H2A C2 H2B 107.5 . . ? 
N4 C3 N1 109.6(4) . . ? 
N4 C3 H3 125.2 . . ? 
N1 C3 H3 125.2 . . ? 
O3 C4 O4 122.8(3) . . ? 
O3 C4 C5 120.4(3) . . ? 
O4 C4 C5 116.8(2) . . ? 
O3 C4 La1 57.73(15) . . ? 
O4 C4 La1 65.44(15) . . ? 
C5 C4 La1 171.7(2) . . ? 
N5 C5 C4 112.6(2) . . ? 
N5 C5 H5A 109.1 . . ? 
C4 C5 H5A 109.1 . . ? 
N5 C5 H5B 109.1 . . ? 
C4 C5 H5B 109.1 . . ? 
H5A C5 H5B 107.8 . . ? 
N8 C6 N5 109.3(4) . . ? 
N8 C6 H6 125.4 . . ? 
N5 C6 H6 125.4 . . ? 
O5 C7 O6 123.1(3) . . ? 
O5 C7 C8 119.8(3) . . ? 
O6 C7 C8 117.1(3) . . ? 
O5 C7 La1 60.65(16) . . ? 
O6 C7 La1 62.97(15) . . ? 
C8 C7 La1 172.8(2) . . ? 
N9 C8 C7 111.1(2) . . ? 
N9 C8 H8C 109.4 . . ? 
C7 C8 H8C 109.4 . . ? 
N9 C8 H8D 109.4 . . ? 
C7 C8 H8D 109.4 . . ? 
H8C C8 H8D 108.0 . . ? 
N12 C9 N9 110.1(3) . . ? 
N12 C9 H9 124.9 . . ? 
N9 C9 H9 124.9 . . ? 
H9A O9 H9B 115.7 . . ? 
H10A O10 H10B 120.6 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O6 La1 O1 C1 -27.8(3) 3_567 . . . ? 
O4 La1 O1 C1 153.2(3) 3_667 . . . ? 
O7 La1 O1 C1 -77.8(4) . . . . ? 
O8 La1 O1 C1 153.4(4) . . . . ? 
O2 La1 O1 C1 15.2(4) 3_567 . . . ? 
O5 La1 O1 C1 86.3(4) . . . . ? 
O3 La1 O1 C1 -121.5(4) . . . . ? 
O6 La1 O1 C1 44.9(3) . . . . ? 
O4 La1 O1 C1 -145.8(3) . . . . ? 
C7 La1 O1 C1 65.7(4) . . . . ? 
C4 La1 O1 C1 -132.3(4) . . . . ? 
O6 La1 O3 C4 136.73(19) 3_567 . . . ? 
O1 La1 O3 C4 -151.6(2) . . . . ? 
O4 La1 O3 C4 -3.4(2) 3_667 . . . ? 
O7 La1 O3 C4 66.36(18) . . . . ? 
O8 La1 O3 C4 -75.25(18) . . . . ? 
O2 La1 O3 C4 81.7(2) 3_567 . . . ? 
O5 La1 O3 C4 -93.6(2) . . . . ? 
O6 La1 O3 C4 -168.27(17) . . . . ? 
O4 La1 O3 C4 -3.94(16) . . . . ? 
C7 La1 O3 C4 -138.58(19) . . . . ? 
O6 La1 O4 C4 -43.83(19) 3_567 . . . ? 
O1 La1 O4 C4 34.35(18) . . . . ? 
O4 La1 O4 C4 -175.6(2) 3_667 . . . ? 
O7 La1 O4 C4 -84.46(17) . . . . ? 
O8 La1 O4 C4 98.03(18) . . . . ? 
O2 La1 O4 C4 -129.53(17) 3_567 . . . ? 
O5 La1 O4 C4 142.26(17) . . . . ? 
O3 La1 O4 C4 3.79(16) . . . . ? 
O6 La1 O4 C4 91.4(3) . . . . ? 
C7 La1 O4 C4 136.33(19) . . . . ? 
O6 La1 O4 La1 131.80(9) 3_567 . . 3_667 ? 
O1 La1 O4 La1 -150.02(9) . . . 3_667 ? 
O4 La1 O4 La1 0.0 3_667 . . 3_667 ? 
O7 La1 O4 La1 91.17(10) . . . 3_667 ? 
O8 La1 O4 La1 -86.35(10) . . . 3_667 ? 
O2 La1 O4 La1 46.10(11) 3_567 . . 3_667 ? 
O5 La1 O4 La1 -42.12(12) . . . 3_667 ? 
O3 La1 O4 La1 179.42(14) . . . 3_667 ? 
O6 La1 O4 La1 -93.0(3) . . . 3_667 ? 
C7 La1 O4 La1 -48.04(18) . . . 3_667 ? 
C4 La1 O4 La1 175.6(2) . . . 3_667 ? 
O6 La1 O5 C7 13.4(2) 3_567 . . . ? 
O1 La1 O5 C7 -58.50(19) . . . . ? 
O4 La1 O5 C7 150.1(2) 3_667 . . . ? 
O7 La1 O5 C7 100.6(2) . . . . ? 
O8 La1 O5 C7 -128.5(2) . . . . ? 
O2 La1 O5 C7 73.87(19) 3_567 . . . ? 
O3 La1 O5 C7 -109.27(19) . . . . ? 
O6 La1 O5 C7 -4.49(17) . . . . ? 
O4 La1 O5 C7 -172.34(17) . . . . ? 
C4 La1 O5 C7 -148.55(18) . . . . ? 
O6 La1 O6 C7 -158.0(2) 3_567 . . . ? 
O1 La1 O6 C7 123.38(19) . . . . ? 
O4 La1 O6 C7 -23.8(2) 3_667 . . . ? 
O7 La1 O6 C7 -122.04(18) . . . . ? 
O8 La1 O6 C7 56.44(18) . . . . ? 
O2 La1 O6 C7 -79.77(18) 3_567 . . . ? 
O5 La1 O6 C7 4.38(17) . . . . ? 
O3 La1 O6 C7 139.82(17) . . . . ? 
O4 La1 O6 C7 62.7(3) . . . . ? 
C4 La1 O6 C7 129.5(2) . . . . ? 
O6 La1 O6 La1 0.0 3_567 . . 3_567 ? 
O1 La1 O6 La1 -78.61(9) . . . 3_567 ? 
O4 La1 O6 La1 134.22(8) 3_667 . . 3_567 ? 
O7 La1 O6 La1 35.98(12) . . . 3_567 ? 
O8 La1 O6 La1 -145.54(9) . . . 3_567 ? 
O2 La1 O6 La1 78.24(9) 3_567 . . 3_567 ? 
O5 La1 O6 La1 162.39(13) . . . 3_567 ? 
O3 La1 O6 La1 -62.17(12) . . . 3_567 ? 
O4 La1 O6 La1 -139.3(2) . . . 3_567 ? 
C7 La1 O6 La1 158.0(2) . . . 3_567 ? 
C4 La1 O6 La1 -72.53(19) . . . 3_567 ? 
C3 N1 N2 N3 -1.3(4) . . . . ? 
C2 N1 N2 N3 178.0(3) . . . . ? 
N1 N2 N3 N4 0.8(5) . . . . ? 
N2 N3 N4 C3 0.0(5) . . . . ? 
C6 N5 N6 N7 -0.4(5) . . . . ? 
C5 N5 N6 N7 176.3(3) . . . . ? 
N5 N6 N7 N8 1.0(6) . . . . ? 
N6 N7 N8 C6 -1.1(6) . . . . ? 
C9 N9 N10 N11 -1.3(5) . . . . ? 
C8 N9 N10 N11 -175.4(3) . . . . ? 
N9 N10 N11 N12 0.6(5) . . . . ? 
N10 N11 N12 C9 0.3(5) . . . . ? 
La1 O1 C1 O2 -8.0(6) . . . . ? 
La1 O1 C1 C2 171.5(3) . . . . ? 
La1 O2 C1 O1 -4.8(5) 3_567 . . . ? 
La1 O2 C1 C2 175.7(2) 3_567 . . . ? 
C3 N1 C2 C1 -50.1(6) . . . . ? 
N2 N1 C2 C1 130.7(3) . . . . ? 
O1 C1 C2 N1 -2.1(5) . . . . ? 
O2 C1 C2 N1 177.5(3) . . . . ? 
N3 N4 C3 N1 -0.8(5) . . . . ? 
N2 N1 C3 N4 1.4(5) . . . . ? 
C2 N1 C3 N4 -177.8(4) . . . . ? 
La1 O3 C4 O4 7.7(3) . . . . ? 
La1 O3 C4 C5 -170.5(2) . . . . ? 
La1 O4 C4 O3 -179.3(3) 3_667 . . . ? 
La1 O4 C4 O3 -7.1(3) . . . . ? 
La1 O4 C4 C5 -1.0(6) 3_667 . . . ? 
La1 O4 C4 C5 171.1(2) . . . . ? 
La1 O4 C4 La1 -172.2(4) 3_667 . . . ? 
O6 La1 C4 O3 -44.47(19) 3_567 . . . ? 
O1 La1 C4 O3 25.71(18) . . . . ? 
O4 La1 C4 O3 176.76(19) 3_667 . . . ? 
O7 La1 C4 O3 -104.13(19) . . . . ? 
O8 La1 C4 O3 99.11(19) . . . . ? 
O2 La1 C4 O3 -121.65(17) 3_567 . . . ? 
O5 La1 C4 O3 118.67(19) . . . . ? 
O6 La1 C4 O3 20.1(3) . . . . ? 
O4 La1 C4 O3 172.9(3) . . . . ? 
C7 La1 C4 O3 82.8(3) . . . . ? 
O6 La1 C4 O4 142.62(17) 3_567 . . . ? 
O1 La1 C4 O4 -147.20(18) . . . . ? 
O4 La1 C4 O4 3.8(2) 3_667 . . . ? 
O7 La1 C4 O4 82.95(17) . . . . ? 
O8 La1 C4 O4 -73.80(17) . . . . ? 
O2 La1 C4 O4 65.4(2) 3_567 . . . ? 
O5 La1 C4 O4 -54.2(2) . . . . ? 
O3 La1 C4 O4 -172.9(3) . . . . ? 
O6 La1 C4 O4 -152.82(16) . . . . ? 
C7 La1 C4 O4 -90.1(3) . . . . ? 
O6 La1 C4 C5 35.4(14) 3_567 . . . ? 
O1 La1 C4 C5 105.5(14) . . . . ? 
O4 La1 C4 C5 -103.4(14) 3_667 . . . ? 
O7 La1 C4 C5 -24.3(14) . . . . ? 
O8 La1 C4 C5 178.9(14) . . . . ? 
O2 La1 C4 C5 -41.8(14) 3_567 . . . ? 
O5 La1 C4 C5 -161.5(13) . . . . ? 
O3 La1 C4 C5 79.8(14) . . . . ? 
O6 La1 C4 C5 99.9(14) . . . . ? 
O4 La1 C4 C5 -107.3(14) . . . . ? 
C7 La1 C4 C5 162.6(13) . . . . ? 
C6 N5 C5 C4 69.7(5) . . . . ? 
N6 N5 C5 C4 -106.2(4) . . . . ? 
O3 C4 C5 N5 -20.4(4) . . . . ? 
O4 C4 C5 N5 161.3(3) . . . . ? 
La1 C4 C5 N5 -95.3(14) . . . . ? 
N7 N8 C6 N5 0.8(5) . . . . ? 
N6 N5 C6 N8 -0.3(5) . . . . ? 
C5 N5 C6 N8 -176.5(3) . . . . ? 
La1 O5 C7 O6 8.6(3) . . . . ? 
La1 O5 C7 C8 -171.7(3) . . . . ? 
La1 O6 C7 O5 -148.6(3) 3_567 . . . ? 
La1 O6 C7 O5 -8.4(3) . . . . ? 
La1 O6 C7 C8 31.7(5) 3_567 . . . ? 
La1 O6 C7 C8 171.9(3) . . . . ? 
La1 O6 C7 La1 -140.2(4) 3_567 . . . ? 
O6 La1 C7 O5 -167.83(19) 3_567 . . . ? 
O1 La1 C7 O5 120.90(19) . . . . ? 
O4 La1 C7 O5 -28.90(19) 3_667 . . . ? 
O7 La1 C7 O5 -107.61(19) . . . . ? 
O8 La1 C7 O5 47.42(18) . . . . ? 
O2 La1 C7 O5 -97.51(19) 3_567 . . . ? 
O3 La1 C7 O5 108.9(2) . . . . ? 
O6 La1 C7 O5 171.9(3) . . . . ? 
O4 La1 C7 O5 12.0(3) . . . . ? 
C4 La1 C7 O5 63.1(3) . . . . ? 
O6 La1 C7 O6 20.2(2) 3_567 . . . ? 
O1 La1 C7 O6 -51.03(18) . . . . ? 
O4 La1 C7 O6 159.17(17) 3_667 . . . ? 
O7 La1 C7 O6 80.5(2) . . . . ? 
O8 La1 C7 O6 -124.51(18) . . . . ? 
O2 La1 C7 O6 90.56(18) 3_567 . . . ? 
O5 La1 C7 O6 -171.9(3) . . . . ? 
O3 La1 C7 O6 -63.0(2) . . . . ? 
O4 La1 C7 O6 -159.89(15) . . . . ? 
C4 La1 C7 O6 -108.8(2) . . . . ? 
O6 La1 C7 C8 -72.5(16) 3_567 . . . ? 
O1 La1 C7 C8 -143.8(16) . . . . ? 
O4 La1 C7 C8 66.4(16) 3_667 . . . ? 
O7 La1 C7 C8 -12.3(17) . . . . ? 
O8 La1 C7 C8 142.7(16) . . . . ? 
O2 La1 C7 C8 -2.2(16) 3_567 . . . ? 
O5 La1 C7 C8 95.3(17) . . . . ? 
O3 La1 C7 C8 -155.8(16) . . . . ? 
O6 La1 C7 C8 -92.8(17) . . . . ? 
O4 La1 C7 C8 107.3(16) . . . . ? 
C4 La1 C7 C8 158.4(16) . . . . ? 
C9 N9 C8 C7 -75.6(4) . . . . ? 
N10 N9 C8 C7 96.9(4) . . . . ? 
O5 C7 C8 N9 35.4(4) . . . . ? 
O6 C7 C8 N9 -144.9(3) . . . . ? 
La1 C7 C8 N9 -55.8(17) . . . . ? 
N11 N12 C9 N9 -1.2(4) . . . . ? 
N10 N9 C9 N12 1.6(4) . . . . ? 
C8 N9 C9 N12 174.8(3) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              26.45 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.439 
_refine_diff_density_min   -1.069 
_refine_diff_density_rms    0.119

data_51023d 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C9 H17 N12 O10 Pr' 
_chemical_formula_weight          594.26 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pr'  'Pr'  -0.2180   2.8214 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    8.7757(10) 
_cell_length_b                    22.283(2) 
_cell_length_c                    10.4045(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.670(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2033.8(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     294(2) 
_cell_measurement_reflns_used     5420 
_cell_measurement_theta_min       2.68 
_cell_measurement_theta_max       26.35 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             lightgreen 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     1.941 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1176 
_exptl_absorpt_coefficient_mu     2.473 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.632891 
_exptl_absorpt_correction_T_max   1.000000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       294(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_standards_decay_%         . 
_diffrn_reflns_number             11363 
_diffrn_reflns_av_R_equivalents   0.0241 
_diffrn_reflns_av_sigmaI/netI     0.0269 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          1.83 
_diffrn_reflns_theta_max          26.38 
_reflns_number_total              4130 
_reflns_number_gt                 3259 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0536P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4130 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0356 
_refine_ls_R_factor_gt            0.0243 
_refine_ls_wR_factor_ref          0.0586 
_refine_ls_wR_factor_gt           0.0549 
_refine_ls_goodness_of_fit_ref    1.186 
_refine_ls_restrained_S_all       1.186 
_refine_ls_shift/su_max           0.003 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pr1 Pr 0.239473(15) 0.501202(6) 0.969928(14) 0.01613(6) Uani 1 1 d . . . 
O1 O 0.0797(2) 0.53858(9) 0.78501(19) 0.0292(5) Uani 1 1 d . . . 
O2 O -0.1715(2) 0.54812(9) 0.81811(19) 0.0261(5) Uani 1 1 d . . . 
O3 O 0.3280(2) 0.60448(9) 0.8786(2) 0.0255(5) Uani 1 1 d . . . 
O4 O 0.5301(2) 0.55456(8) 0.94913(19) 0.0225(4) Uani 1 1 d . . . 
O5 O 0.1828(2) 0.38872(8) 0.9195(2) 0.0279(5) Uani 1 1 d . . . 
O6 O -0.0240(2) 0.44273(8) 0.9433(2) 0.0237(4) Uani 1 1 d . . . 
O7 O 0.3333(2) 0.56628(9) 1.15214(18) 0.0271(5) Uani 1 1 d . . . 
H7A H 0.2754 0.5764 1.2128 0.032 Uiso 1 1 d R . . 
H7B H 0.4281 0.5672 1.1714 0.032 Uiso 1 1 d R . . 
O8 O 0.3672(2) 0.46915(9) 0.7661(2) 0.0292(5) Uani 1 1 d . . . 
H8A H 0.3445 0.4362 0.7289 0.035 Uiso 1 1 d R . . 
H8B H 0.4095 0.4955 0.7205 0.035 Uiso 1 1 d R . . 
N1 N 0.0561(3) 0.59380(12) 0.5510(2) 0.0303(6) Uani 1 1 d . . . 
N2 N 0.0563(3) 0.57763(15) 0.4278(3) 0.0497(8) Uani 1 1 d . . . 
N3 N 0.1878(3) 0.59283(15) 0.3854(3) 0.0513(9) Uani 1 1 d . . . 
N4 N 0.2738(3) 0.61882(17) 0.4784(3) 0.0556(9) Uani 1 1 d . . . 
N5 N 0.5007(3) 0.70044(11) 0.8035(2) 0.0275(6) Uani 1 1 d . . . 
N6 N 0.5540(4) 0.70699(16) 0.6852(3) 0.0638(10) Uani 1 1 d . . . 
N7 N 0.4689(6) 0.7463(2) 0.6286(4) 0.0850(14) Uani 1 1 d . . . 
N8 N 0.3619(4) 0.76658(17) 0.7074(5) 0.0800(13) Uani 1 1 d . . . 
N9 N 0.0222(3) 0.28750(11) 0.9915(3) 0.0291(6) Uani 1 1 d . . . 
N10 N -0.0020(5) 0.27493(16) 1.1149(4) 0.0687(11) Uani 1 1 d . . . 
N11 N 0.0905(4) 0.23170(16) 1.1475(4) 0.0683(11) Uani 1 1 d . . . 
N12 N 0.1755(3) 0.21627(12) 1.0471(3) 0.0464(8) Uani 1 1 d . . . 
C1 C -0.0523(3) 0.55369(12) 0.7542(3) 0.0212(6) Uani 1 1 d . . . 
C2 C -0.0793(3) 0.58430(17) 0.6250(3) 0.0393(9) Uani 1 1 d . . . 
H2A H -0.1507 0.5602 0.5741 0.047 Uiso 1 1 calc R . . 
H2B H -0.1269 0.6229 0.6396 0.047 Uiso 1 1 calc R . . 
C3 C 0.1894(4) 0.61809(18) 0.5813(3) 0.0497(10) Uani 1 1 d . . . 
H3 H 0.2191 0.6324 0.6622 0.060 Uiso 1 1 calc R . . 
C4 C 0.4666(3) 0.60151(12) 0.9057(3) 0.0188(6) Uani 1 1 d . . . 
C5 C 0.5666(3) 0.65634(12) 0.8913(3) 0.0258(7) Uani 1 1 d . . . 
H5A H 0.5834 0.6748 0.9750 0.031 Uiso 1 1 calc R . . 
H5B H 0.6649 0.6439 0.8603 0.031 Uiso 1 1 calc R . . 
C6 C 0.3839(4) 0.73672(16) 0.8141(4) 0.0546(11) Uani 1 1 d . . . 
H6 H 0.3255 0.7406 0.8869 0.066 Uiso 1 1 calc R . . 
C7 C 0.0434(3) 0.39300(12) 0.9303(3) 0.0192(6) Uani 1 1 d . . . 
C8 C -0.0553(3) 0.33711(13) 0.9271(3) 0.0316(7) Uani 1 1 d . . . 
H8C H -0.1503 0.3453 0.9691 0.038 Uiso 1 1 calc R . . 
H8D H -0.0791 0.3262 0.8385 0.038 Uiso 1 1 calc R . . 
C9 C 0.1328(4) 0.25183(15) 0.9538(3) 0.0388(8) Uani 1 1 d . . . 
H9 H 0.1740 0.2522 0.8724 0.047 Uiso 1 1 calc R . . 
O9 O 0.3951(3) 0.38136(10) 0.5793(2) 0.0471(6) Uani 1 1 d . . . 
H9A H 0.3307 0.3532 0.5883 0.056 Uiso 1 1 d R . . 
H9B H 0.4862 0.3702 0.5685 0.056 Uiso 1 1 d R . . 
O10 O 0.5549(3) 0.54490(13) 0.6481(3) 0.0678(9) Uani 1 1 d . . . 
H10A H 0.5776 0.5143 0.6078 0.081 Uiso 1 1 d R . . 
H10B H 0.6205 0.5623 0.6984 0.081 Uiso 1 1 d R . . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Pr1 0.01226(9) 0.01785(9) 0.01836(9) 0.00199(7) 0.00158(6) 0.00120(6) 
O1 0.0168(11) 0.0445(14) 0.0262(12) 0.0111(10) -0.0007(9) -0.0008(9) 
O2 0.0179(10) 0.0343(12) 0.0263(11) 0.0081(9) 0.0058(9) 0.0021(9) 
O3 0.0153(10) 0.0275(11) 0.0335(12) 0.0073(9) -0.0009(9) -0.0003(9) 
O4 0.0215(10) 0.0195(11) 0.0266(11) 0.0053(9) 0.0041(8) 0.0048(8) 
O5 0.0163(10) 0.0240(11) 0.0434(13) -0.0043(10) 0.0019(9) 0.0010(8) 
O6 0.0192(10) 0.0207(11) 0.0310(12) -0.0019(9) 0.0001(8) 0.0033(8) 
O7 0.0158(10) 0.0417(13) 0.0238(11) -0.0072(10) 0.0034(8) 0.0001(9) 
O8 0.0324(12) 0.0282(12) 0.0275(12) -0.0045(10) 0.0076(9) -0.0046(10) 
N1 0.0241(14) 0.0470(17) 0.0199(14) 0.0081(12) 0.0038(11) -0.0005(12) 
N2 0.0441(19) 0.074(2) 0.0310(17) -0.0046(16) 0.0105(15) -0.0149(16) 
N3 0.045(2) 0.075(2) 0.0349(18) -0.0038(17) 0.0171(15) -0.0056(17) 
N4 0.0367(18) 0.096(3) 0.0345(18) 0.0095(18) 0.0098(15) -0.0202(17) 
N5 0.0280(14) 0.0227(13) 0.0318(15) 0.0077(11) 0.0014(12) -0.0038(11) 
N6 0.085(3) 0.067(2) 0.041(2) 0.0194(18) 0.0189(19) -0.002(2) 
N7 0.120(4) 0.080(3) 0.054(3) 0.042(2) -0.012(3) -0.009(3) 
N8 0.076(3) 0.057(2) 0.105(4) 0.044(3) -0.030(3) 0.007(2) 
N9 0.0285(16) 0.0205(13) 0.0384(17) 0.0019(12) 0.0042(13) 0.0002(11) 
N10 0.086(3) 0.066(2) 0.055(2) 0.017(2) 0.036(2) 0.026(2) 
N11 0.090(3) 0.064(2) 0.051(2) 0.0219(19) 0.018(2) 0.020(2) 
N12 0.053(2) 0.0350(17) 0.051(2) 0.0079(15) -0.0011(16) 0.0133(15) 
C1 0.0204(15) 0.0216(15) 0.0215(15) 0.0024(12) -0.0029(12) -0.0011(12) 
C2 0.0205(17) 0.062(2) 0.036(2) 0.0220(18) 0.0089(14) 0.0070(16) 
C3 0.040(2) 0.081(3) 0.028(2) 0.0008(19) 0.0037(16) -0.022(2) 
C4 0.0215(15) 0.0203(15) 0.0148(14) -0.0007(12) 0.0031(11) -0.0006(12) 
C5 0.0215(15) 0.0215(15) 0.0341(18) 0.0046(13) -0.0043(13) -0.0009(12) 
C6 0.046(2) 0.045(2) 0.074(3) 0.021(2) 0.007(2) 0.0169(19) 
C7 0.0200(15) 0.0188(14) 0.0187(15) -0.0020(11) -0.0010(11) 0.0016(12) 
C8 0.0197(15) 0.0221(16) 0.053(2) -0.0007(15) -0.0041(14) -0.0003(13) 
C9 0.046(2) 0.0338(19) 0.037(2) 0.0005(16) 0.0047(16) 0.0119(16) 
O9 0.0409(14) 0.0435(14) 0.0569(17) -0.0131(13) 0.0025(12) -0.0085(11) 
O10 0.0458(16) 0.093(2) 0.064(2) 0.0258(18) -0.0003(14) -0.0191(15) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pr1 O6 2.4601(18) 3_567 ? 
Pr1 O1 2.491(2) . ? 
Pr1 O4 2.4983(18) 3_667 ? 
Pr1 O7 2.5068(19) . ? 
Pr1 O8 2.530(2) . ? 
Pr1 O2 2.5502(19) 3_567 ? 
Pr1 O5 2.6058(19) . ? 
Pr1 O3 2.6163(19) . ? 
Pr1 O6 2.6613(19) . ? 
Pr1 O4 2.8284(19) . ? 
Pr1 C7 2.983(3) . ? 
Pr1 C4 3.081(3) . ? 
O1 C1 1.239(3) . ? 
O2 C1 1.262(3) . ? 
O2 Pr1 2.5502(19) 3_567 ? 
O3 C4 1.243(3) . ? 
O4 C4 1.263(3) . ? 
O4 Pr1 2.4984(18) 3_667 ? 
O5 C7 1.235(3) . ? 
O6 C7 1.265(3) . ? 
O6 Pr1 2.4601(18) 3_567 ? 
O7 H7A 0.8521 . ? 
O7 H7B 0.8506 . ? 
O8 H8A 0.8518 . ? 
O8 H8B 0.8479 . ? 
N1 C3 1.319(4) . ? 
N1 N2 1.332(4) . ? 
N1 C2 1.450(4) . ? 
N2 N3 1.293(4) . ? 
N3 N4 1.341(4) . ? 
N4 C3 1.320(4) . ? 
N5 C6 1.313(4) . ? 
N5 N6 1.337(4) . ? 
N5 C5 1.450(3) . ? 
N6 N7 1.284(5) . ? 
N7 N8 1.343(6) . ? 
N8 C6 1.304(5) . ? 
N9 C9 1.323(4) . ? 
N9 N10 1.337(4) . ? 
N9 C8 1.451(4) . ? 
N10 N11 1.299(5) . ? 
N11 N12 1.346(4) . ? 
N12 C9 1.299(4) . ? 
C1 C2 1.520(4) . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
C3 H3 0.9300 . ? 
C4 C5 1.514(4) . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.517(4) . ? 
C8 H8C 0.9700 . ? 
C8 H8D 0.9700 . ? 
C9 H9 0.9300 . ? 
O9 H9A 0.8513 . ? 
O9 H9B 0.8484 . ? 
O10 H10A 0.8281 . ? 
O10 H10B 0.8595 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O6 Pr1 O1 72.08(7) 3_567 . ? 
O6 Pr1 O4 138.76(7) 3_567 3_667 ? 
O1 Pr1 O4 149.15(7) . 3_667 ? 
O6 Pr1 O7 70.59(6) 3_567 . ? 
O1 Pr1 O7 123.77(7) . . ? 
O4 Pr1 O7 77.76(6) 3_667 . ? 
O6 Pr1 O8 144.60(7) 3_567 . ? 
O1 Pr1 O8 72.55(7) . . ? 
O4 Pr1 O8 76.60(7) 3_667 . ? 
O7 Pr1 O8 130.79(6) . . ? 
O6 Pr1 O2 72.53(6) 3_567 3_567 ? 
O1 Pr1 O2 132.19(6) . 3_567 ? 
O4 Pr1 O2 72.63(6) 3_667 3_567 ? 
O7 Pr1 O2 71.05(6) . 3_567 ? 
O8 Pr1 O2 136.35(7) . 3_567 ? 
O6 Pr1 O5 114.72(6) 3_567 . ? 
O1 Pr1 O5 93.79(7) . . ? 
O4 Pr1 O5 74.78(6) 3_667 . ? 
O7 Pr1 O5 139.94(7) . . ? 
O8 Pr1 O5 69.29(6) . . ? 
O2 Pr1 O5 73.24(7) 3_567 . ? 
O6 Pr1 O3 85.76(6) 3_567 . ? 
O1 Pr1 O3 65.90(6) . . ? 
O4 Pr1 O3 108.30(6) 3_667 . ? 
O7 Pr1 O3 70.81(6) . . ? 
O8 Pr1 O3 78.49(6) . . ? 
O2 Pr1 O3 140.57(6) 3_567 . ? 
O5 Pr1 O3 146.09(6) . . ? 
O6 Pr1 O6 67.18(7) 3_567 . ? 
O1 Pr1 O6 67.39(6) . . ? 
O4 Pr1 O6 118.93(6) 3_667 . ? 
O7 Pr1 O6 128.85(6) . . ? 
O8 Pr1 O6 100.32(6) . . ? 
O2 Pr1 O6 69.81(6) 3_567 . ? 
O5 Pr1 O6 49.30(6) . . ? 
O3 Pr1 O6 131.22(6) . . ? 
O6 Pr1 O4 121.28(6) 3_567 . ? 
O1 Pr1 O4 106.79(6) . . ? 
O4 Pr1 O4 60.79(7) 3_667 . ? 
O7 Pr1 O4 62.45(6) . . ? 
O8 Pr1 O4 68.40(6) . . ? 
O2 Pr1 O4 118.78(6) 3_567 . ? 
O5 Pr1 O4 123.80(6) . . ? 
O3 Pr1 O4 47.51(5) . . ? 
O6 Pr1 O4 168.68(6) . . ? 
O6 Pr1 C7 90.85(7) 3_567 . ? 
O1 Pr1 C7 81.62(7) . . ? 
O4 Pr1 C7 95.88(7) 3_667 . ? 
O7 Pr1 C7 138.36(7) . . ? 
O8 Pr1 C7 85.64(7) . . ? 
O2 Pr1 C7 67.83(7) 3_567 . ? 
O5 Pr1 C7 24.34(6) . . ? 
O3 Pr1 C7 146.81(7) . . ? 
O6 Pr1 C7 25.08(6) . . ? 
O4 Pr1 C7 147.87(6) . . ? 
O6 Pr1 C4 102.73(7) 3_567 . ? 
O1 Pr1 C4 86.74(7) . . ? 
O4 Pr1 C4 84.92(7) 3_667 . ? 
O7 Pr1 C4 62.87(7) . . ? 
O8 Pr1 C4 73.61(7) . . ? 
O2 Pr1 C4 132.01(7) 3_567 . ? 
O5 Pr1 C4 140.81(6) . . ? 
O3 Pr1 C4 23.42(6) . . ? 
O6 Pr1 C4 153.92(7) . . ? 
O4 Pr1 C4 24.19(6) . . ? 
C7 Pr1 C4 158.50(7) . . ? 
C1 O1 Pr1 142.29(18) . . ? 
C1 O2 Pr1 135.74(17) . 3_567 ? 
C4 O3 Pr1 99.78(16) . . ? 
C4 O4 Pr1 151.29(17) . 3_667 ? 
C4 O4 Pr1 89.20(15) . . ? 
Pr1 O4 Pr1 119.20(7) 3_667 . ? 
C7 O5 Pr1 95.22(16) . . ? 
C7 O6 Pr1 148.28(17) . 3_567 ? 
C7 O6 Pr1 91.86(15) . . ? 
Pr1 O6 Pr1 112.82(7) 3_567 . ? 
Pr1 O7 H7A 121.5 . . ? 
Pr1 O7 H7B 119.3 . . ? 
H7A O7 H7B 114.8 . . ? 
Pr1 O8 H8A 121.4 . . ? 
Pr1 O8 H8B 119.0 . . ? 
H8A O8 H8B 116.4 . . ? 
C3 N1 N2 108.4(3) . . ? 
C3 N1 C2 131.9(3) . . ? 
N2 N1 C2 119.7(3) . . ? 
N3 N2 N1 106.5(3) . . ? 
N2 N3 N4 110.8(3) . . ? 
C3 N4 N3 105.3(3) . . ? 
C6 N5 N6 107.8(3) . . ? 
C6 N5 C5 131.5(3) . . ? 
N6 N5 C5 120.6(3) . . ? 
N7 N6 N5 106.4(3) . . ? 
N6 N7 N8 110.9(4) . . ? 
C6 N8 N7 105.1(3) . . ? 
C9 N9 N10 107.3(3) . . ? 
C9 N9 C8 131.2(3) . . ? 
N10 N9 C8 121.2(3) . . ? 
N11 N10 N9 106.9(3) . . ? 
N10 N11 N12 110.1(3) . . ? 
C9 N12 N11 105.7(3) . . ? 
O1 C1 O2 128.3(3) . . ? 
O1 C1 C2 118.1(2) . . ? 
O2 C1 C2 113.6(2) . . ? 
N1 C2 C1 115.2(2) . . ? 
N1 C2 H2A 108.5 . . ? 
C1 C2 H2A 108.5 . . ? 
N1 C2 H2B 108.5 . . ? 
C1 C2 H2B 108.5 . . ? 
H2A C2 H2B 107.5 . . ? 
N1 C3 N4 109.0(3) . . ? 
N1 C3 H3 125.5 . . ? 
N4 C3 H3 125.5 . . ? 
O3 C4 O4 123.0(2) . . ? 
O3 C4 C5 120.0(2) . . ? 
O4 C4 C5 117.0(2) . . ? 
O3 C4 Pr1 56.80(14) . . ? 
O4 C4 Pr1 66.61(14) . . ? 
C5 C4 Pr1 170.82(19) . . ? 
N5 C5 C4 112.8(2) . . ? 
N5 C5 H5A 109.0 . . ? 
C4 C5 H5A 109.0 . . ? 
N5 C5 H5B 109.0 . . ? 
C4 C5 H5B 109.0 . . ? 
H5A C5 H5B 107.8 . . ? 
N8 C6 N5 109.8(4) . . ? 
N8 C6 H6 125.1 . . ? 
N5 C6 H6 125.1 . . ? 
O5 C7 O6 123.0(3) . . ? 
O5 C7 C8 120.1(2) . . ? 
O6 C7 C8 116.9(2) . . ? 
O5 C7 Pr1 60.43(14) . . ? 
O6 C7 Pr1 63.07(14) . . ? 
C8 C7 Pr1 173.3(2) . . ? 
N9 C8 C7 110.8(2) . . ? 
N9 C8 H8C 109.5 . . ? 
C7 C8 H8C 109.5 . . ? 
N9 C8 H8D 109.5 . . ? 
C7 C8 H8D 109.5 . . ? 
H8C C8 H8D 108.1 . . ? 
N12 C9 N9 110.0(3) . . ? 
N12 C9 H9 125.0 . . ? 
N9 C9 H9 125.0 . . ? 
H9A O9 H9B 115.4 . . ? 
H10A O10 H10B 120.9 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O6 Pr1 O1 C1 -26.1(3) 3_567 . . . ? 
O4 Pr1 O1 C1 154.9(3) 3_667 . . . ? 
O7 Pr1 O1 C1 -76.6(3) . . . . ? 
O8 Pr1 O1 C1 155.5(3) . . . . ? 
O2 Pr1 O1 C1 17.9(3) 3_567 . . . ? 
O5 Pr1 O1 C1 88.6(3) . . . . ? 
O3 Pr1 O1 C1 -119.6(3) . . . . ? 
O6 Pr1 O1 C1 46.0(3) . . . . ? 
O4 Pr1 O1 C1 -144.3(3) . . . . ? 
C7 Pr1 O1 C1 67.5(3) . . . . ? 
C4 Pr1 O1 C1 -130.6(3) . . . . ? 
O6 Pr1 O3 C4 136.63(17) 3_567 . . . ? 
O1 Pr1 O3 C4 -151.12(18) . . . . ? 
O4 Pr1 O3 C4 -3.70(18) 3_667 . . . ? 
O7 Pr1 O3 C4 65.72(17) . . . . ? 
O8 Pr1 O3 C4 -75.25(17) . . . . ? 
O2 Pr1 O3 C4 80.97(18) 3_567 . . . ? 
O5 Pr1 O3 C4 -93.49(19) . . . . ? 
O6 Pr1 O3 C4 -168.97(16) . . . . ? 
O4 Pr1 O3 C4 -4.09(15) . . . . ? 
C7 Pr1 O3 C4 -138.32(17) . . . . ? 
O6 Pr1 O4 C4 -43.67(18) 3_567 . . . ? 
O1 Pr1 O4 C4 35.22(17) . . . . ? 
O4 Pr1 O4 C4 -175.6(2) 3_667 . . . ? 
O7 Pr1 O4 C4 -84.60(16) . . . . ? 
O8 Pr1 O4 C4 98.08(17) . . . . ? 
O2 Pr1 O4 C4 -129.82(16) 3_567 . . . ? 
O5 Pr1 O4 C4 141.79(15) . . . . ? 
O3 Pr1 O4 C4 3.97(15) . . . . ? 
O6 Pr1 O4 C4 92.6(3) . . . . ? 
C7 Pr1 O4 C4 136.43(17) . . . . ? 
O6 Pr1 O4 Pr1 131.95(8) 3_567 . . 3_667 ? 
O1 Pr1 O4 Pr1 -149.16(8) . . . 3_667 ? 
O4 Pr1 O4 Pr1 0.001(1) 3_667 . . 3_667 ? 
O7 Pr1 O4 Pr1 91.01(10) . . . 3_667 ? 
O8 Pr1 O4 Pr1 -86.31(9) . . . 3_667 ? 
O2 Pr1 O4 Pr1 45.79(10) 3_567 . . 3_667 ? 
O5 Pr1 O4 Pr1 -42.59(11) . . . 3_667 ? 
O3 Pr1 O4 Pr1 179.58(13) . . . 3_667 ? 
O6 Pr1 O4 Pr1 -91.8(3) . . . 3_667 ? 
C7 Pr1 O4 Pr1 -47.95(16) . . . 3_667 ? 
C4 Pr1 O4 Pr1 175.6(2) . . . 3_667 ? 
O6 Pr1 O5 C7 12.05(19) 3_567 . . . ? 
O1 Pr1 O5 C7 -59.95(17) . . . . ? 
O4 Pr1 O5 C7 149.17(18) 3_667 . . . ? 
O7 Pr1 O5 C7 100.85(18) . . . . ? 
O8 Pr1 O5 C7 -129.69(18) . . . . ? 
O2 Pr1 O5 C7 73.12(17) 3_567 . . . ? 
O3 Pr1 O5 C7 -110.54(17) . . . . ? 
O6 Pr1 O5 C7 -4.38(15) . . . . ? 
O4 Pr1 O5 C7 -173.08(15) . . . . ? 
C4 Pr1 O5 C7 -149.44(16) . . . . ? 
O6 Pr1 O6 C7 -159.6(2) 3_567 . . . ? 
O1 Pr1 O6 C7 121.18(17) . . . . ? 
O4 Pr1 O6 C7 -25.16(18) 3_667 . . . ? 
O7 Pr1 O6 C7 -122.87(16) . . . . ? 
O8 Pr1 O6 C7 55.13(17) . . . . ? 
O2 Pr1 O6 C7 -80.64(16) 3_567 . . . ? 
O5 Pr1 O6 C7 4.26(15) . . . . ? 
O3 Pr1 O6 C7 138.82(15) . . . . ? 
O4 Pr1 O6 C7 60.3(3) . . . . ? 
C4 Pr1 O6 C7 128.86(18) . . . . ? 
O6 Pr1 O6 Pr1 0.0 3_567 . . 3_567 ? 
O1 Pr1 O6 Pr1 -79.26(9) . . . 3_567 ? 
O4 Pr1 O6 Pr1 134.39(8) 3_667 . . 3_567 ? 
O7 Pr1 O6 Pr1 36.69(12) . . . 3_567 ? 
O8 Pr1 O6 Pr1 -145.31(8) . . . 3_567 ? 
O2 Pr1 O6 Pr1 78.91(8) 3_567 . . 3_567 ? 
O5 Pr1 O6 Pr1 163.81(13) . . . 3_567 ? 
O3 Pr1 O6 Pr1 -61.62(11) . . . 3_567 ? 
O4 Pr1 O6 Pr1 -140.2(2) . . . 3_567 ? 
C7 Pr1 O6 Pr1 159.6(2) . . . 3_567 ? 
C4 Pr1 O6 Pr1 -71.59(17) . . . 3_567 ? 
C3 N1 N2 N3 -0.7(4) . . . . ? 
C2 N1 N2 N3 178.0(3) . . . . ? 
N1 N2 N3 N4 -0.1(4) . . . . ? 
N2 N3 N4 C3 0.9(5) . . . . ? 
C6 N5 N6 N7 -0.1(5) . . . . ? 
C5 N5 N6 N7 176.5(3) . . . . ? 
N5 N6 N7 N8 0.9(5) . . . . ? 
N6 N7 N8 C6 -1.3(6) . . . . ? 
C9 N9 N10 N11 -1.5(5) . . . . ? 
C8 N9 N10 N11 -175.4(3) . . . . ? 
N9 N10 N11 N12 0.5(5) . . . . ? 
N10 N11 N12 C9 0.7(5) . . . . ? 
Pr1 O1 C1 O2 -9.0(5) . . . . ? 
Pr1 O1 C1 C2 169.5(2) . . . . ? 
Pr1 O2 C1 O1 -6.0(5) 3_567 . . . ? 
Pr1 O2 C1 C2 175.4(2) 3_567 . . . ? 
C3 N1 C2 C1 -50.7(5) . . . . ? 
N2 N1 C2 C1 130.9(3) . . . . ? 
O1 C1 C2 N1 -1.2(5) . . . . ? 
O2 C1 C2 N1 177.5(3) . . . . ? 
N2 N1 C3 N4 1.3(4) . . . . ? 
C2 N1 C3 N4 -177.2(3) . . . . ? 
N3 N4 C3 N1 -1.3(5) . . . . ? 
Pr1 O3 C4 O4 8.1(3) . . . . ? 
Pr1 O3 C4 C5 -169.9(2) . . . . ? 
Pr1 O4 C4 O3 -179.4(2) 3_667 . . . ? 
Pr1 O4 C4 O3 -7.4(3) . . . . ? 
Pr1 O4 C4 C5 -1.4(5) 3_667 . . . ? 
Pr1 O4 C4 C5 170.6(2) . . . . ? 
Pr1 O4 C4 Pr1 -172.0(4) 3_667 . . . ? 
O6 Pr1 C4 O3 -44.60(18) 3_567 . . . ? 
O1 Pr1 C4 O3 26.21(17) . . . . ? 
O4 Pr1 C4 O3 176.47(17) 3_667 . . . ? 
O7 Pr1 C4 O3 -104.69(18) . . . . ? 
O8 Pr1 C4 O3 98.97(17) . . . . ? 
O2 Pr1 C4 O3 -122.43(16) 3_567 . . . ? 
O5 Pr1 C4 O3 118.21(17) . . . . ? 
O6 Pr1 C4 O3 19.1(3) . . . . ? 
O4 Pr1 C4 O3 172.6(3) . . . . ? 
C7 Pr1 C4 O3 83.3(2) . . . . ? 
O6 Pr1 C4 O4 142.77(15) 3_567 . . . ? 
O1 Pr1 C4 O4 -146.42(16) . . . . ? 
O4 Pr1 C4 O4 3.84(18) 3_667 . . . ? 
O7 Pr1 C4 O4 82.68(16) . . . . ? 
O8 Pr1 C4 O4 -73.66(16) . . . . ? 
O2 Pr1 C4 O4 64.94(18) 3_567 . . . ? 
O5 Pr1 C4 O4 -54.4(2) . . . . ? 
O3 Pr1 C4 O4 -172.6(3) . . . . ? 
O6 Pr1 C4 O4 -153.52(15) . . . . ? 
C7 Pr1 C4 O4 -89.3(2) . . . . ? 
O6 Pr1 C4 C5 28.0(12) 3_567 . . . ? 
O1 Pr1 C4 C5 98.8(12) . . . . ? 
O4 Pr1 C4 C5 -110.9(12) 3_667 . . . ? 
O7 Pr1 C4 C5 -32.1(12) . . . . ? 
O8 Pr1 C4 C5 171.6(12) . . . . ? 
O2 Pr1 C4 C5 -49.8(12) 3_567 . . . ? 
O5 Pr1 C4 C5 -169.2(12) . . . . ? 
O3 Pr1 C4 C5 72.6(12) . . . . ? 
O6 Pr1 C4 C5 91.7(12) . . . . ? 
O4 Pr1 C4 C5 -114.8(13) . . . . ? 
C7 Pr1 C4 C5 155.9(11) . . . . ? 
C6 N5 C5 C4 71.1(4) . . . . ? 
N6 N5 C5 C4 -104.7(3) . . . . ? 
O3 C4 C5 N5 -21.4(4) . . . . ? 
O4 C4 C5 N5 160.5(2) . . . . ? 
Pr1 C4 C5 N5 -88.7(12) . . . . ? 
N7 N8 C6 N5 1.2(5) . . . . ? 
N6 N5 C6 N8 -0.7(5) . . . . ? 
C5 N5 C6 N8 -176.8(3) . . . . ? 
Pr1 O5 C7 O6 8.3(3) . . . . ? 
Pr1 O5 C7 C8 -172.3(2) . . . . ? 
Pr1 O6 C7 O5 -150.4(3) 3_567 . . . ? 
Pr1 O6 C7 O5 -8.1(3) . . . . ? 
Pr1 O6 C7 C8 30.3(5) 3_567 . . . ? 
Pr1 O6 C7 C8 172.5(2) . . . . ? 
Pr1 O6 C7 Pr1 -142.2(4) 3_567 . . . ? 
O6 Pr1 C7 O5 -169.06(17) 3_567 . . . ? 
O1 Pr1 C7 O5 119.19(17) . . . . ? 
O4 Pr1 C7 O5 -29.81(17) 3_667 . . . ? 
O7 Pr1 C7 O5 -107.98(17) . . . . ? 
O8 Pr1 C7 O5 46.21(17) . . . . ? 
O2 Pr1 C7 O5 -98.35(17) 3_567 . . . ? 
O3 Pr1 C7 O5 107.40(18) . . . . ? 
O6 Pr1 C7 O5 172.2(3) . . . . ? 
O4 Pr1 C7 O5 10.9(2) . . . . ? 
C4 Pr1 C7 O5 61.2(3) . . . . ? 
O6 Pr1 C7 O6 18.78(19) 3_567 . . . ? 
O1 Pr1 C7 O6 -52.97(16) . . . . ? 
O4 Pr1 C7 O6 158.03(16) 3_667 . . . ? 
O7 Pr1 C7 O6 79.86(19) . . . . ? 
O8 Pr1 C7 O6 -125.95(16) . . . . ? 
O2 Pr1 C7 O6 89.50(16) 3_567 . . . ? 
O5 Pr1 C7 O6 -172.2(3) . . . . ? 
O3 Pr1 C7 O6 -64.8(2) . . . . ? 
O4 Pr1 C7 O6 -161.30(13) . . . . ? 
C4 Pr1 C7 O6 -110.9(2) . . . . ? 
O6 Pr1 C7 C8 -72.9(16) 3_567 . . . ? 
O1 Pr1 C7 C8 -144.7(16) . . . . ? 
O4 Pr1 C7 C8 66.3(16) 3_667 . . . ? 
O7 Pr1 C7 C8 -11.8(17) . . . . ? 
O8 Pr1 C7 C8 142.4(16) . . . . ? 
O2 Pr1 C7 C8 -2.2(16) 3_567 . . . ? 
O5 Pr1 C7 C8 96.1(16) . . . . ? 
O3 Pr1 C7 C8 -156.5(16) . . . . ? 
O6 Pr1 C7 C8 -91.7(16) . . . . ? 
O4 Pr1 C7 C8 107.0(16) . . . . ? 
C4 Pr1 C7 C8 157.4(15) . . . . ? 
C9 N9 C8 C7 -77.0(4) . . . . ? 
N10 N9 C8 C7 95.3(4) . . . . ? 
O5 C7 C8 N9 37.0(4) . . . . ? 
O6 C7 C8 N9 -143.7(3) . . . . ? 
Pr1 C7 C8 N9 -55.4(17) . . . . ? 
N11 N12 C9 N9 -1.7(4) . . . . ? 
N10 N9 C9 N12 2.0(4) . . . . ? 
C8 N9 C9 N12 175.1(3) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              26.38 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.455 
_refine_diff_density_min   -0.831 
_refine_diff_density_rms    0.093

data_51023e 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C9 H16 N12 Nd O9.50' 
_chemical_formula_weight          588.58 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Nd'  'Nd'  -0.1943   3.0179 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    8.5865(11) 
_cell_length_b                    10.3205(13) 
_cell_length_c                    12.6320(15) 
_cell_angle_alpha                 69.262(2) 
_cell_angle_beta                  78.536(2) 
_cell_angle_gamma                 83.392(2) 
_cell_volume                      1024.8(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     294(2) 
_cell_measurement_reflns_used     4405 
_cell_measurement_theta_min       2.24 
_cell_measurement_theta_max       26.30 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             lightpurple 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     1.907 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              580 
_exptl_absorpt_coefficient_mu     2.607 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.562947 
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       294(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_standards_decay_%         . 
_diffrn_reflns_number             5234 
_diffrn_reflns_av_R_equivalents   0.0180 
_diffrn_reflns_av_sigmaI/netI     0.0320 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.11 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              3581 
_reflns_number_gt                 3298 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.3804P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3581 
_refine_ls_number_parameters      314 
_refine_ls_number_restraints      21 
_refine_ls_R_factor_all           0.0251 
_refine_ls_R_factor_gt            0.0220 
_refine_ls_wR_factor_ref          0.0585 
_refine_ls_wR_factor_gt           0.0569 
_refine_ls_goodness_of_fit_ref    1.110 
_refine_ls_restrained_S_all       1.116 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Nd1 Nd 0.260426(18) -0.017156(17) -0.008305(13) 0.01932(7) Uani 1 1 d . . . 
O1 O 0.2702(3) -0.1920(3) 0.1996(2) 0.0341(6) Uani 1 1 d . . . 
O2 O 0.5020(3) -0.1049(2) 0.11675(18) 0.0258(5) Uani 1 1 d . . . 
O3 O 0.2860(3) 0.1347(3) 0.0992(2) 0.0304(5) Uani 1 1 d . . . 
O4 O 0.5432(3) 0.1801(2) 0.0719(2) 0.0304(5) Uani 1 1 d . . . 
O5 O 0.2431(3) 0.0077(3) -0.21590(19) 0.0325(6) Uani 1 1 d . . . 
O6 O 0.0082(3) 0.0081(2) -0.10845(18) 0.0262(5) Uani 1 1 d . . . 
O7 O 0.1725(3) 0.2351(3) -0.1069(2) 0.0329(6) Uani 1 1 d D . . 
H7A H 0.124(5) 0.257(4) -0.163(2) 0.055(14) Uiso 1 1 d D . . 
H7B H 0.231(5) 0.295(3) -0.104(3) 0.056(14) Uiso 1 1 d D . . 
O8 O 0.1581(4) -0.2492(3) 0.0151(3) 0.0494(8) Uani 1 1 d D . . 
H8C H 0.230(5) -0.305(4) 0.047(5) 0.10(2) Uiso 1 1 d D . . 
H8D H 0.077(5) -0.286(5) 0.010(6) 0.14(3) Uiso 1 1 d D . . 
N1 N 0.3811(4) -0.3621(3) 0.3926(2) 0.0318(7) Uani 1 1 d . . . 
N2 N 0.3834(6) -0.4836(4) 0.3776(3) 0.0716(13) Uani 1 1 d . . . 
N3 N 0.2785(7) -0.5563(4) 0.4588(4) 0.0770(14) Uani 1 1 d . . . 
N4 N 0.2076(5) -0.4855(4) 0.5259(3) 0.0604(11) Uani 1 1 d . . . 
N5 N 0.4789(4) 0.3721(3) 0.1764(2) 0.0339(7) Uani 1 1 d . . . 
N6 N 0.4957(5) 0.5090(4) 0.1213(3) 0.0546(11) Uani 1 1 d . . . 
N7 N 0.6300(6) 0.5343(5) 0.1421(4) 0.0664(13) Uani 1 1 d . . . 
N8 N 0.6985(5) 0.4175(5) 0.2088(4) 0.0721(13) Uani 1 1 d . . . 
N9 N 0.1234(4) 0.0155(3) -0.4010(2) 0.0327(7) Uani 1 1 d . . . 
N10 N 0.1729(5) -0.0908(4) -0.4379(3) 0.0519(10) Uani 1 1 d . . . 
N11 N 0.2715(5) -0.0427(5) -0.5323(3) 0.0620(11) Uani 1 1 d . . . 
N12 N 0.2884(6) 0.0926(5) -0.5572(3) 0.0667(12) Uani 1 1 d . . . 
C1 C 0.4121(4) -0.1797(3) 0.2018(3) 0.0227(7) Uani 1 1 d . . . 
C2 C 0.4790(4) -0.2522(4) 0.3116(3) 0.0321(8) Uani 1 1 d . . . 
H2A H 0.5850 -0.2909 0.2930 0.039 Uiso 1 1 calc R . . 
H2B H 0.4879 -0.1847 0.3471 0.039 Uiso 1 1 calc R . . 
C3 C 0.2727(6) -0.3661(5) 0.4832(4) 0.0544(12) Uani 1 1 d . . . 
H3 H 0.2463 -0.2939 0.5124 0.065 Uiso 1 1 calc R . . 
C4 C 0.0960(4) 0.0053(3) -0.2006(3) 0.0245(7) Uani 1 1 d . . . 
C5 C 0.0143(4) -0.0041(5) -0.2935(3) 0.0378(9) Uani 1 1 d . . . 
H5A H -0.0310 -0.0942 -0.2680 0.045 Uiso 1 1 calc R . . 
H5B H -0.0722 0.0660 -0.3060 0.045 Uiso 1 1 calc R . . 
C6 C 0.1961(7) 0.1244(5) -0.4746(4) 0.0585(13) Uani 1 1 d . . . 
H6 H 0.1834 0.2123 -0.4685 0.070 Uiso 1 1 calc R . . 
C7 C 0.3981(4) 0.1970(3) 0.1067(3) 0.0240(7) Uani 1 1 d . . . 
C8 C 0.3471(4) 0.3028(4) 0.1667(3) 0.0335(8) Uani 1 1 d . . . 
H8A H 0.2746 0.3720 0.1247 0.040 Uiso 1 1 calc R . . 
H8B H 0.2897 0.2566 0.2431 0.040 Uiso 1 1 calc R . . 
C9 C 0.6038(6) 0.3201(5) 0.2274(4) 0.0557(12) Uani 1 1 d . . . 
H9 H 0.6210 0.2273 0.2702 0.067 Uiso 1 1 calc R . . 
O9 O -0.0279(4) 0.6830(4) 0.2935(3) 0.0681(10) Uani 1 1 d D . . 
H9A H -0.0066 0.6066 0.2786 0.082 Uiso 1 1 d RD . . 
H9B H 0.0549 0.7250 0.2903 0.082 Uiso 1 1 d RD . . 
O10 O 0.022(2) 0.465(2) 0.0565(15) 0.100(5) Uani 0.25 1 d PU . 1 
O10' O 0.009(3) 0.431(3) 0.187(2) 0.147(9) Uani 0.25 1 d PU A 2 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Nd1 0.01583(10) 0.02323(11) 0.01802(10) -0.00545(7) -0.00132(7) -0.00529(7) 
O1 0.0225(13) 0.0394(14) 0.0304(13) 0.0020(12) -0.0033(10) -0.0090(11) 
O2 0.0244(12) 0.0271(12) 0.0213(11) -0.0027(10) 0.0002(10) -0.0085(10) 
O3 0.0254(13) 0.0375(14) 0.0325(13) -0.0161(12) -0.0042(10) -0.0057(11) 
O4 0.0277(13) 0.0287(13) 0.0381(14) -0.0164(11) -0.0021(11) -0.0034(10) 
O5 0.0217(13) 0.0524(16) 0.0242(12) -0.0140(12) -0.0025(10) -0.0037(11) 
O6 0.0222(12) 0.0376(14) 0.0184(11) -0.0093(11) -0.0012(9) -0.0057(10) 
O7 0.0309(14) 0.0292(13) 0.0376(15) -0.0056(12) -0.0111(12) -0.0069(11) 
O8 0.0407(18) 0.0427(17) 0.066(2) -0.0228(16) 0.0060(16) -0.0175(15) 
N1 0.0408(18) 0.0274(16) 0.0206(14) -0.0006(13) -0.0037(13) -0.0028(13) 
N2 0.110(4) 0.037(2) 0.056(2) -0.017(2) 0.025(2) -0.021(2) 
N3 0.116(4) 0.039(2) 0.061(3) -0.007(2) 0.014(3) -0.031(2) 
N4 0.073(3) 0.051(2) 0.041(2) -0.001(2) 0.010(2) -0.023(2) 
N5 0.053(2) 0.0263(16) 0.0248(15) -0.0120(13) -0.0006(14) -0.0098(14) 
N6 0.098(3) 0.0316(19) 0.0342(19) -0.0109(16) -0.003(2) -0.019(2) 
N7 0.090(3) 0.062(3) 0.057(2) -0.030(2) 0.009(2) -0.045(3) 
N8 0.061(3) 0.071(3) 0.107(4) -0.054(3) -0.015(3) -0.016(2) 
N9 0.0386(18) 0.0417(18) 0.0212(14) -0.0144(14) -0.0047(13) -0.0034(14) 
N10 0.073(3) 0.044(2) 0.039(2) -0.0175(18) -0.0033(19) -0.0019(19) 
N11 0.074(3) 0.071(3) 0.042(2) -0.029(2) 0.004(2) 0.003(2) 
N12 0.086(3) 0.076(3) 0.0289(19) -0.015(2) 0.015(2) -0.019(2) 
C1 0.0231(18) 0.0216(16) 0.0206(16) -0.0049(14) -0.0001(13) -0.0038(13) 
C2 0.032(2) 0.036(2) 0.0213(17) 0.0013(16) -0.0063(15) -0.0085(16) 
C3 0.068(3) 0.044(3) 0.041(2) -0.013(2) 0.017(2) -0.015(2) 
C4 0.0236(18) 0.0295(18) 0.0194(16) -0.0067(14) -0.0025(13) -0.0054(14) 
C5 0.031(2) 0.065(3) 0.0230(18) -0.0221(19) -0.0008(15) -0.0086(18) 
C6 0.087(4) 0.047(3) 0.038(2) -0.017(2) 0.009(2) -0.018(3) 
C7 0.0290(19) 0.0226(17) 0.0189(16) -0.0055(14) -0.0038(14) -0.0011(14) 
C8 0.035(2) 0.035(2) 0.0329(19) -0.0164(17) 0.0004(16) -0.0042(16) 
C9 0.063(3) 0.040(2) 0.078(3) -0.030(2) -0.028(3) 0.001(2) 
O9 0.057(2) 0.075(2) 0.0522(19) 0.0127(18) -0.0146(16) -0.0283(18) 
O10 0.057(8) 0.124(10) 0.112(9) -0.040(8) -0.004(7) 0.005(7) 
O10' 0.109(11) 0.136(12) 0.178(12) -0.041(9) -0.018(9) 0.016(8) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Nd1 O2 2.425(2) 2_655 ? 
Nd1 O3 2.460(2) . ? 
Nd1 O4 2.466(2) 2_655 ? 
Nd1 O6 2.490(2) 2 ? 
Nd1 O8 2.545(3) . ? 
Nd1 O7 2.554(2) . ? 
Nd1 O5 2.576(2) . ? 
Nd1 O1 2.618(2) . ? 
Nd1 O6 2.662(2) . ? 
Nd1 O2 2.734(2) . ? 
Nd1 C4 2.973(3) . ? 
Nd1 C1 3.045(3) . ? 
O1 C1 1.246(4) . ? 
O2 C1 1.252(4) . ? 
O2 Nd1 2.425(2) 2_655 ? 
O3 C7 1.253(4) . ? 
O4 C7 1.250(4) . ? 
O4 Nd1 2.466(2) 2_655 ? 
O5 C4 1.241(4) . ? 
O6 C4 1.263(4) . ? 
O6 Nd1 2.490(2) 2 ? 
O7 H7A 0.842(10) . ? 
O7 H7B 0.849(10) . ? 
O8 H8C 0.847(10) . ? 
O8 H8D 0.853(10) . ? 
N1 C3 1.315(5) . ? 
N1 N2 1.330(5) . ? 
N1 C2 1.448(4) . ? 
N2 N3 1.292(6) . ? 
N3 N4 1.325(7) . ? 
N4 C3 1.300(5) . ? 
N5 C9 1.323(6) . ? 
N5 N6 1.346(5) . ? 
N5 C8 1.452(5) . ? 
N6 N7 1.306(6) . ? 
N7 N8 1.351(6) . ? 
N8 C9 1.292(6) . ? 
N9 C6 1.307(5) . ? 
N9 N10 1.333(5) . ? 
N9 C5 1.451(4) . ? 
N10 N11 1.289(5) . ? 
N11 N12 1.336(6) . ? 
N12 C6 1.295(6) . ? 
C1 C2 1.515(4) . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
C3 H3 0.9300 . ? 
C4 C5 1.518(4) . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.517(5) . ? 
C8 H8A 0.9700 . ? 
C8 H8B 0.9700 . ? 
C9 H9 0.9300 . ? 
O9 H9A 0.8650 . ? 
O9 H9B 0.8618 . ? 
O10 O10 1.45(3) 2_565 ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O2 Nd1 O3 77.44(8) 2_655 . ? 
O2 Nd1 O4 71.02(8) 2_655 2_655 ? 
O3 Nd1 O4 130.34(8) . 2_655 ? 
O2 Nd1 O6 147.30(8) 2_655 2 ? 
O3 Nd1 O6 75.50(7) . 2 ? 
O4 Nd1 O6 141.55(8) 2_655 2 ? 
O2 Nd1 O8 133.52(9) 2_655 . ? 
O3 Nd1 O8 142.64(9) . . ? 
O4 Nd1 O8 63.93(9) 2_655 . ? 
O6 Nd1 O8 78.80(9) 2 . ? 
O2 Nd1 O7 72.83(8) 2_655 . ? 
O3 Nd1 O7 67.01(8) . . ? 
O4 Nd1 O7 132.98(8) 2_655 . ? 
O6 Nd1 O7 79.89(8) 2 . ? 
O8 Nd1 O7 133.74(10) . . ? 
O2 Nd1 O5 77.66(7) 2_655 . ? 
O3 Nd1 O5 137.86(8) . . ? 
O4 Nd1 O5 70.34(8) 2_655 . ? 
O6 Nd1 O5 111.64(7) 2 . ? 
O8 Nd1 O5 77.16(10) . . ? 
O7 Nd1 O5 73.41(8) . . ? 
O2 Nd1 O1 118.42(7) 2_655 . ? 
O3 Nd1 O1 76.97(8) . . ? 
O4 Nd1 O1 85.41(8) 2_655 . ? 
O6 Nd1 O1 72.54(7) 2 . ? 
O8 Nd1 O1 69.67(10) . . ? 
O7 Nd1 O1 139.01(9) . . ? 
O5 Nd1 O1 145.16(8) . . ? 
O2 Nd1 O6 119.95(7) 2_655 . ? 
O3 Nd1 O6 121.13(7) . . ? 
O4 Nd1 O6 107.78(7) 2_655 . ? 
O6 Nd1 O6 62.10(8) 2 . ? 
O8 Nd1 O6 66.81(10) . . ? 
O7 Nd1 O6 66.94(8) . . ? 
O5 Nd1 O6 49.57(7) . . ? 
O1 Nd1 O6 121.32(7) . . ? 
O2 Nd1 O2 70.31(8) 2_655 . ? 
O3 Nd1 O2 67.22(7) . . ? 
O4 Nd1 O2 66.49(7) 2_655 . ? 
O6 Nd1 O2 114.41(7) 2 . ? 
O8 Nd1 O2 100.40(10) . . ? 
O7 Nd1 O2 125.80(7) . . ? 
O5 Nd1 O2 132.41(7) . . ? 
O1 Nd1 O2 48.17(7) . . ? 
O6 Nd1 O2 166.95(7) . . ? 
O2 Nd1 C4 99.63(8) 2_655 . ? 
O3 Nd1 C4 135.52(9) . . ? 
O4 Nd1 C4 87.73(9) 2_655 . ? 
O6 Nd1 C4 87.22(8) 2 . ? 
O8 Nd1 C4 68.62(10) . . ? 
O7 Nd1 C4 69.78(9) . . ? 
O5 Nd1 C4 24.54(8) . . ? 
O1 Nd1 C4 136.33(8) . . ? 
O6 Nd1 C4 25.13(8) . . ? 
O2 Nd1 C4 154.08(8) . . ? 
O2 Nd1 C1 94.49(8) 2_655 . ? 
O3 Nd1 C1 69.80(8) . . ? 
O4 Nd1 C1 75.44(8) 2_655 . ? 
O6 Nd1 C1 93.10(8) 2 . ? 
O8 Nd1 C1 85.14(10) . . ? 
O7 Nd1 C1 136.64(8) . . ? 
O5 Nd1 C1 145.63(8) . . ? 
O1 Nd1 C1 23.94(8) . . ? 
O6 Nd1 C1 144.91(7) . . ? 
O2 Nd1 C1 24.25(7) . . ? 
C4 Nd1 C1 153.20(9) . . ? 
C1 O1 Nd1 97.61(19) . . ? 
C1 O2 Nd1 157.9(2) . 2_655 ? 
C1 O2 Nd1 91.93(19) . . ? 
Nd1 O2 Nd1 109.70(8) 2_655 . ? 
C7 O3 Nd1 134.6(2) . . ? 
C7 O4 Nd1 142.3(2) . 2_655 ? 
C4 O5 Nd1 95.94(19) . . ? 
C4 O6 Nd1 150.7(2) . 2 ? 
C4 O6 Nd1 91.34(18) . . ? 
Nd1 O6 Nd1 117.90(8) 2 . ? 
Nd1 O7 H7A 121(3) . . ? 
Nd1 O7 H7B 115(3) . . ? 
H7A O7 H7B 117.5(19) . . ? 
Nd1 O8 H8C 101(4) . . ? 
Nd1 O8 H8D 142(4) . . ? 
H8C O8 H8D 117(2) . . ? 
C3 N1 N2 107.1(3) . . ? 
C3 N1 C2 131.9(3) . . ? 
N2 N1 C2 120.9(3) . . ? 
N3 N2 N1 106.6(4) . . ? 
N2 N3 N4 110.9(4) . . ? 
C3 N4 N3 105.2(4) . . ? 
C9 N5 N6 108.3(4) . . ? 
C9 N5 C8 130.1(3) . . ? 
N6 N5 C8 121.3(3) . . ? 
N7 N6 N5 105.2(4) . . ? 
N6 N7 N8 111.0(4) . . ? 
C9 N8 N7 105.5(4) . . ? 
C6 N9 N10 107.4(3) . . ? 
C6 N9 C5 131.7(4) . . ? 
N10 N9 C5 120.9(3) . . ? 
N11 N10 N9 106.6(4) . . ? 
N10 N11 N12 110.5(4) . . ? 
C6 N12 N11 105.2(4) . . ? 
O1 C1 O2 122.2(3) . . ? 
O1 C1 C2 119.9(3) . . ? 
O2 C1 C2 117.9(3) . . ? 
O1 C1 Nd1 58.46(16) . . ? 
O2 C1 Nd1 63.82(17) . . ? 
C2 C1 Nd1 174.9(2) . . ? 
N1 C2 C1 112.5(3) . . ? 
N1 C2 H2A 109.1 . . ? 
C1 C2 H2A 109.1 . . ? 
N1 C2 H2B 109.1 . . ? 
C1 C2 H2B 109.1 . . ? 
H2A C2 H2B 107.8 . . ? 
N4 C3 N1 110.2(4) . . ? 
N4 C3 H3 124.9 . . ? 
N1 C3 H3 124.9 . . ? 
O5 C4 O6 122.6(3) . . ? 
O5 C4 C5 120.3(3) . . ? 
O6 C4 C5 117.1(3) . . ? 
O5 C4 Nd1 59.52(16) . . ? 
O6 C4 Nd1 63.53(16) . . ? 
C5 C4 Nd1 172.4(3) . . ? 
N9 C5 C4 112.0(3) . . ? 
N9 C5 H5A 109.2 . . ? 
C4 C5 H5A 109.2 . . ? 
N9 C5 H5B 109.2 . . ? 
C4 C5 H5B 109.2 . . ? 
H5A C5 H5B 107.9 . . ? 
N12 C6 N9 110.4(4) . . ? 
N12 C6 H6 124.8 . . ? 
N9 C6 H6 124.8 . . ? 
O4 C7 O3 127.3(3) . . ? 
O4 C7 C8 118.2(3) . . ? 
O3 C7 C8 114.5(3) . . ? 
N5 C8 C7 113.6(3) . . ? 
N5 C8 H8A 108.8 . . ? 
C7 C8 H8A 108.8 . . ? 
N5 C8 H8B 108.8 . . ? 
C7 C8 H8B 108.8 . . ? 
H8A C8 H8B 107.7 . . ? 
N8 C9 N5 110.0(4) . . ? 
N8 C9 H9 125.0 . . ? 
N5 C9 H9 125.0 . . ? 
H9A O9 H9B 114.1 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O2 Nd1 O1 C1 -1.7(2) 2_655 . . . ? 
O3 Nd1 O1 C1 -69.4(2) . . . . ? 
O4 Nd1 O1 C1 63.8(2) 2_655 . . . ? 
O6 Nd1 O1 C1 -148.1(2) 2 . . . ? 
O8 Nd1 O1 C1 127.7(2) . . . . ? 
O7 Nd1 O1 C1 -98.0(2) . . . . ? 
O5 Nd1 O1 C1 108.9(2) . . . . ? 
O6 Nd1 O1 C1 171.90(19) . . . . ? 
O2 Nd1 O1 C1 1.57(19) . . . . ? 
C4 Nd1 O1 C1 145.7(2) . . . . ? 
O2 Nd1 O2 C1 175.4(2) 2_655 . . . ? 
O3 Nd1 O2 C1 91.2(2) . . . . ? 
O4 Nd1 O2 C1 -107.4(2) 2_655 . . . ? 
O6 Nd1 O2 C1 30.4(2) 2 . . . ? 
O8 Nd1 O2 C1 -51.9(2) . . . . ? 
O7 Nd1 O2 C1 125.56(19) . . . . ? 
O5 Nd1 O2 C1 -133.95(19) . . . . ? 
O1 Nd1 O2 C1 -1.55(18) . . . . ? 
O6 Nd1 O2 C1 -41.0(4) . . . . ? 
C4 Nd1 O2 C1 -113.8(2) . . . . ? 
O2 Nd1 O2 Nd1 0.0 2_655 . . 2_655 ? 
O3 Nd1 O2 Nd1 -84.25(10) . . . 2_655 ? 
O4 Nd1 O2 Nd1 77.23(9) 2_655 . . 2_655 ? 
O6 Nd1 O2 Nd1 -144.99(8) 2 . . 2_655 ? 
O8 Nd1 O2 Nd1 132.68(10) . . . 2_655 ? 
O7 Nd1 O2 Nd1 -49.85(13) . . . 2_655 ? 
O5 Nd1 O2 Nd1 50.64(14) . . . 2_655 ? 
O1 Nd1 O2 Nd1 -176.97(15) . . . 2_655 ? 
O6 Nd1 O2 Nd1 143.5(2) . . . 2_655 ? 
C4 Nd1 O2 Nd1 70.7(2) . . . 2_655 ? 
C1 Nd1 O2 Nd1 -175.4(2) . . . 2_655 ? 
O2 Nd1 O3 C7 -20.8(3) 2_655 . . . ? 
O4 Nd1 O3 C7 30.5(3) 2_655 . . . ? 
O6 Nd1 O3 C7 177.8(3) 2 . . . ? 
O8 Nd1 O3 C7 129.8(3) . . . . ? 
O7 Nd1 O3 C7 -97.2(3) . . . . ? 
O5 Nd1 O3 C7 -75.8(3) . . . . ? 
O1 Nd1 O3 C7 102.7(3) . . . . ? 
O6 Nd1 O3 C7 -138.3(3) . . . . ? 
O2 Nd1 O3 C7 52.9(3) . . . . ? 
C4 Nd1 O3 C7 -111.8(3) . . . . ? 
C1 Nd1 O3 C7 78.9(3) . . . . ? 
O2 Nd1 O5 C4 -153.0(2) 2_655 . . . ? 
O3 Nd1 O5 C4 -98.0(2) . . . . ? 
O4 Nd1 O5 C4 133.0(2) 2_655 . . . ? 
O6 Nd1 O5 C4 -5.9(2) 2 . . . ? 
O8 Nd1 O5 C4 66.4(2) . . . . ? 
O7 Nd1 O5 C4 -77.5(2) . . . . ? 
O1 Nd1 O5 C4 84.4(2) . . . . ? 
O6 Nd1 O5 C4 -3.98(19) . . . . ? 
O2 Nd1 O5 C4 158.80(19) . . . . ? 
C1 Nd1 O5 C4 127.2(2) . . . . ? 
O2 Nd1 O6 C4 39.3(2) 2_655 . . . ? 
O3 Nd1 O6 C4 132.45(19) . . . . ? 
O4 Nd1 O6 C4 -38.6(2) 2_655 . . . ? 
O6 Nd1 O6 C4 -178.1(2) 2 . . . ? 
O8 Nd1 O6 C4 -88.8(2) . . . . ? 
O7 Nd1 O6 C4 91.3(2) . . . . ? 
O5 Nd1 O6 C4 3.89(18) . . . . ? 
O1 Nd1 O6 C4 -134.16(19) . . . . ? 
O2 Nd1 O6 C4 -100.5(3) . . . . ? 
C1 Nd1 O6 C4 -128.5(2) . . . . ? 
O2 Nd1 O6 Nd1 -142.55(9) 2_655 . . 2 ? 
O3 Nd1 O6 Nd1 -49.41(12) . . . 2 ? 
O4 Nd1 O6 Nd1 139.54(10) 2_655 . . 2 ? 
O6 Nd1 O6 Nd1 0.0 2 . . 2 ? 
O8 Nd1 O6 Nd1 89.30(12) . . . 2 ? 
O7 Nd1 O6 Nd1 -90.55(11) . . . 2 ? 
O5 Nd1 O6 Nd1 -177.98(15) . . . 2 ? 
O1 Nd1 O6 Nd1 43.98(13) . . . 2 ? 
O2 Nd1 O6 Nd1 77.7(3) . . . 2 ? 
C4 Nd1 O6 Nd1 178.1(2) . . . 2 ? 
C1 Nd1 O6 Nd1 49.69(18) . . . 2 ? 
C3 N1 N2 N3 -0.4(6) . . . . ? 
C2 N1 N2 N3 -176.3(4) . . . . ? 
N1 N2 N3 N4 0.2(7) . . . . ? 
N2 N3 N4 C3 0.1(7) . . . . ? 
C9 N5 N6 N7 -0.4(5) . . . . ? 
C8 N5 N6 N7 -175.7(3) . . . . ? 
N5 N6 N7 N8 -0.1(5) . . . . ? 
N6 N7 N8 C9 0.6(6) . . . . ? 
C6 N9 N10 N11 -0.7(5) . . . . ? 
C5 N9 N10 N11 -177.9(4) . . . . ? 
N9 N10 N11 N12 0.6(5) . . . . ? 
N10 N11 N12 C6 -0.2(6) . . . . ? 
Nd1 O1 C1 O2 -3.0(4) . . . . ? 
Nd1 O1 C1 C2 174.4(3) . . . . ? 
Nd1 O2 C1 O1 171.3(4) 2_655 . . . ? 
Nd1 O2 C1 O1 2.9(3) . . . . ? 
Nd1 O2 C1 C2 -6.2(8) 2_655 . . . ? 
Nd1 O2 C1 C2 -174.6(3) . . . . ? 
Nd1 O2 C1 Nd1 168.5(6) 2_655 . . . ? 
O2 Nd1 C1 O1 178.5(2) 2_655 . . . ? 
O3 Nd1 C1 O1 103.7(2) . . . . ? 
O4 Nd1 C1 O1 -112.4(2) 2_655 . . . ? 
O6 Nd1 C1 O1 30.4(2) 2 . . . ? 
O8 Nd1 C1 O1 -48.1(2) . . . . ? 
O7 Nd1 C1 O1 108.9(2) . . . . ? 
O5 Nd1 C1 O1 -106.8(2) . . . . ? 
O6 Nd1 C1 O1 -12.1(3) . . . . ? 
O2 Nd1 C1 O1 -177.1(3) . . . . ? 
C4 Nd1 C1 O1 -59.6(3) . . . . ? 
O2 Nd1 C1 O2 -4.3(2) 2_655 . . . ? 
O3 Nd1 C1 O2 -79.18(19) . . . . ? 
O4 Nd1 C1 O2 64.73(19) 2_655 . . . ? 
O6 Nd1 C1 O2 -152.50(19) 2 . . . ? 
O8 Nd1 C1 O2 129.0(2) . . . . ? 
O7 Nd1 C1 O2 -73.9(2) . . . . ? 
O5 Nd1 C1 O2 70.3(2) . . . . ? 
O1 Nd1 C1 O2 177.1(3) . . . . ? 
O6 Nd1 C1 O2 165.06(15) . . . . ? 
C4 Nd1 C1 O2 117.5(2) . . . . ? 
O2 Nd1 C1 C2 106(3) 2_655 . . . ? 
O3 Nd1 C1 C2 31(3) . . . . ? 
O4 Nd1 C1 C2 175(3) 2_655 . . . ? 
O6 Nd1 C1 C2 -42(3) 2 . . . ? 
O8 Nd1 C1 C2 -121(3) . . . . ? 
O7 Nd1 C1 C2 36(3) . . . . ? 
O5 Nd1 C1 C2 -179(2) . . . . ? 
O1 Nd1 C1 C2 -72(3) . . . . ? 
O6 Nd1 C1 C2 -85(3) . . . . ? 
O2 Nd1 C1 C2 110(3) . . . . ? 
C4 Nd1 C1 C2 -132(2) . . . . ? 
C3 N1 C2 C1 -98.4(5) . . . . ? 
N2 N1 C2 C1 76.4(5) . . . . ? 
O1 C1 C2 N1 17.7(5) . . . . ? 
O2 C1 C2 N1 -164.8(3) . . . . ? 
Nd1 C1 C2 N1 87(3) . . . . ? 
N3 N4 C3 N1 -0.3(6) . . . . ? 
N2 N1 C3 N4 0.4(6) . . . . ? 
C2 N1 C3 N4 175.8(4) . . . . ? 
Nd1 O5 C4 O6 7.6(4) . . . . ? 
Nd1 O5 C4 C5 -171.2(3) . . . . ? 
Nd1 O6 C4 O5 176.1(3) 2 . . . ? 
Nd1 O6 C4 O5 -7.3(3) . . . . ? 
Nd1 O6 C4 C5 -5.1(6) 2 . . . ? 
Nd1 O6 C4 C5 171.5(3) . . . . ? 
Nd1 O6 C4 Nd1 -176.6(4) 2 . . . ? 
O2 Nd1 C4 O5 26.7(2) 2_655 . . . ? 
O3 Nd1 C4 O5 108.5(2) . . . . ? 
O4 Nd1 C4 O5 -43.6(2) 2_655 . . . ? 
O6 Nd1 C4 O5 174.5(2) 2 . . . ? 
O8 Nd1 C4 O5 -106.4(2) . . . . ? 
O7 Nd1 C4 O5 94.3(2) . . . . ? 
O1 Nd1 C4 O5 -124.6(2) . . . . ? 
O6 Nd1 C4 O5 172.9(3) . . . . ? 
O2 Nd1 C4 O5 -37.7(3) . . . . ? 
C1 Nd1 C4 O5 -94.1(3) . . . . ? 
O2 Nd1 C4 O6 -146.17(18) 2_655 . . . ? 
O3 Nd1 C4 O6 -64.3(2) . . . . ? 
O4 Nd1 C4 O6 143.52(19) 2_655 . . . ? 
O6 Nd1 C4 O6 1.6(2) 2 . . . ? 
O8 Nd1 C4 O6 80.71(19) . . . . ? 
O7 Nd1 C4 O6 -78.60(19) . . . . ? 
O5 Nd1 C4 O6 -172.9(3) . . . . ? 
O1 Nd1 C4 O6 62.6(2) . . . . ? 
O2 Nd1 C4 O6 149.48(17) . . . . ? 
C1 Nd1 C4 O6 93.0(3) . . . . ? 
O2 Nd1 C4 C5 117.4(17) 2_655 . . . ? 
O3 Nd1 C4 C5 -160.8(17) . . . . ? 
O4 Nd1 C4 C5 47.0(17) 2_655 . . . ? 
O6 Nd1 C4 C5 -94.8(17) 2 . . . ? 
O8 Nd1 C4 C5 -15.8(17) . . . . ? 
O7 Nd1 C4 C5 -175.1(17) . . . . ? 
O5 Nd1 C4 C5 90.7(17) . . . . ? 
O1 Nd1 C4 C5 -33.9(18) . . . . ? 
O6 Nd1 C4 C5 -96.5(17) . . . . ? 
O2 Nd1 C4 C5 53.0(18) . . . . ? 
C1 Nd1 C4 C5 -3.4(18) . . . . ? 
C6 N9 C5 C4 -68.7(6) . . . . ? 
N10 N9 C5 C4 107.6(4) . . . . ? 
O5 C4 C5 N9 -10.2(5) . . . . ? 
O6 C4 C5 N9 170.9(3) . . . . ? 
Nd1 C4 C5 N9 -96.4(17) . . . . ? 
N11 N12 C6 N9 -0.3(6) . . . . ? 
N10 N9 C6 N12 0.7(6) . . . . ? 
C5 N9 C6 N12 177.4(4) . . . . ? 
Nd1 O4 C7 O3 -16.5(6) 2_655 . . . ? 
Nd1 O4 C7 C8 162.7(2) 2_655 . . . ? 
Nd1 O3 C7 O4 -12.8(5) . . . . ? 
Nd1 O3 C7 C8 168.1(2) . . . . ? 
C9 N5 C8 C7 -59.5(5) . . . . ? 
N6 N5 C8 C7 114.6(4) . . . . ? 
O4 C7 C8 N5 -0.3(4) . . . . ? 
O3 C7 C8 N5 179.0(3) . . . . ? 
N7 N8 C9 N5 -0.9(6) . . . . ? 
N6 N5 C9 N8 0.9(5) . . . . ? 
C8 N5 C9 N8 175.6(4) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.823 
_refine_diff_density_min   -0.598 
_refine_diff_density_rms    0.097

data_51023f 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H30 N24 O18 Sm2' 
_chemical_formula_weight          1171.36 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Sm'  'Sm'  -0.1638   3.4418 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    8.8696(12) 
_cell_length_b                    12.0165(17) 
_cell_length_c                    18.542(3) 
_cell_angle_alpha                 92.244(2) 
_cell_angle_beta                  98.968(2) 
_cell_angle_gamma                 101.927(2) 
_cell_volume                      1904.7(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     4519 
_cell_measurement_theta_min       2.13 
_cell_measurement_theta_max       25.37 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             lightyellow 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     2.042 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1148 
_exptl_absorpt_coefficient_mu     3.159 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.584170 
_exptl_absorpt_correction_T_max   1.000000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_standards_decay_%         . 
_diffrn_reflns_number             9654 
_diffrn_reflns_av_R_equivalents   0.0274 
_diffrn_reflns_av_sigmaI/netI     0.0582 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          1.11 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              6673 
_reflns_number_gt                 5096 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     CONSTR 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6673 
_refine_ls_number_parameters      559 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0541 
_refine_ls_R_factor_gt            0.0362 
_refine_ls_wR_factor_ref          0.1038 
_refine_ls_wR_factor_gt           0.0955 
_refine_ls_goodness_of_fit_ref    1.054 
_refine_ls_restrained_S_all       1.054 
_refine_ls_shift/su_max           0.005 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Sm1 Sm 0.74923(4) 1.02352(3) 0.999164(17) 0.01743(11) Uani 1 1 d . . . 
Sm2 Sm 0.65138(4) 0.37725(3) 0.481501(17) 0.01639(11) Uani 1 1 d . . . 
O1 O 0.5028(6) 0.9711(4) 0.9210(3) 0.0335(12) Uani 1 1 d . . . 
O2 O 0.2641(5) 0.9605(5) 0.8664(3) 0.0327(12) Uani 1 1 d . . . 
O3 O 0.6211(5) 0.8399(4) 1.0297(3) 0.0270(11) Uani 1 1 d . . . 
O4 O 0.3620(5) 0.8091(4) 1.0138(3) 0.0293(12) Uani 1 1 d . . . 
O5 O 0.9662(5) 0.9452(4) 1.0583(2) 0.0233(11) Uani 1 1 d . . . 
O6 O 1.1655(5) 0.8810(4) 1.1134(3) 0.0264(11) Uani 1 1 d . . . 
O7 O 0.9402(5) 1.1921(4) 1.0504(3) 0.0303(12) Uani 1 1 d . . . 
H7A H 1.0295 1.2060 1.0374 0.036 Uiso 1 1 d R . . 
H7B H 0.9183 1.2375 1.0815 0.036 Uiso 1 1 d R . . 
O8 O 0.7664(5) 0.8708(4) 0.9077(3) 0.0294(12) Uani 1 1 d . . . 
H8C H 0.8355 0.8314 0.9169 0.035 Uiso 1 1 d R . . 
H8D H 0.7034 0.8581 0.8673 0.035 Uiso 1 1 d R . . 
O9 O 0.5239(5) 0.4466(4) 0.3752(3) 0.0318(12) Uani 1 1 d . . . 
O10 O 0.3480(6) 0.5435(4) 0.4000(3) 0.0313(12) Uani 1 1 d . . . 
O11 O 0.3857(5) 0.3275(4) 0.4958(3) 0.0272(11) Uani 1 1 d . . . 
O12 O 0.2130(5) 0.4277(4) 0.5207(3) 0.0283(11) Uani 1 1 d . . . 
O13 O 0.8326(5) 0.3613(4) 0.4019(3) 0.0348(13) Uani 1 1 d . . . 
O14 O 0.7786(6) 0.2013(4) 0.3305(3) 0.0449(15) Uani 1 1 d . . . 
O15 O 0.9149(5) 0.3983(4) 0.5547(3) 0.0297(12) Uani 1 1 d . . . 
H15A H 0.9642 0.3450 0.5525 0.036 Uiso 1 1 d R . . 
H15B H 0.9561 0.4588 0.5820 0.036 Uiso 1 1 d R . . 
O16 O 0.5439(5) 0.2005(4) 0.4048(3) 0.0316(12) Uani 1 1 d . . . 
H16A H 0.5970 0.1492 0.4041 0.038 Uiso 1 1 d R . . 
H16B H 0.4536 0.1901 0.3788 0.038 Uiso 1 1 d R . . 
O17 O 0.6468(6) 0.2193(4) 0.5600(3) 0.0320(12) Uani 1 1 d . . . 
H17C H 0.7292 0.2140 0.5888 0.038 Uiso 1 1 d R . . 
H17D H 0.5630 0.1693 0.5585 0.038 Uiso 1 1 d R . . 
N1 N 0.3986(7) 1.0686(5) 0.7523(3) 0.0343(15) Uani 1 1 d . . . 
N2 N 0.4521(9) 1.1799(7) 0.7720(4) 0.054(2) Uani 1 1 d . . . 
N3 N 0.3673(10) 1.2331(7) 0.7299(5) 0.059(2) Uani 1 1 d . . . 
N4 N 0.2589(9) 1.1608(7) 0.6840(4) 0.054(2) Uani 1 1 d . . . 
N5 N 0.3411(7) 0.5948(5) 1.0594(4) 0.0323(15) Uani 1 1 d . . . 
N6 N 0.3038(9) 0.4859(6) 1.0352(5) 0.063(2) Uani 1 1 d . . . 
N7 N 0.1687(10) 0.4438(7) 1.0519(6) 0.075(3) Uani 1 1 d . . . 
N8 N 0.1202(9) 0.5237(7) 1.0890(5) 0.067(3) Uani 1 1 d . . . 
N9 N 0.9970(7) 0.7753(5) 1.2124(3) 0.0310(15) Uani 1 1 d . . . 
N10 N 0.9549(8) 0.6640(6) 1.2198(4) 0.0489(19) Uani 1 1 d . . . 
N11 N 1.0482(9) 0.6445(7) 1.2757(4) 0.055(2) Uani 1 1 d . . . 
N12 N 1.1500(9) 0.7380(7) 1.3053(4) 0.053(2) Uani 1 1 d . . . 
N13 N 0.4477(7) 0.4580(5) 0.2313(3) 0.0243(13) Uani 1 1 d . . . 
N14 N 0.3685(8) 0.3572(6) 0.1984(4) 0.0470(19) Uani 1 1 d . . . 
N15 N 0.4610(9) 0.3196(6) 0.1621(4) 0.056(2) Uani 1 1 d . . . 
N16 N 0.6029(9) 0.3949(6) 0.1709(4) 0.055(2) Uani 1 1 d . . . 
N17 N 0.1657(7) 0.1265(5) 0.4853(3) 0.0256(13) Uani 1 1 d . . . 
N18 N 0.0615(8) 0.0592(5) 0.4330(4) 0.0395(17) Uani 1 1 d . . . 
N19 N 0.1200(8) -0.0284(6) 0.4204(4) 0.0455(18) Uani 1 1 d . . . 
N20 N 0.2600(8) -0.0179(5) 0.4633(4) 0.0431(18) Uani 1 1 d . . . 
N21 N 1.0698(7) 0.2555(5) 0.2928(3) 0.0279(14) Uani 1 1 d . . . 
N22 N 1.0284(9) 0.1809(7) 0.2356(4) 0.059(2) Uani 1 1 d . . . 
N23 N 1.1349(8) 0.1176(6) 0.2384(4) 0.0465(19) Uani 1 1 d . . . 
N24 N 1.2402(8) 0.1612(8) 0.2998(5) 0.058(2) Uani 1 1 d . . . 
C1 C 0.4049(8) 0.9702(6) 0.8654(4) 0.0250(16) Uani 1 1 d . . . 
C2 C 0.4634(9) 0.9831(7) 0.7932(4) 0.038(2) Uani 1 1 d . . . 
H2A H 0.5766 1.0055 0.8021 0.046 Uiso 1 1 calc R . . 
H2B H 0.4335 0.9104 0.7644 0.046 Uiso 1 1 calc R . . 
C3 C 0.2808(10) 1.0606(7) 0.6994(4) 0.044(2) Uani 1 1 d . . . 
H3 H 0.2207 0.9923 0.6759 0.053 Uiso 1 1 calc R . . 
C4 C 0.4873(7) 0.7814(5) 1.0293(4) 0.0211(15) Uani 1 1 d . . . 
C5 C 0.4901(8) 0.6636(6) 1.0537(5) 0.039(2) Uani 1 1 d . . . 
H5A H 0.5369 0.6242 1.0194 0.047 Uiso 1 1 calc R . . 
H5B H 0.5569 0.6709 1.1011 0.047 Uiso 1 1 calc R . . 
C6 C 0.2268(10) 0.6146(7) 1.0922(5) 0.048(2) Uani 1 1 d . . . 
H6 H 0.2239 0.6846 1.1145 0.058 Uiso 1 1 calc R . . 
C7 C 1.0266(8) 0.8894(5) 1.1057(3) 0.0195(14) Uani 1 1 d . . . 
C8 C 0.9205(8) 0.8316(7) 1.1539(4) 0.041(2) Uani 1 1 d . . . 
H8A H 0.8729 0.8877 1.1755 0.049 Uiso 1 1 calc R . . 
H8B H 0.8375 0.7754 1.1242 0.049 Uiso 1 1 calc R . . 
C9 C 1.1151(11) 0.8174(8) 1.2642(5) 0.050(2) Uani 1 1 d . . . 
H9 H 1.1671 0.8936 1.2709 0.060 Uiso 1 1 calc R . . 
C10 C 0.4217(8) 0.5007(6) 0.3589(4) 0.0229(15) Uani 1 1 d . . . 
C11 C 0.3780(8) 0.5207(6) 0.2793(4) 0.0251(16) Uani 1 1 d . . . 
H11A H 0.2652 0.4992 0.2655 0.030 Uiso 1 1 calc R . . 
H11B H 0.4099 0.6014 0.2730 0.030 Uiso 1 1 calc R . . 
C12 C 0.5883(9) 0.4772(7) 0.2136(4) 0.042(2) Uani 1 1 d . . . 
H12 H 0.6664 0.5416 0.2298 0.051 Uiso 1 1 calc R . . 
C13 C 0.2550(7) 0.3371(6) 0.5089(3) 0.0215(15) Uani 1 1 d . . . 
C14 C 0.1337(8) 0.2310(5) 0.5145(4) 0.0269(16) Uani 1 1 d . . . 
H14A H 0.1246 0.2236 0.5657 0.032 Uiso 1 1 calc R . . 
H14B H 0.0336 0.2403 0.4889 0.032 Uiso 1 1 calc R . . 
C15 C 0.2833(9) 0.0774(6) 0.5021(4) 0.0318(18) Uani 1 1 d . . . 
H15 H 0.3714 0.1069 0.5370 0.038 Uiso 1 1 calc R . . 
C16 C 0.8573(8) 0.2965(6) 0.3532(4) 0.0278(17) Uani 1 1 d . . . 
C17 C 0.9985(9) 0.3449(6) 0.3183(4) 0.0368(19) Uani 1 1 d . . . 
H17A H 0.9666 0.3874 0.2773 0.044 Uiso 1 1 calc R . . 
H17B H 1.0749 0.3973 0.3538 0.044 Uiso 1 1 calc R . . 
C18 C 1.2032(8) 0.2423(7) 0.3312(4) 0.0294(17) Uani 1 1 d . . . 
H18 H 1.2584 0.2853 0.3735 0.035 Uiso 1 1 calc R . . 
O18 O 0.8877(7) 0.3613(5) 0.1348(3) 0.0560(18) Uani 1 1 d D . . 
H18A H 0.8065 0.3711 0.1529 0.067 Uiso 1 1 d RD . . 
H18B H 0.9550 0.4205 0.1294 0.067 Uiso 1 1 d RD . . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Sm1 0.01545(19) 0.0170(2) 0.0191(2) 0.00282(14) 0.00021(14) 0.00365(14) 
Sm2 0.01342(19) 0.01543(19) 0.0205(2) 0.00083(14) 0.00306(14) 0.00338(14) 
O1 0.032(3) 0.038(3) 0.028(3) 0.007(2) -0.007(2) 0.009(2) 
O2 0.015(3) 0.053(3) 0.027(3) -0.001(2) 0.003(2) 0.002(2) 
O3 0.021(3) 0.022(3) 0.037(3) 0.003(2) 0.005(2) 0.002(2) 
O4 0.015(2) 0.026(3) 0.051(3) 0.007(2) 0.006(2) 0.011(2) 
O5 0.022(2) 0.029(3) 0.021(3) 0.010(2) 0.001(2) 0.011(2) 
O6 0.018(3) 0.031(3) 0.033(3) 0.010(2) 0.006(2) 0.009(2) 
O7 0.021(3) 0.027(3) 0.041(3) -0.007(2) 0.006(2) 0.002(2) 
O8 0.023(3) 0.032(3) 0.031(3) -0.008(2) -0.004(2) 0.010(2) 
O9 0.028(3) 0.043(3) 0.025(3) 0.012(2) 0.002(2) 0.010(2) 
O10 0.038(3) 0.034(3) 0.024(3) -0.006(2) 0.012(2) 0.008(2) 
O11 0.017(2) 0.027(3) 0.040(3) 0.004(2) 0.012(2) 0.003(2) 
O12 0.025(3) 0.013(2) 0.050(3) 0.003(2) 0.015(2) 0.003(2) 
O13 0.026(3) 0.037(3) 0.041(3) -0.011(3) 0.017(2) 0.001(2) 
O14 0.034(3) 0.029(3) 0.067(4) -0.016(3) 0.021(3) -0.009(3) 
O15 0.019(2) 0.034(3) 0.035(3) 0.002(2) -0.005(2) 0.009(2) 
O16 0.024(3) 0.029(3) 0.039(3) -0.008(2) 0.003(2) 0.003(2) 
O17 0.028(3) 0.023(3) 0.041(3) 0.009(2) -0.005(2) 0.003(2) 
N1 0.041(4) 0.036(4) 0.025(3) 0.004(3) 0.010(3) 0.005(3) 
N2 0.047(5) 0.049(5) 0.056(5) -0.004(4) 0.005(4) -0.010(4) 
N3 0.066(6) 0.038(5) 0.066(6) 0.010(4) 0.012(5) -0.002(4) 
N4 0.070(5) 0.045(5) 0.048(5) 0.013(4) 0.005(4) 0.014(4) 
N5 0.028(3) 0.018(3) 0.058(4) 0.011(3) 0.020(3) 0.009(3) 
N6 0.057(5) 0.025(4) 0.111(7) -0.002(4) 0.036(5) 0.003(4) 
N7 0.050(5) 0.031(5) 0.147(9) -0.001(5) 0.037(6) -0.001(4) 
N8 0.043(5) 0.045(5) 0.124(8) 0.030(5) 0.044(5) 0.012(4) 
N9 0.029(3) 0.042(4) 0.025(3) 0.021(3) 0.006(3) 0.009(3) 
N10 0.045(4) 0.037(4) 0.058(5) 0.018(4) -0.002(4) 0.000(3) 
N11 0.056(5) 0.046(5) 0.067(5) 0.038(4) 0.008(4) 0.016(4) 
N12 0.070(5) 0.055(5) 0.036(4) 0.020(4) -0.003(4) 0.026(4) 
N13 0.026(3) 0.023(3) 0.023(3) -0.003(2) 0.011(3) 0.000(3) 
N14 0.038(4) 0.048(4) 0.049(4) -0.023(4) 0.020(3) -0.009(3) 
N15 0.057(5) 0.051(5) 0.061(5) -0.015(4) 0.030(4) 0.002(4) 
N16 0.050(5) 0.047(5) 0.074(6) -0.018(4) 0.043(4) 0.005(4) 
N17 0.028(3) 0.018(3) 0.030(3) 0.002(3) 0.004(3) 0.005(3) 
N18 0.039(4) 0.030(4) 0.041(4) -0.001(3) -0.002(3) -0.005(3) 
N19 0.047(5) 0.032(4) 0.053(5) -0.004(3) 0.005(4) 0.003(3) 
N20 0.047(4) 0.019(4) 0.067(5) 0.005(3) 0.012(4) 0.013(3) 
N21 0.023(3) 0.032(4) 0.025(3) -0.006(3) 0.011(3) -0.005(3) 
N22 0.052(5) 0.057(5) 0.065(5) -0.016(4) 0.020(4) 0.006(4) 
N23 0.040(4) 0.043(4) 0.069(5) -0.003(4) 0.032(4) 0.020(4) 
N24 0.032(4) 0.085(7) 0.061(6) 0.036(5) 0.008(4) 0.014(4) 
C1 0.022(4) 0.028(4) 0.021(4) -0.001(3) -0.003(3) 0.003(3) 
C2 0.031(4) 0.061(6) 0.030(4) 0.004(4) 0.009(4) 0.023(4) 
C3 0.054(6) 0.040(5) 0.033(5) 0.007(4) -0.004(4) 0.005(4) 
C4 0.020(4) 0.015(3) 0.030(4) -0.001(3) 0.006(3) 0.005(3) 
C5 0.025(4) 0.024(4) 0.072(6) 0.012(4) 0.010(4) 0.008(3) 
C6 0.050(5) 0.035(5) 0.067(6) 0.014(4) 0.030(5) 0.007(4) 
C7 0.025(4) 0.017(3) 0.018(3) 0.002(3) 0.007(3) 0.005(3) 
C8 0.017(4) 0.062(6) 0.048(5) 0.033(4) 0.005(3) 0.012(4) 
C9 0.066(6) 0.042(5) 0.040(5) 0.010(4) -0.004(5) 0.015(5) 
C10 0.022(4) 0.020(4) 0.022(4) 0.002(3) -0.003(3) -0.003(3) 
C11 0.023(4) 0.028(4) 0.025(4) 0.000(3) 0.005(3) 0.008(3) 
C12 0.031(4) 0.037(5) 0.050(5) -0.009(4) 0.010(4) -0.013(4) 
C13 0.018(4) 0.025(4) 0.017(3) 0.001(3) -0.003(3) -0.002(3) 
C14 0.016(3) 0.021(4) 0.046(5) 0.003(3) 0.011(3) 0.006(3) 
C15 0.029(4) 0.020(4) 0.049(5) 0.007(3) 0.007(4) 0.011(3) 
C16 0.024(4) 0.038(5) 0.024(4) -0.001(3) 0.008(3) 0.013(3) 
C17 0.036(4) 0.031(4) 0.048(5) -0.002(4) 0.026(4) 0.005(4) 
C18 0.020(4) 0.046(5) 0.017(4) -0.007(3) -0.006(3) 0.003(4) 
O18 0.047(4) 0.033(3) 0.094(5) -0.006(3) 0.042(4) 0.002(3) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Sm1 O1 2.376(5) . ? 
Sm1 O3 2.397(4) . ? 
Sm1 O7 2.409(5) . ? 
Sm1 O4 2.421(5) 2_677 ? 
Sm1 O5 2.441(4) . ? 
Sm1 O8 2.494(5) . ? 
Sm1 O2 2.517(5) 2_677 ? 
Sm1 O6 2.562(4) 2_777 ? 
Sm1 O5 2.851(4) 2_777 ? 
Sm1 O1 2.877(5) 2_677 ? 
Sm1 C1 3.046(7) 2_677 ? 
Sm1 C7 3.055(6) 2_777 ? 
Sm2 O10 2.360(5) 2_666 ? 
Sm2 O11 2.367(4) . ? 
Sm2 O13 2.375(5) . ? 
Sm2 O9 2.383(5) . ? 
Sm2 O12 2.409(4) 2_666 ? 
Sm2 O17 2.434(4) . ? 
Sm2 O16 2.439(5) . ? 
Sm2 O15 2.471(4) . ? 
O1 C1 1.238(8) . ? 
O1 Sm1 2.877(5) 2_677 ? 
O2 C1 1.233(8) . ? 
O2 Sm1 2.517(5) 2_677 ? 
O3 C4 1.246(8) . ? 
O4 C4 1.220(7) . ? 
O4 Sm1 2.421(4) 2_677 ? 
O5 C7 1.248(7) . ? 
O5 Sm1 2.850(4) 2_777 ? 
O6 C7 1.244(8) . ? 
O6 Sm1 2.562(4) 2_777 ? 
O7 H7A 0.8500 . ? 
O7 H7B 0.8499 . ? 
O8 H8C 0.8500 . ? 
O8 H8D 0.8500 . ? 
O9 C10 1.229(8) . ? 
O10 C10 1.239(8) . ? 
O10 Sm2 2.360(5) 2_666 ? 
O11 C13 1.248(8) . ? 
O12 C13 1.243(8) . ? 
O12 Sm2 2.409(4) 2_666 ? 
O13 C16 1.245(8) . ? 
O14 C16 1.230(8) . ? 
O15 H15A 0.8499 . ? 
O15 H15B 0.8500 . ? 
O16 H16A 0.8499 . ? 
O16 H16B 0.8499 . ? 
O17 H17C 0.8500 . ? 
O17 H17D 0.8500 . ? 
N1 C3 1.303(10) . ? 
N1 N2 1.338(9) . ? 
N1 C2 1.459(9) . ? 
N2 N3 1.280(10) . ? 
N3 N4 1.321(10) . ? 
N4 C3 1.294(10) . ? 
N5 C6 1.317(10) . ? 
N5 N6 1.323(9) . ? 
N5 C5 1.428(9) . ? 
N6 N7 1.291(10) . ? 
N7 N8 1.338(11) . ? 
N8 C6 1.281(10) . ? 
N9 C9 1.306(11) . ? 
N9 N10 1.332(8) . ? 
N9 C8 1.453(8) . ? 
N10 N11 1.282(9) . ? 
N11 N12 1.326(10) . ? 
N12 C9 1.300(10) . ? 
N13 C12 1.315(9) . ? 
N13 N14 1.338(8) . ? 
N13 C11 1.433(9) . ? 
N14 N15 1.278(9) . ? 
N15 N16 1.372(9) . ? 
N16 C12 1.282(10) . ? 
N17 C15 1.304(9) . ? 
N17 N18 1.341(8) . ? 
N17 C14 1.447(8) . ? 
N18 N19 1.295(9) . ? 
N19 N20 1.345(9) . ? 
N20 C15 1.290(10) . ? 
N21 N22 1.315(9) . ? 
N21 C18 1.325(9) . ? 
N21 C17 1.453(9) . ? 
N22 N23 1.326(10) . ? 
N23 N24 1.364(10) . ? 
N24 C18 1.243(11) . ? 
C1 C2 1.512(10) . ? 
C1 Sm1 3.046(7) 2_677 ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
C3 H3 0.9300 . ? 
C4 C5 1.507(9) . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.486(9) . ? 
C7 Sm1 3.055(6) 2_777 ? 
C8 H8A 0.9700 . ? 
C8 H8B 0.9700 . ? 
C9 H9 0.9300 . ? 
C10 C11 1.507(9) . ? 
C11 H11A 0.9700 . ? 
C11 H11B 0.9700 . ? 
C12 H12 0.9300 . ? 
C13 C14 1.508(9) . ? 
C14 H14A 0.9700 . ? 
C14 H14B 0.9700 . ? 
C15 H15 0.9300 . ? 
C16 C17 1.519(9) . ? 
C17 H17A 0.9700 . ? 
C17 H17B 0.9700 . ? 
C18 H18 0.9300 . ? 
O18 H18A 0.8664 . ? 
O18 H18B 0.8498 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1 Sm1 O3 72.29(16) . . ? 
O1 Sm1 O7 139.83(17) . . ? 
O3 Sm1 O7 142.04(16) . . ? 
O1 Sm1 O4 71.54(17) . 2_677 ? 
O3 Sm1 O4 126.51(15) . 2_677 ? 
O7 Sm1 O4 69.55(16) . 2_677 ? 
O1 Sm1 O5 142.38(17) . . ? 
O3 Sm1 O5 77.11(15) . . ? 
O7 Sm1 O5 77.30(16) . . ? 
O4 Sm1 O5 146.00(16) 2_677 . ? 
O1 Sm1 O8 72.50(17) . . ? 
O3 Sm1 O8 69.08(16) . . ? 
O7 Sm1 O8 130.02(16) . . ? 
O4 Sm1 O8 131.63(16) 2_677 . ? 
O5 Sm1 O8 76.52(15) . . ? 
O1 Sm1 O2 114.83(16) . 2_677 ? 
O3 Sm1 O2 72.86(16) . 2_677 ? 
O7 Sm1 O2 73.77(16) . 2_677 ? 
O4 Sm1 O2 88.35(17) 2_677 2_677 ? 
O5 Sm1 O2 75.08(16) . 2_677 ? 
O8 Sm1 O2 136.45(17) . 2_677 ? 
O1 Sm1 O6 83.02(16) . 2_777 ? 
O3 Sm1 O6 138.53(16) . 2_777 ? 
O7 Sm1 O6 76.27(16) . 2_777 ? 
O4 Sm1 O6 72.50(16) 2_677 2_777 ? 
O5 Sm1 O6 107.20(14) . 2_777 ? 
O8 Sm1 O6 71.99(16) . 2_777 ? 
O2 Sm1 O6 148.61(16) 2_677 2_777 ? 
O1 Sm1 O5 121.20(15) . 2_777 ? 
O3 Sm1 O5 121.54(14) . 2_777 ? 
O7 Sm1 O5 65.82(15) . 2_777 ? 
O4 Sm1 O5 110.65(14) 2_677 2_777 ? 
O5 Sm1 O5 59.70(16) . 2_777 ? 
O8 Sm1 O5 64.24(14) . 2_777 ? 
O2 Sm1 O5 123.92(14) 2_677 2_777 ? 
O6 Sm1 O5 47.53(13) 2_777 2_777 ? 
O1 Sm1 O1 68.76(18) . 2_677 ? 
O3 Sm1 O1 65.87(15) . 2_677 ? 
O7 Sm1 O1 102.63(15) . 2_677 ? 
O4 Sm1 O1 64.95(15) 2_677 2_677 ? 
O5 Sm1 O1 117.19(14) . 2_677 ? 
O8 Sm1 O1 127.17(15) . 2_677 ? 
O2 Sm1 O1 47.00(14) 2_677 2_677 ? 
O6 Sm1 O1 134.32(14) 2_777 2_677 ? 
O5 Sm1 O1 168.24(14) 2_777 2_677 ? 
O1 Sm1 C1 91.83(18) . 2_677 ? 
O3 Sm1 C1 65.88(17) . 2_677 ? 
O7 Sm1 C1 89.16(17) . 2_677 ? 
O4 Sm1 C1 77.32(17) 2_677 2_677 ? 
O5 Sm1 C1 95.21(16) . 2_677 ? 
O8 Sm1 C1 134.91(17) . 2_677 ? 
O2 Sm1 C1 23.21(16) 2_677 2_677 ? 
O6 Sm1 C1 149.47(17) 2_777 2_677 ? 
O5 Sm1 C1 146.97(15) 2_777 2_677 ? 
O1 Sm1 C1 23.91(15) 2_677 2_677 ? 
O1 Sm1 C7 103.19(17) . 2_777 ? 
O3 Sm1 C7 135.57(17) . 2_777 ? 
O7 Sm1 C7 67.84(17) . 2_777 ? 
O4 Sm1 C7 90.50(17) 2_677 2_777 ? 
O5 Sm1 C7 83.77(16) . 2_777 ? 
O8 Sm1 C7 67.60(17) . 2_777 ? 
O2 Sm1 C7 139.33(17) 2_677 2_777 ? 
O6 Sm1 C7 23.55(15) 2_777 2_777 ? 
O5 Sm1 C7 24.08(14) 2_777 2_777 ? 
O1 Sm1 C7 155.40(16) 2_677 2_777 ? 
C1 Sm1 C7 156.69(18) 2_677 2_777 ? 
O10 Sm2 O11 76.40(17) 2_666 . ? 
O10 Sm2 O13 138.70(17) 2_666 . ? 
O11 Sm2 O13 144.88(17) . . ? 
O10 Sm2 O9 121.43(17) 2_666 . ? 
O11 Sm2 O9 77.97(16) . . ? 
O13 Sm2 O9 81.09(17) . . ? 
O10 Sm2 O12 76.81(17) 2_666 2_666 ? 
O11 Sm2 O12 122.32(15) . 2_666 ? 
O13 Sm2 O12 77.51(16) . 2_666 ? 
O9 Sm2 O12 74.24(17) . 2_666 ? 
O10 Sm2 O17 74.65(17) 2_666 . ? 
O11 Sm2 O17 77.18(16) . . ? 
O13 Sm2 O17 107.01(17) . . ? 
O9 Sm2 O17 145.65(16) . . ? 
O12 Sm2 O17 139.79(16) 2_666 . ? 
O10 Sm2 O16 139.90(16) 2_666 . ? 
O11 Sm2 O16 75.01(16) . . ? 
O13 Sm2 O16 73.50(16) . . ? 
O9 Sm2 O16 78.90(17) . . ? 
O12 Sm2 O16 142.96(16) 2_666 . ? 
O17 Sm2 O16 72.02(16) . . ? 
O10 Sm2 O15 70.96(17) 2_666 . ? 
O11 Sm2 O15 139.58(16) . . ? 
O13 Sm2 O15 70.74(17) . . ? 
O9 Sm2 O15 140.08(16) . . ? 
O12 Sm2 O15 72.50(16) 2_666 . ? 
O17 Sm2 O15 71.76(16) . . ? 
O16 Sm2 O15 117.40(16) . . ? 
C1 O1 Sm1 157.0(5) . . ? 
C1 O1 Sm1 85.7(4) . 2_677 ? 
Sm1 O1 Sm1 111.23(18) . 2_677 ? 
C1 O2 Sm1 103.3(4) . 2_677 ? 
C4 O3 Sm1 140.5(4) . . ? 
C4 O4 Sm1 141.2(4) . 2_677 ? 
C7 O5 Sm1 152.5(4) . . ? 
C7 O5 Sm1 87.2(4) . 2_777 ? 
Sm1 O5 Sm1 120.30(16) . 2_777 ? 
C7 O6 Sm1 101.1(4) . 2_777 ? 
Sm1 O7 H7A 119.9 . . ? 
Sm1 O7 H7B 120.1 . . ? 
H7A O7 H7B 120.0 . . ? 
Sm1 O8 H8C 119.9 . . ? 
Sm1 O8 H8D 120.1 . . ? 
H8C O8 H8D 120.0 . . ? 
C10 O9 Sm2 138.7(5) . . ? 
C10 O10 Sm2 146.5(5) . 2_666 ? 
C13 O11 Sm2 160.3(4) . . ? 
C13 O12 Sm2 130.4(4) . 2_666 ? 
C16 O13 Sm2 142.0(5) . . ? 
Sm2 O15 H15A 120.0 . . ? 
Sm2 O15 H15B 120.0 . . ? 
H15A O15 H15B 120.0 . . ? 
Sm2 O16 H16A 119.8 . . ? 
Sm2 O16 H16B 120.2 . . ? 
H16A O16 H16B 120.0 . . ? 
Sm2 O17 H17C 120.0 . . ? 
Sm2 O17 H17D 120.0 . . ? 
H17C O17 H17D 120.0 . . ? 
C3 N1 N2 106.6(7) . . ? 
C3 N1 C2 132.4(7) . . ? 
N2 N1 C2 120.7(7) . . ? 
N3 N2 N1 106.7(7) . . ? 
N2 N3 N4 110.8(7) . . ? 
C3 N4 N3 105.3(8) . . ? 
C6 N5 N6 107.0(7) . . ? 
C6 N5 C5 132.0(7) . . ? 
N6 N5 C5 120.6(7) . . ? 
N7 N6 N5 107.0(7) . . ? 
N6 N7 N8 109.8(7) . . ? 
C6 N8 N7 105.7(7) . . ? 
C9 N9 N10 107.6(6) . . ? 
C9 N9 C8 129.7(7) . . ? 
N10 N9 C8 122.7(7) . . ? 
N11 N10 N9 105.5(7) . . ? 
N10 N11 N12 112.4(7) . . ? 
C9 N12 N11 104.0(7) . . ? 
C12 N13 N14 107.8(6) . . ? 
C12 N13 C11 131.8(6) . . ? 
N14 N13 C11 120.3(6) . . ? 
N15 N14 N13 106.4(6) . . ? 
N14 N15 N16 110.5(7) . . ? 
C12 N16 N15 104.6(7) . . ? 
C15 N17 N18 107.9(6) . . ? 
C15 N17 C14 131.5(6) . . ? 
N18 N17 C14 120.5(6) . . ? 
N19 N18 N17 106.1(6) . . ? 
N18 N19 N20 110.1(7) . . ? 
C15 N20 N19 105.7(6) . . ? 
N22 N21 C18 109.6(7) . . ? 
N22 N21 C17 132.2(7) . . ? 
C18 N21 C17 118.2(7) . . ? 
N21 N22 N23 107.6(7) . . ? 
N22 N23 N24 104.3(7) . . ? 
C18 N24 N23 111.9(7) . . ? 
O2 C1 O1 123.5(7) . . ? 
O2 C1 C2 119.0(6) . . ? 
O1 C1 C2 117.5(6) . . ? 
O2 C1 Sm1 53.5(3) . 2_677 ? 
O1 C1 Sm1 70.4(4) . 2_677 ? 
C2 C1 Sm1 169.2(5) . 2_677 ? 
N1 C2 C1 110.8(6) . . ? 
N1 C2 H2A 109.5 . . ? 
C1 C2 H2A 109.5 . . ? 
N1 C2 H2B 109.5 . . ? 
C1 C2 H2B 109.5 . . ? 
H2A C2 H2B 108.1 . . ? 
N4 C3 N1 110.6(8) . . ? 
N4 C3 H3 124.7 . . ? 
N1 C3 H3 124.7 . . ? 
O4 C4 O3 128.5(6) . . ? 
O4 C4 C5 119.2(6) . . ? 
O3 C4 C5 112.4(6) . . ? 
N5 C5 C4 115.2(6) . . ? 
N5 C5 H5A 108.5 . . ? 
C4 C5 H5A 108.5 . . ? 
N5 C5 H5B 108.5 . . ? 
C4 C5 H5B 108.5 . . ? 
H5A C5 H5B 107.5 . . ? 
N8 C6 N5 110.4(8) . . ? 
N8 C6 H6 124.8 . . ? 
N5 C6 H6 124.8 . . ? 
O6 C7 O5 123.7(6) . . ? 
O6 C7 C8 120.8(6) . . ? 
O5 C7 C8 115.4(6) . . ? 
O6 C7 Sm1 55.4(3) . 2_777 ? 
O5 C7 Sm1 68.7(3) . 2_777 ? 
C8 C7 Sm1 172.3(5) . 2_777 ? 
N9 C8 C7 114.2(6) . . ? 
N9 C8 H8A 108.7 . . ? 
C7 C8 H8A 108.7 . . ? 
N9 C8 H8B 108.7 . . ? 
C7 C8 H8B 108.7 . . ? 
H8A C8 H8B 107.6 . . ? 
N12 C9 N9 110.6(8) . . ? 
N12 C9 H9 124.7 . . ? 
N9 C9 H9 124.7 . . ? 
O9 C10 O10 128.3(6) . . ? 
O9 C10 C11 117.9(6) . . ? 
O10 C10 C11 113.8(6) . . ? 
N13 C11 C10 113.3(6) . . ? 
N13 C11 H11A 108.9 . . ? 
C10 C11 H11A 108.9 . . ? 
N13 C11 H11B 108.9 . . ? 
C10 C11 H11B 108.9 . . ? 
H11A C11 H11B 107.7 . . ? 
N16 C12 N13 110.7(7) . . ? 
N16 C12 H12 124.7 . . ? 
N13 C12 H12 124.7 . . ? 
O12 C13 O11 126.5(6) . . ? 
O12 C13 C14 114.3(6) . . ? 
O11 C13 C14 119.1(6) . . ? 
N17 C14 C13 114.9(6) . . ? 
N17 C14 H14A 108.6 . . ? 
C13 C14 H14A 108.6 . . ? 
N17 C14 H14B 108.6 . . ? 
C13 C14 H14B 108.6 . . ? 
H14A C14 H14B 107.5 . . ? 
N20 C15 N17 110.2(7) . . ? 
N20 C15 H15 124.9 . . ? 
N17 C15 H15 124.9 . . ? 
O14 C16 O13 126.9(7) . . ? 
O14 C16 C17 118.7(6) . . ? 
O13 C16 C17 114.4(7) . . ? 
N21 C17 C16 111.7(6) . . ? 
N21 C17 H17A 109.3 . . ? 
C16 C17 H17A 109.3 . . ? 
N21 C17 H17B 109.3 . . ? 
C16 C17 H17B 109.3 . . ? 
H17A C17 H17B 107.9 . . ? 
N24 C18 N21 106.7(7) . . ? 
N24 C18 H18 126.7 . . ? 
N21 C18 H18 126.7 . . ? 
H18A O18 H18B 117.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O3 Sm1 O1 C1 -154.4(13) . . . . ? 
O7 Sm1 O1 C1 50.8(14) . . . . ? 
O4 Sm1 O1 C1 65.7(13) 2_677 . . . ? 
O5 Sm1 O1 C1 -117.3(12) . . . . ? 
O8 Sm1 O1 C1 -81.4(13) . . . . ? 
O2 Sm1 O1 C1 144.9(13) 2_677 . . . ? 
O6 Sm1 O1 C1 -8.1(13) 2_777 . . . ? 
O5 Sm1 O1 C1 -37.7(13) 2_777 . . . ? 
O1 Sm1 O1 C1 135.3(14) 2_677 . . . ? 
C1 Sm1 O1 C1 141.7(12) 2_677 . . . ? 
C7 Sm1 O1 C1 -20.3(13) 2_777 . . . ? 
O3 Sm1 O1 Sm1 70.34(18) . . . 2_677 ? 
O7 Sm1 O1 Sm1 -84.5(3) . . . 2_677 ? 
O4 Sm1 O1 Sm1 -69.57(19) 2_677 . . 2_677 ? 
O5 Sm1 O1 Sm1 107.4(3) . . . 2_677 ? 
O8 Sm1 O1 Sm1 143.3(2) . . . 2_677 ? 
O2 Sm1 O1 Sm1 9.6(2) 2_677 . . 2_677 ? 
O6 Sm1 O1 Sm1 -143.4(2) 2_777 . . 2_677 ? 
O5 Sm1 O1 Sm1 -173.01(13) 2_777 . . 2_677 ? 
O1 Sm1 O1 Sm1 0.0 2_677 . . 2_677 ? 
C1 Sm1 O1 Sm1 6.4(2) 2_677 . . 2_677 ? 
C7 Sm1 O1 Sm1 -155.62(18) 2_777 . . 2_677 ? 
O1 Sm1 O3 C4 -29.0(7) . . . . ? 
O7 Sm1 O3 C4 124.5(7) . . . . ? 
O4 Sm1 O3 C4 20.5(8) 2_677 . . . ? 
O5 Sm1 O3 C4 173.2(7) . . . . ? 
O8 Sm1 O3 C4 -106.5(7) . . . . ? 
O2 Sm1 O3 C4 95.1(7) 2_677 . . . ? 
O6 Sm1 O3 C4 -85.3(7) 2_777 . . . ? 
O5 Sm1 O3 C4 -145.2(7) 2_777 . . . ? 
O1 Sm1 O3 C4 45.2(7) 2_677 . . . ? 
C1 Sm1 O3 C4 71.4(7) 2_677 . . . ? 
C7 Sm1 O3 C4 -119.9(7) 2_777 . . . ? 
O1 Sm1 O5 C7 -73.9(10) . . . . ? 
O3 Sm1 O5 C7 -37.9(9) . . . . ? 
O7 Sm1 O5 C7 113.9(10) . . . . ? 
O4 Sm1 O5 C7 100.9(10) 2_677 . . . ? 
O8 Sm1 O5 C7 -109.1(10) . . . . ? 
O2 Sm1 O5 C7 37.6(9) 2_677 . . . ? 
O6 Sm1 O5 C7 -175.1(9) 2_777 . . . ? 
O5 Sm1 O5 C7 -176.9(11) 2_777 . . . ? 
O1 Sm1 O5 C7 16.0(10) 2_677 . . . ? 
C1 Sm1 O5 C7 25.9(10) 2_677 . . . ? 
C7 Sm1 O5 C7 -177.5(9) 2_777 . . . ? 
O1 Sm1 O5 Sm1 103.0(3) . . . 2_777 ? 
O3 Sm1 O5 Sm1 139.0(2) . . . 2_777 ? 
O7 Sm1 O5 Sm1 -69.2(2) . . . 2_777 ? 
O4 Sm1 O5 Sm1 -82.2(3) 2_677 . . 2_777 ? 
O8 Sm1 O5 Sm1 67.8(2) . . . 2_777 ? 
O2 Sm1 O5 Sm1 -145.5(2) 2_677 . . 2_777 ? 
O6 Sm1 O5 Sm1 1.8(2) 2_777 . . 2_777 ? 
O5 Sm1 O5 Sm1 0.0 2_777 . . 2_777 ? 
O1 Sm1 O5 Sm1 -167.05(16) 2_677 . . 2_777 ? 
C1 Sm1 O5 Sm1 -157.2(2) 2_677 . . 2_777 ? 
C7 Sm1 O5 Sm1 -0.6(2) 2_777 . . 2_777 ? 
O10 Sm2 O9 C10 -20.6(7) 2_666 . . . ? 
O11 Sm2 O9 C10 45.0(7) . . . . ? 
O13 Sm2 O9 C10 -163.3(7) . . . . ? 
O12 Sm2 O9 C10 -83.9(7) 2_666 . . . ? 
O17 Sm2 O9 C10 89.5(7) . . . . ? 
O16 Sm2 O9 C10 121.9(7) . . . . ? 
O15 Sm2 O9 C10 -118.4(6) . . . . ? 
O10 Sm2 O11 C13 52.2(13) 2_666 . . . ? 
O13 Sm2 O11 C13 -129.4(12) . . . . ? 
O9 Sm2 O11 C13 -74.7(13) . . . . ? 
O12 Sm2 O11 C13 -12.3(14) 2_666 . . . ? 
O17 Sm2 O11 C13 129.2(13) . . . . ? 
O16 Sm2 O11 C13 -156.3(13) . . . . ? 
O15 Sm2 O11 C13 88.9(13) . . . . ? 
O10 Sm2 O13 C16 147.4(7) 2_666 . . . ? 
O11 Sm2 O13 C16 -30.4(9) . . . . ? 
O9 Sm2 O13 C16 -84.2(8) . . . . ? 
O12 Sm2 O13 C16 -159.9(8) 2_666 . . . ? 
O17 Sm2 O13 C16 61.4(8) . . . . ? 
O16 Sm2 O13 C16 -3.3(8) . . . . ? 
O15 Sm2 O13 C16 124.5(8) . . . . ? 
C3 N1 N2 N3 -1.1(9) . . . . ? 
C2 N1 N2 N3 -175.7(7) . . . . ? 
N1 N2 N3 N4 0.8(10) . . . . ? 
N2 N3 N4 C3 -0.2(11) . . . . ? 
C6 N5 N6 N7 1.6(11) . . . . ? 
C5 N5 N6 N7 175.6(8) . . . . ? 
N5 N6 N7 N8 -2.0(12) . . . . ? 
N6 N7 N8 C6 1.7(12) . . . . ? 
C9 N9 N10 N11 0.4(9) . . . . ? 
C8 N9 N10 N11 179.0(7) . . . . ? 
N9 N10 N11 N12 -0.1(10) . . . . ? 
N10 N11 N12 C9 -0.3(11) . . . . ? 
C12 N13 N14 N15 -0.5(9) . . . . ? 
C11 N13 N14 N15 -177.2(7) . . . . ? 
N13 N14 N15 N16 0.3(10) . . . . ? 
N14 N15 N16 C12 0.0(11) . . . . ? 
C15 N17 N18 N19 0.3(8) . . . . ? 
C14 N17 N18 N19 -177.6(6) . . . . ? 
N17 N18 N19 N20 -0.4(8) . . . . ? 
N18 N19 N20 C15 0.4(9) . . . . ? 
C18 N21 N22 N23 1.3(9) . . . . ? 
C17 N21 N22 N23 -179.5(7) . . . . ? 
N21 N22 N23 N24 -0.7(9) . . . . ? 
N22 N23 N24 C18 -0.2(9) . . . . ? 
Sm1 O2 C1 O1 8.5(8) 2_677 . . . ? 
Sm1 O2 C1 C2 -170.7(6) 2_677 . . . ? 
Sm1 O1 C1 O2 -146.1(9) . . . . ? 
Sm1 O1 C1 O2 -7.3(7) 2_677 . . . ? 
Sm1 O1 C1 C2 33.1(17) . . . . ? 
Sm1 O1 C1 C2 171.9(6) 2_677 . . . ? 
Sm1 O1 C1 Sm1 -138.9(13) . . . 2_677 ? 
C3 N1 C2 C1 -98.1(10) . . . . ? 
N2 N1 C2 C1 74.9(9) . . . . ? 
O2 C1 C2 N1 47.3(10) . . . . ? 
O1 C1 C2 N1 -131.9(7) . . . . ? 
Sm1 C1 C2 N1 3(3) 2_677 . . . ? 
N3 N4 C3 N1 -0.5(10) . . . . ? 
N2 N1 C3 N4 1.0(10) . . . . ? 
C2 N1 C3 N4 174.8(8) . . . . ? 
Sm1 O4 C4 O3 -18.2(13) 2_677 . . . ? 
Sm1 O4 C4 C5 159.7(6) 2_677 . . . ? 
Sm1 O3 C4 O4 -5.1(13) . . . . ? 
Sm1 O3 C4 C5 176.9(5) . . . . ? 
C6 N5 C5 C4 -50.3(12) . . . . ? 
N6 N5 C5 C4 137.3(8) . . . . ? 
O4 C4 C5 N5 -2.5(11) . . . . ? 
O3 C4 C5 N5 175.8(7) . . . . ? 
N7 N8 C6 N5 -0.7(11) . . . . ? 
N6 N5 C6 N8 -0.6(11) . . . . ? 
C5 N5 C6 N8 -173.7(8) . . . . ? 
Sm1 O6 C7 O5 -7.9(7) 2_777 . . . ? 
Sm1 O6 C7 C8 172.1(6) 2_777 . . . ? 
Sm1 O5 C7 O6 -175.7(6) . . . . ? 
Sm1 O5 C7 O6 7.0(7) 2_777 . . . ? 
Sm1 O5 C7 C8 4.3(13) . . . . ? 
Sm1 O5 C7 C8 -173.0(6) 2_777 . . . ? 
Sm1 O5 C7 Sm1 177.3(9) . . . 2_777 ? 
C9 N9 C8 C7 57.5(12) . . . . ? 
N10 N9 C8 C7 -120.7(8) . . . . ? 
O6 C7 C8 N9 4.9(11) . . . . ? 
O5 C7 C8 N9 -175.1(7) . . . . ? 
Sm1 C7 C8 N9 63(4) 2_777 . . . ? 
N11 N12 C9 N9 0.6(11) . . . . ? 
N10 N9 C9 N12 -0.6(10) . . . . ? 
C8 N9 C9 N12 -179.0(8) . . . . ? 
Sm2 O9 C10 O10 2.4(12) . . . . ? 
Sm2 O9 C10 C11 -178.2(4) . . . . ? 
Sm2 O10 C10 O9 28.2(13) 2_666 . . . ? 
Sm2 O10 C10 C11 -151.2(6) 2_666 . . . ? 
C12 N13 C11 C10 -80.3(10) . . . . ? 
N14 N13 C11 C10 95.5(8) . . . . ? 
O9 C10 C11 N13 8.7(9) . . . . ? 
O10 C10 C11 N13 -171.9(6) . . . . ? 
N15 N16 C12 N13 -0.3(10) . . . . ? 
N14 N13 C12 N16 0.5(10) . . . . ? 
C11 N13 C12 N16 176.7(7) . . . . ? 
Sm2 O12 C13 O11 3.5(10) 2_666 . . . ? 
Sm2 O12 C13 C14 -179.0(4) 2_666 . . . ? 
Sm2 O11 C13 O12 7.9(18) . . . . ? 
Sm2 O11 C13 C14 -169.5(10) . . . . ? 
C15 N17 C14 C13 58.9(10) . . . . ? 
N18 N17 C14 C13 -123.7(7) . . . . ? 
O12 C13 C14 N17 166.7(6) . . . . ? 
O11 C13 C14 N17 -15.6(9) . . . . ? 
N19 N20 C15 N17 -0.2(9) . . . . ? 
N18 N17 C15 N20 -0.1(9) . . . . ? 
C14 N17 C15 N20 177.5(7) . . . . ? 
Sm2 O13 C16 O14 -3.2(14) . . . . ? 
Sm2 O13 C16 C17 175.2(5) . . . . ? 
N22 N21 C17 C16 75.5(10) . . . . ? 
C18 N21 C17 C16 -105.3(8) . . . . ? 
O14 C16 C17 N21 -31.1(10) . . . . ? 
O13 C16 C17 N21 150.3(7) . . . . ? 
N23 N24 C18 N21 1.0(9) . . . . ? 
N22 N21 C18 N24 -1.4(9) . . . . ? 
C17 N21 C18 N24 179.3(6) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.823 
_refine_diff_density_min   -1.282 
_refine_diff_density_rms    0.165