######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 02-05-18 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_at76 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H12 Cu1 N4 O6 S2' _chemical_formula_moiety ? _chemical_formula_weight 507.99 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 8.2400(7) _cell_length_b 11.5350(10) _cell_length_c 20.719(2) _cell_angle_alpha 90.00000 _cell_angle_beta 94.356(2) _cell_angle_gamma 90.00000 _cell_volume 1963.6(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.3 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.371 _exptl_crystal_description prism _exptl_crystal_size_max .36 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .17 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_violet _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .73 _exptl_absorpt_correction_T_max .93 _diffrn_reflns_number 40357 _reflns_number_total 10287 _reflns_Friedel_coverage 0 _reflns_number_gt 7354 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.58 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .035 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_number_reflns 7354 _refine_ls_number_parameters 328 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .006 _refine_diff_density_min -.651 _refine_diff_density_max .712 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 48 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 8 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .35680(2) .304950(10) .069230(10) .01887(7) Uani ? ? 1.00000 ? ? S1 .66843(4) .15996(4) -.08314(2) .02553(15) Uani ? ? 1.00000 ? ? C2 .48771(16) .18661(12) -.05017(7) .0201(5) Uani ? ? 1.00000 ? ? C21 .33073(16) .15126(12) -.08366(6) .0210(6) Uani ? ? 1.00000 ? ? C22 .22995(18) .07512(14) -.05322(7) .0252(6) Uani ? ? 1.00000 ? ? C23 .08471(19) .03864(15) -.08532(7) .0285(7) Uani ? ? 1.00000 ? ? C24 .03863(19) .07992(15) -.14695(8) .0283(7) Uani ? ? 1.00000 ? ? C25 .1384(2) .15669(16) -.17694(8) .0318(7) Uani ? ? 1.00000 ? ? C26 .28526(19) .19185(14) -.14574(7) .0271(7) Uani ? ? 1.00000 ? ? N3 .50649(13) .23772(10) .00670(6) .0194(5) Uani ? ? 1.00000 ? ? C4 .66980(16) .25729(12) .02568(7) .0199(5) Uani ? ? 1.00000 ? ? C5 .77479(17) .22084(13) -.01751(7) .0239(6) Uani ? ? 1.00000 ? ? S1' .80356(4) .44473(3) .18082(2) .02432(15) Uani ? ? 1.00000 ? ? C2' .59741(16) .43444(12) .16135(7) .0202(5) Uani ? ? 1.00000 ? ? C21' .47743(16) .50133(12) .19443(7) .0211(6) Uani ? ? 1.00000 ? ? C22' .33977(18) .54575(13) .15937(8) .0260(6) Uani ? ? 1.00000 ? ? C23' .2251(2) .60782(15) .19084(9) .0312(7) Uani ? ? 1.00000 ? ? C24' .2482(2) .62724(15) .25702(9) .0334(8) Uani ? ? 1.00000 ? ? C25' .3860(2) .58502(16) .29193(8) .0325(8) Uani ? ? 1.00000 ? ? C26' .50041(19) .52224(15) .26101(7) .0266(6) Uani ? ? 1.00000 ? ? N3' .56205(13) .36580(10) .11136(5) .0188(5) Uani ? ? 1.00000 ? ? C4' .70041(16) .32167(11) .08569(7) .0195(5) Uani ? ? 1.00000 ? ? C5' .84235(17) .35348(13) .11867(7) .0228(6) Uani ? ? 1.00000 ? ? N1 .21889(14) .18950(11) .15743(6) .0219(5) Uani ? ? 1.00000 ? ? O11 .24051(13) .29855(9) .15018(5) .0247(5) Uani ? ? 1.00000 ? ? O12 .27155(14) .12183(10) .11668(5) .0285(5) Uani ? ? 1.00000 ? ? O13 .14753(16) .15428(12) .20374(6) .0366(6) Uani ? ? 1.00000 ? ? N2 .15085(15) .39386(12) -.01853(7) .0286(6) Uani ? ? 1.00000 ? ? O21 .14745(12) .30173(9) .01736(5) .0237(4) Uani ? ? 1.00000 ? ? O22 .27488(16) .45514(12) -.01087(8) .0467(7) Uani ? ? 1.00000 ? ? O23 .03441(16) .41462(13) -.05694(7) .0447(7) Uani ? ? 1.00000 ? ? H22 .263(2) .0472(17) -.0084(9) .028(5) Uiso ? ? 1.00000 ? ? H23 .018(2) -.0161(18) -.0628(9) .029(5) Uiso ? ? 1.00000 ? ? H24 -.058(2) .0557(17) -.1654(9) .028(5) Uiso ? ? 1.00000 ? ? H25 .117(3) .183(2) -.2166(11) .042(6) Uiso ? ? 1.00000 ? ? H26 .353(3) .2394(18) -.1679(10) .042(6) Uiso ? ? 1.00000 ? ? H5 .889(3) .2299(19) -.0170(10) .039(6) Uiso ? ? 1.00000 ? ? H22' .325(2) .5326(17) .1142(9) .025(5) Uiso ? ? 1.00000 ? ? H23' .131(3) .6411(18) .1672(10) .033(5) Uiso ? ? 1.00000 ? ? H24' .182(3) .667(2) .2790(11) .046(6) Uiso ? ? 1.00000 ? ? H25' .410(3) .600(2) .3333(12) .052(7) Uiso ? ? 1.00000 ? ? H26' .593(3) .488(2) .2832(10) .046(6) Uiso ? ? 1.00000 ? ? H5' .948(2) .3388(16) .1070(9) .022(4) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu .01313(7) .02236(8) .02105(8) -.00085(6) .00092(5) -.00096(6) S1 .02112(15) .02847(17) .02777(16) -.00178(13) .00688(12) -.00583(13) C2 .0185(5) .0205(6) .0214(6) -.0010(4) .0031(4) .0002(5) C21 .0199(6) .0209(6) .0222(6) -.0019(5) .0021(4) -.0024(5) C22 .0240(6) .0308(7) .0205(6) -.0052(5) .0007(5) .0006(5) C23 .0239(7) .0343(8) .0273(7) -.0090(6) .0020(5) -.0034(6) C24 .0229(7) .0325(8) .0286(7) -.0014(6) -.0030(5) -.0063(6) C25 .0337(8) .0356(8) .0249(7) -.0001(7) -.0049(6) .0034(6) C26 .0285(7) .0282(7) .0243(6) -.0032(6) .0008(5) .0034(5) N3 .0155(5) .0202(5) .0225(5) -.0014(4) .0013(4) -.0008(4) C4 .0155(5) .0198(6) .0244(6) -.0011(4) .0019(4) .0003(5) C5 .0173(6) .0253(7) .0295(7) -.0018(5) .0040(5) -.0033(5) S1' .01770(14) .02976(18) .02483(16) -.00264(12) -.00283(11) -.00235(13) C2' .0176(5) .0215(6) .0213(6) -.0015(4) -.0008(4) .0012(5) C21' .0193(6) .0204(6) .0237(6) -.0025(5) .0018(4) -.0023(5) C22' .0254(7) .0233(7) .0289(7) .0022(5) -.0010(5) -.0018(5) C23' .0260(7) .0260(7) .0414(9) .0046(6) .0015(6) -.0030(6) C24' .0296(8) .0284(8) .0435(9) -.0010(6) .0116(7) -.0077(7) C25' .0336(8) .0370(9) .0278(7) -.0042(7) .0080(6) -.0078(6) C26' .0249(7) .0304(7) .0245(6) -.0032(6) .0020(5) -.0034(5) N3' .0154(5) .0195(5) .0214(5) -.0007(4) .0009(4) .0001(4) C4' .0152(5) .0200(6) .0232(6) .0002(4) .0009(4) .0012(4) C5' .0164(5) .0255(7) .0262(6) -.0004(5) -.0002(5) .0004(5) N1 .0170(5) .0271(6) .0218(5) -.0008(4) .0024(4) -.0018(4) O11 .0235(5) .0214(5) .0299(5) -.0028(4) .0065(4) -.0026(4) O12 .0349(6) .0251(5) .0259(5) .0025(4) .0059(4) -.0028(4) O13 .0417(7) .0363(6) .0340(6) -.0089(5) .0173(5) .0008(5) N2 .0216(6) .0298(7) .0334(7) -.0022(5) -.0045(5) .0086(5) O21 .0176(4) .0250(5) .0283(5) -.0007(4) -.0006(3) .0055(4) O22 .0292(6) .0386(7) .0690(9) -.0139(5) -.0173(6) .0251(7) O23 .0290(6) .0537(8) .0486(8) -.0067(6) -.0168(5) .0230(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N3 . . 2.0109(12) ? Cu N3' . . 1.9725(11) ? Cu O11 . . 1.9954(11) ? Cu O12 . . 2.4549(12) ? Cu O21 . . 1.9623(10) ? Cu O22 . . 2.4578(15) ? S1 C2 . . 1.7127(14) ? S1 C5 . . 1.7115(15) ? C2 C21 . . 1.4781(19) ? C2 N3 . . 1.3162(18) ? C21 C22 . . 1.392(2) ? C21 C26 . . 1.393(2) ? C22 C23 . . 1.390(2) ? C22 H22 . . 1.000(19) ? C23 C24 . . 1.389(2) ? C23 H23 . . .98(2) ? C24 C25 . . 1.387(2) ? C24 H24 . . .90(2) ? C25 C26 . . 1.389(2) ? C25 H25 . . .88(2) ? C26 H26 . . .93(2) ? N3 C4 . . 1.3914(17) ? C4 C5 . . 1.358(2) ? C4 C4' . . 1.4538(19) ? C5 H5 . . .95(2) ? S1' C2' . . 1.7200(14) ? S1' C5' . . 1.7120(15) ? C2' C21' . . 1.465(2) ? C2' N3' . . 1.3186(17) ? C21' C22' . . 1.397(2) ? C21' C26' . . 1.399(2) ? C22' C23' . . 1.387(2) ? C22' H22' . . .947(18) ? C23' C24' . . 1.388(3) ? C23' H23' . . .97(2) ? C24' C25' . . 1.388(2) ? C24' H24' . . .87(2) ? C25' C26' . . 1.384(2) ? C25' H25' . . .88(2) ? C26' H26' . . .95(2) ? N3' C4' . . 1.3907(18) ? C4' C5' . . 1.3594(19) ? C5' H5' . . .940(19) ? N1 O11 . . 1.2809(16) ? N1 O12 . . 1.2515(17) ? N1 O13 . . 1.2317(18) ? N2 O21 . . 1.2986(18) ? N2 O22 . . 1.2429(19) ? N2 O23 . . 1.2227(18) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N3 Cu N3' . . . 82.82(5) ? N3 Cu O11 . . . 152.19(5) ? N3 Cu O12 . . . 97.72(4) ? N3 Cu O21 . . . 101.34(4) ? N3 Cu O22 . . . 89.28(5) ? N3' Cu O11 . . . 95.25(5) ? N3' Cu O12 . . . 113.00(4) ? N3' Cu O21 . . . 159.66(5) ? N3' Cu O22 . . . 103.31(5) ? O11 Cu O12 . . . 57.40(4) ? O11 Cu O21 . . . 90.08(4) ? O11 Cu O22 . . . 117.96(5) ? O12 Cu O21 . . . 86.37(4) ? O12 Cu O22 . . . 143.57(4) ? O21 Cu O22 . . . 57.22(4) ? C2 S1 C5 . . . 91.01(7) ? S1 C2 C21 . . . 121.31(10) ? S1 C2 N3 . . . 113.01(10) ? C21 C2 N3 . . . 125.67(12) ? C2 C21 C22 . . . 119.48(12) ? C2 C21 C26 . . . 120.34(13) ? C22 C21 C26 . . . 120.16(13) ? C21 C22 C23 . . . 119.73(13) ? C21 C22 H22 . . . 119.8(11) ? C23 C22 H22 . . . 120.5(11) ? C22 C23 C24 . . . 120.11(15) ? C22 C23 H23 . . . 117.5(11) ? C24 C23 H23 . . . 122.4(11) ? C23 C24 C25 . . . 120.07(15) ? C23 C24 H24 . . . 117.0(12) ? C25 C24 H24 . . . 122.9(12) ? C24 C25 C26 . . . 120.21(15) ? C24 C25 H25 . . . 123.4(15) ? C26 C25 H25 . . . 116.3(15) ? C21 C26 C25 . . . 119.70(15) ? C21 C26 H26 . . . 121.6(13) ? C25 C26 H26 . . . 118.6(13) ? Cu N3 C2 . . . 135.51(9) ? Cu N3 C4 . . . 112.51(9) ? C2 N3 C4 . . . 111.78(11) ? N3 C4 C5 . . . 114.49(12) ? N3 C4 C4' . . . 115.20(12) ? C5 C4 C4' . . . 130.09(12) ? S1 C5 C4 . . . 109.71(10) ? S1 C5 H5 . . . 120.3(13) ? C4 C5 H5 . . . 129.9(13) ? C2' S1' C5' . . . 91.07(7) ? S1' C2' C21' . . . 122.93(10) ? S1' C2' N3' . . . 112.40(10) ? C21' C2' N3' . . . 124.55(12) ? C2' C21' C22' . . . 120.01(13) ? C2' C21' C26' . . . 120.44(12) ? C22' C21' C26' . . . 119.55(13) ? C21' C22' C23' . . . 120.01(14) ? C21' C22' H22' . . . 119.7(11) ? C23' C22' H22' . . . 120.3(11) ? C22' C23' C24' . . . 120.01(15) ? C22' C23' H23' . . . 121.1(12) ? C24' C23' H23' . . . 118.8(12) ? C23' C24' C25' . . . 120.26(17) ? C23' C24' H24' . . . 123.9(15) ? C25' C24' H24' . . . 115.8(15) ? C24' C25' C26' . . . 120.10(16) ? C24' C25' H25' . . . 123.3(16) ? C26' C25' H25' . . . 116.4(16) ? C21' C26' C25' . . . 120.05(14) ? C21' C26' H26' . . . 116.7(14) ? C25' C26' H26' . . . 123.1(14) ? Cu N3' C2' . . . 133.80(9) ? Cu N3' C4' . . . 113.62(9) ? C2' N3' C4' . . . 112.43(11) ? C4 C4' N3' . . . 114.84(11) ? C4 C4' C5' . . . 130.88(13) ? N3' C4' C5' . . . 114.08(12) ? S1' C5' C4' . . . 109.96(11) ? S1' C5' H5' . . . 122.3(11) ? C4' C5' H5' . . . 127.1(11) ? O11 N1 O12 . . . 118.35(12) ? O11 N1 O13 . . . 119.61(13) ? O12 N1 O13 . . . 122.03(13) ? Cu O11 N1 . . . 102.41(8) ? Cu O12 N1 . . . 81.84(8) ? O21 N2 O22 . . . 116.46(13) ? O21 N2 O23 . . . 118.88(13) ? O22 N2 O23 . . . 124.66(15) ? Cu O21 N2 . . . 103.99(8) ? Cu O22 N2 . . . 82.32(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1028 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -35 _reflns_limit_l_max 35 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 10.308 _diffrn_reflns_av_sigmaI/netI .077 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .057 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all .961 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end