######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-09 _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 Nedlands Western Australia 6907 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 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Chemistry, University of Western Australia, Crawley WA 6009 Australia. ; _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. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_csznno # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'Cs2 N4 O8 Zn1' _chemical_formula_moiety 'Cs2 N4 O8 Zn1' _chemical_formula_weight 515.22 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M F_d_d_d _symmetry_space_group_name_Hall -f_2uv_2vw loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/4-x,1/4-y,+z +x,1/4-y,1/4-z 1/4-x,+y,1/4-z -x,-y,-z 3/4+x,3/4+y,-z -x,3/4+y,3/4+z 3/4+x,-y,3/4+z +x,1/2+y,1/2+z 1/2+x,+y,1/2+z 1/2+x,1/2+y,+z 1/4-x,3/4-y,1/2+z 3/4-x,1/4-y,1/2+z 3/4-x,3/4-y,+z +x,3/4-y,3/4-z 1/2+x,1/4-y,3/4-z 1/2+x,3/4-y,1/4-z 1/4-x,1/2+y,3/4-z 3/4-x,+y,3/4-z 3/4-x,1/2+y,1/4-z -x,1/2-y,1/2-z 1/2-x,-y,1/2-z 1/2-x,1/2-y,-z 3/4+x,1/4+y,1/2-z 1/4+x,3/4+y,1/2-z 1/4+x,1/4+y,-z -x,1/4+y,1/4+z 1/2-x,3/4+y,1/4+z 1/2-x,1/4+y,3/4+z 3/4+x,1/2-y,1/4+z 1/4+x,-y,1/4+z 1/4+x,1/2-y,3/4+z _cell_length_a 6.2050(10) _cell_length_b 13.089(3) _cell_length_c 26.214(6) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2129.0(8) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 3.215 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5047 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 9.078 _exptl_crystal_description block _exptl_crystal_size_max .15 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _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 .396 _exptl_absorpt_correction_T_max .564 _diffrn_reflns_number 5047 _reflns_number_total 676 _reflns_Friedel_coverage 0 _reflns_number_gt 630 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.8 _diffrn_reflns_theta_full 28.8 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .027 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .021 _refine_ls_wR_factor_ref .034 _refine_ls_goodness_of_fit_ref 1.3 _refine_ls_number_reflns 630 _refine_ls_number_parameters 37 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment none _refine_ls_shift/su_max .049 _refine_diff_density_min -.634 _refine_diff_density_max .775 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 629(69) # 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 Cs ? 0 16 -.644 2.119 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 64 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Zn ? 0 8 .222 1.431 '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 Cs .37500 -.12500 .056580(10) .0232(2) Uani ? ? 1.00000 ? ? Zn .12500 .12500 .12500 .0201(4) Uani ? ? 1.00000 ? ? N -.1520(4) .0441(3) .05659(12) .0285(16) Uani ? ? 1.00000 ? ? O1 -.0585(4) .00843(19) .09303(10) .0340(12) Uani ? ? 1.00000 ? ? O2 -.1148(4) .1364(3) .04782(14) .0353(15) Uani ? ? 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 Cs .0337(2) .0167(2) .0192(2) .00608(8) .00000 .00000 Zn .0236(4) .0135(4) .0232(4) .00000 .00000 .00000 N .0238(12) .0175(15) .044(2) -.0022(10) .0013(11) -.0091(12) O1 .0397(11) .0271(12) .0353(13) -.0049(11) -.0015(11) .0037(11) O2 .0366(15) .0223(15) .0471(14) .0015(8) -.0058(11) .0061(13) # 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 Cs O1 . . 3.346(3) ? Cs O2 . 2 3.132(3) ? Cs O1 . 4 3.185(3) ? Cs N . 5 3.441(3) ? Cs O2 . 5 3.181(3) ? Cs N . '6 545' 3.441(3) ? Cs O2 . '6 545' 3.181(3) ? Cs O2 . '11 545' 3.132(3) ? Cs O1 . '14 545' 3.346(3) ? Cs O1 . '17 545' 3.185(3) ? Zn O1 . . 2.080(3) ? Zn O2 . . 2.516(3) ? Zn O1 . 2 2.080(3) ? Zn O2 . 2 2.516(3) ? Zn O1 . 3 2.080(3) ? Zn O2 . 3 2.516(3) ? Zn O1 . 4 2.080(3) ? Zn O2 . 4 2.516(3) ? N O1 . . 1.211(4) ? N O2 . . 1.251(5) ? 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 O1 Cs O2 . . 2 58.95(6) ? O1 Cs O1 . . 4 51.23(6) ? O1 Cs N . . 5 76.25(7) ? O1 Cs O2 . . 5 82.07(7) ? O1 Cs N . . '6 545' 136.90(7) ? O1 Cs O2 . . '6 545' 128.99(7) ? O1 Cs O2 . . '11 545' 123.89(6) ? O1 Cs O1 . . '14 545' 146.82(6) ? O1 Cs O1 . . '17 545' 98.88(6) ? O2 Cs O1 2 . 4 60.74(8) ? O2 Cs N 2 . 5 67.77(9) ? O2 Cs O2 2 . 5 88.47(9) ? O2 Cs N 2 . '6 545' 104.59(9) ? O2 Cs O2 2 . '6 545' 84.29(9) ? O2 Cs O2 2 . '11 545' 171.59(10) ? O2 Cs O1 2 . '14 545' 123.89(6) ? O2 Cs O1 2 . '17 545' 127.58(8) ? O1 Cs N 4 . 5 119.44(7) ? O1 Cs O2 4 . 5 132.12(7) ? O1 Cs N 4 . '6 545' 158.96(7) ? O1 Cs O2 4 . '6 545' 138.67(8) ? O1 Cs O2 4 . '11 545' 127.58(8) ? O1 Cs O1 4 . '14 545' 98.88(7) ? O1 Cs O1 4 . '17 545' 68.58(7) ? N Cs O2 5 . 5 21.33(8) ? N Cs N 5 . '6 545' 60.86(7) ? N Cs O2 5 . '6 545' 56.49(7) ? N Cs O2 5 . '11 545' 104.59(9) ? N Cs O1 5 . '14 545' 136.90(7) ? N Cs O1 5 . '17 545' 158.96(7) ? O2 Cs N 5 . '6 545' 56.49(7) ? O2 Cs O2 5 . '6 545' 61.29(7) ? O2 Cs O2 5 . '11 545' 84.29(9) ? O2 Cs O1 5 . '14 545' 128.99(7) ? O2 Cs O1 5 . '17 545' 138.67(8) ? N Cs O2 '6 545' . '6 545' 21.33(8) ? N Cs O2 '6 545' . '11 545' 67.77(9) ? N Cs O1 '6 545' . '14 545' 76.25(7) ? N Cs O1 '6 545' . '17 545' 119.44(7) ? O2 Cs O2 '6 545' . '11 545' 88.47(9) ? O2 Cs O1 '6 545' . '14 545' 82.07(7) ? O2 Cs O1 '6 545' . '17 545' 132.12(7) ? O2 Cs O1 '11 545' . '14 545' 58.95(6) ? O2 Cs O1 '11 545' . '17 545' 60.74(8) ? O1 Cs O1 '14 545' . '17 545' 51.23(6) ? O1 Zn O2 . . . 52.82(10) ? O1 Zn O1 . . 2 132.48(10) ? O1 Zn O2 . . 2 87.49(10) ? O1 Zn O1 . . 3 113.63(10) ? O1 Zn O2 . . 3 87.53(10) ? O1 Zn O1 . . 4 85.63(10) ? O1 Zn O2 . . 4 133.72(10) ? O2 Zn O1 . . 2 87.49(10) ? O2 Zn O2 . . 2 72.93(9) ? O2 Zn O1 . . 3 87.53(10) ? O2 Zn O2 . . 3 107.49(9) ? O2 Zn O1 . . 4 133.72(11) ? O2 Zn O2 . . 4 173.21(11) ? Cs Zn O1 2 . 2 55.76(7) ? Cs Zn O2 2 . 2 85.30(8) ? Cs Zn O1 2 . 3 51.30(7) ? Cs Zn O2 2 . 3 100.24(7) ? Cs Zn O1 2 . 4 169.39(7) ? Cs Zn O2 2 . 4 122.41(8) ? O1 Zn O2 2 . 2 52.82(10) ? O1 Zn O1 2 . 3 85.63(10) ? O1 Zn O2 2 . 3 133.72(11) ? O1 Zn O1 2 . 4 113.63(10) ? O1 Zn O2 2 . 4 87.53(10) ? O2 Zn O1 2 . 3 133.72(11) ? O2 Zn O2 2 . 3 173.21(11) ? O2 Zn O1 2 . 4 87.53(10) ? O2 Zn O2 2 . 4 107.49(9) ? O1 Zn O2 3 . 3 52.82(10) ? O1 Zn O1 3 . 4 132.48(10) ? O1 Zn O2 3 . 4 87.49(10) ? O2 Zn O1 3 . 4 87.49(10) ? O2 Zn O2 3 . 4 72.93(9) ? O1 Zn O2 4 . 4 52.82(10) ? O1 N O2 . . . 115.4(3) ? Cs O1 Zn . . . 93.32(9) ? Cs O1 N . . . 111.2(2) ? Cs O1 Cs . . 4 93.09(7) ? Zn O1 N . . . 107.3(2) ? Zn O1 Cs . . 4 98.06(9) ? N O1 Cs . . 4 143.2(2) ? Zn O2 N . . . 84.5(2) ? Zn O2 Cs . . 2 90.69(10) ? Zn O2 Cs . . 5 171.61(13) ? N O2 Cs . . 2 161.0(2) ? N O2 Cs . . 5 91.1(2) ? Cs O2 Cs 2 . 5 95.71(9) ? _exptl_crystal_F_000 1856 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 8 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _reflns_number_observed ? _reflns_d_resolution_high .738 _reflns_d_resolution_low 6.545 _diffrn_reflns_av_sigmaI/netI .014 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .022 _refine_ls_wR_factor_all .035 _refine_ls_goodness_of_fit_all 1.286 _refine_ls_shift/su_mean .003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end