# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yonglin An' _publ_contact_author_email YLAN@DLUT.EDU.CN _publ_section_title ; (H2en)2Cu8Sn3S12: a trigonal CuS3-Based open-framework sulfide with interesting ion-exchange properties ; loop_ _publ_author_name 'Yonglin An.' 'Min Ji.' 'Shouhua Ji.' 'Mei-Chen Liu.' 'Hua-Gang Yao.' ; Ren-Chun Zhang ; # Attachment '1_and_Cs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 728547' #TrackingRef '1_and_Cs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 Cu80 N24 S120 Sn30' _chemical_formula_weight 13115.58 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 25.4484(4) _cell_length_b 25.4484(4) _cell_length_c 25.4484(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16480.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6670 _cell_measurement_theta_min 2.264 _cell_measurement_theta_max 22.331 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12104 _exptl_absorpt_coefficient_mu 8.037 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Smart Apex II CCD' _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_% 0 _diffrn_reflns_number 3172 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3172 _reflns_number_gt 2195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3172 _refine_ls_number_parameters 93 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.996 _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 Sn1 Sn 0.115013(13) 0.566896(13) 0.378707(13) 0.02541(11) Uani 1 1 d . . . Sn2 Sn 0.0000 0.7500 0.2500 0.02313(16) Uani 1 4 d S . . Cu4 Cu 0.10367(2) 0.51888(3) 0.50700(3) 0.03676(18) Uani 1 1 d . . . Cu1 Cu 0.08943(3) 0.62480(3) 0.25286(2) 0.03719(18) Uani 1 1 d . . . Cu3 Cu 0.06638(3) 0.43362(3) 0.43362(3) 0.0360(3) Uani 1 3 d S . . S5 S 0.05344(5) 0.69107(5) 0.30059(5) 0.0305(3) Uani 1 1 d . . . S1 S 0.13569(5) 0.49037(5) 0.43044(5) 0.0292(3) Uani 1 1 d . . . S3 S 0.02348(5) 0.58394(5) 0.39590(5) 0.0275(3) Uani 1 1 d . . . Cu2 Cu -0.00899(2) 0.65211(2) 0.34873(2) 0.034 Uani 1 1 d . . . S2 S 0.16596(5) 0.64244(5) 0.40467(5) 0.0295(3) Uani 1 1 d . . . S4 S 0.12310(6) 0.55074(6) 0.28688(5) 0.0474(4) Uani 1 1 d . . . N1 N 0.09465(19) 0.7500 0.40535(19) 0.0472(18) Uiso 1 2 d SD . . N2 N -0.0094(2) 0.7500 0.5094(2) 0.068(2) Uiso 1 2 d SD . . C1 C 0.0437(4) 0.7393(6) 0.4306(5) 0.081(5) Uiso 0.50 1 d PD . . C2 C 0.0435(4) 0.7558(5) 0.4878(5) 0.072(4) Uiso 0.50 1 d PD . . 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 Sn1 0.0267(2) 0.0241(2) 0.0255(2) 0.00286(14) -0.00140(14) -0.00005(14) Sn2 0.0275(4) 0.0209(2) 0.0209(2) 0.000 0.000 0.000 Cu4 0.0376(4) 0.0387(4) 0.0340(4) 0.0058(3) -0.0028(3) -0.0029(3) Cu1 0.0420(4) 0.0385(4) 0.0311(4) 0.0011(3) 0.0002(3) 0.0013(3) Cu3 0.0360(3) 0.0360(3) 0.0360(3) 0.0038(3) -0.0038(3) -0.0038(3) S5 0.0372(7) 0.0299(7) 0.0243(7) 0.0035(5) -0.0014(6) 0.0053(6) S1 0.0277(7) 0.0262(7) 0.0338(8) 0.0047(5) -0.0050(5) 0.0000(5) S3 0.0237(7) 0.0277(7) 0.0311(7) 0.0070(5) -0.0019(5) -0.0022(5) Cu2 0.039 0.032 0.030 0.001 -0.002 -0.001 S2 0.0241(7) 0.0276(7) 0.0366(8) 0.0011(6) 0.0019(6) -0.0026(5) S4 0.0754(11) 0.0405(9) 0.0263(8) -0.0012(6) -0.0006(7) 0.0181(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 Sn1 S4 2.3818(14) . ? Sn1 S1 2.4090(12) . ? Sn1 S3 2.4095(13) . ? Sn1 S2 2.4110(12) . ? Sn2 S5 2.3991(12) 4_565 ? Sn2 S5 2.3992(12) 41_565 ? Sn2 S5 2.3992(12) . ? Sn2 S5 2.3992(12) 44_566 ? Cu4 S1 2.2330(14) . ? Cu4 S3 2.2353(13) 7 ? Cu4 S3 2.2653(14) 34_566 ? Cu4 Cu3 3.0157(10) . ? Cu1 S4 2.2441(15) . ? Cu1 S2 2.2616(13) 23 ? Cu1 S5 2.2712(14) . ? Cu3 S1 2.2811(12) . ? Cu3 S1 2.2811(12) 7 ? Cu3 S1 2.2811(12) 10 ? Cu3 Cu4 3.0157(10) 10 ? Cu3 Cu4 3.0157(10) 7 ? S5 Cu2 2.2379(14) . ? S3 Cu4 2.2353(13) 10 ? S3 Cu4 2.2653(14) 31_566 ? S3 Cu2 2.2655(13) . ? Cu2 S2 2.2368(14) 31_566 ? S2 Cu2 2.2368(14) 34_566 ? S2 Cu1 2.2616(13) 21 ? N1 C1 1.473(8) . ? N1 C1 1.473(8) 24_565 ? N2 C2 1.462(8) 24_565 ? N2 C2 1.462(8) . ? C1 C2 1.514(9) . ? 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 S4 Sn1 S1 112.19(5) . . ? S4 Sn1 S3 107.03(5) . . ? S1 Sn1 S3 104.92(4) . . ? S4 Sn1 S2 111.10(5) . . ? S1 Sn1 S2 112.17(4) . . ? S3 Sn1 S2 109.06(4) . . ? S5 Sn2 S5 108.74(3) 4_565 41_565 ? S5 Sn2 S5 110.94(6) 4_565 . ? S5 Sn2 S5 108.74(3) 41_565 . ? S5 Sn2 S5 108.74(3) 4_565 44_566 ? S5 Sn2 S5 110.94(6) 41_565 44_566 ? S5 Sn2 S5 108.74(3) . 44_566 ? S1 Cu4 S3 127.29(5) . 7 ? S1 Cu4 S3 123.61(5) . 34_566 ? S3 Cu4 S3 107.49(3) 7 34_566 ? S1 Cu4 Cu3 48.76(4) . . ? S3 Cu4 Cu3 101.36(4) 7 . ? S3 Cu4 Cu3 137.20(4) 34_566 . ? S4 Cu1 S2 121.23(5) . 23 ? S4 Cu1 S5 124.85(5) . . ? S2 Cu1 S5 113.73(5) 23 . ? S1 Cu3 S1 118.985(15) . 7 ? S1 Cu3 S1 118.985(15) . 10 ? S1 Cu3 S1 118.984(15) 7 10 ? S1 Cu3 Cu4 47.40(4) . . ? S1 Cu3 Cu4 98.81(4) 7 . ? S1 Cu3 Cu4 134.71(5) 10 . ? S1 Cu3 Cu4 98.81(4) . 10 ? S1 Cu3 Cu4 134.71(5) 7 10 ? S1 Cu3 Cu4 47.40(4) 10 10 ? Cu4 Cu3 Cu4 88.61(3) . 10 ? S1 Cu3 Cu4 134.71(5) . 7 ? S1 Cu3 Cu4 47.40(4) 7 7 ? S1 Cu3 Cu4 98.81(4) 10 7 ? Cu4 Cu3 Cu4 88.61(3) . 7 ? Cu4 Cu3 Cu4 88.61(3) 10 7 ? Cu2 S5 Cu1 104.48(5) . . ? Cu2 S5 Sn2 99.69(5) . . ? Cu1 S5 Sn2 113.94(5) . . ? Cu4 S1 Cu3 83.83(5) . . ? Cu4 S1 Sn1 97.73(5) . . ? Cu3 S1 Sn1 111.24(5) . . ? Cu4 S3 Cu4 95.75(5) 10 31_566 ? Cu4 S3 Cu2 119.83(6) 10 . ? Cu4 S3 Cu2 105.67(5) 31_566 . ? Cu4 S3 Sn1 108.02(5) 10 . ? Cu4 S3 Sn1 113.13(5) 31_566 . ? Cu2 S3 Sn1 113.22(5) . . ? S2 Cu2 S5 133.04(5) 31_566 . ? S2 Cu2 S3 115.20(5) 31_566 . ? S5 Cu2 S3 111.74(5) . . ? Cu2 S2 Cu1 96.25(5) 34_566 21 ? Cu2 S2 Sn1 105.34(5) 34_566 . ? Cu1 S2 Sn1 112.69(5) 21 . ? Cu1 S4 Sn1 101.56(6) . . ? C2 C1 N1 158.3(16) 24_565 . ? N1 C1 C2 111.7(8) . . ? C1 C2 N2 151.8(17) 24_565 . ? N2 C2 C1 109.6(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.109 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.151 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 8 1 ' ' 2 0.000 0.000 0.500 8 1 ' ' 3 0.183 0.237 0.244 2282 696 ' ' 4 0.000 0.500 0.000 8 1 ' ' 5 0.000 0.500 0.500 8 1 ' ' 6 -0.185 0.731 0.737 2282 696 ' ' 7 0.500 0.000 0.000 8 1 ' ' 8 0.500 0.000 0.500 8 1 ' ' 9 0.500 0.500 0.000 8 1 ' ' 10 0.500 0.500 0.500 8 1 ' ' _platon_squeeze_details ; ; #===END data_1Cs _database_code_depnum_ccdc_archive 'CCDC 753511' #TrackingRef '1_and_Cs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 Cs5.64 Cu80 N24 S120 Sn30' _chemical_formula_weight 13867.79 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 25.3455(15) _cell_length_b 25.3455(15) _cell_length_c 25.3455(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16281.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13764 _cell_measurement_theta_min 2.263 _cell_measurement_theta_max 28.059 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12732 _exptl_absorpt_coefficient_mu 8.765 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Smart Apex II CCD' _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_% 0 _diffrn_reflns_number 3577 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 29.02 _reflns_number_total 3577 _reflns_number_gt 2949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1591P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3577 _refine_ls_number_parameters 115 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 N1 N 0.4070(3) 0.7500 0.4070(3) 0.050(3) Uiso 1 2 d SD . . N2 N 0.5112(4) 0.7500 0.5112(4) 0.057(3) Uiso 1 2 d SD . . C1 C 0.4574(6) 0.7607(9) 0.4314(7) 0.063(5) Uiso 0.50 1 d PD . . C2 C 0.4589(7) 0.7432(9) 0.4883(7) 0.072(6) Uiso 0.50 1 d PD . . Sn2 Sn 0.2500 0.7500 0.5000 0.0209(2) Uani 1 4 d S . . Sn1 Sn 0.378170(18) 0.567061(18) 0.384928(18) 0.02216(19) Uani 1 1 d . . . Cu2 Cu 0.34856(3) 0.65215(3) 0.50935(4) 0.0313(3) Uani 1 1 d . . . Cu4 Cu 0.48090(4) 0.60354(4) 0.49307(4) 0.0335(3) Uani 1 1 d . . . Cu3 Cu 0.56612(4) 0.56612(4) 0.56612(4) 0.0325(4) Uani 1 3 d S . . Cu1 Cu 0.25275(3) 0.62497(4) 0.41007(4) 0.0342(3) Uani 1 1 d . . . S1 S 0.43036(6) 0.49040(6) 0.36434(6) 0.0262(4) Uani 1 1 d . . . S3 S 0.39549(6) 0.58405(6) 0.47654(6) 0.0253(4) Uani 1 1 d . . . S5 S 0.30087(6) 0.69106(6) 0.44676(7) 0.0281(4) Uani 1 1 d . . . S2 S 0.40413(7) 0.64272(6) 0.33410(6) 0.0273(4) Uani 1 1 d . . . S4 S 0.28648(7) 0.55066(8) 0.37629(9) 0.0395(5) Uani 1 1 d . . . Cs1 Cs 0.2500 0.5990(4) 0.2500 0.102(3) Uiso 0.32 4 d SP . . Cs1' Cs 0.2500 0.4980(10) 0.2500 0.096(6) Uiso 0.10 4 d SP . . Cs3 Cs 0.3160(8) 0.7500 0.3160(8) 0.101(8) Uiso 0.06 2 d SP . . Cs2 Cs 0.3196(13) 0.4380(12) 0.2895(13) 0.092(8) Uiso 0.03 1 d P . . Cs5 Cs 0.2500 0.6169(8) 0.2500 0.095(5) Uiso 0.16 4 d SP . . Cs4 Cs 0.3164(13) 0.4085(12) 0.3504(12) 0.097(8) Uiso 0.03 1 d P . . 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 Sn2 0.0186(3) 0.0186(3) 0.0254(4) 0.000 0.000 0.000 Sn1 0.0220(3) 0.0221(3) 0.0223(3) -0.00050(15) 0.00053(15) 0.00203(15) Cu2 0.0283(4) 0.0289(5) 0.0367(5) 0.0012(3) 0.0011(3) 0.0013(3) Cu4 0.0341(5) 0.0367(5) 0.0298(5) 0.0018(3) 0.0041(4) 0.0022(4) Cu3 0.0325(4) 0.0325(4) 0.0325(4) 0.0031(4) 0.0031(4) 0.0031(4) Cu1 0.0289(5) 0.0347(5) 0.0390(6) -0.0014(4) 0.0003(3) 0.0015(3) S1 0.0292(8) 0.0244(8) 0.0252(8) -0.0002(6) 0.0042(6) 0.0055(6) S3 0.0285(8) 0.0261(8) 0.0212(7) 0.0015(6) 0.0012(6) 0.0052(6) S5 0.0229(7) 0.0276(8) 0.0337(8) -0.0055(6) 0.0009(6) 0.0045(6) S2 0.0351(9) 0.0254(8) 0.0216(7) 0.0042(6) -0.0023(6) 0.0005(6) S4 0.0229(8) 0.0375(10) 0.0581(12) -0.0151(8) -0.0025(8) -0.0012(7) _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 N1 C1 1.445(9) . ? N1 C1 1.445(9) 22_565 ? N2 C2 1.459(10) . ? N2 C2 1.459(10) 22_565 ? C1 C2 1.509(10) . ? Sn2 S5 2.3906(16) 39_666 ? Sn2 S5 2.3906(16) 40_566 ? Sn2 S5 2.3906(16) . ? Sn2 S5 2.3906(16) 2_565 ? Sn1 S4 2.3709(18) . ? Sn1 S2 2.4021(16) . ? Sn1 S3 2.4020(16) . ? Sn1 S1 2.4078(15) . ? Cu2 S5 2.2250(19) . ? Cu2 S2 2.2314(19) 33_666 ? Cu2 S3 2.2550(18) . ? Cu4 S1 2.2267(19) 33_666 ? Cu4 S3 2.2327(18) 29_666 ? Cu4 S3 2.2596(19) . ? Cu4 Cu3 2.9989(14) . ? Cu3 S1 2.2731(16) 33_666 ? Cu3 S1 2.2731(16) 25_666 ? Cu3 S1 2.2731(16) 29_666 ? Cu3 Cu4 2.9989(14) 9 ? Cu3 Cu4 2.9989(14) 5 ? Cu1 S4 2.239(2) . ? Cu1 S2 2.2518(18) 23 ? Cu1 S5 2.2709(19) . ? S1 Cu4 2.2267(19) 29_666 ? S1 Cu3 2.2731(16) 25_666 ? S3 Cu4 2.2327(18) 33_666 ? S2 Cu2 2.2314(19) 29_666 ? S2 Cu1 2.2518(18) 21 ? 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 C2 C1 N1 157(2) 22_565 . ? N1 C1 C2 112.1(12) . . ? C1 C2 N2 155(3) 22_565 . ? N2 C2 C1 111.6(13) . . ? S5 Sn2 S5 111.27(8) 39_666 40_566 ? S5 Sn2 S5 108.58(4) 39_666 . ? S5 Sn2 S5 108.58(4) 40_566 . ? S5 Sn2 S5 108.58(4) 39_666 2_565 ? S5 Sn2 S5 108.58(4) 40_566 2_565 ? S5 Sn2 S5 111.27(8) . 2_565 ? S4 Sn1 S2 111.03(7) . . ? S4 Sn1 S3 107.45(7) . . ? S2 Sn1 S3 108.98(6) . . ? S4 Sn1 S1 112.15(6) . . ? S2 Sn1 S1 112.18(6) . . ? S3 Sn1 S1 104.70(6) . . ? S5 Cu2 S2 133.26(7) . 33_666 ? S5 Cu2 S3 111.27(7) . . ? S2 Cu2 S3 115.45(7) 33_666 . ? S1 Cu4 S3 126.95(7) 33_666 29_666 ? S1 Cu4 S3 123.67(7) 33_666 . ? S3 Cu4 S3 107.64(5) 29_666 . ? S1 Cu4 Cu3 48.87(5) 33_666 . ? S3 Cu4 Cu3 101.31(5) 29_666 . ? S3 Cu4 Cu3 137.34(6) . . ? S1 Cu3 S1 118.88(2) 33_666 25_666 ? S1 Cu3 S1 118.88(2) 33_666 29_666 ? S1 Cu3 S1 118.88(2) 25_666 29_666 ? S1 Cu3 Cu4 134.93(7) 33_666 9 ? S1 Cu3 Cu4 99.03(5) 25_666 9 ? S1 Cu3 Cu4 47.55(5) 29_666 9 ? S1 Cu3 Cu4 99.03(5) 33_666 5 ? S1 Cu3 Cu4 47.55(5) 25_666 5 ? S1 Cu3 Cu4 134.93(7) 29_666 5 ? Cu4 Cu3 Cu4 88.76(5) 9 5 ? S1 Cu3 Cu4 47.55(5) 33_666 . ? S1 Cu3 Cu4 134.93(7) 25_666 . ? S1 Cu3 Cu4 99.03(5) 29_666 . ? Cu4 Cu3 Cu4 88.76(5) 9 . ? Cu4 Cu3 Cu4 88.76(5) 5 . ? S4 Cu1 S2 121.05(7) . 23 ? S4 Cu1 S5 124.90(7) . . ? S2 Cu1 S5 113.89(7) 23 . ? Cu4 S1 Cu3 83.58(7) 29_666 25_666 ? Cu4 S1 Sn1 97.82(7) 29_666 . ? Cu3 S1 Sn1 111.22(7) 25_666 . ? Cu4 S3 Cu2 119.85(8) 33_666 . ? Cu4 S3 Cu4 95.23(7) 33_666 . ? Cu2 S3 Cu4 105.65(7) . . ? Cu4 S3 Sn1 108.18(7) 33_666 . ? Cu2 S3 Sn1 113.41(7) . . ? Cu4 S3 Sn1 113.17(7) . . ? Cu2 S5 Cu1 104.88(7) . . ? Cu2 S5 Sn2 99.64(7) . . ? Cu1 S5 Sn2 113.73(7) . . ? Cu2 S2 Cu1 96.13(7) 29_666 21 ? Cu2 S2 Sn1 105.33(7) 29_666 . ? Cu1 S2 Sn1 112.53(7) 21 . ? Cu1 S4 Sn1 101.04(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.454 _refine_diff_density_min -2.317 _refine_diff_density_rms 0.230 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 8 1 ' ' 2 0.000 0.000 0.500 8 1 ' ' 3 0.000 0.500 0.000 8 1 ' ' 4 0.000 0.500 0.500 8 1 ' ' 5 0.250 0.250 0.250 76 5 ' ' 6 0.500 0.000 0.000 8 1 ' ' 7 0.500 0.000 0.500 8 1 ' ' 8 0.500 0.500 0.000 8 1 ' ' 9 0.500 0.500 0.500 8 1 ' ' 10 0.750 0.750 0.750 76 5 ' ' _platon_squeeze_details ; ;