Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Vidyasagar, K.' 'Devi, M. Suseela' _publ_contact_author_name 'Dr K Vidyasagar' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Madras, Chennai 600 036 INDIA ; _publ_contact_author_email 'KVSAGAR@IITM.AC.IN' _publ_section_title ; First examples of sulfides in the quaternary A/Cd/Sn/S (A=Li, Na) systems: Molten flux synthesis and single crystal x-ray structures of Li2CdSnS4, Na2CdSnS4 and Na6CdSn4S12. ; data_sus1 _database_code_CSD 173898 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Li2CdSnS4' _chemical_formula_weight 378.266 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z' 'x, -y+1/2, z' '-x+1/2, -y+1/2, z' '-x, -y, -z' 'x-1/2, -y, -z' '-x, y-1/2, -z' 'x-1/2, y-1/2, -z' _cell_length_a 7.9654(15) _cell_length_b 6.4917(15) _cell_length_c 6.9685(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 360.33(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.11 _cell_measurement_theta_max 15.23 _exptl_crystal_description 'needle shaped' _exptl_crystal_colour 'orange colour' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.440 _exptl_crystal_density_method ? _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 7.450 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6963 _exptl_absorpt_correction_T_max 0.9985 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70730 _diffrn_radiation_type MoK/a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 0% _diffrn_reflns_number 689 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 24.84 _reflns_number_total 378 _reflns_number_observed 343 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD$ programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+6.1594P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0110(32) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 378 _refine_ls_number_parameters 33 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_obs 0.0495 _refine_ls_wR_factor_all 0.1476 _refine_ls_wR_factor_obs 0.1449 _refine_ls_goodness_of_fit_all 1.302 _refine_ls_goodness_of_fit_obs 1.348 _refine_ls_restrained_S_all 1.302 _refine_ls_restrained_S_obs 1.348 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd Cd 0.2500 0.2500 0.6567(2) 0.0221(7) Uani 1 d S . Sn Sn 0.2500 0.7500 0.3298(2) 0.0129(7) Uani 1 d S . S(1) S 0.2500 0.1190(14) 0.3152(10) 0.025(2) Uani 0.50 d SP . S(2) S 0.2500 0.6355(10) 0.6571(8) 0.014(2) Uani 0.50 d SP . S(3) S 0.5068(5) 0.1234(10) 0.8375(6) 0.0184(13) Uani 0.50 d P . Li Li 0.4930(27) 0.2500 0.1675(33) 0.020 Uiso 1 d S . 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 Cd 0.0222(10) 0.0222(11) 0.0219(10) 0.000 0.000 0.000 Sn 0.0111(9) 0.0110(10) 0.0166(9) 0.000 0.000 0.000 S(1) 0.029(4) 0.023(4) 0.024(3) -0.001(3) 0.000 0.000 S(2) 0.019(3) 0.001(4) 0.023(3) 0.001(2) 0.000 0.000 S(3) 0.019(3) 0.015(3) 0.021(3) 0.000(2) 0.001(2) 0.000(2) _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 Cd S(2) 2.503(7) 3 ? Cd S(2) 2.503(7) . ? Cd S(1) 2.527(8) . ? Cd S(1) 2.527(8) 3 ? Cd S(3) 2.539(5) 3 ? Cd S(3) 2.539(5) . ? Cd S(3) 2.539(5) 2 ? Cd S(3) 2.539(5) 4 ? Sn S(1) 2.397(9) 3 ? Sn S(1) 2.397(9) 1_565 ? Sn S(2) 2.399(6) 3_565 ? Sn S(2) 2.399(6) . ? Sn S(3) 2.406(5) 8_566 ? Sn S(3) 2.406(5) 6_566 ? Sn S(3) 2.406(5) 7_666 ? Sn S(3) 2.406(5) 5_666 ? S(1) S(1) 1.70(2) 3 ? S(1) Li 2.35(2) 2 ? S(1) Li 2.35(2) . ? S(1) Sn 2.397(9) 1_545 ? S(2) S(2) 1.486(13) 3_565 ? S(2) Li 2.50(2) 5_666 ? S(2) Li 2.50(2) 6_566 ? S(3) S(3) 1.644(14) 3 ? S(3) Sn 2.406(5) 5_666 ? S(3) Li 2.424(7) 5_656 ? S(3) Li 2.45(2) 1_556 ? Li S(1) 2.35(2) 3 ? Li S(3) 2.424(7) 5_656 ? Li S(3) 2.424(7) 7_666 ? Li S(3) 2.45(2) 1_554 ? Li S(3) 2.45(2) 3_554 ? Li S(2) 2.50(2) 5_666 ? Li S(2) 2.50(2) 7_656 ? 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 S(2) Cd S(2) 179.9(3) 3 . ? S(2) Cd S(1) 70.4(2) 3 . ? S(2) Cd S(1) 109.7(2) . . ? S(2) Cd S(1) 109.7(2) 3 3 ? S(2) Cd S(1) 70.4(2) . 3 ? S(1) Cd S(1) 39.3(4) . 3 ? S(2) Cd S(3) 108.9(2) 3 3 ? S(2) Cd S(3) 71.1(2) . 3 ? S(1) Cd S(3) 125.19(11) . 3 ? S(1) Cd S(3) 111.0(2) 3 3 ? S(2) Cd S(3) 71.1(2) 3 . ? S(2) Cd S(3) 108.9(2) . . ? S(1) Cd S(3) 111.0(2) . . ? S(1) Cd S(3) 125.19(11) 3 . ? S(3) Cd S(3) 37.8(3) 3 . ? S(2) Cd S(3) 71.1(2) 3 2 ? S(2) Cd S(3) 108.9(2) . 2 ? S(1) Cd S(3) 111.0(2) . 2 ? S(1) Cd S(3) 125.19(11) 3 2 ? S(3) Cd S(3) 120.5(2) 3 2 ? S(3) Cd S(3) 107.3(2) . 2 ? S(2) Cd S(3) 108.9(2) 3 4 ? S(2) Cd S(3) 71.1(2) . 4 ? S(1) Cd S(3) 125.19(11) . 4 ? S(1) Cd S(3) 111.0(2) 3 4 ? S(3) Cd S(3) 107.3(2) 3 4 ? S(3) Cd S(3) 120.5(2) . 4 ? S(3) Cd S(3) 37.8(3) 2 4 ? S(1) Sn S(1) 175.1(3) 3 1_565 ? S(1) Sn S(2) 110.5(2) 3 3_565 ? S(1) Sn S(2) 74.4(2) 1_565 3_565 ? S(1) Sn S(2) 74.4(2) 3 . ? S(1) Sn S(2) 110.5(2) 1_565 . ? S(2) Sn S(2) 36.1(3) 3_565 . ? S(1) Sn S(3) 68.8(2) 3 8_566 ? S(1) Sn S(3) 108.7(2) 1_565 8_566 ? S(2) Sn S(3) 124.51(12) 3_565 8_566 ? S(2) Sn S(3) 110.8(2) . 8_566 ? S(1) Sn S(3) 108.7(2) 3 6_566 ? S(1) Sn S(3) 68.8(2) 1_565 6_566 ? S(2) Sn S(3) 110.79(15) 3_565 6_566 ? S(2) Sn S(3) 124.51(12) . 6_566 ? S(3) Sn S(3) 40.0(3) 8_566 6_566 ? S(1) Sn S(3) 68.8(2) 3 7_666 ? S(1) Sn S(3) 108.7(2) 1_565 7_666 ? S(2) Sn S(3) 124.51(12) 3_565 7_666 ? S(2) Sn S(3) 110.79(15) . 7_666 ? S(3) Sn S(3) 107.3(2) 8_566 7_666 ? S(3) Sn S(3) 122.0(2) 6_566 7_666 ? S(1) Sn S(3) 108.7(2) 3 5_666 ? S(1) Sn S(3) 68.8(2) 1_565 5_666 ? S(2) Sn S(3) 110.8(2) 3_565 5_666 ? S(2) Sn S(3) 124.51(12) . 5_666 ? S(3) Sn S(3) 122.0(2) 8_566 5_666 ? S(3) Sn S(3) 107.3(2) 6_566 5_666 ? S(3) Sn S(3) 40.0(3) 7_666 5_666 ? S(1) S(1) Li 68.8(3) 3 2 ? S(1) S(1) Li 68.8(3) 3 . ? Li S(1) Li 110.8(10) 2 . ? S(1) S(1) Sn 177.6(2) 3 1_545 ? Li S(1) Sn 112.3(3) 2 1_545 ? Li S(1) Sn 112.3(3) . 1_545 ? S(1) S(1) Cd 70.3(2) 3 . ? Li S(1) Cd 106.9(6) 2 . ? Li S(1) Cd 106.9(6) . . ? Sn S(1) Cd 107.2(3) 1_545 . ? S(2) S(2) Sn 72.0(2) 3_565 . ? S(2) S(2) Li 72.7(2) 3_565 5_666 ? Sn S(2) Li 111.9(5) . 5_666 ? S(2) S(2) Li 72.7(2) 3_565 6_566 ? Sn S(2) Li 111.9(5) . 6_566 ? Li S(2) Li 110.1(9) 5_666 6_566 ? S(2) S(2) Cd 179.93(14) 3_565 . ? Sn S(2) Cd 108.0(2) . . ? Li S(2) Cd 107.3(2) 5_666 . ? Li S(2) Cd 107.3(2) 6_566 . ? S(3) S(3) Sn 70.0(2) 3 5_666 ? S(3) S(3) Li 179.2(5) 3 5_656 ? Sn S(3) Li 109.5(6) 5_666 5_656 ? S(3) S(3) Li 70.4(2) 3 1_556 ? Sn S(3) Li 112.2(5) 5_666 1_556 ? Li S(3) Li 110.5(4) 5_656 1_556 ? S(3) S(3) Cd 71.11(15) 3 . ? Sn S(3) Cd 107.3(2) 5_666 . ? Li S(3) Cd 108.5(6) 5_656 . ? Li S(3) Cd 108.8(5) 1_556 . ? S(1) Li S(1) 42.4(6) . 3 ? S(1) Li S(3) 69.2(4) . 5_656 ? S(1) Li S(3) 111.6(7) 3 5_656 ? S(1) Li S(3) 111.6(7) . 7_666 ? S(1) Li S(3) 69.2(4) 3 7_666 ? S(3) Li S(3) 178.3(11) 5_656 7_666 ? S(1) Li S(3) 109.1(7) . 1_554 ? S(1) Li S(3) 124.8(9) 3 1_554 ? S(3) Li S(3) 69.5(4) 5_656 1_554 ? S(3) Li S(3) 108.8(7) 7_666 1_554 ? S(1) Li S(3) 124.8(9) . 3_554 ? S(1) Li S(3) 109.1(7) 3 3_554 ? S(3) Li S(3) 108.8(7) 5_656 3_554 ? S(3) Li S(3) 69.5(4) 7_666 3_554 ? S(3) Li S(3) 39.3(5) 1_554 3_554 ? S(1) Li S(2) 124.6(10) . 5_666 ? S(1) Li S(2) 110.7(8) 3 5_666 ? S(3) Li S(2) 107.7(7) 5_656 5_666 ? S(3) Li S(2) 73.1(4) 7_666 5_666 ? S(3) Li S(2) 121.6(9) 1_554 5_666 ? S(3) Li S(2) 108.9(7) 3_554 5_666 ? S(1) Li S(2) 110.7(8) . 7_656 ? S(1) Li S(2) 124.6(10) 3 7_656 ? S(3) Li S(2) 73.1(4) 5_656 7_656 ? S(3) Li S(2) 107.7(7) 7_666 7_656 ? S(3) Li S(2) 108.9(7) 1_554 7_656 ? S(3) Li S(2) 121.6(9) 3_554 7_656 ? S(2) Li S(2) 34.6(4) 5_666 7_656 ? _refine_diff_density_max 4.987 _refine_diff_density_min -2.623 _refine_diff_density_rms 0.372 #===END data_sus2 _database_code_CSD 173899 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Na2CdSnS4' _chemical_formula_weight 405.364 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -1.0050 1.2020 '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' 'Na' 'Na' 0.0362 0.0249 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 9.282(1) _cell_length_b 9.421(3) _cell_length_c 6.593(9) _cell_angle_alpha 90.00 _cell_angle_beta 134.83(9) _cell_angle_gamma 90.00 _cell_volume 408.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.12 _cell_measurement_theta_max 16.82 _exptl_crystal_description 'block shaped' _exptl_crystal_colour 'bright yellow colour' _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.292 _exptl_crystal_density_method ? _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 6.499 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6881 _exptl_absorpt_correction_T_max 0.9947 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 0% _diffrn_reflns_number 789 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 24.95 _reflns_number_total 728 _reflns_number_observed 669 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD4 programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+1.6078P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0064(23) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.17(13) _refine_ls_number_reflns 728 _refine_ls_number_parameters 40 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_obs 0.0588 _refine_ls_wR_factor_all 0.1532 _refine_ls_wR_factor_obs 0.1437 _refine_ls_goodness_of_fit_all 1.158 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.157 _refine_ls_restrained_S_obs 1.134 _refine_ls_shift/esd_max -0.012 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd Cd 0.0000 0.0054(2) 0.5000 0.0332(7) Uani 1 d S . Sn Sn 0.0000 0.25505(6) 0.0000 0.0230(5) Uani 1 d S . Na1 Na 0.0000 0.7966(20) 0.0000 0.070(6) Uani 1 d S . Na2 Na 0.0000 0.5373(21) 0.5000 0.062(6) Uani 1 d S . S1 S 0.2329(8) 0.3827(6) 0.0259(10) 0.0456(12) Uani 1 d . . S2 S 0.7069(7) 0.6266(6) 0.4382(10) 0.0481(13) Uani 1 d . . 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 Cd 0.0445(12) 0.0233(10) 0.0437(12) 0.000 0.0354(11) 0.000 Sn 0.0271(7) 0.0224(8) 0.0246(7) 0.000 0.0201(6) 0.000 Na1 0.059(7) 0.108(20) 0.052(6) 0.000 0.042(6) 0.000 Na2 0.050(7) 0.101(18) 0.040(6) 0.000 0.033(6) 0.000 S1 0.046(2) 0.064(3) 0.034(2) -0.007(2) 0.031(2) -0.019(2) S2 0.033(2) 0.074(3) 0.041(2) 0.033(3) 0.028(2) 0.015(2) _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 Cd S2 2.502(5) 3_445 ? Cd S2 2.502(5) 4_546 ? Cd S1 2.515(6) 3_445 ? Cd S1 2.515(6) 4_546 ? Cd Na1 3.839(10) 1_545 ? Cd Na1 3.839(10) 1_546 ? Sn S1 2.373(5) . ? Sn S1 2.373(5) 2 ? Sn S2 2.382(5) 4_545 ? Sn S2 2.382(5) 3_445 ? Na1 S1 2.726(8) 4 ? Na1 S1 2.726(8) 3_455 ? Na1 S2 3.078(13) 1_454 ? Na1 S2 3.078(13) 2_656 ? Na1 Cd 3.839(10) 1_565 ? Na1 Cd 3.839(10) 1_564 ? Na1 Na2 3.997(14) 3 ? Na1 Na2 3.997(13) 3_454 ? Na1 Na2 4.103(14) 1_554 ? Na1 Na2 4.103(14) . ? Na2 S2 2.591(8) 2_656 ? Na2 S2 2.591(8) 1_455 ? Na2 S1 2.872(13) 2 ? Na2 S1 2.872(13) 1_556 ? Na2 Na1 3.997(14) 3_445 ? Na2 Na1 3.997(13) 3_546 ? Na2 Na1 4.103(14) 1_556 ? S1 Cd 2.515(6) 3 ? S1 Na1 2.726(8) 3_545 ? S1 Na2 2.872(13) 1_554 ? S2 Sn 2.382(5) 3 ? S2 Cd 2.502(5) 3 ? S2 Na2 2.591(8) 1_655 ? S2 Na1 3.078(13) 1_656 ? 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 S2 Cd S2 125.7(3) 3_445 4_546 ? S2 Cd S1 101.8(2) 3_445 3_445 ? S2 Cd S1 102.4(2) 4_546 3_445 ? S2 Cd S1 102.4(2) 3_445 4_546 ? S2 Cd S1 101.8(2) 4_546 4_546 ? S1 Cd S1 125.3(3) 3_445 4_546 ? S2 Cd Na1 68.2(3) 3_445 1_545 ? S2 Cd Na1 146.96(12) 4_546 1_545 ? S1 Cd Na1 45.1(2) 3_445 1_545 ? S1 Cd Na1 103.6(2) 4_546 1_545 ? S2 Cd Na1 146.96(12) 3_445 1_546 ? S2 Cd Na1 68.2(3) 4_546 1_546 ? S1 Cd Na1 103.6(2) 3_445 1_546 ? S1 Cd Na1 45.1(2) 4_546 1_546 ? Na1 Cd Na1 118.3(5) 1_545 1_546 ? S1 Sn S1 119.1(3) . 2 ? S1 Sn S2 105.0(2) . 4_545 ? S1 Sn S2 104.8(2) 2 4_545 ? S1 Sn S2 104.8(2) . 3_445 ? S1 Sn S2 105.0(2) 2 3_445 ? S2 Sn S2 118.9(3) 4_545 3_445 ? S1 Na1 S1 145.4(8) 4 3_455 ? S1 Na1 S2 98.7(2) 4 1_454 ? S1 Na1 S2 99.2(2) 3_455 1_454 ? S1 Na1 S2 99.2(2) 4 2_656 ? S1 Na1 S2 98.7(2) 3_455 2_656 ? S2 Na1 S2 117.3(7) 1_454 2_656 ? S1 Na1 Cd 116.9(5) 4 1_565 ? S1 Na1 Cd 40.8(2) 3_455 1_565 ? S2 Na1 Cd 139.89(12) 1_454 1_565 ? S2 Na1 Cd 76.61(14) 2_656 1_565 ? S1 Na1 Cd 40.8(2) 4 1_564 ? S1 Na1 Cd 116.9(5) 3_455 1_564 ? S2 Na1 Cd 76.61(14) 1_454 1_564 ? S2 Na1 Cd 139.89(12) 2_656 1_564 ? Cd Na1 Cd 118.3(5) 1_565 1_564 ? S1 Na1 Na2 45.9(2) 4 3 ? S1 Na1 Na2 111.0(4) 3_455 3 ? S2 Na1 Na2 144.56(12) 1_454 3 ? S2 Na1 Na2 77.0(3) 2_656 3 ? Cd Na1 Na2 72.8(2) 1_565 3 ? Cd Na1 Na2 73.4(2) 1_564 3 ? S1 Na1 Na2 111.0(4) 4 3_454 ? S1 Na1 Na2 45.9(2) 3_455 3_454 ? S2 Na1 Na2 77.0(3) 1_454 3_454 ? S2 Na1 Na2 144.56(12) 2_656 3_454 ? Cd Na1 Na2 73.4(2) 1_565 3_454 ? Cd Na1 Na2 72.8(2) 1_564 3_454 ? Na2 Na1 Na2 110.9(5) 3 3_454 ? S1 Na1 Na2 67.1(3) 4 1_554 ? S1 Na1 Na2 138.0(3) 3_455 1_554 ? S2 Na1 Na2 39.1(2) 1_454 1_554 ? S2 Na1 Na2 99.0(4) 2_656 1_554 ? Cd Na1 Na2 174.3(4) 1_565 1_554 ? Cd Na1 Na2 67.4(2) 1_564 1_554 ? Na2 Na1 Na2 110.04(8) 3 1_554 ? Na2 Na1 Na2 109.45(11) 3_454 1_554 ? S1 Na1 Na2 138.0(3) 4 . ? S1 Na1 Na2 67.1(3) 3_455 . ? S2 Na1 Na2 99.0(4) 1_454 . ? S2 Na1 Na2 39.1(2) 2_656 . ? Cd Na1 Na2 67.4(2) 1_565 . ? Cd Na1 Na2 174.3(4) 1_564 . ? Na2 Na1 Na2 109.45(11) 3 . ? Na2 Na1 Na2 110.04(8) 3_454 . ? Na2 Na1 Na2 106.9(5) 1_554 . ? S2 Na2 S2 142.1(9) 2_656 1_455 ? S2 Na2 S1 99.7(2) 2_656 2 ? S2 Na2 S1 99.3(2) 1_455 2 ? S2 Na2 S1 99.3(2) 2_656 1_556 ? S2 Na2 S1 99.7(2) 1_455 1_556 ? S1 Na2 S1 119.1(7) 2 1_556 ? S2 Na2 Na1 142.6(3) 2_656 3_445 ? S2 Na2 Na1 64.8(3) 1_455 3_445 ? S1 Na2 Na1 43.0(2) 2 3_445 ? S1 Na2 Na1 99.0(4) 1_556 3_445 ? S2 Na2 Na1 64.8(3) 2_656 3_546 ? S2 Na2 Na1 142.6(3) 1_455 3_546 ? S1 Na2 Na1 99.0(4) 2 3_546 ? S1 Na2 Na1 43.0(2) 1_556 3_546 ? Na1 Na2 Na1 110.9(5) 3_445 3_546 ? S2 Na2 Na1 106.0(4) 2_656 1_556 ? S2 Na2 Na1 48.6(3) 1_455 1_556 ? S1 Na2 Na1 147.7(2) 2 1_556 ? S1 Na2 Na1 76.0(3) 1_556 1_556 ? Na1 Na2 Na1 110.04(8) 3_445 1_556 ? Na1 Na2 Na1 109.45(11) 3_546 1_556 ? S2 Na2 Na1 48.6(3) 2_656 . ? S2 Na2 Na1 106.0(4) 1_455 . ? S1 Na2 Na1 76.0(3) 2 . ? S1 Na2 Na1 147.7(2) 1_556 . ? Na1 Na2 Na1 109.45(11) 3_445 . ? Na1 Na2 Na1 110.04(8) 3_546 . ? Na1 Na2 Na1 106.9(5) 1_556 . ? Sn S1 Cd 111.9(2) . 3 ? Sn S1 Na1 131.9(5) . 3_545 ? Cd S1 Na1 94.1(3) 3 3_545 ? Sn S1 Na2 107.3(2) . 1_554 ? Cd S1 Na2 120.7(4) 3 1_554 ? Na1 S1 Na2 91.1(3) 3_545 1_554 ? Sn S2 Cd 112.0(2) 3 3 ? Sn S2 Na2 102.4(3) 3 1_655 ? Cd S2 Na2 131.9(5) 3 1_655 ? Sn S2 Na1 117.9(4) 3 1_656 ? Cd S2 Na1 99.8(2) 3 1_656 ? Na2 S2 Na1 92.3(3) 1_655 1_656 ? _refine_diff_density_max 3.613 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.387 #===END data_sus3 _database_code_CSD 173900 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Na6CdSn4S12' _chemical_formula_weight 1109.98 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Na' 'Na' 0.0362 0.0249 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -1.0050 1.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 6.622(4) _cell_length_b 11.489(8) _cell_length_c 6.999(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.56(4) _cell_angle_gamma 90.00 _cell_volume 504.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.01 _cell_measurement_theta_max 13.40 _exptl_crystal_description 'needle shaped' _exptl_crystal_colour 'brownish yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.651 _exptl_crystal_density_method ? _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 7.198 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7204 _exptl_absorpt_correction_T_max 0.9580 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 0% _diffrn_reflns_number 970 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 24.89 _reflns_number_total 470 _reflns_number_observed 453 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 program' _computing_cell_refinement 'CAD4 program' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+1.4186P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0122(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 470 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_obs 0.0243 _refine_ls_wR_factor_all 0.0773 _refine_ls_wR_factor_obs 0.0768 _refine_ls_goodness_of_fit_all 1.221 _refine_ls_goodness_of_fit_obs 1.236 _refine_ls_restrained_S_all 1.221 _refine_ls_restrained_S_obs 1.236 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn Sn 0.0000 0.16754(3) 0.5000 0.0063(3) Uani 1 d S . Cd Cd 0.5000 0.0000 0.5000 0.0187(4) Uani 0.50 d SP . S1 S 0.2166(3) 0.0000 0.7186(3) 0.0096(4) Uani 1 d S . S2 S 0.2471(2) 0.17855(11) 0.2809(2) 0.0105(4) Uani 1 d . . Na1 Na 0.5000 0.1601(2) 0.0000 0.0177(9) Uani 1 d S . Na2 Na 0.0000 0.0000 0.0000 0.0177(10) Uani 1 d S . 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 Sn 0.0069(4) 0.0056(4) 0.0066(4) 0.000 0.0025(2) 0.000 Cd 0.0158(8) 0.0145(8) 0.0264(9) 0.000 0.0078(7) 0.000 S1 0.0145(8) 0.0081(8) 0.0049(7) 0.000 0.0013(6) 0.000 S2 0.0116(7) 0.0145(7) 0.0054(7) -0.0018(4) 0.0029(5) -0.0040(4) Na1 0.018(2) 0.017(2) 0.015(2) 0.000 0.0016(14) 0.000 Na2 0.021(2) 0.020(2) 0.015(2) 0.000 0.010(2) 0.000 _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 Sn S2 2.577(2) 2_556 ? Sn S2 2.577(2) . ? Sn S2 2.578(2) 7_556 ? Sn S2 2.578(2) 8_455 ? Sn S1 2.590(2) 5_556 ? Sn S1 2.590(2) . ? Cd S1 2.774(2) 5_656 ? Cd S1 2.774(2) . ? Cd S2 2.780(2) 6 ? Cd S2 2.780(2) 2_656 ? Cd S2 2.780(2) . ? Cd S2 2.780(2) 5_656 ? S1 Sn 2.590(2) 5_556 ? S1 Na2 2.781(2) 1_556 ? S1 Na1 2.904(2) 1_556 ? S1 Na1 2.904(2) 5_656 ? S2 Sn 2.578(2) 7_556 ? S2 Na1 2.816(2) 7 ? S2 Na2 2.950(2) . ? S2 Na1 2.968(2) . ? Na1 S2 2.816(2) 8 ? Na1 S2 2.816(2) 7 ? Na1 S1 2.904(2) 1_554 ? Na1 S1 2.904(2) 5_656 ? Na1 S2 2.968(2) 2_655 ? Na1 Na1 3.679(6) 5_655 ? Na1 Na2 3.788(2) . ? Na1 Na2 3.788(2) 1_655 ? Na1 Na1 3.903(3) 7_655 ? Na1 Na1 3.903(3) 7 ? Na1 Na2 3.905(4) 3 ? Na2 S1 2.781(2) 5_556 ? Na2 S1 2.781(2) 1_554 ? Na2 S2 2.950(2) 5 ? Na2 S2 2.950(2) 2 ? Na2 S2 2.950(2) 6 ? Na2 Na1 3.788(2) 5 ? Na2 Na1 3.788(2) 5_655 ? Na2 Na1 3.788(2) 1_455 ? Na2 Na1 3.905(4) 7 ? Na2 Na1 3.905(4) 3_445 ? 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 S2 Sn S2 174.37(6) 2_556 . ? S2 Sn S2 91.59(5) 2_556 7_556 ? S2 Sn S2 84.54(6) . 7_556 ? S2 Sn S2 84.54(6) 2_556 8_455 ? S2 Sn S2 91.59(5) . 8_455 ? S2 Sn S2 93.39(8) 7_556 8_455 ? S2 Sn S1 92.92(6) 2_556 5_556 ? S2 Sn S1 91.26(5) . 5_556 ? S2 Sn S1 173.66(5) 7_556 5_556 ? S2 Sn S1 91.48(7) 8_455 5_556 ? S2 Sn S1 91.26(5) 2_556 . ? S2 Sn S1 92.92(6) . . ? S2 Sn S1 91.48(7) 7_556 . ? S2 Sn S1 173.66(5) 8_455 . ? S1 Sn S1 83.97(8) 5_556 . ? S1 Cd S1 180.0 5_656 . ? S1 Cd S2 95.18(5) 5_656 6 ? S1 Cd S2 84.82(5) . 6 ? S1 Cd S2 84.82(5) 5_656 2_656 ? S1 Cd S2 95.18(5) . 2_656 ? S2 Cd S2 180.0 6 2_656 ? S1 Cd S2 95.18(5) 5_656 . ? S1 Cd S2 84.82(5) . . ? S2 Cd S2 95.11(8) 6 . ? S2 Cd S2 84.89(8) 2_656 . ? S1 Cd S2 84.82(5) 5_656 5_656 ? S1 Cd S2 95.18(5) . 5_656 ? S2 Cd S2 84.89(8) 6 5_656 ? S2 Cd S2 95.11(8) 2_656 5_656 ? S2 Cd S2 180.0 . 5_656 ? Sn S1 Sn 96.03(8) 5_556 . ? Sn S1 Cd 91.07(5) 5_556 . ? Sn S1 Cd 91.07(5) . . ? Sn S1 Na2 96.03(6) 5_556 1_556 ? Sn S1 Na2 96.03(6) . 1_556 ? Cd S1 Na2 169.36(7) . 1_556 ? Sn S1 Na1 171.28(7) 5_556 1_556 ? Sn S1 Na1 92.67(6) . 1_556 ? Cd S1 Na1 88.24(6) . 1_556 ? Na2 S1 Na1 83.54(5) 1_556 1_556 ? Sn S1 Na1 92.67(6) 5_556 5_656 ? Sn S1 Na1 171.28(7) . 5_656 ? Cd S1 Na1 88.24(6) . 5_656 ? Na2 S1 Na1 83.54(5) 1_556 5_656 ? Na1 S1 Na1 78.62(10) 1_556 5_656 ? Sn S2 Sn 95.46(6) . 7_556 ? Sn S2 Cd 91.19(5) . . ? Sn S2 Cd 90.86(7) 7_556 . ? Sn S2 Na1 96.29(5) . 7 ? Sn S2 Na1 94.98(7) 7_556 7 ? Cd S2 Na1 170.02(6) . 7 ? Sn S2 Na2 92.27(5) . . ? Sn S2 Na2 172.19(6) 7_556 . ? Cd S2 Na2 87.90(6) . . ? Na1 S2 Na2 85.22(7) 7 . ? Sn S2 Na1 171.68(7) . . ? Sn S2 Na1 92.66(6) 7_556 . ? Cd S2 Na1 86.84(6) . . ? Na1 S2 Na1 84.81(6) 7 . ? Na2 S2 Na1 79.58(6) . . ? S2 Na1 S2 97.68(10) 8 7 ? S2 Na1 S1 175.52(5) 8 1_554 ? S2 Na1 S1 80.62(7) 7 1_554 ? S2 Na1 S1 80.62(7) 8 5_656 ? S2 Na1 S1 175.52(5) 7 5_656 ? S1 Na1 S1 101.38(10) 1_554 5_656 ? S2 Na1 S2 79.37(6) 8 . ? S2 Na1 S2 95.19(6) 7 . ? S1 Na1 S2 96.62(6) 1_554 . ? S1 Na1 S2 88.58(6) 5_656 . ? S2 Na1 S2 95.19(6) 8 2_655 ? S2 Na1 S2 79.37(6) 7 2_655 ? S1 Na1 S2 88.58(6) 1_554 2_655 ? S1 Na1 S2 96.62(6) 5_656 2_655 ? S2 Na1 S2 171.81(11) . 2_655 ? S2 Na1 Na1 131.16(5) 8 5_655 ? S2 Na1 Na1 131.16(5) 7 5_655 ? S1 Na1 Na1 50.69(5) 1_554 5_655 ? S1 Na1 Na1 50.69(5) 5_656 5_655 ? S2 Na1 Na1 94.09(6) . 5_655 ? S2 Na1 Na1 94.09(6) 2_655 5_655 ? S2 Na1 Na2 129.30(4) 8 . ? S2 Na1 Na2 90.34(5) 7 . ? S1 Na1 Na2 46.84(5) 1_554 . ? S1 Na1 Na2 93.94(8) 5_656 . ? S2 Na1 Na2 50.00(4) . . ? S2 Na1 Na2 135.41(6) 2_655 . ? Na1 Na1 Na2 60.94(4) 5_655 . ? S2 Na1 Na2 90.34(5) 8 1_655 ? S2 Na1 Na2 129.30(4) 7 1_655 ? S1 Na1 Na2 93.94(8) 1_554 1_655 ? S1 Na1 Na2 46.84(5) 5_656 1_655 ? S2 Na1 Na2 135.41(6) . 1_655 ? S2 Na1 Na2 50.00(4) 2_655 1_655 ? Na1 Na1 Na2 60.94(4) 5_655 1_655 ? Na2 Na1 Na2 121.89(8) . 1_655 ? S2 Na1 Na1 49.24(5) 8 7_655 ? S2 Na1 Na1 87.49(9) 7 7_655 ? S1 Na1 Na1 134.48(5) 1_554 7_655 ? S1 Na1 Na1 88.28(6) 5_656 7_655 ? S2 Na1 Na1 128.30(8) . 7_655 ? S2 Na1 Na1 45.95(4) 2_655 7_655 ? Na1 Na1 Na1 121.96(7) 5_655 7_655 ? Na2 Na1 Na1 177.10(10) . 7_655 ? Na2 Na1 Na1 61.01(5) 1_655 7_655 ? S2 Na1 Na1 87.49(9) 8 7 ? S2 Na1 Na1 49.24(5) 7 7 ? S1 Na1 Na1 88.28(6) 1_554 7 ? S1 Na1 Na1 134.48(5) 5_656 7 ? S2 Na1 Na1 45.95(4) . 7 ? S2 Na1 Na1 128.30(8) 2_655 7 ? Na1 Na1 Na1 121.96(7) 5_655 7 ? Na2 Na1 Na1 61.01(5) . 7 ? Na2 Na1 Na1 177.10(10) 1_655 7 ? Na1 Na1 Na1 116.09(13) 7_655 7 ? S2 Na1 Na2 48.84(5) 8 3 ? S2 Na1 Na2 48.84(5) 7 3 ? S1 Na1 Na2 129.31(5) 1_554 3 ? S1 Na1 Na2 129.31(5) 5_656 3 ? S2 Na1 Na2 85.91(6) . 3 ? S2 Na1 Na2 85.91(6) 2_655 3 ? Na1 Na1 Na2 180.0 5_655 3 ? Na2 Na1 Na2 119.06(4) . 3 ? Na2 Na1 Na2 119.06(4) 1_655 3 ? Na1 Na1 Na2 58.04(7) 7_655 3 ? Na1 Na1 Na2 58.04(7) 7 3 ? S1 Na2 S1 180.0 5_556 1_554 ? S1 Na2 S2 80.20(5) 5_556 . ? S1 Na2 S2 99.80(5) 1_554 . ? S1 Na2 S2 99.80(5) 5_556 5 ? S1 Na2 S2 80.20(5) 1_554 5 ? S2 Na2 S2 180.0 . 5 ? S1 Na2 S2 99.80(5) 5_556 2 ? S1 Na2 S2 80.20(5) 1_554 2 ? S2 Na2 S2 91.89(7) . 2 ? S2 Na2 S2 88.11(7) 5 2 ? S1 Na2 S2 80.20(5) 5_556 6 ? S1 Na2 S2 99.80(5) 1_554 6 ? S2 Na2 S2 88.11(7) . 6 ? S2 Na2 S2 91.89(7) 5 6 ? S2 Na2 S2 180.0 2 6 ? S1 Na2 Na1 49.62(4) 5_556 5 ? S1 Na2 Na1 130.38(4) 1_554 5 ? S2 Na2 Na1 129.58(4) . 5 ? S2 Na2 Na1 50.42(4) 5 5 ? S2 Na2 Na1 92.19(6) 2 5 ? S2 Na2 Na1 87.81(6) 6 5 ? S1 Na2 Na1 130.38(4) 5_556 . ? S1 Na2 Na1 49.62(4) 1_554 . ? S2 Na2 Na1 50.42(4) . . ? S2 Na2 Na1 129.58(4) 5 . ? S2 Na2 Na1 87.81(6) 2 . ? S2 Na2 Na1 92.19(6) 6 . ? Na1 Na2 Na1 180.0 5 . ? S1 Na2 Na1 130.38(4) 5_556 5_655 ? S1 Na2 Na1 49.62(4) 1_554 5_655 ? S2 Na2 Na1 92.19(6) . 5_655 ? S2 Na2 Na1 87.81(6) 5 5_655 ? S2 Na2 Na1 129.58(4) 2 5_655 ? S2 Na2 Na1 50.42(4) 6 5_655 ? Na1 Na2 Na1 121.89(8) 5 5_655 ? Na1 Na2 Na1 58.11(8) . 5_655 ? S1 Na2 Na1 49.62(4) 5_556 1_455 ? S1 Na2 Na1 130.38(4) 1_554 1_455 ? S2 Na2 Na1 87.81(6) . 1_455 ? S2 Na2 Na1 92.19(6) 5 1_455 ? S2 Na2 Na1 50.42(4) 2 1_455 ? S2 Na2 Na1 129.58(4) 6 1_455 ? Na1 Na2 Na1 58.11(8) 5 1_455 ? Na1 Na2 Na1 121.89(8) . 1_455 ? Na1 Na2 Na1 180.0 5_655 1_455 ? S1 Na2 Na1 90.0 5_556 7 ? S1 Na2 Na1 90.0 1_554 7 ? S2 Na2 Na1 45.94(4) . 7 ? S2 Na2 Na1 134.06(4) 5 7 ? S2 Na2 Na1 45.94(4) 2 7 ? S2 Na2 Na1 134.06(4) 6 7 ? Na1 Na2 Na1 119.06(4) 5 7 ? Na1 Na2 Na1 60.94(4) . 7 ? Na1 Na2 Na1 119.06(4) 5_655 7 ? Na1 Na2 Na1 60.94(4) 1_455 7 ? S1 Na2 Na1 90.0 5_556 3_445 ? S1 Na2 Na1 90.0 1_554 3_445 ? S2 Na2 Na1 134.06(4) . 3_445 ? S2 Na2 Na1 45.94(4) 5 3_445 ? S2 Na2 Na1 134.06(4) 2 3_445 ? S2 Na2 Na1 45.94(4) 6 3_445 ? Na1 Na2 Na1 60.94(4) 5 3_445 ? Na1 Na2 Na1 119.06(4) . 3_445 ? Na1 Na2 Na1 60.94(4) 5_655 3_445 ? Na1 Na2 Na1 119.06(4) 1_455 3_445 ? Na1 Na2 Na1 180.0 7 3_445 ? _refine_diff_density_max 0.882 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.222 #===END