data_pd3ag2s _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag2 Pd3 S' _chemical_formula_weight 567.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 212 _space_group_name_H-M_alt 'P 43 3 2' _space_group_name_Hall 'P 4acd 2ab 3' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, -x+3/4, z+1/4' '-y+3/4, x+1/4, z+3/4' 'x+1/4, z+3/4, -y+3/4' '-x+3/4, z+1/4, y+3/4' '-x+1/4, -z+1/4, -y+1/4' 'x+3/4, -z+3/4, y+1/4' 'z+1/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+1/4' '-z+3/4, y+1/4, x+3/4' '-z+1/4, -y+1/4, -x+1/4' _cell_length_a 7.2470(8) _cell_length_b 7.2470(8) _cell_length_c 7.2470(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 380.61(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 9.895 _exptl_crystal_F_000 992 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 24.311 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4414 _diffrn_reflns_av_unetI/netI 0.0060 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.977 _diffrn_reflns_theta_max 30.164 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 196 _reflns_number_gt 196 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.361 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0066P)^2^+1.1973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 52 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(2) _chemical_absolute_configuration ? _refine_ls_number_reflns 196 _refine_ls_number_parameters 13 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0107 _refine_ls_R_factor_gt 0.0107 _refine_ls_wR_factor_ref 0.0269 _refine_ls_wR_factor_gt 0.0269 _refine_ls_goodness_of_fit_ref 1.456 _refine_ls_restrained_S_all 1.456 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.1250 0.69456(5) 0.55544(5) 0.01456(14) Uani 0.996(12) 2 d S T . . . Ag Ag 0.05751(4) 0.55751(4) 0.94249(4) 0.01578(17) Uani 0.996(12) 3 d S T . . . S S 0.3750 0.8750 0.6250 0.0118(7) Uani 1 6 d S T 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 Pd 0.0124(2) 0.01563(16) 0.01563(16) -0.00299(16) -0.00190(11) -0.00190(11) Ag 0.01578(17) 0.01578(17) 0.01578(17) -0.00051(12) -0.00051(12) 0.00051(12) S 0.0118(7) 0.0118(7) 0.0118(7) 0.0002(5) 0.0002(5) -0.0002(5) _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 Pd S 2.2905(3) 4_466 ? Pd S 2.2905(3) . ? Pd Ag 2.9441(6) 15_454 ? Pd Ag 2.9441(6) 3_556 ? Pd Pd 2.9832(5) 12_565 ? Pd Pd 2.9832(5) 8_656 ? Pd Pd 2.9833(5) 6_456 ? Pd Pd 2.9833(5) 11_466 ? Pd Ag 3.0155(7) 16_554 ? Pd Ag 3.0156(7) . ? Pd Ag 3.0497(4) 2_564 ? Pd Ag 3.0497(4) 13_456 ? Ag Ag 2.7426(4) 15_455 ? Ag Ag 2.7426(4) 16_554 ? Ag Ag 2.7426(4) 13_456 ? Ag Pd 2.9441(6) 3_546 ? Ag Pd 2.9441(6) 6_457 ? Ag Pd 2.9441(6) 9_456 ? Ag Pd 3.0156(7) 11_466 ? Ag Pd 3.0156(7) 8_656 ? Ag Pd 3.0497(4) 12_565 ? Ag Pd 3.0497(4) 7_565 ? Ag Pd 3.0497(4) 2_565 ? S Pd 2.2905(3) 5_565 ? S Pd 2.2905(3) 11_466 ? S Pd 2.2905(3) 10_655 ? S Pd 2.2905(3) 4_566 ? S Pd 2.2905(3) 8_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 Pd S 151.27(2) 4_466 . ? S Pd Ag 81.036(9) 4_466 15_454 ? S Pd Ag 81.036(9) . 15_454 ? S Pd Ag 81.036(9) 4_466 3_556 ? S Pd Ag 81.036(9) . 3_556 ? Ag Pd Ag 102.18(2) 15_454 3_556 ? S Pd Pd 49.367(8) 4_466 12_565 ? S Pd Pd 157.451(15) . 12_565 ? Ag Pd Pd 119.776(5) 15_454 12_565 ? Ag Pd Pd 101.126(9) 3_556 12_565 ? S Pd Pd 157.451(15) 4_466 8_656 ? S Pd Pd 49.367(8) . 8_656 ? Ag Pd Pd 101.126(9) 15_454 8_656 ? Ag Pd Pd 119.776(5) 3_556 8_656 ? Pd Pd Pd 113.415(3) 12_565 8_656 ? S Pd Pd 49.367(8) 4_466 6_456 ? S Pd Pd 135.275(7) . 6_456 ? Ag Pd Pd 61.926(5) 15_454 6_456 ? Ag Pd Pd 128.367(4) 3_556 6_456 ? Pd Pd Pd 60.0 12_565 6_456 ? Pd Pd Pd 111.644(5) 8_656 6_456 ? S Pd Pd 135.275(7) 4_466 11_466 ? S Pd Pd 49.366(8) . 11_466 ? Ag Pd Pd 128.367(4) 15_454 11_466 ? Ag Pd Pd 61.926(5) 3_556 11_466 ? Pd Pd Pd 111.644(5) 12_565 11_466 ? Pd Pd Pd 60.0 8_656 11_466 ? Pd Pd Pd 166.276(8) 6_456 11_466 ? S Pd Ag 96.409(11) 4_466 16_554 ? S Pd Ag 109.284(13) . 16_554 ? Ag Pd Ag 102.513(8) 15_454 16_554 ? Ag Pd Ag 154.449(13) 3_556 16_554 ? Pd Pd Ag 60.355(5) 12_565 16_554 ? Pd Pd Ag 61.111(9) 8_656 16_554 ? Pd Pd Ag 60.354(5) 6_456 16_554 ? Pd Pd Ag 106.369(10) 11_466 16_554 ? S Pd Ag 109.284(13) 4_466 . ? S Pd Ag 96.409(11) . . ? Ag Pd Ag 154.449(13) 15_454 . ? Ag Pd Ag 102.513(8) 3_556 . ? Pd Pd Ag 61.111(9) 12_565 . ? Pd Pd Ag 60.355(5) 8_656 . ? Pd Pd Ag 106.369(10) 6_456 . ? Pd Pd Ag 60.355(5) 11_466 . ? Ag Pd Ag 54.097(9) 16_554 . ? S Pd Ag 108.162(10) 4_466 2_564 ? S Pd Ag 78.713(10) . 2_564 ? Ag Pd Ag 54.426(10) 15_454 2_564 ? Ag Pd Ag 151.094(17) 3_556 2_564 ? Pd Pd Ag 105.502(8) 12_565 2_564 ? Pd Pd Ag 58.407(15) 8_656 2_564 ? Pd Pd Ag 59.968(12) 6_456 2_564 ? Pd Pd Ag 116.400(14) 11_466 2_564 ? Ag Pd Ag 53.764(5) 16_554 2_564 ? Ag Pd Ag 100.064(12) . 2_564 ? S Pd Ag 78.713(10) 4_466 13_456 ? S Pd Ag 108.162(10) . 13_456 ? Ag Pd Ag 151.094(17) 15_454 13_456 ? Ag Pd Ag 54.426(10) 3_556 13_456 ? Pd Pd Ag 58.407(15) 12_565 13_456 ? Pd Pd Ag 105.502(8) 8_656 13_456 ? Pd Pd Ag 116.400(14) 6_456 13_456 ? Pd Pd Ag 59.968(12) 11_466 13_456 ? Ag Pd Ag 100.064(12) 16_554 13_456 ? Ag Pd Ag 53.764(5) . 13_456 ? Ag Pd Ag 152.964(18) 2_564 13_456 ? Ag Ag Ag 115.873(5) 15_455 16_554 ? Ag Ag Ag 115.873(5) 15_455 13_456 ? Ag Ag Ag 115.873(5) 16_554 13_456 ? Ag Ag Pd 127.739(16) 15_455 3_546 ? Ag Ag Pd 64.750(8) 16_554 3_546 ? Ag Ag Pd 107.171(1) 13_456 3_546 ? Ag Ag Pd 64.750(7) 15_455 6_457 ? Ag Ag Pd 107.171(1) 16_554 6_457 ? Ag Ag Pd 127.739(16) 13_456 6_457 ? Pd Ag Pd 65.909(16) 3_546 6_457 ? Ag Ag Pd 107.171(1) 15_455 9_456 ? Ag Ag Pd 127.739(16) 16_554 9_456 ? Ag Ag Pd 64.750(8) 13_456 9_456 ? Pd Ag Pd 65.909(16) 3_546 9_456 ? Pd Ag Pd 65.909(16) 6_457 9_456 ? Ag Ag Pd 112.944(13) 15_455 . ? Ag Ag Pd 62.951(5) 16_554 . ? Ag Ag Pd 63.755(10) 13_456 . ? Pd Ag Pd 111.830(10) 3_546 . ? Pd Ag Pd 168.463(8) 6_457 . ? Pd Ag Pd 124.365(3) 9_456 . ? Ag Ag Pd 63.755(10) 15_455 11_466 ? Ag Ag Pd 112.944(13) 16_554 11_466 ? Ag Ag Pd 62.952(5) 13_456 11_466 ? Pd Ag Pd 168.464(8) 3_546 11_466 ? Pd Ag Pd 124.364(3) 6_457 11_466 ? Pd Ag Pd 111.830(10) 9_456 11_466 ? Pd Ag Pd 59.292(10) . 11_466 ? Ag Ag Pd 62.952(5) 15_455 8_656 ? Ag Ag Pd 63.755(10) 16_554 8_656 ? Ag Ag Pd 112.944(13) 13_456 8_656 ? Pd Ag Pd 124.365(4) 3_546 8_656 ? Pd Ag Pd 111.830(10) 6_457 8_656 ? Pd Ag Pd 168.464(8) 9_456 8_656 ? Pd Ag Pd 59.292(10) . 8_656 ? Pd Ag Pd 59.292(10) 11_466 8_656 ? Ag Ag Pd 171.809(19) 15_455 12_565 ? Ag Ag Pd 62.482(13) 16_554 12_565 ? Ag Ag Pd 60.824(15) 13_456 12_565 ? Pd Ag Pd 59.667(10) 3_546 12_565 ? Pd Ag Pd 123.395(17) 6_457 12_565 ? Pd Ag Pd 78.606(8) 9_456 12_565 ? Pd Ag Pd 58.922(5) . 12_565 ? Pd Ag Pd 108.939(11) 11_466 12_565 ? Pd Ag Pd 110.621(11) 8_656 12_565 ? Ag Ag Pd 60.824(15) 15_455 7_565 ? Ag Ag Pd 171.809(19) 16_554 7_565 ? Ag Ag Pd 62.482(13) 13_456 7_565 ? Pd Ag Pd 123.395(17) 3_546 7_565 ? Pd Ag Pd 78.606(8) 6_457 7_565 ? Pd Ag Pd 59.667(10) 9_456 7_565 ? Pd Ag Pd 110.622(11) . 7_565 ? Pd Ag Pd 58.922(5) 11_466 7_565 ? Pd Ag Pd 108.939(11) 8_656 7_565 ? Pd Ag Pd 119.579(2) 12_565 7_565 ? Ag Ag Pd 62.482(13) 15_455 2_565 ? Ag Ag Pd 60.824(15) 16_554 2_565 ? Ag Ag Pd 171.809(19) 13_456 2_565 ? Pd Ag Pd 78.606(8) 3_546 2_565 ? Pd Ag Pd 59.667(10) 6_457 2_565 ? Pd Ag Pd 123.395(17) 9_456 2_565 ? Pd Ag Pd 108.938(11) . 2_565 ? Pd Ag Pd 110.621(11) 11_466 2_565 ? Pd Ag Pd 58.922(5) 8_656 2_565 ? Pd Ag Pd 119.579(2) 12_565 2_565 ? Pd Ag Pd 119.579(2) 7_565 2_565 ? Pd S Pd 88.72(2) 5_565 11_466 ? Pd S Pd 81.267(16) 5_565 10_655 ? Pd S Pd 111.984(4) 11_466 10_655 ? Pd S Pd 81.267(16) 5_565 4_566 ? Pd S Pd 162.094(13) 11_466 4_566 ? Pd S Pd 81.267(16) 10_655 4_566 ? Pd S Pd 111.984(4) 5_565 8_656 ? Pd S Pd 81.267(16) 11_466 8_656 ? Pd S Pd 162.094(13) 10_655 8_656 ? Pd S Pd 88.72(2) 4_566 8_656 ? Pd S Pd 162.094(13) 5_565 . ? Pd S Pd 81.267(16) 11_466 . ? Pd S Pd 88.73(2) 10_655 . ? Pd S Pd 111.985(4) 4_566 . ? Pd S Pd 81.266(16) 8_656 . ? _refine_diff_density_max 0.387 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.145 _shelxl_version_number 2014/6 _shelx_res_file ; TITL pd3ag2s in P4(3)32 CELL 0.71073 7.2470 7.2470 7.2470 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0008 0.0008 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SYMM Z, X, Y SYMM 0.5+Z, 0.5-X, -Y SYMM 0.5-Z, -X, 0.5+Y SYMM -Z, 0.5+X, 0.5-Y SYMM Y, Z, X SYMM -Y, 0.5+Z, 0.5-X SYMM 0.5+Y, 0.5-Z, -X SYMM 0.5-Y, -Z, 0.5+X SYMM 0.25+Y, 0.75+X, 0.75-Z SYMM 0.25-Y, 0.25-X, 0.25-Z SYMM 0.75+Y, 0.75-X, 0.25+Z SYMM 0.75-Y, 0.25+X, 0.75+Z SYMM 0.25+X, 0.75+Z, 0.75-Y SYMM 0.75-X, 0.25+Z, 0.75+Y SYMM 0.25-X, 0.25-Z, 0.25-Y SYMM 0.75+X, 0.75-Z, 0.25+Y SYMM 0.25+Z, 0.75+Y, 0.75-X SYMM 0.75+Z, 0.75-Y, 0.25+X SYMM 0.75-Z, 0.25+Y, 0.75+X SYMM 0.25-Z, 0.25-Y, 0.25-X SFAC S PD AG UNIT 4 12 8 L.S. 10 BOND FMAP 2 PLAN 20 ACTA WGHT 0.006600 1.197300 FVAR 0.30057 PD 2 0.125000 0.694558 0.555442 0.49783 0.01241 0.01563 = 0.01563 -0.00299 -0.00190 -0.00190 AG 3 0.057506 0.557506 0.942494 0.33202 0.01578 0.01578 = 0.01578 -0.00051 -0.00051 0.00051 S 1 0.375000 0.875000 0.625000 10.16667 0.01182 0.01182 = 0.01182 0.00017 0.00017 -0.00017 HKLF 4 REM pd3ag2s in P4(3)32 REM R1 = 0.0107 for 196 Fo > 4sig(Fo) and 0.0107 for all 196 data REM 13 parameters refined using 0 restraints END WGHT 0.0065 1.2564 REM Highest difference peak 0.387, deepest hole -0.525, 1-sigma level 0.145 Q1 1 0.0150 0.5487 0.6260 11.00000 0.05 0.39 Q2 1 0.3393 0.7101 0.5178 11.00000 0.05 0.38 Q3 1 0.0415 0.5028 0.5927 11.00000 0.05 0.38 Q4 1 0.2609 0.6070 0.6606 11.00000 0.05 0.38 Q5 1 0.0055 0.5573 0.5799 11.00000 0.05 0.34 Q6 1 0.2962 1.0141 0.5575 11.00000 0.05 0.32 Q7 1 0.0719 0.4832 0.5645 11.00000 0.05 0.29 Q8 1 -0.0336 0.5373 0.7480 11.00000 0.05 0.29 Q9 1 0.0049 0.8312 0.5446 11.00000 0.05 0.28 Q10 1 0.0371 0.8749 0.5669 11.00000 0.05 0.27 Q11 1 -0.0956 0.6215 0.8723 11.00000 0.05 0.27 Q12 1 -0.0965 0.5970 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