#------------------------------------------------------------------------------ #$Date: 2023-08-16 04:49:24 +0300 (Wed, 16 Aug 2023) $ #$Revision: 285784 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312275.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2312275 loop_ _publ_author_name 'Treece, Megan M.' 'Kelly, Jordan C.' 'Rosello, Kate E.' 'Craig, Andrew J.' 'Aitken, Jennifer A.' _publ_section_title ; Accurate X-ray diffraction data required for proper evaluation of bond valence sums and global instability indexes: redetermination of the crystal structures of diamond-like Cu2CdSiS4 and Cu2HgSnS4 as a case study. ; _journal_coeditor_code VX3001 _journal_issue 9 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229623006848 _journal_volume 79 _journal_year 2023 _chemical_absolute_configuration inapplicable _chemical_formula_iupac 'Cu2 Cd Si S4' _chemical_formula_moiety 'Cd Cu2 S4 Si' _chemical_formula_sum 'Cd Cu2 S4 Si' _chemical_formula_weight 395.81 _chemical_name_common 'Copper cadmium silicon sulfide' _chemical_name_systematic 'Copper cadmium silicon sulfide' _space_group_crystal_system orthorhombic _space_group_IT_number 31 _space_group_name_Hall 'P 2ac -2' _space_group_name_H-M_alt 'P m n 21' _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.60853(11) _cell_length_b 6.48071(9) _cell_length_c 6.24923(10) _cell_measurement_reflns_used 5413 _cell_measurement_temperature 296 _cell_measurement_theta_max 32.755 _cell_measurement_theta_min 3.140 _cell_volume 308.141(8) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; SMART (Bruker, 2001) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; ShelXle (H\"ubschle et al., 2011) ; _computing_publication_material ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\f and \w Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3842 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 3.143 _diffrn_source 'fine focus sealed tube X-ray source' _exptl_absorpt_coefficient_mu 11.669 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.3569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 2002) ; _exptl_crystal_colour green-yellow _exptl_crystal_density_diffrn 4.266 _exptl_crystal_description polyhedra _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.135 _exptl_crystal_size_min 0.090 _refine_diff_density_max 1.330 _refine_diff_density_min -2.257 _refine_ls_abs_structure_details ; Flack x determined using 305 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.006(10) _refine_ls_extinction_coef 0.446(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015<>i>b) ; _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 44 _refine_ls_number_reflns 723 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.268 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0221 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0278P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0470 _reflns_number_gt 719 _reflns_number_total 723 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vx3001sup1.cif _cod_data_source_block Cu2CdSiS4 _cod_database_code 2312275 _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. ; _shelx_estimated_absorpt_t_min 0.158 _shelx_estimated_absorpt_t_max 0.420 _shelx_hkl_file ; 0 0 -1 0.62 0.07 0 0 -2 510.21 22.33 0 0 -3 0.38 0.11 0 0 -3 0.38 0.11 0 0 -4 221.44 10.81 0 0 -4 265.58 11.07 0 0 -4 257.94 10.94 0 0 -5 0.15 0.10 0 0 -5 0.13 0.11 0 0 -5 0.05 0.11 0 0 -6 398.70 17.53 0 0 -6 410.63 17.62 0 0 7 0.07 0.13 0 0 -7 -0.02 0.13 0 0 -8 281.94 12.56 0 1 0 7.65 0.42 0 1 0 7.71 0.39 0 -1 0 6.89 0.37 0 -1 0 8.25 0.46 0 1 -1 2.74 0.15 0 1 -1 2.80 0.15 0 1 -1 2.96 0.22 0 -1 -1 2.68 0.18 0 1 -2 14.11 0.74 0 -1 2 11.54 0.67 0 -1 -2 13.20 0.67 0 -1 -2 14.04 0.73 0 -1 -2 14.28 0.68 0 1 -2 14.10 0.64 0 -1 -3 24.16 1.19 0 1 -3 24.98 1.27 0 -1 -3 24.79 1.28 0 1 -3 25.87 1.19 0 -1 -4 23.88 1.16 0 1 -4 23.71 1.18 0 -1 -4 23.47 1.18 0 -1 4 20.59 1.16 0 1 -4 24.48 1.26 0 -1 -5 7.84 0.56 0 -1 5 6.87 0.53 0 -1 -5 7.98 0.53 0 1 -5 7.87 0.61 0 -1 -5 8.21 0.65 0 1 -5 8.22 0.57 0 -1 -6 15.39 1.06 0 -1 -6 14.97 0.92 0 -1 -6 15.35 0.89 0 1 -6 15.15 1.00 0 -1 6 13.28 0.90 0 -1 -7 19.95 1.31 0 -1 7 18.77 1.17 0 1 -7 18.42 1.22 0 -1 -7 17.81 1.14 0 -1 -7 17.35 1.09 0 1 -8 0.25 0.24 0 1 -9 51.98 2.87 0 2 0 409.44 20.08 0 -2 0 495.51 20.09 0 -2 0 434.58 19.94 0 2 0 488.38 20.21 0 2 -1 455.96 17.46 0 -2 -1 421.15 17.93 0 2 1 396.90 17.80 0 2 1 339.28 17.50 0 2 -1 390.61 17.64 0 -2 -1 422.69 17.60 0 2 -1 449.72 17.85 0 -2 1 342.73 17.56 0 2 -2 284.80 12.53 0 -2 -2 266.51 12.83 0 -2 2 327.66 12.84 0 2 -2 286.10 12.86 0 2 2 282.34 12.68 0 2 -2 274.77 12.57 0 -2 2 301.74 12.96 0 -2 -3 711.32 28.88 0 -2 3 617.47 28.89 0 2 -3 651.81 28.92 0 -2 -3 621.32 28.75 0 2 3 655.36 28.51 0 -2 4 110.01 5.11 0 2 -4 110.73 4.98 0 2 -4 117.39 5.21 0 -2 -4 119.00 5.06 0 2 4 112.17 5.05 0 -2 -5 457.14 21.48 0 -2 -5 515.93 21.54 0 2 5 521.12 21.87 0 2 -5 466.41 21.47 0 -2 5 512.13 21.98 0 2 -6 175.88 8.21 0 -2 6 184.68 8.13 0 2 6 186.40 8.20 0 -2 -6 178.26 8.27 0 -2 -6 181.38 8.03 0 -2 -7 129.20 6.36 0 -2 -7 138.92 6.58 0 2 -7 137.00 6.52 0 -2 7 152.94 6.46 0 2 -8 74.53 3.94 0 -2 8 80.45 3.89 0 2 -9 69.49 3.69 0 3 0 4.79 0.41 0 -3 0 4.39 0.35 0 3 0 4.52 0.36 0 3 0 4.85 0.34 0 -3 0 5.16 0.50 0 3 1 59.72 2.72 0 -3 1 60.25 2.68 0 3 -1 56.18 2.78 0 -3 -1 58.65 2.84 0 -3 -1 57.94 2.64 0 3 -1 57.15 2.67 0 3 -1 59.28 2.60 0 -3 1 57.99 2.81 0 3 1 61.30 2.68 0 -3 -1 56.04 2.69 0 3 -2 0.77 0.07 0 -3 -2 0.71 0.07 0 -3 -2 0.69 0.17 0 3 -2 0.81 0.13 0 -3 -2 0.68 0.07 0 3 -2 0.66 0.19 0 3 -2 0.82 0.13 0 -3 -2 0.81 0.19 0 3 3 13.87 0.82 0 3 -3 15.81 0.70 0 3 -3 16.31 0.71 0 -3 -3 16.93 0.97 0 3 -3 16.32 1.01 0 -3 3 14.55 0.93 0 -3 -3 15.96 0.88 0 3 -4 32.59 1.66 0 -3 -4 31.82 1.47 0 3 4 24.30 1.38 0 -3 4 25.40 1.51 0 -3 -5 53.67 2.58 0 -3 5 51.49 2.68 0 3 -5 55.24 2.80 0 -3 -5 55.79 2.78 0 -3 -6 58.40 2.88 0 -3 -6 53.51 2.61 0 3 -6 57.16 2.88 0 -3 6 46.33 2.69 0 -3 -7 31.21 1.94 0 -3 7 32.04 1.85 0 3 -7 29.27 1.89 0 -3 8 11.60 1.03 0 3 8 9.99 0.96 0 3 -8 10.49 1.02 0 4 0 405.29 17.87 0 4 0 415.48 17.75 0 4 0 384.12 17.78 0 -4 0 438.69 18.08 0 -4 0 414.74 18.03 0 4 1 373.09 16.23 0 -4 1 354.72 16.43 0 4 -1 379.16 16.15 0 -4 1 420.24 16.58 0 -4 -1 331.03 16.42 0 -4 -1 388.76 16.43 0 4 -1 371.03 16.23 0 4 -1 378.85 16.38 0 4 1 380.03 16.57 0 -4 -2 235.09 11.72 0 4 -2 263.03 11.54 0 4 -2 270.09 11.48 0 -4 -2 261.04 11.46 0 -4 2 282.32 11.60 0 4 -2 260.87 11.77 0 -4 -2 259.99 11.47 0 -4 2 278.05 11.79 0 4 2 280.95 11.61 0 -4 -2 267.09 11.65 0 4 -3 551.29 25.21 0 -4 -3 598.70 25.55 0 -4 -3 526.90 25.09 0 -4 3 596.95 26.10 0 4 3 633.75 25.81 0 -4 4 61.10 2.82 0 4 -4 52.78 2.85 0 -4 -4 52.61 2.75 0 -4 -4 52.28 2.65 0 -4 -5 339.05 15.61 0 4 -5 345.56 15.90 0 -4 5 388.18 15.84 0 -4 -5 361.32 15.82 0 4 -6 60.16 3.16 0 -4 -6 56.95 2.84 0 -4 6 53.66 2.99 0 -4 -6 61.24 3.10 0 -4 7 85.54 4.12 0 4 -7 75.56 4.17 0 -4 8 91.32 4.60 0 4 8 88.39 4.54 0 4 -8 89.60 4.71 0 -5 0 65.61 3.34 0 5 0 67.78 3.06 0 -5 0 64.97 3.08 0 5 0 64.57 3.09 0 5 0 64.78 3.19 0 5 1 65.55 3.10 0 5 -1 66.62 3.02 0 5 1 62.90 3.08 0 5 -1 65.92 3.11 0 -5 1 63.69 3.10 0 -5 1 63.29 3.35 0 -5 -1 67.93 3.07 0 5 1 64.44 3.15 0 -5 -1 70.30 3.40 0 5 -1 67.36 3.26 0 -5 2 69.70 3.55 0 5 -2 68.64 3.27 0 5 2 71.85 3.33 0 -5 2 71.70 3.31 0 5 -2 68.04 3.48 0 -5 -2 71.27 3.57 0 -5 -2 69.44 3.19 0 -5 -3 7.12 0.70 0 5 -3 6.89 0.71 0 5 -3 7.30 0.50 0 -5 -3 7.10 0.64 0 -5 -4 13.86 0.99 0 5 -4 13.18 1.11 0 -5 -4 13.88 1.00 0 -5 -5 21.82 1.38 0 5 -5 22.74 1.61 0 -5 5 23.66 1.55 0 -5 6 8.33 0.88 0 5 -7 59.00 3.37 0 5 7 57.49 3.13 0 -5 7 56.29 3.21 0 -5 8 30.62 2.14 0 6 0 646.10 27.97 0 -6 0 600.12 27.75 0 6 0 617.57 27.48 0 -6 0 662.98 27.80 0 6 0 656.83 27.44 0 6 1 5.79 0.59 0 -6 1 6.10 0.55 0 6 -1 6.79 0.57 0 -6 -1 6.38 0.73 0 6 -1 6.26 0.63 0 -6 1 6.14 0.73 0 -6 -1 5.75 0.50 0 6 1 5.77 0.52 0 -6 2 408.57 16.40 0 6 -2 360.18 16.57 0 6 2 408.04 16.40 0 6 -2 346.55 16.32 0 -6 -2 384.94 16.24 0 -6 -2 337.09 16.62 0 -6 2 379.27 16.73 0 6 -3 12.91 0.83 0 6 3 14.03 0.95 0 6 -3 12.98 1.10 0 -6 3 14.59 1.19 0 -6 -3 11.74 1.08 0 -6 -4 109.30 5.39 0 6 4 111.92 5.22 0 6 -4 109.21 5.48 0 -6 4 113.02 5.50 0 6 -4 109.95 4.88 0 -6 -5 20.34 1.48 0 6 5 20.11 1.37 0 6 -5 20.46 1.58 0 -6 5 20.17 1.55 0 6 -6 171.98 8.43 0 -6 6 175.10 8.36 0 6 6 177.85 8.15 0 6 7 21.48 1.56 0 6 -7 20.30 1.75 0 -6 7 20.97 1.71 0 -7 0 11.17 1.01 0 7 0 11.36 0.83 0 -7 0 10.96 0.79 0 -7 -1 14.92 0.95 0 -7 -1 16.43 1.25 0 7 -1 15.28 1.02 0 7 -1 14.56 1.10 0 7 -2 87.39 4.14 0 -7 -2 91.17 4.01 0 -7 2 81.23 4.13 0 -7 -2 91.88 4.50 0 7 2 88.12 4.16 0 7 -2 86.20 4.35 0 -7 2 84.88 4.49 0 7 3 36.70 2.16 0 -7 3 35.28 2.45 0 7 -3 45.30 2.13 0 7 -3 43.44 2.44 0 -7 -3 42.27 2.51 0 7 4 84.39 4.00 0 7 -4 76.45 3.67 0 -7 4 86.25 4.41 0 7 -4 82.91 4.27 0 -7 -4 74.23 4.22 0 7 -5 22.27 1.78 0 7 5 25.21 1.61 0 -7 5 25.88 1.92 0 7 -6 5.53 0.88 0 7 6 7.68 0.85 0 -7 6 7.51 1.05 0 8 0 56.59 2.85 0 -8 0 55.41 2.80 0 -8 0 57.42 3.14 0 -8 -1 77.83 3.86 0 8 -1 75.95 3.55 0 -8 1 67.87 3.81 0 -8 -1 73.40 3.42 0 -8 1 65.58 3.48 0 8 -2 24.47 1.69 0 -8 2 25.51 1.67 0 8 -2 26.55 1.54 0 8 2 26.60 1.56 0 -8 -2 27.13 1.83 0 -8 2 26.33 1.87 0 -8 -2 25.74 1.38 0 8 -3 158.78 7.58 0 8 -3 161.74 7.24 0 -8 -3 164.13 7.70 0 -8 3 153.50 7.74 0 8 3 159.43 7.35 0 -8 4 31.80 2.26 0 8 -4 33.14 2.15 0 8 -4 32.99 1.67 0 8 4 30.05 1.90 0 8 5 157.66 7.28 0 8 -5 150.49 7.54 0 -9 0 25.56 1.81 0 9 0 26.43 1.58 0 -9 0 25.42 1.50 0 -9 1 31.45 2.12 0 -9 1 32.13 1.81 0 -9 -1 30.77 2.02 0 9 -1 30.85 1.81 0 -9 -1 32.03 2.07 0 -9 -2 22.14 1.73 0 -9 -2 23.50 1.41 0 -9 2 30.04 1.99 0 -9 2 27.33 1.60 0 -9 -3 14.72 1.34 -1 0 0 0.03 0.03 -1 0 0 0.08 0.02 1 0 0 0.09 0.03 -1 0 -1 82.50 3.89 1 0 -1 99.90 4.00 1 0 -1 92.50 3.94 1 0 1 83.53 3.87 1 0 -2 0.05 0.05 1 0 -2 0.16 0.07 -1 0 -2 0.04 0.05 1 0 2 0.14 0.07 -1 0 -2 0.09 0.06 1 0 -3 103.26 4.60 -1 0 -3 109.49 4.65 1 0 -3 105.82 4.68 1 0 -3 103.01 4.65 -1 0 -3 105.16 4.65 -1 0 -4 0.02 0.07 1 0 -4 0.14 0.10 1 0 -4 0.00 0.07 -1 0 -4 0.40 0.14 -1 0 -4 0.02 0.06 1 0 -5 167.72 7.17 -1 0 -5 166.31 7.14 1 0 -5 152.69 7.15 -1 0 -5 156.88 7.09 -1 0 5 158.77 7.05 1 0 -6 0.19 0.17 1 0 -6 0.03 0.12 -1 0 -6 0.24 0.14 -1 0 6 0.06 0.10 1 0 6 -0.05 0.13 -1 0 -6 0.08 0.13 -1 0 -7 84.68 4.06 1 0 -7 86.11 4.11 1 0 -8 0.05 0.20 1 0 8 0.29 0.22 1 -1 0 76.67 3.41 -1 1 0 75.30 3.49 1 -1 0 77.44 3.41 -1 -1 0 72.62 3.47 -1 1 0 81.03 3.46 1 -1 0 83.57 3.45 1 1 0 77.52 3.42 1 1 0 78.42 3.41 1 1 0 81.74 3.49 -1 -1 0 82.55 3.47 1 1 1 64.91 2.80 -1 -1 1 66.76 2.72 1 -1 -1 55.30 2.72 1 -1 -1 64.54 2.75 -1 1 -1 66.42 2.80 -1 -1 1 63.27 2.82 -1 1 -1 58.68 2.86 1 -1 -1 61.62 2.72 -1 1 -1 58.23 2.75 1 -1 -1 64.63 2.76 1 1 -1 57.68 2.75 -1 -1 -1 56.56 2.72 1 -1 1 62.16 2.76 1 1 -1 64.36 2.73 -1 -1 -1 64.05 2.74 -1 -1 -1 65.58 2.77 1 1 -1 67.82 2.71 1 -1 1 65.02 2.76 1 1 -1 64.07 2.78 -1 1 -2 173.58 7.38 1 -1 -2 188.22 7.40 1 1 2 150.13 7.28 1 -1 -2 171.53 7.25 -1 1 -2 166.76 7.31 -1 -1 2 155.68 7.37 -1 1 2 156.64 7.37 1 -1 2 164.68 7.30 -1 -1 -2 171.34 7.50 1 1 -2 172.47 7.28 -1 -1 -2 172.33 7.33 1 1 -2 159.24 7.27 -1 1 -3 49.78 2.29 1 -1 -3 50.46 2.32 -1 -1 3 48.08 2.28 1 -1 -3 51.49 2.23 -1 1 -3 50.88 2.36 1 1 -3 50.70 2.35 -1 -1 -3 45.52 2.34 -1 -1 -3 52.05 2.30 1 -1 3 48.18 2.23 1 1 -3 50.44 2.25 -1 -1 -3 51.20 2.25 -1 1 -4 104.62 4.67 -1 1 -4 100.28 4.58 1 -1 -4 103.37 4.61 -1 -1 4 104.38 4.58 1 -1 -4 104.55 4.52 1 -1 -4 101.67 4.64 1 1 -4 99.38 4.56 -1 -1 -4 89.67 4.65 -1 -1 -4 104.54 4.59 -1 -1 -4 103.65 4.55 1 1 -4 105.42 4.67 1 -1 4 108.78 4.55 1 -1 -5 62.63 2.94 -1 -1 5 62.72 2.90 1 -1 -5 63.36 3.00 1 -1 -5 59.02 2.82 -1 1 -5 63.23 2.99 -1 -1 -5 62.31 2.87 1 1 -5 62.85 3.00 1 -1 5 57.70 2.93 -1 -1 -5 62.70 2.90 1 1 -5 63.34 2.92 -1 -1 -5 61.12 3.02 1 -1 -6 0.11 0.11 -1 1 -6 0.14 0.15 1 -1 -6 0.08 0.16 -1 -1 6 0.58 0.19 1 1 6 0.58 0.23 1 -1 6 0.50 0.18 -1 -1 -6 0.03 0.11 -1 -1 -6 0.08 0.11 1 1 -6 0.20 0.17 -1 1 -7 34.04 1.88 1 -1 -7 32.20 1.93 1 1 7 32.74 1.88 -1 1 7 34.89 1.86 1 -1 7 34.54 1.83 1 1 -7 32.23 1.88 -1 -1 -7 32.00 1.77 -1 1 -8 36.01 2.01 1 -1 8 31.14 1.91 1 1 -8 35.51 2.04 -1 -1 -8 33.43 1.88 1 1 -9 3.59 0.67 -1 2 0 223.13 10.09 1 -2 0 220.34 10.05 1 2 0 241.31 10.28 1 -2 0 227.74 10.25 -1 -2 0 255.07 10.33 1 -2 0 226.37 10.21 1 2 0 215.70 10.14 1 2 0 245.75 10.14 -1 2 0 231.33 10.12 1 -2 -1 31.50 1.50 -1 -2 1 31.11 1.64 1 -2 -1 31.69 1.49 -1 2 -1 30.73 1.65 1 2 1 33.76 1.56 1 2 1 32.90 1.45 1 2 1 32.47 1.47 -1 -2 1 32.72 1.47 1 -2 -1 31.41 1.45 -1 2 -1 30.81 1.46 1 2 -1 31.49 1.52 1 -2 1 32.66 1.41 1 -2 1 34.71 1.54 -1 -2 -1 31.61 1.49 1 2 -1 32.20 1.46 -1 2 1 33.40 1.55 -1 -2 -1 30.58 1.45 1 -2 1 34.17 1.53 -1 2 1 34.06 1.51 1 2 -1 31.57 1.53 1 -2 -2 187.75 8.68 1 2 2 195.29 8.59 1 -2 -2 196.87 8.53 -1 -2 2 189.79 8.57 1 2 2 196.53 8.62 -1 2 -2 195.14 8.57 -1 -2 2 208.68 8.51 -1 2 -2 192.31 8.65 -1 2 -2 186.04 8.52 1 2 -2 197.21 8.57 1 2 -2 186.02 8.53 -1 -2 -2 196.19 8.52 1 -2 2 207.88 8.75 1 2 -2 204.85 8.54 1 2 -2 189.99 8.65 1 -2 2 208.82 8.51 -1 2 2 192.01 8.51 1 -2 -3 1.70 0.17 1 2 3 1.11 0.13 -1 2 -3 1.73 0.27 -1 -2 3 1.49 0.22 1 -2 3 1.32 0.20 -1 -2 -3 1.47 0.19 -1 -2 -3 1.64 0.27 -1 2 3 1.18 0.18 1 2 -3 1.87 0.16 1 2 -3 1.67 0.24 -1 2 -4 62.48 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84.92 4.50 -10 -1 0 77.07 3.67 -10 1 0 74.46 3.67 10 1 1 100.26 4.85 -10 1 -1 100.14 4.66 10 -1 -1 103.35 4.76 -10 -1 1 98.33 4.68 10 -1 -1 101.07 4.81 10 1 -1 104.82 4.88 10 1 -1 105.08 4.77 -10 1 1 98.89 4.72 10 -1 1 99.99 4.76 -10 1 1 107.74 5.42 10 -1 1 95.73 4.76 -10 -1 -1 105.02 4.68 10 1 2 52.13 2.68 10 -1 -2 49.64 2.66 10 -1 -2 50.04 2.56 -10 1 -2 46.95 2.45 10 -1 2 52.38 2.61 -10 -1 -2 50.10 2.46 10 1 -2 51.33 2.59 10 1 -2 50.72 2.70 -10 1 2 56.11 3.14 10 -1 -3 149.23 7.08 -10 -1 3 158.16 7.47 10 1 3 147.65 7.04 10 -1 -3 156.79 6.96 -10 1 -3 145.77 6.77 -10 -1 -3 152.38 6.77 10 1 -3 149.94 7.10 10 1 -3 159.42 7.02 -10 1 3 161.36 7.56 10 1 4 24.79 1.57 -10 -1 4 27.20 1.93 -10 1 4 25.34 1.92 10 1 -4 24.52 1.84 -10 2 0 3.70 0.45 10 2 0 4.10 0.52 10 2 0 3.23 0.54 -10 -2 0 4.20 0.47 10 -2 0 4.33 0.52 -10 2 0 3.96 0.90 10 -2 0 4.07 0.51 10 -2 -1 4.08 0.51 -10 2 -1 5.16 1.07 10 2 1 5.87 0.65 -10 2 -1 4.31 0.47 10 -2 -1 4.14 0.54 10 2 -1 4.17 0.53 -10 -2 -1 4.08 0.46 10 2 -1 4.51 0.60 10 -2 1 6.19 0.59 -10 2 1 7.03 0.99 -10 2 -2 6.36 0.53 10 -2 -2 6.36 0.66 10 2 2 4.31 0.61 10 -2 -2 6.50 0.62 10 2 -2 6.72 0.71 10 2 -2 7.22 0.66 -10 2 2 4.74 0.91 -10 -2 -2 6.46 0.53 10 -2 -3 21.48 1.44 10 -2 -3 23.54 1.35 10 2 3 23.71 1.50 -10 2 3 21.91 1.78 10 2 -3 20.98 1.48 -10 -2 -3 22.57 1.18 10 2 4 2.36 0.49 -10 -2 4 3.13 0.75 -10 -2 -4 1.39 0.40 10 -3 0 205.03 9.47 10 3 0 206.59 9.67 -10 -3 0 210.73 9.42 -10 3 0 205.19 9.42 -10 3 0 221.84 10.31 10 -3 0 216.37 9.53 10 3 0 218.35 9.54 10 -3 -1 0.35 0.23 -10 3 -1 0.48 0.22 -10 3 -1 0.86 0.57 10 3 1 0.71 0.33 -10 -3 1 1.17 0.31 -10 -3 -1 1.12 0.42 10 3 -1 0.30 0.27 -10 3 1 0.70 0.47 10 -3 1 0.48 0.26 10 3 -1 0.76 0.30 -10 3 -2 150.56 7.60 10 3 2 140.13 6.77 10 -3 -2 141.63 6.67 10 3 -2 136.96 6.77 -10 3 2 151.42 7.31 10 3 3 2.01 0.54 10 -3 -3 1.93 0.46 10 3 -3 1.53 0.46 10 4 0 23.36 1.62 -10 4 0 23.46 2.01 -10 4 -1 2.69 0.81 10 4 1 4.53 0.79 10 4 -1 2.69 0.58 -10 4 -2 22.20 1.99 10 -4 -2 18.44 1.31 10 4 -2 21.35 2.15 11 0 0 0.06 0.20 -11 0 1 54.80 2.84 11 0 1 56.69 2.91 11 0 -1 55.01 2.92 11 0 2 0.12 0.23 11 1 0 26.06 1.67 11 -1 0 27.24 1.64 11 -1 -1 3.02 0.51 11 1 1 2.51 0.50 -11 1 1 3.82 1.19 11 -1 1 2.21 0.56 11 1 -1 3.38 0.62 11 -1 1 2.33 0.44 11 1 2 22.49 1.68 -11 1 2 23.53 1.96 11 -2 0 2.70 0.49 -11 2 0 3.74 0.96 11 -2 -1 15.60 1.20 -11 2 1 19.08 1.77 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 97105 _shelx_res_file ; TITL 1_MT3_2_Cu2CdSiS4_Y1retry in Pmn2(1) 1_MT3_2_Cu2CdSiS4_Y1retry.res created by SHELXL-2018/3 at 13:35:25 on 13-Dec-2022 CELL 0.71073 7.60853 6.48071 6.24923 90.0000 90.0000 90.0000 ZERR 2.00 0.00011 0.00009 0.00010 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.5+X, -Y, 0.5+Z SYMM -X, Y, Z SFAC SI S CU CD UNIT 2 8 4 2 ACTA LIST 4 TEMP 20.000 SIZE 0.09 0.135 0.25 L.S. 4 BOND FMAP 2 PLAN 20 SHEL 999 0.77 WGHT 0.024900 0.027800 EXTI 0.445527 FVAR 0.28711 MOLE MOLE 1 CD1 4 0.000000 0.347573 0.872831 10.50000 0.01558 0.01448 = 0.01622 -0.00027 0.00000 0.00000 CU1 3 0.247793 0.176670 0.367050 11.00000 0.01939 0.01796 = 0.01880 -0.00031 -0.00092 -0.00103 SI1 1 0.000000 0.680415 0.374247 10.50000 0.00830 0.00590 = 0.00903 0.00016 0.00000 0.00000 S1 2 0.000000 0.364171 0.468023 10.50000 0.01284 0.00630 = 0.01299 0.00039 0.00000 0.00000 S2 2 0.000000 0.704509 0.033731 10.50000 0.01129 0.01100 = 0.00845 0.00131 0.00000 0.00000 S3 2 0.275931 0.161547 0.998319 11.00000 0.01060 0.00873 = 0.01069 0.00053 0.00127 -0.00186 MOLE 2 HKLF 4 REM 1_MT3_2_Cu2CdSiS4_Y1retry in Pmn2(1) REM wR2 = 0.0470, GooF = S = 1.269, Restrained GooF = 1.268 for all data REM R1 = 0.0221 for 719 Fo > 4sig(Fo) and 0.0221 for all 723 data REM 44 parameters refined using 1 restraints END WGHT 0.0249 0.0278 REM Highest difference peak 1.330, deepest hole -2.257, 1-sigma level 0.277 Q1 1 0.0000 0.3291 0.7522 10.50000 0.05 1.33 Q2 1 0.0000 0.3338 0.9967 10.50000 0.05 1.16 Q3 1 0.2478 0.1577 0.2540 11.00000 0.05 0.93 Q4 1 0.2513 0.1616 0.4914 11.00000 0.05 0.84 Q5 1 0.0000 0.6680 0.2572 10.50000 0.05 0.81 Q6 1 0.0000 0.3350 0.6007 10.50000 0.05 0.66 Q7 1 0.2686 0.1584 1.1333 11.00000 0.05 0.54 Q8 1 0.0000 0.6716 0.4864 10.50000 0.05 0.50 Q9 1 0.0000 0.6627 0.1298 10.50000 0.05 0.47 Q10 1 0.1071 0.3896 0.8683 11.00000 0.05 0.46 Q11 1 0.0000 0.3465 0.3476 10.50000 0.05 0.45 Q12 1 0.1432 0.8394 0.1780 11.00000 0.05 0.36 Q13 1 0.1313 0.6235 0.1779 11.00000 0.05 0.34 Q14 1 0.1417 0.1159 0.3402 11.00000 0.05 0.33 Q15 1 0.1227 0.1475 0.1797 11.00000 0.05 0.33 Q16 1 0.1355 0.0018 0.1866 11.00000 0.05 0.33 Q17 1 0.3885 0.1688 1.0160 11.00000 0.05 0.32 Q18 1 0.3589 0.1161 0.3704 11.00000 0.05 0.31 Q19 1 0.1092 0.4777 0.2280 11.00000 0.05 0.30 Q20 1 0.3714 0.0834 1.0255 11.00000 0.05 0.30 ; _shelx_res_checksum 21236 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' loop_ _atom_site_type_symbol _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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.000000 0.34757(5) 0.87283(5) 0.0154(2) Uani d 1 . . Cu Cu1 0.24779(7) 0.17667(7) 0.36705(17) 0.0187(2) Uani d 1 . . Si Si1 0.000000 0.68042(19) 0.3742(6) 0.0077(3) Uani d 1 . . S S1 0.000000 0.3642(2) 0.4680(3) 0.0107(4) Uani d 1 . . S S2 0.000000 0.7045(2) 0.0337(3) 0.0102(3) Uani d 1 . . S S3 0.27593(17) 0.16155(17) 0.9983(2) 0.0100(3) Uani d 1 . . 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 Cd1 0.0156(3) 0.0145(3) 0.0162(3) 0.000 0.000 -0.0003(2) Cu1 0.0194(3) 0.0180(3) 0.0188(4) -0.00103(18) -0.0009(3) -0.0003(3) Si1 0.0083(7) 0.0059(6) 0.0090(9) 0.000 0.000 0.0002(7) S1 0.0128(7) 0.0063(6) 0.0130(8) 0.000 0.000 0.0004(5) S2 0.0113(6) 0.0110(7) 0.0084(7) 0.000 0.000 0.0013(6) S3 0.0106(4) 0.0087(5) 0.0107(6) -0.0019(3) 0.0013(4) 0.0005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 _geom_angle _geom_angle_publ_flag S2 Cd1 S1 1_556 . 111.06(5) ? S2 Cd1 S3 1_556 . 108.16(4) ? S1 Cd1 S3 . . 109.15(4) ? S2 Cd1 S3 1_556 4 108.16(4) ? S1 Cd1 S3 . 4 109.15(4) ? S3 Cd1 S3 . 4 111.17(5) ? S2 Cu1 S3 2_565 1_554 112.65(7) ? S2 Cu1 S1 2_565 . 112.05(6) ? S3 Cu1 S1 1_554 . 111.49(7) ? S2 Cu1 S3 2_565 2_554 102.54(8) ? S3 Cu1 S3 1_554 2_554 108.38(6) ? S1 Cu1 S3 . 2_554 109.27(6) ? S1 Si1 S2 . . 110.15(15) ? S1 Si1 S3 . 2_564 111.19(13) ? S2 Si1 S3 . 2_564 109.10(11) ? S1 Si1 S3 . 3_464 111.19(13) ? S2 Si1 S3 . 3_464 109.10(11) ? S3 Si1 S3 2_564 3_464 106.00(13) ? Si1 S1 Cu1 . . 115.27(9) ? Si1 S1 Cu1 . 4 115.27(9) ? Cu1 S1 Cu1 . 4 108.02(7) ? Si1 S1 Cd1 . . 108.39(12) ? Cu1 S1 Cd1 . . 104.38(6) ? Cu1 S1 Cd1 4 . 104.38(6) ? Si1 S2 Cu1 . 3_464 118.23(8) ? Si1 S2 Cu1 . 2_564 118.23(8) ? Cu1 S2 Cu1 3_464 2_564 111.96(10) ? Si1 S2 Cd1 . 1_554 109.30(7) ? Cu1 S2 Cd1 3_464 1_554 97.22(7) ? Cu1 S2 Cd1 2_564 1_554 97.22(7) ? Si1 S3 Cu1 2_565 1_556 114.51(13) ? Si1 S3 Cu1 2_565 2 112.49(11) ? Cu1 S3 Cu1 1_556 2 112.34(6) ? Si1 S3 Cd1 2_565 . 108.64(7) ? Cu1 S3 Cd1 1_556 . 102.14(5) ? Cu1 S3 Cd1 2 . 105.74(6) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 S2 1_556 2.5223(18) ? Cd1 S1 . 2.5320(18) ? Cd1 S3 . 2.5448(13) ? Cd1 S3 4 2.5448(13) ? Cu1 S2 2_565 2.3152(13) ? Cu1 S3 1_554 2.316(2) ? Cu1 S1 . 2.3301(11) ? Cu1 S3 2_554 2.3473(16) ? Si1 S1 . 2.132(2) ? Si1 S2 . 2.134(5) ? Si1 S3 2_564 2.135(2) ? Si1 S3 3_464 2.135(2) ? _cod_database_fobs_code 2312275