#------------------------------------------------------------------------------ #$Date: 2021-01-25 11:46:09 +0200 (Mon, 25 Jan 2021) $ #$Revision: 261187 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/01/1560195.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1560195 loop_ _publ_author_name 'Owen P. Missen' 'Anthony R. Kampf' 'Stuart J. Mills' 'Robert M. Housley' 'John Spratt' 'Mark D. Welch' 'Mark F. Coolbaugh' 'Joe Marty' 'Marek Chorazewicz' 'Cristiano Ferraris' _publ_section_title ; The crystal structures of the mixed-valence tellurium oxysalts tlapallite, (Ca,Pb)3CaCu6[Te4+3Te6+O12]2(Te4+O3)2(SO4)2 . 3H2O, and carlfriesite, CaTe4+2Te6+O8 ; _journal_name_full 'Mineralogical Magazine' _journal_page_first 439 _journal_page_last 549 _journal_paper_doi 10.1180/mgm.2019.9 _journal_volume 83 _journal_year 2019 _chemical_formula_moiety 'Cu6 O30 Pb0.39 Sb0.27 Te9.73, 2(O4 S), 3(H2 O), 3.613(Ca)' _chemical_formula_sum 'Ca1.81 Cu3 H3 O20.5 Pb0.19 S Sb0.13 Te4.87' _chemical_formula_weight 1303.50 _chemical_name_common tlapallite _space_group_crystal_system trigonal _space_group_IT_number 150 _space_group_name_Hall 'P 3 2"' _space_group_name_H-M_alt 'P 3 2 1' _atom_sites_solution_hydrogens difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 9.1219(17) _cell_length_b 9.1219(17) _cell_length_c 11.9320(9) _cell_measurement_reflns_used 660 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.241 _cell_measurement_theta_min 3.093 _cell_volume 859.8(2) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'three-circle diffractometer, Rigaku R-Axis Rapid II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_unetI/netI 0.0494 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4092 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 23.241 _diffrn_reflns_theta_max 23.241 _diffrn_reflns_theta_min 3.093 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 14.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Higashi, 2001)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 5.035 _exptl_crystal_description 'partial hexagonal plate' _exptl_crystal_F_000 1164 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.004 _exptl_transmission_factor_max 0.944 _exptl_transmission_factor_min 0.592 _refine_diff_density_max 0.848 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.195 _refine_ls_abs_structure_details ; Flack x determined using 283 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 102 _refine_ls_number_reflns 832 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0296 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+5.2653P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0625 _reflns_Friedel_coverage 0.651 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 786 _reflns_number_total 832 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file CIF_tlapallite_Missen_et_al.cif _cod_data_source_block 14584-84 _cod_original_cell_volume 859.8(3) _cod_original_formula_sum 'Ca1.81 H3 Cu3 O20.50 Pb0.19 S Sb0.13 Te4.87' _cod_database_code 1560195 _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 0.592 _shelx_estimated_absorpt_t_max 0.944 _shelx_res_file ; TITL tlapallite in P321 14584-84.res created by SHELXL-2018/3 at 00:23:03 on 15-Jan-2019 CELL 0.71075 9.12191 9.12191 11.93200 90.00000 90.00000 120.00000 ZERR 2 0.00170 0.00170 0.00085 0.00000 0.00000 0.00000 LATT -1 SYMM -Y, +X-Y, +Z SYMM -X+Y, -X, +Z SYMM +Y, +X, -Z SYMM -X, -X+Y, -Z SYMM +X-Y, -Y, -Z SFAC CA CU H O S TE PB SB UNIT 3.612 6 6 41 1.99998 9.73224 0.38802 0.26772 LIST 4 SHEL 99999 0.9 L.S. 10 omit 0 1 1 EXYZ CA2 PB2 EADP CA2 PB2 EXYZ TE1 SB1 EADP TE1 SB1 FMAP 2 PLAN 20 CONN 12 3.5 TE2 CONN 12 3.5 TE3 CONN 7 3.2 Cu ACTA HTAB OW O1 DFIX 0.90 0.05 OW H SIZE 0.040 0.040 0.004 WGHT 0.016100 5.265300 EXTI 0.000314 FVAR 0.25476 0.87066 TE1 6 0.000000 0.000000 0.214659 10.28871 0.00900 0.00900 = 0.01584 0.00000 0.00000 0.00450 SB1 8 0.000000 0.000000 0.214659 10.04462 0.00900 0.00900 = 0.01584 0.00000 0.00000 0.00450 TE2 6 0.084916 0.412199 0.311805 11.00000 0.01068 0.01214 = 0.01671 -0.00045 -0.00030 0.00668 TE3 6 0.666667 0.333333 0.107074 10.33333 0.01541 0.01541 = 0.02491 0.00000 0.00000 0.00770 CU 2 0.369432 0.384867 0.139724 11.00000 0.01215 0.01204 = 0.02206 -0.00291 0.00077 0.00255 CA1 1 0.000000 0.000000 0.500000 10.16667 0.01425 0.01425 = 0.02459 0.00000 0.00000 0.00712 CA2 1 0.000000 0.250696 0.000000 20.50000 0.01492 0.01825 = 0.02322 -0.00103 -0.00207 0.00746 PB2 7 0.000000 0.250696 0.000000 -20.50000 0.01492 0.01825 = 0.02322 -0.00103 -0.00207 0.00746 S1 5 0.666667 0.333333 0.399182 10.33333 0.01511 0.01511 = 0.01790 0.00000 0.00000 0.00755 O1 4 0.503057 0.301370 0.356860 11.00000 0.01905 0.04077 = 0.03165 -0.00346 -0.00692 0.01652 O2 4 0.666667 0.333333 0.522789 10.33333 0.04687 0.04687 = 0.00998 0.00000 0.00000 0.02344 O3 4 0.161411 0.171176 0.118193 11.00000 0.00319 0.00730 = 0.01031 -0.00313 0.00038 -0.00249 O4 4 0.475537 0.301878 0.027827 11.00000 0.01323 0.01712 = 0.01383 -0.00456 0.00384 0.00404 O5 4 -0.002213 0.407869 0.167934 11.00000 0.02160 0.01310 = 0.01094 -0.00778 -0.00864 0.01509 O6 4 0.304364 0.465791 0.266419 11.00000 0.01512 0.01453 = 0.01568 -0.00411 0.00259 0.00173 O7 4 -0.001720 0.163521 0.317033 11.00000 0.01596 0.01387 = 0.00655 -0.00328 0.00088 0.00855 OW 4 0.256173 0.256173 0.500000 10.50000 0.03232 0.03232 = 0.01881 -0.00668 0.00668 0.00069 H 3 0.340944 0.264397 0.458328 11.00000 -1.20000 HKLF 4 REM tlapallite in P321 REM wR2 = 0.0625, GooF = S = 1.072, Restrained GooF = 1.071 for all data REM R1 = 0.0296 for 786 Fo > 4sig(Fo) and 0.0329 for all 832 data REM 102 parameters refined using 1 restraints END WGHT 0.0161 5.2653 REM Highest difference peak 0.848, deepest hole -1.220, 1-sigma level 0.195 Q1 1 0.5952 0.3224 0.0022 11.00000 0.05 0.85 Q2 1 0.4417 0.2121 -0.0102 11.00000 0.05 0.76 Q3 1 0.3388 0.2650 -0.0323 11.00000 0.05 0.71 Q4 1 0.0927 0.4137 0.3887 11.00000 0.05 0.69 Q5 1 0.6011 0.2307 0.1837 11.00000 0.05 0.67 Q6 1 0.1256 0.4503 0.1134 11.00000 0.05 0.62 Q7 1 0.0078 0.3704 0.2369 11.00000 0.05 0.62 Q8 1 -0.0068 0.4731 0.2474 11.00000 0.05 0.60 Q9 1 0.0000 0.0000 0.0000 10.16667 0.05 0.60 Q10 1 0.3453 0.3454 0.5000 10.50000 0.05 0.59 Q11 1 0.4591 0.5363 0.0584 11.00000 0.05 0.57 Q12 1 0.5567 0.2705 0.3173 11.00000 0.05 0.56 Q13 1 -0.0696 0.4439 0.0812 11.00000 0.05 0.55 Q14 1 0.2036 0.2036 0.0000 10.50000 0.05 0.55 Q15 1 0.0456 0.4097 0.1160 11.00000 0.05 0.55 Q16 1 0.0000 0.0000 0.1203 10.33333 0.05 0.55 Q17 1 0.3607 0.3939 0.2333 11.00000 0.05 0.55 Q18 1 0.0000 0.0000 0.3018 10.33333 0.05 0.54 Q19 1 0.4106 0.4215 0.0501 11.00000 0.05 0.54 Q20 1 0.3911 0.2589 0.0755 11.00000 0.05 0.54 ; _shelx_res_checksum 91279 _shelx_hkl_file ; -1 0 -1 15.66 5.49 1 0 1 5.64 5.30 -1 1 1 15.26 9.56 1 -1 -1 18.17 5.75 -1 1 -1 60.96 8.28 1 0 -1 75.92 9.46 -1 0 1 74.96 6.15 0 1 1 64.20 10.29 1 -1 1 59.92 5.09 0 0 2 2805.15 68.34 0 1 -2 223.22 4.35 1 -1 -2 243.51 14.53 1 0 2 200.42 12.06 -1 1 2 244.75 14.13 -1 0 -2 242.07 13.54 -1 0 2 902.73 22.72 -1 1 -2 933.78 20.90 0 1 2 985.06 41.40 1 0 -2 918.74 23.12 1 -1 2 902.94 25.65 -1 -1 0 712.26 27.83 1 -2 0 575.50 39.63 1 1 0 633.88 23.92 2 -1 0 749.77 29.29 -1 2 0 670.35 33.77 -2 1 0 665.73 28.55 2 -1 1 572.62 25.19 1 -2 -1 556.40 29.71 1 1 1 596.50 41.18 -2 1 1 515.93 24.35 -1 -1 1 548.73 28.79 1 -2 1 527.14 29.31 -1 -1 -1 554.87 28.55 -2 1 -1 504.98 24.57 1 1 -1 523.46 17.03 -1 2 -1 561.34 20.21 -1 2 1 537.38 41.53 2 -1 -1 586.47 26.51 0 0 3 750.51 31.37 -2 0 0 846.57 34.48 0 2 0 618.12 34.36 -2 2 0 775.50 33.26 2 0 0 846.19 33.56 2 -2 0 793.36 49.63 2 0 1 1410.43 54.56 -2 0 -1 1397.18 53.01 0 2 -1 1328.98 49.73 2 -2 -1 1470.71 58.00 -2 2 1 1378.88 55.65 2 -2 1 1643.11 54.93 -2 2 -1 1631.34 52.61 -2 0 1 1716.90 77.33 2 0 -1 1664.72 56.64 0 2 1 1499.29 71.57 2 -1 -2 639.51 30.12 1 1 2 595.64 33.66 -1 2 2 572.23 35.02 2 -1 2 635.75 26.31 -1 -1 2 622.44 25.60 -1 2 -2 653.87 23.39 1 -2 -2 646.34 36.06 -2 1 -2 650.88 26.82 1 -2 2 608.42 23.27 -2 1 2 580.64 28.14 1 1 -2 664.04 21.09 1 0 3 543.92 22.07 -1 0 -3 543.99 22.97 1 -1 -3 533.18 26.26 -1 1 3 443.31 24.16 1 0 -3 2869.56 76.11 -1 0 3 2672.28 84.03 0 1 3 2883.59 108.04 1 -1 3 2696.55 74.01 -1 1 -3 2898.06 77.80 2 -2 2 1512.23 47.44 -2 2 -2 1589.83 62.74 0 2 2 1632.04 78.76 2 0 -2 1567.93 52.90 -2 0 2 1501.83 50.23 2 -2 -2 1612.94 91.69 -2 2 2 1573.60 64.70 -2 0 -2 1551.24 61.38 2 0 2 1511.06 60.82 0 2 -2 1643.63 40.24 0 2 -2 1637.29 57.53 -1 2 -3 6029.70 161.70 -1 2 3 5229.04 238.74 1 1 -3 6019.20 177.90 2 -1 -3 6302.29 237.85 -2 1 3 5892.09 222.89 1 -2 -3 6036.88 261.51 -2 1 -3 6231.48 220.84 2 -1 3 6081.66 240.41 1 -2 3 5625.01 166.32 1 1 3 5900.26 245.99 -1 -1 3 5872.62 187.77 2 -3 0 327.96 24.17 -3 1 0 264.72 24.66 -2 3 0 403.39 21.73 1 2 0 301.22 19.07 -2 -1 0 376.73 23.17 2 1 0 284.93 23.08 3 -2 0 322.16 24.75 -1 3 0 328.97 20.78 -3 2 0 358.89 36.15 1 -3 0 308.55 40.47 3 -1 0 382.92 37.11 0 0 4 474.58 18.30 3 -1 -1 4685.29 184.64 -1 3 1 4240.72 182.92 -3 1 1 4692.73 183.13 2 1 -1 4787.79 173.93 1 2 1 4667.65 229.69 -2 -1 1 4444.50 167.73 -3 2 -1 4677.13 178.29 -2 3 -1 4662.58 160.81 3 -2 1 4557.06 179.46 2 -3 1 4676.40 174.52 1 -3 -1 4185.63 197.85 -2 3 1 488.54 31.90 -2 -1 -1 500.89 30.81 1 2 -1 454.58 33.25 -3 2 1 455.87 28.87 3 -2 -1 500.77 31.64 3 -1 1 544.55 30.13 -1 -2 1 431.17 24.76 1 -3 1 350.31 36.98 2 1 1 483.33 44.55 2 -3 -1 522.42 49.12 -1 3 -1 507.50 36.79 -3 1 -1 503.86 29.08 0 2 3 385.43 29.44 2 -2 3 281.93 14.16 -2 2 -3 315.02 20.66 -2 0 3 303.09 24.00 2 0 -3 325.51 16.88 0 2 -3 1451.07 30.02 2 0 3 1363.41 55.86 2 -2 -3 1531.27 64.37 -2 2 3 1434.69 87.34 0 2 -3 1480.96 32.06 -2 0 -3 1425.91 58.89 1 -1 -4 518.18 27.36 -1 1 4 425.57 24.35 1 0 4 493.49 22.72 1 0 -4 1579.21 42.45 1 -1 4 1392.87 40.60 0 1 4 1368.30 80.35 -1 0 4 1409.78 38.99 -1 1 -4 1542.18 37.37 -1 -2 2 2912.57 100.45 -2 -1 -2 3259.07 167.05 1 2 -2 3273.00 121.97 -1 3 -2 3204.04 101.07 1 -3 2 3004.06 127.39 -3 1 -2 3373.53 127.17 3 -1 2 3161.11 124.47 -3 2 2 3130.24 125.50 2 -3 -2 3494.75 146.62 3 -2 -2 3323.55 132.91 -2 3 2 3031.42 131.62 2 1 2 3206.08 132.53 -3 2 -2 1541.48 56.11 3 -2 2 1378.81 54.32 -2 3 -2 1298.95 50.52 2 1 -2 1417.62 48.63 1 2 2 1497.28 68.80 2 -3 2 1370.18 47.26 3 -1 -2 1402.15 58.99 -1 3 2 1220.28 65.21 -3 1 2 1452.68 57.55 1 -3 -2 1451.98 76.49 -2 -1 2 1333.18 47.98 3 0 0 9654.62 435.25 3 -3 0 9828.36 451.88 -3 0 0 9999.00 445.67 -3 3 0 9527.55 427.87 0 3 0 8151.17 459.17 -3 0 1 436.94 27.15 3 -3 1 379.61 26.59 -3 3 -1 402.46 37.24 0 3 1 434.63 50.50 3 0 -1 427.16 26.66 3 -3 -1 506.60 34.57 -3 3 1 491.27 32.95 3 0 1 526.63 34.11 0 3 -1 392.62 43.51 -3 0 -1 540.77 31.87 1 -2 4 744.88 14.89 -1 2 4 805.36 44.46 1 1 -4 863.53 24.91 -2 1 4 828.91 34.39 -1 -1 4 838.91 23.96 1 1 4 848.46 42.82 2 -1 -4 954.95 37.89 -2 1 -4 971.59 45.79 2 -1 4 835.41 43.27 1 -2 -4 887.43 51.29 0 3 2 302.74 31.87 -3 3 -2 299.72 18.81 -3 0 2 266.29 21.37 3 0 -2 268.59 20.64 3 -3 2 270.52 19.46 0 3 -2 455.71 23.84 -3 0 -2 418.25 32.27 3 -3 -2 454.48 33.50 -3 3 2 472.39 33.46 0 3 -2 459.83 20.93 3 0 2 464.96 32.54 2 -3 3 118.42 15.64 3 -2 3 177.96 14.96 -3 1 3 149.96 16.27 1 2 3 163.85 20.60 3 -1 -3 189.97 16.55 -1 3 3 141.00 21.32 -3 2 -3 177.39 14.62 -2 3 -3 141.24 8.44 1 -3 -3 149.52 39.85 -2 -1 3 134.46 11.46 2 1 -3 122.87 17.38 -2 3 3 201.70 21.21 3 -2 -3 173.98 29.80 -3 1 -3 176.89 16.81 2 -3 -3 202.16 23.26 3 -1 3 179.56 16.68 1 -3 3 147.11 13.86 -1 -2 3 137.62 9.47 -1 3 -3 145.11 8.25 1 2 -3 147.71 9.16 -2 -1 -3 200.77 31.39 -3 2 3 164.20 17.92 2 1 3 214.66 19.28 0 0 5 3747.43 128.53 2 -2 -4 363.24 27.14 -2 2 4 333.58 24.06 2 0 4 286.42 22.97 -2 0 -4 349.40 24.86 -2 2 -4 832.21 24.95 0 2 4 808.02 52.02 2 -2 4 822.98 25.48 2 0 -4 945.80 43.22 -2 0 4 797.38 29.79 0 1 5 643.84 34.89 1 0 -5 708.26 32.16 -1 0 5 577.55 20.17 1 -1 5 572.08 16.99 1 -1 -5 499.10 25.96 0 -1 5 376.98 7.97 -1 1 5 416.95 22.97 0 -1 5 384.83 9.94 1 0 5 440.15 30.97 2 2 0 39.04 11.97 2 -4 0 62.56 20.99 -2 4 0 30.13 17.62 4 -2 0 25.68 13.44 -4 2 0 53.48 13.38 -2 -2 0 29.74 13.26 -2 4 1 45.41 12.64 2 -4 -1 1.49 13.74 -4 2 -1 24.89 11.59 4 -2 1 27.94 11.99 2 2 1 22.47 11.84 -2 -2 1 20.29 10.49 2 2 -1 9.16 8.90 4 -2 -1 8.74 12.67 -4 2 1 3.93 11.78 2 -4 1 23.53 10.76 -2 4 -1 32.52 8.50 -2 -2 -1 35.58 13.17 -3 3 -3 636.71 27.55 0 3 3 626.37 49.59 -3 0 3 617.36 30.03 3 0 -3 639.38 30.14 3 -3 3 570.75 27.85 -3 3 3 1553.02 76.72 3 -3 -3 1687.46 82.20 -3 0 -3 1647.16 99.47 3 0 3 1648.63 101.82 0 3 -3 1549.76 49.24 0 3 -3 1713.88 58.23 1 3 0 208.50 21.05 3 1 0 251.90 24.31 1 -4 0 222.61 27.90 4 -1 0 341.41 25.09 -1 4 0 287.70 21.59 4 -3 0 309.56 26.49 -4 1 0 237.78 25.27 -3 4 0 283.47 22.84 -3 -1 0 258.67 24.38 -4 3 0 244.38 23.89 3 -4 0 229.34 25.38 4 -3 -1 177.04 23.31 1 3 -1 143.20 24.39 3 1 1 156.98 21.03 -3 -1 -1 167.41 21.72 4 -1 1 185.22 21.53 -4 1 -1 159.29 20.96 -1 4 -1 215.43 27.64 -4 3 1 149.45 20.91 -3 4 1 159.78 21.80 3 -4 -1 175.42 22.61 -3 4 -1 270.93 20.77 1 -4 -1 237.01 31.98 4 -3 1 285.05 24.20 -4 3 -1 262.59 23.66 -3 -1 1 244.24 22.65 4 -1 -1 266.57 25.87 -4 1 1 276.29 24.87 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79.48 36.07 -8 -2 2 41.54 34.48 10 -5 5 197.33 58.59 -5 10 5 167.76 95.37 -5 10 -5 118.63 48.16 10 -5 -5 251.54 64.22 -10 5 -5 211.43 77.17 5 -10 -5 172.23 79.45 -10 5 5 180.80 54.21 5 5 -5 176.69 37.53 5 5 5 230.64 89.43 -7 -3 4 124.34 37.29 7 3 -4 105.86 33.07 3 7 4 68.49 59.12 10 -3 -4 12.21 46.67 3 7 4 87.49 69.94 3 7 4 12.71 68.39 7 -10 4 106.61 38.55 -7 10 -4 80.54 30.76 -10 7 -4 96.76 40.94 10 -7 4 5.94 44.13 -3 10 4 110.62 47.23 -10 3 4 120.46 42.78 3 7 -4 599.07 85.20 3 7 -4 563.87 69.00 7 3 4 648.45 107.38 -10 3 -4 718.54 97.80 -3 10 -4 449.96 96.30 -7 10 4 708.69 101.61 -10 7 4 651.69 99.00 7 -10 -4 555.33 125.18 10 -7 -4 646.92 112.15 10 -3 4 631.62 98.13 2 2 13 186.24 40.64 -4 2 13 94.27 29.29 2 2 13 28.80 65.73 4 -2 13 172.77 39.34 4 -2 13 146.97 32.28 -2 4 13 255.22 42.55 1 6 10 280.24 67.49 -6 -1 10 157.04 32.41 7 -1 -10 273.60 43.48 -7 6 -10 153.15 33.70 7 -6 10 199.36 35.09 -1 7 10 262.61 97.52 1 6 10 288.70 65.40 6 1 -10 181.99 52.62 -7 1 10 5.67 39.30 -1 7 10 489.91 66.51 -6 7 10 125.63 42.07 6 -7 -10 119.31 85.67 7 -6 -10 103.18 45.72 -7 6 10 89.36 60.29 7 -1 10 8.18 39.62 6 1 10 82.86 43.18 -1 1 14 89.38 34.04 -1 1 14 89.92 33.19 0 1 14 360.98 42.95 0 1 14 379.24 43.29 10 -4 -5 71.22 37.00 6 4 -5 58.91 24.77 -6 10 -5 35.47 20.99 -6 -4 5 -1.55 26.52 10 -6 5 48.96 52.15 4 6 5 15.58 58.43 -10 4 5 32.14 33.23 6 -10 5 11.54 29.23 -4 10 5 44.78 37.87 -10 6 -5 -34.74 48.22 -10 4 -5 247.62 84.11 -6 10 5 196.77 58.89 10 -4 5 156.64 56.20 6 -10 -5 162.55 77.98 4 6 -5 162.49 55.40 -10 6 5 264.86 57.39 -4 10 -5 120.01 30.58 6 4 5 181.62 60.65 10 -6 -5 210.01 62.53 -1 4 13 21.14 40.28 1 3 13 -9.63 26.90 -4 1 13 15.73 21.55 1 3 13 43.77 25.38 -1 4 13 19.78 26.04 -4 3 13 -1.67 19.71 3 1 13 2.74 26.31 -3 4 13 109.00 23.13 4 -1 13 -20.49 23.09 4 -1 13 7.93 18.70 3 1 13 20.28 22.08 -8 6 9 16.64 31.62 -6 8 9 13.01 56.48 -8 2 -9 57.93 32.83 8 -2 9 42.78 31.96 6 2 9 -20.37 35.60 8 -6 -9 62.81 39.54 6 -8 -9 54.09 48.57 2 6 9 195.13 69.95 -2 8 9 203.23 99.67 2 6 9 278.89 58.88 8 -2 -9 210.85 46.35 -6 -2 9 152.79 31.97 -8 6 -9 84.55 54.54 6 2 -9 143.56 33.76 8 -6 9 155.29 38.77 -2 10 -3 504.36 63.45 10 -2 3 475.29 135.36 8 2 3 511.54 91.21 10 -8 -3 15.28 144.55 8 -10 -3 495.01 153.16 -8 -2 -3 545.02 98.02 -10 2 -3 432.72 131.22 2 8 -3 502.73 59.56 -8 10 3 514.02 87.05 -10 8 3 479.71 132.69 -2 10 -3 396.36 65.69 2 8 3 770.16 117.73 -10 8 -3 942.41 107.40 8 -10 3 20.27 170.86 -8 10 -3 934.57 140.22 2 8 3 776.61 134.51 -8 -2 3 880.01 107.56 -10 2 3 828.72 113.27 -2 10 3 987.38 123.01 10 -8 3 736.77 123.90 10 -2 -3 944.87 118.03 8 2 -3 1034.38 151.27 0 9 4 15.18 39.40 -9 0 4 48.96 29.93 0 9 4 6.58 38.49 9 0 -4 11.92 29.91 -9 9 -4 24.42 27.77 9 -9 4 58.89 33.39 9 -9 -4 101.41 48.46 -9 9 4 93.48 42.27 9 0 4 33.48 42.00 0 9 -4 85.12 26.06 0 9 -4 0.17 27.09 -9 0 -4 37.58 43.15 -5 5 12 -1.71 24.01 5 -5 -12 33.06 32.60 0 5 12 25.62 31.27 0 5 12 0.74 31.00 5 0 -12 14.49 15.85 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68164 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' '-x, -x+y, -z' 'x-y, -y, -z' 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 Te1 Te 0.000000 0.000000 0.21466(15) 0.0113(5) Uani 0.8661 3 d S T P . . Sb1 Sb 0.000000 0.000000 0.21466(15) 0.0113(5) Uani 0.1339 3 d S T P . . Te2 Te 0.08492(15) 0.41220(15) 0.31180(9) 0.0127(3) Uani 1 1 d . . . . . Te3 Te 0.666667 0.333333 0.10707(17) 0.0186(5) Uani 1 3 d S T P . . Cu Cu 0.3694(3) 0.3849(3) 0.13972(19) 0.0170(6) Uani 1 1 d . . . . . Ca1 Ca 0.000000 0.000000 0.500000 0.018(2) Uani 1 6 d S T P . . Ca2 Ca 0.000000 0.2507(4) 0.000000 0.0192(13) Uani 0.871(5) 2 d S T P . . Pb2 Pb 0.000000 0.2507(4) 0.000000 0.0192(13) Uani 0.129(5) 2 d S T P . . S1 S 0.666667 0.333333 0.3992(6) 0.0160(17) Uani 1 3 d S T P . . O1 O 0.5031(16) 0.3014(16) 0.3569(11) 0.030(4) Uani 1 1 d . . . . . O2 O 0.666667 0.333333 0.5228(16) 0.035(6) Uani 1 3 d S T P . . O3 O 0.1614(13) 0.1712(13) 0.1182(9) 0.009(3) Uani 1 1 d . . . . . O4 O 0.4755(15) 0.3019(15) 0.0278(10) 0.016(3) Uani 1 1 d . . . . . O5 O -0.0022(15) 0.4079(14) 0.1679(10) 0.012(3) Uani 1 1 d . . . . . O6 O 0.3044(14) 0.4658(15) 0.2664(10) 0.018(3) Uani 1 1 d . . . . . O7 O -0.0017(13) 0.1635(14) 0.3170(8) 0.012(3) Uani 1 1 d . . . . . OW O 0.256(2) 0.256(2) 0.500000 0.035(6) Uani 1 2 d DS T P . . H H 0.341(19) 0.26(3) 0.458(15) 0.042 Uiso 1 1 d D U . . . 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 Te1 0.0090(7) 0.0090(7) 0.0158(10) 0.000 0.000 0.0045(3) Sb1 0.0090(7) 0.0090(7) 0.0158(10) 0.000 0.000 0.0045(3) Te2 0.0107(7) 0.0121(6) 0.0167(6) -0.0004(5) -0.0003(5) 0.0067(6) Te3 0.0154(7) 0.0154(7) 0.0249(12) 0.000 0.000 0.0077(3) Cu 0.0121(12) 0.0120(12) 0.0221(13) -0.0029(9) 0.0008(9) 0.0025(11) Ca1 0.014(3) 0.014(3) 0.025(5) 0.000 0.000 0.0071(15) Ca2 0.015(2) 0.0183(17) 0.023(2) -0.0010(8) -0.0021(16) 0.0075(11) Pb2 0.015(2) 0.0183(17) 0.023(2) -0.0010(8) -0.0021(16) 0.0075(11) S1 0.015(3) 0.015(3) 0.018(4) 0.000 0.000 0.0076(13) O1 0.019(8) 0.041(9) 0.032(8) -0.003(6) -0.007(6) 0.017(7) O2 0.047(9) 0.047(9) 0.010(11) 0.000 0.000 0.023(5) O3 0.003(6) 0.007(6) 0.010(6) -0.003(5) 0.000(5) -0.002(5) O4 0.013(7) 0.017(7) 0.014(6) -0.005(5) 0.004(5) 0.004(5) O5 0.022(7) 0.013(7) 0.011(6) -0.008(5) -0.009(5) 0.015(6) O6 0.015(7) 0.015(7) 0.016(7) -0.004(5) 0.003(6) 0.002(6) O7 0.016(7) 0.014(7) 0.007(6) -0.003(5) 0.001(4) 0.009(6) OW 0.032(9) 0.032(9) 0.019(12) -0.007(5) 0.007(5) 0.001(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ca Ca 0.2262 0.3064 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O3 Te1 O3 87.3(5) 2 3 O3 Te1 O3 87.3(5) 2 . O3 Te1 O3 87.3(5) 3 . O3 Te1 O7 177.2(4) 2 3 O3 Te1 O7 92.9(4) 3 3 O3 Te1 O7 95.5(5) . 3 O3 Te1 O7 92.9(4) 2 2 O3 Te1 O7 95.5(5) 3 2 O3 Te1 O7 177.2(4) . 2 O7 Te1 O7 84.4(5) 3 2 O3 Te1 O7 95.5(5) 2 . O3 Te1 O7 177.2(4) 3 . O3 Te1 O7 92.9(4) . . O7 Te1 O7 84.4(5) 3 . O7 Te1 O7 84.4(5) 2 . O3 Te1 Ca1 127.2(3) 2 . O3 Te1 Ca1 127.2(3) 3 . O3 Te1 Ca1 127.2(3) . . O7 Te1 Ca1 50.8(3) 3 . O7 Te1 Ca1 50.8(3) 2 . O7 Te1 Ca1 50.8(3) . . O3 Te1 Ca2 42.4(3) 2 2 O3 Te1 Ca2 46.2(3) 3 2 O3 Te1 Ca2 94.6(3) . 2 O7 Te1 Ca2 137.2(3) 3 2 O7 Te1 Ca2 87.4(3) 2 2 O7 Te1 Ca2 136.5(3) . 2 Ca1 Te1 Ca2 138.24(5) . 2 O3 Te1 Ca2 94.6(3) 2 3 O3 Te1 Ca2 42.4(3) 3 3 O3 Te1 Ca2 46.2(3) . 3 O7 Te1 Ca2 87.4(3) 3 3 O7 Te1 Ca2 136.5(3) 2 3 O7 Te1 Ca2 137.2(3) . 3 Ca1 Te1 Ca2 138.24(5) . 3 Ca2 Te1 Ca2 70.45(8) 2 3 O3 Te1 Ca2 46.2(3) 2 . O3 Te1 Ca2 94.6(3) 3 . O3 Te1 Ca2 42.4(3) . . O7 Te1 Ca2 136.5(3) 3 . O7 Te1 Ca2 137.2(3) 2 . O7 Te1 Ca2 87.4(3) . . Ca1 Te1 Ca2 138.24(5) . . Ca2 Te1 Ca2 70.45(8) 2 . Ca2 Te1 Ca2 70.45(8) 3 . O3 Te1 Cu 22.6(3) 2 2 O3 Te1 Cu 104.1(3) 3 2 O3 Te1 Cu 102.9(3) . 2 O7 Te1 Cu 155.4(3) 3 2 O7 Te1 Cu 76.5(3) 2 2 O7 Te1 Cu 78.5(3) . 2 Ca1 Te1 Cu 104.56(5) . 2 Ca2 Te1 Cu 58.03(4) 2 2 Ca2 Te1 Cu 117.17(8) 3 2 Ca2 Te1 Cu 60.67(4) . 2 O5 Te2 O6 97.2(5) . . O5 Te2 O7 94.7(4) . . O6 Te2 O7 94.0(4) . . O5 Te2 O6 73.0(4) . 3_565 O6 Te2 O6 87.5(6) . 3_565 O7 Te2 O6 167.6(4) . 3_565 O5 Te2 O2 139.2(4) . 4_556 O6 Te2 O2 72.4(4) . 4_556 O7 Te2 O2 124.8(3) . 4_556 O6 Te2 O2 67.3(3) 3_565 4_556 O5 Te2 O1 78.9(4) . 2 O6 Te2 O1 160.0(4) . 2 O7 Te2 O1 67.0(4) . 2 O6 Te2 O1 109.7(4) 3_565 2 O2 Te2 O1 123.0(3) 4_556 2 O5 Te2 O1 76.4(4) . 3_565 O6 Te2 O1 153.7(4) . 3_565 O7 Te2 O1 111.8(4) . 3_565 O6 Te2 O1 66.2(4) 3_565 3_565 O2 Te2 O1 95.5(3) 4_556 3_565 O1 Te2 O1 44.8(4) 2 3_565 O5 Te2 Cu 36.9(3) . 3_565 O6 Te2 Cu 99.9(4) . 3_565 O7 Te2 Cu 130.6(3) . 3_565 O6 Te2 Cu 37.2(3) 3_565 3_565 O2 Te2 Cu 104.55(19) 4_556 3_565 O1 Te2 Cu 88.8(2) 2 3_565 O1 Te2 Cu 59.7(2) 3_565 3_565 O5 Te2 Cu 77.2(4) . . O6 Te2 Cu 25.8(4) . . O7 Te2 Cu 79.6(3) . . O6 Te2 Cu 97.0(3) 3_565 . O2 Te2 Cu 98.23(19) 4_556 . O1 Te2 Cu 136.8(2) 2 . O1 Te2 Cu 152.0(2) 3_565 . Cu Te2 Cu 93.15(9) 3_565 . O5 Te2 OW 149.8(4) . . O6 Te2 OW 69.6(4) . . O7 Te2 OW 60.7(4) . . O6 Te2 OW 130.8(4) 3_565 . O2 Te2 OW 64.5(3) 4_556 . O1 Te2 OW 104.0(4) 2 . O1 Te2 OW 127.1(3) 3_565 . Cu Te2 OW 166.3(3) 3_565 . Cu Te2 OW 80.95(13) . . O5 Te2 O3 66.4(4) . . O6 Te2 O3 56.8(4) . . O7 Te2 O3 52.8(3) . . O6 Te2 O3 119.4(3) 3_565 . O2 Te2 O3 127.3(2) 4_556 . O1 Te2 O3 104.3(3) 2 . O1 Te2 O3 136.5(3) 3_565 . Cu Te2 O3 97.71(19) 3_565 . Cu Te2 O3 32.62(17) . . OW Te2 O3 84.0(2) . . O4 Te3 O4 96.8(5) 2_655 3_665 O4 Te3 O4 96.8(5) 2_655 . O4 Te3 O4 96.8(5) 3_665 . O4 Te3 O5 76.0(4) 2_655 1_655 O4 Te3 O5 70.6(4) 3_665 1_655 O4 Te3 O5 164.2(4) . 1_655 O4 Te3 O5 70.6(4) 2_655 3 O4 Te3 O5 164.2(4) 3_665 3 O4 Te3 O5 76.0(4) . 3 O5 Te3 O5 113.7(2) 1_655 3 O4 Te3 O5 164.2(4) 2_655 2_665 O4 Te3 O5 76.0(4) 3_665 2_665 O4 Te3 O5 70.6(4) . 2_665 O5 Te3 O5 113.7(2) 1_655 2_665 O5 Te3 O5 113.7(2) 3 2_665 O4 Te3 Cu 41.0(4) 2_655 2_655 O4 Te3 Cu 133.5(4) 3_665 2_655 O4 Te3 Cu 105.2(4) . 2_655 O5 Te3 Cu 78.7(2) 1_655 2_655 O5 Te3 Cu 39.6(2) 3 2_655 O5 Te3 Cu 150.0(2) 2_665 2_655 O4 Te3 Cu 105.2(4) 2_655 3_665 O4 Te3 Cu 41.0(4) 3_665 3_665 O4 Te3 Cu 133.5(4) . 3_665 O5 Te3 Cu 39.6(2) 1_655 3_665 O5 Te3 Cu 150.0(2) 3 3_665 O5 Te3 Cu 78.7(2) 2_665 3_665 Cu Te3 Cu 118.34(2) 2_655 3_665 O4 Te3 Cu 133.5(4) 2_655 . O4 Te3 Cu 105.2(4) 3_665 . O4 Te3 Cu 41.0(4) . . O5 Te3 Cu 150.0(2) 1_655 . O5 Te3 Cu 78.7(2) 3 . O5 Te3 Cu 39.6(2) 2_665 . Cu Te3 Cu 118.34(2) 2_655 . Cu Te3 Cu 118.34(2) 3_665 . O4 Te3 O1 130.4(4) 2_655 3_665 O4 Te3 O1 95.6(4) 3_665 3_665 O4 Te3 O1 129.0(4) . 3_665 O5 Te3 O1 63.6(3) 1_655 3_665 O5 Te3 O1 99.9(3) 3 3_665 O5 Te3 O1 64.9(3) 2_665 3_665 Cu Te3 O1 101.1(2) 2_655 3_665 Cu Te3 O1 59.3(2) 3_665 3_665 Cu Te3 O1 88.0(2) . 3_665 O4 Te3 O1 95.6(4) 2_655 2_655 O4 Te3 O1 129.0(4) 3_665 2_655 O4 Te3 O1 130.4(4) . 2_655 O5 Te3 O1 64.9(3) 1_655 2_655 O5 Te3 O1 63.6(3) 3 2_655 O5 Te3 O1 99.9(3) 2_665 2_655 Cu Te3 O1 59.3(2) 2_655 2_655 Cu Te3 O1 88.0(2) 3_665 2_655 Cu Te3 O1 101.1(2) . 2_655 O1 Te3 O1 42.4(4) 3_665 2_655 O4 Te3 O1 129.0(4) 2_655 . O4 Te3 O1 130.4(4) 3_665 . O4 Te3 O1 95.6(4) . . O5 Te3 O1 99.9(3) 1_655 . O5 Te3 O1 65.0(3) 3 . O5 Te3 O1 63.6(3) 2_665 . Cu Te3 O1 88.0(2) 2_655 . Cu Te3 O1 101.1(2) 3_665 . Cu Te3 O1 59.3(2) . . O1 Te3 O1 42.4(4) 3_665 . O1 Te3 O1 42.4(4) 2_655 . O6 Cu O3 99.0(5) . . O6 Cu O5 82.6(5) . 2_665 O3 Cu O5 174.2(5) . 2_665 O6 Cu O4 168.0(5) . . O3 Cu O4 87.0(5) . . O5 Cu O4 90.5(5) 2_665 . O6 Cu O4 110.5(5) . 4 O3 Cu O4 86.8(4) . 4 O5 Cu O4 97.9(5) 2_665 4 O4 Cu O4 80.1(5) . 4 O6 Cu Te3 130.2(4) . . O3 Cu Te3 109.4(3) . . O5 Cu Te3 65.8(4) 2_665 . O4 Cu Te3 37.8(4) . . O4 Cu Te3 111.1(3) 4 . O6 Cu O1 70.7(4) . . O3 Cu O1 99.8(4) . . O5 Cu O1 75.4(4) 2_665 . O4 Cu O1 98.0(4) . . O4 Cu O1 173.1(4) 4 . Te3 Cu O1 64.8(2) . . OW Ca1 OW 120.000(5) 3 2 OW Ca1 OW 120.000(2) 3 . OW Ca1 OW 120.000(3) 2 . OW Ca1 O7 73.3(2) 3 2 OW Ca1 O7 73.8(2) 2 2 OW Ca1 O7 124.5(2) . 2 OW Ca1 O7 124.5(2) 3 5_556 OW Ca1 O7 73.8(2) 2 5_556 OW Ca1 O7 73.3(2) . 5_556 O7 Ca1 O7 147.6(4) 2 5_556 OW Ca1 O7 73.3(2) 3 4_556 OW Ca1 O7 124.5(2) 2 4_556 OW Ca1 O7 73.8(2) . 4_556 O7 Ca1 O7 146.6(4) 2 4_556 O7 Ca1 O7 58.7(4) 5_556 4_556 OW Ca1 O7 124.5(2) 3 . OW Ca1 O7 73.3(2) 2 . OW Ca1 O7 73.8(2) . . O7 Ca1 O7 58.7(4) 2 . O7 Ca1 O7 111.0(4) 5_556 . O7 Ca1 O7 147.6(5) 4_556 . OW Ca1 O7 73.8(2) 3 3 OW Ca1 O7 124.5(2) 2 3 OW Ca1 O7 73.3(2) . 3 O7 Ca1 O7 58.7(4) 2 3 O7 Ca1 O7 146.6(4) 5_556 3 O7 Ca1 O7 111.0(4) 4_556 3 O7 Ca1 O7 58.7(4) . 3 OW Ca1 O7 73.8(2) 3 6_556 OW Ca1 O7 73.3(2) 2 6_556 OW Ca1 O7 124.5(2) . 6_556 O7 Ca1 O7 111.0(5) 2 6_556 O7 Ca1 O7 58.7(4) 5_556 6_556 O7 Ca1 O7 58.7(4) 4_556 6_556 O7 Ca1 O7 146.6(4) . 6_556 O7 Ca1 O7 147.6(4) 3 6_556 OW Ca1 Te1 90.0 3 4_556 OW Ca1 Te1 90.0 2 4_556 OW Ca1 Te1 90.000(1) . 4_556 O7 Ca1 Te1 145.5(2) 2 4_556 O7 Ca1 Te1 34.5(2) 5_556 4_556 O7 Ca1 Te1 34.5(2) 4_556 4_556 O7 Ca1 Te1 145.5(2) . 4_556 O7 Ca1 Te1 145.5(2) 3 4_556 O7 Ca1 Te1 34.5(2) 6_556 4_556 OW Ca1 Te1 90.0 3 . OW Ca1 Te1 90.0 2 . OW Ca1 Te1 90.000(1) . . O7 Ca1 Te1 34.5(2) 2 . O7 Ca1 Te1 145.5(2) 5_556 . O7 Ca1 Te1 145.5(2) 4_556 . O7 Ca1 Te1 34.5(2) . . O7 Ca1 Te1 34.5(2) 3 . O7 Ca1 Te1 145.5(2) 6_556 . Te1 Ca1 Te1 180.0 4_556 . O3 Ca2 O3 104.9(5) . 5 O3 Ca2 O5 146.1(4) . 5 O3 Ca2 O5 83.3(3) 5 5 O3 Ca2 O5 83.3(3) . . O3 Ca2 O5 146.1(4) 5 . O5 Ca2 O5 108.5(5) 5 . O3 Ca2 O4 74.6(4) . 4 O3 Ca2 O4 126.4(3) 5 4 O5 Ca2 O4 74.2(4) 5 4 O5 Ca2 O4 87.5(4) . 4 O3 Ca2 O4 126.4(3) . 2 O3 Ca2 O4 74.6(4) 5 2 O5 Ca2 O4 87.5(4) 5 2 O5 Ca2 O4 74.2(4) . 2 O4 Ca2 O4 148.7(6) 4 2 O3 Ca2 O3 64.6(5) . 2 O3 Ca2 O3 70.0(4) 5 2 O5 Ca2 O3 145.8(4) 5 2 O5 Ca2 O3 85.0(4) . 2 O4 Ca2 O3 139.1(4) 4 2 O4 Ca2 O3 65.5(4) 2 2 O3 Ca2 O3 70.0(4) . 4 O3 Ca2 O3 64.6(5) 5 4 O5 Ca2 O3 85.0(4) 5 4 O5 Ca2 O3 145.8(4) . 4 O4 Ca2 O3 65.5(4) 4 4 O4 Ca2 O3 139.1(4) 2 4 O3 Ca2 O3 101.5(5) 2 4 O3 Ca2 Cu 131.6(3) . 5 O3 Ca2 Cu 34.0(2) 5 5 O5 Ca2 Cu 71.8(3) 5 5 O5 Ca2 Cu 118.2(3) . 5 O4 Ca2 Cu 142.4(3) 4 5 O4 Ca2 Cu 44.1(3) 2 5 O3 Ca2 Cu 74.2(3) 2 5 O3 Ca2 Cu 95.8(2) 4 5 O3 Ca2 Cu 34.0(2) . . O3 Ca2 Cu 131.6(3) 5 . O5 Ca2 Cu 118.2(3) 5 . O5 Ca2 Cu 71.8(3) . . O4 Ca2 Cu 44.1(3) 4 . O4 Ca2 Cu 142.4(3) 2 . O3 Ca2 Cu 95.8(2) 2 . O3 Ca2 Cu 74.2(3) 4 . Cu Ca2 Cu 164.38(14) 5 . O3 Ca2 Te1 32.4(2) . . O3 Ca2 Te1 91.9(3) 5 . O5 Ca2 Te1 174.0(3) 5 . O5 Ca2 Te1 77.5(3) . . O4 Ca2 Te1 106.2(3) 4 . O4 Ca2 Te1 94.6(3) 2 . O3 Ca2 Te1 33.0(2) 2 . O3 Ca2 Te1 89.8(3) 4 . Cu Ca2 Te1 106.03(7) 5 . Cu Ca2 Te1 62.80(5) . . O1 S1 O1 108.7(6) 2_655 3_665 O1 S1 O1 108.7(6) 2_655 . O1 S1 O1 108.7(6) 3_665 . O1 S1 O2 110.2(5) 2_655 . O1 S1 O2 110.2(5) 3_665 . O1 S1 O2 110.2(5) . . O1 S1 Te3 69.8(5) 2_655 . O1 S1 Te3 69.8(5) 3_665 . O1 S1 Te3 69.8(5) . . O2 S1 Te3 180.0 . . O1 S1 Te2 57.1(5) 2_655 3 O1 S1 Te2 143.2(6) 3_665 3 O1 S1 Te2 56.4(5) . 3 O2 S1 Te2 106.54(11) . 3 Te3 S1 Te2 73.46(11) . 3 O1 S1 Te2 56.4(5) 2_655 1_655 O1 S1 Te2 57.1(5) 3_665 1_655 O1 S1 Te2 143.2(6) . 1_655 O2 S1 Te2 106.54(11) . 1_655 Te3 S1 Te2 73.46(11) . 1_655 Te2 S1 Te2 112.24(10) 3 1_655 O1 S1 Te2 143.2(6) 2_655 2_665 O1 S1 Te2 56.4(5) 3_665 2_665 O1 S1 Te2 57.1(5) . 2_665 O2 S1 Te2 106.54(11) . 2_665 Te3 S1 Te2 73.46(11) . 2_665 Te2 S1 Te2 112.24(10) 3 2_665 Te2 S1 Te2 112.24(10) 1_655 2_665 O1 S1 Te2 86.6(5) 2_655 5_656 O1 S1 Te2 97.2(5) 3_665 5_656 O1 S1 Te2 142.8(6) . 5_656 O2 S1 Te2 33.63(6) . 5_656 Te3 S1 Te2 146.37(6) . 5_656 Te2 S1 Te2 113.97(10) 3 5_656 Te2 S1 Te2 73.53(6) 1_655 5_656 Te2 S1 Te2 126.03(12) 2_665 5_656 O1 S1 Te2 142.8(6) 2_655 6_666 O1 S1 Te2 86.6(5) 3_665 6_666 O1 S1 Te2 97.2(5) . 6_666 O2 S1 Te2 33.63(6) . 6_666 Te3 S1 Te2 146.37(6) . 6_666 Te2 S1 Te2 126.03(12) 3 6_666 Te2 S1 Te2 113.97(10) 1_655 6_666 Te2 S1 Te2 73.53(6) 2_665 6_666 Te2 S1 Te2 57.33(9) 5_656 6_666 O1 S1 Te2 97.2(5) 2_655 4_556 O1 S1 Te2 142.8(6) 3_665 4_556 O1 S1 Te2 86.6(5) . 4_556 O2 S1 Te2 33.63(6) . 4_556 Te3 S1 Te2 146.37(6) . 4_556 Te2 S1 Te2 73.53(6) 3 4_556 Te2 S1 Te2 126.03(12) 1_655 4_556 Te2 S1 Te2 113.97(10) 2_665 4_556 Te2 S1 Te2 57.33(9) 5_656 4_556 Te2 S1 Te2 57.33(9) 6_666 4_556 O1 S1 Cu 30.0(5) 2_655 2_655 O1 S1 Cu 103.7(6) 3_665 2_655 O1 S1 Cu 83.1(5) . 2_655 O2 S1 Cu 136.15(7) . 2_655 Te3 S1 Cu 43.85(7) . 2_655 Te2 S1 Cu 45.61(6) 3 2_655 Te2 S1 Cu 69.98(9) 1_655 2_655 Te2 S1 Cu 115.22(17) 2_665 2_655 Te2 S1 Cu 116.64(4) 5_656 2_655 Te2 S1 Cu 168.97(12) 6_666 2_655 Te2 S1 Cu 111.79(4) 4_556 2_655 S1 O1 Te2 100.5(6) . 3 S1 O1 Cu 136.4(7) . . Te2 O1 Cu 95.2(3) 3 . S1 O1 Te2 99.7(6) . 2_665 Te2 O1 Te2 155.5(4) 3 2_665 Cu O1 Te2 60.4(2) . 2_665 S1 O1 Te3 85.5(6) . . Te2 O1 Te3 84.1(3) 3 . Cu O1 Te3 55.9(2) . . Te2 O1 Te3 83.8(3) 2_665 . S1 O1 Te2 73.6(5) . 4_556 Te2 O1 Te2 76.5(3) 3 4_556 Cu O1 Te2 150.0(4) . 4_556 Te2 O1 Te2 122.8(4) 2_665 4_556 Te3 O1 Te2 148.1(4) . 4_556 S1 O1 Te2 154.8(7) . . Te2 O1 Te2 102.9(3) 3 . Cu O1 Te2 50.06(18) . . Te2 O1 Te2 60.5(2) 2_665 . Te3 O1 Te2 105.9(3) . . Te2 O1 Te2 103.0(3) 4_556 . S1 O1 Te2 64.3(5) . 6_666 Te2 O1 Te2 129.4(4) 3 6_666 Cu O1 Te2 130.0(4) . 6_666 Te2 O1 Te2 72.5(2) 2_665 6_666 Te3 O1 Te2 136.7(3) . 6_666 Te2 O1 Te2 53.12(15) 4_556 6_666 Te2 O1 Te2 93.4(2) . 6_666 S1 O2 Te2 130.7(3) . 5_656 S1 O2 Te2 130.7(3) . 4_556 Te2 O2 Te2 82.1(4) 5_656 4_556 S1 O2 Te2 130.7(3) . 6_666 Te2 O2 Te2 82.1(4) 5_656 6_666 Te2 O2 Te2 82.1(4) 4_556 6_666 S1 O2 Te2 54.4(2) . 3 Te2 O2 Te2 125.20(2) 5_656 3 Te2 O2 Te2 77.06(7) 4_556 3 Te2 O2 Te2 141.96(4) 6_666 3 S1 O2 Te2 54.4(2) . 1_655 Te2 O2 Te2 77.06(7) 5_656 1_655 Te2 O2 Te2 141.96(4) 4_556 1_655 Te2 O2 Te2 125.20(2) 6_666 1_655 Te2 O2 Te2 89.5(3) 3 1_655 S1 O2 Te2 54.4(2) . 2_665 Te2 O2 Te2 141.96(4) 5_656 2_665 Te2 O2 Te2 125.20(2) 4_556 2_665 Te2 O2 Te2 77.06(7) 6_666 2_665 Te2 O2 Te2 89.5(3) 3 2_665 Te2 O2 Te2 89.5(3) 1_655 2_665 Te1 O3 Cu 135.2(6) . . Te1 O3 Ca2 105.3(4) . . Cu O3 Ca2 102.3(5) . . Te1 O3 Ca2 100.8(4) . 3 Cu O3 Ca2 103.9(4) . 3 Ca2 O3 Ca2 107.2(4) . 3 Te1 O3 Te2 78.5(3) . . Cu O3 Te2 71.5(3) . . Ca2 O3 Te2 81.5(3) . . Ca2 O3 Te2 171.0(4) 3 . Te1 O3 Cu 158.5(5) . 4 Cu O3 Cu 65.7(3) . 4 Ca2 O3 Cu 68.2(3) . 4 Ca2 O3 Cu 63.9(2) 3 4 Te2 O3 Cu 119.1(3) . 4 Te1 O3 Te2 62.9(3) . 3 Cu O3 Te2 92.5(4) . 3 Ca2 O3 Te2 165.1(4) . 3 Ca2 O3 Te2 68.6(2) 3 3 Te2 O3 Te2 103.5(3) . 3 Cu O3 Te2 119.2(3) 4 3 Te1 O3 Te3 125.9(4) . . Cu O3 Te3 43.9(2) . . Ca2 O3 Te3 128.7(4) . . Ca2 O3 Te3 63.3(2) 3 . Te2 O3 Te3 109.8(3) . . Cu O3 Te3 62.68(16) 4 . Te2 O3 Te3 63.28(16) 3 . Te3 O4 Cu 101.2(6) . . Te3 O4 Cu 143.9(6) . 4 Cu O4 Cu 99.6(5) . 4 Te3 O4 Ca2 115.1(5) . 3 Cu O4 Ca2 102.7(5) . 3 Cu O4 Ca2 88.5(4) 4 3 Te3 O4 Cu 47.4(3) . 2_655 Cu O4 Cu 116.5(5) . 2_655 Cu O4 Cu 139.9(4) 4 2_655 Ca2 O4 Cu 67.9(3) 3 2_655 Te3 O4 Cu 75.6(4) . 5_655 Cu O4 Cu 163.4(5) . 5_655 Cu O4 Cu 91.8(3) 4 5_655 Ca2 O4 Cu 65.4(3) 3 5_655 Cu O4 Cu 49.39(15) 2_655 5_655 Te3 O4 Te2 115.7(5) . 4 Cu O4 Te2 143.1(5) . 4 Cu O4 Te2 49.9(2) 4 4 Ca2 O4 Te2 62.2(2) 3 4 Cu O4 Te2 90.0(2) 2_655 4 Cu O4 Te2 43.17(12) 5_655 4 Te3 O4 Te3 131.8(5) . 4 Cu O4 Te3 65.2(3) . 4 Cu O4 Te3 39.1(2) 4 4 Ca2 O4 Te3 113.1(4) 3 4 Cu O4 Te3 177.9(3) 2_655 4 Cu O4 Te3 129.1(3) 5_655 4 Te2 O4 Te3 88.9(2) 4 4 Te3 O4 Te2 70.3(4) . 2_665 Cu O4 Te2 36.1(3) . 2_665 Cu O4 Te2 114.6(4) 4 2_665 Ca2 O4 Te2 132.6(4) 3 2_665 Cu O4 Te2 105.1(3) 2_655 2_665 Cu O4 Te2 145.8(3) 5_655 2_665 Te2 O4 Te2 161.9(3) 4 2_665 Te3 O4 Te2 75.69(19) 4 2_665 Te3 O4 Te2 68.8(3) . 3 Cu O4 Te2 77.6(3) . 3 Cu O4 Te2 145.1(4) 4 3 Ca2 O4 Te2 59.1(2) 3 3 Cu O4 Te2 42.41(12) 2_655 3 Cu O4 Te2 86.1(2) 5_655 3 Te2 O4 Te2 114.3(3) 4 3 Te3 O4 Te2 139.6(3) 4 3 Te2 O4 Te2 83.8(2) 2_665 3 Te2 O5 Cu 108.4(5) . 3_565 Te2 O5 Ca2 128.7(5) . . Cu O5 Ca2 115.9(5) 3_565 . Te2 O5 Te3 128.7(6) . 1_455 Cu O5 Te3 74.6(4) 3_565 1_455 Ca2 O5 Te3 88.3(3) . 1_455 Te2 O5 Cu 71.3(3) . . Cu O5 Cu 117.2(5) 3_565 . Ca2 O5 Cu 66.4(3) . . Te3 O5 Cu 154.6(4) 1_455 . Te2 O5 Cu 105.8(5) . 2 Cu O5 Cu 127.1(5) 3_565 2 Ca2 O5 Cu 66.3(3) . 2 Te3 O5 Cu 52.56(19) 1_455 2 Cu O5 Cu 111.3(3) . 2 Te2 O5 Cu 154.5(5) . 6_565 Cu O5 Cu 52.5(3) 3_565 6_565 Ca2 O5 Cu 63.8(3) . 6_565 Te3 O5 Cu 67.3(2) 1_455 6_565 Cu O5 Cu 101.0(3) . 6_565 Cu O5 Cu 99.6(3) 2 6_565 Te2 O5 Te3 120.5(5) . 4 Cu O5 Te3 68.7(3) 3_565 4 Ca2 O5 Te3 59.3(2) . 4 Te3 O5 Te3 108.4(3) 1_455 4 Cu O5 Te3 61.10(19) . 4 Cu O5 Te3 123.0(3) 2 4 Cu O5 Te3 41.51(12) 6_565 4 Te2 O5 Te2 64.2(3) . 3_565 Cu O5 Te2 47.8(3) 3_565 3_565 Ca2 O5 Te2 136.5(4) . 3_565 Te3 O5 Te2 115.8(3) 1_455 3_565 Cu O5 Te2 85.9(2) . 3_565 Cu O5 Te2 157.0(3) 2 3_565 Cu O5 Te2 91.5(2) 6_565 3_565 Te3 O5 Te2 78.3(2) 4 3_565 Te2 O6 Cu 128.6(6) . . Te2 O6 Te2 137.0(6) . 2_665 Cu O6 Te2 93.6(5) . 2_665 Te2 O6 Cu 51.8(3) . 3_565 Cu O6 Cu 104.0(5) . 3_565 Te2 O6 Cu 117.0(4) 2_665 3_565 Te2 O6 Te2 74.6(3) . 3_565 Cu O6 Te2 129.3(5) . 3_565 Te2 O6 Te2 71.3(3) 2_665 3_565 Cu O6 Te2 50.75(15) 3_565 3_565 Te2 O6 Te3 152.1(5) . . Cu O6 Te3 30.8(2) . . Te2 O6 Te3 69.8(3) 2_665 . Cu O6 Te3 131.9(3) 3_565 . Te2 O6 Te3 131.4(3) 3_565 . Te1 O7 Te2 134.9(5) . . Te1 O7 Ca1 94.7(4) . . Te2 O7 Ca1 123.7(4) . . Te1 O7 Cu 72.3(3) . . Te2 O7 Cu 67.7(3) . . Ca1 O7 Cu 121.8(3) . . Te1 O7 Cu 70.6(3) . 2 Te2 O7 Cu 103.5(4) . 2 Ca1 O7 Cu 119.6(3) . 2 Cu O7 Cu 109.0(3) . 2 Te1 O7 Te2 60.7(3) . 2 Te2 O7 Te2 148.7(4) . 2 Ca1 O7 Te2 70.2(2) . 2 Cu O7 Te2 132.6(3) . 2 Cu O7 Te2 51.12(14) 2 2 Te1 O7 Te2 49.4(3) . 3 Te2 O7 Te2 125.3(4) . 3 Ca1 O7 Te2 62.8(2) . 3 Cu O7 Te2 66.88(17) . 3 Cu O7 Te2 118.9(3) 2 3 Te2 O7 Te2 85.8(2) 2 3 Ca1 OW Te2 88.8(3) . . Ca1 OW Te2 88.8(3) . 4_556 Te2 OW Te2 177.7(7) . 4_556 Ca1 OW Te2 145.52(16) . 6_666 Te2 OW Te2 119.6(4) . 6_666 Te2 OW Te2 62.53(19) 4_556 6_666 Ca1 OW Te2 145.52(16) . 2_665 Te2 OW Te2 62.53(19) . 2_665 Te2 OW Te2 119.6(4) 4_556 2_665 Te2 OW Te2 69.0(3) 6_666 2_665 Ca1 OW Te2 72.7(3) . 3 Te2 OW Te2 103.41(14) . 3 Te2 OW Te2 75.88(9) 4_556 3 Te2 OW Te2 114.3(2) 6_666 3 Te2 OW Te2 94.49(16) 2_665 3 Ca1 OW Te2 72.7(3) . 5_556 Te2 OW Te2 75.88(9) . 5_556 Te2 OW Te2 103.41(14) 4_556 5_556 Te2 OW Te2 94.49(16) 6_666 5_556 Te2 OW Te2 114.3(2) 2_665 5_556 Te2 OW Te2 145.4(5) 3 5_556 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Te1 O3 1.906(10) 2 Te1 O3 1.906(10) 3 Te1 O3 1.906(10) . Te1 O7 1.934(10) 3 Te1 O7 1.934(10) 2 Te1 O7 1.934(10) . Te1 Ca1 3.4047(18) . Te1 Ca2 3.434(3) 2 Te1 Ca2 3.434(3) 3 Te1 Ca2 3.434(3) . Te1 Cu 3.557(2) 2 Te2 O5 1.884(11) . Te2 O6 1.887(11) . Te2 O7 1.995(11) . Te2 O6 2.379(11) 3_565 Te2 O2 3.026(13) 4_556 Te2 O1 3.103(13) 2 Te2 O1 3.121(13) 3_565 Te2 Cu 3.138(2) 3_565 Te2 Cu 3.415(3) . Te2 OW 3.4252(13) . Te2 O3 3.492(10) . Te3 O4 1.875(12) 2_655 Te3 O4 1.875(12) 3_665 Te3 O4 1.875(12) . Te3 O5 2.839(12) 1_655 Te3 O5 2.839(12) 3 Te3 O5 2.839(12) 2_665 Te3 Cu 3.000(2) 2_655 Te3 Cu 3.000(2) 3_665 Te3 Cu 3.000(2) . Te3 O1 3.280(13) 3_665 Te3 O1 3.280(13) 2_655 Te3 O1 3.280(13) . Cu O6 1.903(12) . Cu O3 1.941(11) . Cu O5 1.985(11) 2_665 Cu O4 2.006(12) . Cu O4 2.360(12) 4 Cu O1 3.116(13) . Ca1 OW 2.34(2) 3 Ca1 OW 2.34(2) 2 Ca1 OW 2.34(2) . Ca1 O7 2.649(10) 2 Ca1 O7 2.649(10) 5_556 Ca1 O7 2.649(10) 4_556 Ca1 O7 2.649(10) . Ca1 O7 2.649(10) 3 Ca1 O7 2.649(10) 6_556 Ca2 O3 2.398(11) . Ca2 O3 2.398(11) 5 Ca2 O5 2.470(11) 5 Ca2 O5 2.470(11) . Ca2 O4 2.500(12) 4 Ca2 O4 2.500(12) 2 Ca2 O3 2.522(10) 2 Ca2 O3 2.522(10) 4 S1 O1 1.460(12) 2_655 S1 O1 1.460(12) 3_665 S1 O1 1.460(12) . S1 O2 1.47(2) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag OW H O1 0.89(7) 1.81(8) 2.689(16) 170(20) . yes