#------------------------------------------------------------------------------ #$Date: 2017-12-16 07:46:09 +0200 (Sat, 16 Dec 2017) $ #$Revision: 204308 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/97/7229761.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_7229761 loop_ _publ_author_name 'Fu, Xiuwei' 'V\'illora, Encarnaci\'on G.' 'Matsushita, Yoshitaka' 'Kitanaka, Yuuki' 'Noguchi, Yuji' 'Miyayama, Masaru' 'Shimamura, Kiyoshi' 'Ohashi, Naoki' _publ_section_title ; Resistivity and piezoelectric properties of Ca3TaGa1.5Al1.5Si2O14 single crystals for high temperature sensors ; _journal_issue 89 _journal_name_full 'RSC Advances' _journal_page_first 56697 _journal_paper_doi 10.1039/C7RA11926G _journal_volume 7 _journal_year 2017 _chemical_formula_sum 'Al1.5 Ca3 Ga1.5 O14 Si2 Ta' _chemical_formula_weight 726.42 _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' _symmetry_space_group_name_Hall 'P 3 2"' _symmetry_space_group_name_H-M 'P 3 2 1' _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 8.0801(6) _cell_length_b 8.0801(6) _cell_length_c 4.9553(4) _cell_measurement_reflns_used 6511 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 46.06 _cell_measurement_theta_min 2.91 _cell_volume 280.18(4) _computing_cell_refinement 'CrystalClear (Rigaku, 1997--2002)' _computing_data_collection 'CrystalClear (Rigaku, 1997--2002)' _computing_data_reduction 'CrystalClear (Rigaku, 1997--2002)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device ; Rigaku AFC11 Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_radiation_detector CCD _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_unetI/netI 0.0358 _diffrn_reflns_Laue_measured_fraction_full 0.962 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 5938 _diffrn_reflns_point_group_measured_fraction_full 0.942 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 46.053 _diffrn_reflns_theta_min 2.911 _exptl_absorpt_coefficient_mu 15.129 _exptl_absorpt_correction_T_max 0.5055 _exptl_absorpt_correction_T_min 0.2586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrystalClear (Rigaku, 1997--2002) ; _exptl_crystal_colour Clear _exptl_crystal_density_diffrn 4.305 _exptl_crystal_description Chunk _exptl_crystal_F_000 339 _exptl_crystal_size_max 0.189 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.044 _refine_diff_density_max 4.046 _refine_diff_density_min -3.012 _refine_diff_density_rms 0.687 _refine_ls_abs_structure_details ; Flack x determined using 673 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.018(5) _refine_ls_extinction_coef 0.128(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 43 _refine_ls_number_reflns 1606 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.212 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0237 _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^)+(0.0305P)^2^+0.0430P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.0597 _reflns_Friedel_coverage 0.723 _reflns_Friedel_fraction_full 0.910 _reflns_Friedel_fraction_max 0.941 _reflns_number_gt 1605 _reflns_number_total 1606 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ra11926g1.cif _cod_data_source_block shelx _cod_original_cell_volume 280.18(5) _cod_original_formula_sum 'Al1.50 Ca3 Ga1.50 O14 Si2 Ta' _cod_database_code 7229761 _shelx_shelxl_version_number 2016/6 _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 0.162 _shelx_estimated_absorpt_t_max 0.556 _shelx_res_file ; TITL shelxt_b.res in P321 shelx.res created by SHELXL-2016/6 at 12:00:28 on 04-Dec-2017 CELL 0.71073 8.0801 8.0801 4.9553 90.000 90.000 120.000 ZERR 1.00 0.0006 0.0006 0.0004 0.000 0.000 0.000 LATT -1 SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM Y, X, - Z SYMM X - Y, - Y, - Z SYMM - X, - X + Y, - Z SFAC O AL SI CA GA TA UNIT 14 1.5 2 3 1.5 1 MERG 2 FMAP 2 PLAN 20 BOND acta size 0.075 0.189 0.044 LIST 6 exyz Ga Al eadp Ga Al omit 0 7 0 omit -4 6 2 omit -7 7 2 L.S. 100 TEMP 20.00 WGHT 0.030500 0.043000 EXTI 0.128453 FVAR 0.24415 1.00600 0.50092 0.90550 1.03999 1.00610 TA 6 1.000000 1.000000 1.000000 10.16667 0.00676 0.00676 = 0.00576 0.00000 0.00000 0.00338 AL 2 0.745080 1.000000 0.500000 10.25000 0.00724 0.00696 = 0.00660 0.00084 0.00042 0.00348 GA 5 0.745080 1.000000 0.500000 10.25000 0.00724 0.00696 = 0.00660 0.00084 0.00042 0.00348 CA 4 0.424258 1.000000 0.000000 10.50000 0.01033 0.01688 = 0.00874 0.00151 0.00076 0.00844 SI 3 0.333333 0.666667 0.453368 10.33333 0.00643 0.00643 = 0.00642 0.00000 0.00000 0.00321 O1 1 0.333333 0.666667 0.775627 10.33333 0.01372 0.01372 = 0.00729 0.00000 0.00000 0.00686 O2 1 0.526054 0.843797 0.316163 11.00000 0.00771 0.01066 = 0.01135 0.00285 -0.00069 0.00114 O3 1 0.774437 0.863202 0.762268 11.00000 0.00867 0.00912 = 0.00996 0.00017 -0.00314 0.00284 HKLF 4 REM shelxt_b.res in P321 REM R1 = 0.0237 for 1605 Fo > 4sig(Fo) and 0.0237 for all 1606 data REM 43 parameters refined using 0 restraints END WGHT 0.0305 0.0430 REM Highest difference peak 4.046, deepest hole -3.012, 1-sigma level 0.687 Q1 1 1.0000 1.0000 1.0971 10.33333 0.05 3.33 Q2 1 1.0565 1.1236 1.0001 11.00000 0.05 2.63 Q3 1 0.9425 1.0500 1.1160 11.00000 0.05 2.09 Q4 1 0.5753 1.0000 0.0000 10.50000 0.05 2.03 Q5 1 0.4980 1.0000 0.0000 10.50000 0.05 1.73 Q6 1 0.5450 1.0717 0.0005 11.00000 0.05 1.72 Q7 1 0.5333 1.0443 0.0984 11.00000 0.05 1.53 Q8 1 0.7147 1.0338 0.3845 11.00000 0.05 1.51 Q9 1 0.2222 0.6204 0.3830 11.00000 0.05 1.46 Q10 1 0.5075 1.0493 -0.1027 11.00000 0.05 1.40 Q11 1 0.7805 1.1166 0.5048 11.00000 0.05 1.40 Q12 1 0.5106 0.8595 0.2467 11.00000 0.05 1.37 Q13 1 0.4915 1.1213 -0.0069 11.00000 0.05 1.35 Q14 1 0.2418 0.6681 0.4925 11.00000 0.05 1.31 Q15 1 0.7539 0.7539 0.5000 10.50000 0.05 1.31 Q16 1 0.7409 1.0917 0.6057 11.00000 0.05 1.28 Q17 1 0.2839 0.6363 0.5939 11.00000 0.05 1.26 Q18 1 0.3333 0.6667 0.2896 10.33333 0.05 1.25 Q19 1 0.6305 0.9585 0.4869 11.00000 0.05 1.19 Q20 1 0.4979 1.1236 -0.2183 11.00000 0.05 1.14 ; _shelx_res_checksum 23800 _shelx_hkl_file ; 1 0 0 95.10 7.37 2 1 0 60.98 4.38 1 -3 0 54.74 4.51 1 -3 0 53.02 4.37 -3 3 0 383.27 22.44 -3 3 0 399.51 30.32 -3 3 0 379.14 26.83 0 -3 0 370.67 30.30 3 0 0 387.65 30.31 -3 0 0 426.37 30.31 -4 3 0 189.88 10.86 3 1 0 178.81 14.67 -4 3 0 199.72 12.99 1 -4 0 195.80 14.66 1 -4 0 181.68 15.16 -4 4 0 304.81 17.26 -4 4 0 311.58 24.10 4 0 0 296.31 23.31 -4 4 0 301.22 20.64 0 -4 0 296.16 24.10 0 4 0 275.65 23.31 -4 0 0 313.68 20.63 0 4 0 305.82 17.26 1 4 0 376.07 29.35 1 4 0 369.07 21.72 -5 1 0 381.25 25.98 5 -1 0 380.07 21.72 -4 5 0 376.59 25.99 5 -1 0 374.37 29.35 -4 5 0 393.30 21.73 2 3 0 164.30 12.19 -5 2 0 165.63 10.79 -3 5 0 150.79 10.79 5 -2 0 146.19 12.18 -3 5 0 155.73 9.02 5 -2 0 159.38 9.02 3 2 0 161.37 12.08 -5 3 0 159.93 10.70 -5 3 0 172.73 8.94 2 -5 0 144.27 12.47 5 -3 0 162.91 12.08 -2 5 0 135.83 10.69 -2 5 0 152.69 8.94 5 -4 0 179.59 13.94 -5 5 0 165.90 10.88 5 0 0 152.05 9.08 -5 5 0 150.28 9.09 5 0 0 146.70 12.28 -5 0 0 174.25 10.87 0 5 0 159.90 9.09 1 5 0 19.63 1.56 -6 1 0 20.24 1.39 1 5 0 19.31 1.15 -6 2 0 55.21 4.23 2 4 0 56.28 4.78 2 4 0 53.84 3.53 6 -2 0 69.23 3.54 6 -2 0 61.88 4.78 -4 6 0 70.91 4.25 -6 3 0 272.99 17.27 3 3 0 268.94 19.51 3 3 0 253.62 14.43 -3 6 0 235.15 14.44 -3 6 0 226.57 17.26 2 -6 0 48.46 4.21 -6 4 0 53.23 3.63 4 2 0 49.55 3.02 4 2 0 51.42 4.10 -6 4 0 56.74 3.04 6 -4 0 54.79 4.10 -6 5 0 18.73 1.07 5 1 0 18.46 1.07 5 1 0 17.53 1.45 -6 5 0 19.10 1.29 -6 5 0 17.17 1.47 6 0 0 117.59 6.78 -6 6 0 113.32 6.79 -6 6 0 112.97 8.12 6 0 0 107.56 9.16 0 6 0 131.94 6.78 -6 0 0 122.70 8.11 1 6 0 21.74 1.24 1 6 0 18.36 1.67 -7 1 0 23.27 1.49 2 5 0 220.99 17.83 2 5 0 220.18 13.19 -7 2 0 234.33 15.79 -5 7 0 239.60 15.80 7 -2 0 219.18 17.83 -5 7 0 243.27 13.21 7 -2 0 231.00 13.20 3 4 0 168.96 10.24 3 4 0 165.87 13.83 -7 3 0 178.57 12.26 -4 7 0 188.31 10.25 -4 7 0 188.68 12.26 7 -3 0 180.72 10.25 7 -3 0 176.82 13.83 -7 4 0 184.70 9.95 -7 4 0 186.81 11.90 4 3 0 156.50 13.43 4 3 0 174.53 9.93 7 -4 0 183.42 13.43 -3 7 0 156.62 11.88 -3 7 0 168.47 9.95 5 2 0 231.99 12.81 -7 5 0 225.67 15.34 5 2 0 221.54 17.32 -7 5 0 215.85 12.82 -5 -2 0 243.04 15.31 -2 7 0 220.89 12.82 7 -5 0 214.12 17.31 -2 7 0 211.68 15.31 6 1 0 21.27 1.24 6 1 0 20.91 1.68 -7 6 0 20.74 1.25 -7 6 0 21.65 1.51 7 -7 0 79.13 6.18 -8 1 0 163.63 10.88 1 7 0 155.17 9.09 -7 8 0 167.73 10.90 8 -1 0 150.87 12.29 -7 8 0 149.57 9.10 8 -1 0 161.73 9.09 -8 2 0 6.50 0.50 2 6 0 6.70 0.41 3 5 0 96.53 5.42 3 5 0 102.25 7.33 -8 3 0 103.52 6.51 -5 8 0 87.10 6.50 8 -3 0 91.39 7.33 -5 8 0 91.20 5.44 8 -3 0 87.05 5.43 4 4 0 192.26 15.71 -8 4 0 205.38 13.92 8 -4 0 213.12 15.71 8 -4 0 207.24 11.64 -4 8 0 201.69 13.91 -4 8 0 194.59 11.64 -8 5 0 99.64 6.60 -8 5 0 98.67 5.51 5 3 0 99.00 7.44 -3 8 0 85.52 6.57 -3 8 0 90.17 5.51 8 -5 0 99.83 7.43 -8 6 0 6.05 0.37 6 2 0 5.07 0.49 -8 6 0 6.11 0.46 -8 7 0 154.98 10.39 -8 7 0 152.16 8.68 7 1 0 150.24 11.72 8 -7 0 135.63 11.71 -1 8 0 160.57 8.68 -8 8 0 132.36 9.34 8 0 0 132.55 10.53 -8 0 0 141.68 9.31 0 8 0 134.42 7.79 -9 1 0 71.01 4.38 8 -9 0 60.40 4.95 1 8 0 71.79 3.67 -8 9 0 56.63 4.39 9 -1 0 58.98 4.94 -8 9 0 59.78 3.67 7 -9 0 59.43 5.32 9 -2 0 66.73 3.93 9 -2 0 71.69 5.31 -7 9 0 69.78 4.72 -7 9 0 71.75 3.94 3 6 0 91.42 6.08 9 -3 0 75.21 6.07 9 -3 0 74.01 4.50 -6 9 0 72.36 5.38 -6 9 0 75.87 4.50 -5 9 0 61.03 3.35 9 -4 0 58.20 3.34 -5 9 0 55.95 3.99 9 -4 0 54.89 4.50 5 4 0 73.58 4.86 -4 9 0 61.92 3.60 9 -5 0 59.56 4.84 9 -5 0 58.35 3.60 -4 9 0 56.59 4.28 -9 6 0 89.95 5.81 6 3 0 87.63 6.54 -3 9 0 79.85 4.85 9 -6 0 77.99 6.53 -9 7 0 78.80 4.49 7 2 0 75.36 6.06 9 -7 0 82.27 6.06 -2 9 0 73.97 4.49 8 1 0 66.44 5.21 -9 8 0 66.97 3.87 -9 8 0 68.65 4.64 9 -8 0 72.59 5.21 -1 9 0 58.30 3.85 -9 9 0 176.49 9.92 9 0 0 168.40 13.39 -9 9 0 170.52 11.87 0 9 0 173.10 9.90 -1 -9 0 35.54 3.01 10 -1 0 35.98 2.84 -9 10 0 36.72 2.54 -9 10 0 34.86 2.11 -10 2 0 69.07 4.93 -8 10 0 73.17 4.95 -8 10 0 72.56 4.13 -2 -8 0 67.95 5.73 10 -2 0 72.43 5.57 3 7 0 42.64 3.13 -7 10 0 39.70 2.33 -7 10 0 36.74 2.78 -10 4 0 13.03 0.98 4 6 0 13.49 1.08 -10 5 0 129.85 8.67 5 5 0 128.50 9.77 -5 10 0 121.68 8.65 10 -5 0 126.31 9.77 -5 10 0 124.56 7.24 10 -5 0 122.21 7.24 -10 6 0 12.61 0.91 6 4 0 11.51 0.99 -10 7 0 47.38 3.03 7 3 0 46.79 3.39 10 -7 0 40.59 3.38 -3 10 0 40.95 2.51 10 -7 0 39.39 2.52 -10 8 0 62.40 3.85 -10 8 0 63.54 4.62 8 2 0 61.44 5.19 -2 10 0 77.79 3.86 -10 9 0 23.78 1.45 -10 9 0 24.67 1.76 1 -10 0 24.62 2.10 -10 10 0 20.50 1.47 -10 10 0 19.69 1.22 -10 11 0 33.33 2.40 -10 11 0 34.22 2.01 -9 11 0 27.43 1.95 -9 11 0 26.99 1.63 -11 3 0 41.69 2.56 -3 -8 0 31.41 3.01 -8 11 0 36.23 2.13 -8 11 0 34.73 2.54 -11 4 0 150.02 9.95 4 7 0 131.07 11.20 -7 11 0 145.79 9.94 11 -4 0 141.15 11.21 11 -4 0 146.09 8.31 -7 11 0 150.08 8.32 -11 5 0 11.72 0.89 5 6 0 10.91 0.96 11 -5 0 11.48 0.97 -6 11 0 11.84 0.86 -6 11 0 12.20 0.74 11 -5 0 12.09 0.73 6 5 0 11.58 0.96 -11 6 0 10.82 0.88 -5 11 0 12.12 0.73 11 -6 0 11.90 0.73 11 -6 0 11.35 0.96 -11 7 0 144.16 10.11 11 -7 0 141.45 11.38 11 -7 0 149.86 8.45 -4 11 0 149.96 8.44 -11 8 0 43.52 2.81 -3 11 0 37.28 2.31 11 -8 0 37.64 2.33 -11 10 0 40.98 2.93 -11 10 0 41.75 2.44 -11 11 0 26.54 1.64 -11 11 0 28.04 1.97 -11 12 0 20.41 1.26 -11 12 0 20.62 1.50 -10 12 0 18.39 1.35 -10 12 0 18.49 1.14 -12 3 0 86.14 5.69 -9 12 0 79.72 5.68 -9 12 0 79.41 4.75 -12 4 0 78.98 5.86 -8 12 0 86.94 5.86 -8 12 0 87.26 4.91 -12 5 0 73.42 5.34 -7 12 0 73.93 5.31 -7 12 0 79.75 4.46 12 -5 0 79.54 4.46 -12 6 0 46.75 3.40 -6 12 0 48.10 2.83 12 -6 0 49.78 2.83 -12 7 0 73.10 5.38 -5 12 0 78.48 4.48 12 -7 0 79.69 4.49 -12 8 0 76.07 5.86 12 -8 0 88.53 4.91 -4 12 0 88.08 4.89 -12 9 0 81.98 5.72 12 -9 0 84.54 4.78 -3 12 0 79.19 4.75 -12 10 0 24.88 1.64 12 -10 0 19.73 1.36 -12 11 0 20.26 1.50 -12 12 0 120.43 8.35 -12 13 0 13.44 1.03 -11 13 0 15.03 0.97 -11 13 0 15.85 1.16 -10 13 0 8.83 0.60 -10 13 0 8.86 0.70 -9 13 0 22.82 1.38 -9 13 0 22.46 1.63 -13 5 0 34.31 2.34 -8 13 0 31.07 1.95 -7 13 0 8.46 0.56 13 -7 0 9.07 0.61 -6 13 0 9.27 0.60 -13 8 0 33.40 2.32 13 -8 0 32.67 1.93 -5 13 0 30.68 1.91 13 -9 0 22.92 1.40 -4 13 0 22.76 1.38 13 -10 0 9.28 0.63 -13 11 0 17.81 1.26 13 -11 0 15.42 1.05 -13 12 0 17.02 1.16 13 -12 0 13.29 0.97 -13 13 0 16.91 1.29 13 -13 0 17.65 1.11 13 -14 0 16.41 1.11 -13 14 0 18.05 1.29 -12 14 0 19.45 1.43 -11 14 0 16.30 1.03 -11 14 0 16.44 1.22 -10 14 0 27.94 2.07 -10 14 0 30.36 1.76 -14 5 0 24.42 1.95 -9 14 0 29.82 1.64 -8 14 0 4.68 0.36 -14 7 0 49.26 3.38 -7 14 0 45.96 2.80 14 -8 0 4.61 0.36 -6 14 0 4.80 0.36 -14 9 0 26.22 2.07 -5 14 0 28.70 1.72 14 -9 0 31.19 1.74 -14 10 0 28.52 2.17 14 -10 0 31.67 1.83 -14 11 0 18.38 1.33 14 -11 0 16.82 1.11 -14 12 0 19.24 1.44 14 -12 0 19.59 1.22 -14 13 0 15.34 1.27 14 -13 0 19.04 1.10 -14 14 0 16.82 1.28 14 -14 0 17.52 1.10 -13 15 0 10.62 0.82 -12 15 0 33.03 2.35 -11 15 0 17.26 1.08 -10 15 0 10.37 0.69 -15 6 0 19.93 1.65 -9 15 0 25.65 1.40 -15 7 0 19.27 1.32 -8 15 0 15.75 1.08 -15 8 0 19.24 1.33 -7 15 0 16.22 1.09 -15 9 0 20.42 1.63 -6 15 0 24.07 1.36 -15 10 0 8.05 0.74 15 -10 0 10.29 0.63 -15 11 0 12.62 0.98 -15 12 0 32.75 2.55 15 -12 0 39.03 2.17 -15 13 0 5.76 0.52 -11 16 0 34.23 2.05 -10 16 0 5.22 0.39 -16 7 0 19.80 1.40 -9 16 0 18.18 1.17 -16 8 0 42.54 2.84 -8 16 0 37.18 2.36 -16 9 0 21.57 1.44 -7 16 0 17.18 1.18 -16 10 0 8.74 0.72 -16 11 0 36.60 2.63 -1 0 -1 80.40 6.32 0 1 -1 78.16 6.54 1 -1 -1 83.26 6.54 0 1 -1 82.28 6.32 1 0 1 82.83 6.55 1 0 1 79.39 6.32 -1 1 1 84.36 6.54 0 -1 1 79.70 6.54 1 0 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41.68 2.50 -3 7 8 40.43 2.50 -4 -3 8 39.65 2.99 -7 5 -8 25.00 1.92 7 -5 8 29.20 1.65 -5 -2 8 26.43 1.95 -2 7 8 26.27 1.64 -6 -1 8 17.38 1.34 7 -6 8 18.65 1.13 -1 7 8 17.26 1.13 -7 7 -8 47.12 3.29 0 7 8 46.87 2.77 -7 0 8 45.32 3.30 -7 8 -8 22.24 1.49 -8 1 8 19.06 1.49 1 7 8 18.66 1.25 -7 9 -8 24.52 1.61 2 7 8 20.72 1.34 -9 2 8 20.00 1.60 1 -9 8 13.69 1.07 0 -8 8 37.35 2.64 8 0 8 35.82 2.19 -1 -7 8 16.49 1.24 8 -1 8 16.02 1.03 8 -2 8 10.43 0.70 -2 -6 8 10.11 0.83 -5 8 8 14.38 0.94 8 -3 8 15.01 0.95 -3 -5 8 14.93 1.14 8 -4 8 35.86 2.13 -4 8 8 34.95 2.13 -4 -4 8 35.48 2.55 -8 5 -8 27.00 1.69 -5 -3 8 20.65 1.69 8 -5 8 22.95 1.43 -3 8 8 21.75 1.42 -6 -2 8 9.46 0.77 -2 8 8 8.94 0.65 8 -6 8 9.85 0.65 -8 7 -8 19.85 1.49 -7 -1 8 19.58 1.51 8 -7 8 20.33 1.27 -1 8 8 21.66 1.28 -8 8 -8 40.41 2.90 -8 0 8 39.93 2.91 0 8 8 42.27 2.45 -8 9 -8 11.89 0.95 1 8 8 12.92 0.82 -9 1 8 11.94 0.96 9 -1 8 12.02 0.76 -1 -8 8 10.89 0.92 -2 -7 8 14.20 1.14 9 -2 8 15.73 0.96 -3 -6 8 9.15 0.75 9 -3 8 9.41 0.64 9 -4 8 23.46 1.46 -4 -5 8 24.06 1.74 -5 9 8 23.45 1.45 -4 9 8 20.76 1.30 9 -5 8 20.50 1.30 -5 -4 8 21.46 1.55 -3 9 8 9.76 0.68 -6 -3 8 10.02 0.81 9 -6 8 10.29 0.69 -9 7 -8 20.30 1.62 -7 -2 8 23.01 1.65 -2 9 8 22.77 1.39 9 -7 8 23.82 1.40 -9 8 -8 13.25 0.92 -1 9 8 11.39 0.77 -8 -1 8 10.93 0.91 9 -8 8 11.26 0.79 0 0 9 50.12 3.55 -1 1 9 8.80 0.72 0 -1 9 9.14 0.74 1 0 9 8.24 0.70 -1 0 9 6.90 0.62 1 -1 9 7.37 0.62 0 1 9 7.11 0.59 -2 1 9 51.46 3.71 1 -2 9 53.40 3.73 -3 2 9 17.20 1.24 1 -3 9 17.81 1.28 2 1 9 13.84 1.03 0 -2 9 57.71 3.93 -2 2 9 52.76 3.88 -1 -1 9 42.69 3.06 2 -1 9 42.42 3.03 -2 0 9 31.81 2.32 2 -2 9 31.83 2.31 1 2 9 21.87 1.48 -3 1 9 25.02 1.78 2 -3 9 25.04 1.79 -4 2 9 47.49 3.34 2 2 9 43.93 2.80 2 -4 9 49.01 3.36 3 2 9 30.87 1.91 -5 3 9 31.84 2.27 2 -5 9 31.17 2.30 1 -4 9 17.23 1.35 3 1 9 17.27 1.11 -4 3 9 17.64 1.31 0 -3 9 28.60 2.00 -3 3 9 27.14 1.94 3 0 9 24.63 1.64 3 -1 9 13.68 1.02 -1 -2 9 17.51 1.24 -2 -1 9 23.74 1.72 3 -2 9 21.96 1.67 3 -3 9 19.15 1.35 0 3 9 15.77 1.12 -3 0 9 18.41 1.37 -4 1 9 5.30 0.51 3 -4 9 5.51 0.51 1 3 9 5.11 0.42 -5 2 9 40.11 2.82 3 -5 9 40.66 2.84 2 3 9 36.91 2.36 3 3 9 29.27 1.82 3 -6 9 31.23 2.20 -6 3 9 28.85 2.16 4 3 9 7.19 0.52 3 -7 9 6.86 0.63 -7 4 9 6.80 0.60 2 -6 9 16.45 1.25 4 2 9 14.05 1.02 -6 4 9 17.36 1.22 -5 4 9 20.94 1.53 1 -5 9 20.49 1.58 4 1 9 20.77 1.30 4 0 9 2.74 0.29 0 -4 9 2.87 0.37 -1 -3 9 9.42 0.81 4 -1 9 9.66 0.66 4 -2 9 46.21 2.89 -2 -2 9 50.79 3.48 -1 4 9 0.83 0.16 4 -3 9 1.30 0.22 -3 -1 9 1.18 0.23 4 -4 9 1.81 0.26 -4 0 9 1.12 0.25 0 4 9 1.41 0.23 -5 1 9 22.66 1.68 1 4 9 20.44 1.39 4 -5 9 23.98 1.68 4 -6 9 14.94 1.14 -6 2 9 14.18 1.12 2 4 9 14.10 0.94 3 4 9 11.70 0.79 4 -7 9 12.06 0.96 -7 3 9 11.51 0.93 5 2 9 48.64 2.80 -7 5 9 43.54 3.33 2 -7 9 48.53 3.38 -6 5 9 19.07 1.45 5 1 9 20.41 1.24 1 -6 9 19.43 1.50 5 0 9 14.63 0.92 0 -5 9 13.50 1.12 -1 -4 9 20.10 1.57 5 -1 9 21.37 1.30 5 -2 9 35.82 2.20 -2 -3 9 37.23 2.66 5 -3 9 41.14 2.52 -3 -2 9 42.79 3.04 5 -3 9 42.47 3.01 -1 5 9 23.11 1.58 5 -4 9 27.97 1.89 -4 -1 9 26.29 1.91 0 5 9 19.88 1.38 -5 0 9 22.35 1.67 5 -5 9 24.70 1.66 -6 1 9 21.17 1.60 1 5 9 19.99 1.34 5 -6 9 22.99 1.61 -7 2 9 45.03 3.25 2 5 9 42.07 2.72 5 -7 9 49.47 3.27 6 0 9 22.48 1.35 0 -6 9 20.64 1.62 -1 -5 9 11.24 0.92 6 -1 9 11.09 0.75 -2 -4 9 20.21 1.53 6 -2 9 19.95 1.26 -3 -3 9 23.47 1.80 6 -3 9 24.85 1.49 6 -4 9 18.09 1.29 -4 -2 9 18.46 1.34 -2 6 9 15.51 1.09 6 -4 9 17.43 1.10 -1 6 9 13.98 1.00 6 -5 9 16.83 1.19 -5 -1 9 16.25 1.22 0 6 9 29.60 1.83 -6 0 9 30.50 2.20 7 -2 9 45.84 2.68 -2 -5 9 43.52 3.20 -3 -4 9 5.02 0.49 7 -3 9 5.02 0.39 -3 7 9 11.23 0.82 -4 -3 9 12.35 1.00 7 -4 9 14.30 0.84 -5 -2 9 45.10 2.93 -2 7 9 36.23 2.43 0 -1 10 16.25 1.25 1 -1 10 12.39 0.99 -1 0 10 12.40 0.98 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 88228 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+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 Ta Ta 1.000000 1.000000 1.000000 0.00643(7) Uani 1 6 d S T P Al Al 0.74508(8) 1.000000 0.500000 0.00696(9) Uani 0.5 2 d S T P Ga Ga 0.74508(8) 1.000000 0.500000 0.00696(9) Uani 0.5 2 d S T P Ca Ca 0.42426(11) 1.000000 0.000000 0.01125(13) Uani 1 2 d S T P Si Si 0.333333 0.666667 0.4534(2) 0.00642(14) Uani 1 3 d S T P O1 O 0.333333 0.666667 0.7756(6) 0.0116(4) Uani 1 3 d S T P O2 O 0.5261(3) 0.8438(4) 0.3162(5) 0.0114(3) Uani 1 1 d . . . O3 O 0.7744(3) 0.8632(3) 0.7623(4) 0.0100(3) Uani 1 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 Ta 0.00676(7) 0.00676(7) 0.00576(8) 0.000 0.000 0.00338(4) Al 0.00724(16) 0.0070(2) 0.0066(2) 0.00084(14) 0.00042(7) 0.00348(10) Ga 0.00724(16) 0.0070(2) 0.0066(2) 0.00084(14) 0.00042(7) 0.00348(10) Ca 0.01033(19) 0.0169(3) 0.0087(3) 0.00151(18) 0.00076(9) 0.00844(16) Si 0.0064(2) 0.0064(2) 0.0064(3) 0.000 0.000 0.00321(10) O1 0.0137(7) 0.0137(7) 0.0073(9) 0.000 0.000 0.0069(3) O2 0.0077(6) 0.0107(7) 0.0113(7) 0.0029(6) -0.0007(5) 0.0011(5) O3 0.0087(6) 0.0091(7) 0.0100(6) 0.0002(4) -0.0031(4) 0.0028(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 '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 Ta O3 168.75(12) . 6_767 O3 Ta O3 100.17(13) . 5_677 O3 Ta O3 88.20(9) 6_767 5_677 O3 Ta O3 88.20(9) . 2_765 O3 Ta O3 84.59(12) 6_767 2_765 O3 Ta O3 168.75(12) 5_677 2_765 O3 Ta O3 84.59(12) . 4_557 O3 Ta O3 88.20(9) 6_767 4_557 O3 Ta O3 88.20(9) 5_677 4_557 O3 Ta O3 100.17(13) 2_765 4_557 O3 Ta O3 88.20(9) . 3_675 O3 Ta O3 100.17(13) 6_767 3_675 O3 Ta O3 84.59(12) 5_677 3_675 O3 Ta O3 88.20(9) 2_765 3_675 O3 Ta O3 168.75(12) 4_557 3_675 O3 Ta Ca 42.29(6) . 3_566 O3 Ta Ca 129.92(6) 6_767 3_566 O3 Ta Ca 95.63(6) 5_677 3_566 O3 Ta Ca 95.63(6) 2_765 3_566 O3 Ta Ca 42.29(6) 4_557 3_566 O3 Ta Ca 129.92(6) 3_675 3_566 O3 Ta Ca 129.92(6) . 1_656 O3 Ta Ca 42.29(6) 6_767 1_656 O3 Ta Ca 129.92(6) 5_677 1_656 O3 Ta Ca 42.29(6) 2_765 1_656 O3 Ta Ca 95.63(6) 4_557 1_656 O3 Ta Ca 95.63(6) 3_675 1_656 Ca Ta Ca 120.0 3_566 1_656 O3 Ta Ca 95.63(6) . 2_776 O3 Ta Ca 95.63(6) 6_767 2_776 O3 Ta Ca 42.29(6) 5_677 2_776 O3 Ta Ca 129.92(6) 2_765 2_776 O3 Ta Ca 129.92(6) 4_557 2_776 O3 Ta Ca 42.29(6) 3_675 2_776 Ca Ta Ca 120.000(1) 3_566 2_776 Ca Ta Ca 120.0 1_656 2_776 O3 Ga O3 127.85(14) 5_676 . O3 Ga O2 103.45(10) 5_676 . O3 Ga O2 108.46(10) . . O3 Ga O2 108.46(10) 5_676 5_676 O3 Ga O2 103.45(10) . 5_676 O2 Ga O2 102.66(17) . 5_676 O3 Ga Ca 79.52(7) 5_676 . O3 Ga Ca 144.83(7) . . O2 Ga Ca 37.15(8) . . O2 Ga Ca 83.90(8) 5_676 . O3 Ga Ca 144.83(7) 5_676 1_556 O3 Ga Ca 79.52(7) . 1_556 O2 Ga Ca 83.90(8) . 1_556 O2 Ga Ca 37.15(8) 5_676 1_556 Ca Ga Ca 87.41(3) . 1_556 O3 Ca O3 68.28(10) 2_664 6_666 O3 Ca O2 134.91(8) 2_664 . O3 Ca O2 107.24(8) 6_666 . O3 Ca O2 107.24(8) 2_664 5_675 O3 Ca O2 134.91(8) 6_666 5_675 O2 Ca O2 105.46(12) . 5_675 O3 Ca O1 128.94(6) 2_664 4_566 O3 Ca O1 75.70(6) 6_666 4_566 O2 Ca O1 89.26(7) . 4_566 O2 Ca O1 74.56(8) 5_675 4_566 O3 Ca O1 75.70(6) 2_664 1_554 O3 Ca O1 128.94(6) 6_666 1_554 O2 Ca O1 74.56(8) . 1_554 O2 Ca O1 89.26(7) 5_675 1_554 O1 Ca O1 153.35(4) 4_566 1_554 O3 Ca O2 79.23(7) 2_664 2_665 O3 Ca O2 71.11(7) 6_666 2_665 O2 Ca O2 58.34(10) . 2_665 O2 Ca O2 153.96(4) 5_675 2_665 O1 Ca O2 121.65(7) 4_566 2_665 O1 Ca O2 67.51(7) 1_554 2_665 O3 Ca O2 71.11(7) 2_664 6_665 O3 Ca O2 79.23(7) 6_666 6_665 O2 Ca O2 153.96(4) . 6_665 O2 Ca O2 58.34(10) 5_675 6_665 O1 Ca O2 67.51(7) 4_566 6_665 O1 Ca O2 121.65(7) 1_554 6_665 O2 Ca O2 144.06(10) 2_665 6_665 O3 Ca Si 107.87(5) 2_664 . O3 Ca Si 90.03(5) 6_666 . O2 Ca Si 28.41(5) . . O2 Ca Si 130.90(6) 5_675 . O1 Ca Si 107.07(5) 4_566 . O1 Ca Si 67.72(6) 1_554 . O2 Ca Si 29.95(5) 2_665 . O2 Ca Si 168.83(5) 6_665 . O3 Ca Si 90.03(5) 2_664 4_565 O3 Ca Si 107.87(5) 6_666 4_565 O2 Ca Si 130.90(6) . 4_565 O2 Ca Si 28.41(5) 5_675 4_565 O1 Ca Si 67.72(6) 4_566 4_565 O1 Ca Si 107.07(5) 1_554 4_565 O2 Ca Si 168.83(5) 2_665 4_565 O2 Ca Si 29.95(5) 6_665 4_565 Si Ca Si 158.60(3) . 4_565 O3 Ca Ta 34.14(5) 2_664 1_454 O3 Ca Ta 34.14(5) 6_666 1_454 O2 Ca Ta 127.27(6) . 1_454 O2 Ca Ta 127.27(6) 5_675 1_454 O1 Ca Ta 103.324(19) 4_566 1_454 O1 Ca Ta 103.325(19) 1_554 1_454 O2 Ca Ta 72.03(5) 2_665 1_454 O2 Ca Ta 72.03(5) 6_665 1_454 Si Ca Ta 100.702(15) . 1_454 Si Ca Ta 100.701(15) 4_565 1_454 O3 Ca Al 104.79(5) 2_664 1_554 O3 Ca Al 160.28(5) 6_666 1_554 O2 Ca Al 90.76(7) . 1_554 O2 Ca Al 27.29(6) 5_675 1_554 O1 Ca Al 97.05(4) 4_566 1_554 O1 Ca Al 62.88(4) 1_554 1_554 O2 Ca Al 126.98(5) 2_665 1_554 O2 Ca Al 81.05(5) 6_665 1_554 Si Ca Al 109.68(2) . 1_554 Si Ca Al 52.756(11) 4_565 1_554 Ta Ca Al 136.295(13) 1_454 1_554 O1 Si O2 114.41(9) . 2_665 O1 Si O2 114.41(9) . . O2 Si O2 104.11(10) 2_665 . O1 Si O2 114.41(9) . 3_565 O2 Si O2 104.11(10) 2_665 3_565 O2 Si O2 104.11(10) . 3_565 O1 Si Ca 132.973(14) . . O2 Si Ca 60.18(10) 2_665 . O2 Si Ca 43.96(9) . . O2 Si Ca 111.84(9) 3_565 . O1 Si Ca 132.972(14) . 2_665 O2 Si Ca 43.96(9) 2_665 2_665 O2 Si Ca 111.84(9) . 2_665 O2 Si Ca 60.18(10) 3_565 2_665 Ca Si Ca 78.64(2) . 2_665 O1 Si Ca 132.972(14) . 3_565 O2 Si Ca 111.84(9) 2_665 3_565 O2 Si Ca 60.18(10) . 3_565 O2 Si Ca 43.96(9) 3_565 3_565 Ca Si Ca 78.64(2) . 3_565 Ca Si Ca 78.64(2) 2_665 3_565 O1 Si Ca 41.678(12) . 1_556 O2 Si Ca 96.47(9) 2_665 1_556 O2 Si Ca 84.86(9) . 1_556 O2 Si Ca 154.53(9) 3_565 1_556 Ca Si Ca 91.295(8) . 1_556 Ca Si Ca 138.797(5) 2_665 1_556 Ca Si Ca 138.797(5) 3_565 1_556 O1 Si Ca 41.678(12) . 2_666 O2 Si Ca 84.86(9) 2_665 2_666 O2 Si Ca 154.53(9) . 2_666 O2 Si Ca 96.47(9) 3_565 2_666 Ca Si Ca 138.798(5) . 2_666 Ca Si Ca 91.295(8) 2_665 2_666 Ca Si Ca 138.797(5) 3_565 2_666 Ca Si Ca 70.319(19) 1_556 2_666 O1 Si Ca 41.678(12) . 3_566 O2 Si Ca 154.53(9) 2_665 3_566 O2 Si Ca 96.47(9) . 3_566 O2 Si Ca 84.86(9) 3_565 3_566 Ca Si Ca 138.797(5) . 3_566 Ca Si Ca 138.797(5) 2_665 3_566 Ca Si Ca 91.295(8) 3_565 3_566 Ca Si Ca 70.319(19) 1_556 3_566 Ca Si Ca 70.319(19) 2_666 3_566 Si O1 Ca 114.75(6) . 1_556 Si O1 Ca 114.75(6) . 2_666 Ca O1 Ca 103.71(6) 1_556 2_666 Si O1 Ca 114.75(6) . 3_566 Ca O1 Ca 103.71(6) 1_556 3_566 Ca O1 Ca 103.71(6) 2_666 3_566 Si O2 Ga 124.40(14) . . Si O2 Ca 107.64(12) . . Ga O2 Ca 115.56(12) . . Si O2 Ca 89.87(11) . 3_565 Ga O2 Ca 110.06(11) . 3_565 Ca O2 Ca 104.80(8) . 3_565 Ga O3 Ta 117.06(10) . . Ga O3 Ca 136.74(11) . 3_566 Ta O3 Ca 103.57(8) . 3_566 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ta O3 1.979(2) . Ta O3 1.979(2) 6_767 Ta O3 1.979(2) 5_677 Ta O3 1.979(2) 2_765 Ta O3 1.979(2) 4_557 Ta O3 1.979(2) 3_675 Ta Ca 3.4280(9) 3_566 Ta Ca 3.4280(9) 1_656 Ta Ca 3.4280(9) 2_776 Ga O3 1.797(2) 5_676 Ga O3 1.797(2) . Ga O2 1.822(2) . Ga O2 1.822(2) 5_676 Ga Ca 3.5859(8) . Ga Ca 3.5859(8) 1_556 Ca O3 2.373(2) 2_664 Ca O3 2.373(2) 6_666 Ca O2 2.400(3) . Ca O2 2.400(3) 5_675 Ca O1 2.6555(12) 4_566 Ca O1 2.6555(12) 1_554 Ca O2 2.859(3) 2_665 Ca O2 2.859(3) 6_665 Ca Si 3.2958(8) . Ca Si 3.2958(8) 4_565 Si O1 1.597(3) . Si O2 1.645(2) 2_665 Si O2 1.645(2) . Si O2 1.645(2) 3_565