#------------------------------------------------------------------------------ #$Date: 2021-09-07 15:04:19 +0100 (Tue, 07 Sep 2021) $ #$Revision: 269031 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/03/3000313.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_3000313 loop_ _publ_author_name 'M\"unchhalfen, Marie' 'Schreuer, J\"urgen' 'Reuther, Christoph' 'Mehner, Erik' 'St\"ocker, Hartmut' _publ_section_title ; Elastic, piezoelectric, and dielectric properties of rare-earth calcium oxoborates RCa4O(BO3)3 (R = Er, Y, Dy, Gd, Sm, Nd, La) ; _journal_issue 9 _journal_name_full 'Journal of Applied Physics' _journal_page_first 095102 _journal_paper_doi 10.1063/5.0061747 _journal_volume 130 _journal_year 2021 _chemical_formula_moiety 'Y Ca4 O (B O3 )3' _chemical_formula_sum 'B3 Ca4 O10 Y' _chemical_formula_weight 441.66 _chemical_name_common 'yttrium calcium oxoborate' _space_group_crystal_system monoclinic _space_group_IT_number 8 _space_group_name_Hall 'C -2y' _space_group_name_H-M_alt 'C 1 m 1' _atom_sites_solution_hydrogens . _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 101.166(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.0737(2) _cell_length_b 16.0088(5) _cell_length_c 3.52827(11) _cell_measurement_reflns_used 3695 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 42.1860 _cell_measurement_theta_min 3.6570 _cell_volume 447.40(2) _computing_cell_refinement 'CrysAlisPro 1.171.36.24 (Rigaku OD, 2012)' _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlisPro 1.171.36.24 (Rigaku OD, 2012)' _computing_molecular_graphics 'VESTA 3 ( Momma & Izumi, 2011 )' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.867 _diffrn_measurement_device_type 'Xcalibur with Sapphire2 CCD-area detector' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0397 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.867 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 4266 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.756 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 42.522 _diffrn_reflns_theta_min 4.606 _exptl_absorpt_coefficient_mu 8.853 _exptl_absorpt_correction_T_max 0.352 _exptl_absorpt_correction_T_min 0.129 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.278 _exptl_crystal_density_meas 3.271(3) _exptl_crystal_density_method buoyancy _exptl_crystal_F_000 428 _exptl_crystal_size_max 0.3602 _exptl_crystal_size_mid 0.3346 _exptl_crystal_size_min 0.1610 _refine_diff_density_max 0.962 _refine_diff_density_min -1.601 _refine_diff_density_rms 0.172 _refine_ls_abs_structure_details ; Flack x determined using 985 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.035(4) _refine_ls_extinction_coef 0.131(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 2500 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0277 _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^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0661 _reflns_Friedel_coverage 0.737 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.645 _reflns_number_gt 2444 _reflns_number_total 2500 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file YCOB.cif _cod_data_source_block YCOB _cod_depositor_comments 'Releasing structure 3000313 into public domain as published material.' _cod_original_sg_symbol_H-M 'C m' _cod_database_code 3000313 _shelx_shelxl_version_number 2014/7 _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_res_file ; YCOB30-01-kT.res created by SHELXL-2014/7 TITL YCOB30-01-kT in Cm REM Cm (#8 in standard setting) CELL 0.71073 8.073681 16.008822 3.528266 90.0000 101.1658 90.0000 ZERR 2.00 0.000202 0.000519 0.000105 0.0000 0.0027 0.0000 LATT -7 SYMM x,-y, z SFAC B O Ca Y UNIT 6.00 20.00 8.00 2.00 L.S. 10 BOND FMAP 2 PLAN 20 sump 0.5 0.001 0.5 2 1.0 3 exyz Y-X Ca-X exyz Ca-Y Y-Y eadp Y-X Ca-X eadp Ca-Y Y-Y acta WGHT 0.035500 EXTI 0.130716 FVAR 8.02882 0.83220 0.08309 Y-X 4 0.000394 0.000000 0.001896 20.50000 0.00616 0.00968 = 0.00689 0.00000 0.00141 0.00000 CA-Y 3 -0.359787 -0.112307 0.327190 -31.00000 0.00713 0.00840 = 0.00834 0.00009 0.00101 -0.00018 CA-Z 3 0.256830 0.181038 -0.350749 11.00000 0.00933 0.01570 = 0.00920 -0.00087 0.00232 -0.00077 CA-X 3 0.000394 0.000000 0.001896 -20.50000 0.00616 0.00968 = 0.00689 0.00000 0.00141 0.00000 Y-Y 4 -0.359787 -0.112307 0.327190 31.00000 0.00713 0.00840 = 0.00834 0.00009 0.00101 -0.00018 O1 2 -0.173708 0.000000 0.420299 10.50000 0.00796 0.01091 = 0.01016 0.00000 0.00054 0.00000 O2 2 0.198240 0.000000 -0.396771 10.50000 0.00451 0.02725 = 0.01334 0.00000 0.00145 0.00000 O3 2 0.079677 0.141721 0.072907 11.00000 0.00951 0.01156 = 0.01124 0.00034 0.00210 0.00261 O4 2 -0.533317 -0.230652 0.273743 11.00000 0.01531 0.01267 = 0.01493 -0.00543 0.00534 -0.00396 O5 2 -0.213780 -0.174080 -0.118625 11.00000 0.00858 0.01668 = 0.01141 0.00022 0.00020 0.00349 O6 2 0.458810 0.074440 -0.251845 11.00000 0.01220 0.01017 = 0.01356 -0.00004 0.00121 -0.00320 B1 1 0.372070 0.000000 -0.300348 10.50000 0.00589 0.00834 = 0.00645 0.00000 0.00035 0.00000 B2 1 -0.555146 -0.305459 0.076761 11.00000 0.00810 0.00923 = 0.00961 0.00086 0.00157 -0.00187 HKLF 4 REM YCOB30-01-kT in Cm REM R1 = 0.0277 for 2444 Fo > 4sig(Fo) and 0.0285 for all 2500 data REM 91 parameters refined using 3 restraints END WGHT 0.0355 0.0000 REM Highest difference peak 0.962, deepest hole -1.601, 1-sigma level 0.172 Q1 1 -0.0807 -0.0111 0.0266 11.00000 0.05 0.96 Q2 1 0.0767 0.0205 -0.0254 11.00000 0.05 0.95 Q3 1 0.1240 0.0000 0.0770 10.50000 0.05 0.85 Q4 1 -0.0387 -0.0330 -0.0486 11.00000 0.05 0.84 Q5 1 -0.2811 -0.0964 0.3178 11.00000 0.05 0.77 Q6 1 -0.4773 -0.1112 0.2520 11.00000 0.05 0.72 Q7 1 -0.4358 -0.0931 0.3473 11.00000 0.05 0.72 Q8 1 0.0466 0.0369 0.0698 11.00000 0.05 0.65 Q9 1 -0.1662 0.0000 0.7725 10.50000 0.05 0.63 Q10 1 0.3456 0.1611 -0.3629 11.00000 0.05 0.62 Q11 1 0.2616 0.0000 -0.3482 10.50000 0.05 0.61 Q12 1 0.2921 0.1480 -0.3030 11.00000 0.05 0.61 Q13 1 -0.4379 -0.1296 0.3319 11.00000 0.05 0.61 Q14 1 -0.1418 0.0000 -0.1359 10.50000 0.05 0.60 Q15 1 0.3415 0.1923 -0.3775 11.00000 0.05 0.58 Q16 1 0.1852 0.1611 -0.3181 11.00000 0.05 0.56 Q17 1 -0.4424 -0.2256 0.2702 11.00000 0.05 0.56 Q18 1 -0.2923 -0.1379 0.3102 11.00000 0.05 0.55 Q19 1 -0.0286 0.0972 0.2228 11.00000 0.05 0.54 Q20 1 0.3350 0.1165 -0.2468 11.00000 0.05 0.54 ; _shelx_res_checksum 43599 _shelx_hkl_file ; -14 0 0 30264.0 2699.93 3 -14 0 1 34368.8 2771.86 3 -14 0 2 43851.3 3170.82 3 -14 2 1 2890.89 983.578 3 -14 -2 1 3696.41 999.440 3 -14 2 2 24986.0 2487.10 3 -14 -2 2 21418.6 2213.90 3 -14 -4 1 32902.7 2546.85 3 -14 4 1 35444.3 3038.82 3 -13 1 -1 16716.8 2018.53 3 -13 1 0 17899.0 2114.39 3 -13 -1 0 18595.0 2048.93 3 -13 -1 1 62843.3 3788.55 3 -13 1 1 68534.6 4043.87 3 -13 -1 2 17231.6 1955.87 3 -13 1 2 17486.9 2085.34 3 -13 1 3 123.705 500.566 3 -13 -1 3-756.036 824.221 3 -13 3 -1 235.681 376.080 3 -13 -3 0 110065. 4818.28 3 -13 3 0 120990. 5709.06 3 -13 -3 1 15175.1 1801.76 3 -13 3 1 16517.6 2094.09 3 -13 3 2 1871.71 858.869 3 -13 -3 2 734.400 451.064 3 -13 3 3 72127.8 4455.21 3 -13 -3 3 61612.1 3863.71 3 -13 5 -1 89963.1 4922.80 3 -13 5 0 13197.9 1914.07 3 -13 -5 1 7712.34 1275.16 3 -13 5 1 8794.84 1620.09 3 -13 -5 2 79372.2 4132.69 3 -13 5 2 95138.6 5275.11 3 -13 -5 3 9826.06 1572.39 3 -13 5 3 15652.7 2246.95 3 -13 7 0 9684.99 1710.43 3 -13 7 1 34682.1 3167.47 3 -13 -7 2 18782.8 1974.48 3 -13 7 2 26169.2 2944.78 3 -13 7 3 12828.1 2027.17 3 -13 -7 3 8231.27 1389.67 3 -13 9 0 9531.18 1734.21 3 -13 9 1 103298. 5704.09 3 -13 9 2 26863.4 2983.04 3 -13 11 1 5654.23 1468.76 3 -12 0 -1 90206.1 4615.05 3 -12 0 0 22092.2 2245.93 3 -12 0 1 28925.8 2528.83 3 -12 0 2 187700. 6821.15 3 -12 0 3 37572.4 3059.96 3 -12 2 -2 41948.0 3326.40 3 -12 2 -1 38692.4 3083.69 3 -12 -2 -1 41157.1 2995.62 3 -12 -2 0 15589.3 1856.83 3 -12 2 0 11871.1 1716.65 3 -12 2 1 75367.0 4341.28 3 -12 -2 1 66757.0 3736.62 3 -12 2 2 38164.1 3114.71 3 -12 -2 2 33752.3 2761.63 3 -12 2 3 5298.05 1184.46 3 -12 4 -2 64167.6 4235.82 3 -12 4 -1 1694.83 721.608 3 -12 -4 0 28452.9 2333.82 3 -12 4 0 34574.3 3000.91 3 -12 4 1 72971.9 4416.16 3 -12 -4 1 54857.2 3260.60 3 -12 4 2 4141.61 1124.05 3 -12 -4 2 1781.47 604.579 3 -12 4 3 25975.4 2711.13 3 -12 4 4 55440.0 4117.17 3 -12 6 -2 3669.55 1058.57 3 -12 6 -1 8349.87 1533.27 3 -12 6 0 93813.3 5167.69 3 -12 -6 1 6518.94 1136.16 3 -12 6 1 9855.09 1653.71 3 -12 -6 2 28190.9 2374.96 3 -12 6 2 38183.1 3356.41 3 -12 6 3 51470.5 4054.45 3 -12 6 4 19841.3 2503.28 3 -12 8 -1 98832.3 5362.46 3 -12 8 0 60066.1 4404.41 3 -12 8 1 36533.9 3321.39 3 -12 8 2 93279.1 5461.97 3 -12 -8 2 65616.4 3617.81 3 -12 8 3 96485.8 5879.46 3 -12 10 -1 25615.2 2741.39 3 -12 10 0 8886.30 1682.14 3 -12 10 1 10167.5 1826.31 3 -12 10 2 68001.8 4800.69 3 -12 10 3 12542.7 2133.32 3 -12 12 0 21261.1 2654.28 3 -12 12 1 25436.7 2979.67 3 -12 12 2 15027.9 2300.38 3 -12 12 3 27644.3 3247.64 3 -12 14 0 6381.01 1419.75 3 -12 14 1 162964. 7792.91 3 -12 14 2 6684.38 1559.03 3 -11 1 -2 15533.8 1998.74 3 -11 -1 -1 168.547 345.704 3 -11 1 -1-42.2561 496.197 3 -11 -1 0 145496. 5607.69 3 -11 1 0 157191. 5977.50 3 -11 1 1 32260.2 2743.11 3 -11 -1 1 31699.3 2524.35 3 -11 1 2-27.7195 453.452 3 -11 -1 2 717.437 459.469 3 -11 3 -2 8039.26 1466.44 3 -11 3 -1 153132. 6271.64 3 -11 -3 -1 158176. 5815.15 3 -11 -3 0 28182.8 2367.19 3 -11 3 0 28421.6 2587.84 3 -11 3 1 5565.84 1223.96 3 -11 -3 1 4270.24 997.571 3 -11 -3 2 114927. 4984.69 3 -11 3 2 136805. 6085.79 3 -11 3 3 1523.68 676.998 3 -11 5 -2 67214.5 4314.29 3 -11 5 -1 16662.5 2035.17 3 -11 5 0 17447.2 2133.94 3 -11 -5 0 17506.2 1784.64 3 -11 -5 1 80486.8 3856.92 3 -11 5 1 89409.1 4845.76 3 -11 5 2 65729.3 4374.90 3 -11 5 3 23790.5 2710.11 3 -11 7 -2 24507.3 2695.12 3 -11 7 -1 25992.5 2598.32 3 -11 7 0 49595.9 3681.68 3 -11 -7 1 38160.9 2580.59 3 -11 7 1 48296.6 3617.25 3 -11 7 2 46366.1 3734.28 3 -11 7 3 29347.1 3218.89 3 -11 7 4 11697.9 2023.75 3 -11 9 -2 44881.3 3751.67 3 -11 9 -1 15973.1 2089.24 3 -11 9 0 117056. 5970.45 3 -11 9 1 96418.8 5276.99 3 -11 9 2 25201.9 2885.22 3 -11 9 3 50740.9 4263.02 3 -11 9 4 80571.0 5555.72 3 -11 11 -2 15685.3 2113.25 3 -11 11 -1 3250.26 1082.09 3 -11 11 0 44497.6 3737.05 3 -11 11 1 22948.4 2645.62 3 -11 11 2 2364.14 1102.87 3 -11 11 3 103826. 6134.04 3 -11 11 4 31651.6 3485.17 3 -11 13 -1 105463. 5613.11 3 -11 13 0 3756.58 1096.25 3 -11 13 1 17379.1 2368.68 3 -11 13 2 102829. 5813.14 3 -11 13 3 10190.7 1964.69 3 -11 15 -1 48722.1 3963.55 3 -11 15 0 7136.40 1518.39 3 -11 15 1 5401.14 1393.48 3 -11 15 2 31009.7 3212.27 3 -11 17 0 61452.7 4391.78 3 -11 17 1 16942.7 2441.82 3 -10 0 -2 188169. 6663.82 3 -10 0 -1 36808.5 2770.89 3 -10 0 0 37105.1 2707.64 3 -10 0 0 33253.0 2519.51 1 -10 0 1 259097. 7292.85 1 -10 0 1 288945. 8130.59 3 -10 2 -3 43964.0 3418.19 3 -10 2 -2 40089.0 3101.89 3 -10 -2 -1 21619.6 2091.34 3 -10 2 -1 19988.2 2121.28 3 -10 -2 0 80067.7 3898.03 3 -10 2 0 84063.6 4220.45 3 -10 -2 0 79308.2 3658.30 1 -10 -2 1 25538.6 2170.96 1 -10 2 1 26287.4 2388.76 3 -10 -2 1 25250.2 2227.47 3 -10 2 2 71965.4 4183.00 3 -10 4 -3 53028.9 3849.64 3 -10 4 -2 2716.62 1110.67 3 -10 4 -1 34557.3 2842.34 3 -10 -4 -1 37248.3 2613.15 3 -10 -4 0 125280. 4836.38 3 -10 4 0 123587. 5333.34 3 -10 -4 1 5140.99 955.911 3 -10 4 1 3923.44 1073.83 3 -10 -4 1 3610.66 781.321 1 -10 4 2 67732.7 4315.17 3 -10 6 -3 11578.5 1832.13 3 -10 6 -2 40012.2 3283.04 3 -10 6 -1 32726.7 2826.64 3 -10 6 0 61991.0 3810.04 3 -10 -6 0 62594.9 3250.12 3 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-10 -14 4 31907.7 2652.23 2 -10 16 -1 2525.63 989.453 3 -10 16 0 2014.05 991.570 3 -10 16 1 77473.1 4897.38 3 -10 16 2 8284.84 1550.11 3 -10 18 -1 38296.2 3474.92 3 -10 18 0 6618.47 1571.66 3 -10 18 1 86431.8 5041.56 3 -9 1 -3 22294.0 2308.24 3 -9 1 -2 2338.02 680.271 3 -9 -1 -2 2857.24 713.552 3 -9 -1 -1 195305. 6367.06 3 -9 -1 -1 181399. 5631.04 1 -9 1 -1 194847. 6550.63 3 -9 -1 0 49880.1 2975.40 3 -9 1 0 45425.5 2921.03 1 -9 -1 0 46760.4 2848.99 1 -9 1 0 46494.2 2971.35 3 -9 -1 1 1352.81 554.950 3 -9 1 1-82.6880 253.872 1 -9 1 1 924.720 613.809 3 -9 -1 1 734.531 515.350 1 -9 -1 2 92682.9 4318.51 1 -9 1 2 97982.3 4555.20 1 -9 3 -3 5821.04 1214.82 3 -9 3 -2 107595. 4957.83 3 -9 3 -1 5914.42 1210.19 3 -9 -3 -1 7028.22 1131.39 3 -9 3 -1 6958.54 1151.88 1 -9 3 0 56985.6 3397.47 1 -9 3 0 57968.1 3405.05 3 -9 -3 0 56286.7 3048.36 3 -9 -3 0 54188.9 2894.37 1 -9 3 1 195061. 6556.15 1 -9 -3 1 208020. 6166.37 1 -9 -3 1 195513. 6067.31 3 -9 3 1 204277. 6795.13 3 -9 3 2 36754.7 2838.72 1 -9 -3 2 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10 -5 21503.7 2581.84 4 10 10 -4 85726.6 5123.06 4 10 10 -3 11713.8 1751.18 4 10 10 -2 14833.1 1895.50 4 10 10 -1 107554. 4839.02 4 10 10 0 23939.9 2317.95 4 10 10 1 3736.42 1053.95 4 10 10 2 62900.9 4173.23 4 10 10 3 5744.01 1437.79 4 10 12 -5 21049.5 2592.90 4 10 12 -4 4890.92 1229.43 4 10 12 -3 28351.8 2782.03 4 10 12 -2 67397.7 4011.24 4 10 12 -1 35357.3 2791.99 4 10 12 0 42996.5 3085.61 4 10 12 1 50967.1 3537.61 4 10 12 2 9559.64 1596.72 4 10 12 3 8231.74 1681.17 4 10 14 -4 22420.2 2540.66 4 10 14 -3 73680.7 4412.37 4 10 14 -2 10675.0 1541.78 4 10 14 -1 11534.7 1604.43 4 10 14 0 115382. 5167.51 4 10 14 1 15311.1 1966.36 4 10 14 2 14155.5 2028.00 4 10 14 3 92466.2 5108.81 4 10 16 -4 32806.2 2975.93 4 10 16 -3 568.755 426.269 4 10 16 -2 20121.2 2086.70 4 10 16 -1 59146.7 3587.14 4 10 16 0-24.5775 449.958 4 10 16 1 9528.50 1501.38 4 10 16 2 33136.9 2993.00 4 10 18 -2 22635.8 2197.51 4 10 18 -1 87068.0 4305.07 4 10 18 0 14828.4 1856.31 4 10 18 1 22882.7 2357.19 4 10 18 2 55836.7 3796.96 4 10 20 0 39923.9 2892.69 4 10 20 1 4405.68 1006.85 4 11 -1 -5 7240.37 1638.57 4 11 1 -5 5999.88 1617.43 4 11 -1 -4 20441.9 2521.43 4 11 1 -4 18008.7 2411.40 4 11 -1 -3 105214. 5418.11 4 11 1 -3 101936. 5451.14 4 11 -1 -2 4693.63 1149.89 4 11 1 -2 5965.85 1276.75 4 11 1 -1 17239.3 1937.01 4 11 -1 -1 18832.7 1934.79 4 11 1 0 155806. 5993.97 4 11 -1 0 156809. 5932.78 4 11 1 1 5763.41 1249.32 4 11 -1 1 5323.74 1151.91 4 11 1 2 9548.41 1761.84 4 11 -1 2 9296.99 1580.23 4 11 1 3 48645.1 3796.62 4 11 -1 3 46257.2 3664.40 4 11 -3 -5 73825.9 4837.02 4 11 3 -5 74811.6 5021.67 4 11 -3 -4 8421.63 1626.58 4 11 3 -4 7645.88 1760.73 4 11 -3 -3 9617.15 1732.94 4 11 3 -3 9758.85 1640.62 4 11 -3 -2 131773. 5823.39 4 11 3 -2 124522. 5770.56 4 11 3 -1 4340.09 1046.41 4 11 -3 -1 4929.58 1031.05 4 11 3 0 49215.5 3352.91 4 11 -3 0 51724.6 3374.58 4 11 3 1 145627. 6141.05 4 11 -3 1 135703. 5746.70 4 11 3 2 4672.53 1008.81 4 11 -3 2 4277.67 1065.37 4 11 3 3 14080.7 2179.91 4 11 -5 -5 35934.7 3318.45 4 11 5 -5 33209.0 3408.21 4 11 -5 -4 112635. 5638.72 4 11 5 -4 115563. 6224.63 4 11 -5 -3 20384.0 2319.23 4 11 5 -3 20518.1 2466.01 4 11 -5 -2 41853.8 3241.51 4 11 5 -2 43043.0 3327.72 4 11 5 -1 107267. 4932.87 4 11 -5 -1 120757. 5118.35 4 11 5 0 6581.65 1244.60 4 11 -5 0 7285.43 1274.96 4 11 5 1 7430.01 1482.53 4 11 5 2 97404.1 5215.37 4 11 5 3 4563.43 1217.91 4 11 -7 -5 8283.38 1619.10 4 11 7 -5 5984.34 1535.73 4 11 -7 -4 3308.58 1170.39 4 11 7 -4 2048.40 1014.83 4 11 -7 -3 22579.1 2443.49 4 11 7 -3 19987.4 2423.13 4 11 7 -2 36182.0 3054.98 4 11 7 -1 18517.0 2009.60 4 11 7 0 44462.5 3163.90 4 11 7 1 26681.5 2584.97 4 11 7 2 24954.4 2658.67 4 11 7 3 30910.7 3077.34 4 11 9 -5 10256.8 1892.77 4 11 9 -4 41022.6 3645.72 4 11 9 -3 61319.1 4254.34 4 11 9 -2 38430.8 3129.01 4 11 9 -1 54556.8 3511.67 4 11 9 0 147606. 5937.80 4 11 9 1 29700.2 2796.34 4 11 9 2 34677.3 3136.76 4 11 9 3 61704.0 4277.46 4 11 11 -4 39304.1 3551.87 4 11 11 -3 79978.9 4837.20 4 11 11 -2 5080.66 1095.79 4 11 11 -1 46115.4 3293.66 4 11 11 0 36292.2 2935.96 4 11 11 1 5182.35 1208.45 4 11 11 2 30740.3 2967.79 4 11 13 -4 15938.0 2204.64 4 11 13 -3 4034.03 1254.66 4 11 13 -2 71679.9 4139.50 4 11 13 -1 18606.7 2062.25 4 11 13 0 10917.1 1610.54 4 11 13 1 98874.3 5028.66 4 11 13 2 17011.4 2194.31 4 11 15 -4 6043.28 1198.75 4 11 15 -3 1592.06 413.154 4 11 15 -2 24978.0 2411.40 4 11 15 -1 15503.3 1847.71 4 11 15 0 13048.5 1716.16 4 11 15 1 42648.6 3260.42 4 11 15 2 14201.5 1955.81 4 11 17 -3 68980.1 4021.70 4 11 17 -2 8330.98 1439.31 4 11 17 -1 10781.9 1620.52 4 11 17 0 64925.1 3916.24 4 11 17 1 25058.5 2481.67 4 11 19 -2 35124.3 2751.18 4 11 19 -1 16334.8 1932.10 4 11 19 0 40832.3 2990.79 4 11 19 1 18181.7 2066.99 4 12 0 -5 81801.3 5340.85 4 12 0 -4 22436.7 2774.73 4 12 0 -3 35206.6 3231.42 4 12 0 -2 169830. 6773.71 4 12 0 -1 48078.5 3308.73 4 12 0 0 17272.5 2077.77 4 12 0 1 92519.4 4831.81 4 12 0 2 68020.5 4357.25 4 12 0 3 17669.1 2247.02 4 12 -2 -5 9450.48 1872.71 4 12 2 -5 9542.35 1998.38 4 12 -2 -4 32421.3 3263.54 4 12 2 -4 34535.5 3474.97 4 12 -2 -3 174.759 517.476 4 12 2 -3 197.735 529.810 4 12 -2 -2 53742.1 3702.02 4 12 2 -2 52824.1 3756.73 4 12 2 -1 51614.5 3481.74 4 12 -2 -1 58852.6 3669.20 4 12 2 0 4763.16 1218.50 4 12 -2 0 6706.30 1304.12 4 12 2 1 56700.6 3795.36 4 12 -2 1 57870.3 3864.36 4 12 2 2 27365.0 2774.04 4 12 2 3 2642.06 1052.10 4 12 -4 -5 2201.74 1013.01 4 12 4 -5 2068.92 916.398 4 12 -4 -4 51958.3 4064.37 4 12 4 -4 53826.1 4381.79 4 12 -4 -3 37269.1 3253.44 4 12 4 -3 35418.8 3258.61 4 12 -4 -2 13176.7 1861.15 4 12 4 -2 10167.2 1628.59 4 12 4 -1 54774.6 3612.41 4 12 -4 -1 58276.0 3686.92 4 12 4 0 47678.0 3418.79 4 12 -4 0 55040.4 3586.99 4 12 4 1 2337.94 960.617 4 12 4 2 40495.9 3437.65 4 12 4 3 25715.4 2767.59 4 12 -6 -4 13914.4 2017.65 4 12 6 -4 12725.9 2110.27 4 12 -6 -3 51755.6 3781.86 4 12 6 -3 47984.3 3864.29 4 12 6 -2 15109.1 1958.97 4 12 6 -1 2410.11 751.563 4 12 6 0 110372. 5198.83 4 12 6 1 4413.00 1210.03 4 12 6 2 3906.54 1104.46 4 12 8 -4 19172.2 2636.84 4 12 8 -3 45002.8 3730.70 4 12 8 -2 93591.4 5020.46 4 12 8 -1 33921.1 2877.24 4 12 8 0 32315.5 2840.42 4 12 8 1 111420. 5422.70 4 12 8 2 15641.1 2178.76 4 12 10 -4 14335.5 2256.07 4 12 10 -3 9000.25 1655.94 4 12 10 -2 63396.7 4041.31 4 12 10 -1 21851.3 2304.51 4 12 10 0 8908.59 1510.99 4 12 10 1 31518.6 2812.38 4 12 10 2 7547.73 1501.46 4 12 12 -4 9264.65 1773.41 4 12 12 -3 31321.4 3015.56 4 12 12 -2 7494.52 1384.81 4 12 12 -1 9715.66 1599.47 4 12 12 0 36443.7 3017.03 4 12 12 1 3739.98 1009.18 4 12 12 2 11227.8 1715.79 4 12 14 -3 3144.87 854.067 4 12 14 -2 15384.7 1983.42 4 12 14 -1 114547. 5248.00 4 12 14 0 13498.6 1762.09 4 12 14 1 17581.3 2129.94 4 12 16 -3 15655.0 1940.43 4 12 16 -2 27438.1 2573.60 4 12 16 -1 7203.23 1399.27 4 12 16 0 21810.6 2311.74 4 12 16 1 11339.2 1681.71 4 12 18 -2 44690.6 3137.46 4 12 18 -1 11504.9 1656.50 4 12 18 0 7254.48 1374.42 4 13 -1 -4 55175.3 4339.03 4 13 1 -4 62507.2 4679.59 4 13 -1 -3 6379.83 1448.95 4 13 1 -3 6503.06 1376.58 4 13 -1 -2 8996.01 1524.66 4 13 1 -2 6906.21 1250.29 4 13 1 -1 66217.7 4048.80 4 13 -1 -1 73134.6 4221.34 4 13 1 0 34528.3 2929.52 4 13 -1 0 33535.7 2916.12 4 13 -1 1 16100.3 2087.87 4 13 1 1 14668.7 1961.89 4 13 1 2 23750.0 2538.02 4 13 -3 -4 38790.7 3618.87 4 13 3 -4 40461.6 3832.93 4 13 -3 -3 56655.8 4091.87 4 13 3 -3 56643.0 4227.11 4 13 -3 -2 5164.73 1102.19 4 13 3 -2 3318.73 888.359 4 13 3 -1 27724.6 2641.88 4 13 -3 -1 29910.7 2714.23 4 13 3 0 80526.9 4488.91 4 13 -3 0 87425.5 4670.65 4 13 3 1 5947.12 1274.42 4 13 3 2 10148.5 1729.17 4 13 -5 -4 4847.42 1384.82 4 13 5 -4 3271.02 1039.97 4 13 -5 -3 10279.0 1706.39 4 13 5 -3 9278.51 1791.88 4 13 5 -2 103728. 5295.43 4 13 5 -1 4133.06 1152.75 4 13 5 0 12078.1 1820.22 4 13 5 1 118721. 5591.44 4 13 5 2 7296.41 1451.71 4 13 7 -4 12042.7 2081.08 4 13 7 -3 5994.72 1441.98 4 13 7 -2 14524.4 1872.56 4 13 7 -1 36512.8 3056.68 4 13 7 0 6126.51 1185.96 4 13 7 1 18611.6 2201.47 4 13 7 2 32855.5 2983.43 4 13 9 -4 71480.5 4937.67 4 13 9 -3 17435.7 2280.29 4 13 9 -2 10965.9 1710.67 4 13 9 -1 95302.7 4889.71 4 13 9 0 5871.25 1185.71 4 13 9 1 5104.92 1247.31 4 13 11 -3 3889.44 915.458 4 13 11 -2 38091.7 3126.44 4 13 11 -1 5321.20 1258.55 4 13 11 0 15853.3 2065.12 4 13 11 1 33196.1 2951.51 4 13 13 -3 40756.6 3274.54 4 13 13 -2 11724.0 1790.98 4 13 13 -1 7650.22 1468.78 4 13 13 0 68279.0 4130.97 4 13 15 -2 19560.4 2203.95 4 13 15 -1 17258.2 2169.93 4 13 15 0 19355.3 2140.70 4 14 0 -3 42677.4 3591.29 4 14 0 -2 66684.1 4124.07 4 14 0 -1 39829.6 3140.59 4 14 0 0 25861.1 2594.23 4 14 0 1 93150.0 4875.57 4 14 -2 -3 48937.0 3739.31 4 14 2 -3 44813.8 3674.56 4 14 2 -2 10637.1 1617.34 4 14 -2 -2 10328.5 1614.69 4 14 2 -1 256.092 693.803 4 14 -2 -1 637.840 610.087 4 14 2 0 25814.5 2554.84 4 14 2 1 7127.97 1316.85 4 14 4 -3 1262.73 601.642 4 14 4 -2 34351.5 2997.04 4 14 4 -1 55304.3 3730.95 4 14 4 0 4198.36 1213.05 4 14 4 1 27265.0 2640.02 4 14 6 -3 563.181 677.152 4 14 6 -2 12339.8 1854.75 4 14 6 -1 91368.6 4853.00 4 14 6 0 1876.22 968.627 4 14 6 1 17617.5 2127.84 4 14 8 -3 65563.7 4400.11 4 14 8 -2 2938.32 964.607 4 14 8 -1 3324.40 1073.12 4 14 8 0 64494.5 4094.25 4 14 10 -2 15042.3 1961.92 4 14 10 -1 5742.68 1346.91 4 14 10 0 17026.0 2051.41 4 14 12 -1 34808.4 2951.55 4 15 1 -2 20708.4 2291.81 4 15 -1 -2 22316.0 2385.03 4 15 1 -1 50914.8 3579.10 4 15 -1 -1 54206.4 3658.42 4 15 1 0 8217.74 1423.68 4 15 3 -2 5577.57 1290.48 4 15 3 -1 15185.7 2024.96 4 15 5 -2 3954.49 1054.97 4 15 5 -1 26520.4 2644.10 4 0 0 0 0.00 0.00 0 TITL YCOB30-01-kT in Cm REM Cm (#8 in standard setting) CELL 0.71073 8.073681 16.008822 3.528266 90.0000 101.1658 90.0000 ZERR 2.00 0.000202 0.000519 0.000105 0.0000 0.0027 0.0000 LATT -7 SYMM x,-y, z SFAC B O Ca Y UNIT 6.00 20.00 8.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 44224 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, 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 Y-X Y 0.00039(4) 0.0000 0.00190(7) 0.00756(10) Uani 0.832(4) 2 d S T P . . Ca-Y Ca -0.35979(6) -0.11231(3) 0.32719(12) 0.00802(12) Uani 0.9169(18) 1 d . . P . . Ca-Z Ca 0.25683(7) 0.18104(4) -0.35075(15) 0.01134(12) Uani 1 1 d . . . . . Ca-X Ca 0.00039(4) 0.0000 0.00190(7) 0.00756(10) Uani 0.168(4) 2 d S T P . . Y-Y Y -0.35979(6) -0.11231(3) 0.32719(12) 0.00802(12) Uani 0.0831(18) 1 d . . P . . O1 O -0.1737(4) 0.0000 0.4203(9) 0.0098(5) Uani 1 2 d S T P . . O2 O 0.1982(4) 0.0000 -0.3968(10) 0.0151(6) Uani 1 2 d S T P . . O3 O 0.0797(3) 0.14172(15) 0.0729(6) 0.0108(4) Uani 1 1 d . . . . . O4 O -0.5333(3) -0.23065(15) 0.2737(7) 0.0140(4) Uani 1 1 d . . . . . O5 O -0.2138(3) -0.17408(15) -0.1186(6) 0.0125(4) Uani 1 1 d . . . . . O6 O 0.4588(3) 0.07444(15) -0.2518(6) 0.0122(4) Uani 1 1 d . . . . . B1 B 0.3721(5) 0.0000 -0.3003(12) 0.0070(6) Uani 1 2 d S T P . . B2 B -0.5551(4) -0.3055(2) 0.0768(9) 0.0090(5) 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 Y-X 0.00616(14) 0.0097(2) 0.00689(16) 0.000 0.00141(11) 0.000 Ca-Y 0.00713(18) 0.0084(2) 0.0083(2) 0.00009(15) 0.00101(14) -0.00018(15) Ca-Z 0.00933(19) 0.0157(3) 0.0092(2) -0.00087(18) 0.00232(16) -0.00077(18) Ca-X 0.00616(14) 0.0097(2) 0.00689(16) 0.000 0.00141(11) 0.000 Y-Y 0.00713(18) 0.0084(2) 0.0083(2) 0.00009(15) 0.00101(14) -0.00018(15) O1 0.0080(10) 0.0109(13) 0.0102(11) 0.000 0.0005(9) 0.000 O2 0.0045(10) 0.027(2) 0.0133(13) 0.000 0.0015(9) 0.000 O3 0.0095(7) 0.0116(10) 0.0112(8) 0.0003(7) 0.0021(6) 0.0026(7) O4 0.0153(9) 0.0127(10) 0.0149(10) -0.0054(7) 0.0053(7) -0.0040(8) O5 0.0086(7) 0.0167(11) 0.0114(9) 0.0002(7) 0.0002(6) 0.0035(7) O6 0.0122(8) 0.0102(10) 0.0136(9) 0.0000(7) 0.0012(7) -0.0032(7) B1 0.0059(12) 0.0083(17) 0.0065(15) 0.000 0.0004(11) 0.000 B2 0.0081(10) 0.0092(13) 0.0096(11) 0.0009(9) 0.0016(9) -0.0019(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 O1 Y-X O1 103.97(12) . 1_554 O1 Y-X O2 175.86(11) . . O1 Y-X O2 80.17(11) 1_554 . O1 Y-X O3 97.05(5) . . O1 Y-X O3 101.86(6) 1_554 . O2 Y-X O3 81.95(6) . . O1 Y-X O3 97.05(5) . 2 O1 Y-X O3 101.86(6) 1_554 2 O2 Y-X O3 81.95(5) . 2 O3 Y-X O3 148.47(10) . 2 O1 Y-X O2 79.11(11) . 1_556 O1 Y-X O2 176.92(11) 1_554 1_556 O2 Y-X O2 96.75(11) . 1_556 O3 Y-X O2 77.59(6) . 1_556 O3 Y-X O2 77.59(6) 2 1_556 O1 Y-X Ca-X 38.26(8) . 1_556 O1 Y-X Ca-X 142.23(8) 1_554 1_556 O2 Y-X Ca-X 137.59(8) . 1_556 O3 Y-X Ca-X 86.92(5) . 1_556 O3 Y-X Ca-X 86.92(5) 2 1_556 O2 Y-X Ca-X 40.85(7) 1_556 1_556 O1 Y-X Y-X 38.26(8) . 1_556 O1 Y-X Y-X 142.23(8) 1_554 1_556 O2 Y-X Y-X 137.59(8) . 1_556 O3 Y-X Y-X 86.92(5) . 1_556 O3 Y-X Y-X 86.92(5) 2 1_556 O2 Y-X Y-X 40.85(7) 1_556 1_556 Ca-X Y-X Y-X 0.0 1_556 1_556 O1 Y-X Y-X 141.74(8) . 1_554 O1 Y-X Y-X 37.77(8) 1_554 1_554 O2 Y-X Y-X 42.40(8) . 1_554 O3 Y-X Y-X 93.08(5) . 1_554 O3 Y-X Y-X 93.08(5) 2 1_554 O2 Y-X Y-X 139.15(7) 1_556 1_554 Ca-X Y-X Y-X 180.0 1_556 1_554 Y-X Y-X Y-X 180.0 1_556 1_554 O1 Y-X Ca-X 141.74(8) . 1_554 O1 Y-X Ca-X 37.77(8) 1_554 1_554 O2 Y-X Ca-X 42.40(8) . 1_554 O3 Y-X Ca-X 93.08(5) . 1_554 O3 Y-X Ca-X 93.08(5) 2 1_554 O2 Y-X Ca-X 139.15(7) 1_556 1_554 Ca-X Y-X Ca-X 180.0 1_556 1_554 Y-X Y-X Ca-X 180.0 1_556 1_554 Y-X Y-X Ca-X 0.000(11) 1_554 1_554 O1 Y-X Y-Y 34.67(4) . 2 O1 Y-X Y-Y 84.00(7) 1_554 2 O2 Y-X Y-Y 147.44(4) . 2 O3 Y-X Y-Y 73.69(5) . 2 O3 Y-X Y-Y 129.36(5) 2 2 O2 Y-X Y-Y 98.70(7) 1_556 2 Ca-X Y-X Y-Y 63.100(9) 1_556 2 Y-X Y-X Y-Y 63.100(9) 1_556 2 Y-X Y-X Y-Y 116.901(9) 1_554 2 Ca-X Y-X Y-Y 116.901(9) 1_554 2 O1 Y-X Ca-Y 34.67(4) . 2 O1 Y-X Ca-Y 84.00(7) 1_554 2 O2 Y-X Ca-Y 147.44(4) . 2 O3 Y-X Ca-Y 73.69(5) . 2 O3 Y-X Ca-Y 129.36(5) 2 2 O2 Y-X Ca-Y 98.70(7) 1_556 2 Ca-X Y-X Ca-Y 63.100(9) 1_556 2 Y-X Y-X Ca-Y 63.100(9) 1_556 2 Y-X Y-X Ca-Y 116.901(9) 1_554 2 Ca-X Y-X Ca-Y 116.901(9) 1_554 2 Y-Y Y-X Ca-Y 0.0 2 2 O5 Ca-Y O1 90.09(9) 1_556 . O5 Ca-Y O4 85.46(9) 1_556 . O1 Ca-Y O4 175.51(9) . . O5 Ca-Y O6 168.33(9) 1_556 2_455 O1 Ca-Y O6 101.54(9) . 2_455 O4 Ca-Y O6 82.90(9) . 2_455 O5 Ca-Y O5 98.43(8) 1_556 . O1 Ca-Y O5 91.47(9) . . O4 Ca-Y O5 88.60(8) . . O6 Ca-Y O5 80.57(7) 2_455 . O5 Ca-Y O6 81.59(8) 1_556 2_456 O1 Ca-Y O6 100.10(9) . 2_456 O4 Ca-Y O6 79.86(8) . 2_456 O6 Ca-Y O6 97.05(8) 2_455 2_456 O5 Ca-Y O6 168.43(9) . 2_456 O5 Ca-Y B2 75.70(8) 1_556 4_545 O1 Ca-Y B2 80.81(9) . 4_545 O4 Ca-Y B2 97.48(9) . 4_545 O6 Ca-Y B2 105.05(8) 2_455 4_545 O5 Ca-Y B2 25.22(8) . 4_545 O6 Ca-Y B2 157.28(8) 2_456 4_545 O5 Ca-Y B1 99.46(9) 1_556 1_456 O1 Ca-Y B1 88.74(8) . 1_456 O4 Ca-Y B1 92.56(7) . 1_456 O6 Ca-Y B1 81.85(9) 2_455 1_456 O5 Ca-Y B1 162.11(9) . 1_456 O6 Ca-Y B1 21.20(8) 2_456 1_456 B2 Ca-Y B1 168.41(9) 4_545 1_456 O5 Ca-Y Ca-Y 41.38(6) 1_556 1_556 O1 Ca-Y Ca-Y 89.07(8) . 1_556 O4 Ca-Y Ca-Y 87.98(6) . 1_556 O6 Ca-Y Ca-Y 138.45(5) 2_455 1_556 O5 Ca-Y Ca-Y 139.81(5) . 1_556 O6 Ca-Y Ca-Y 41.40(5) 2_456 1_556 B2 Ca-Y Ca-Y 116.32(6) 4_545 1_556 B1 Ca-Y Ca-Y 58.08(7) 1_456 1_556 O5 Ca-Y Y-Y 41.38(6) 1_556 1_556 O1 Ca-Y Y-Y 89.07(8) . 1_556 O4 Ca-Y Y-Y 87.98(6) . 1_556 O6 Ca-Y Y-Y 138.45(5) 2_455 1_556 O5 Ca-Y Y-Y 139.81(5) . 1_556 O6 Ca-Y Y-Y 41.40(5) 2_456 1_556 B2 Ca-Y Y-Y 116.32(6) 4_545 1_556 B1 Ca-Y Y-Y 58.08(7) 1_456 1_556 Ca-Y Ca-Y Y-Y 0.00(2) 1_556 1_556 O5 Ca-Y Ca-Y 138.62(6) 1_556 1_554 O1 Ca-Y Ca-Y 90.93(8) . 1_554 O4 Ca-Y Ca-Y 92.02(6) . 1_554 O6 Ca-Y Ca-Y 41.55(5) 2_455 1_554 O5 Ca-Y Ca-Y 40.19(5) . 1_554 O6 Ca-Y Ca-Y 138.60(5) 2_456 1_554 B2 Ca-Y Ca-Y 63.68(6) 4_545 1_554 B1 Ca-Y Ca-Y 121.92(7) 1_456 1_554 Ca-Y Ca-Y Ca-Y 180.00(3) 1_556 1_554 Y-Y Ca-Y Ca-Y 180.0 1_556 1_554 O5 Ca-Y Y-Y 138.62(6) 1_556 1_554 O1 Ca-Y Y-Y 90.93(8) . 1_554 O4 Ca-Y Y-Y 92.02(6) . 1_554 O6 Ca-Y Y-Y 41.55(5) 2_455 1_554 O5 Ca-Y Y-Y 40.19(5) . 1_554 O6 Ca-Y Y-Y 138.60(5) 2_456 1_554 B2 Ca-Y Y-Y 63.68(6) 4_545 1_554 B1 Ca-Y Y-Y 121.92(7) 1_456 1_554 Ca-Y Ca-Y Y-Y 180.00(3) 1_556 1_554 Y-Y Ca-Y Y-Y 180.00(3) 1_556 1_554 Ca-Y Ca-Y Y-Y 0.0 1_554 1_554 O3 Ca-Z O6 103.01(8) 1_554 . O3 Ca-Z O3 97.84(8) 1_554 . O6 Ca-Z O3 101.69(8) . . O3 Ca-Z O5 123.26(8) 1_554 3 O6 Ca-Z O5 128.29(8) . 3 O3 Ca-Z O5 94.15(8) . 3 O3 Ca-Z O4 89.29(8) 1_554 2_654 O6 Ca-Z O4 77.54(8) . 2_654 O3 Ca-Z O4 172.79(8) . 2_654 O5 Ca-Z O4 81.00(8) 3 2_654 O3 Ca-Z O4 176.58(8) 1_554 2_655 O6 Ca-Z O4 77.17(8) . 2_655 O3 Ca-Z O4 85.44(8) . 2_655 O5 Ca-Z O4 55.26(7) 3 2_655 O4 Ca-Z O4 87.41(8) 2_654 2_655 O3 Ca-Z B2 147.95(10) 1_554 2_655 O6 Ca-Z B2 98.67(9) . 2_655 O3 Ca-Z B2 100.58(9) . 2_655 O5 Ca-Z B2 29.68(8) 3 2_655 O4 Ca-Z B2 72.59(9) 2_654 2_655 O4 Ca-Z B2 29.46(9) 2_655 2_655 O3 Ca-Z O4 54.27(7) 1_554 3_554 O6 Ca-Z O4 157.28(7) . 3_554 O3 Ca-Z O4 83.17(7) . 3_554 O5 Ca-Z O4 72.70(7) 3 3_554 O4 Ca-Z O4 100.32(6) 2_654 3_554 O4 Ca-Z O4 125.53(5) 2_655 3_554 B2 Ca-Z O4 102.25(8) 2_655 3_554 O3 Ca-Z B2 27.77(9) 1_554 3_554 O6 Ca-Z B2 129.88(9) . 3_554 O3 Ca-Z B2 84.83(8) . 3_554 O5 Ca-Z B2 100.12(9) 3 3_554 O4 Ca-Z B2 101.21(8) 2_654 3_554 O4 Ca-Z B2 152.67(9) 2_655 3_554 B2 Ca-Z B2 129.29(5) 2_655 3_554 O4 Ca-Z B2 27.70(8) 3_554 3_554 O3 Ca-Z O2 67.71(9) 1_554 . O6 Ca-Z O2 52.29(8) . . O3 Ca-Z O2 70.05(9) . . O5 Ca-Z O2 162.72(9) 3 . O4 Ca-Z O2 114.01(9) 2_654 . O4 Ca-Z O2 114.54(9) 2_655 . B2 Ca-Z O2 143.71(9) 2_655 . O4 Ca-Z O2 110.90(8) 3_554 . B2 Ca-Z O2 85.79(9) 3_554 . O3 Ca-Z B1 85.58(10) 1_554 . O6 Ca-Z B1 25.68(9) . . O3 Ca-Z B1 85.66(10) . . O5 Ca-Z B1 150.76(9) 3 . O4 Ca-Z B1 95.96(10) 2_654 . O4 Ca-Z B1 95.67(9) 2_655 . B2 Ca-Z B1 121.68(10) 2_655 . O4 Ca-Z B1 135.96(9) 3_554 . B2 Ca-Z B1 108.96(10) 3_554 . O2 Ca-Z B1 26.61(10) . . O3 Ca-Z B2 91.35(8) 1_554 3 O6 Ca-Z B2 124.85(8) . 3 O3 Ca-Z B2 23.16(8) . 3 O5 Ca-Z B2 79.17(8) 3 3 O4 Ca-Z B2 156.65(9) 2_654 3 O4 Ca-Z B2 91.32(8) 2_655 3 B2 Ca-Z B2 95.38(9) 2_655 3 O4 Ca-Z B2 61.95(7) 3_554 3 B2 Ca-Z B2 70.53(7) 3_554 3 O2 Ca-Z B2 87.68(9) . 3 B1 Ca-Z B2 107.36(10) . 3 Y-X O1 Ca-X 104.0 . 1_556 Y-X O1 Y-X 103.97(12) . 1_556 Ca-X O1 Y-X 0.0 1_556 1_556 Y-X O1 Y-Y 112.33(9) . 2 Ca-X O1 Y-Y 113.64(9) 1_556 2 Y-X O1 Y-Y 113.64(9) 1_556 2 Y-X O1 Ca-Y 112.33(9) . 2 Ca-X O1 Ca-Y 113.64(9) 1_556 2 Y-X O1 Ca-Y 113.64(9) 1_556 2 Y-Y O1 Ca-Y 0.0 2 2 Y-X O1 Ca-Y 112.33(9) . . Ca-X O1 Ca-Y 113.64(9) 1_556 . Y-X O1 Ca-Y 113.64(9) 1_556 . Y-Y O1 Ca-Y 101.3 2 . Ca-Y O1 Ca-Y 101.29(11) 2 . B1 O2 Y-X 129.6(3) . . B1 O2 Ca-X 133.7(3) . 1_554 Y-X O2 Ca-X 96.7 . 1_554 B1 O2 Y-X 133.7(3) . 1_554 Y-X O2 Y-X 96.75(11) . 1_554 Ca-X O2 Y-X 0.0 1_554 1_554 B1 O2 Ca-Z 80.85(6) . 2 Y-X O2 Ca-Z 95.09(6) . 2 Ca-X O2 Ca-Z 96.99(7) 1_554 2 Y-X O2 Ca-Z 96.99(7) 1_554 2 B1 O2 Ca-Z 80.85(6) . . Y-X O2 Ca-Z 95.09(6) . . Ca-X O2 Ca-Z 96.99(7) 1_554 . Y-X O2 Ca-Z 96.99(7) 1_554 . Ca-Z O2 Ca-Z 161.60(12) 2 . B2 O3 Ca-Z 100.22(18) 3 1_556 B2 O3 Ca-Z 114.90(18) 3 . Ca-Z O3 Ca-Z 97.84(8) 1_556 . B2 O3 Y-X 113.09(18) 3 . Ca-Z O3 Y-X 117.38(10) 1_556 . Ca-Z O3 Y-X 112.15(9) . . B2 O4 Ca-Y 139.40(19) . . B2 O4 Ca-Z 120.97(18) . 2_456 Ca-Y O4 Ca-Z 99.10(9) . 2_456 B2 O4 Ca-Z 80.86(16) . 2_455 Ca-Y O4 Ca-Z 95.82(9) . 2_455 Ca-Z O4 Ca-Z 87.41(8) 2_456 2_455 B2 O4 Ca-Z 79.39(17) . 3_446 Ca-Y O4 Ca-Z 86.47(7) . 3_446 Ca-Z O4 Ca-Z 119.94(9) 2_456 3_446 Ca-Z O4 Ca-Z 151.93(9) 2_455 3_446 B2 O5 Y-Y 143.6(2) 4_545 1_554 B2 O5 Ca-Y 143.6(2) 4_545 1_554 Y-Y O5 Ca-Y 0.0 1_554 1_554 B2 O5 Ca-Y 107.68(18) 4_545 . Y-Y O5 Ca-Y 98.4 1_554 . Ca-Y O5 Ca-Y 98.43(8) 1_554 . B2 O5 Ca-Z 87.86(18) 4_545 3_445 Y-Y O5 Ca-Z 97.01(8) 1_554 3_445 Ca-Y O5 Ca-Z 97.01(8) 1_554 3_445 Ca-Y O5 Ca-Z 126.16(10) . 3_445 B1 O6 Ca-Z 106.85(19) . . B1 O6 Y-Y 123.2(2) . 2_655 Ca-Z O6 Y-Y 103.92(9) . 2_655 B1 O6 Ca-Y 123.2(2) . 2_655 Ca-Z O6 Ca-Y 103.92(9) . 2_655 Y-Y O6 Ca-Y 0.0 2_655 2_655 B1 O6 Ca-Y 120.5(2) . 2_654 Ca-Z O6 Ca-Y 102.62(9) . 2_654 Y-Y O6 Ca-Y 97.0 2_655 2_654 Ca-Y O6 Ca-Y 97.05(8) 2_655 2_654 B1 O6 Y-Y 120.5(2) . 2_654 Ca-Z O6 Y-Y 102.62(9) . 2_654 Y-Y O6 Y-Y 97.05(8) 2_655 2_654 Ca-Y O6 Y-Y 97.05(8) 2_655 2_654 Ca-Y O6 Y-Y 0.00(3) 2_654 2_654 O6 B1 O6 120.0(4) 2 . O6 B1 O2 120.00(18) 2 . O6 B1 O2 120.00(18) . . O6 B1 Ca-Z 167.4(2) 2 . O6 B1 Ca-Z 47.46(12) . . O2 B1 Ca-Z 72.54(7) . . O6 B1 Ca-Z 47.46(12) 2 2 O6 B1 Ca-Z 167.4(2) . 2 O2 B1 Ca-Z 72.54(8) . 2 Ca-Z B1 Ca-Z 145.04(15) . 2 O6 B1 Ca-Y 99.5(2) 2 2_654 O6 B1 Ca-Y 38.30(15) . 2_654 O2 B1 Ca-Y 128.38(19) . 2_654 Ca-Z B1 Ca-Y 70.85(4) . 2_654 Ca-Z B1 Ca-Y 135.90(12) 2 2_654 O6 B1 Ca-Y 38.30(15) 2 1_654 O6 B1 Ca-Y 99.5(2) . 1_654 O2 B1 Ca-Y 128.38(19) . 1_654 Ca-Z B1 Ca-Y 135.90(12) . 1_654 Ca-Z B1 Ca-Y 70.85(4) 2 1_654 Ca-Y B1 Ca-Y 66.51(8) 2_654 1_654 O5 B2 O4 118.5(3) 4_445 . O5 B2 O3 120.7(3) 4_445 3_445 O4 B2 O3 120.9(3) . 3_445 O5 B2 Ca-Z 62.46(16) 4_445 2_455 O4 B2 Ca-Z 69.68(17) . 2_455 O3 B2 Ca-Z 141.8(2) 3_445 2_455 O5 B2 Ca-Z 158.1(2) 4_445 3_446 O4 B2 Ca-Z 72.92(16) . 3_446 O3 B2 Ca-Z 52.00(14) 3_445 3_446 Ca-Z B2 Ca-Z 137.73(13) 2_455 3_446 O5 B2 Ca-Y 47.10(14) 4_445 4_445 O4 B2 Ca-Y 105.01(18) . 4_445 O3 B2 Ca-Y 114.7(2) 3_445 4_445 Ca-Z B2 Ca-Y 94.59(9) 2_455 4_445 Ca-Z B2 Ca-Y 113.71(10) 3_446 4_445 O5 B2 Y-Y 47.10(14) 4_445 4_445 O4 B2 Y-Y 105.01(18) . 4_445 O3 B2 Y-Y 114.7(2) 3_445 4_445 Ca-Z B2 Y-Y 94.59(9) 2_455 4_445 Ca-Z B2 Y-Y 113.71(10) 3_446 4_445 Ca-Y B2 Y-Y 0.00(2) 4_445 4_445 O5 B2 Ca-X 81.76(18) 4_445 3_445 O4 B2 Ca-X 152.9(2) . 3_445 O3 B2 Ca-X 43.26(15) 3_445 3_445 Ca-Z B2 Ca-X 137.25(12) 2_455 3_445 Ca-Z B2 Ca-X 82.39(8) 3_446 3_445 Ca-Y B2 Ca-X 74.70(7) 4_445 3_445 Y-Y B2 Ca-X 74.70(7) 4_445 3_445 O5 B2 Ca-Z 119.5(2) 4_445 3_445 O4 B2 Ca-Z 105.20(17) . 3_445 O3 B2 Ca-Z 41.94(13) 3_445 3_445 Ca-Z B2 Ca-Z 101.04(9) 2_455 3_445 Ca-Z B2 Ca-Z 70.53(7) 3_446 3_445 Ca-Y B2 Ca-Z 149.26(12) 4_445 3_445 Y-Y B2 Ca-Z 149.26(12) 4_445 3_445 Ca-X B2 Ca-Z 75.86(7) 3_445 3_445 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Y-X O1 2.227(3) . Y-X O1 2.252(3) 1_554 Y-X O2 2.324(3) . Y-X O3 2.358(2) . Y-X O3 2.358(2) 2 Y-X O2 2.396(3) 1_556 Y-X Ca-X 3.52825(10) 1_556 Y-X Y-X 3.52825(10) 1_556 Y-X Y-X 3.52828(10) 1_554 Y-X Ca-X 3.52828(10) 1_554 Y-X Y-Y 3.7813(5) 2 Y-X Ca-Y 3.7813(5) 2 Ca-Y O5 2.302(2) 1_556 Ca-Y O1 2.3251(19) . Ca-Y O4 2.342(2) . Ca-Y O6 2.351(2) 2_455 Ca-Y O5 2.358(2) . Ca-Y O6 2.358(2) 2_456 Ca-Y B2 3.067(3) 4_545 Ca-Y B1 3.278(3) 1_456 Ca-Y Ca-Y 3.52825(10) 1_556 Ca-Y Y-Y 3.52825(10) 1_556 Ca-Y Ca-Y 3.52828(11) 1_554 Ca-Y Y-Y 3.52828(11) 1_554 Ca-Z O3 2.335(2) 1_554 Ca-Z O6 2.339(2) . Ca-Z O3 2.346(2) . Ca-Z O5 2.456(2) 3 Ca-Z O4 2.475(2) 2_654 Ca-Z O4 2.629(2) 2_655 Ca-Z B2 2.768(3) 2_655 Ca-Z O4 2.835(3) 3_554 Ca-Z B2 2.916(3) 3_554 Ca-Z O2 2.9360(8) . Ca-Z B1 3.0385(14) . Ca-Z B2 3.184(3) 3 O1 Ca-X 2.252(3) 1_556 O1 Y-X 2.252(3) 1_556 O1 Y-Y 2.3251(19) 2 O1 Ca-Y 2.3251(19) 2 O2 B1 1.379(5) . O2 Ca-X 2.396(3) 1_554 O2 Y-X 2.396(3) 1_554 O2 Ca-Z 2.9360(8) 2 O3 B2 1.381(4) 3 O3 Ca-Z 2.335(2) 1_556 O4 B2 1.379(4) . O4 Ca-Z 2.475(2) 2_456 O4 Ca-Z 2.629(2) 2_455 O4 Ca-Z 2.835(3) 3_446 O5 B2 1.371(4) 4_545 O5 Y-Y 2.302(2) 1_554 O5 Ca-Y 2.302(2) 1_554 O5 Ca-Z 2.456(2) 3_445 O6 B1 1.376(3) . O6 Y-Y 2.351(2) 2_655 O6 Ca-Y 2.351(2) 2_655 O6 Ca-Y 2.358(2) 2_654 O6 Y-Y 2.358(2) 2_654 B1 O6 1.376(3) 2 B1 Ca-Z 3.0386(14) 2 B1 Ca-Y 3.278(3) 2_654 B1 Ca-Y 3.278(3) 1_654 B2 O5 1.371(4) 4_445 B2 O3 1.380(4) 3_445 B2 Ca-Z 2.768(3) 2_455 B2 Ca-Z 2.916(3) 3_446 B2 Ca-Y 3.067(3) 4_445 B2 Y-Y 3.067(3) 4_445 B2 Ca-X 3.165(4) 3_445 B2 Ca-Z 3.184(3) 3_445