#------------------------------------------------------------------------------ #$Date: 2021-11-26 01:55:05 +0200 (Fri, 26 Nov 2021) $ #$Revision: 270882 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/89/7708933.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_7708933 loop_ _publ_author_name 'Cong, Zhenzhong' 'Zhu, Mingchang' 'Zhang, Ying' 'Yao, Wei' 'Kosinova, Marina' 'Fedin, Vladimir P.' 'Wu, Shuangyan' 'Gao, Enjun' _publ_section_title ; Three novel metal-organic frameworks with different coordination modes for trace detection of anthrax biomarkers ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03760A _journal_year 2021 _chemical_formula_moiety 'C24 H14 Ca3 O22' _chemical_formula_sum 'C24 H22 Ca3 O22' _chemical_formula_weight 782.65 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-08-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-06 deposited with the CCDC. 2021-11-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.9800(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9374(2) _cell_length_b 22.5281(5) _cell_length_c 19.6837(5) _cell_measurement_reflns_used 9968 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 26.31 _cell_measurement_theta_min 2.75 _cell_volume 3514.97(15) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 48264 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 2.072 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.994 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0696 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.3877. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.479 _exptl_crystal_description block _exptl_crystal_F_000 1608 _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.912 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 454 _refine_ls_number_reflns 7169 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0548 _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^)+(0.1057P)^2^+3.4557P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1638 _refine_ls_wR_factor_ref 0.1747 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5692 _reflns_number_total 7169 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03760a2.cif _cod_data_source_block mo_1023_18_0m _cod_database_code 7708933 _shelx_shelxl_version_number 2017/1 _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_max 0.994 _shelx_estimated_absorpt_t_min 0.994 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 3. Others Fixed Sof: O6(0.5) O7(0.5) 4.a Rotating group: O00E(H00A,H00B), O00M(H00C,H00D), O00O(H00E,H00F) 4.b Aromatic/amide H refined with riding coordinates: C00T(H00T), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C015(H015), C018(H018), C01B(H01B) ; _smtbx_masks_void_probe_radius 0.01 _smtbx_masks_void_truncation_radius 0.01 _shelx_res_file ; TITL mo_1023_18_0m_a.res in P2(1)/c mo_1023_18_0m.res created by SHELXL-2017/1 at 16:59:50 on 06-Aug-2021 REM Old TITL mo_1023_18_0m in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.121, Rweak 0.005, Alpha 0.022 REM 0.486 for 201 systematic absences, Orientation as input REM Formula found by SHELXT: C34 Ca3 O20 CELL 0.71073 7.9374 22.5281 19.6837 90 92.98 90 ZERR 4 0.0002 0.0005 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ca O UNIT 96 88 12 88 EQIV $1 +X,0.5-Y,-0.5+Z EQIV $2 -X,1-Y,1-Z ISOR 0.001 0.002 O3 L.S. 20 PLAN 4 SIZE 0.01 0.01 0.01 TEMP -123.15 FREE Ca01 C00S FREE Ca03 C00P_$1 FREE Ca03 Ca01 FREE Ca02 Ca01_$2 CONF list 4 MORE -1 BOND $H ABIN fmap 2 acta OMIT -1 4 5 OMIT -1 0 4 REM REM REM WGHT 0.105700 3.455700 FVAR 0.40932 CA01 3 1.121773 0.220812 0.196614 11.00000 0.02424 0.02594 = 0.02550 -0.00012 0.00219 0.00045 CA02 3 0.269185 0.639694 0.231692 11.00000 0.02721 0.02963 = 0.03337 0.00222 0.00457 0.00027 CA03 3 0.899755 0.367621 0.158499 11.00000 0.03461 0.03155 = 0.03293 -0.00193 0.00268 0.00345 O004 4 0.901296 0.247333 0.615449 11.00000 0.03125 0.03489 = 0.02615 -0.00036 0.00095 -0.00222 O005 4 1.059317 0.634134 0.322141 11.00000 0.03122 0.02672 = 0.03141 0.00155 0.00278 -0.00136 O006 4 0.938357 0.211854 0.294568 11.00000 0.03047 0.03265 = 0.02971 -0.00579 0.00443 -0.00121 O007 4 0.314226 0.293689 0.609216 11.00000 0.02967 0.03845 = 0.02893 -0.00175 0.00415 -0.00470 O008 4 0.718389 0.634144 0.269741 11.00000 0.03420 0.02944 = 0.03413 0.00279 -0.00036 -0.00491 O009 4 0.307592 0.266791 0.285463 11.00000 0.03358 0.03264 = 0.03076 -0.00058 -0.00233 -0.00219 O00A 4 1.176131 0.325379 0.151471 11.00000 0.03256 0.03357 = 0.03322 -0.00136 0.00389 0.00073 O00B 4 0.975586 0.427834 0.473941 11.00000 0.05459 0.02654 = 0.03038 0.00117 -0.00455 -0.00294 O00C 4 0.948471 0.304339 0.258645 11.00000 0.04135 0.03573 = 0.02604 0.00100 0.00272 0.00056 O00D 4 0.294134 0.216864 0.537104 11.00000 0.04875 0.03305 = 0.03427 0.00077 0.00760 -0.00574 O00E 4 0.372322 0.710735 0.316467 11.00000 0.02768 0.04831 = 0.04079 -0.00740 0.00297 0.00113 AFIX 7 H00A 2 0.467570 0.697738 0.337127 11.00000 -1.50000 H00B 2 0.301706 0.713155 0.349919 11.00000 -1.50000 AFIX 0 O00F 4 0.634169 0.443748 0.480576 11.00000 0.05187 0.03776 = 0.02966 -0.00133 0.00930 -0.01641 O00G 4 0.443766 0.691845 0.161269 11.00000 0.03476 0.04999 = 0.03697 0.00366 0.00356 -0.00975 O00H 4 0.356612 0.361994 0.261086 11.00000 0.04849 0.03848 = 0.03284 0.00301 -0.00214 -0.01024 O00I 4 1.083757 0.555533 0.255942 11.00000 0.04321 0.03482 = 0.04254 -0.00749 0.01501 -0.00642 O00J 4 0.845701 0.174038 0.543480 11.00000 0.06523 0.03289 = 0.03463 0.00055 0.00502 -0.01144 O00K 4 0.483437 0.584027 0.287424 11.00000 0.02691 0.03687 = 0.08277 0.01359 -0.00331 -0.00024 O00M 4 1.044528 0.432907 0.237566 11.00000 0.06550 0.04177 = 0.05161 -0.00354 -0.00870 0.00210 AFIX 7 H00C 2 1.045570 0.470247 0.221315 11.00000 -1.50000 H00D 2 1.154648 0.423660 0.242094 11.00000 -1.50000 AFIX 0 C00N 1 0.918667 0.288669 0.377096 11.00000 0.02419 0.03192 = 0.02772 -0.00041 0.00019 0.00252 O00O 4 0.622125 0.334843 0.177048 11.00000 0.04994 0.06783 = 0.09329 -0.00988 0.01732 0.00192 AFIX 7 H00E 2 0.621241 0.299404 0.201686 11.00000 -1.50000 H00F 2 0.564364 0.360406 0.205409 11.00000 -1.50000 AFIX 0 C00P 1 0.881177 0.227582 0.555146 11.00000 0.03186 0.03328 = 0.03046 -0.00041 0.00251 -0.00151 C00Q 1 0.326894 0.270630 0.551011 11.00000 0.02564 0.03517 = 0.03020 -0.00069 0.00443 -0.00337 C00R 1 0.893347 0.468469 0.431737 11.00000 0.04526 0.02539 = 0.02350 -0.00298 -0.00018 -0.00048 C00S 1 0.932884 0.267671 0.305084 11.00000 0.02388 0.03452 = 0.02932 -0.00241 0.00280 -0.00027 C00T 1 0.897941 0.249113 0.430159 11.00000 0.02852 0.03067 = 0.02923 -0.00262 0.00035 -0.00364 AFIX 43 H00T 2 0.881264 0.208090 0.420868 11.00000 -1.20000 AFIX 0 C00U 1 0.901615 0.269611 0.497009 11.00000 0.02772 0.03168 = 0.02719 0.00086 0.00121 -0.00084 C00V 1 0.386133 0.309382 0.495032 11.00000 0.02841 0.03256 = 0.02992 -0.00221 0.00385 0.00132 C00W 1 1.020262 0.581514 0.304970 11.00000 0.02630 0.03256 = 0.02964 0.00031 -0.00173 -0.00009 C00X 1 0.939402 0.349092 0.390740 11.00000 0.03132 0.03336 = 0.02818 0.00208 0.00163 0.00012 AFIX 43 H00X 2 0.950438 0.376561 0.354623 11.00000 -1.20000 AFIX 0 C00Y 1 0.926268 0.329608 0.510906 11.00000 0.03169 0.03280 = 0.02702 -0.00033 0.00054 0.00117 AFIX 43 H00Y 2 0.931075 0.343696 0.556456 11.00000 -1.20000 AFIX 0 C00Z 1 0.348778 0.294594 0.426998 11.00000 0.02517 0.02810 = 0.03534 0.00056 0.00271 -0.00113 AFIX 43 H00Z 2 0.287788 0.259318 0.415914 11.00000 -1.20000 AFIX 0 C010 1 0.478723 0.360126 0.511230 11.00000 0.03361 0.03486 = 0.02864 -0.00070 0.00380 -0.00185 AFIX 43 H010 2 0.502889 0.370570 0.557472 11.00000 -1.20000 AFIX 0 C011 1 0.906752 0.546433 0.348590 11.00000 0.03415 0.02583 = 0.02779 -0.00256 0.00315 -0.00270 C012 1 0.400721 0.331408 0.375615 11.00000 0.02526 0.03257 = 0.03358 -0.00280 0.00387 0.00076 C013 1 0.943678 0.368439 0.457225 11.00000 0.03245 0.02816 = 0.03028 0.00009 0.00211 -0.00030 C014 1 0.719262 0.476000 0.432754 11.00000 0.04202 0.02889 = 0.02997 -0.00402 0.00670 -0.01009 C015 1 0.640074 0.517035 0.390566 11.00000 0.03366 0.03431 = 0.03461 -0.00178 0.00692 -0.00411 AFIX 43 H015 2 0.521107 0.521483 0.390942 11.00000 -1.20000 AFIX 0 C016 1 0.730686 0.552236 0.347268 11.00000 0.03083 0.02536 = 0.03626 -0.00025 0.00200 -0.00001 C017 1 0.351284 0.318636 0.302630 11.00000 0.02667 0.03572 = 0.03353 0.00145 0.00247 -0.00027 C018 1 0.985441 0.503796 0.390292 11.00000 0.03233 0.03041 = 0.03167 -0.00249 0.00086 0.00043 AFIX 43 H018 2 1.104330 0.498978 0.390184 11.00000 -1.20000 AFIX 0 C019 1 0.535941 0.395600 0.459486 11.00000 0.03404 0.02912 = 0.03541 -0.00083 0.00644 -0.00372 C01A 1 0.638315 0.594029 0.298504 11.00000 0.02793 0.02900 = 0.03995 -0.00226 0.00340 0.00222 C01B 1 0.496364 0.382201 0.391650 11.00000 0.03439 0.03291 = 0.02989 0.00113 0.00446 -0.00387 AFIX 43 H01B 2 0.533714 0.407182 0.356577 11.00000 -1.20000 AFIX 0 O2 4 1.029098 0.435871 0.075950 11.00000 0.17659 0.06653 = 0.06964 0.01342 0.02441 0.00530 O3 4 0.718069 0.455100 0.149129 11.00000 0.09949 0.09307 = 0.10595 -0.00111 -0.00835 0.00796 O6 4 0.308284 0.569722 0.141889 10.50000 0.06124 0.05294 = 0.06206 -0.02659 0.02594 -0.01118 O7 4 0.194073 0.600196 0.120049 10.50000 0.11086 0.06168 = 0.04332 -0.00402 0.00612 -0.02377 HKLF 4 REM mo_1023_18_0m_a.res in P2(1)/c REM R1 = 0.0548 for 5692 Fo > 4sig(Fo) and 0.0661 for all 7169 data REM 454 parameters refined using 6 restraints END WGHT 0.1037 4.0986 REM Highest difference peak 1.912, deepest hole -0.699, 1-sigma level 0.090 Q1 1 0.8503 0.4545 0.1021 11.00000 0.05 1.91 Q2 1 0.0597 0.5706 0.0690 11.00000 0.05 1.49 Q3 1 0.3136 0.5020 0.1057 11.00000 0.05 1.38 Q4 1 0.8351 0.5080 0.1187 11.00000 0.05 1.07 ; _shelx_res_checksum 21362 _shelx_hkl_file ; 1 0 0 4180.18 83.19 -1 0 0 4291.77 83.29 -1 0 0 4211.68 83.19 -2 0 0 4012.70 83.79 2 0 0 3920.31 83.59 -2 0 0 4005.30 83.79 3 0 0 3207.58 73.09 -3 0 0 3267.07 73.69 3 0 0 3150.58 72.89 -3 0 0 3242.28 73.59 -4 0 0 1656.73 46.30 4 0 0 1656.33 46.10 -4 0 0 1677.83 46.80 4 0 0 1657.73 46.50 5 0 0 6321.17 135.59 -5 0 0 6367.16 136.39 -5 0 0 6277.77 135.69 5 0 0 6170.58 135.29 -6 0 0 518.95 24.50 -6 0 0 571.64 25.30 6 0 0 549.35 24.90 6 0 0 509.05 24.40 7 0 0 62.69 10.80 7 0 0 66.99 11.70 -7 0 0 54.49 9.80 -8 0 0 88.99 12.10 -8 0 0 96.59 13.20 9 0 0 9.60 6.40 9 0 0 29.30 9.50 -9 0 0 1.10 5.00 -9 0 0 6.30 5.80 1 -1 0 13.90 3.00 -1 -1 0 22.50 3.10 -1 -1 0 22.50 3.00 1 -1 0 13.50 3.10 -1 1 0 19.80 3.40 -1 1 0 17.70 3.10 1 1 0 17.20 2.90 2 -1 0 9742.93 189.48 -2 -1 0 9988.30 188.08 2 -1 0 9643.73 189.38 -2 -1 0 9426.56 187.48 2 1 0 9556.24 187.78 -2 1 0 9999.00 190.08 -2 1 0 9445.85 189.18 -3 -1 0 7103.99 141.99 3 -1 0 6895.91 143.09 -3 -1 0 7010.20 141.79 3 -1 0 6847.02 142.99 -3 1 0 6936.91 143.49 -3 1 0 6854.51 142.89 3 1 0 6993.60 141.79 4 -1 0 559.64 23.60 -4 -1 0 543.95 22.70 4 -1 0 519.05 22.90 -4 -1 0 527.25 22.40 4 1 0 559.04 22.50 -4 1 0 558.34 23.80 4 1 0 516.85 22.30 -4 1 0 546.65 23.30 -5 -1 0 3327.87 80.69 5 -1 0 3379.56 81.49 5 -1 0 3393.36 81.89 -5 -1 0 3462.05 81.39 -5 1 0 3364.36 82.39 5 1 0 3292.27 80.49 -5 1 0 3378.76 81.99 5 1 0 3441.96 80.99 -6 -1 0 110.79 12.10 6 -1 0 125.69 14.80 -6 -1 0 110.09 11.70 6 -1 0 104.69 12.10 -6 1 0 109.19 13.90 -6 1 0 100.39 13.20 6 1 0 97.89 13.00 7 -1 0 117.19 12.90 -7 -1 0 131.89 17.00 -7 -1 0 117.49 12.50 7 -1 0 104.39 13.60 7 1 0 103.09 12.70 -7 1 0 112.69 12.60 -8 -1 0 43.00 8.90 -8 -1 0 39.20 7.90 8 -1 0 25.90 8.40 8 1 0 33.00 8.40 -8 1 0 33.10 8.00 -8 1 0 24.40 7.40 -9 -1 0 8.70 6.30 -9 -1 0 12.10 6.40 9 -1 0 28.40 8.80 9 1 0 19.90 6.60 -9 1 0 8.90 6.20 9 1 0 36.20 10.50 -9 1 0 10.90 6.40 -1 -2 0 678.23 17.00 -1 -2 0 699.73 17.20 1 -2 0 659.03 19.20 1 -2 0 718.53 19.60 -1 2 0 648.34 19.00 1 2 0 654.13 17.00 -1 2 0 695.63 19.60 2 -2 0 321.47 15.20 2 -2 0 332.87 15.50 -2 -2 0 312.27 13.10 -2 -2 0 315.97 13.10 -2 2 0 341.87 15.50 2 2 0 302.37 13.20 -2 2 0 315.67 14.80 3 -2 0 45.10 8.40 -3 -2 0 46.10 7.20 -3 -2 0 44.40 7.10 3 -2 0 46.50 8.00 -3 2 0 45.90 7.50 3 2 0 47.30 7.50 -3 2 0 58.79 8.90 -4 -2 0 3594.04 81.99 4 -2 0 3549.04 84.29 4 -2 0 3610.24 84.49 -4 -2 0 3653.63 82.29 -4 2 0 3523.25 83.99 -4 2 0 3528.25 84.59 4 2 0 3637.64 82.19 -5 -2 0 1062.89 34.80 5 -2 0 1063.89 36.20 -5 -2 0 1023.70 34.50 5 -2 0 1017.10 35.80 -5 2 0 997.00 35.80 -5 2 0 1015.80 35.70 5 2 0 1031.70 34.30 6 -2 0 114.59 13.40 6 -2 0 122.29 12.70 -6 -2 0 116.59 12.00 -6 -2 0 93.29 11.40 6 2 0 115.99 11.50 6 2 0 112.19 12.10 -6 2 0 115.59 12.50 -6 2 0 112.89 12.40 7 -2 0 11.80 7.50 -7 -2 0 17.10 7.00 -7 -2 0 4.00 5.00 7 -2 0 10.30 6.10 7 2 0 21.70 7.40 -7 2 0 1.40 5.20 8 -2 0 2.70 6.10 -8 -2 0 4.70 5.40 8 -2 0 4.00 4.90 -8 -2 0 6.50 4.70 -8 2 0 3.00 4.80 -8 2 0 -0.20 4.90 8 2 0 2.00 4.30 -9 -2 0 27.20 6.80 -9 -2 0 15.30 6.30 9 -2 0 19.80 8.90 9 2 0 9.60 5.50 -9 2 0 15.60 6.70 9 2 0 1.70 8.90 0 -3 0 -0.30 1.80 0 -3 0 -2.10 1.70 0 3 0 -1.10 1.00 -1 -3 0 1729.73 37.60 -1 -3 0 1819.12 37.80 1 -3 0 1736.83 40.60 1 -3 0 1688.83 40.70 -1 3 0 1782.32 41.10 -1 3 0 1737.93 40.70 1 3 0 1738.13 37.50 2 -3 0 508.55 20.20 -2 -3 0 522.65 17.10 2 -3 0 528.65 20.10 -2 3 0 503.95 19.70 2 3 0 547.85 17.60 -2 3 0 511.25 20.10 -3 -3 0 686.13 23.00 3 -3 0 668.73 25.60 -3 -3 0 679.13 22.80 3 -3 0 697.93 26.00 3 3 0 664.83 22.80 -3 3 0 695.83 26.10 -3 3 0 657.03 25.20 -4 -3 0 214.38 13.60 -4 -3 0 218.88 13.70 4 -3 0 187.98 14.60 4 -3 0 196.48 14.80 -4 3 0 192.58 14.40 -4 3 0 207.08 15.40 4 3 0 193.18 13.50 5 -3 0 44.90 9.40 5 -3 0 37.20 8.90 -5 -3 0 27.10 7.10 -5 -3 0 25.50 6.50 5 3 0 30.50 7.40 -5 3 0 37.30 7.90 -5 3 0 35.70 8.20 -6 -3 0 401.26 20.70 -6 -3 0 423.16 21.30 6 -3 0 439.96 23.00 6 -3 0 400.36 22.50 6 3 0 404.06 20.70 -6 3 0 428.26 22.70 -6 3 0 436.56 23.10 7 -3 0 25.20 7.40 7 -3 0 41.80 10.10 -7 -3 0 29.60 7.50 -7 -3 0 33.80 7.60 -7 3 0 18.20 7.40 7 3 0 30.50 7.30 8 -3 0 15.00 6.40 -8 -3 0 9.70 5.30 8 -3 0 4.10 6.50 -8 -3 0 5.80 5.00 8 3 0 2.20 4.80 -8 3 0 3.80 5.20 -8 3 0 11.20 7.30 -9 -3 0 13.50 6.40 9 -3 0 41.00 10.00 9 -3 0 16.30 7.40 -9 -3 0 20.80 7.00 -9 3 0 18.30 7.60 9 3 0 18.90 13.60 9 3 0 32.00 10.40 -9 3 0 51.39 10.10 0 -4 0 149.49 8.50 0 -4 0 152.88 8.40 0 4 0 167.08 8.60 -1 -4 0 1184.38 28.40 1 -4 0 1155.38 31.70 1 -4 0 1190.18 31.60 -1 -4 0 1248.88 28.70 1 4 0 1216.78 28.70 -1 4 0 1223.48 32.20 -1 4 0 1192.58 31.60 -2 -4 0 244.08 11.00 2 -4 0 222.38 13.50 -2 -4 0 237.68 11.10 2 -4 0 237.28 14.00 -2 4 0 250.57 14.20 -2 4 0 229.28 13.30 2 4 0 182.28 12.80 2 4 0 211.38 16.90 3 -4 0 228.28 15.10 -3 -4 0 235.48 12.60 3 -4 0 234.98 15.30 -3 -4 0 247.68 12.90 -3 4 0 239.48 15.50 3 4 0 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41.50 9.80 3 -5 15 41.60 9.70 -3 5 -15 44.60 9.80 -3 5 -15 29.00 8.70 3 5 15 27.30 8.30 3 5 15 15.00 7.80 4 -5 15 -9.20 5.70 -4 -5 -15 11.30 6.70 4 -5 15 -2.70 6.50 -4 -5 -15 4.50 6.30 4 5 15 1.00 6.50 4 5 15 3.40 6.30 -4 5 -15 6.90 7.00 -4 5 -15 6.50 6.50 5 -5 15 48.90 10.60 -5 -5 -15 28.70 9.50 5 -5 15 53.39 11.40 -5 5 -15 35.30 9.70 5 5 15 44.50 10.80 5 5 15 43.60 11.60 -5 5 -15 37.70 10.30 -6 -5 -15 -12.40 6.90 6 -5 15 -9.10 8.50 6 -5 15 6.50 7.70 -6 -5 -15 -10.50 6.10 -6 5 -15 -0.50 8.00 6 5 15 -9.80 7.30 -6 5 -15 6.40 8.30 6 5 15 -6.20 5.60 -7 -5 -15 26.20 11.50 7 -5 15 38.00 12.40 -7 -5 -15 26.20 9.20 7 -5 15 20.20 8.60 -7 5 -15 28.80 10.00 -7 5 -15 5.30 8.90 7 5 15 30.50 10.70 7 -6 -15 111.59 13.70 7 -6 -15 152.08 13.80 -7 6 15 119.19 11.60 -7 6 15 88.99 11.60 6 -6 -15 13.00 6.90 6 -6 -15 9.80 6.70 -6 6 15 16.90 5.80 -6 6 15 6.30 5.80 5 -6 -15 2.70 7.30 -5 6 15 14.90 5.60 -5 6 15 0.10 4.20 4 -6 -15 155.28 16.50 -4 6 15 176.28 13.80 -4 6 15 159.58 13.80 -3 -6 15 135.69 7.70 -3 -6 15 138.19 8.10 3 -6 -15 130.59 13.30 3 -6 -15 115.09 13.60 -3 6 15 127.79 12.50 -2 -6 15 13.40 7.10 -2 -6 15 4.70 3.50 2 -6 -15 10.50 6.20 2 -6 -15 1.80 6.20 -2 6 15 4.60 5.00 2 6 -15 3.80 3.40 -2 6 15 10.10 5.60 2 6 -15 0.50 4.20 -1 -6 15 -2.10 3.50 1 -6 -15 -6.50 5.10 1 -6 -15 1.80 5.90 -1 -6 15 4.20 4.10 -1 6 15 0.50 4.70 1 6 -15 -0.30 3.80 -1 6 15 -0.60 4.80 1 6 -15 -1.00 4.30 0 -6 -15 53.69 11.10 0 -6 15 38.80 8.00 0 -6 15 33.90 7.00 0 -6 -15 26.60 7.90 0 6 15 31.60 8.60 0 6 15 49.80 9.30 0 6 -15 37.90 7.20 0 6 -15 45.30 8.10 -1 -6 -15 2068.99 60.19 1 -6 15 2005.90 55.79 1 -6 15 2012.00 55.49 -1 -6 -15 1962.50 58.79 -1 6 -15 1989.80 55.49 1 6 15 2042.10 58.89 1 6 15 2045.30 59.09 2 -6 15 85.49 11.90 -2 -6 -15 67.19 11.80 -2 -6 -15 81.39 12.80 2 -6 15 99.69 12.20 2 6 15 108.99 13.50 -2 6 -15 109.49 13.10 2 6 15 81.29 12.10 -2 6 -15 117.39 13.00 3 -6 15 26.80 8.90 -3 -6 -15 15.50 7.50 -3 -6 -15 16.80 7.40 -3 6 -15 23.60 9.30 3 6 15 28.00 8.20 3 6 15 26.00 7.70 -3 6 -15 32.20 8.60 4 -6 15 67.79 11.60 -4 -6 -15 64.49 11.80 4 -6 15 63.09 11.40 -4 6 -15 57.79 11.70 -4 6 -15 56.79 11.70 4 6 15 59.49 11.40 4 6 15 57.59 11.80 5 -6 15 8.10 8.40 -5 -6 -15 23.00 12.40 -5 -6 -15 20.60 8.80 5 -6 15 12.40 7.30 5 6 15 27.50 9.00 5 6 15 8.80 7.80 -5 6 -15 13.50 8.80 -5 6 -15 15.20 7.80 -6 -6 -15 346.47 23.90 -6 -6 -15 311.97 23.10 6 -6 15 381.96 24.20 -6 6 -15 356.16 25.40 6 6 15 343.07 24.40 -6 6 -15 331.37 24.00 6 6 15 374.96 24.30 -7 -6 -15 84.99 13.20 7 -6 15 71.89 12.10 7 -6 15 79.39 15.00 -7 -6 -15 84.49 14.40 7 6 15 104.99 15.00 -7 6 -15 82.79 14.30 -7 6 -15 98.79 15.60 7 6 15 77.09 18.60 7 -7 -15 11.90 6.50 7 -7 -15 13.10 7.30 -7 7 15 -13.30 5.20 -7 7 15 3.70 4.80 6 -7 -15 273.17 21.30 6 -7 -15 311.87 18.60 -6 7 15 303.27 17.90 -6 7 15 324.27 19.00 -5 7 15 18.80 6.90 -5 7 15 25.30 6.70 4 -7 -15 441.56 23.30 -4 7 15 447.16 22.00 -4 7 15 425.96 22.10 3 -7 -15 67.09 10.80 3 -7 -15 67.79 10.00 -3 7 15 93.79 11.40 -3 7 15 78.69 13.60 -2 -7 15 5.60 3.30 -2 -7 15 7.80 4.10 2 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12 13 -2.2771 0.0464 7 13 0 -3.3837 0.0425 7 13 1 -1.6136 0.0231 7 13 2 -1.1511 -0.0434 7 13 3 1.0350 -0.0148 7 13 4 -2.6798 -0.0867 7 13 5 1.9968 -0.0190 7 13 6 1.5850 0.0613 7 13 7 1.9120 -0.0106 7 13 8 2.6366 -0.0457 7 13 9 0.9687 0.0189 7 13 10 1.8991 0.1350 7 13 11 0.6187 -0.1266 7 13 12 0.1539 -0.2198 7 14 0 0.4786 -0.0225 7 14 1 1.3089 0.0248 7 14 2 1.9970 -0.0585 7 14 3 -1.0879 0.0093 7 14 4 -1.8814 0.0299 7 14 5 0.6030 -0.0408 7 14 6 -0.2595 -0.0092 7 14 7 -2.2605 0.0710 7 14 8 -3.3508 0.0872 7 14 9 -0.4887 -0.0173 7 14 10 -1.3510 -0.0104 7 14 11 -1.7712 0.0066 7 15 0 -2.6808 0.0678 7 15 1 -2.3378 0.0206 7 15 2 1.3532 -0.0674 7 15 3 0.3476 0.0295 7 15 4 0.7329 0.0106 7 15 5 -0.3800 -0.0219 7 15 6 1.1227 -0.0217 7 15 7 1.5666 -0.0447 7 15 8 1.0422 0.0636 7 15 9 -0.0297 -0.1073 7 15 10 1.5850 -0.1257 7 16 0 -0.5280 -0.0047 7 16 1 1.0503 0.0047 7 16 2 1.8116 0.0196 7 16 3 -1.1803 0.0395 7 16 4 -0.0873 -0.0090 7 16 5 -0.5088 -0.0435 7 16 6 0.7514 0.0843 7 16 7 -0.2392 0.0050 7 16 8 -4.0320 -0.0958 7 16 9 -0.6859 0.0103 7 17 0 -3.8683 -0.0906 7 17 1 -0.7286 -0.0050 7 17 2 -0.8456 0.0553 7 17 3 0.0470 -0.0161 7 17 4 1.0063 -0.0582 7 17 5 -0.3268 0.0183 7 17 6 1.3789 0.0113 7 17 7 2.2750 -0.0101 7 17 8 0.2561 -0.0273 7 18 0 -0.1007 -0.0776 7 18 1 1.9680 -0.0153 7 18 2 0.0222 -0.0447 7 18 3 0.6070 0.0394 7 18 4 -1.1667 0.0634 7 18 5 -1.4066 0.0524 7 18 6 -0.2094 -0.1053 7 19 0 -1.0409 -0.0467 7 19 1 -0.0656 0.0217 7 19 2 -1.0633 0.0577 7 19 3 2.9206 0.0481 7 19 4 0.3454 -0.0932 8 0 0 -2.8615 -0.4522 8 0 2 2.5762 0.3912 8 0 4 -3.2822 -0.2935 8 0 6 -2.1155 0.0342 8 0 8 -3.1421 0.0697 8 0 10 0.9587 0.0701 8 0 12 -0.5832 -0.3238 8 1 0 -1.7043 -0.1556 8 1 1 2.3020 -0.3728 8 1 2 -2.3262 0.1443 8 1 3 1.2970 0.2256 8 1 4 -0.6367 -0.1984 8 1 5 0.8727 -0.0922 8 1 6 0.4497 0.2949 8 1 7 1.6365 0.0541 8 1 8 -0.7873 -0.2370 8 1 9 -0.0936 -0.1233 8 1 10 0.1727 -0.0549 8 1 11 1.9269 0.1560 8 1 12 0.1667 0.2962 8 1 13 1.7508 0.1313 8 2 0 -1.9052 -0.2236 8 2 1 4.2762 0.1206 8 2 2 0.2344 0.2422 8 2 3 1.2825 0.0726 8 2 4 -3.3528 -0.2164 8 2 5 -3.3827 -0.0388 8 2 6 -0.0667 -0.1097 8 2 7 1.3914 -0.1010 8 2 8 -3.0224 0.1725 8 2 9 1.6671 0.2131 8 2 10 -1.1841 -0.1559 8 2 11 0.4528 -0.1814 8 2 12 -1.9558 0.0685 8 2 13 0.4303 0.0280 8 3 0 -2.0086 0.0508 8 3 1 0.9731 -0.0516 8 3 2 -1.6031 -0.0793 8 3 3 2.0545 -0.0237 8 3 4 2.0147 0.1021 8 3 5 0.9526 0.0525 8 3 6 3.4932 0.0012 8 3 7 1.3152 -0.0657 8 3 8 -0.2140 -0.0665 8 3 9 1.6128 0.1148 8 3 10 -2.2668 0.0773 8 3 11 0.3714 -0.0254 8 3 12 -0.2695 0.0879 8 3 13 1.0980 -0.1130 8 4 0 -1.8354 -0.1078 8 4 1 0.2170 0.0946 8 4 2 -1.1276 0.1259 8 4 3 0.5805 0.0227 8 4 4 -3.8675 -0.0758 8 4 5 -4.5413 0.0357 8 4 6 2.8143 0.0013 8 4 7 -0.0629 -0.0938 8 4 8 -0.4549 0.0137 8 4 9 -0.2341 0.1545 8 4 10 -0.1053 -0.0619 8 4 11 -1.2430 -0.1143 8 4 12 -1.7586 0.1331 8 4 13 0.8377 0.0118 8 5 0 0.0461 -0.0873 8 5 1 -0.1445 -0.1465 8 5 2 0.9345 0.0263 8 5 3 2.7931 0.0491 8 5 4 1.5313 -0.0742 8 5 5 -0.3552 0.0018 8 5 6 2.9228 0.0491 8 5 7 -3.3016 0.0239 8 5 8 -1.5861 -0.0472 8 5 9 -2.1235 -0.0468 8 5 10 -0.7254 0.0813 8 5 11 -1.0068 -0.0000 8 5 12 0.6645 -0.0321 8 6 0 -1.7482 -0.1246 8 6 1 -1.4022 0.0408 8 6 2 1.2290 0.0455 8 6 3 1.7171 0.0500 8 6 4 -0.7825 -0.0278 8 6 5 -1.9107 0.0408 8 6 6 4.3938 0.0052 8 6 7 1.3741 -0.0183 8 6 8 2.0621 0.0487 8 6 9 -0.0767 -0.0207 8 6 10 0.1936 0.0846 8 6 11 0.0691 -0.0759 8 6 12 -0.7258 -0.0346 8 7 0 -0.5292 0.0381 8 7 1 -1.8045 0.1486 8 7 2 -1.9793 -0.1077 8 7 3 -0.4985 -0.1466 8 7 4 -1.4096 0.0379 8 7 5 -2.9152 0.0774 8 7 6 -0.1827 0.0017 8 7 7 -4.4756 -0.0921 8 7 8 -2.0734 0.0122 8 7 9 -0.4879 0.0174 8 7 10 -0.1119 0.0209 8 7 11 1.2465 0.0076 8 7 12 1.9205 0.0171 8 8 0 0.0648 -0.0283 8 8 1 -0.3795 0.0620 8 8 2 2.2220 -0.0387 8 8 3 4.2952 -0.0607 8 8 4 0.6429 0.0066 8 8 5 0.8333 0.0152 8 8 6 2.3157 -0.0346 8 8 7 2.6319 -0.0396 8 8 8 -0.0155 0.0230 8 8 9 -1.1162 0.1777 8 8 10 -1.6650 0.0339 8 8 11 0.2350 -0.1224 8 9 0 -0.2503 0.0158 8 9 1 -0.3946 -0.0605 8 9 2 -0.9272 -0.0491 8 9 3 -0.4501 0.0041 8 9 4 -0.8396 -0.0400 8 9 5 0.5125 -0.0338 8 9 6 0.4723 0.0731 8 9 7 -1.0949 0.1070 8 9 8 -0.0525 0.0177 8 9 9 0.4775 -0.0345 8 9 10 1.3019 -0.0686 8 9 11 1.5968 -0.0367 8 10 0 -0.1257 -0.0099 8 10 1 -3.2938 -0.0042 8 10 2 -0.4530 -0.0416 8 10 3 0.8283 -0.0106 8 10 4 -0.6819 0.0909 8 10 5 -1.8698 0.0719 8 10 6 -0.3648 -0.0386 8 10 7 1.0141 -0.0278 8 10 8 -0.4060 -0.0154 8 10 9 -1.4571 0.0487 8 10 10 -1.4736 -0.0289 8 11 0 3.8137 0.0375 8 11 1 0.5820 0.1508 8 11 2 2.0273 -0.0619 8 11 3 0.3995 -0.1538 8 11 4 1.8821 -0.0211 8 11 5 0.9493 0.0724 8 11 6 0.7007 0.0225 8 11 7 1.3830 -0.0228 8 11 8 -0.0056 -0.0090 8 11 9 0.1987 0.0366 8 12 0 0.0210 0.0220 8 12 1 -3.1163 -0.0162 8 12 2 -0.2447 -0.0505 8 12 3 0.6936 -0.0090 8 12 4 3.0778 0.0758 8 12 5 -2.0837 0.0121 8 12 6 0.1722 -0.0373 8 12 7 0.1147 -0.0286 8 12 8 1.0298 -0.0429 8 12 9 -0.5016 -0.0141 8 13 0 0.4190 0.0149 8 13 1 0.9648 -0.0240 8 13 2 -0.3889 -0.0864 8 13 3 -2.2683 0.0389 8 13 4 0.1373 0.1099 8 13 5 -0.7940 -0.0674 8 13 6 0.0643 -0.1139 8 13 7 -0.2351 0.0768 8 13 8 -0.9190 -0.0242 8 14 0 0.3033 -0.0242 8 14 1 1.2887 0.0215 8 14 2 0.1489 0.1351 8 14 3 1.8308 -0.0401 8 14 4 1.9726 -0.1405 8 14 5 -0.4548 -0.0157 8 14 6 -1.3315 0.0373 8 15 0 -1.8659 -0.0400 8 15 1 1.4519 -0.0757 8 15 2 -2.6940 0.1063 8 15 3 -0.0135 -0.0853 8 15 4 -0.8230 -0.0673 8 15 5 2.0628 0.1212 8 16 0 1.3024 0.0750 8 16 1 1.6001 -0.0210 8 16 2 -0.8561 0.0116 8 16 3 -0.2715 -0.0147 9 0 0 5.3681 -0.1427 9 0 2 1.4449 0.0195 9 0 4 4.8935 0.1337 9 0 6 -0.1100 -0.2196 9 0 8 -1.3312 0.1499 9 1 0 1.8418 0.2480 9 1 1 -3.0534 0.0386 9 1 2 2.1507 0.0030 9 1 3 -1.1293 -0.0689 9 1 4 3.2579 -0.2853 9 1 5 -1.9608 0.0131 9 1 6 2.1660 0.4653 9 1 7 0.1070 0.1274 9 1 8 1.3627 -0.3748 9 1 9 2.6323 -0.3381 9 2 0 2.8591 -0.1446 9 2 1 -2.4542 -0.2660 9 2 2 0.4440 0.1275 9 2 3 -2.9400 0.3497 9 2 4 2.6739 0.0112 9 2 5 -3.0821 -0.2280 9 2 6 0.7458 -0.0926 9 2 7 -2.5731 0.1001 9 2 8 0.3424 0.1531 9 2 9 -0.0176 -0.0357 9 3 0 2.1936 0.1371 9 3 1 -1.0706 0.0412 9 3 2 2.9738 -0.0693 9 3 3 0.8822 -0.0449 9 3 4 1.2655 -0.0057 9 3 5 -2.0042 0.0101 9 3 6 1.3944 0.0945 9 3 7 -1.4484 -0.0583 9 3 8 1.2348 -0.0545 9 4 0 0.3190 -0.0957 9 4 1 -2.1101 0.0278 9 4 2 -1.8907 0.0285 9 4 3 -2.1432 0.1594 9 4 4 1.1979 -0.0126 9 4 5 1.2555 -0.1233 9 4 6 -0.0359 -0.0287 9 4 7 -0.6564 -0.0438 9 4 8 2.1397 0.1291 9 5 0 0.4414 -0.0020 9 5 1 -1.6525 0.0723 9 5 2 1.0878 -0.0890 9 5 3 0.1218 -0.0241 9 5 4 -1.8867 0.0167 9 5 5 1.8491 -0.0426 9 5 6 -1.3298 0.0339 9 5 7 1.5776 0.0919 9 5 8 0.1058 -0.0641 9 6 0 0.5467 -0.0811 9 6 1 0.1458 -0.0229 9 6 2 0.0456 0.0500 9 6 3 -1.4710 0.0683 9 6 4 -1.1673 -0.0296 9 6 5 2.4331 -0.0985 9 6 6 -2.4344 0.0046 9 6 7 -0.0871 0.1470 9 7 0 0.6957 -0.0347 9 7 1 0.3437 -0.1288 9 7 2 1.9684 0.0063 9 7 3 0.6053 0.0139 9 7 4 -0.1392 -0.0140 9 7 5 0.6221 -0.0188 9 7 6 -1.0011 -0.0013 9 7 7 0.6391 0.0763 9 8 0 0.1247 -0.1379 9 8 1 -0.2807 -0.0390 9 8 2 0.1325 0.1578 9 8 3 -3.3761 0.0972 9 8 4 -0.2483 -0.0644 9 8 5 1.5390 -0.0181 9 8 6 -0.4427 -0.0242 9 9 0 0.1212 0.0829 9 9 1 -1.3626 -0.0102 9 9 2 1.8779 0.0224 9 9 3 -1.2836 -0.0007 9 9 4 1.4183 -0.1559 9 9 5 -0.9503 -0.0432 9 10 0 -0.1317 -0.0632 9 10 1 1.5409 -0.0959 9 10 2 0.2423 0.0315 9 10 3 -2.1309 -0.0222 9 10 4 1.6838 -0.0593 9 11 0 -2.6335 0.0335 9 11 1 -1.6134 0.0126 9 11 2 0.4677 0.0490 0 0 0 0.0 0.0 ; _shelx_fab_checksum 11320 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Ca01 Ca 1.12177(7) 0.22081(3) 0.19661(3) 0.02520(16) Uani 1 1 d . . . . . Ca02 Ca 0.26919(8) 0.63969(3) 0.23169(3) 0.02996(17) Uani 1 1 d . . . . . Ca03 Ca 0.89976(9) 0.36762(3) 0.15850(3) 0.03300(18) Uani 1 1 d . . . . . O004 O 0.9013(3) 0.24733(10) 0.61545(11) 0.0308(5) Uani 1 1 d . . . . . O005 O 1.0593(3) 0.63413(10) 0.32214(11) 0.0297(5) Uani 1 1 d . . . . . O006 O 0.9384(3) 0.21185(10) 0.29457(11) 0.0308(5) Uani 1 1 d . . . . . O007 O 0.3142(3) 0.29369(10) 0.60922(11) 0.0323(5) Uani 1 1 d . . . . . O008 O 0.7184(3) 0.63414(10) 0.26974(12) 0.0327(5) Uani 1 1 d . . . . . O009 O 0.3076(3) 0.26679(10) 0.28546(12) 0.0325(5) Uani 1 1 d . . . . . O00A O 1.1761(3) 0.32538(10) 0.15147(12) 0.0330(5) Uani 1 1 d . . . . . O00B O 0.9756(3) 0.42783(10) 0.47394(12) 0.0374(6) Uani 1 1 d . . . . . O00C O 0.9485(3) 0.30434(11) 0.25865(11) 0.0343(5) Uani 1 1 d . . . . . O00D O 0.2941(3) 0.21686(11) 0.53710(12) 0.0385(6) Uani 1 1 d . . . . . O00E O 0.3723(3) 0.71073(11) 0.31647(13) 0.0389(6) Uani 1 1 d . . . . . H00A H 0.467570 0.697738 0.337127 0.058 Uiso 1 1 d GR . . . . H00B H 0.301706 0.713155 0.349919 0.058 Uiso 1 1 d GR . . . . O00F O 0.6342(3) 0.44375(11) 0.48058(12) 0.0395(6) Uani 1 1 d . . . . . O00G O 0.4438(3) 0.69185(12) 0.16127(12) 0.0405(6) Uani 1 1 d . . . . . O00H O 0.3566(3) 0.36199(11) 0.26109(13) 0.0401(6) Uani 1 1 d . . . . . O00I O 1.0838(3) 0.55553(11) 0.25594(13) 0.0397(6) Uani 1 1 d . . . . . O00J O 0.8457(4) 0.17404(11) 0.54348(13) 0.0442(6) Uani 1 1 d . . . . . O00K O 0.4834(3) 0.58403(12) 0.28742(17) 0.0491(7) Uani 1 1 d . . . . . O00M O 1.0445(4) 0.43291(13) 0.23757(15) 0.0534(7) Uani 1 1 d . . . . . H00C H 1.045570 0.470247 0.221315 0.080 Uiso 1 1 d GR . . . . H00D H 1.154648 0.423660 0.242094 0.080 Uiso 1 1 d GR . . . . C00N C 0.9187(4) 0.28867(14) 0.37710(16) 0.0280(6) Uani 1 1 d . . . . . O00O O 0.6221(4) 0.33484(17) 0.1770(2) 0.0699(9) Uani 1 1 d . . . . . H00E H 0.621241 0.299404 0.201686 0.105 Uiso 1 1 d GR . . . . H00F H 0.564364 0.360406 0.205409 0.105 Uiso 1 1 d GR . . . . C00P C 0.8812(4) 0.22758(15) 0.55515(17) 0.0318(7) Uani 1 1 d . . . . . C00Q C 0.3269(4) 0.27063(15) 0.55101(17) 0.0302(7) Uani 1 1 d . . . . . C00R C 0.8933(4) 0.46847(14) 0.43174(16) 0.0315(7) Uani 1 1 d . . . . . C00S C 0.9329(4) 0.26767(15) 0.30508(16) 0.0292(6) Uani 1 1 d . . . . . C00T C 0.8979(4) 0.24911(14) 0.43016(16) 0.0295(6) Uani 1 1 d . . . . . H00T H 0.881264 0.208090 0.420868 0.035 Uiso 1 1 calc R . . . . C00U C 0.9016(4) 0.26961(14) 0.49701(16) 0.0289(6) Uani 1 1 d . . . . . C00V C 0.3861(4) 0.30938(15) 0.49503(16) 0.0302(7) Uani 1 1 d . . . . . C00W C 1.0203(4) 0.58151(14) 0.30497(16) 0.0296(7) Uani 1 1 d . . . . . C00X C 0.9394(4) 0.34909(15) 0.39074(17) 0.0309(7) Uani 1 1 d . . . . . H00X H 0.950438 0.376561 0.354623 0.037 Uiso 1 1 calc R . . . . C00Y C 0.9263(4) 0.32961(15) 0.51091(16) 0.0305(7) Uani 1 1 d . . . . . H00Y H 0.931075 0.343696 0.556456 0.037 Uiso 1 1 calc R . . . . C00Z C 0.3488(4) 0.29459(14) 0.42700(17) 0.0295(6) Uani 1 1 d . . . . . H00Z H 0.287788 0.259318 0.415914 0.035 Uiso 1 1 calc R . . . . C010 C 0.4787(4) 0.36013(15) 0.51123(17) 0.0323(7) Uani 1 1 d . . . . . H010 H 0.502889 0.370570 0.557472 0.039 Uiso 1 1 calc R . . . . C011 C 0.9068(4) 0.54643(14) 0.34859(16) 0.0292(6) Uani 1 1 d . . . . . C012 C 0.4007(4) 0.33141(15) 0.37562(17) 0.0304(7) Uani 1 1 d . . . . . C013 C 0.9437(4) 0.36844(14) 0.45723(17) 0.0303(7) Uani 1 1 d . . . . . C014 C 0.7193(4) 0.47600(15) 0.43275(17) 0.0335(7) Uani 1 1 d . . . . . C015 C 0.6401(4) 0.51704(15) 0.39057(17) 0.0340(7) Uani 1 1 d . . . . . H015 H 0.521107 0.521483 0.390942 0.041 Uiso 1 1 calc R . . . . C016 C 0.7307(4) 0.55224(14) 0.34727(17) 0.0308(7) Uani 1 1 d . . . . . C017 C 0.3513(4) 0.31864(15) 0.30263(17) 0.0319(7) Uani 1 1 d . . . . . C018 C 0.9854(4) 0.50380(14) 0.39029(16) 0.0315(7) Uani 1 1 d . . . . . H018 H 1.104330 0.498978 0.390184 0.038 Uiso 1 1 calc R . . . . C019 C 0.5359(4) 0.39560(15) 0.45949(17) 0.0327(7) Uani 1 1 d . . . . . C01A C 0.6383(4) 0.59403(14) 0.29850(18) 0.0322(7) Uani 1 1 d . . . . . C01B C 0.4964(4) 0.38220(15) 0.39165(17) 0.0323(7) Uani 1 1 d . . . . . H01B H 0.533714 0.407182 0.356577 0.039 Uiso 1 1 calc R . . . . O2 O 1.0291(8) 0.43587(19) 0.0759(2) 0.1036(16) Uani 1 1 d . . . . . O3 O 0.7181(6) 0.4551(2) 0.1491(3) 0.1000(14) Uani 1 1 d . U . . . O6 O 0.3083(8) 0.5697(3) 0.1419(3) 0.0580(16) Uani 0.5 1 d . . P . . O7 O 0.1941(12) 0.6002(3) 0.1200(3) 0.072(2) Uani 0.5 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca01 0.0242(3) 0.0259(3) 0.0255(3) -0.0001(2) 0.0022(2) 0.0004(2) Ca02 0.0272(3) 0.0296(3) 0.0334(4) 0.0022(3) 0.0046(3) 0.0003(2) Ca03 0.0346(4) 0.0315(3) 0.0329(4) -0.0019(3) 0.0027(3) 0.0035(3) O004 0.0313(11) 0.0349(12) 0.0262(11) -0.0004(9) 0.0010(9) -0.0022(9) O005 0.0312(11) 0.0267(11) 0.0314(11) 0.0016(9) 0.0028(9) -0.0014(9) O006 0.0305(11) 0.0327(12) 0.0297(11) -0.0058(9) 0.0044(9) -0.0012(9) O007 0.0297(11) 0.0385(12) 0.0289(11) -0.0018(10) 0.0041(9) -0.0047(9) O008 0.0342(12) 0.0294(12) 0.0341(12) 0.0028(9) -0.0004(10) -0.0049(9) O009 0.0336(12) 0.0326(12) 0.0308(12) -0.0006(9) -0.0023(9) -0.0022(9) O00A 0.0326(11) 0.0336(12) 0.0332(12) -0.0014(9) 0.0039(9) 0.0007(9) O00B 0.0546(15) 0.0265(11) 0.0304(12) 0.0012(9) -0.0046(11) -0.0029(10) O00C 0.0413(13) 0.0357(12) 0.0260(11) 0.0010(10) 0.0027(10) 0.0006(10) O00D 0.0487(14) 0.0330(13) 0.0343(13) 0.0008(10) 0.0076(11) -0.0057(11) O00E 0.0277(11) 0.0483(15) 0.0408(13) -0.0074(11) 0.0030(10) 0.0011(10) O00F 0.0519(15) 0.0378(13) 0.0297(12) -0.0013(10) 0.0093(11) -0.0164(11) O00G 0.0348(12) 0.0500(15) 0.0370(13) 0.0037(11) 0.0036(10) -0.0098(11) O00H 0.0485(15) 0.0385(13) 0.0328(13) 0.0030(10) -0.0021(11) -0.0102(11) O00I 0.0432(13) 0.0348(13) 0.0425(14) -0.0075(11) 0.0150(11) -0.0064(10) O00J 0.0652(17) 0.0329(13) 0.0346(13) 0.0005(10) 0.0050(12) -0.0114(12) O00K 0.0269(12) 0.0369(14) 0.083(2) 0.0136(14) -0.0033(12) -0.0002(10) O00M 0.0655(19) 0.0418(15) 0.0516(17) -0.0035(13) -0.0087(14) 0.0021(13) C00N 0.0242(14) 0.0319(16) 0.0277(15) -0.0004(12) 0.0002(12) 0.0025(12) O00O 0.0499(18) 0.068(2) 0.093(3) -0.010(2) 0.0173(17) 0.0019(16) C00P 0.0319(16) 0.0333(17) 0.0305(16) -0.0004(13) 0.0025(13) -0.0015(13) C00Q 0.0256(15) 0.0352(17) 0.0302(16) -0.0007(13) 0.0044(12) -0.0034(12) C00R 0.0453(18) 0.0254(15) 0.0235(14) -0.0030(12) -0.0002(13) -0.0005(13) C00S 0.0239(14) 0.0345(16) 0.0293(16) -0.0024(13) 0.0028(12) -0.0003(12) C00T 0.0285(15) 0.0307(16) 0.0292(15) -0.0026(13) 0.0004(12) -0.0036(12) C00U 0.0277(15) 0.0317(16) 0.0272(15) 0.0009(13) 0.0012(12) -0.0008(12) C00V 0.0284(15) 0.0326(16) 0.0299(16) -0.0022(13) 0.0039(12) 0.0013(12) C00W 0.0263(15) 0.0326(16) 0.0296(16) 0.0003(13) -0.0017(12) -0.0001(12) C00X 0.0313(16) 0.0334(16) 0.0282(15) 0.0021(13) 0.0016(13) 0.0001(13) C00Y 0.0317(15) 0.0328(16) 0.0270(15) -0.0003(13) 0.0005(12) 0.0012(13) C00Z 0.0252(14) 0.0281(15) 0.0353(17) 0.0006(13) 0.0027(12) -0.0011(12) C010 0.0336(16) 0.0349(17) 0.0286(16) -0.0007(13) 0.0038(13) -0.0018(13) C011 0.0341(16) 0.0258(15) 0.0278(15) -0.0026(12) 0.0032(13) -0.0027(12) C012 0.0253(15) 0.0326(16) 0.0336(17) -0.0028(13) 0.0039(12) 0.0008(12) C013 0.0324(16) 0.0282(15) 0.0303(16) 0.0001(13) 0.0021(13) -0.0003(12) C014 0.0420(18) 0.0289(16) 0.0300(16) -0.0040(13) 0.0067(14) -0.0101(14) C015 0.0337(16) 0.0343(17) 0.0346(17) -0.0018(14) 0.0069(14) -0.0041(13) C016 0.0308(15) 0.0254(15) 0.0363(17) -0.0002(13) 0.0020(13) 0.0000(12) C017 0.0267(15) 0.0357(17) 0.0335(17) 0.0014(13) 0.0025(13) -0.0003(13) C018 0.0323(16) 0.0304(16) 0.0317(16) -0.0025(13) 0.0009(13) 0.0004(13) C019 0.0340(16) 0.0291(16) 0.0354(17) -0.0008(13) 0.0064(14) -0.0037(13) C01A 0.0279(15) 0.0290(16) 0.0399(18) -0.0023(14) 0.0034(13) 0.0022(12) C01B 0.0344(16) 0.0329(16) 0.0299(16) 0.0011(13) 0.0045(13) -0.0039(13) O2 0.177(5) 0.067(3) 0.070(3) 0.013(2) 0.024(3) 0.005(3) O3 0.099(2) 0.093(2) 0.106(2) -0.0011(16) -0.0084(16) 0.0080(16) O6 0.061(4) 0.053(4) 0.062(4) -0.027(3) 0.026(3) -0.011(3) O7 0.111(6) 0.062(4) 0.043(3) -0.004(3) 0.006(4) -0.024(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Ca Ca 0.2262 0.3064 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O004 Ca01 Ca02 79.46(6) 4_565 2_645 ? O004 Ca01 O005 74.76(8) 4_565 2_745 ? O004 Ca01 O006 95.96(8) 4_565 . ? O004 Ca01 O009 137.10(8) 4_565 1_655 ? O004 Ca01 O00A 68.09(8) 4_565 . ? O004 Ca01 O00C 73.73(7) 4_565 . ? O005 Ca01 Ca02 38.00(5) 2_745 2_645 ? O005 Ca01 O006 71.83(7) 2_745 . ? O005 Ca01 O009 140.50(8) 2_745 1_655 ? O005 Ca01 O00A 142.31(8) 2_745 . ? O005 Ca01 O00C 108.68(8) 2_745 . ? O006 Ca01 Ca02 34.62(5) . 2_645 ? O006 Ca01 O00A 117.39(8) . . ? O006 Ca01 O00C 50.52(7) . . ? O007 Ca01 Ca02 138.10(6) 4_665 2_645 ? O007 Ca01 O004 91.88(8) 4_665 4_565 ? O007 Ca01 O005 100.12(8) 4_665 2_745 ? O007 Ca01 O006 166.74(8) 4_665 . ? O007 Ca01 O008 74.83(8) 4_665 2_745 ? O007 Ca01 O009 100.84(8) 4_665 1_655 ? O007 Ca01 O00A 75.51(8) 4_665 . ? O007 Ca01 O00C 142.53(8) 4_665 . ? O008 Ca01 Ca02 86.48(6) 2_745 2_645 ? O008 Ca01 O004 141.03(8) 2_745 4_565 ? O008 Ca01 O005 71.94(8) 2_745 2_745 ? O008 Ca01 O006 92.43(8) 2_745 . ? O008 Ca01 O009 81.81(8) 2_745 1_655 ? O008 Ca01 O00A 138.30(8) 2_745 . ? O008 Ca01 O00C 136.50(8) 2_745 . ? O009 Ca01 Ca02 113.37(6) 1_655 2_645 ? O009 Ca01 O006 80.57(8) 1_655 . ? O009 Ca01 O00A 75.74(8) 1_655 . ? O009 Ca01 O00C 71.41(8) 1_655 . ? O00A Ca01 Ca02 134.67(5) . 2_645 ? O00A Ca01 O00C 67.04(7) . . ? O00C Ca01 Ca02 74.18(5) . 2_645 ? O005 Ca02 Ca01 36.89(5) 1_455 2_655 ? O005 Ca02 C00W 26.60(8) 1_455 1_455 ? O006 Ca02 Ca01 36.86(5) 2_655 2_655 ? O006 Ca02 O005 72.94(8) 2_655 1_455 ? O006 Ca02 O00E 84.41(8) 2_655 . ? O006 Ca02 O00I 98.97(9) 2_655 1_455 ? O006 Ca02 C00W 86.13(9) 2_655 1_455 ? O006 Ca02 O6 114.1(2) 2_655 . ? O006 Ca02 O7 85.3(2) 2_655 . ? O00E Ca02 Ca01 71.95(6) . 2_655 ? O00E Ca02 O005 75.93(8) . 1_455 ? O00E Ca02 O00I 123.98(9) . 1_455 ? O00E Ca02 C00W 100.07(9) . 1_455 ? O00G Ca02 Ca01 119.02(7) . 2_655 ? O00G Ca02 O005 152.51(9) . 1_455 ? O00G Ca02 O006 87.26(9) . 2_655 ? O00G Ca02 O00E 83.48(9) . . ? O00G Ca02 O00I 152.16(9) . 1_455 ? O00G Ca02 O00K 96.26(10) . . ? O00G Ca02 C00W 172.14(9) . 1_455 ? O00G Ca02 O6 77.83(17) . . ? O00G Ca02 O7 76.75(19) . . ? O00I Ca02 Ca01 78.29(6) 1_455 2_655 ? O00I Ca02 O005 52.92(7) 1_455 1_455 ? O00I Ca02 C00W 26.33(9) 1_455 1_455 ? O00K Ca02 Ca01 130.52(8) . 2_655 ? O00K Ca02 O005 97.70(9) . 1_455 ? O00K Ca02 O006 163.13(10) . 2_655 ? O00K Ca02 O00E 79.62(10) . . ? O00K Ca02 O00I 85.62(9) . 1_455 ? O00K Ca02 C00W 91.29(9) . 1_455 ? O00K Ca02 O6 82.8(2) . . ? O00K Ca02 O7 111.6(2) . . ? C00W Ca02 Ca01 56.37(7) 1_455 2_655 ? O6 Ca02 Ca01 134.84(17) . 2_655 ? O6 Ca02 O005 127.37(15) . 1_455 ? O6 Ca02 O00E 152.70(17) . . ? O6 Ca02 O00I 74.85(16) . 1_455 ? O6 Ca02 C00W 101.05(16) . 1_455 ? O6 Ca02 O7 28.8(2) . . ? O7 Ca02 Ca01 109.6(2) . 2_655 ? O7 Ca02 O005 119.1(2) . 1_455 ? O7 Ca02 O00E 158.09(18) . . ? O7 Ca02 O00I 76.77(18) . 1_455 ? O7 Ca02 C00W 98.47(19) . 1_455 ? O00A Ca03 O004 65.59(7) . 4_565 ? O00A Ca03 O00C 73.08(8) . . ? O00A Ca03 O00J 84.97(9) . 4_565 ? O00A Ca03 O2 78.39(14) . . ? O00A Ca03 O3 148.49(14) . . ? O00C Ca03 O004 72.17(7) . 4_565 ? O00C Ca03 O00J 122.02(8) . 4_565 ? O00C Ca03 O2 146.10(15) . . ? O00J Ca03 O004 49.96(7) 4_565 4_565 ? O00J Ca03 O2 72.23(13) 4_565 . ? O00M Ca03 O004 140.99(9) . 4_565 ? O00M Ca03 O00A 82.63(10) . . ? O00M Ca03 O00C 77.50(9) . . ? O00M Ca03 O00J 152.33(11) . 4_565 ? O00M Ca03 O2 81.08(14) . . ? O00M Ca03 O3 79.33(13) . . ? O00O Ca03 O004 76.77(10) . 4_565 ? O00O Ca03 O00A 138.13(11) . . ? O00O Ca03 O00C 78.68(12) . . ? O00O Ca03 O00J 84.50(12) . 4_565 ? O00O Ca03 O00M 120.69(12) . . ? O00O Ca03 O2 135.17(17) . . ? O00O Ca03 O3 73.33(15) . . ? O2 Ca03 O004 111.98(11) . 4_565 ? O3 Ca03 O004 139.05(12) . 4_565 ? O3 Ca03 O00C 126.77(14) . . ? O3 Ca03 O00J 99.42(13) . 4_565 ? O3 Ca03 O2 73.45(17) . . ? Ca01 O004 Ca03 95.25(8) 4_566 4_566 ? C00P O004 Ca01 140.7(2) . 4_566 ? C00P O004 Ca03 87.44(19) . 4_566 ? Ca01 O005 Ca02 105.11(8) 2_755 1_655 ? C00W O005 Ca01 125.0(2) . 2_755 ? C00W O005 Ca02 91.13(19) . 1_655 ? Ca02 O006 Ca01 108.52(9) 2_645 . ? C00S O006 Ca01 94.14(19) . . ? C00S O006 Ca02 133.4(2) . 2_645 ? C00Q O007 Ca01 132.9(2) . 4_466 ? C01A O008 Ca01 137.1(2) . 2_755 ? C017 O009 Ca01 136.8(2) . 1_455 ? Ca03 O00A Ca01 99.99(8) . . ? C00R O00B C013 114.8(2) . . ? Ca03 O00C Ca01 96.09(8) . . ? C00S O00C Ca01 86.63(19) . . ? C00S O00C Ca03 164.1(2) . . ? Ca02 O00E H00A 110.3 . . ? Ca02 O00E H00B 110.3 . . ? H00A O00E H00B 103.6 . . ? C019 O00F C014 119.4(3) . . ? C00W O00I Ca02 93.32(19) . 1_655 ? C00P O00J Ca03 99.8(2) . 4_566 ? C01A O00K Ca02 131.7(2) . . ? Ca03 O00M H00C 110.9 . . ? Ca03 O00M H00D 110.7 . . ? H00C O00M H00D 103.0 . . ? C00T C00N C00S 121.6(3) . . ? C00T C00N C00X 119.9(3) . . ? C00X C00N C00S 118.3(3) . . ? Ca03 O00O H00E 112.2 . . ? Ca03 O00O H00F 112.8 . . ? H00E O00O H00F 101.5 . . ? O004 C00P Ca03 67.13(18) . 4_566 ? O004 C00P C00U 118.6(3) . . ? O00J C00P Ca03 55.38(17) . 4_566 ? O00J C00P O004 121.5(3) . . ? O00J C00P C00U 119.9(3) . . ? C00U C00P Ca03 168.4(2) . 4_566 ? O007 C00Q C00V 117.9(3) . . ? O00D C00Q O007 124.3(3) . . ? O00D C00Q C00V 117.8(3) . . ? O00B C00R C014 120.8(3) . . ? C018 C00R O00B 119.5(3) . . ? C018 C00R C014 119.7(3) . . ? O006 C00S C00N 117.9(3) . . ? O00C C00S O006 122.0(3) . . ? O00C C00S C00N 119.9(3) . . ? C00N C00T H00T 120.0 . . ? C00N C00T C00U 120.0(3) . . ? C00U C00T H00T 120.0 . . ? C00T C00U C00P 120.9(3) . . ? C00Y C00U C00P 118.9(3) . . ? C00Y C00U C00T 120.2(3) . . ? C00Z C00V C00Q 120.4(3) . . ? C010 C00V C00Q 119.6(3) . . ? C010 C00V C00Z 120.0(3) . . ? O005 C00W Ca02 62.27(17) . 1_655 ? O005 C00W C011 119.1(3) . . ? O00I C00W Ca02 60.35(17) . 1_655 ? O00I C00W O005 122.6(3) . . ? O00I C00W C011 118.1(3) . . ? C011 C00W Ca02 172.6(2) . 1_655 ? C00N C00X H00X 120.4 . . ? C013 C00X C00N 119.2(3) . . ? C013 C00X H00X 120.4 . . ? C00U C00Y H00Y 120.6 . . ? C013 C00Y C00U 118.9(3) . . ? C013 C00Y H00Y 120.6 . . ? C00V C00Z H00Z 120.0 . . ? C012 C00Z C00V 120.0(3) . . ? C012 C00Z H00Z 120.0 . . ? C00V C010 H010 120.2 . . ? C00V C010 C019 119.7(3) . . ? C019 C010 H010 120.2 . . ? C016 C011 C00W 124.6(3) . . ? C018 C011 C00W 115.9(3) . . ? C018 C011 C016 119.5(3) . . ? C00Z C012 C017 120.8(3) . . ? C00Z C012 C01B 120.2(3) . . ? C01B C012 C017 119.0(3) . . ? C00X C013 O00B 121.4(3) . . ? C00X C013 C00Y 121.8(3) . . ? C00Y C013 O00B 116.7(3) . . ? O00F C014 C00R 117.6(3) . . ? C015 C014 O00F 122.5(3) . . ? C015 C014 C00R 119.8(3) . . ? C014 C015 H015 119.4 . . ? C014 C015 C016 121.3(3) . . ? C016 C015 H015 119.4 . . ? C011 C016 C01A 121.4(3) . . ? C015 C016 C011 118.8(3) . . ? C015 C016 C01A 119.7(3) . . ? O009 C017 O00H 123.8(3) . . ? O009 C017 C012 119.4(3) . . ? O00H C017 C012 116.9(3) . . ? C00R C018 C011 120.9(3) . . ? C00R C018 H018 119.6 . . ? C011 C018 H018 119.6 . . ? O00F C019 C010 115.5(3) . . ? O00F C019 C01B 123.6(3) . . ? C01B C019 C010 120.9(3) . . ? O008 C01A O00K 124.3(3) . . ? O008 C01A C016 119.7(3) . . ? O00K C01A C016 115.9(3) . . ? C012 C01B H01B 120.4 . . ? C019 C01B C012 119.2(3) . . ? C019 C01B H01B 120.4 . . ? O7 O6 Ca02 76.3(4) . . ? O6 O7 Ca02 74.8(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca01 Ca02 3.9264(9) 2_645 ? Ca01 O004 2.416(2) 4_565 ? Ca01 O005 2.441(2) 2_745 ? Ca01 O006 2.484(2) . ? Ca01 O007 2.382(2) 4_665 ? Ca01 O008 2.403(2) 2_745 ? Ca01 O009 2.457(2) 1_655 ? Ca01 O00A 2.562(2) . ? Ca01 O00C 2.664(2) . ? Ca02 O005 2.504(2) 1_455 ? Ca02 O006 2.353(2) 2_655 ? Ca02 O00E 2.424(3) . ? Ca02 O00G 2.328(2) . ? Ca02 O00I 2.462(2) 1_455 ? Ca02 O00K 2.340(3) . ? Ca02 C00W 2.828(3) 1_455 ? Ca02 O6 2.401(5) . ? Ca02 O7 2.417(7) . ? Ca03 O004 2.725(2) 4_565 ? Ca03 O00A 2.402(2) . ? Ca03 O00C 2.447(2) . ? Ca03 O00J 2.468(3) 4_565 ? Ca03 O00M 2.392(3) . ? Ca03 O00O 2.370(3) . ? Ca03 O2 2.496(4) . ? Ca03 O3 2.443(5) . ? O004 C00P 1.270(4) . ? O005 C00W 1.267(4) . ? O006 C00S 1.275(4) . ? O007 C00Q 1.267(4) . ? O008 C01A 1.256(4) . ? O009 C017 1.260(4) . ? O00B C00R 1.378(4) . ? O00B C013 1.398(4) . ? O00C C00S 1.243(4) . ? O00D C00Q 1.266(4) . ? O00E H00A 0.8892 . ? O00E H00B 0.8883 . ? O00F C014 1.392(4) . ? O00F C019 1.387(4) . ? O00H C017 1.276(4) . ? O00I C00W 1.256(4) . ? O00J C00P 1.257(4) . ? O00K C01A 1.258(4) . ? O00M H00C 0.9002 . ? O00M H00D 0.8985 . ? C00N C00S 1.504(4) . ? C00N C00T 1.389(4) . ? C00N C00X 1.396(5) . ? O00O H00E 0.9343 . ? O00O H00F 0.9381 . ? C00P C00U 1.501(4) . ? C00Q C00V 1.500(5) . ? C00R C014 1.393(5) . ? C00R C018 1.377(5) . ? C00T H00T 0.9500 . ? C00T C00U 1.393(4) . ? C00U C00Y 1.391(5) . ? C00V C00Z 1.397(5) . ? C00V C010 1.387(5) . ? C00W C011 1.501(4) . ? C00X H00X 0.9500 . ? C00X C013 1.378(5) . ? C00Y H00Y 0.9500 . ? C00Y C013 1.384(5) . ? C00Z H00Z 0.9500 . ? C00Z C012 1.387(5) . ? C010 H010 0.9500 . ? C010 C019 1.389(5) . ? C011 C016 1.402(5) . ? C011 C018 1.390(5) . ? C012 C017 1.497(5) . ? C012 C01B 1.400(5) . ? C014 C015 1.373(5) . ? C015 H015 0.9500 . ? C015 C016 1.391(5) . ? C016 C01A 1.507(5) . ? C018 H018 0.9500 . ? C019 C01B 1.389(5) . ? C01B H01B 0.9500 . ? O6 O7 1.199(10) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ca01 O004 C00P Ca03 95.2(3) 4_566 . . 4_566 ? Ca01 O004 C00P O00J 106.0(4) 4_566 . . . ? Ca01 O004 C00P C00U -73.7(4) 4_566 . . . ? Ca01 O005 C00W Ca02 109.41(19) 2_755 . . 1_655 ? Ca01 O005 C00W O00I 107.2(3) 2_755 . . . ? Ca01 O005 C00W C011 -78.9(3) 2_755 . . . ? Ca01 O006 C00S O00C 27.8(3) . . . . ? Ca01 O006 C00S C00N -148.0(2) . . . . ? Ca01 O007 C00Q O00D -35.8(5) 4_466 . . . ? Ca01 O007 C00Q C00V 144.8(2) 4_466 . . . ? Ca01 O008 C01A O00K 119.6(4) 2_755 . . . ? Ca01 O008 C01A C016 -63.6(4) 2_755 . . . ? Ca01 O009 C017 O00H -28.7(5) 1_455 . . . ? Ca01 O009 C017 C012 151.4(2) 1_455 . . . ? Ca01 O00C C00S O006 -25.8(3) . . . . ? Ca01 O00C C00S C00N 150.0(3) . . . . ? Ca02 O005 C00W O00I -2.2(3) 1_655 . . . ? Ca02 O005 C00W C011 171.7(3) 1_655 . . . ? Ca02 O006 C00S O00C -92.6(4) 2_645 . . . ? Ca02 O006 C00S C00N 91.5(3) 2_645 . . . ? Ca02 O00I C00W O005 2.3(3) 1_655 . . . ? Ca02 O00I C00W C011 -171.7(2) 1_655 . . . ? Ca02 O00K C01A O008 -13.6(6) . . . . ? Ca02 O00K C01A C016 169.5(2) . . . . ? Ca03 O004 C00P O00J 10.8(3) 4_566 . . . ? Ca03 O004 C00P C00U -168.8(3) 4_566 . . . ? Ca03 O00C C00S O006 74.7(9) . . . . ? Ca03 O00C C00S C00N -109.5(8) . . . . ? Ca03 O00J C00P O004 -12.2(4) 4_566 . . . ? Ca03 O00J C00P C00U 167.5(2) 4_566 . . . ? Ca03 C00P C00U C00T 56.4(12) 4_566 . . . ? Ca03 C00P C00U C00Y -122.9(11) 4_566 . . . ? O004 C00P C00U C00T 173.4(3) . . . . ? O004 C00P C00U C00Y -5.9(5) . . . . ? O005 C00W C011 C016 79.7(4) . . . . ? O005 C00W C011 C018 -103.3(3) . . . . ? O007 C00Q C00V C00Z -157.7(3) . . . . ? O007 C00Q C00V C010 22.4(5) . . . . ? O00B C00R C014 O00F 3.8(4) . . . . ? O00B C00R C014 C015 179.6(3) . . . . ? O00B C00R C018 C011 -178.1(3) . . . . ? O00D C00Q C00V C00Z 22.9(5) . . . . ? O00D C00Q C00V C010 -157.1(3) . . . . ? O00F C014 C015 C016 174.5(3) . . . . ? O00F C019 C01B C012 177.9(3) . . . . ? O00I C00W C011 C016 -106.1(4) . . . . ? O00I C00W C011 C018 70.9(4) . . . . ? O00J C00P C00U C00T -6.2(5) . . . . ? O00J C00P C00U C00Y 174.5(3) . . . . ? C00N C00T C00U C00P -179.4(3) . . . . ? C00N C00T C00U C00Y -0.1(5) . . . . ? C00N C00X C013 O00B 175.6(3) . . . . ? C00N C00X C013 C00Y -0.7(5) . . . . ? C00P C00U C00Y C013 -179.5(3) . . . . ? C00Q C00V C00Z C012 178.5(3) . . . . ? C00Q C00V C010 C019 179.0(3) . . . . ? C00R O00B C013 C00X 42.7(4) . . . . ? C00R O00B C013 C00Y -140.8(3) . . . . ? C00R C014 C015 C016 -1.1(5) . . . . ? C00S C00N C00T C00U 173.8(3) . . . . ? C00S C00N C00X C013 -173.6(3) . . . . ? C00T C00N C00S O006 -5.3(4) . . . . ? C00T C00N C00S O00C 178.8(3) . . . . ? C00T C00N C00X C013 1.8(5) . . . . ? C00T C00U C00Y C013 1.2(5) . . . . ? C00U C00Y C013 O00B -177.3(3) . . . . ? C00U C00Y C013 C00X -0.9(5) . . . . ? C00V C00Z C012 C017 -175.6(3) . . . . ? C00V C00Z C012 C01B 2.5(5) . . . . ? C00V C010 C019 O00F -177.0(3) . . . . ? C00V C010 C019 C01B 2.4(5) . . . . ? C00W C011 C016 C015 -179.8(3) . . . . ? C00W C011 C016 C01A 2.3(5) . . . . ? C00W C011 C018 C00R -179.1(3) . . . . ? C00X C00N C00S O006 170.0(3) . . . . ? C00X C00N C00S O00C -5.9(4) . . . . ? C00X C00N C00T C00U -1.4(5) . . . . ? C00Z C00V C010 C019 -0.9(5) . . . . ? C00Z C012 C017 O009 -21.3(5) . . . . ? C00Z C012 C017 O00H 158.8(3) . . . . ? C00Z C012 C01B C019 -1.0(5) . . . . ? C010 C00V C00Z C012 -1.6(5) . . . . ? C010 C019 C01B C012 -1.5(5) . . . . ? C011 C016 C01A O008 -16.8(5) . . . . ? C011 C016 C01A O00K 160.3(3) . . . . ? C013 O00B C00R C014 70.3(4) . . . . ? C013 O00B C00R C018 -112.5(3) . . . . ? C014 O00F C019 C010 169.7(3) . . . . ? C014 O00F C019 C01B -9.8(5) . . . . ? C014 C00R C018 C011 -0.9(5) . . . . ? C014 C015 C016 C011 -1.8(5) . . . . ? C014 C015 C016 C01A 176.1(3) . . . . ? C015 C016 C01A O008 165.4(3) . . . . ? C015 C016 C01A O00K -17.5(5) . . . . ? C016 C011 C018 C00R -1.9(5) . . . . ? C017 C012 C01B C019 177.1(3) . . . . ? C018 C00R C014 O00F -173.3(3) . . . . ? C018 C00R C014 C015 2.4(5) . . . . ? C018 C011 C016 C015 3.3(5) . . . . ? C018 C011 C016 C01A -174.6(3) . . . . ? C019 O00F C014 C00R -106.2(4) . . . . ? C019 O00F C014 C015 78.1(4) . . . . ? C01B C012 C017 O009 160.6(3) . . . . ? C01B C012 C017 O00H -19.3(4) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.941 -0.797 -0.203 1258.4 171.3 ? 2 0.000 0.158 0.250 0.0 0.0 ? 3 0.000 0.342 0.750 0.0 0.0 ? 4 0.000 0.658 0.250 0.0 0.0 ? 5 0.000 0.842 0.750 0.0 0.0 ? 6 0.025 0.008 0.000 0.0 -0.0 ? 7 0.025 0.492 0.500 0.0 0.0 ? 8 0.025 0.508 0.490 0.0 0.0 ? 9 0.025 0.992 0.990 0.0 0.0 ? 10 0.075 0.217 0.600 0.0 0.0 ? 11 0.075 0.283 0.100 0.0 0.0 ? 12 0.125 0.233 0.300 0.0 0.0 ? 13 0.125 0.267 0.800 0.0 0.0 ? 14 0.200 0.683 0.330 0.0 0.0 ? 15 0.200 0.817 0.830 0.0 0.0 ? 16 0.250 0.200 0.720 0.0 -0.0 ? 17 0.250 0.300 0.220 0.0 -0.0 ? 18 0.250 0.708 0.860 0.0 0.0 ? 19 0.250 0.792 0.360 0.0 0.0 ? 20 0.275 0.192 0.720 0.0 0.0 ? 21 0.275 0.308 0.220 0.0 0.0 ? 22 0.300 0.225 0.460 0.0 0.0 ? 23 0.300 0.275 0.960 0.0 0.0 ? 24 0.350 0.158 0.300 0.0 0.0 ? 25 0.350 0.342 0.800 0.0 0.0 ? 26 0.400 0.158 0.290 0.0 0.0 ? 27 0.400 0.342 0.790 0.0 0.0 ? 28 0.450 0.158 0.100 0.0 0.0 ? 29 0.450 0.342 0.600 0.0 0.0 ? 30 0.475 0.158 0.190 0.0 0.0 ? 31 0.475 0.342 0.690 0.0 0.0 ? 32 0.487 0.650 0.320 0.0 0.0 ? 33 0.487 0.850 0.820 0.0 0.0 ? 34 0.512 0.150 0.180 0.0 0.0 ? 35 0.500 0.250 0.390 0.0 0.0 ? 36 0.500 0.250 0.890 0.0 0.0 ? 37 0.512 0.350 0.680 0.0 0.0 ? 38 0.500 0.750 0.110 0.0 0.0 ? 39 0.500 0.750 0.610 0.0 0.0 ? 40 0.525 0.658 0.310 0.0 0.0 ? 41 0.525 0.842 0.810 0.0 0.0 ? 42 0.550 0.658 0.400 0.0 0.0 ? 43 0.550 0.842 0.900 0.0 0.0 ? 44 0.600 0.658 0.210 0.0 0.0 ? 45 0.600 0.842 0.710 0.0 0.0 ? 46 0.650 0.658 0.200 0.0 0.0 ? 47 0.650 0.842 0.700 0.0 0.0 ? 48 0.700 0.725 0.040 0.0 0.0 ? 49 0.700 0.775 0.540 0.0 0.0 ? 50 0.725 0.692 0.780 0.0 0.0 ? 51 0.725 0.808 0.280 0.0 0.0 ? 52 0.750 0.208 0.640 0.0 0.0 ? 53 0.750 0.292 0.140 0.0 0.0 ? 54 0.750 0.700 0.780 0.0 -0.0 ? 55 0.750 0.800 0.280 0.0 -0.0 ? 56 0.800 0.183 0.170 0.0 0.0 ? 57 0.800 0.317 0.670 0.0 0.0 ? 58 0.875 0.733 0.200 0.0 0.0 ? 59 0.875 0.767 0.700 0.0 0.0 ? 60 0.925 0.717 0.900 0.0 0.0 ? 61 0.925 0.783 0.400 0.0 0.0 ? 62 0.975 0.008 0.010 0.0 0.0 ? 63 0.975 0.492 0.510 0.0 0.0 ? 64 0.975 0.508 0.500 0.0 -0.0 ? 65 0.975 0.992 0.000 0.0 0.0 ?