#------------------------------------------------------------------------------ #$Date: 2024-07-31 00:26:47 +0300 (Wed, 31 Jul 2024) $ #$Revision: 293593 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/22/1572206.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_1572206 loop_ _publ_author_name 'Bhochiya, Rahul' 'Mondal, Pradip Kumar' 'Shah, Jaimin Balkrishna' _publ_section_title ; A Novel pH-Sensitive Method for the Quantification of Ca+2 Ions by Complexometric Titration with Na3HEDTA ; _journal_name_full 'Analytical Methods' _journal_paper_doi 10.1039/D4AY00782D _journal_year 2024 _chemical_formula_sum 'C40 H96 Ca8 N8 O59' _chemical_formula_weight 1953.88 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 81.259(2) _cell_angle_beta 87.322(2) _cell_angle_gamma 68.522(2) _cell_formula_units_Z 1 _cell_length_a 10.1835(7) _cell_length_b 12.9146(9) _cell_length_c 16.3030(11) _cell_measurement_reflns_used 9704 _cell_measurement_temperature 140(2) _cell_measurement_theta_max 66.77 _cell_measurement_theta_min 4.29 _cell_volume 1971.9(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 140(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 59059 _diffrn_reflns_point_group_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 62.490 _diffrn_reflns_theta_max 62.490 _diffrn_reflns_theta_min 2.742 _exptl_absorpt_coefficient_mu 5.695 _exptl_absorpt_correction_T_max 0.726 _exptl_absorpt_correction_T_min 0.482 _exptl_absorpt_correction_type multi-scan _exptl_crystal_density_diffrn 1.645 _exptl_crystal_description Plate _exptl_crystal_F_000 1024 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.782 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 546 _refine_ls_number_reflns 6121 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0531 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+5.0551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.1440 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5693 _reflns_number_total 6121 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ay00782d1.cif _cod_data_source_block CaEDTA _cod_database_code 1572206 _shelx_shelxl_version_number 2018/3 _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 0.482 _shelx_estimated_absorpt_t_max 0.726 _shelx_res_file ; TITL f1_a-copy(2)_a.res in P-1 1.res created by SHELXL-2018/3 at 12:18:00 on 29-Mar-2023 REM Old TITL f1_a-copy(2)_a.res in P-1 REM SHELXT solution in P-1: R1 0.124, Rweak 0.004, Alpha 0.069 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C52 Ca8 N19 O36 CELL 1.54178 10.1835 12.9146 16.303 81.259 87.322 68.522 ZERR 1 0.0007 0.0009 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H Ca N O DISP $C 0.01916 0.00957 85.93609!source kissel DISP $H -0.00001 0.00000 0.64302!source kissel DISP $Ca 0.36596 1.29368 11269.04559!source kissel DISP $N 0.03298 0.01886 166.49108!source kissel DISP $O 0.05170 0.03357 293.70081!source kissel UNIT 40 96 8 8 59 L.S. 10 PLAN 4 TEMP -133.15 CONF BOND SIZE 0.15 0.1 0.06 LIST 6 MORE -1 BOND $H fmap 2 acta OMIT -2 125 OMIT -1 1 2 OMIT -3 -5 2 OMIT 4 3 5 OMIT 2 3 7 OMIT 1 -3 4 OMIT 3 2 5 OMIT 2 -1 1 OMIT 1 -2 3 OMIT -2 -1 4 OMIT 4 1 3 OMIT -1 0 9 OMIT -6 -1 3 OMIT -4 -1 3 OMIT 1 2 3 OMIT -1 6 5 OMIT 0 5 4 OMIT 2 6 0 OMIT 5 -1 6 REM REM REM WGHT 0.069000 5.055100 FVAR 0.73247 CA01 3 0.500774 0.155291 0.501739 11.00000 0.00664 0.00652 = 0.00794 -0.00201 -0.00056 -0.00199 CA02 3 0.993258 0.654433 1.005355 11.00000 0.00858 0.00652 = 0.00785 -0.00190 -0.00061 -0.00262 CA03 3 0.196910 -0.091142 0.286715 11.00000 0.00980 0.00845 = 0.00891 -0.00159 -0.00170 -0.00448 CA04 3 0.723257 0.397854 0.781584 11.00000 0.01262 0.00886 = 0.00950 -0.00154 -0.00211 -0.00541 O005 5 0.397308 0.048700 0.427075 11.00000 0.00863 0.00892 = 0.01258 -0.00336 -0.00046 -0.00294 O006 5 0.443486 0.440465 0.296788 11.00000 0.01583 0.01058 = 0.01626 0.00126 0.00005 -0.00639 O007 5 0.669706 0.303116 0.682759 11.00000 0.02156 0.01289 = 0.01668 -0.00337 -0.00827 -0.00678 O008 5 0.905096 0.545599 0.926655 11.00000 0.01413 0.00879 = 0.01304 -0.00254 -0.00313 -0.00230 O009 5 0.318466 0.142736 0.592891 11.00000 0.01563 0.01160 = 0.01400 -0.00396 0.00583 -0.00615 O00A 5 1.136669 0.815605 1.189320 11.00000 0.02385 0.01259 = 0.01746 -0.00405 -0.00836 -0.00674 O00B 5 0.632883 0.196785 0.599845 11.00000 0.01528 0.01074 = 0.01630 -0.00421 -0.00754 -0.00306 O00C 5 1.034864 0.798921 0.907314 11.00000 0.01193 0.01334 = 0.01492 0.00125 -0.00302 -0.00477 O00D 5 0.962436 0.928953 0.795691 11.00000 0.01472 0.01159 = 0.01499 0.00212 -0.00156 -0.00595 O00E 5 0.534396 0.300048 0.399617 11.00000 0.00879 0.01252 = 0.01859 0.00152 -0.00179 -0.00200 O00F 5 0.802245 0.646922 1.092433 11.00000 0.01751 0.01190 = 0.01527 -0.00444 0.00626 -0.00663 O00G 5 0.607480 0.727552 1.162765 11.00000 0.01699 0.02113 = 0.02254 -0.00887 0.01026 -0.01043 O00H 5 0.127162 0.223797 0.665177 11.00000 0.01552 0.01873 = 0.02210 -0.00830 0.00877 -0.00841 O00I 5 1.110497 0.706824 1.104941 11.00000 0.02139 0.01046 = 0.01617 -0.00359 -0.00814 -0.00510 O00J 5 0.703023 0.059768 0.419452 11.00000 0.01459 0.01143 = 0.01756 -0.00417 0.00369 -0.00530 AFIX 7 H00A 2 0.697536 -0.002715 0.409034 11.00000 -1.50000 H00B 2 0.698239 0.099776 0.370817 11.00000 -1.50000 AFIX 0 O00K 5 0.207181 0.041592 0.367890 11.00000 0.01599 0.01259 = 0.02554 -0.00518 -0.00831 -0.00610 O00L 5 0.020021 -0.105776 0.378030 11.00000 0.02389 0.03218 = 0.02682 -0.01322 0.00897 -0.01862 AFIX 7 H00C 2 -0.020722 -0.146776 0.360098 11.00000 -1.50000 H00D 2 0.057927 -0.143486 0.425403 11.00000 -1.50000 AFIX 0 O00M 5 0.401773 -0.091888 0.213049 11.00000 0.01532 0.01332 = 0.02707 -0.00570 0.00459 -0.00407 AFIX 7 H00E 2 0.462317 -0.160775 0.215883 11.00000 -1.50000 H00F 2 0.444445 -0.057453 0.237810 11.00000 -1.50000 AFIX 0 O00N 5 0.926268 0.408046 0.711299 11.00000 0.01670 0.01470 = 0.02918 -0.00343 0.00492 -0.00327 AFIX 7 H00G 2 0.993468 0.341466 0.717251 11.00000 -1.50000 H00H 2 0.960212 0.449398 0.735107 11.00000 -1.50000 AFIX 0 O00O 5 0.727501 0.533139 0.858183 11.00000 0.02688 0.01421 = 0.03137 -0.00658 -0.01396 -0.00745 AFIX 6 O00P 5 0.479949 0.949866 0.742115 11.00000 0.02404 0.03142 = 0.01932 -0.00675 -0.00103 -0.01249 H00M 2 0.405428 0.934605 0.757887 11.00000 -1.50000 H00N 2 0.472106 0.965280 0.688321 11.00000 -1.50000 AFIX 0 N00Q 4 0.365997 0.346937 0.563465 11.00000 0.01078 0.01005 = 0.00965 -0.00152 -0.00155 -0.00563 N00R 4 0.845654 0.852892 1.061832 11.00000 0.01119 0.01025 = 0.00907 -0.00139 -0.00135 -0.00448 AFIX 6 O00S 5 0.043383 0.557688 0.747573 11.00000 0.03039 0.03648 = 0.03032 -0.01040 -0.00652 -0.01234 H00O 2 0.069249 0.547390 0.799187 11.00000 -1.50000 H00P 2 0.104829 0.581118 0.719903 11.00000 -1.50000 AFIX 6 O00T 5 0.249585 0.878242 0.750075 11.00000 0.02580 0.03837 = 0.04002 -0.00282 0.00546 -0.01227 H00Q 2 0.270203 0.825806 0.792941 11.00000 -1.50000 H00R 2 0.200750 0.858082 0.717597 11.00000 -1.50000 AFIX 0 N00U 4 0.266855 0.281232 0.421251 11.00000 0.00882 0.00823 = 0.01105 -0.00409 0.00200 -0.00407 AFIX 6 O00V 5 0.068642 0.872472 0.548541 11.00000 0.02554 0.04612 = 0.04296 -0.02088 0.00806 -0.01930 H00S 2 0.002168 0.901308 0.583055 11.00000 -1.50000 H00T 2 0.132255 0.900654 0.555646 11.00000 -1.50000 AFIX 0 N00W 4 0.768203 0.777233 0.916646 11.00000 0.00987 0.00767 = 0.01144 -0.00376 0.00204 -0.00378 AFIX 6 O00X 5 1.200175 0.558575 0.924715 11.00000 0.04511 0.01532 = 0.05202 -0.01596 0.03215 -0.01670 H00I 2 1.202140 0.496689 0.908847 11.00000 -1.50000 H00J 2 1.241926 0.587770 0.885170 11.00000 -1.50000 AFIX 0 C00Y 1 0.600051 0.290050 0.626233 11.00000 0.01597 0.01190 = 0.00944 -0.00083 -0.00207 -0.00945 O00Z 5 0.565958 0.363733 0.881367 11.00000 0.05901 0.07905 = 0.04444 -0.03836 0.03287 -0.05997 AFIX 7 H00K 2 0.498168 0.353350 0.857050 11.00000 -1.50000 H00L 2 0.523487 0.424023 0.904419 11.00000 -1.50000 AFIX 0 C010 1 0.266681 0.431019 0.502044 11.00000 0.01210 0.00521 = 0.01487 -0.00300 -0.00060 0.00020 AFIX 23 H01A 2 0.320016 0.461629 0.459046 11.00000 -1.20000 H01B 2 0.203555 0.493963 0.529763 11.00000 -1.20000 AFIX 0 C011 1 0.440644 0.356714 0.346251 11.00000 0.01341 0.00991 = 0.00942 -0.00494 0.00400 -0.00294 C012 1 0.950648 0.850989 0.848254 11.00000 0.01151 0.00702 = 0.01033 -0.00322 0.00171 -0.00068 C013 1 0.751574 0.931999 0.996159 11.00000 0.01250 0.00662 = 0.01589 -0.00391 -0.00023 0.00007 AFIX 23 H01C 2 0.807845 0.961836 0.954697 11.00000 -1.20000 H01D 2 0.683118 0.996093 1.020504 11.00000 -1.20000 AFIX 0 C014 1 1.072905 0.800667 1.130772 11.00000 0.01715 0.01337 = 0.00861 0.00033 -0.00329 -0.00937 C015 1 0.270694 0.092019 0.400037 11.00000 0.01186 0.00897 = 0.00779 -0.00182 -0.00022 -0.00425 C016 1 0.782690 0.585923 0.894031 11.00000 0.01555 0.01013 = 0.00964 -0.00060 -0.00176 -0.00643 AFIX 6 O017 5 0.300164 0.791999 0.964457 11.00000 0.05646 0.07378 = 0.06005 0.00135 -0.00919 -0.04152 H01Y 2 0.214764 0.791881 0.969485 11.00000 -1.50000 H 2 0.314879 0.814202 0.912934 11.00000 -1.50000 AFIX 0 C018 1 0.948124 0.896710 1.088542 11.00000 0.01472 0.00812 = 0.01691 -0.00389 -0.00370 -0.00470 AFIX 23 H01E 2 0.902944 0.951094 1.127503 11.00000 -1.20000 H01F 2 0.980739 0.936428 1.039843 11.00000 -1.20000 AFIX 0 C019 1 0.827520 0.813085 0.837465 11.00000 0.01282 0.00957 = 0.00783 -0.00014 -0.00042 -0.00298 AFIX 23 H01G 2 0.751633 0.875794 0.805191 11.00000 -1.20000 H01H 2 0.859942 0.749744 0.804794 11.00000 -1.20000 AFIX 0 C01A 1 0.689907 0.706710 0.901168 11.00000 0.01006 0.01177 = 0.01484 -0.00213 -0.00249 -0.00519 AFIX 23 H01I 2 0.634467 0.740497 0.849154 11.00000 -1.20000 H01J 2 0.622437 0.706679 0.946896 11.00000 -1.20000 AFIX 0 C01B 1 0.473723 0.387839 0.587561 11.00000 0.01664 0.00875 = 0.01814 -0.00271 -0.00555 -0.00627 AFIX 23 H01K 2 0.433407 0.441286 0.627792 11.00000 -1.20000 H01L 2 0.503669 0.428050 0.538037 11.00000 -1.20000 AFIX 0 O01C 5 0.372911 0.654273 0.829553 11.00000 0.06268 0.04292 = 0.06847 -0.00750 0.03399 -0.01620 C01D 1 0.721164 0.725926 1.128186 11.00000 0.01587 0.01148 = 0.00803 -0.00131 -0.00065 -0.00301 AFIX 6 O01E 5 0.210574 0.649363 0.634496 11.00000 0.03181 0.04854 = 0.08530 -0.00584 0.00430 -0.01403 H01Z 2 0.288663 0.651660 0.652128 11.00000 -1.50000 HA 2 0.193732 0.693095 0.586971 11.00000 -1.50000 AFIX 0 C01F 1 0.241548 0.221334 0.630404 11.00000 0.01320 0.01048 = 0.00778 -0.00097 0.00041 -0.00304 C01G 1 0.316824 0.318232 0.339685 11.00000 0.01182 0.01118 = 0.00786 -0.00048 -0.00111 -0.00296 AFIX 23 H01M 2 0.237845 0.380975 0.309809 11.00000 -1.20000 H01N 2 0.345956 0.255381 0.306575 11.00000 -1.20000 AFIX 0 C01H 1 0.183016 0.213158 0.409948 11.00000 0.00827 0.01151 = 0.01542 -0.00300 -0.00257 -0.00384 AFIX 23 H01O 2 0.121988 0.248705 0.360187 11.00000 -1.20000 H01P 2 0.120700 0.213315 0.458429 11.00000 -1.20000 AFIX 0 C01I 1 0.178500 0.379913 0.461113 11.00000 0.00705 0.00920 = 0.01343 -0.00331 -0.00095 0.00071 AFIX 23 H01Q 2 0.118169 0.356314 0.503440 11.00000 -1.20000 H01R 2 0.115812 0.437792 0.418650 11.00000 -1.20000 AFIX 0 C01J 1 0.672563 0.875981 0.953607 11.00000 0.00785 0.00933 = 0.01423 -0.00313 -0.00104 0.00047 AFIX 23 H01S 2 0.610902 0.851437 0.994421 11.00000 -1.20000 H01T 2 0.611423 0.931462 0.909336 11.00000 -1.20000 AFIX 0 C01K 1 0.292059 0.317159 0.637380 11.00000 0.01594 0.01571 = 0.01249 -0.00673 0.00304 -0.00709 AFIX 23 H01U 2 0.209608 0.384312 0.647313 11.00000 -1.20000 H01V 2 0.356119 0.295401 0.686035 11.00000 -1.20000 AFIX 0 C01L 1 0.766051 0.825358 1.133777 11.00000 0.01676 0.01566 = 0.01390 -0.00731 0.00383 -0.00770 AFIX 23 H01W 2 0.680636 0.892261 1.139777 11.00000 -1.20000 H01X 2 0.824765 0.808197 1.184358 11.00000 -1.20000 AFIX 0 O01M 5 0.500000 0.500000 1.000000 10.50000 0.05649 0.24560 = 0.15606 -0.15622 -0.01514 -0.02153 HKLF 4 REM f1_a-copy(2)_a.res in P-1 REM wR2 = 0.1440, GooF = S = 1.074, Restrained GooF = 1.074 for all data REM R1 = 0.0531 for 5693 Fo > 4sig(Fo) and 0.0554 for all 6121 data REM 546 parameters refined using 0 restraints END WGHT 0.0690 5.0310 REM Highest difference peak 1.782, deepest hole -0.612, 1-sigma level 0.088 Q1 1 0.2608 0.6160 0.7536 11.00000 0.05 1.78 Q2 1 0.5555 0.3902 1.0370 11.00000 0.05 1.40 Q3 1 0.1825 0.7286 0.5416 11.00000 0.05 0.84 Q4 1 0.4563 0.4814 1.0182 11.00000 0.05 0.71 ; _shelx_res_checksum 61495 _shelx_hkl_file ; -1 0 0 4.60 2.10 -1 0 0 4.60 1.40 -1 0 0 5.10 1.20 1 0 0 2.90 1.90 1 0 0 4.00 1.30 1 0 0 4.00 1.00 1 0 0 5.20 1.20 3 0 0 144.39 12.60 3 0 0 159.88 14.30 -5 0 0 24.00 18.10 5 0 0 32.70 6.70 5 0 0 37.70 8.60 5 0 0 27.00 8.30 -6 0 0 181.78 36.40 -6 0 0 162.58 16.00 6 0 0 179.88 20.50 6 0 0 160.78 16.40 6 0 0 182.88 17.10 6 0 0 133.69 17.10 6 0 0 164.78 19.80 6 0 0 144.19 14.50 -7 0 0 15.90 7.00 -7 0 0 15.50 5.80 -7 0 0 27.90 9.70 -7 0 0 37.40 10.90 -7 0 0 25.60 8.10 -7 0 0 11.30 19.50 -7 0 0 13.10 7.30 -7 0 0 13.10 7.20 -7 0 0 15.50 9.20 7 0 0 31.80 10.60 7 0 0 27.40 7.80 7 0 0 25.10 7.70 7 0 0 14.80 8.50 7 0 0 20.90 8.00 7 0 0 30.10 6.70 7 0 0 18.20 9.00 -8 0 0 66.99 15.50 -8 0 0 66.89 16.60 -8 0 0 52.69 11.50 -8 0 0 87.79 43.10 -8 0 0 85.69 19.80 -8 0 0 41.90 11.50 -8 0 0 66.29 15.60 -8 0 0 57.09 13.00 8 0 0 73.29 15.90 8 0 0 72.39 13.40 8 0 0 62.29 10.90 8 0 0 64.69 10.40 8 0 0 76.29 14.80 8 0 0 88.19 16.70 -9 0 0 525.75 45.90 -9 0 0 489.95 42.20 -9 0 0 396.96 42.40 -9 0 0 459.35 47.00 -9 0 0 407.46 46.30 9 0 0 576.44 48.20 9 0 0 488.35 41.80 9 0 0 535.15 41.50 9 0 0 598.14 46.70 9 0 0 579.84 41.10 -10 0 0 855.31 70.99 -10 0 0 872.41 65.09 -10 0 0 850.91 69.39 -10 0 0 874.91 66.49 -10 0 0 921.31 72.89 10 0 0 807.82 70.69 10 0 0 757.42 66.19 10 0 0 887.51 65.79 10 0 0 948.71 66.69 10 0 0 908.91 70.49 -11 0 0 38.30 11.00 -11 0 0 37.30 6.40 -11 0 0 52.89 11.60 11 0 0 37.00 8.70 11 0 0 33.70 6.10 11 0 0 46.50 6.80 11 -1 0 1003.40 71.99 11 -1 0 1060.59 72.39 -11 1 0 868.81 75.79 10 -1 0 295.17 22.70 10 -1 0 194.08 24.00 10 -1 0 280.17 21.90 10 -1 0 263.27 25.40 -10 1 0 248.48 24.70 -10 1 0 231.68 28.00 -10 1 0 254.17 22.40 -10 1 0 238.78 26.90 9 -1 0 63.09 14.30 9 -1 0 67.99 9.20 9 -1 0 87.39 12.30 9 -1 0 81.09 15.80 9 -1 0 74.39 10.60 -9 1 0 80.19 19.20 -9 1 0 58.69 10.00 -9 1 0 72.89 15.50 -9 1 0 88.89 18.20 -9 1 0 79.79 18.80 -9 1 0 81.09 12.50 -9 1 0 55.79 13.80 -9 1 0 57.89 13.00 8 -1 0 35.80 10.70 8 -1 0 17.10 6.90 8 -1 0 22.70 6.70 8 -1 0 32.10 12.00 8 -1 0 20.10 7.80 8 -1 0 30.60 6.80 -8 1 0 16.40 7.60 -8 1 0 20.80 9.80 -8 1 0 29.10 12.40 -8 1 0 27.40 10.00 -8 1 0 26.50 12.50 -8 1 0 18.40 24.80 -8 1 0 25.90 9.80 -8 1 0 36.60 9.10 -8 1 0 24.90 7.50 7 -1 0 715.83 66.29 7 -1 0 651.03 60.69 7 -1 0 712.93 63.39 7 -1 0 709.63 57.39 7 -1 0 694.23 65.09 7 -1 0 644.04 58.49 7 -1 0 781.22 60.59 -7 1 0 691.83 60.99 -7 1 0 843.62 61.69 -7 1 0 896.61 65.79 -7 1 0 782.02 60.09 -7 1 0 704.53 59.59 -7 1 0 780.32 64.59 -7 1 0 897.31 66.99 -7 1 0 841.42 65.09 6 -1 0 342.57 35.00 6 -1 0 345.87 31.40 6 -1 0 444.36 34.30 6 -1 0 443.96 32.50 6 -1 0 411.36 30.30 -6 1 0 329.37 52.09 -6 1 0 339.07 31.40 -6 1 0 293.17 34.20 5 -1 0 40.90 9.70 5 -1 0 42.90 7.90 5 -1 0 53.39 10.10 -5 1 0 64.19 25.40 -5 1 0 50.19 8.60 4 -1 0 275.57 22.70 4 -1 0 263.77 21.10 4 -1 0 270.87 23.60 -4 1 0 192.38 33.00 -3 1 0 2058.59 176.48 -3 1 0 2518.75 168.28 2 -1 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6.70 7.60 -6 -12 3 9.10 6.60 -6 -12 3 6.30 3.90 -6 -12 3 9.90 4.60 5 12 -3 287.77 30.20 5 12 -3 313.27 30.70 5 12 -3 219.28 32.50 -5 -12 3 289.37 29.60 -5 -12 3 291.37 25.80 -5 -12 3 311.57 25.40 -5 -12 3 325.57 32.60 4 12 -3 -19.20 11.60 4 12 -3 1.70 5.00 4 12 -3 10.00 7.20 4 12 -3 7.80 8.00 -4 -12 3 2.30 3.60 -4 -12 3 4.30 6.60 -4 -12 3 1.00 3.50 -4 -12 3 0.70 5.10 3 12 -3 1250.87 90.19 3 12 -3 979.50 87.49 3 12 -3 1156.58 95.79 3 12 -3 1027.80 97.29 3 12 -3 1125.39 96.39 3 12 -3 1110.29 92.59 -3 -12 3 1194.48 93.89 -3 -12 3 1283.77 87.09 -3 -12 3 1157.98 87.29 -3 -12 3 1270.37 92.49 2 12 -3 48.20 19.40 2 12 -3 16.10 9.00 2 12 -3 18.10 9.40 2 12 -3 18.30 6.00 2 12 -3 25.00 13.00 2 12 -3 16.30 6.70 2 12 -3 28.00 12.60 -2 -12 3 14.30 5.00 -2 -12 3 13.20 8.20 -2 -12 3 26.30 8.70 -2 -12 3 21.70 5.70 1 12 -3 379.36 42.30 1 12 -3 418.86 39.50 1 12 -3 429.46 44.80 1 12 -3 367.46 41.60 1 12 -3 359.06 39.00 1 12 -3 375.46 40.60 1 12 -3 447.56 36.10 -1 -12 3 415.96 36.70 -1 -12 3 379.46 32.80 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11 -3 65.99 15.90 -8 -11 3 113.89 20.00 -8 -11 3 50.69 7.90 -8 -11 3 78.69 17.00 -8 -11 3 65.79 11.10 7 11 -3 15.30 9.70 -7 -11 3 7.90 6.80 -7 -11 3 13.40 5.70 -7 -11 3 10.80 4.30 -7 -11 3 11.30 9.90 -7 -11 3 6.00 7.20 -7 -11 3 8.80 4.30 6 11 -3 527.35 47.50 -6 -11 3 496.25 45.50 -6 -11 3 533.85 40.80 -6 -11 3 509.55 48.20 -6 -11 3 476.65 41.00 5 11 -3 -7.50 11.40 5 11 -3 12.60 7.20 5 11 -3 21.00 10.00 5 11 -3 14.40 11.20 -5 -11 3 15.40 5.20 -5 -11 3 8.20 6.80 -5 -11 3 16.40 9.40 -5 -11 3 16.00 8.40 -5 -11 3 8.20 4.30 4 11 -3 3538.05 268.17 4 11 -3 3069.59 267.17 4 11 -3 3617.74 267.57 4 11 -3 3457.15 261.77 4 11 -3 3761.52 265.97 4 11 -3 3166.78 261.47 -4 -11 3 3950.70 263.17 -4 -11 3 3749.22 265.47 -4 -11 3 3564.74 256.57 -4 -11 3 3632.84 257.47 -4 -11 3 3528.75 261.07 3 11 -3 97.19 17.70 3 11 -3 94.29 21.40 3 11 -3 81.59 24.70 3 11 -3 93.89 22.10 3 11 -3 170.28 23.00 3 11 -3 138.09 18.50 3 11 -3 102.79 16.90 3 11 -3 102.69 13.90 -3 -11 3 128.59 13.40 -3 -11 3 114.59 16.00 -3 -11 3 106.19 12.20 -3 -11 3 92.39 14.80 -3 -11 3 119.79 17.80 2 11 -3 208.68 29.60 2 11 -3 192.68 31.00 2 11 -3 179.58 21.20 2 11 -3 191.28 25.80 2 11 -3 173.18 24.50 2 11 -3 167.08 26.70 2 11 -3 158.18 22.30 2 11 -3 162.68 19.20 2 11 -3 192.38 26.00 -2 -11 3 173.88 20.60 -2 -11 3 171.98 16.80 -2 -11 3 177.08 20.00 -2 -11 3 172.38 22.60 -2 -11 3 179.08 17.60 1 11 -3 8.90 7.30 1 11 -3 17.20 10.50 1 11 -3 7.40 12.20 1 11 -3 13.40 9.90 1 11 -3 8.50 8.00 1 11 -3 19.60 13.20 1 11 -3 11.00 10.00 1 11 -3 35.10 15.70 1 11 -3 9.50 6.40 -1 -11 3 12.90 6.80 -1 -11 3 9.60 4.60 -1 -11 3 12.30 4.60 -1 -11 3 9.40 8.00 -1 -11 3 16.10 7.50 0 11 -3 232.08 24.50 0 11 -3 199.08 28.30 0 11 -3 167.88 23.70 0 11 -3 161.88 25.80 0 11 -3 170.38 20.20 0 11 -3 196.78 27.40 0 11 -3 144.89 22.80 0 -11 3 185.58 20.20 0 -11 3 166.78 17.00 0 -11 3 153.48 16.00 -1 11 -3 12.00 12.60 -1 11 -3 13.40 7.00 -1 11 -3 17.70 10.00 -1 11 -3 12.10 9.20 -1 11 -3 34.10 15.60 -1 11 -3 16.90 10.60 -1 11 -3 25.30 12.10 -1 11 -3 16.20 7.70 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9.20 -7 -11 4 89.49 10.40 -7 -11 4 72.39 16.40 6 11 -4 28.80 11.40 -6 -11 4 16.70 9.70 -6 -11 4 22.30 8.70 -6 -11 4 16.80 5.40 -6 -11 4 15.20 5.20 5 11 -4 643.84 59.39 5 11 -4 748.03 60.69 5 11 -4 568.14 62.09 -5 -11 4 724.93 55.09 -5 -11 4 770.22 63.09 -5 -11 4 711.13 54.29 -5 -11 4 725.03 59.69 4 11 -4 1.60 13.30 4 11 -4 42.50 12.70 4 11 -4 22.50 9.10 4 11 -4 35.50 14.50 4 11 -4 2.40 13.90 -4 -11 4 29.60 6.80 -4 -11 4 34.60 10.40 -4 -11 4 39.20 11.40 -4 -11 4 36.90 12.40 -4 -11 4 37.90 7.50 3 11 -4 83.99 26.80 3 11 -4 110.19 17.80 3 11 -4 90.39 24.10 3 11 -4 66.39 17.50 3 11 -4 89.19 15.60 3 11 -4 85.69 20.30 3 11 -4 100.49 16.20 -3 -11 4 83.89 11.50 -3 -11 4 95.99 14.70 -3 -11 4 101.99 15.00 -3 -11 4 91.89 11.00 -3 -11 4 111.19 17.20 2 11 -4 21.60 7.40 2 11 -4 28.90 10.80 2 11 -4 32.50 10.50 2 11 -4 41.90 13.90 2 11 -4 21.80 14.70 2 11 -4 32.00 17.70 2 11 -4 39.20 17.20 2 11 -4 37.00 12.60 -2 -11 4 40.90 13.30 -2 -11 4 40.50 12.40 -2 -11 4 45.10 11.50 -2 -11 4 35.20 7.30 -2 -11 4 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5.30 6.00 7 10 -9 -2.70 6.90 -7 -10 9 0.00 4.90 -7 -10 9 1.30 6.20 6 10 -9 28.10 10.60 -6 -10 9 15.90 8.20 -6 -10 9 10.60 7.90 5 10 -9 1171.28 87.79 -5 -10 9 1115.89 80.29 -5 -10 9 1155.08 88.49 -5 -10 9 975.90 81.09 -5 -10 9 1077.29 85.99 -5 -10 9 1038.30 80.69 4 10 -9 2.70 5.60 4 10 -9 1.30 4.80 4 10 -9 3.20 4.40 4 10 -9 8.00 8.10 -4 -10 9 5.60 10.90 -4 -10 9 8.00 4.70 -4 -10 9 0.30 3.40 -4 -10 9 1.50 3.50 -4 -10 9 -0.80 8.00 -4 -10 9 4.90 7.20 3 10 -9 470.35 40.50 3 10 -9 541.95 40.00 3 10 -9 492.35 44.70 -3 -10 9 503.35 39.20 -3 -10 9 410.26 42.40 -3 -10 9 474.15 45.40 -3 -10 9 529.85 39.60 -3 -10 9 506.35 38.90 2 10 -9 0.50 4.30 2 10 -9 -2.50 3.90 2 10 -9 3.10 6.90 -2 -10 9 3.20 3.60 -2 -10 9 1.40 5.30 -2 -10 9 -1.50 3.60 -2 -10 9 2.30 5.90 -2 -10 9 0.00 3.10 1 10 -9 969.80 79.79 1 10 -9 1003.60 76.29 1 10 -9 963.70 79.99 1 10 -9 1023.60 77.39 -1 -10 9 1062.79 83.09 -1 -10 9 993.30 80.39 -1 -10 9 1062.89 76.59 -1 -10 9 1059.89 76.09 -1 -10 9 973.60 75.99 0 10 -9 5.30 8.00 0 10 -9 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5.70 5.50 9 7 -9 22.70 6.80 9 7 -9 8.60 10.40 9 7 -9 10.00 5.00 -9 -7 9 17.20 8.60 8 7 -9 513.25 41.90 8 7 -9 482.45 46.10 8 7 -9 524.15 47.80 -8 -7 9 538.05 45.60 7 7 -9 60.39 11.40 7 7 -9 72.49 16.50 7 7 -9 101.09 10.20 7 7 -9 82.39 16.90 -7 -7 9 62.49 14.50 6 7 -9 517.75 44.00 6 7 -9 554.34 51.29 6 7 -9 504.05 43.30 6 7 -9 514.75 42.40 6 7 -9 512.95 41.90 6 7 -9 566.84 50.49 -6 -7 9 512.75 47.70 -6 -7 9 581.94 44.00 -6 -7 9 628.24 50.89 5 7 -9 341.07 29.70 5 7 -9 362.46 30.90 5 7 -9 409.16 38.90 5 7 -9 399.16 32.60 -5 -7 9 350.46 35.80 -5 -7 9 411.96 32.40 -5 -7 9 360.26 37.70 4 7 -9 1786.62 126.49 4 7 -9 1681.63 127.59 4 7 -9 1727.53 134.19 4 7 -9 1786.92 133.99 -4 -7 9 1500.65 130.49 -4 -7 9 1576.74 125.09 -4 -7 9 1758.72 127.29 -4 -7 9 1722.03 126.09 -4 -7 9 1891.21 135.39 3 7 -9 1.10 8.10 3 7 -9 5.80 5.30 3 7 -9 5.40 4.60 3 7 -9 7.60 8.50 -3 -7 9 3.10 7.30 -3 -7 9 6.20 6.80 -3 -7 9 6.20 4.10 -3 -7 9 5.80 4.40 -3 -7 9 7.40 7.10 -3 -7 9 7.30 7.90 -3 -7 9 9.90 5.40 2 7 -9 281.07 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342.17 2 -7 9 5361.66 344.97 2 -7 9 4861.61 336.27 -3 7 -9 16.30 8.20 -3 7 -9 -8.00 7.90 -3 7 -9 5.00 7.40 3 -7 9 6.90 6.30 3 -7 9 5.70 4.60 3 -7 9 10.50 7.80 3 -7 9 9.50 4.60 3 -7 9 10.90 4.80 -4 7 -9 43.20 12.20 -4 7 -9 33.90 14.00 -4 7 -9 59.99 16.10 4 -7 9 63.59 9.40 4 -7 9 45.20 11.10 4 -7 9 53.39 12.70 4 -7 9 59.49 9.00 4 -7 9 62.59 10.30 -5 7 -9 75.39 13.80 -5 7 -9 45.20 11.00 -5 7 -9 62.59 11.60 5 -7 9 75.59 8.70 5 -7 9 82.59 9.30 5 -7 9 70.99 8.00 5 -7 9 60.19 10.00 5 -7 9 48.20 10.90 -6 7 -9 798.62 61.39 -6 7 -9 639.94 57.79 6 -7 9 834.62 56.79 6 -7 9 773.82 56.39 6 -7 9 665.53 58.59 6 -7 9 862.01 57.49 11 6 -9 423.86 34.20 10 6 -9 13.00 4.80 10 6 -9 8.90 2.80 10 6 -9 8.70 5.80 -10 -6 9 15.00 6.00 9 6 -9 346.57 28.00 9 6 -9 264.17 30.30 -9 -6 9 336.37 30.50 8 6 -9 17.30 5.40 8 6 -9 31.00 13.40 8 6 -9 37.20 7.30 8 6 -9 24.00 10.30 8 6 -9 26.20 7.90 -8 -6 9 32.40 10.60 7 6 -9 375.66 40.80 7 6 -9 422.56 43.80 7 6 -9 438.36 36.80 7 6 -9 493.25 39.30 7 6 -9 516.25 45.70 7 6 -9 467.15 36.40 -7 -6 9 455.75 41.80 -7 -6 9 478.95 41.90 6 6 -9 53.69 9.90 6 6 -9 40.80 8.10 6 6 -9 48.70 15.10 6 6 -9 72.49 10.90 6 6 -9 78.39 16.40 6 6 -9 84.49 18.00 -6 -6 9 78.29 10.00 -6 -6 9 52.89 13.10 -6 -6 9 40.40 11.90 5 6 -9 3340.47 237.88 5 6 -9 3194.78 238.98 5 6 -9 3410.86 238.68 5 6 -9 3461.05 247.28 5 6 -9 3351.46 247.18 -5 -6 9 3195.18 238.98 -5 -6 9 3337.87 245.68 -5 -6 9 3034.10 242.78 4 6 -9 90.79 13.80 4 6 -9 99.39 12.20 4 6 -9 84.09 20.00 4 6 -9 65.59 15.80 4 6 -9 94.49 11.10 4 6 -9 118.09 12.90 4 6 -9 122.49 18.80 -4 -6 9 94.39 11.30 -4 -6 9 106.59 12.30 -4 -6 9 80.09 17.50 -4 -6 9 111.49 16.10 -4 -6 9 51.89 23.30 3 6 -9 750.72 59.49 3 6 -9 602.14 57.39 3 6 -9 718.33 51.49 3 6 -9 712.93 52.89 3 6 -9 512.45 58.39 -3 -6 9 657.43 55.89 -3 -6 9 598.84 55.49 -3 -6 9 667.53 51.19 -3 -6 9 608.64 54.89 -3 -6 9 667.73 72.49 -3 -6 9 657.43 52.09 -3 -6 9 663.53 57.99 -3 -6 9 696.33 50.69 2 6 -9 -0.50 6.80 2 6 -9 4.70 4.20 2 6 -9 -0.60 7.10 2 6 -9 -1.40 4.20 2 6 -9 2.70 6.80 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39.50 -8 4 -9 13.00 5.40 -8 4 -9 19.90 7.40 8 -4 9 25.40 5.50 8 -4 9 17.50 4.00 8 -4 9 12.40 3.50 8 -4 9 17.10 5.90 11 3 -9 41.90 5.00 -11 -3 9 44.60 5.50 -11 -3 9 42.10 6.80 10 3 -9 22.50 7.90 10 3 -9 28.50 5.80 10 3 -9 26.50 7.50 -10 -3 9 38.50 11.40 -10 -3 9 23.70 7.80 9 3 -9 6.20 7.90 9 3 -9 2.00 6.90 9 3 -9 7.10 6.30 9 3 -9 5.50 4.50 9 3 -9 6.20 4.90 -9 -3 9 6.30 5.20 -9 -3 9 7.10 5.80 8 3 -9 94.39 16.00 8 3 -9 95.99 12.80 8 3 -9 106.89 20.60 -8 -3 9 84.89 12.90 -8 -3 9 85.39 13.90 -8 -3 9 97.29 14.10 -8 -3 9 91.79 14.40 -8 -3 9 64.69 15.10 7 3 -9 537.95 56.59 7 3 -9 662.93 57.59 7 3 -9 719.23 51.69 7 3 -9 644.64 55.79 7 3 -9 717.73 52.69 -7 -3 9 646.54 53.29 -7 -3 9 591.14 80.19 -7 -3 9 557.24 53.09 -7 -3 9 681.33 54.09 -7 -3 9 643.34 56.49 6 3 -9 383.66 35.80 6 3 -9 371.76 33.20 6 3 -9 384.36 39.10 6 3 -9 388.56 32.30 -6 -3 9 380.76 33.20 -6 -3 9 383.86 55.59 -6 -3 9 329.47 34.00 -6 -3 9 399.76 34.80 -6 -3 9 357.06 31.70 5 3 -9 22.20 7.50 5 3 -9 20.20 5.90 5 3 -9 19.40 5.10 5 3 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2081.79 143.89 4 -3 9 1787.12 142.59 4 -3 9 1889.91 138.29 -5 3 -9 -10.90 7.10 -5 3 -9 -0.80 6.80 5 -3 9 1.90 6.80 5 -3 9 4.60 7.20 5 -3 9 0.40 3.60 5 -3 9 2.10 5.60 5 -3 9 0.80 3.60 -6 3 -9 2480.35 222.58 -6 3 -9 3091.19 222.78 6 -3 9 3220.88 220.18 6 -3 9 2935.51 214.78 6 -3 9 2804.32 221.38 6 -3 9 3196.58 214.58 -7 3 -9 187.58 20.00 -7 3 -9 152.78 20.50 7 -3 9 170.78 16.40 7 -3 9 166.78 15.70 7 -3 9 151.38 19.10 7 -3 9 179.18 21.50 7 -3 9 176.38 17.50 -8 3 -9 7.50 5.10 -8 3 -9 13.10 6.80 8 -3 9 16.90 5.80 8 -3 9 13.30 4.20 8 -3 9 1.40 7.80 8 -3 9 13.30 4.30 8 -3 9 8.90 6.20 -9 3 -9 241.48 20.00 -9 3 -9 208.48 18.30 9 -3 9 189.58 19.40 9 -3 9 221.48 17.10 11 2 -9 143.29 11.40 -11 -2 9 109.09 12.60 -11 -2 9 153.18 11.80 10 2 -9 82.19 9.20 10 2 -9 116.19 19.10 10 2 -9 82.19 10.70 10 2 -9 78.19 12.20 -10 -2 9 75.79 13.40 -10 -2 9 87.19 12.70 -10 -2 9 73.49 9.50 9 2 -9 186.98 17.80 9 2 -9 194.88 20.30 9 2 -9 201.18 18.80 9 2 -9 200.08 22.60 -9 -2 9 193.18 18.10 -9 -2 9 181.68 22.50 -9 -2 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1 1 19 7.50 5.70 -2 -1 -19 13.70 4.70 -2 -1 -19 -0.20 4.50 2 1 19 1.90 4.90 -3 -1 -19 31.50 5.70 -3 -1 -19 19.70 6.60 3 1 19 40.90 8.20 4 1 19 142.99 13.80 3 -2 -19 101.99 12.70 -3 2 19 124.69 12.80 -3 2 19 111.79 13.40 2 -2 -19 83.39 12.70 2 -2 -19 98.19 10.50 2 -2 -19 97.29 10.10 -2 2 19 119.19 14.10 -2 2 19 86.79 12.20 1 -2 -19 211.98 20.00 1 -2 -19 233.28 19.80 1 -2 -19 280.57 24.60 1 -2 -19 203.98 19.50 -1 2 19 238.28 24.00 -1 2 19 230.08 23.70 0 -2 -19 16.90 5.10 0 -2 -19 15.70 7.10 0 -2 -19 12.30 4.80 0 -2 -19 17.70 5.20 0 2 19 22.50 5.90 0 2 19 16.30 7.40 -1 -2 -19 800.62 64.29 -1 -2 -19 838.12 65.39 1 2 19 959.20 66.89 -2 -2 -19 1.60 2.80 -2 -2 -19 -0.10 4.60 -2 -2 -19 5.80 4.10 2 2 19 5.40 5.20 -3 -2 -19 351.96 30.10 3 2 19 409.36 32.50 4 2 19 51.69 8.40 3 -3 -19 0.90 2.90 -3 3 19 4.20 3.40 -3 3 19 1.40 3.40 -3 3 19 -0.60 3.60 2 -3 -19 217.18 24.40 2 -3 -19 307.97 23.30 2 -3 -19 286.67 22.80 -2 3 19 329.07 27.40 -2 3 19 225.88 25.00 -2 3 19 304.37 26.60 1 -3 -19 61.89 8.30 1 -3 -19 58.99 7.60 1 -3 -19 38.50 9.70 1 -3 -19 53.09 6.90 -1 3 19 31.70 7.90 -1 3 19 53.59 11.80 -1 3 19 76.99 12.10 0 -3 -19 1855.31 125.99 0 -3 -19 1764.82 126.19 0 -3 -19 1799.42 126.29 0 3 19 1461.65 130.39 -1 -3 -19 42.20 7.40 -1 -3 -19 28.90 6.00 -1 -3 -19 20.70 7.60 -1 -3 -19 38.90 6.80 1 3 19 47.40 12.10 1 3 19 34.40 6.90 -2 -3 -19 72.19 8.70 -2 -3 -19 78.39 9.50 -2 -3 -19 84.19 13.00 2 3 19 101.29 11.90 -3 -3 -19 55.49 7.50 3 3 19 72.49 10.40 -4 -3 -19 1239.58 93.39 -5 -3 -19 1.50 2.80 5 3 19 -2.00 2.90 3 -4 -19 175.38 16.70 -3 4 19 234.68 19.20 2 -4 -19 92.19 9.50 2 -4 -19 73.79 9.50 -2 4 19 93.59 12.50 -2 4 19 96.49 12.30 1 -4 -19 314.57 24.60 1 -4 -19 331.87 25.30 -1 4 19 234.08 24.60 -1 4 19 278.17 28.30 -1 4 19 352.66 29.00 0 -4 -19 7.40 5.40 0 -4 -19 18.70 5.60 0 -4 -19 20.90 5.50 0 -4 -19 19.80 5.50 0 4 19 18.40 5.70 0 4 19 20.10 7.00 0 4 19 19.40 8.20 -1 -4 -19 15.60 6.90 -1 -4 -19 15.00 5.10 -1 -4 -19 20.80 5.80 -1 -4 -19 21.90 5.70 1 4 19 21.90 8.90 1 4 19 12.30 5.10 -2 -4 -19 12.90 4.40 -2 -4 -19 1.90 5.10 -2 -4 -19 8.10 4.00 -2 -4 -19 15.60 5.10 2 4 19 6.70 6.60 2 4 19 12.40 4.80 2 4 19 3.60 4.40 -3 -4 -19 210.18 19.90 -3 -4 -19 229.88 24.10 -3 -4 -19 277.37 21.60 3 4 19 300.47 22.60 -4 -4 -19 3.10 4.50 -4 -4 -19 3.40 2.90 4 4 19 5.40 4.50 -5 -4 -19 0.50 2.70 5 4 19 3.00 3.50 2 -5 -19 953.00 76.69 -2 5 19 1188.38 79.59 -2 5 19 991.80 79.79 1 -5 -19 -1.00 3.30 1 -5 -19 3.90 3.50 -1 5 19 2.60 3.30 -1 5 19 0.60 3.80 -1 5 19 3.20 4.60 0 -5 -19 28.70 6.20 0 -5 -19 21.60 7.60 0 -5 -19 31.90 6.40 0 -5 -19 23.00 5.40 0 5 19 15.00 5.60 0 5 19 19.40 8.30 0 5 19 25.90 7.20 -1 -5 -19 22.30 5.30 -1 -5 -19 14.80 6.30 -1 -5 -19 18.60 5.40 -1 -5 -19 15.00 4.80 1 5 19 20.80 6.10 1 5 19 8.40 5.10 1 5 19 17.40 7.80 -2 -5 -19 177.18 16.10 -2 -5 -19 185.88 19.80 -2 -5 -19 204.68 16.60 -2 -5 -19 173.58 15.50 2 5 19 141.59 16.90 2 5 19 167.38 20.30 2 5 19 181.78 17.40 -3 -5 -19 0.70 2.90 -3 -5 -19 -0.30 3.80 -3 -5 -19 3.40 3.50 3 5 19 3.30 3.60 3 5 19 -0.50 4.50 -4 -5 -19 77.09 8.00 -4 -5 -19 65.99 10.10 -5 -5 -19 10.20 3.90 5 5 19 7.50 3.40 1 -6 -19 502.55 37.40 -1 6 19 456.85 40.40 0 -6 -19 0.60 3.30 0 -6 -19 -0.30 3.30 0 6 19 0.10 4.30 0 6 19 -1.40 3.40 -1 -6 -19 1032.00 68.09 -1 -6 -19 855.61 67.39 -1 -6 -19 970.80 67.49 1 6 19 750.32 70.89 -2 -6 -19 76.69 8.60 -2 -6 -19 75.19 10.70 -2 -6 -19 74.79 8.80 -2 -6 -19 65.59 8.10 2 6 19 63.89 10.90 2 6 19 66.09 10.00 -3 -6 -19 -0.80 3.50 -3 -6 -19 2.50 3.10 -3 -6 -19 2.10 3.20 3 6 19 0.40 3.90 3 6 19 -0.60 3.30 -4 -6 -19 3.30 3.70 -4 -6 -19 9.70 4.50 -4 -6 -19 3.90 2.40 4 6 19 5.60 3.90 4 6 19 5.30 3.50 0 7 19 123.49 14.00 0 7 19 156.58 15.30 -1 -7 -19 7.60 3.50 -1 -7 -19 0.30 3.60 1 7 19 3.30 3.70 1 7 19 2.70 4.10 -2 -7 -19 6.70 5.20 -2 -7 -19 6.50 4.00 -2 -7 -19 3.90 5.60 -2 -7 -19 11.30 3.90 2 7 19 4.90 4.50 2 7 19 4.80 4.70 -3 -7 -19 3.40 3.90 -3 -7 -19 -1.20 2.50 -3 -7 -19 1.50 4.50 3 7 19 1.00 3.40 3 7 19 2.20 3.30 -4 -7 -19 245.38 23.60 4 7 19 299.07 24.20 -2 -8 -19 -1.00 2.50 2 8 19 -1.90 2.60 1 0 -20 0.80 3.20 -1 0 20 -2.10 3.50 0 0 -20 228.18 23.70 0 0 20 321.77 22.70 -1 0 -20 -0.50 2.70 1 0 20 3.60 2.80 1 0 20 3.40 2.90 1 -1 -20 186.98 18.30 -1 1 20 198.68 17.60 0 -1 -20 16.60 5.50 0 1 20 26.20 6.10 1 1 20 27.00 6.90 1 1 20 26.90 5.00 -2 -1 -20 39.70 6.90 2 1 20 57.09 7.30 1 -2 -20 141.59 11.70 -1 2 20 131.19 13.90 0 -2 -20 581.84 47.20 0 -2 -20 556.34 42.80 0 2 20 618.84 47.30 -1 -2 -20 21.50 6.10 -1 -2 -20 23.80 6.40 1 2 20 26.20 6.40 -2 -2 -20 125.49 12.90 2 2 20 98.39 12.20 1 -3 -20 857.61 63.39 1 -3 -20 867.71 66.39 0 -3 -20 235.78 20.80 0 3 20 198.88 20.60 -1 -3 -20 85.09 14.20 -1 -3 -20 105.99 13.20 -1 -3 -20 104.29 9.50 1 3 20 113.39 13.40 1 3 20 119.39 12.20 -2 -3 -20 9.50 4.10 2 3 20 24.40 6.30 0 -4 -20 346.77 28.30 0 4 20 320.57 31.10 0 4 20 435.16 31.70 -1 -4 -20 2.70 2.50 -1 -4 -20 6.00 3.90 1 4 20 4.80 4.60 -2 -4 -20 28.10 5.90 -2 -4 -20 37.80 8.00 2 4 20 32.10 8.30 -1 -5 -20 283.87 26.70 1 5 20 366.86 29.10 -2 -5 -20 1.30 3.20 -2 -5 -20 4.70 2.50 2 5 20 3.40 3.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 63008 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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 _atom_site_disorder_assembly _atom_site_disorder_group Ca01 Ca 0.50077(6) 0.15529(5) 0.50174(3) 0.00702(18) Uani 1 1 d . . . . . Ca02 Ca 0.99326(6) 0.65443(5) 1.00535(3) 0.00757(18) Uani 1 1 d . . . . . Ca03 Ca 0.19691(6) -0.09114(5) 0.28671(4) 0.00863(18) Uani 1 1 d . . . . . Ca04 Ca 0.72326(6) 0.39785(5) 0.78158(4) 0.00980(18) Uani 1 1 d . . . . . O005 O 0.3973(2) 0.04870(17) 0.42708(13) 0.0099(4) Uani 1 1 d . . . . . O006 O 0.4435(2) 0.44047(18) 0.29679(13) 0.0141(5) Uani 1 1 d . . . . . O007 O 0.6697(2) 0.30312(18) 0.68276(14) 0.0165(5) Uani 1 1 d . . . . . O008 O 0.9051(2) 0.54560(17) 0.92666(13) 0.0123(5) Uani 1 1 d . . . . . O009 O 0.3185(2) 0.14274(18) 0.59289(13) 0.0134(5) Uani 1 1 d . . . . . O00A O 1.1367(2) 0.81561(18) 1.18932(14) 0.0174(5) Uani 1 1 d . . . . . O00B O 0.6329(2) 0.19678(18) 0.59985(13) 0.0141(5) Uani 1 1 d . . . . . O00C O 1.0349(2) 0.79892(18) 0.90731(13) 0.0136(5) Uani 1 1 d . . . . . O00D O 0.9624(2) 0.92895(18) 0.79569(13) 0.0138(5) Uani 1 1 d . . . . . O00E O 0.5344(2) 0.30005(18) 0.39962(14) 0.0142(5) Uani 1 1 d . . . . . O00F O 0.8022(2) 0.64692(18) 1.09243(13) 0.0145(5) Uani 1 1 d . . . . . O00G O 0.6075(2) 0.7276(2) 1.16276(14) 0.0189(5) Uani 1 1 d . . . . . O00H O 0.1272(2) 0.22380(19) 0.66518(14) 0.0179(5) Uani 1 1 d . . . . . O00I O 1.1105(2) 0.70682(18) 1.10494(14) 0.0157(5) Uani 1 1 d . . . . . O00J O 0.7030(2) 0.05977(18) 0.41945(14) 0.0143(5) Uani 1 1 d . . . . . H00A H 0.697536 -0.002715 0.409034 0.021 Uiso 1 1 d R U . . . H00B H 0.698239 0.099776 0.370817 0.021 Uiso 1 1 d R U . . . O00K O 0.2072(2) 0.04159(18) 0.36789(14) 0.0172(5) Uani 1 1 d . . . . . O00L O 0.0200(3) -0.1058(2) 0.37803(16) 0.0245(6) Uani 1 1 d . . . . . H00C H -0.020722 -0.146776 0.360098 0.037 Uiso 1 1 d R U . . . H00D H 0.057927 -0.143486 0.425403 0.037 Uiso 1 1 d R U . . . O00M O 0.4018(2) -0.09189(19) 0.21305(15) 0.0187(5) Uani 1 1 d . . . . . H00E H 0.462317 -0.160775 0.215883 0.028 Uiso 1 1 d R U . . . H00F H 0.444445 -0.057453 0.237810 0.028 Uiso 1 1 d R U . . . O00N O 0.9263(2) 0.4080(2) 0.71130(15) 0.0210(5) Uani 1 1 d . . . . . H00G H 0.993468 0.341466 0.717251 0.032 Uiso 1 1 d R U . . . H00H H 0.960212 0.449398 0.735107 0.032 Uiso 1 1 d R U . . . O00O O 0.7275(3) 0.53314(19) 0.85818(16) 0.0233(6) Uani 1 1 d . . . . . O00P O 0.4799(3) 0.9499(2) 0.74211(15) 0.0239(6) Uani 1 1 d G . . . . H00M H 0.405428 0.934605 0.757887 0.036 Uiso 1 1 d G U . . . H00N H 0.472106 0.965280 0.688321 0.036 Uiso 1 1 d G U . . . N00Q N 0.3660(3) 0.3469(2) 0.56347(15) 0.0096(5) Uani 1 1 d . . . . . N00R N 0.8457(3) 0.8529(2) 1.06183(15) 0.0100(5) Uani 1 1 d . . . . . O00S O 0.0434(3) 0.5577(2) 0.74757(17) 0.0315(6) Uani 1 1 d G . . . . H00O H 0.069249 0.547390 0.799187 0.047 Uiso 1 1 d G U . . . H00P H 0.104829 0.581118 0.719903 0.047 Uiso 1 1 d G U . . . O00T O 0.2496(3) 0.8782(2) 0.75007(18) 0.0351(7) Uani 1 1 d G . . . . H00Q H 0.270203 0.825806 0.792941 0.053 Uiso 1 1 d G U . . . H00R H 0.200750 0.858082 0.717597 0.053 Uiso 1 1 d G U . . . N00U N 0.2669(3) 0.2812(2) 0.42125(15) 0.0089(5) Uani 1 1 d . . . . . O00V O 0.0686(3) 0.8725(2) 0.54854(18) 0.0351(7) Uani 1 1 d G . . . . H00S H 0.002168 0.901308 0.583055 0.053 Uiso 1 1 d G U . . . H00T H 0.132255 0.900654 0.555646 0.053 Uiso 1 1 d G U . . . N00W N 0.7682(3) 0.7772(2) 0.91665(15) 0.0093(5) Uani 1 1 d . . . . . O00X O 1.2002(3) 0.5586(2) 0.92472(19) 0.0357(7) Uani 1 1 d G . . . . H00I H 1.202140 0.496689 0.908847 0.054 Uiso 1 1 d G U . . . H00J H 1.241926 0.587770 0.885170 0.054 Uiso 1 1 d G U . . . C00Y C 0.6001(3) 0.2900(3) 0.62623(19) 0.0112(6) Uani 1 1 d . . . . . O00Z O 0.5660(4) 0.3637(3) 0.88137(19) 0.0487(9) Uani 1 1 d . . . . . H00K H 0.498168 0.353350 0.857050 0.073 Uiso 1 1 d R U . . . H00L H 0.523487 0.424023 0.904419 0.073 Uiso 1 1 d R U . . . C010 C 0.2667(3) 0.4310(2) 0.50204(19) 0.0115(6) Uani 1 1 d . . . . . H01A H 0.320016 0.461629 0.459046 0.014 Uiso 1 1 calc R U . . . H01B H 0.203555 0.493963 0.529763 0.014 Uiso 1 1 calc R U . . . C011 C 0.4406(3) 0.3567(3) 0.34625(18) 0.0110(6) Uani 1 1 d . . . . . C012 C 0.9506(3) 0.8510(2) 0.84825(18) 0.0102(6) Uani 1 1 d . . . . . C013 C 0.7516(3) 0.9320(2) 0.99616(19) 0.0124(6) Uani 1 1 d . . . . . H01C H 0.807845 0.961836 0.954697 0.015 Uiso 1 1 calc R U . . . H01D H 0.683118 0.996093 1.020504 0.015 Uiso 1 1 calc R U . . . C014 C 1.0729(3) 0.8007(3) 1.13077(18) 0.0121(6) Uani 1 1 d . . . . . C015 C 0.2707(3) 0.0920(2) 0.40004(18) 0.0093(6) Uani 1 1 d . . . . . C016 C 0.7827(3) 0.5859(3) 0.89403(18) 0.0113(6) Uani 1 1 d . . . . . O017 O 0.3002(4) 0.7920(3) 0.9645(2) 0.0592(10) Uani 1 1 d G . . . . H01Y H 0.214764 0.791881 0.969485 0.089 Uiso 1 1 d G U . . . H H 0.314879 0.814202 0.912934 0.089 Uiso 1 1 d G U . . . C018 C 0.9481(3) 0.8967(3) 1.0885(2) 0.0127(6) Uani 1 1 d . . . . . H01E H 0.902944 0.951094 1.127503 0.015 Uiso 1 1 calc R U . . . H01F H 0.980739 0.936428 1.039843 0.015 Uiso 1 1 calc R U . . . C019 C 0.8275(3) 0.8131(2) 0.83747(18) 0.0105(6) Uani 1 1 d . . . . . H01G H 0.751633 0.875794 0.805191 0.013 Uiso 1 1 calc R U . . . H01H H 0.859942 0.749744 0.804794 0.013 Uiso 1 1 calc R U . . . C01A C 0.6899(3) 0.7067(3) 0.90117(19) 0.0118(6) Uani 1 1 d . . . . . H01I H 0.634467 0.740497 0.849154 0.014 Uiso 1 1 calc R U . . . H01J H 0.622437 0.706679 0.946896 0.014 Uiso 1 1 calc R U . . . C01B C 0.4737(3) 0.3878(3) 0.5876(2) 0.0138(7) Uani 1 1 d . . . . . H01K H 0.433407 0.441286 0.627792 0.017 Uiso 1 1 calc R U . . . H01L H 0.503669 0.428050 0.538037 0.017 Uiso 1 1 calc R U . . . O01C O 0.3729(4) 0.6543(3) 0.8296(2) 0.0601(10) Uani 1 1 d . . . . . C01D C 0.7212(3) 0.7259(3) 1.12819(18) 0.0123(7) Uani 1 1 d . . . . . O01E O 0.2106(3) 0.6494(3) 0.6345(3) 0.0559(9) Uani 1 1 d G . . . . H01Z H 0.288663 0.651660 0.652128 0.084 Uiso 1 1 d G U . . . HA H 0.193732 0.693095 0.586971 0.084 Uiso 1 1 d G U . . . C01F C 0.2415(3) 0.2213(3) 0.63040(18) 0.0109(6) Uani 1 1 d . . . . . C01G C 0.3168(3) 0.3182(3) 0.33969(18) 0.0107(6) Uani 1 1 d . . . . . H01M H 0.237845 0.380975 0.309809 0.013 Uiso 1 1 calc R U . . . H01N H 0.345956 0.255381 0.306575 0.013 Uiso 1 1 calc R U . . . C01H C 0.1830(3) 0.2132(3) 0.40995(19) 0.0115(6) Uani 1 1 d . . . . . H01O H 0.121988 0.248705 0.360187 0.014 Uiso 1 1 calc R U . . . H01P H 0.120700 0.213315 0.458429 0.014 Uiso 1 1 calc R U . . . C01I C 0.1785(3) 0.3799(2) 0.46111(19) 0.0107(6) Uani 1 1 d . . . . . H01Q H 0.118169 0.356314 0.503440 0.013 Uiso 1 1 calc R U . . . H01R H 0.115812 0.437792 0.418650 0.013 Uiso 1 1 calc R U . . . C01J C 0.6726(3) 0.8760(2) 0.95361(19) 0.0113(6) Uani 1 1 d . . . . . H01S H 0.610902 0.851437 0.994421 0.014 Uiso 1 1 calc R U . . . H01T H 0.611423 0.931462 0.909336 0.014 Uiso 1 1 calc R U . . . C01K C 0.2921(3) 0.3172(3) 0.63738(19) 0.0139(7) Uani 1 1 d . . . . . H01U H 0.209608 0.384312 0.647313 0.017 Uiso 1 1 calc R U . . . H01V H 0.356119 0.295401 0.686035 0.017 Uiso 1 1 calc R U . . . C01L C 0.7661(3) 0.8254(3) 1.1338(2) 0.0145(7) Uani 1 1 d . . . . . H01W H 0.680636 0.892261 1.139777 0.017 Uiso 1 1 calc R U . . . H01X H 0.824765 0.808197 1.184358 0.017 Uiso 1 1 calc R U . . . O01M O 0.500000 0.500000 1.000000 0.148(5) Uani 1 2 d S . 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 0.0066(3) 0.0065(3) 0.0079(3) -0.0020(2) -0.0006(2) -0.0020(2) Ca02 0.0086(3) 0.0065(3) 0.0079(3) -0.0019(2) -0.0006(2) -0.0026(2) Ca03 0.0098(3) 0.0085(3) 0.0089(3) -0.0016(2) -0.0017(2) -0.0045(2) Ca04 0.0126(3) 0.0089(3) 0.0095(3) -0.0015(2) -0.0021(2) -0.0054(2) O005 0.0086(11) 0.0089(10) 0.0126(10) -0.0034(8) -0.0005(8) -0.0029(8) O006 0.0158(11) 0.0106(11) 0.0163(11) 0.0013(9) 0.0000(9) -0.0064(9) O007 0.0216(12) 0.0129(11) 0.0167(11) -0.0034(9) -0.0083(9) -0.0068(9) O008 0.0141(11) 0.0088(10) 0.0130(11) -0.0025(8) -0.0031(9) -0.0023(9) O009 0.0156(11) 0.0116(11) 0.0140(11) -0.0040(9) 0.0058(9) -0.0062(9) O00A 0.0238(12) 0.0126(11) 0.0175(12) -0.0040(9) -0.0084(10) -0.0067(9) O00B 0.0153(11) 0.0107(11) 0.0163(11) -0.0042(9) -0.0075(9) -0.0031(9) O00C 0.0119(11) 0.0133(11) 0.0149(11) 0.0012(9) -0.0030(9) -0.0048(9) O00D 0.0147(11) 0.0116(11) 0.0150(11) 0.0021(9) -0.0016(9) -0.0059(9) O00E 0.0088(11) 0.0125(11) 0.0186(12) 0.0015(9) -0.0018(9) -0.0020(9) O00F 0.0175(11) 0.0119(11) 0.0153(11) -0.0044(9) 0.0063(9) -0.0066(9) O00G 0.0170(12) 0.0211(12) 0.0225(12) -0.0089(10) 0.0103(10) -0.0104(10) O00H 0.0155(12) 0.0187(12) 0.0221(12) -0.0083(10) 0.0088(10) -0.0084(10) O00I 0.0214(12) 0.0105(11) 0.0162(11) -0.0036(9) -0.0081(9) -0.0051(9) O00J 0.0146(11) 0.0114(11) 0.0176(11) -0.0042(9) 0.0037(9) -0.0053(9) O00K 0.0160(11) 0.0126(11) 0.0255(13) -0.0052(9) -0.0083(9) -0.0061(9) O00L 0.0239(13) 0.0322(14) 0.0268(13) -0.0132(11) 0.0090(10) -0.0186(11) O00M 0.0153(11) 0.0133(11) 0.0271(13) -0.0057(10) 0.0046(10) -0.0041(9) O00N 0.0167(12) 0.0147(12) 0.0292(13) -0.0034(10) 0.0049(10) -0.0033(9) O00O 0.0269(13) 0.0142(12) 0.0314(14) -0.0066(10) -0.0140(11) -0.0074(10) O00P 0.0240(13) 0.0314(14) 0.0193(13) -0.0067(11) -0.0010(10) -0.0125(11) N00Q 0.0108(12) 0.0100(12) 0.0096(12) -0.0015(10) -0.0016(10) -0.0056(10) N00R 0.0112(13) 0.0102(12) 0.0091(12) -0.0014(10) -0.0013(10) -0.0045(10) O00S 0.0304(15) 0.0365(16) 0.0303(15) -0.0104(12) -0.0065(12) -0.0123(12) O00T 0.0258(15) 0.0384(16) 0.0400(16) -0.0028(13) 0.0055(12) -0.0123(12) N00U 0.0088(12) 0.0082(12) 0.0111(13) -0.0041(10) 0.0020(10) -0.0041(10) O00V 0.0255(14) 0.0461(17) 0.0430(17) -0.0209(13) 0.0081(12) -0.0193(13) N00W 0.0099(12) 0.0077(12) 0.0114(13) -0.0038(10) 0.0020(10) -0.0038(10) O00X 0.0451(17) 0.0153(13) 0.0520(18) -0.0160(12) 0.0321(14) -0.0167(12) C00Y 0.0160(16) 0.0119(16) 0.0094(14) -0.0008(12) -0.0021(12) -0.0094(13) O00Z 0.059(2) 0.079(2) 0.0444(18) -0.0384(17) 0.0329(16) -0.060(2) C010 0.0121(15) 0.0052(14) 0.0149(16) -0.0030(12) -0.0006(12) 0.0002(12) C011 0.0134(16) 0.0099(15) 0.0094(15) -0.0049(12) 0.0040(12) -0.0029(12) C012 0.0115(15) 0.0070(14) 0.0103(15) -0.0032(12) 0.0017(12) -0.0007(12) C013 0.0125(15) 0.0066(14) 0.0159(16) -0.0039(12) -0.0002(12) 0.0001(12) C014 0.0171(16) 0.0134(16) 0.0086(15) 0.0003(12) -0.0033(12) -0.0094(13) C015 0.0119(15) 0.0090(15) 0.0078(14) -0.0018(11) -0.0002(11) -0.0043(12) C016 0.0156(16) 0.0101(15) 0.0096(15) -0.0006(12) -0.0018(12) -0.0064(13) O017 0.056(2) 0.074(3) 0.060(2) 0.0014(19) -0.0092(18) -0.042(2) C018 0.0147(16) 0.0081(15) 0.0169(16) -0.0039(12) -0.0037(13) -0.0047(12) C019 0.0128(15) 0.0096(15) 0.0078(14) -0.0001(11) -0.0004(12) -0.0030(12) C01A 0.0101(15) 0.0118(15) 0.0148(15) -0.0021(12) -0.0025(12) -0.0052(12) C01B 0.0166(16) 0.0088(15) 0.0181(16) -0.0027(12) -0.0055(13) -0.0063(13) O01C 0.063(2) 0.0429(19) 0.068(2) -0.0075(17) 0.0340(19) -0.0162(17) C01D 0.0159(16) 0.0115(15) 0.0080(15) -0.0013(12) -0.0006(12) -0.0030(13) O01E 0.0318(18) 0.049(2) 0.085(3) -0.0058(18) 0.0043(17) -0.0140(15) C01F 0.0132(16) 0.0105(15) 0.0078(14) -0.0010(12) 0.0004(12) -0.0030(12) C01G 0.0118(15) 0.0112(15) 0.0079(14) -0.0005(12) -0.0011(12) -0.0030(12) C01H 0.0083(14) 0.0115(15) 0.0154(16) -0.0030(12) -0.0026(12) -0.0038(12) C01I 0.0071(14) 0.0092(15) 0.0134(15) -0.0033(12) -0.0009(12) 0.0007(12) C01J 0.0079(14) 0.0093(15) 0.0142(15) -0.0031(12) -0.0010(12) 0.0005(12) C01K 0.0159(16) 0.0157(16) 0.0125(15) -0.0067(12) 0.0030(12) -0.0071(13) C01L 0.0168(16) 0.0157(16) 0.0139(16) -0.0073(13) 0.0038(13) -0.0077(13) O01M 0.056(4) 0.246(11) 0.156(8) -0.156(8) -0.015(4) -0.022(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0192 0.0096 '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 0.3660 1.2937 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0330 0.0189 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0517 0.0336 '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 O009 Ca01 O00B 96.30(8) . . ? O009 Ca01 O00E 135.50(8) . . ? O00B Ca01 O00E 89.73(8) . . ? O009 Ca01 O00J 148.11(8) . . ? O00B Ca01 O00J 95.73(8) . . ? O00E Ca01 O00J 73.89(7) . . ? O009 Ca01 O005 78.99(7) . . ? O00B Ca01 O005 160.77(8) . . ? O00E Ca01 O005 106.78(7) . . ? O00J Ca01 O005 79.96(7) . . ? O009 Ca01 O005 77.55(7) . 2_656 ? O00B Ca01 O005 86.69(7) . 2_656 ? O00E Ca01 O005 146.94(7) . 2_656 ? O00J Ca01 O005 73.79(7) . 2_656 ? O005 Ca01 O005 74.10(8) . 2_656 ? O009 Ca01 N00U 75.06(8) . . ? O00B Ca01 N00U 130.89(8) . . ? O00E Ca01 N00U 68.08(7) . . ? O00J Ca01 N00U 117.15(8) . . ? O005 Ca01 N00U 66.29(7) . . ? O005 Ca01 N00U 135.13(7) 2_656 . ? O009 Ca01 N00Q 67.74(8) . . ? O00B Ca01 N00Q 65.04(7) . . ? O00E Ca01 N00Q 75.37(8) . . ? O00J Ca01 N00Q 143.61(8) . . ? O005 Ca01 N00Q 127.93(7) . . ? O005 Ca01 N00Q 131.14(7) 2_656 . ? N00U Ca01 N00Q 67.10(8) . . ? O009 Ca01 C01F 18.77(8) . . ? O00B Ca01 C01F 86.45(8) . . ? O00E Ca01 C01F 119.73(8) . . ? O00J Ca01 C01F 166.28(8) . . ? O005 Ca01 C01F 93.52(7) . . ? O005 Ca01 C01F 92.86(7) 2_656 . ? N00U Ca01 C01F 70.09(8) . . ? N00Q Ca01 C01F 48.98(8) . . ? O009 Ca01 Ca01 75.23(5) . 2_656 ? O00B Ca01 Ca01 123.11(6) . 2_656 ? O00E Ca01 Ca01 135.31(6) . 2_656 ? O00J Ca01 Ca01 73.44(5) . 2_656 ? O005 Ca01 Ca01 37.68(5) . 2_656 ? O005 Ca01 Ca01 36.43(5) 2_656 2_656 ? N00U Ca01 Ca01 101.66(6) . 2_656 ? N00Q Ca01 Ca01 142.90(6) . 2_656 ? C01F Ca01 Ca01 93.99(6) . 2_656 ? O00I Ca02 O00F 95.64(8) . . ? O00I Ca02 O00C 86.66(8) . . ? O00F Ca02 O00C 134.48(8) . . ? O00I Ca02 O008 163.06(8) . . ? O00F Ca02 O008 81.44(8) . . ? O00C Ca02 O008 107.35(7) . . ? O00I Ca02 O00X 98.19(10) . . ? O00F Ca02 O00X 149.50(8) . . ? O00C Ca02 O00X 73.57(8) . . ? O008 Ca02 O00X 77.44(9) . . ? O00I Ca02 O008 89.70(7) . 2_767 ? O00F Ca02 O008 80.23(7) . 2_767 ? O00C Ca02 O008 145.28(8) . 2_767 ? O008 Ca02 O008 73.37(8) . 2_767 ? O00X Ca02 O008 72.82(8) . 2_767 ? O00I Ca02 N00W 129.03(8) . . ? O00F Ca02 N00W 75.56(8) . . ? O00C Ca02 N00W 68.32(7) . . ? O008 Ca02 N00W 66.60(7) . . ? O00X Ca02 N00W 114.68(10) . . ? O008 Ca02 N00W 135.54(8) 2_767 . ? O00I Ca02 N00R 63.90(8) . . ? O00F Ca02 N00R 66.68(8) . . ? O00C Ca02 N00R 74.01(8) . . ? O008 Ca02 N00R 128.34(8) . . ? O00X Ca02 N00R 143.65(8) . . ? O008 Ca02 N00R 133.86(7) 2_767 . ? N00W Ca02 N00R 66.70(8) . . ? O00I Ca02 Ca02 125.95(6) . 2_767 ? O00F Ca02 Ca02 78.54(5) . 2_767 ? O00C Ca02 Ca02 134.56(6) . 2_767 ? O008 Ca02 Ca02 37.11(5) . 2_767 ? O00X Ca02 Ca02 71.32(6) . 2_767 ? O008 Ca02 Ca02 36.26(5) 2_767 2_767 ? N00W Ca02 Ca02 101.79(6) . 2_767 ? N00R Ca02 Ca02 145.00(6) . 2_767 ? O00I Ca02 Ca04 23.36(5) . 2_767 ? O00F Ca02 Ca04 93.06(6) . 2_767 ? O00C Ca02 Ca04 104.72(5) . 2_767 ? O008 Ca02 Ca04 139.74(5) . 2_767 ? O00X Ca02 Ca04 89.11(8) . 2_767 ? O008 Ca02 Ca04 66.41(5) 2_767 2_767 ? N00W Ca02 Ca04 150.30(6) . 2_767 ? N00R Ca02 Ca04 83.60(5) . 2_767 ? Ca02 Ca02 Ca04 102.65(2) 2_767 2_767 ? O00L Ca03 O00K 84.07(8) . . ? O00L Ca03 O00M 170.47(9) . . ? O00K Ca03 O00M 92.80(8) . . ? O00L Ca03 O00A 93.45(9) . 1_444 ? O00K Ca03 O00A 165.15(8) . 1_444 ? O00M Ca03 O00A 91.83(8) . 1_444 ? O00L Ca03 O00D 92.37(9) . 2_666 ? O00K Ca03 O00D 83.15(8) . 2_666 ? O00M Ca03 O00D 96.20(8) . 2_666 ? O00A Ca03 O00D 82.33(8) 1_444 2_666 ? O00L Ca03 O00B 87.28(9) . 2_656 ? O00K Ca03 O00B 73.49(7) . 2_656 ? O00M Ca03 O00B 83.19(8) . 2_656 ? O00A Ca03 O00B 121.10(8) 1_444 2_656 ? O00D Ca03 O00B 156.56(8) 2_666 2_656 ? O00L Ca03 O007 90.56(8) . 2_656 ? O00K Ca03 O007 125.41(7) . 2_656 ? O00M Ca03 O007 83.91(8) . 2_656 ? O00A Ca03 O007 69.13(8) 1_444 2_656 ? O00D Ca03 O007 151.43(7) 2_666 2_656 ? O00B Ca03 O007 51.97(7) 2_656 2_656 ? O00L Ca03 C00Y 91.49(9) . 2_656 ? O00K Ca03 C00Y 99.61(8) . 2_656 ? O00M Ca03 C00Y 80.13(8) . 2_656 ? O00A Ca03 C00Y 95.08(8) 1_444 2_656 ? O00D Ca03 C00Y 175.47(8) 2_666 2_656 ? O00B Ca03 C00Y 26.16(8) 2_656 2_656 ? O007 Ca03 C00Y 26.07(8) 2_656 2_656 ? O00L Ca03 Ca04 93.22(6) . 2_656 ? O00K Ca03 Ca04 158.08(6) . 2_656 ? O00M Ca03 Ca04 86.32(6) . 2_656 ? O00A Ca03 Ca04 36.45(5) 1_444 2_656 ? O00D Ca03 Ca04 118.74(6) 2_666 2_656 ? O00B Ca03 Ca04 84.66(5) 2_656 2_656 ? O007 Ca03 Ca04 32.70(5) 2_656 2_656 ? C00Y Ca03 Ca04 58.63(6) 2_656 2_656 ? O00L Ca03 H00C 17.4 . . ? O00K Ca03 H00C 101.3 . . ? O00M Ca03 H00C 164.5 . . ? O00A Ca03 H00C 76.1 1_444 . ? O00D Ca03 H00C 91.9 2_666 . ? O00B Ca03 H00C 94.6 2_656 . ? O007 Ca03 H00C 82.7 2_656 . ? C00Y Ca03 H00C 91.1 2_656 . ? Ca04 Ca03 H00C 78.2 2_656 . ? O00L Ca03 H00D 17.5 . . ? O00K Ca03 H00D 79.7 . . ? O00M Ca03 H00D 153.0 . . ? O00A Ca03 H00D 102.0 1_444 . ? O00D Ca03 H00D 108.4 2_666 . ? O00B Ca03 H00D 69.8 2_656 . ? O007 Ca03 H00D 79.7 2_656 . ? C00Y Ca03 H00D 75.7 2_656 . ? Ca04 Ca03 H00D 91.2 2_656 . ? H00C Ca03 H00D 29.1 . . ? O00L Ca03 H00E 156.1 . . ? O00K Ca03 H00E 102.8 . . ? O00M Ca03 H00E 17.3 . . ? O00A Ca03 H00E 85.4 1_444 . ? O00D Ca03 H00E 111.1 2_666 . ? O00B Ca03 H00E 73.2 2_656 . ? O007 Ca03 H00E 66.7 2_656 . ? C00Y Ca03 H00E 64.9 2_656 . ? Ca04 Ca03 H00E 71.8 2_656 . ? H00C Ca03 H00E 148.4 . . ? H00D Ca03 H00E 140.4 . . ? O00L Ca03 H00F 156.3 . . ? O00K Ca03 H00F 75.9 . . ? O00M Ca03 H00F 17.3 . . ? O00A Ca03 H00F 109.1 1_444 . ? O00D Ca03 H00F 97.6 2_666 . ? O00B Ca03 H00F 75.1 2_656 . ? O007 Ca03 H00F 90.8 2_656 . ? C00Y Ca03 H00F 79.7 2_656 . ? Ca04 Ca03 H00F 100.6 2_656 . ? H00C Ca03 H00F 169.7 . . ? H00D Ca03 H00F 141.7 . . ? H00E Ca03 H00F 28.8 . . ? O00O Ca04 O00Z 85.55(10) . . ? O00O Ca04 O00N 89.45(9) . . ? O00Z Ca04 O00N 164.24(11) . . ? O00O Ca04 O007 164.00(8) . . ? O00Z Ca04 O007 95.39(9) . . ? O00N Ca04 O007 93.52(9) . . ? O00O Ca04 O006 80.78(8) . 2_666 ? O00Z Ca04 O006 96.82(11) . 2_666 ? O00N Ca04 O006 97.12(8) . 2_666 ? O007 Ca04 O006 83.25(8) . 2_666 ? O00O Ca04 O00I 75.43(8) . 2_767 ? O00Z Ca04 O00I 80.48(11) . 2_767 ? O00N Ca04 O00I 83.80(8) . 2_767 ? O007 Ca04 O00I 120.51(7) . 2_767 ? O006 Ca04 O00I 156.19(8) 2_666 2_767 ? O00O Ca04 O00A 127.27(8) . 2_767 ? O00Z Ca04 O00A 85.74(11) . 2_767 ? O00N Ca04 O00A 85.43(8) . 2_767 ? O007 Ca04 O00A 68.69(8) . 2_767 ? O006 Ca04 O00A 151.93(8) 2_666 2_767 ? O00I Ca04 O00A 51.84(7) 2_767 2_767 ? O00O Ca04 C014 101.35(9) . 2_767 ? O00Z Ca04 C014 84.69(12) . 2_767 ? O00N Ca04 C014 81.65(9) . 2_767 ? O007 Ca04 C014 94.64(8) . 2_767 ? O006 Ca04 C014 177.50(8) 2_666 2_767 ? O00I Ca04 C014 26.02(8) 2_767 2_767 ? O00A Ca04 C014 26.01(8) 2_767 2_767 ? O00O Ca04 Ca03 160.10(6) . 2_656 ? O00Z Ca04 Ca03 89.61(8) . 2_656 ? O00N Ca04 Ca03 90.05(6) . 2_656 ? O007 Ca04 Ca03 35.78(5) . 2_656 ? O006 Ca04 Ca03 119.00(6) 2_666 2_656 ? O00I Ca04 Ca03 84.73(5) 2_767 2_656 ? O00A Ca04 Ca03 32.93(5) 2_767 2_656 ? C014 Ca04 Ca03 58.92(6) 2_767 2_656 ? O00O Ca04 Ca02 53.53(6) . 2_767 ? O00Z Ca04 Ca02 85.49(8) . 2_767 ? O00N Ca04 Ca02 79.53(6) . 2_767 ? O007 Ca04 Ca02 142.47(6) . 2_767 ? O006 Ca04 Ca02 134.03(6) 2_666 2_767 ? O00I Ca04 Ca02 22.63(5) 2_767 2_767 ? O00A Ca04 Ca02 73.99(5) 2_767 2_767 ? C014 Ca04 Ca02 47.97(6) 2_767 2_767 ? Ca03 Ca04 Ca02 106.885(17) 2_656 2_767 ? O00O Ca04 H00G 98.7 . . ? O00Z Ca04 H00G 150.3 . . ? O00N Ca04 H00G 17.3 . . ? O007 Ca04 H00G 88.4 . . ? O006 Ca04 H00G 112.9 2_666 . ? O00I Ca04 H00G 72.4 2_767 . ? O00A Ca04 H00G 68.2 2_767 . ? C014 Ca04 H00G 65.6 2_767 . ? Ca03 Ca04 H00G 76.4 2_656 . ? Ca02 Ca04 H00G 74.1 2_767 . ? O00O Ca04 H00H 72.4 . . ? O00Z Ca04 H00H 151.9 . . ? O00N Ca04 H00H 17.3 . . ? O007 Ca04 H00H 110.7 . . ? O006 Ca04 H00H 96.6 2_666 . ? O00I Ca04 H00H 77.3 2_767 . ? O00A Ca04 H00H 93.8 2_767 . ? C014 Ca04 H00H 82.9 2_767 . ? Ca03 Ca04 H00H 105.2 2_656 . ? Ca02 Ca04 H00H 67.5 2_767 . ? H00G Ca04 H00H 28.9 . . ? O00O Ca04 H00K 98.6 . . ? O00Z Ca04 H00K 17.4 . . ? O00N Ca04 H00K 171.2 . . ? O007 Ca04 H00K 79.7 . . ? O006 Ca04 H00K 87.7 2_666 . ? O00I Ca04 H00K 94.8 2_767 . ? O00A Ca04 H00K 86.9 2_767 . ? C014 Ca04 H00K 93.3 2_767 . ? Ca03 Ca04 H00K 81.2 2_656 . ? Ca02 Ca04 H00K 102.5 2_767 . ? H00G Ca04 H00K 154.9 . . ? H00H Ca04 H00K 169.2 . . ? O00O Ca04 H00L 69.9 . . ? O00Z Ca04 H00L 17.4 . . ? O00N Ca04 H00L 158.2 . . ? O007 Ca04 H00L 108.3 . . ? O006 Ca04 H00L 86.8 2_666 . ? O00I Ca04 H00L 84.1 2_767 . ? O00A Ca04 H00L 101.2 2_767 . ? C014 Ca04 H00L 95.2 2_767 . ? Ca03 Ca04 H00L 106.9 2_656 . ? Ca02 Ca04 H00L 82.3 2_767 . ? H00G Ca04 H00L 156.0 . . ? H00H Ca04 H00L 141.0 . . ? H00K Ca04 H00L 29.0 . . ? C015 O005 Ca01 121.29(18) . . ? C015 O005 Ca01 121.13(18) . 2_656 ? Ca01 O005 Ca01 105.90(8) . 2_656 ? C011 O006 Ca04 137.0(2) . 2_666 ? C00Y O007 Ca04 156.7(2) . . ? C00Y O007 Ca03 90.67(18) . 2_656 ? Ca04 O007 Ca03 111.52(8) . 2_656 ? C016 O008 Ca02 122.02(18) . . ? C016 O008 Ca02 121.17(19) . 2_767 ? Ca02 O008 Ca02 106.63(8) . 2_767 ? C01F O009 Ca01 124.07(19) . . ? C014 O00A Ca03 159.5(2) . 1_666 ? C014 O00A Ca04 89.73(18) . 2_767 ? Ca03 O00A Ca04 110.62(9) 1_666 2_767 ? C00Y O00B Ca01 125.45(19) . . ? C00Y O00B Ca03 94.42(18) . 2_656 ? Ca01 O00B Ca03 137.07(9) . 2_656 ? C012 O00C Ca02 120.96(19) . . ? C012 O00D Ca03 135.5(2) . 2_666 ? C011 O00E Ca01 120.81(19) . . ? C01D O00F Ca02 125.6(2) . . ? C014 O00I Ca02 127.4(2) . . ? C014 O00I Ca04 95.81(18) . 2_767 ? Ca02 O00I Ca04 134.00(10) . 2_767 ? Ca01 O00J H00A 109.5 . . ? Ca01 O00J H00B 109.5 . . ? H00A O00J H00B 104.5 . . ? C015 O00K Ca03 153.0(2) . . ? Ca03 O00L H00C 109.5 . . ? Ca03 O00L H00D 109.3 . . ? H00C O00L H00D 104.5 . . ? Ca03 O00M H00E 109.6 . . ? Ca03 O00M H00F 109.6 . . ? H00E O00M H00F 104.4 . . ? Ca04 O00N H00G 109.8 . . ? Ca04 O00N H00H 109.7 . . ? H00G O00N H00H 104.3 . . ? C016 O00O Ca04 156.1(2) . . ? H00M O00P H00N 104.5 . . ? C01K N00Q C01B 109.9(2) . . ? C01K N00Q C010 111.3(2) . . ? C01B N00Q C010 111.0(2) . . ? C01K N00Q Ca01 106.07(17) . . ? C01B N00Q Ca01 107.45(18) . . ? C010 N00Q Ca01 111.01(17) . . ? C018 N00R C01L 109.6(2) . . ? C018 N00R C013 111.6(2) . . ? C01L N00R C013 111.6(2) . . ? C018 N00R Ca02 107.67(17) . . ? C01L N00R Ca02 106.12(17) . . ? C013 N00R Ca02 110.03(17) . . ? H00O O00S H00P 104.5 . . ? H00Q O00T H00R 104.5 . . ? C01H N00U C01G 109.2(2) . . ? C01H N00U C01I 109.3(2) . . ? C01G N00U C01I 110.6(2) . . ? C01H N00U Ca01 109.91(17) . . ? C01G N00U Ca01 103.31(17) . . ? C01I N00U Ca01 114.35(17) . . ? H00S O00V H00T 104.4 . . ? C01A N00W C019 109.1(2) . . ? C01A N00W C01J 109.5(2) . . ? C019 N00W C01J 111.0(2) . . ? C01A N00W Ca02 109.38(17) . . ? C019 N00W Ca02 102.90(17) . . ? C01J N00W Ca02 114.60(17) . . ? Ca02 O00X H00I 115.7 . . ? Ca02 O00X H00J 128.6 . . ? H00I O00X H00J 104.5 . . ? O007 C00Y O00B 121.7(3) . . ? O007 C00Y C01B 119.9(3) . . ? O00B C00Y C01B 118.4(3) . . ? O007 C00Y Ca03 63.26(16) . 2_656 ? O00B C00Y Ca03 59.41(15) . 2_656 ? C01B C00Y Ca03 170.1(2) . 2_656 ? Ca04 O00Z H00K 109.5 . . ? Ca04 O00Z H00L 109.5 . . ? H00K O00Z H00L 104.4 . . ? N00Q C010 C01I 111.3(2) . . ? N00Q C010 H01A 109.4 . . ? C01I C010 H01A 109.4 . . ? N00Q C010 H01B 109.4 . . ? C01I C010 H01B 109.4 . . ? H01A C010 H01B 108.0 . . ? O006 C011 O00E 124.7(3) . . ? O006 C011 C01G 118.0(3) . . ? O00E C011 C01G 117.3(3) . . ? O00C C012 O00D 125.1(3) . . ? O00C C012 C019 117.2(3) . . ? O00D C012 C019 117.6(3) . . ? N00R C013 C01J 111.4(2) . . ? N00R C013 H01C 109.4 . . ? C01J C013 H01C 109.4 . . ? N00R C013 H01D 109.4 . . ? C01J C013 H01D 109.4 . . ? H01C C013 H01D 108.0 . . ? O00A C014 O00I 121.7(3) . . ? O00A C014 C018 120.2(3) . . ? O00I C014 C018 118.1(3) . . ? O00A C014 Ca04 64.26(16) . 2_767 ? O00I C014 Ca04 58.16(16) . 2_767 ? C018 C014 Ca04 170.8(2) . 2_767 ? O00K C015 O005 125.3(3) . . ? O00K C015 C01H 115.1(3) . . ? O005 C015 C01H 119.5(3) . . ? O00O C016 O008 125.4(3) . . ? O00O C016 C01A 115.4(3) . . ? O008 C016 C01A 119.1(3) . . ? H01Y O017 H 109.5 . . ? N00R C018 C014 109.7(2) . . ? N00R C018 H01E 109.7 . . ? C014 C018 H01E 109.7 . . ? N00R C018 H01F 109.7 . . ? C014 C018 H01F 109.7 . . ? H01E C018 H01F 108.2 . . ? N00W C019 C012 114.0(2) . . ? N00W C019 H01G 108.7 . . ? C012 C019 H01G 108.7 . . ? N00W C019 H01H 108.7 . . ? C012 C019 H01H 108.7 . . ? H01G C019 H01H 107.6 . . ? N00W C01A C016 114.0(2) . . ? N00W C01A H01I 108.7 . . ? C016 C01A H01I 108.7 . . ? N00W C01A H01J 108.7 . . ? C016 C01A H01J 108.7 . . ? H01I C01A H01J 107.6 . . ? N00Q C01B C00Y 110.1(2) . . ? N00Q C01B H01K 109.6 . . ? C00Y C01B H01K 109.6 . . ? N00Q C01B H01L 109.6 . . ? C00Y C01B H01L 109.6 . . ? H01K C01B H01L 108.2 . . ? O00F C01D O00G 124.8(3) . . ? O00F C01D C01L 118.1(3) . . ? O00G C01D C01L 117.0(3) . . ? H01Z O01E HA 104.5 . . ? O009 C01F O00H 123.9(3) . . ? O009 C01F C01K 118.1(3) . . ? O00H C01F C01K 118.0(3) . . ? O009 C01F Ca01 37.17(14) . . ? O00H C01F Ca01 158.2(2) . . ? C01K C01F Ca01 82.39(17) . . ? N00U C01G C011 113.0(2) . . ? N00U C01G H01M 109.0 . . ? C011 C01G H01M 109.0 . . ? N00U C01G H01N 109.0 . . ? C011 C01G H01N 109.0 . . ? H01M C01G H01N 107.8 . . ? N00U C01H C015 114.1(2) . . ? N00U C01H H01O 108.7 . . ? C015 C01H H01O 108.7 . . ? N00U C01H H01P 108.7 . . ? C015 C01H H01P 108.7 . . ? H01O C01H H01P 107.6 . . ? N00U C01I C010 112.4(2) . . ? N00U C01I H01Q 109.1 . . ? C010 C01I H01Q 109.1 . . ? N00U C01I H01R 109.1 . . ? C010 C01I H01R 109.1 . . ? H01Q C01I H01R 107.9 . . ? N00W C01J C013 112.7(2) . . ? N00W C01J H01S 109.1 . . ? C013 C01J H01S 109.1 . . ? N00W C01J H01T 109.1 . . ? C013 C01J H01T 109.1 . . ? H01S C01J H01T 107.8 . . ? N00Q C01K C01F 113.6(2) . . ? N00Q C01K H01U 108.8 . . ? C01F C01K H01U 108.8 . . ? N00Q C01K H01V 108.8 . . ? C01F C01K H01V 108.8 . . ? H01U C01K H01V 107.7 . . ? N00R C01L C01D 114.1(2) . . ? N00R C01L H01W 108.7 . . ? C01D C01L H01W 108.7 . . ? N00R C01L H01X 108.7 . . ? C01D C01L H01X 108.7 . . ? H01W C01L H01X 107.6 . . ? 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 O009 2.360(2) . ? Ca01 O00B 2.376(2) . ? Ca01 O00E 2.419(2) . ? Ca01 O00J 2.439(2) . ? Ca01 O005 2.486(2) . ? Ca01 O005 2.558(2) 2_656 ? Ca01 N00U 2.617(3) . ? Ca01 N00Q 2.676(3) . ? Ca01 C01F 3.236(3) . ? Ca01 Ca01 4.0258(11) 2_656 ? Ca02 O00I 2.372(2) . ? Ca02 O00F 2.376(2) . ? Ca02 O00C 2.414(2) . ? Ca02 O008 2.451(2) . ? Ca02 O00X 2.455(3) . ? Ca02 O008 2.500(2) 2_767 ? Ca02 N00W 2.610(3) . ? Ca02 N00R 2.728(3) . ? Ca02 Ca02 3.9710(11) 2_767 ? Ca02 Ca04 4.4330(8) 2_767 ? Ca03 O00L 2.326(2) . ? Ca03 O00K 2.353(2) . ? Ca03 O00M 2.356(2) . ? Ca03 O00A 2.358(2) 1_444 ? Ca03 O00D 2.384(2) 2_666 ? Ca03 O00B 2.467(2) 2_656 ? Ca03 O007 2.552(2) 2_656 ? Ca03 C00Y 2.857(3) 2_656 ? Ca03 Ca04 4.0607(9) 2_656 ? Ca03 H00C 2.7416 . ? Ca03 H00D 2.7403 . ? Ca03 H00E 2.7733 . ? Ca03 H00F 2.7729 . ? Ca04 O00O 2.310(2) . ? Ca04 O00Z 2.337(3) . ? Ca04 O00N 2.353(2) . ? Ca04 O007 2.358(2) . ? Ca04 O006 2.381(2) 2_666 ? Ca04 O00I 2.444(2) 2_767 ? Ca04 O00A 2.578(2) 2_767 ? Ca04 C014 2.862(3) 2_767 ? Ca04 H00G 2.7744 . ? Ca04 H00H 2.7735 . ? Ca04 H00K 2.7540 . ? Ca04 H00L 2.7540 . ? O005 C015 1.273(4) . ? O006 C011 1.256(4) . ? O007 C00Y 1.256(4) . ? O008 C016 1.269(4) . ? O009 C01F 1.257(4) . ? O00A C014 1.255(4) . ? O00B C00Y 1.264(4) . ? O00C C012 1.254(4) . ? O00D C012 1.257(4) . ? O00E C011 1.256(4) . ? O00F C01D 1.258(4) . ? O00G C01D 1.258(4) . ? O00H C01F 1.263(4) . ? O00I C014 1.262(4) . ? O00J H00A 0.8710 . ? O00J H00B 0.8710 . ? O00K C015 1.249(4) . ? O00L H00C 0.8702 . ? O00L H00D 0.8709 . ? O00M H00E 0.8731 . ? O00M H00F 0.8729 . ? O00N H00G 0.8758 . ? O00N H00H 0.8752 . ? O00O C016 1.247(4) . ? O00P H00M 0.8699 . ? O00P H00N 0.8700 . ? N00Q C01K 1.467(4) . ? N00Q C01B 1.471(4) . ? N00Q C010 1.471(4) . ? N00R C018 1.466(4) . ? N00R C01L 1.468(4) . ? N00R C013 1.468(4) . ? O00S H00O 0.8696 . ? O00S H00P 0.8703 . ? O00T H00Q 0.8699 . ? O00T H00R 0.8699 . ? N00U C01H 1.466(4) . ? N00U C01G 1.476(4) . ? N00U C01I 1.488(4) . ? O00V H00S 0.8701 . ? O00V H00T 0.8706 . ? N00W C01A 1.466(4) . ? N00W C019 1.482(4) . ? N00W C01J 1.486(4) . ? O00X H00I 0.8699 . ? O00X H00J 0.8697 . ? C00Y C01B 1.514(4) . ? O00Z H00K 0.8725 . ? O00Z H00L 0.8728 . ? C010 C01I 1.520(4) . ? C010 H01A 0.9900 . ? C010 H01B 0.9900 . ? C011 C01G 1.528(4) . ? C012 C019 1.529(4) . ? C013 C01J 1.511(4) . ? C013 H01C 0.9900 . ? C013 H01D 0.9900 . ? C014 C018 1.515(4) . ? C015 C01H 1.520(4) . ? C016 C01A 1.518(4) . ? O017 H01Y 0.8702 . ? O017 H 0.8699 . ? C018 H01E 0.9900 . ? C018 H01F 0.9900 . ? C019 H01G 0.9900 . ? C019 H01H 0.9900 . ? C01A H01I 0.9900 . ? C01A H01J 0.9900 . ? C01B H01K 0.9900 . ? C01B H01L 0.9900 . ? C01D C01L 1.528(4) . ? O01E H01Z 0.8701 . ? O01E HA 0.8702 . ? C01F C01K 1.524(4) . ? C01G H01M 0.9900 . ? C01G H01N 0.9900 . ? C01H H01O 0.9900 . ? C01H H01P 0.9900 . ? C01I H01Q 0.9900 . ? C01I H01R 0.9900 . ? C01J H01S 0.9900 . ? C01J H01T 0.9900 . ? C01K H01U 0.9900 . ? C01K H01V 0.9900 . ? C01L H01W 0.9900 . ? C01L H01X 0.9900 . ? 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 Ca04 O007 C00Y O00B -173.7(4) . . . . ? Ca03 O007 C00Y O00B -11.1(3) 2_656 . . . ? Ca04 O007 C00Y C01B 6.8(7) . . . . ? Ca03 O007 C00Y C01B 169.3(3) 2_656 . . . ? Ca04 O007 C00Y Ca03 -162.5(5) . . . 2_656 ? Ca01 O00B C00Y O007 174.6(2) . . . . ? Ca03 O00B C00Y O007 11.6(3) 2_656 . . . ? Ca01 O00B C00Y C01B -5.8(4) . . . . ? Ca03 O00B C00Y C01B -168.9(2) 2_656 . . . ? Ca01 O00B C00Y Ca03 163.0(2) . . . 2_656 ? C01K N00Q C010 C01I -71.4(3) . . . . ? C01B N00Q C010 C01I 165.9(2) . . . . ? Ca01 N00Q C010 C01I 46.5(3) . . . . ? Ca04 O006 C011 O00E -156.6(2) 2_666 . . . ? Ca04 O006 C011 C01G 25.4(4) 2_666 . . . ? Ca01 O00E C011 O006 172.4(2) . . . . ? Ca01 O00E C011 C01G -9.6(3) . . . . ? Ca02 O00C C012 O00D 178.2(2) . . . . ? Ca02 O00C C012 C019 -4.4(3) . . . . ? Ca03 O00D C012 O00C -150.5(2) 2_666 . . . ? Ca03 O00D C012 C019 32.1(4) 2_666 . . . ? C018 N00R C013 C01J 165.3(2) . . . . ? C01L N00R C013 C01J -71.7(3) . . . . ? Ca02 N00R C013 C01J 45.8(3) . . . . ? Ca03 O00A C014 O00I 177.0(4) 1_666 . . . ? Ca04 O00A C014 O00I -9.7(3) 2_767 . . . ? Ca03 O00A C014 C018 -2.4(8) 1_666 . . . ? Ca04 O00A C014 C018 170.9(3) 2_767 . . . ? Ca03 O00A C014 Ca04 -173.3(6) 1_666 . . 2_767 ? Ca02 O00I C014 O00A 173.4(2) . . . . ? Ca04 O00I C014 O00A 10.3(3) 2_767 . . . ? Ca02 O00I C014 C018 -7.2(4) . . . . ? Ca04 O00I C014 C018 -170.3(2) 2_767 . . . ? Ca02 O00I C014 Ca04 163.1(2) . . . 2_767 ? Ca03 O00K C015 O005 -34.8(6) . . . . ? Ca03 O00K C015 C01H 148.2(3) . . . . ? Ca01 O005 C015 O00K -174.0(2) . . . . ? Ca01 O005 C015 O00K -36.1(4) 2_656 . . . ? Ca01 O005 C015 C01H 2.9(4) . . . . ? Ca01 O005 C015 C01H 140.8(2) 2_656 . . . ? Ca04 O00O C016 O008 -29.6(8) . . . . ? Ca04 O00O C016 C01A 153.2(4) . . . . ? Ca02 O008 C016 O00O -174.8(2) . . . . ? Ca02 O008 C016 O00O -34.2(4) 2_767 . . . ? Ca02 O008 C016 C01A 2.3(4) . . . . ? Ca02 O008 C016 C01A 142.9(2) 2_767 . . . ? C01L N00R C018 C014 76.6(3) . . . . ? C013 N00R C018 C014 -159.3(2) . . . . ? Ca02 N00R C018 C014 -38.5(3) . . . . ? O00A C014 C018 N00R -146.8(3) . . . . ? O00I C014 C018 N00R 33.7(4) . . . . ? C01A N00W C019 C012 -159.8(2) . . . . ? C01J N00W C019 C012 79.3(3) . . . . ? Ca02 N00W C019 C012 -43.7(3) . . . . ? O00C C012 C019 N00W 36.6(4) . . . . ? O00D C012 C019 N00W -145.8(3) . . . . ? C019 N00W C01A C016 79.6(3) . . . . ? C01J N00W C01A C016 -158.7(2) . . . . ? Ca02 N00W C01A C016 -32.3(3) . . . . ? O00O C016 C01A N00W -160.2(3) . . . . ? O008 C016 C01A N00W 22.4(4) . . . . ? C01K N00Q C01B C00Y 75.7(3) . . . . ? C010 N00Q C01B C00Y -160.8(2) . . . . ? Ca01 N00Q C01B C00Y -39.3(3) . . . . ? O007 C00Y C01B N00Q -147.1(3) . . . . ? O00B C00Y C01B N00Q 33.3(4) . . . . ? Ca02 O00F C01D O00G 167.8(2) . . . . ? Ca02 O00F C01D C01L -15.1(4) . . . . ? Ca01 O009 C01F O00H 164.9(2) . . . . ? Ca01 O009 C01F C01K -17.7(4) . . . . ? C01H N00U C01G C011 -161.8(2) . . . . ? C01I N00U C01G C011 77.9(3) . . . . ? Ca01 N00U C01G C011 -44.8(3) . . . . ? O006 C011 C01G N00U -141.1(3) . . . . ? O00E C011 C01G N00U 40.7(4) . . . . ? C01G N00U C01H C015 80.1(3) . . . . ? C01I N00U C01H C015 -158.8(2) . . . . ? Ca01 N00U C01H C015 -32.5(3) . . . . ? O00K C015 C01H N00U -160.9(3) . . . . ? O005 C015 C01H N00U 21.9(4) . . . . ? C01H N00U C01I C010 159.9(2) . . . . ? C01G N00U C01I C010 -79.9(3) . . . . ? Ca01 N00U C01I C010 36.2(3) . . . . ? N00Q C010 C01I N00U -56.5(3) . . . . ? C01A N00W C01J C013 161.7(2) . . . . ? C019 N00W C01J C013 -77.7(3) . . . . ? Ca02 N00W C01J C013 38.3(3) . . . . ? N00R C013 C01J N00W -58.0(3) . . . . ? C01B N00Q C01K C01F -148.8(3) . . . . ? C010 N00Q C01K C01F 87.9(3) . . . . ? Ca01 N00Q C01K C01F -32.9(3) . . . . ? O009 C01F C01K N00Q 36.5(4) . . . . ? O00H C01F C01K N00Q -145.9(3) . . . . ? Ca01 C01F C01K N00Q 25.8(2) . . . . ? C018 N00R C01L C01D -147.7(3) . . . . ? C013 N00R C01L C01D 88.1(3) . . . . ? Ca02 N00R C01L C01D -31.7(3) . . . . ? O00F C01D C01L N00R 34.0(4) . . . . ? O00G C01D C01L N00R -148.6(3) . . . . ?