#------------------------------------------------------------------------------ #$Date: 2017-10-17 08:15:37 +0300 (Tue, 17 Oct 2017) $ #$Revision: 202050 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/93/7229341.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_7229341 loop_ _publ_author_name 'Dong, Xiu-Yan' 'Li, Xiao-Yan' 'Liu, Ling-Zhi' 'Zhang, Han' 'Ding, Yu-Jie' 'Dong, Wen-Kui' _publ_section_title ; Tri- and hexanuclear heterometallic Ni(ii)--M(ii) (M = Ca, Sr and Ba) bis(salamo)-type complexes: synthesis, structure and fluorescence properties ; _journal_issue 76 _journal_name_full 'RSC Adv.' _journal_page_first 48394 _journal_paper_doi 10.1039/C7RA07826A _journal_volume 7 _journal_year 2017 _chemical_formula_moiety 'C38 H42 Ca N4 Ni2 O16, 2(C H Cl3), 2(C2 H6 O)' _chemical_formula_sum 'C44 H56 Ca Cl6 N4 Ni2 O18' _chemical_formula_weight 1299.12 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-07-15 deposited with the CCDC. 2017-10-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.627(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.4086(8) _cell_length_b 12.0628(6) _cell_length_c 29.5294(9) _cell_measurement_reflns_used 3718 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.11 _cell_volume 5394.5(4) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXTL (Bruker, 2008)' _diffrn_ambient_temperature 291(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0117 _diffrn_reflns_av_unetI/netI 0.0615 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 21343 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 1.397 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2008' _exptl_crystal_colour 'clear dark green' _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2680 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _refine_diff_density_max 2.325 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 642 _refine_ls_number_reflns 10337 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0469 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.03P)^2^+1.22P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.0986 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7204 _reflns_number_total 10337 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ra07826a2.cif _cod_data_source_block D847_2 _cod_database_code 7229341 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.767 _shelx_estimated_absorpt_t_max 0.801 _shelx_res_file ; TITL D847_2 in P21/n #14 D847_2.res created by SHELXL-2016/6 at 23:23:34 on 08-Jul-2017 CELL 0.71073 15.40857 12.06281 29.52935 90 100.6271 90 ZERR 4 0.00075 0.00062 0.00087 0 0.0052 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ca Cl N Ni O UNIT 176 224 4 24 16 8 72 L.S. 15 ACTA BOND $H FMAP 2 PLAN 5 HTAB omit -1 52 dfix 1.47 0.001 c37 c38 c39 c40 dfix 1.23 0.001 c37 o17 c39 o18 dfix 2.15 0.001 H37A H41E H39A H42E delu 0.002 O1 C2 O3 C9 O7 C23 N2 C11 C27 C28 O13 C35 size 0.24 0.22 0.20 CONF temp 18 WGHT 0.030000 1.220000 FVAR 0.11258 C1 1 0.945926 0.376005 -0.034988 11.00000 0.04950 0.04193 = 0.04061 0.01051 0.00823 -0.00896 AFIX 137 H1A 2 0.979747 0.343652 -0.055846 11.00000 -1.50000 H1B 2 0.984629 0.415677 -0.011257 11.00000 -1.50000 H1C 2 0.903101 0.426185 -0.051533 11.00000 -1.50000 AFIX 0 C2 1 0.831078 0.243364 -0.043929 11.00000 0.02793 0.03975 = 0.03019 0.00763 0.00562 0.00683 C3 1 0.788008 0.161407 -0.021259 11.00000 0.03668 0.03608 = 0.03459 0.00466 0.00917 0.00728 C4 1 0.715947 0.104338 -0.047184 11.00000 0.03202 0.04679 = 0.03412 -0.00794 0.00673 0.00841 C5 1 0.687590 0.134125 -0.094639 11.00000 0.04335 0.04058 = 0.04188 -0.00549 -0.00618 -0.00659 AFIX 43 H5 2 0.639043 0.099067 -0.112229 11.00000 -1.20000 AFIX 0 C6 1 0.733483 0.216781 -0.114635 11.00000 0.04701 0.05981 = 0.03498 0.01064 0.00743 0.00003 AFIX 43 H6 2 0.714219 0.238451 -0.145053 11.00000 -1.20000 AFIX 0 C7 1 0.803485 0.262445 -0.089764 11.00000 0.04303 0.04414 = 0.02811 0.00774 0.00814 0.00740 AFIX 43 H7 2 0.836418 0.310946 -0.104316 11.00000 -1.20000 AFIX 0 C8 1 0.670162 0.016215 -0.028809 11.00000 0.03435 0.03995 = 0.03904 -0.00959 -0.00632 0.00502 AFIX 43 H8 2 0.627748 -0.021803 -0.049550 11.00000 -1.20000 AFIX 0 C9 1 0.648945 -0.157669 0.061667 11.00000 0.04403 0.03591 = 0.04747 0.00767 0.01046 -0.01184 AFIX 23 H9A 2 0.709295 -0.138807 0.075330 11.00000 -1.20000 H9B 2 0.645448 -0.237688 0.058627 11.00000 -1.20000 AFIX 0 C10 1 0.589744 -0.121113 0.092999 11.00000 0.04677 0.04669 = 0.03794 -0.01019 0.00679 -0.01955 AFIX 23 H10A 2 0.531130 -0.150153 0.081471 11.00000 -1.20000 H10B 2 0.610317 -0.154036 0.123030 11.00000 -1.20000 AFIX 0 C11 1 0.670610 0.095218 0.153544 11.00000 0.03620 0.05061 = 0.03194 -0.01142 0.00887 -0.01631 AFIX 43 H11 2 0.623710 0.081783 0.168607 11.00000 -1.20000 AFIX 66 C12 1 0.740854 0.175078 0.176504 11.00000 0.03181 0.04113 = 0.03396 -0.00767 0.00883 -0.00632 C13 1 0.806256 0.212452 0.153513 11.00000 0.03928 0.04222 = 0.02819 -0.00757 0.00749 0.01137 C14 1 0.868699 0.288462 0.174558 11.00000 0.03510 0.03766 = 0.03675 0.01016 0.01258 -0.00747 C15 1 0.865739 0.327099 0.218593 11.00000 0.03250 0.03854 = 0.03286 -0.00414 0.00857 -0.00226 C16 1 0.800337 0.289727 0.241585 11.00000 0.03387 0.05072 = 0.03099 -0.00785 0.00698 -0.00875 C21 1 0.737894 0.213716 0.220541 11.00000 0.03457 0.04789 = 0.03257 0.00941 0.01053 -0.00360 AFIX 0 C17 1 0.787980 0.335726 0.284366 11.00000 0.03636 0.04281 = 0.03699 -0.01022 0.00862 -0.00827 AFIX 43 H17 2 0.824125 0.394013 0.296862 11.00000 -1.20000 AFIX 0 C18 1 0.724580 0.297494 0.308131 11.00000 0.04008 0.04573 = 0.03745 -0.01023 0.01387 -0.01054 AFIX 43 H18 2 0.717029 0.332020 0.335296 11.00000 -1.20000 AFIX 0 C19 1 0.672765 0.208425 0.291545 11.00000 0.04736 0.04661 = 0.03991 -0.00756 0.01789 -0.00956 AFIX 43 H19 2 0.634712 0.176231 0.308813 11.00000 -1.20000 AFIX 0 C20 1 0.678858 0.168141 0.248502 11.00000 0.04386 0.04179 = 0.03759 -0.00925 0.01199 -0.01317 AFIX 43 H20 2 0.643172 0.108666 0.236904 11.00000 -1.20000 AFIX 0 C22 1 0.937157 0.400640 0.242174 11.00000 0.03519 0.04871 = 0.03357 -0.01131 0.01010 0.00288 AFIX 43 H22 2 0.941321 0.407969 0.273854 11.00000 -1.20000 AFIX 0 C23 1 1.067016 0.619512 0.252983 11.00000 0.04085 0.04665 = 0.04273 -0.01545 0.00639 -0.01335 AFIX 23 H23A 2 1.112845 0.648823 0.276970 11.00000 -1.20000 H23B 2 1.011647 0.652584 0.257151 11.00000 -1.20000 AFIX 0 C24 1 1.085684 0.657096 0.207828 11.00000 0.04105 0.03404 = 0.04551 -0.01215 0.01034 0.00414 AFIX 23 H24A 2 1.035222 0.640045 0.183978 11.00000 -1.20000 H24B 2 1.093337 0.736933 0.208590 11.00000 -1.20000 AFIX 0 C25 1 1.209146 0.483317 0.149533 11.00000 0.03742 0.03916 = 0.04050 0.01058 0.00478 -0.00170 AFIX 43 H25 2 1.260877 0.523226 0.159224 11.00000 -1.20000 AFIX 0 C26 1 1.213120 0.397337 0.118634 11.00000 0.03232 0.04120 = 0.03748 0.01055 0.00850 -0.00547 C27 1 1.296434 0.368752 0.107372 11.00000 0.03382 0.04023 = 0.04849 0.00583 0.01085 0.00546 AFIX 43 H27 2 1.346678 0.406591 0.121638 11.00000 -1.20000 AFIX 0 C28 1 1.304627 0.286660 0.075951 11.00000 0.03294 0.05507 = 0.04289 -0.00491 0.01425 -0.00472 AFIX 43 H28 2 1.360225 0.265479 0.071105 11.00000 -1.20000 AFIX 0 C29 1 1.231401 0.237023 0.052187 11.00000 0.03759 0.03997 = 0.04587 0.00788 0.01425 0.00752 AFIX 43 H29 2 1.236914 0.188522 0.028401 11.00000 -1.20000 AFIX 0 C30 1 1.148644 0.256456 0.062309 11.00000 0.03670 0.03512 = 0.02953 0.00356 0.00900 0.00610 C31 1 1.139192 0.337236 0.095858 11.00000 0.03970 0.03363 = 0.03412 0.01085 0.01089 -0.00781 C32 1 1.076350 0.123711 0.008799 11.00000 0.04616 0.04229 = 0.05330 -0.01716 0.01785 -0.00834 AFIX 137 H32A 2 1.090276 0.156299 -0.018648 11.00000 -1.50000 H32B 2 1.020894 0.085482 0.001423 11.00000 -1.50000 H32C 2 1.121875 0.072193 0.021478 11.00000 -1.50000 AFIX 0 C33 1 0.886124 0.525476 0.091600 11.00000 0.05127 0.02723 = 0.03728 -0.00660 0.01498 -0.01185 C34 1 0.828003 0.622486 0.076084 11.00000 0.03836 0.04526 = 0.04682 -0.00696 0.00411 0.00910 AFIX 137 H34A 2 0.838072 0.679409 0.099179 11.00000 -1.50000 H34B 2 0.767305 0.599707 0.071365 11.00000 -1.50000 H34C 2 0.841269 0.650706 0.047735 11.00000 -1.50000 AFIX 0 C35 1 0.923643 -0.025432 0.104064 11.00000 0.03624 0.03796 = 0.03762 -0.01079 0.01077 -0.00516 C36 1 0.976169 -0.120286 0.126479 11.00000 0.04288 0.04024 = 0.04908 0.00814 -0.00635 -0.01185 AFIX 137 H36D 2 0.939047 -0.184539 0.125252 11.00000 -1.50000 H36E 2 0.999459 -0.102224 0.158043 11.00000 -1.50000 H36F 2 1.023961 -0.135420 0.110635 11.00000 -1.50000 AFIX 0 C37 1 0.664626 0.386242 -0.001298 11.00000 0.26508 AFIX 23 H37A 2 0.621480 0.381630 0.018755 11.00000 -1.20000 H37B 2 0.646970 0.336911 -0.027306 11.00000 -1.20000 AFIX 0 C38 1 0.673221 0.500692 -0.016888 11.00000 0.18089 AFIX 137 H38A 2 0.665616 0.551164 0.007211 11.00000 -1.50000 H38B 2 0.628936 0.514789 -0.043687 11.00000 -1.50000 H38C 2 0.730730 0.510917 -0.024377 11.00000 -1.50000 AFIX 0 C39 1 1.171143 0.110400 0.163729 11.00000 0.26381 AFIX 23 H39A 2 1.171029 0.120844 0.196289 11.00000 -1.20000 H39B 2 1.215980 0.157812 0.154810 11.00000 -1.20000 AFIX 0 C40 1 1.187045 -0.006326 0.153643 11.00000 0.17079 AFIX 137 H40A 2 1.143310 -0.051961 0.163798 11.00000 -1.50000 H40B 2 1.244704 -0.027758 0.169479 11.00000 -1.50000 H40C 2 1.183511 -0.015536 0.121063 11.00000 -1.50000 AFIX 0 C41 1 0.554977 0.200595 0.024158 11.00000 0.03829 0.06035 = 0.05505 -0.01772 0.00721 -0.00640 AFIX 137 H41D 2 0.539214 0.123792 0.019955 11.00000 -1.50000 H41E 2 0.544586 0.237384 -0.005173 11.00000 -1.50000 H41F 2 0.519789 0.234604 0.043971 11.00000 -1.50000 AFIX 0 C42 1 1.191088 0.298388 0.234622 11.00000 0.04654 0.04910 = 0.04908 -0.00714 -0.01198 -0.00813 AFIX 137 H42D 2 1.202679 0.374299 0.243481 11.00000 -1.50000 H42E 2 1.239980 0.269135 0.222435 11.00000 -1.50000 H42F 2 1.183248 0.255849 0.261048 11.00000 -1.50000 AFIX 0 C43 1 0.614136 0.433675 0.116893 11.00000 0.05915 0.05791 = 0.04337 -0.01511 -0.00386 0.01490 AFIX 13 H43 2 0.646097 0.384339 0.099316 11.00000 -1.20000 AFIX 0 C44 1 0.482919 0.565409 0.248436 11.00000 0.04473 0.05424 = 0.05141 -0.01975 0.01232 -0.00923 AFIX 13 H44 2 0.471509 0.615696 0.272738 11.00000 -1.20000 AFIX 0 CA1 3 0.926776 0.249314 0.073495 11.00000 0.02821 0.03123 = 0.02855 -0.00586 0.00678 -0.00703 CL1 4 0.687575 0.501443 0.156847 11.00000 0.04826 0.06735 = 0.05416 -0.01011 -0.00960 -0.01185 CL2 4 0.550480 0.525131 0.079259 11.00000 0.05604 0.06928 = 0.05730 0.01352 0.00735 0.01218 CL3 4 0.541430 0.353645 0.143723 11.00000 0.05151 0.05436 = 0.06371 -0.00929 0.01299 -0.00891 CL4 4 0.471632 0.642655 0.195769 11.00000 0.06508 0.05363 = 0.05463 0.01378 0.01147 0.01076 CL5 4 0.399628 0.465273 0.239585 11.00000 0.05469 0.06748 = 0.05565 0.01320 -0.01194 -0.01616 CL6 4 0.581862 0.512660 0.264478 11.00000 0.04833 0.06159 = 0.05340 0.00817 -0.01010 -0.00844 N1 5 0.681507 -0.013918 0.011630 11.00000 0.03318 0.04215 = 0.04450 -0.01364 0.01200 -0.01005 N2 5 0.669461 0.044367 0.115416 11.00000 0.03835 0.03847 = 0.03991 -0.00556 0.01417 -0.01459 N3 5 0.994234 0.455728 0.224305 11.00000 0.03700 0.03670 = 0.03560 -0.01125 0.00854 -0.00861 N4 5 1.141543 0.513131 0.165997 11.00000 0.03240 0.04302 = 0.04246 -0.00510 -0.00672 -0.00304 NI1 6 0.745397 0.079670 0.066592 11.00000 0.03406 0.03814 = 0.03451 -0.00850 0.00853 -0.00876 NI2 6 1.029158 0.419036 0.161726 11.00000 0.03449 0.03673 = 0.03490 -0.00792 0.00874 -0.00849 O1 7 0.901797 0.290573 -0.014677 11.00000 0.03995 0.04476 = 0.03734 -0.00439 0.01088 -0.01075 O2 7 0.818361 0.142684 0.022483 11.00000 0.03979 0.04105 = 0.03223 -0.01087 0.00892 -0.00625 O3 7 0.627871 -0.108629 0.016516 11.00000 0.04397 0.04356 = 0.03638 -0.00933 0.00558 -0.01402 O4 7 0.583005 -0.006514 0.098674 11.00000 0.03261 0.04391 = 0.04574 0.00707 0.01372 -0.00762 O5 7 0.806689 0.192202 0.108779 11.00000 0.03988 0.04015 = 0.03197 -0.00679 0.00929 -0.01013 O6 7 0.935954 0.305406 0.152366 11.00000 0.03454 0.04046 = 0.03830 -0.01067 0.01092 -0.01116 O7 7 1.061392 0.502679 0.260018 11.00000 0.04836 0.04464 = 0.03480 -0.00586 0.01058 -0.00703 O8 7 1.162875 0.606569 0.196172 11.00000 0.03798 0.04004 = 0.04810 -0.01338 0.01150 -0.00682 O9 7 1.057339 0.354785 0.103003 11.00000 0.03145 0.03971 = 0.04169 -0.00656 0.01016 -0.00794 O10 7 1.070408 0.208702 0.041723 11.00000 0.04023 0.04673 = 0.04178 -0.01415 0.01444 -0.01093 O11 7 0.944994 0.537312 0.125811 11.00000 0.03745 0.03852 = 0.03976 -0.00814 0.00696 -0.00755 O12 7 0.872436 0.435623 0.067653 11.00000 0.03706 0.04237 = 0.03820 -0.00782 -0.00497 -0.00740 O13 7 0.964433 0.062210 0.098099 11.00000 0.03484 0.03643 = 0.04283 0.00944 -0.00427 0.00369 O14 7 0.842428 -0.036715 0.090694 11.00000 0.03756 0.03671 = 0.03867 -0.00554 -0.00577 -0.00686 O15 7 0.646759 0.209578 0.044688 11.00000 0.03101 0.04778 = 0.04576 -0.00767 -0.00476 -0.00657 AFIX 3 H15A 2 0.684799 0.206238 0.027228 11.00000 -1.20000 AFIX 0 O16 7 1.112700 0.292256 0.200231 11.00000 0.03548 0.04582 = 0.04275 -0.00526 0.00757 -0.00587 AFIX 3 H16A 2 1.066661 0.285256 0.212021 11.00000 -1.20000 AFIX 0 O17 7 0.738791 0.362679 0.019713 11.00000 0.22827 AFIX 3 H17C 2 0.761271 0.397729 0.044023 11.00000 -1.50000 AFIX 0 O18 7 1.098113 0.130759 0.140593 11.00000 0.22608 AFIX 3 H18C 2 1.052132 0.098019 0.145843 11.00000 -1.50000 AFIX 0 HKLF 4 REM D847_2 in P21/n #14 REM R1 = 0.0469 for 7204 Fo > 4sig(Fo) and 0.0645 for all 10337 data REM 642 parameters refined using 12 restraints END WGHT 0.0511 0.0000 REM Instructions for potential hydrogen bonds HTAB C9 O14 HTAB C24 O11 EQIV $1 x+1, y, z HTAB C25 Cl5_$1 HTAB C37 Cl2 EQIV $2 -x+1, -y+1, -z HTAB C38 Cl2_$2 HTAB C43 O15 HTAB O16 N3 HTAB O17 O12 HTAB O18 O13 REM Highest difference peak 2.325, deepest hole -0.348, 1-sigma level 0.082 Q1 1 0.7414 0.4212 0.0660 11.00000 0.05 2.32 Q2 1 1.0253 0.0804 0.1594 11.00000 0.05 2.23 Q3 1 1.1160 0.0968 0.1607 11.00000 0.05 0.91 Q4 1 0.7044 0.4056 0.0245 11.00000 0.05 0.78 Q5 1 1.1964 0.0476 0.1497 11.00000 0.05 0.59 ; _shelx_res_checksum 16667 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 C1 C 0.9459(2) 0.3760(3) -0.03499(12) 0.0440(9) Uani 1 1 d . . H1A H 0.979747 0.343652 -0.055846 0.066 Uiso 1 1 calc R U H1B H 0.984629 0.415677 -0.011257 0.066 Uiso 1 1 calc R U H1C H 0.903101 0.426185 -0.051533 0.066 Uiso 1 1 calc R U C2 C 0.8311(2) 0.2434(3) -0.04393(12) 0.0326(8) Uani 1 1 d . U C3 C 0.7880(2) 0.1614(3) -0.02126(11) 0.0355(8) Uani 1 1 d . . C4 C 0.7159(2) 0.1043(3) -0.04718(11) 0.0376(9) Uani 1 1 d . . C5 C 0.6876(2) 0.1341(3) -0.09464(12) 0.0437(9) Uani 1 1 d . . H5 H 0.639043 0.099067 -0.112229 0.052 Uiso 1 1 calc R U C6 C 0.7335(2) 0.2168(3) -0.11463(13) 0.0473(10) Uani 1 1 d . . H6 H 0.714219 0.238451 -0.145053 0.057 Uiso 1 1 calc R U C7 C 0.8035(2) 0.2624(3) -0.08976(12) 0.0382(9) Uani 1 1 d . . H7 H 0.836418 0.310946 -0.104316 0.046 Uiso 1 1 calc R U C8 C 0.6702(2) 0.0162(3) -0.02881(12) 0.0394(9) Uani 1 1 d . . H8 H 0.627748 -0.021803 -0.049550 0.047 Uiso 1 1 calc R U C9 C 0.6489(2) -0.1577(3) 0.06167(12) 0.0422(9) Uani 1 1 d . U H9A H 0.709295 -0.138807 0.075330 0.051 Uiso 1 1 calc R U H9B H 0.645448 -0.237688 0.058627 0.051 Uiso 1 1 calc R U C10 C 0.5897(2) -0.1211(3) 0.09300(12) 0.0439(9) Uani 1 1 d . . H10A H 0.531130 -0.150153 0.081471 0.053 Uiso 1 1 calc R U H10B H 0.610317 -0.154036 0.123030 0.053 Uiso 1 1 calc R U C11 C 0.6706(2) 0.0952(3) 0.15354(11) 0.0393(9) Uani 1 1 d . U H11 H 0.623710 0.081783 0.168607 0.047 Uiso 1 1 calc R U C12 C 0.74085(12) 0.17508(18) 0.17650(7) 0.0353(8) Uani 1 1 d G . C13 C 0.80626(13) 0.21245(19) 0.15351(5) 0.0364(8) Uani 1 1 d G . C14 C 0.86870(12) 0.28846(19) 0.17456(7) 0.0357(8) Uani 1 1 d G . C15 C 0.86574(12) 0.32710(18) 0.21859(7) 0.0343(8) Uani 1 1 d G . C16 C 0.80034(13) 0.28973(19) 0.24158(5) 0.0384(9) Uani 1 1 d G . C21 C 0.73789(12) 0.21372(19) 0.22054(7) 0.0378(8) Uani 1 1 d G . C17 C 0.7880(2) 0.3357(3) 0.28437(11) 0.0385(9) Uani 1 1 d . . H17 H 0.824125 0.394013 0.296862 0.046 Uiso 1 1 calc R U C18 C 0.7246(2) 0.2975(3) 0.30813(12) 0.0402(9) Uani 1 1 d . . H18 H 0.717029 0.332020 0.335296 0.048 Uiso 1 1 calc R U C19 C 0.6728(2) 0.2084(3) 0.29154(12) 0.0434(9) Uani 1 1 d . . H19 H 0.634712 0.176231 0.308813 0.052 Uiso 1 1 calc R U C20 C 0.6789(2) 0.1681(3) 0.24850(11) 0.0405(9) Uani 1 1 d . . H20 H 0.643172 0.108666 0.236904 0.049 Uiso 1 1 calc R U C22 C 0.9372(2) 0.4006(3) 0.24217(12) 0.0387(9) Uani 1 1 d . . H22 H 0.941321 0.407969 0.273854 0.046 Uiso 1 1 calc R U C23 C 1.0670(2) 0.6195(3) 0.25298(12) 0.0436(9) Uani 1 1 d . U H23A H 1.112845 0.648823 0.276970 0.052 Uiso 1 1 calc R U H23B H 1.011647 0.652584 0.257151 0.052 Uiso 1 1 calc R U C24 C 1.0857(2) 0.6571(3) 0.20783(12) 0.0399(9) Uani 1 1 d . . H24A H 1.035222 0.640045 0.183978 0.048 Uiso 1 1 calc R U H24B H 1.093337 0.736933 0.208590 0.048 Uiso 1 1 calc R U C25 C 1.2091(2) 0.4833(3) 0.14953(12) 0.0393(9) Uani 1 1 d . . H25 H 1.260877 0.523226 0.159224 0.047 Uiso 1 1 calc R U C26 C 1.2131(2) 0.3973(3) 0.11863(12) 0.0367(8) Uani 1 1 d . . C27 C 1.2964(2) 0.3688(3) 0.10737(12) 0.0404(8) Uani 1 1 d . U H27 H 1.346678 0.406591 0.121638 0.049 Uiso 1 1 calc R U C28 C 1.3046(2) 0.2867(3) 0.07595(12) 0.0427(9) Uani 1 1 d . U H28 H 1.360225 0.265479 0.071105 0.051 Uiso 1 1 calc R U C29 C 1.2314(2) 0.2370(3) 0.05219(13) 0.0403(9) Uani 1 1 d . . H29 H 1.236914 0.188522 0.028401 0.048 Uiso 1 1 calc R U C30 C 1.1486(2) 0.2565(3) 0.06231(12) 0.0334(9) Uani 1 1 d . . C31 C 1.1392(2) 0.3372(3) 0.09586(11) 0.0353(8) Uani 1 1 d . . C32 C 1.0763(2) 0.1237(3) 0.00880(12) 0.0461(10) Uani 1 1 d . . H32A H 1.090276 0.156299 -0.018648 0.069 Uiso 1 1 calc R U H32B H 1.020894 0.085482 0.001423 0.069 Uiso 1 1 calc R U H32C H 1.121875 0.072193 0.021478 0.069 Uiso 1 1 calc R U C33 C 0.8861(2) 0.5255(3) 0.09160(12) 0.0377(9) Uani 1 1 d . . C34 C 0.8280(2) 0.6225(3) 0.07608(12) 0.0440(9) Uani 1 1 d . . H34A H 0.838072 0.679409 0.099179 0.066 Uiso 1 1 calc R U H34B H 0.767305 0.599707 0.071365 0.066 Uiso 1 1 calc R U H34C H 0.841269 0.650706 0.047735 0.066 Uiso 1 1 calc R U C35 C 0.9236(2) -0.0254(3) 0.10406(12) 0.0368(8) Uani 1 1 d . U C36 C 0.9762(2) -0.1203(3) 0.12648(12) 0.0460(9) Uani 1 1 d . . H36D H 0.939047 -0.184539 0.125252 0.069 Uiso 1 1 calc R U H36E H 0.999459 -0.102224 0.158043 0.069 Uiso 1 1 calc R U H36F H 1.023961 -0.135420 0.110635 0.069 Uiso 1 1 calc R U C37 C 0.6646(5) 0.3862(7) -0.0013(4) 0.265(6) Uiso 1 1 d D . H37A H 0.621480 0.381630 0.018755 0.318 Uiso 1 1 calc DR U H37B H 0.646970 0.336911 -0.027306 0.318 Uiso 1 1 calc R U C38 C 0.6732(5) 0.5007(7) -0.0169(3) 0.181(3) Uiso 1 1 d D . H38A H 0.665616 0.551164 0.007211 0.271 Uiso 1 1 calc R U H38B H 0.628936 0.514789 -0.043687 0.271 Uiso 1 1 calc R U H38C H 0.730730 0.510917 -0.024377 0.271 Uiso 1 1 calc R U C39 C 1.1711(5) 0.1104(6) 0.1637(3) 0.264(6) Uiso 1 1 d D . H39A H 1.171029 0.120844 0.196289 0.317 Uiso 1 1 calc DR U H39B H 1.215980 0.157812 0.154810 0.317 Uiso 1 1 calc R U C40 C 1.1870(5) -0.0063(6) 0.1536(3) 0.171(3) Uiso 1 1 d D . H40A H 1.143310 -0.051961 0.163798 0.256 Uiso 1 1 calc R U H40B H 1.244704 -0.027758 0.169479 0.256 Uiso 1 1 calc R U H40C H 1.183511 -0.015536 0.121063 0.256 Uiso 1 1 calc R U C41 C 0.5550(2) 0.2006(3) 0.02416(13) 0.0514(10) Uani 1 1 d . . H41D H 0.539214 0.123792 0.019955 0.077 Uiso 1 1 calc R U H41E H 0.544586 0.237384 -0.005173 0.077 Uiso 1 1 calc DR U H41F H 0.519789 0.234604 0.043971 0.077 Uiso 1 1 calc R U C42 C 1.1911(2) 0.2984(3) 0.23462(13) 0.0509(10) Uani 1 1 d . . H42D H 1.202679 0.374299 0.243481 0.076 Uiso 1 1 calc R U H42E H 1.239980 0.269135 0.222435 0.076 Uiso 1 1 calc DR U H42F H 1.183248 0.255849 0.261048 0.076 Uiso 1 1 calc R U C43 C 0.6141(3) 0.4337(3) 0.11689(13) 0.0552(11) Uani 1 1 d . . H43 H 0.646097 0.384339 0.099316 0.066 Uiso 1 1 calc R U C44 C 0.4829(2) 0.5654(3) 0.24844(13) 0.0497(10) Uani 1 1 d . . H44 H 0.471509 0.615696 0.272738 0.060 Uiso 1 1 calc R U Ca1 Ca 0.92678(4) 0.24931(5) 0.07350(2) 0.02913(17) Uani 1 1 d . . Cl1 Cl 0.68758(6) 0.50144(9) 0.15685(3) 0.0590(3) Uani 1 1 d . . Cl2 Cl 0.55048(7) 0.52513(10) 0.07926(4) 0.0613(3) Uani 1 1 d . . Cl3 Cl 0.54143(6) 0.35365(9) 0.14372(4) 0.0562(3) Uani 1 1 d . . Cl4 Cl 0.47163(7) 0.64265(9) 0.19577(3) 0.0577(3) Uani 1 1 d . . Cl5 Cl 0.39963(7) 0.46527(10) 0.23959(4) 0.0621(3) Uani 1 1 d . . Cl6 Cl 0.58186(6) 0.51266(9) 0.26448(3) 0.0569(3) Uani 1 1 d . . N1 N 0.68151(17) -0.0139(2) 0.01163(10) 0.0393(7) Uani 1 1 d . . N2 N 0.66946(17) 0.0444(2) 0.11542(9) 0.0380(7) Uani 1 1 d . U N3 N 0.99423(17) 0.4557(2) 0.22430(9) 0.0362(7) Uani 1 1 d . . N4 N 1.14154(17) 0.5131(2) 0.16600(10) 0.0410(7) Uani 1 1 d . . Ni1 Ni 0.74540(3) 0.07967(4) 0.06659(2) 0.03529(13) Uani 1 1 d . . Ni2 Ni 1.02916(3) 0.41904(4) 0.16173(2) 0.03508(13) Uani 1 1 d . . O1 O 0.90180(14) 0.2906(2) -0.01468(8) 0.0402(6) Uani 1 1 d . U O2 O 0.81836(14) 0.14268(19) 0.02248(7) 0.0374(6) Uani 1 1 d . . O3 O 0.62787(14) -0.1086(2) 0.01652(8) 0.0415(6) Uani 1 1 d . U O4 O 0.58300(13) -0.0065(2) 0.09867(8) 0.0399(6) Uani 1 1 d . . O5 O 0.80669(13) 0.19220(19) 0.10878(7) 0.0370(6) Uani 1 1 d . . O6 O 0.93595(13) 0.30541(19) 0.15237(7) 0.0372(6) Uani 1 1 d . . O7 O 1.06139(14) 0.5027(2) 0.26002(8) 0.0422(6) Uani 1 1 d . U O8 O 1.16288(14) 0.6066(2) 0.19617(8) 0.0416(6) Uani 1 1 d . . O9 O 1.05734(13) 0.35478(19) 0.10300(7) 0.0372(6) Uani 1 1 d . . O10 O 1.07041(14) 0.2087(2) 0.04172(8) 0.0420(6) Uani 1 1 d . . O11 O 0.94499(14) 0.53731(19) 0.12581(8) 0.0386(6) Uani 1 1 d . . O12 O 0.87244(14) 0.4356(2) 0.06765(8) 0.0407(6) Uani 1 1 d . . O13 O 0.96443(14) 0.06221(19) 0.09810(8) 0.0395(6) Uani 1 1 d . U O14 O 0.84243(14) -0.03672(19) 0.09069(7) 0.0393(6) Uani 1 1 d . . O15 O 0.64676(14) 0.2096(2) 0.04469(8) 0.0430(6) Uani 1 1 d . . H15A H 0.684799 0.206238 0.027228 0.052 Uiso 1 1 d R U O16 O 1.11270(14) 0.2923(2) 0.20023(8) 0.0413(6) Uani 1 1 d . . H16A H 1.066661 0.285256 0.212021 0.050 Uiso 1 1 d R U O17 O 0.7388(4) 0.3627(6) 0.0197(2) 0.228(3) Uiso 1 1 d D . H17C H 0.761271 0.397729 0.044023 0.342 Uiso 1 1 d R U O18 O 1.0981(5) 0.1308(6) 0.1406(2) 0.226(3) Uiso 1 1 d D . H18C H 1.052132 0.098019 0.145843 0.339 Uiso 1 1 d R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(2) 0.042(3) 0.041(2) 0.0105(17) 0.0082(17) -0.0090(17) C2 0.0279(18) 0.040(2) 0.030(2) 0.0076(14) 0.0056(14) 0.0068(13) C3 0.037(2) 0.036(2) 0.035(2) 0.0047(16) 0.0092(16) 0.0073(16) C4 0.0320(19) 0.047(3) 0.034(2) -0.0079(17) 0.0067(16) 0.0084(16) C5 0.043(2) 0.041(2) 0.042(2) -0.0055(18) -0.0062(17) -0.0066(17) C6 0.047(2) 0.060(3) 0.035(2) 0.011(2) 0.0074(19) 0.000(2) C7 0.043(2) 0.044(3) 0.028(2) 0.0077(16) 0.0081(18) 0.0074(16) C8 0.034(2) 0.040(2) 0.039(2) -0.0096(18) -0.0063(16) 0.0050(16) C9 0.044(2) 0.036(2) 0.0475(19) 0.0077(16) 0.0105(17) -0.0118(16) C10 0.047(2) 0.047(3) 0.038(2) -0.0102(18) 0.0068(17) -0.0196(18) C11 0.036(2) 0.051(3) 0.0319(18) -0.0114(15) 0.0089(16) -0.0163(16) C12 0.0318(18) 0.041(2) 0.034(2) -0.0077(16) 0.0088(15) -0.0063(15) C13 0.039(2) 0.042(2) 0.0282(19) -0.0076(16) 0.0075(16) 0.0114(17) C14 0.0351(19) 0.038(2) 0.037(2) 0.0102(17) 0.0126(16) -0.0075(16) C15 0.0325(18) 0.039(2) 0.033(2) -0.0041(16) 0.0086(15) -0.0023(15) C16 0.0339(19) 0.051(3) 0.031(2) -0.0078(17) 0.0070(16) -0.0087(17) C21 0.035(2) 0.048(2) 0.033(2) 0.0094(17) 0.0105(16) -0.0036(17) C17 0.036(2) 0.043(2) 0.037(2) -0.0102(17) 0.0086(16) -0.0083(16) C18 0.040(2) 0.046(3) 0.037(2) -0.0102(17) 0.0139(17) -0.0105(17) C19 0.047(2) 0.047(3) 0.040(2) -0.0076(18) 0.0179(18) -0.0096(18) C20 0.044(2) 0.042(2) 0.038(2) -0.0093(17) 0.0120(17) -0.0132(16) C22 0.035(2) 0.049(3) 0.034(2) -0.0113(17) 0.0101(16) 0.0029(16) C23 0.041(2) 0.0467(19) 0.043(2) -0.0154(17) 0.0064(17) -0.0134(17) C24 0.041(2) 0.034(2) 0.046(2) -0.0121(17) 0.0103(17) 0.0041(16) C25 0.037(2) 0.039(2) 0.040(2) 0.0106(17) 0.0048(16) -0.0017(16) C26 0.0323(19) 0.041(2) 0.037(2) 0.0106(17) 0.0085(16) -0.0055(16) C27 0.0338(19) 0.040(2) 0.048(2) 0.0058(15) 0.0108(17) 0.0055(16) C28 0.033(2) 0.055(3) 0.043(2) -0.0049(17) 0.0142(17) -0.0047(18) C29 0.038(2) 0.040(3) 0.046(2) 0.0079(17) 0.0143(19) 0.0075(16) C30 0.037(2) 0.035(2) 0.030(2) 0.0036(14) 0.0090(17) 0.0061(15) C31 0.040(2) 0.034(2) 0.0341(19) 0.0109(16) 0.0109(16) -0.0078(15) C32 0.046(2) 0.042(3) 0.053(2) -0.0172(19) 0.0179(19) -0.0083(17) C33 0.051(2) 0.027(2) 0.037(2) -0.0066(17) 0.0150(18) -0.0118(17) C34 0.038(2) 0.045(3) 0.047(2) -0.0070(18) 0.0041(17) 0.0091(17) C35 0.036(2) 0.038(2) 0.038(2) -0.0108(17) 0.0108(16) -0.0052(15) C36 0.043(2) 0.040(3) 0.049(2) 0.0081(18) -0.0064(17) -0.0119(17) C41 0.038(2) 0.060(3) 0.055(3) -0.018(2) 0.0072(19) -0.0064(19) C42 0.047(2) 0.049(3) 0.049(2) -0.007(2) -0.0120(19) -0.0081(19) C43 0.059(3) 0.058(3) 0.043(2) -0.015(2) -0.0039(19) 0.015(2) C44 0.045(2) 0.054(3) 0.051(2) -0.0198(19) 0.0123(19) -0.0092(18) Ca1 0.0282(4) 0.0312(5) 0.0286(4) -0.0059(3) 0.0068(3) -0.0070(3) Cl1 0.0483(6) 0.0674(8) 0.0542(6) -0.0101(5) -0.0096(5) -0.0119(5) Cl2 0.0560(6) 0.0693(8) 0.0573(7) 0.0135(6) 0.0074(5) 0.0122(5) Cl3 0.0515(6) 0.0544(7) 0.0637(7) -0.0093(5) 0.0130(5) -0.0089(5) Cl4 0.0651(7) 0.0536(7) 0.0546(6) 0.0138(5) 0.0115(5) 0.0108(5) Cl5 0.0547(6) 0.0675(8) 0.0556(6) 0.0132(6) -0.0119(5) -0.0162(5) Cl6 0.0483(6) 0.0616(8) 0.0534(6) 0.0082(5) -0.0101(5) -0.0084(5) N1 0.0332(16) 0.042(2) 0.0445(19) -0.0136(15) 0.0120(14) -0.0100(13) N2 0.0383(16) 0.0385(19) 0.0399(16) -0.0056(13) 0.0142(14) -0.0146(13) N3 0.0370(16) 0.0367(19) 0.0356(16) -0.0112(13) 0.0085(13) -0.0086(13) N4 0.0324(16) 0.043(2) 0.0425(18) -0.0051(14) -0.0067(13) -0.0030(13) Ni1 0.0341(3) 0.0381(3) 0.0345(3) -0.0085(2) 0.0085(2) -0.00876(19) Ni2 0.0345(3) 0.0367(3) 0.0349(3) -0.0079(2) 0.0087(2) -0.00849(19) O1 0.0399(14) 0.0448(16) 0.0373(14) -0.0044(12) 0.0109(11) -0.0107(11) O2 0.0398(13) 0.0410(16) 0.0322(13) -0.0109(11) 0.0089(11) -0.0063(11) O3 0.0440(14) 0.0436(17) 0.0364(13) -0.0093(11) 0.0056(11) -0.0140(11) O4 0.0326(13) 0.0439(17) 0.0457(14) 0.0071(12) 0.0137(11) -0.0076(11) O5 0.0399(13) 0.0402(16) 0.0320(13) -0.0068(11) 0.0093(10) -0.0101(11) O6 0.0345(13) 0.0405(16) 0.0383(14) -0.0107(11) 0.0109(11) -0.0112(11) O7 0.0484(14) 0.0446(15) 0.0348(13) -0.0059(11) 0.0106(11) -0.0070(12) O8 0.0380(14) 0.0400(16) 0.0481(15) -0.0134(12) 0.0115(11) -0.0068(11) O9 0.0314(13) 0.0397(16) 0.0417(14) -0.0066(11) 0.0102(11) -0.0079(10) O10 0.0402(14) 0.0467(17) 0.0418(15) -0.0141(12) 0.0144(12) -0.0109(12) O11 0.0374(14) 0.0385(16) 0.0398(15) -0.0081(11) 0.0070(12) -0.0075(11) O12 0.0371(14) 0.0424(17) 0.0382(14) -0.0078(11) -0.0050(11) -0.0074(11) O13 0.0348(14) 0.0364(15) 0.0428(14) 0.0094(11) -0.0043(11) 0.0037(10) O14 0.0376(14) 0.0367(16) 0.0387(14) -0.0055(11) -0.0058(11) -0.0069(11) O15 0.0310(13) 0.0478(17) 0.0458(15) -0.0077(12) -0.0048(11) -0.0066(11) O16 0.0355(14) 0.0458(17) 0.0427(15) -0.0053(12) 0.0076(11) -0.0059(11) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 O1 C1 H1A 109.5 O1 C1 H1B 109.5 H1A C1 H1B 109.5 O1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C7 C2 O1 128.1(3) C7 C2 C3 119.8(3) O1 C2 C3 112.0(3) O2 C3 C4 123.7(3) O2 C3 C2 118.1(3) C4 C3 C2 118.2(3) C3 C4 C5 118.5(3) C3 C4 C8 123.4(3) C5 C4 C8 118.2(3) C6 C5 C4 119.9(3) C6 C5 H5 120.0 C4 C5 H5 120.0 C7 C6 C5 119.1(4) C7 C6 H6 120.4 C5 C6 H6 120.4 C6 C7 C2 124.1(4) C6 C7 H7 118.0 C2 C7 H7 118.0 N1 C8 C4 126.4(3) N1 C8 H8 116.8 C4 C8 H8 116.8 O3 C9 C10 113.4(3) O3 C9 H9A 108.9 C10 C9 H9A 108.9 O3 C9 H9B 108.9 C10 C9 H9B 108.9 H9A C9 H9B 107.7 O4 C10 C9 115.9(3) O4 C10 H10A 108.3 C9 C10 H10A 108.3 O4 C10 H10B 108.3 C9 C10 H10B 108.3 H10A C10 H10B 107.4 N2 C11 C12 126.3(3) N2 C11 H11 116.8 C12 C11 H11 116.8 C13 C12 C21 120.0 C13 C12 C11 120.72(17) C21 C12 C11 119.25(17) O5 C13 C12 123.80(16) O5 C13 C14 115.51(16) C12 C13 C14 120.0 O6 C14 C13 114.58(16) O6 C14 C15 124.62(16) C13 C14 C15 120.0 C16 C15 C14 120.0 C16 C15 C22 120.44(17) C14 C15 C22 119.35(17) C21 C16 C15 120.0 C21 C16 C17 117.31(18) C15 C16 C17 122.30(18) C16 C21 C12 120.0 C16 C21 C20 116.89(18) C12 C21 C20 122.66(19) C18 C17 C16 122.9(3) C18 C17 H17 118.6 C16 C17 H17 118.6 C17 C18 C19 119.9(3) C17 C18 H18 120.1 C19 C18 H18 120.1 C20 C19 C18 118.0(3) C20 C19 H19 121.0 C18 C19 H19 121.0 C19 C20 C21 123.3(3) C19 C20 H20 118.3 C21 C20 H20 118.3 N3 C22 C15 128.2(3) N3 C22 H22 115.9 C15 C22 H22 115.9 O7 C23 C24 117.3(3) O7 C23 H23A 108.0 C24 C23 H23A 108.0 O7 C23 H23B 108.0 C24 C23 H23B 108.0 H23A C23 H23B 107.2 O8 C24 C23 113.1(3) O8 C24 H24A 109.0 C23 C24 H24A 109.0 O8 C24 H24B 109.0 C23 C24 H24B 109.0 H24A C24 H24B 107.8 N4 C25 C26 126.6(3) N4 C25 H25 116.7 C26 C25 H25 116.7 C25 C26 C31 124.5(3) C25 C26 C27 118.9(3) C31 C26 C27 116.5(3) C28 C27 C26 121.9(3) C28 C27 H27 119.0 C26 C27 H27 119.0 C29 C28 C27 119.7(3) C29 C28 H28 120.1 C27 C28 H28 120.1 C28 C29 C30 121.8(4) C28 C29 H29 119.1 C30 C29 H29 119.1 O10 C30 C29 127.1(3) O10 C30 C31 113.8(3) C29 C30 C31 119.1(3) O9 C31 C26 123.1(3) O9 C31 C30 116.2(3) C26 C31 C30 120.6(3) O10 C32 H32A 109.5 O10 C32 H32B 109.5 H32A C32 H32B 109.5 O10 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 O11 C33 O12 124.5(3) O11 C33 C34 118.0(3) O12 C33 C34 117.5(3) C33 C34 H34A 109.5 C33 C34 H34B 109.5 H34A C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 O14 C35 O13 123.0(3) O14 C35 C36 119.3(3) O13 C35 C36 117.7(3) C35 C36 H36D 109.5 C35 C36 H36E 109.5 H36D C36 H36E 109.5 C35 C36 H36F 109.5 H36D C36 H36F 109.5 H36E C36 H36F 109.5 O17 C37 C38 104.3(7) O17 C37 H37A 110.9 C38 C37 H37A 110.9 O17 C37 H37B 110.9 C38 C37 H37B 110.9 H37A C37 H37B 108.9 C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 O18 C39 C40 104.4(7) O18 C39 H39A 110.9 C40 C39 H39A 110.9 O18 C39 H39B 110.9 C40 C39 H39B 110.9 H39A C39 H39B 108.9 C39 C40 H40A 109.5 C39 C40 H40B 109.5 H40A C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 O15 C41 H41D 109.5 O15 C41 H41E 109.5 H41D C41 H41E 109.5 O15 C41 H41F 109.5 H41D C41 H41F 109.5 H41E C41 H41F 109.5 O16 C42 H42D 109.5 O16 C42 H42E 109.5 H42D C42 H42E 109.5 O16 C42 H42F 109.5 H42D C42 H42F 109.5 H42E C42 H42F 109.5 Cl1 C43 Cl2 111.5(2) Cl1 C43 Cl3 110.4(2) Cl2 C43 Cl3 107.7(2) Cl1 C43 H43 109.1 Cl2 C43 H43 109.1 Cl3 C43 H43 109.1 Cl6 C44 Cl5 113.2(2) Cl6 C44 Cl4 112.9(2) Cl5 C44 Cl4 106.2(2) Cl6 C44 H44 108.2 Cl5 C44 H44 108.2 Cl4 C44 H44 108.2 O5 Ca1 O12 90.77(8) O5 Ca1 O6 64.54(7) O12 Ca1 O6 76.28(8) O5 Ca1 O2 67.31(7) O12 Ca1 O2 105.29(8) O6 Ca1 O2 131.84(7) O5 Ca1 O9 131.22(8) O12 Ca1 O9 77.73(8) O6 Ca1 O9 66.68(7) O2 Ca1 O9 161.47(8) O5 Ca1 O13 76.17(8) O12 Ca1 O13 164.39(8) O6 Ca1 O13 90.21(8) O2 Ca1 O13 77.80(8) O9 Ca1 O13 104.34(8) O5 Ca1 O10 151.85(8) O12 Ca1 O10 117.38(8) O6 Ca1 O10 119.98(8) O2 Ca1 O10 102.24(7) O9 Ca1 O10 61.33(7) O13 Ca1 O10 76.06(8) O5 Ca1 O1 120.48(8) O12 Ca1 O1 76.33(8) O6 Ca1 O1 152.21(8) O2 Ca1 O1 61.28(7) O9 Ca1 O1 102.73(7) O13 Ca1 O1 117.57(8) O10 Ca1 O1 69.83(7) O5 Ca1 Ni1 33.61(5) O12 Ca1 Ni1 106.54(6) O6 Ca1 Ni1 97.29(5) O2 Ca1 Ni1 35.10(5) O9 Ca1 Ni1 162.35(6) O13 Ca1 Ni1 66.94(5) O10 Ca1 Ni1 127.00(6) O1 Ca1 Ni1 94.91(5) O5 Ca1 Ni2 97.16(6) O12 Ca1 Ni2 66.62(5) O6 Ca1 Ni2 33.51(5) O2 Ca1 Ni2 162.99(5) O9 Ca1 Ni2 34.75(5) O13 Ca1 Ni2 106.05(6) O10 Ca1 Ni2 94.75(5) O1 Ca1 Ni2 127.01(6) Ni1 Ca1 Ni2 130.53(2) C8 N1 O3 110.6(3) C8 N1 Ni1 124.2(3) O3 N1 Ni1 123.7(2) C11 N2 O4 111.2(2) C11 N2 Ni1 126.8(2) O4 N2 Ni1 116.61(18) C22 N3 O7 110.7(3) C22 N3 Ni2 124.4(2) O7 N3 Ni2 117.76(17) C25 N4 O8 110.3(3) C25 N4 Ni2 123.9(3) O8 N4 Ni2 124.42(19) O5 Ni1 O2 83.63(9) O5 Ni1 N2 88.15(10) O2 Ni1 N2 169.72(10) O5 Ni1 N1 167.96(11) O2 Ni1 N1 86.59(10) N2 Ni1 N1 100.74(11) O5 Ni1 O14 91.05(9) O2 Ni1 O14 91.39(9) N2 Ni1 O14 94.94(11) N1 Ni1 O14 96.21(10) O5 Ni1 O15 85.37(9) O2 Ni1 O15 88.79(9) N2 Ni1 O15 84.38(10) N1 Ni1 O15 87.42(10) O14 Ni1 O15 176.37(9) O5 Ni1 Ca1 42.29(6) O2 Ni1 Ca1 43.23(6) N2 Ni1 Ca1 129.88(8) N1 Ni1 Ca1 129.38(8) O14 Ni1 Ca1 81.74(6) O15 Ni1 Ca1 95.95(6) O5 Ni1 H15A 87.7 O2 Ni1 H15A 66.5 N2 Ni1 H15A 107.1 N1 Ni1 H15A 81.9 O14 Ni1 H15A 157.9 O15 Ni1 H15A 22.8 Ca1 Ni1 H15A 82.5 O6 Ni2 O9 83.04(8) O6 Ni2 N3 88.35(10) O9 Ni2 N3 169.62(10) O6 Ni2 N4 168.08(11) O9 Ni2 N4 87.27(10) N3 Ni2 N4 100.51(11) O6 Ni2 O11 92.06(9) O9 Ni2 O11 92.18(9) N3 Ni2 O11 93.92(10) N4 Ni2 O11 95.25(10) O6 Ni2 O16 85.99(9) O9 Ni2 O16 88.79(9) N3 Ni2 O16 84.83(10) N4 Ni2 O16 86.88(10) O11 Ni2 O16 177.70(8) O6 Ni2 Ca1 42.42(6) O9 Ni2 Ca1 42.75(6) N3 Ni2 Ca1 130.02(7) N4 Ni2 Ca1 129.47(8) O11 Ni2 Ca1 82.36(6) O16 Ni2 Ca1 96.96(6) C2 O1 C1 114.6(3) C2 O1 Ca1 119.96(18) C1 O1 Ca1 124.30(19) C3 O2 Ni1 124.12(19) C3 O2 Ca1 127.3(2) Ni1 O2 Ca1 101.67(9) N1 O3 C9 112.6(2) C10 O4 N2 111.8(2) C13 O5 Ni1 131.31(17) C13 O5 Ca1 121.41(15) Ni1 O5 Ca1 104.10(9) C14 O6 Ni2 130.38(17) C14 O6 Ca1 121.21(15) Ni2 O6 Ca1 104.07(9) C23 O7 N3 109.5(2) C24 O8 N4 112.2(2) C31 O9 Ni2 123.81(19) C31 O9 Ca1 127.7(2) Ni2 O9 Ca1 102.50(8) C30 O10 C32 116.2(2) C30 O10 Ca1 119.78(19) C32 O10 Ca1 123.09(18) C33 O11 Ni2 129.2(2) C33 O12 Ca1 136.9(2) C35 O13 Ca1 136.9(2) C35 O14 Ni1 130.6(2) C41 O15 Ni1 130.1(2) C41 O15 H15A 118.4 Ni1 O15 H15A 68.1 C42 O16 Ni2 132.4(2) C42 O16 H16A 111.9 Ni2 O16 H16A 80.0 C37 O17 H17C 120.5 C39 O18 H18C 121.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 O1 1.426(4) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C2 C7 1.361(5) C2 O1 1.382(4) C2 C3 1.425(4) C3 O2 1.310(4) C3 C4 1.407(5) C4 C5 1.435(5) C4 C8 1.436(5) C5 C6 1.413(5) C5 H5 0.9300 C6 C7 1.309(5) C6 H6 0.9300 C7 H7 0.9300 C8 N1 1.229(4) C8 H8 0.9300 C9 O3 1.440(4) C9 C10 1.481(4) C9 H9A 0.9700 C9 H9B 0.9700 C10 O4 1.399(4) C10 H10A 0.9700 C10 H10B 0.9700 C11 N2 1.279(4) C11 C12 1.513(3) C11 H11 0.9300 C12 C13 1.3900 C12 C21 1.3900 C13 O5 1.345(2) C13 C14 1.3900 C14 O6 1.340(2) C14 C15 1.3900 C15 C16 1.3900 C15 C22 1.483(4) C16 C21 1.3900 C16 C17 1.424(3) C21 C20 1.445(3) C17 C18 1.383(4) C17 H17 0.9300 C18 C19 1.374(5) C18 H18 0.9300 C19 C20 1.380(4) C19 H19 0.9300 C20 H20 0.9300 C22 N3 1.290(4) C22 H22 0.9300 C23 O7 1.430(4) C23 C24 1.486(4) C23 H23A 0.9700 C23 H23B 0.9700 C24 O8 1.434(4) C24 H24A 0.9700 C24 H24B 0.9700 C25 N4 1.280(4) C25 C26 1.390(5) C25 H25 0.9300 C26 C31 1.412(5) C26 C27 1.427(4) C27 C28 1.379(5) C27 H27 0.9300 C28 C29 1.354(5) C28 H28 0.9300 C29 C30 1.382(4) C29 H29 0.9300 C30 O10 1.373(4) C30 C31 1.416(5) C31 O9 1.333(4) C32 O10 1.427(4) C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 O11 1.235(4) C33 O12 1.290(4) C33 C34 1.493(5) C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600 C35 O14 1.248(4) C35 O13 1.259(4) C35 C36 1.485(5) C36 H36D 0.9600 C36 H36E 0.9600 C36 H36F 0.9600 C37 O17 1.2289(10) C37 C38 1.4690(10) C37 H37A 0.9700 C37 H37B 0.9700 C38 H38A 0.9600 C38 H38B 0.9600 C38 H38C 0.9600 C39 O18 1.2287(10) C39 C40 1.4691(10) C39 H39A 0.9700 C39 H39B 0.9700 C40 H40A 0.9600 C40 H40B 0.9600 C40 H40C 0.9600 C41 O15 1.436(4) C41 H41D 0.9600 C41 H41E 0.9600 C41 H41F 0.9600 C42 O16 1.429(4) C42 H42D 0.9600 C42 H42E 0.9600 C42 H42F 0.9600 C43 Cl1 1.688(4) C43 Cl2 1.736(4) C43 Cl3 1.773(4) C43 H43 0.9800 C44 Cl6 1.639(4) C44 Cl5 1.747(4) C44 Cl4 1.794(4) C44 H44 0.9800 Ca1 O5 2.386(2) Ca1 O12 2.393(2) Ca1 O6 2.404(2) Ca1 O2 2.405(2) Ca1 O9 2.404(2) Ca1 O13 2.409(2) Ca1 O10 2.605(2) Ca1 O1 2.609(2) Ca1 Ni1 3.4395(8) Ca1 Ni2 3.4572(8) N1 O3 1.433(3) N1 Ni1 2.071(3) N2 O4 1.467(3) N2 Ni1 2.062(2) N3 O7 1.450(3) N3 Ni2 2.066(3) N4 O8 1.437(3) N4 Ni2 2.055(3) Ni1 O5 1.963(2) Ni1 O2 2.020(2) Ni1 O14 2.079(2) Ni1 O15 2.196(2) Ni1 H15A 2.0381 Ni2 O6 1.968(2) Ni2 O9 2.018(2) Ni2 O11 2.082(2) Ni2 O16 2.179(2) O15 H15A 0.8500 O16 H16A 0.8501 O17 H17C 0.8499 O18 H18C 0.8500 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 C7 C2 C3 O2 177.7(3) O1 C2 C3 O2 0.8(4) C7 C2 C3 C4 -1.7(5) O1 C2 C3 C4 -178.5(3) O2 C3 C4 C5 178.6(3) C2 C3 C4 C5 -2.1(5) O2 C3 C4 C8 -2.6(5) C2 C3 C4 C8 176.7(3) C3 C4 C5 C6 1.9(5) C8 C4 C5 C6 -177.0(3) C4 C5 C6 C7 2.3(6) C5 C6 C7 C2 -6.6(6) O1 C2 C7 C6 -177.4(3) C3 C2 C7 C6 6.3(5) C3 C4 C8 N1 7.0(6) C5 C4 C8 N1 -174.2(3) O3 C9 C10 O4 -54.7(4) N2 C11 C12 C13 9.4(5) N2 C11 C12 C21 -172.6(3) C21 C12 C13 O5 -170.0(2) C11 C12 C13 O5 8.0(3) C21 C12 C13 C14 0.0 C11 C12 C13 C14 178.0(3) O5 C13 C14 O6 -19.0(2) C12 C13 C14 O6 170.2(2) O5 C13 C14 C15 170.8(2) C12 C13 C14 C15 0.0 O6 C14 C15 C16 -169.2(2) C13 C14 C15 C16 0.0 O6 C14 C15 C22 5.6(3) C13 C14 C15 C22 174.8(3) C14 C15 C16 C21 0.0 C22 C15 C16 C21 -174.7(3) C14 C15 C16 C17 -172.6(3) C22 C15 C16 C17 12.6(3) C15 C16 C21 C12 0.0 C17 C16 C21 C12 173.0(3) C15 C16 C21 C20 172.5(3) C17 C16 C21 C20 -14.5(3) C13 C12 C21 C16 0.0 C11 C12 C21 C16 -178.0(3) C13 C12 C21 C20 -172.0(3) C11 C12 C21 C20 9.9(3) C21 C16 C17 C18 8.8(4) C15 C16 C17 C18 -178.4(3) C16 C17 C18 C19 2.8(6) C17 C18 C19 C20 -7.6(6) C18 C19 C20 C21 1.1(6) C16 C21 C20 C19 10.3(4) C12 C21 C20 C19 -177.4(3) C16 C15 C22 N3 -168.5(3) C14 C15 C22 N3 16.8(5) O7 C23 C24 O8 -53.3(4) N4 C25 C26 C31 8.3(6) N4 C25 C26 C27 -173.9(3) C25 C26 C27 C28 -178.0(3) C31 C26 C27 C28 -0.1(5) C26 C27 C28 C29 5.3(6) C27 C28 C29 C30 -8.0(6) C28 C29 C30 O10 -177.8(3) C28 C29 C30 C31 5.3(5) C25 C26 C31 O9 -2.4(5) C27 C26 C31 O9 179.9(3) C25 C26 C31 C30 175.2(3) C27 C26 C31 C30 -2.5(5) O10 C30 C31 O9 0.6(4) C29 C30 C31 O9 177.9(3) O10 C30 C31 C26 -177.2(3) C29 C30 C31 C26 0.1(5) C4 C8 N1 O3 -176.4(3) C4 C8 N1 Ni1 16.9(5) C12 C11 N2 O4 -167.5(3) C12 C11 N2 Ni1 -14.7(5) C15 C22 N3 O7 -170.6(3) C15 C22 N3 Ni2 -21.1(5) C26 C25 N4 O8 -178.9(3) C26 C25 N4 Ni2 14.2(5) C7 C2 O1 C1 5.5(5) C3 C2 O1 C1 -178.0(3) C7 C2 O1 Ca1 173.9(3) C3 C2 O1 Ca1 -9.6(3) C4 C3 O2 Ni1 -25.5(4) C2 C3 O2 Ni1 155.2(2) C4 C3 O2 Ca1 -170.9(2) C2 C3 O2 Ca1 9.8(4) C8 N1 O3 C9 170.8(3) Ni1 N1 O3 C9 -22.5(3) C10 C9 O3 N1 97.2(3) C9 C10 O4 N2 -57.2(4) C11 N2 O4 C10 -121.8(3) Ni1 N2 O4 C10 82.4(3) C12 C13 O5 Ni1 -19.3(3) C14 C13 O5 Ni1 170.22(15) C12 C13 O5 Ca1 -175.81(12) C14 C13 O5 Ca1 13.7(2) C13 C14 O6 Ni2 168.99(15) C15 C14 O6 Ni2 -21.3(3) C13 C14 O6 Ca1 16.3(2) C15 C14 O6 Ca1 -173.99(12) C24 C23 O7 N3 -57.0(3) C22 N3 O7 C23 -125.6(3) Ni2 N3 O7 C23 82.6(3) C23 C24 O8 N4 97.4(3) C25 N4 O8 C24 167.9(3) Ni2 N4 O8 C24 -25.3(4) C26 C31 O9 Ni2 -25.4(4) C30 C31 O9 Ni2 156.9(2) C26 C31 O9 Ca1 -173.3(2) C30 C31 O9 Ca1 9.0(4) C29 C30 O10 C32 5.2(5) C31 C30 O10 C32 -177.8(3) C29 C30 O10 Ca1 174.5(3) C31 C30 O10 Ca1 -8.4(4) O12 C33 O11 Ni2 -8.9(5) C34 C33 O11 Ni2 172.7(2) O11 C33 O12 Ca1 7.8(5) C34 C33 O12 Ca1 -173.8(2) O14 C35 O13 Ca1 10.8(5) C36 C35 O13 Ca1 -171.6(2) O13 C35 O14 Ni1 -11.9(5) C36 C35 O14 Ni1 170.5(2)