#------------------------------------------------------------------------------ #$Date: 2020-06-03 01:48:43 +0300 (Wed, 03 Jun 2020) $ #$Revision: 252548 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/50/4135046.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_4135046 loop_ _publ_author_name 'McNeece, Andrew J.' 'Jesse, Kate' 'Xie, Jiaze' 'Filatov, Alexander S.' 'Anderson, John S.' _publ_section_title ; Generation and Oxidative Reactivity of a Ni(II) Superoxo Complex via Ligand-Based Redox Non-Innocence. ; _journal_name_full 'Journal of the American Chemical Society' _journal_paper_doi 10.1021/jacs.0c03244 _journal_year 2020 _chemical_formula_moiety 'C58 H68 F6 N10 Ni2 O6 S2' _chemical_formula_sum 'C58 H68 F6 N10 Ni2 O6 S2' _chemical_formula_weight 1296.76 _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 geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-12-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 71.701(12) _cell_angle_beta 76.170(11) _cell_angle_gamma 69.672(13) _cell_formula_units_Z 2 _cell_length_a 12.197(6) _cell_length_b 15.166(8) _cell_length_c 21.970(11) _cell_measurement_reflns_used 9910 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 19.93 _cell_measurement_theta_min 2.83 _cell_volume 3579(3) _computing_cell_refinement 'SAINT V.8.35A (Bruker AXS Inc., 2013)' _computing_data_collection 'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V.8.35A (Bruker AXS Inc., 2013)' _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program Dolomanov et al., 2009 Mercury: visualization and analysis of crystal structures Macrae, et al., 2006 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann. J. Appl. Cryst. (2009). 42, 339-341; C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457. ; _computing_publication_material ; APEX3 v.2015.5-2 (Bruker AXS Inc., 2015) OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement 'XL-2018/3 (Sheldrick, 2015b)' _computing_structure_solution 'XT 2014/5 (Sheldrick, 2015a)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker PHOTON 100' _diffrn_detector_area_resol_mean 10.4167 _diffrn_detector_type CMOS _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator mirrors _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_unetI/netI 0.0739 _diffrn_reflns_Laue_measured_fraction_full 0.958 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 18028 _diffrn_reflns_point_group_measured_fraction_full 0.958 _diffrn_reflns_point_group_measured_fraction_max 0.958 _diffrn_reflns_theta_full 18.809 _diffrn_reflns_theta_max 18.809 _diffrn_reflns_theta_min 2.146 _diffrn_source 'micro-focus X-ray tube' _diffrn_source_type 'INCOATEC ImuS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_correction_T_min 0.3798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1452 before and 0.1060 after correction. The Ratio of minimum to maximum transmission is 0.6569. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.203 _exptl_crystal_description block _exptl_crystal_F_000 1352 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _refine_diff_density_max 1.482 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 883 _refine_ls_number_reflns 5349 _refine_ls_number_restraints 1703 _refine_ls_restrained_S_all 0.917 _refine_ls_R_factor_all 0.1917 _refine_ls_R_factor_gt 0.1592 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+178.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3329 _refine_ls_wR_factor_ref 0.3534 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3820 _reflns_number_total 5349 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja0c03244_si_003.cif _cod_data_source_block Ni _cod_database_code 4135046 _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_max 0.870 _shelx_estimated_absorpt_t_min 0.800 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances S1-C61 = S4-C62 1.81 with sigma of 0.005 F2-C61 1.32 with sigma of 0.01 F6A-C62A = F6-C62 1.32 with sigma of 0.01 S1A-O2A \\sim S1-O2 with sigma of 0.01 S1A-C61A \\sim S1-C61 with sigma of 0.01 F2A-C61A \\sim F3-C61 \\sim F1-C61 \\sim F3A-C61A \\sim F2-C61 \\sim F1A-C61A with sigma of 0.005 F3-F1 \\sim F1-F2 \\sim F3-F2 with sigma of 0.005 F2A-F1A \\sim F1A-F3A \\sim F2A-F3A with sigma of 0.005 S4-O4 \\sim S4A-O4A with sigma of 0.01 S4-C62 \\sim S4A-C62A with sigma of 0.01 F4-C62 \\sim F6-C62 \\sim F5-C62 \\sim F5A-C62A \\sim F4A-C62A \\sim F6A-C62A with sigma of 0.01 F4-F6 \\sim F6-F5 \\sim F4-F5 with sigma of 0.01 F4A-F6A \\sim F6A-F5A \\sim F4A-F5A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 5. Others Sof(S1A)=Sof(O2A)=Sof(C61A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1) Sof(S1)=Sof(O2)=Sof(C61)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1) Sof(S4A)=Sof(O4A)=Sof(C62A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2) Sof(S4)=Sof(O4)=Sof(C62)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2) 6.a Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C19(H19), C20(H20), C22(H22), C23(H23), C39(H39), C40(H40), C42(H42), C43(H43), C46(H46), C47(H47), C51(H51), C52(H52), C54(H54), C55(H55) 6.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C24(H24A, H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B, H37C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A, H60B,H60C) ; _shelx_res_file ; TITL 12_3_try_a.res in P-1 2.res created by SHELXL-2018/3 at 17:27:03 on 04-Dec-2019 REM Old TITL 12_3_try in P-1 REM SHELXT solution in P-1: R1 0.324, Rweak 0.034, Alpha 0.272 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C67 N13 O5 F2A Ni2 CELL 0.71073 12.1972 15.166 21.9697 71.701 76.17 69.672 ZERR 2 0.0061 0.0078 0.0111 0.012 0.011 0.013 LATT 1 SFAC C H F N Ni O S UNIT 116 136 12 20 4 12 4 DFIX 1.81 0.005 S1 C61 S4 C62 DFIX 1.32 0.01 F2 C61 DFIX 1.32 0.01 F6A C62A F6 C62 SADI 0.01 S1A O2A S1 O2 SADI 0.01 S1A C61A S1 C61 SADI 0.005 F2A C61A F3 C61 F1 C61 F3A C61A F2 C61 F1A C61A SADI 0.005 F3 F1 F1 F2 F3 F2 SADI 0.005 F2A F1A F1A F3A F2A F3A SADI 0.01 S4 O4 S4A O4A SADI 0.01 S4 C62 S4A C62A SADI 0.01 F4 C62 F6 C62 F5 C62 F5A C62A F4A C62A F6A C62A SADI 0.01 F4 F6 F6 F5 F4 F5 SADI 0.01 F4A F6A F6A F5A F4A F5A SIMU 0.01 0.02 2 RIGU 0.005 0.005 ISOR 0.01 0.02 C34 L.S. 16 0 0 PLAN 8 SIZE 0.22 0.24 0.36 TEMP -173(2) list 4 BOND $H fmap 2 53 acta ABIN OMIT 1 2 2 REM REM REM WGHT 0.029000 178.000000 FVAR 0.09551 0.46628 0.48321 NI1 5 0.773851 0.255139 0.751710 11.00000 0.03868 0.08056 = 0.02506 0.02432 -0.01823 -0.03394 NI2 5 0.279891 0.244908 0.748077 11.00000 0.03783 0.08324 = 0.02152 0.02541 -0.01650 -0.03455 N1 4 0.772048 0.164094 0.838780 11.00000 0.04796 0.07835 = 0.02738 0.02031 -0.01770 -0.03672 N2 4 0.781824 0.178763 0.894570 11.00000 0.05094 0.08262 = 0.02731 0.02126 -0.01723 -0.03797 N3 4 0.790004 0.354943 0.783396 11.00000 0.04655 0.07994 = 0.02774 0.01543 -0.01588 -0.02882 N4 4 0.781600 0.429542 0.642423 11.00000 0.04715 0.07887 = 0.02822 0.01939 -0.01553 -0.03536 N5 4 0.774936 0.339825 0.662011 11.00000 0.04344 0.07681 = 0.02526 0.02116 -0.01976 -0.03700 N6 4 0.278746 0.160495 0.839351 11.00000 0.03816 0.07123 = 0.02772 0.02215 -0.01057 -0.03084 N7 4 0.338992 0.071725 0.857487 11.00000 0.04972 0.07680 = 0.02456 0.02395 -0.01028 -0.02241 N8 4 0.405067 0.142563 0.715439 11.00000 0.04469 0.08185 = 0.02471 0.02093 -0.01463 -0.03894 N9 4 0.341937 0.319301 0.605812 11.00000 0.05156 0.08264 = 0.01785 0.02316 -0.00966 -0.02749 N10 4 0.279795 0.337031 0.660927 11.00000 0.04554 0.08225 = 0.01743 0.02083 -0.01447 -0.02533 C1 1 0.762001 0.046031 0.786278 11.00000 0.06645 0.05359 = 0.03476 0.02859 -0.02100 -0.03034 AFIX 137 H1A 2 0.686809 0.088044 0.771405 11.00000 -1.50000 H1B 2 0.768460 -0.021976 0.791069 11.00000 -1.50000 H1C 2 0.827546 0.063434 0.754493 11.00000 -1.50000 AFIX 0 C2 1 0.766912 0.059270 0.850789 11.00000 0.05914 0.07700 = 0.03584 0.02161 -0.02042 -0.03941 C3 1 0.878133 -0.010614 0.879571 11.00000 0.07761 0.10364 = 0.06427 0.02631 -0.04013 -0.03179 AFIX 137 H3A 2 0.948487 -0.001535 0.848707 11.00000 -1.50000 H3B 2 0.876977 -0.077777 0.888321 11.00000 -1.50000 H3C 2 0.879979 0.002830 0.920069 11.00000 -1.50000 AFIX 0 C4 1 0.660993 0.046394 0.901509 11.00000 0.08200 0.10752 = 0.06281 0.00345 -0.00294 -0.06491 AFIX 137 H4A 2 0.679970 0.036349 0.944545 11.00000 -1.50000 H4B 2 0.641082 -0.010168 0.900127 11.00000 -1.50000 H4C 2 0.593472 0.104680 0.892636 11.00000 -1.50000 AFIX 0 C5 1 0.768455 0.241323 1.169740 11.00000 0.11644 0.13064 = 0.04184 0.00768 -0.01366 -0.05276 AFIX 137 H5A 2 0.712680 0.204719 1.194239 11.00000 -1.50000 H5B 2 0.740669 0.305888 1.178122 11.00000 -1.50000 H5C 2 0.846483 0.206518 1.183268 11.00000 -1.50000 AFIX 0 C6 1 0.776462 0.251226 1.102595 11.00000 0.08650 0.10426 = 0.03891 0.01095 -0.01549 -0.04252 C7 1 0.818383 0.171112 1.078381 11.00000 0.07165 0.09667 = 0.03287 0.02021 -0.01734 -0.04532 AFIX 43 H7 2 0.843300 0.108612 1.106965 11.00000 -1.20000 AFIX 0 C8 1 0.825318 0.178678 1.014257 11.00000 0.06143 0.09350 = 0.03200 0.02402 -0.01818 -0.04474 AFIX 43 H8 2 0.861571 0.120475 1.000308 11.00000 -1.20000 AFIX 0 C9 1 0.785163 0.261932 0.967965 11.00000 0.06017 0.08900 = 0.03186 0.02039 -0.01517 -0.04299 C10 1 0.728422 0.347655 0.993074 11.00000 0.07660 0.09551 = 0.03802 0.01564 -0.00820 -0.04162 AFIX 43 H10 2 0.692354 0.408239 0.965462 11.00000 -1.20000 AFIX 0 C11 1 0.727527 0.339641 1.060454 11.00000 0.08808 0.10349 = 0.04128 0.00831 -0.01043 -0.04114 AFIX 43 H11 2 0.692663 0.396130 1.076437 11.00000 -1.20000 AFIX 0 C12 1 0.790243 0.264013 0.899232 11.00000 0.05043 0.08440 = 0.03169 0.01677 -0.02033 -0.03766 C13 1 0.804419 0.349007 0.847437 11.00000 0.04935 0.08175 = 0.03164 0.01430 -0.01831 -0.03249 C14 1 0.829308 0.433516 0.849659 11.00000 0.04839 0.08146 = 0.03381 0.01270 -0.01907 -0.03117 AFIX 43 H14 2 0.845512 0.444146 0.886545 11.00000 -1.20000 AFIX 0 C15 1 0.825743 0.494012 0.791375 11.00000 0.04909 0.08221 = 0.03371 0.01258 -0.01894 -0.03023 AFIX 43 H15 2 0.836338 0.556778 0.778845 11.00000 -1.20000 AFIX 0 C16 1 0.802833 0.446756 0.750718 11.00000 0.04695 0.08134 = 0.02954 0.01233 -0.01617 -0.03124 C17 1 0.787155 0.482511 0.683281 11.00000 0.04786 0.07949 = 0.03015 0.01790 -0.01342 -0.03786 C18 1 0.782607 0.581518 0.646347 11.00000 0.05482 0.08299 = 0.03922 0.02216 -0.01879 -0.03736 C19 1 0.726634 0.658577 0.675442 11.00000 0.06701 0.08762 = 0.05359 0.01575 -0.02295 -0.03391 AFIX 43 H19 2 0.693439 0.643586 0.719828 11.00000 -1.20000 AFIX 0 C20 1 0.715346 0.760962 0.642491 11.00000 0.07684 0.08799 = 0.06298 0.01797 -0.02220 -0.03456 AFIX 43 H20 2 0.679479 0.810822 0.664753 11.00000 -1.20000 AFIX 0 C21 1 0.760381 0.781281 0.576318 11.00000 0.08272 0.08874 = 0.06296 0.02099 -0.02239 -0.03850 C22 1 0.814848 0.703413 0.544820 11.00000 0.07144 0.08808 = 0.05124 0.02494 -0.02105 -0.04003 AFIX 43 H22 2 0.844243 0.716414 0.499809 11.00000 -1.20000 AFIX 0 C23 1 0.823998 0.605586 0.582671 11.00000 0.05927 0.08808 = 0.03883 0.02529 -0.02261 -0.03858 AFIX 43 H23 2 0.861611 0.554594 0.561489 11.00000 -1.20000 AFIX 0 C24 1 0.757245 0.878898 0.536630 11.00000 0.12004 0.09050 = 0.08078 0.02030 -0.02736 -0.04560 AFIX 137 H24A 2 0.683138 0.909260 0.518263 11.00000 -1.50000 H24B 2 0.824177 0.875333 0.501461 11.00000 -1.50000 H24C 2 0.762309 0.917812 0.563450 11.00000 -1.50000 AFIX 0 C25 1 0.767080 0.307080 0.603571 11.00000 0.06107 0.07949 = 0.02822 0.01891 -0.02086 -0.03832 C26 1 0.766499 0.198973 0.629335 11.00000 0.07443 0.07846 = 0.03395 0.00925 -0.01175 -0.04051 AFIX 137 H26A 2 0.840426 0.158950 0.646394 11.00000 -1.50000 H26B 2 0.759159 0.176074 0.593875 11.00000 -1.50000 H26C 2 0.699547 0.193960 0.663928 11.00000 -1.50000 AFIX 0 C27 1 0.655267 0.373946 0.574049 11.00000 0.08446 0.10048 = 0.07084 0.00905 -0.05574 -0.02768 AFIX 137 H27A 2 0.585231 0.366358 0.605690 11.00000 -1.50000 H27B 2 0.653237 0.356504 0.535081 11.00000 -1.50000 H27C 2 0.655976 0.441651 0.562533 11.00000 -1.50000 AFIX 0 C28 1 0.880912 0.311818 0.552555 11.00000 0.08135 0.09949 = 0.04337 0.01875 -0.00527 -0.04475 AFIX 137 H28A 2 0.879831 0.379807 0.533590 11.00000 -1.50000 H28B 2 0.882730 0.282526 0.518272 11.00000 -1.50000 H28C 2 0.951244 0.276077 0.573951 11.00000 -1.50000 AFIX 0 C33 1 0.196980 0.191787 0.897240 11.00000 0.04986 0.08084 = 0.03375 0.01647 -0.00809 -0.02614 C34 1 0.122581 0.298762 0.873167 11.00000 0.06088 0.07649 = 0.02244 0.01078 -0.02175 -0.02780 AFIX 137 H34A 2 0.165568 0.342401 0.873596 11.00000 -1.50000 H34B 2 0.046831 0.311499 0.901764 11.00000 -1.50000 H34C 2 0.108311 0.310014 0.828921 11.00000 -1.50000 AFIX 0 C35 1 0.115611 0.126375 0.928196 11.00000 0.05469 0.10380 = 0.07262 0.02849 0.01033 -0.03874 AFIX 137 H35A 2 0.068252 0.131285 0.896321 11.00000 -1.50000 H35B 2 0.063064 0.147395 0.965658 11.00000 -1.50000 H35C 2 0.163715 0.058800 0.942318 11.00000 -1.50000 AFIX 0 C36 1 0.270028 0.182631 0.947623 11.00000 0.07054 0.11215 = 0.04776 0.00528 -0.02628 -0.01653 AFIX 137 H36A 2 0.328225 0.118141 0.955439 11.00000 -1.50000 H36B 2 0.217758 0.191251 0.988158 11.00000 -1.50000 H36C 2 0.311026 0.232619 0.931637 11.00000 -1.50000 AFIX 0 C37 1 0.581348 -0.388529 0.955162 11.00000 0.13845 0.08442 = 0.09366 0.04402 0.02787 -0.00052 AFIX 137 H37A 2 0.661809 -0.419742 0.936617 11.00000 -1.50000 H37B 2 0.526555 -0.418400 0.949101 11.00000 -1.50000 H37C 2 0.578418 -0.396939 1.001552 11.00000 -1.50000 AFIX 0 C38 1 0.546293 -0.281392 0.921578 11.00000 0.08769 0.07950 = 0.06059 0.02935 -0.00407 -0.01692 C39 1 0.517174 -0.204006 0.951497 11.00000 0.06989 0.08086 = 0.05236 0.03106 -0.01059 -0.02130 AFIX 43 H39 2 0.525152 -0.219401 0.995908 11.00000 -1.20000 AFIX 0 C40 1 0.478365 -0.108813 0.919353 11.00000 0.05947 0.07887 = 0.04401 0.02745 -0.01633 -0.02744 AFIX 43 H40 2 0.458815 -0.058942 0.941036 11.00000 -1.20000 AFIX 0 C41 1 0.467702 -0.085576 0.853038 11.00000 0.05527 0.07621 = 0.04190 0.02241 -0.01517 -0.02806 C42 1 0.498551 -0.165024 0.822993 11.00000 0.06934 0.07569 = 0.05173 0.02206 -0.01469 -0.02629 AFIX 43 H42 2 0.497330 -0.153202 0.778021 11.00000 -1.20000 AFIX 0 C43 1 0.528057 -0.253317 0.859681 11.00000 0.08569 0.07742 = 0.06173 0.02664 -0.00760 -0.01935 AFIX 43 H43 2 0.537806 -0.303833 0.840201 11.00000 -1.20000 AFIX 0 C44 1 0.419561 0.018425 0.819342 11.00000 0.05016 0.07646 = 0.02808 0.01686 -0.01498 -0.02680 C45 1 0.459096 0.056843 0.749572 11.00000 0.05046 0.08050 = 0.02645 0.01323 -0.01318 -0.03432 C46 1 0.559746 0.007696 0.709044 11.00000 0.05752 0.08266 = 0.02697 0.01605 -0.00857 -0.03043 AFIX 43 H46 2 0.614774 -0.054175 0.722646 11.00000 -1.20000 AFIX 0 C47 1 0.560291 0.066405 0.648572 11.00000 0.05720 0.08005 = 0.02798 0.01612 -0.00660 -0.03409 AFIX 43 H47 2 0.614580 0.055305 0.610816 11.00000 -1.20000 AFIX 0 C48 1 0.457674 0.151448 0.654489 11.00000 0.05138 0.08000 = 0.02647 0.01768 -0.01192 -0.03502 C49 1 0.421682 0.235611 0.599372 11.00000 0.04976 0.08274 = 0.02314 0.01809 -0.00754 -0.03382 C50 1 0.472073 0.232542 0.531933 11.00000 0.05888 0.09292 = 0.02429 0.01774 -0.00876 -0.03450 C51 1 0.504593 0.147567 0.508259 11.00000 0.07567 0.09986 = 0.02943 0.01108 -0.01085 -0.03179 AFIX 43 H51 2 0.497250 0.087866 0.537391 11.00000 -1.20000 AFIX 0 C52 1 0.547743 0.151797 0.441579 11.00000 0.08828 0.10590 = 0.03055 0.00616 -0.01074 -0.03031 AFIX 43 H52 2 0.570999 0.093743 0.427691 11.00000 -1.20000 AFIX 0 C53 1 0.556955 0.233554 0.397789 11.00000 0.08707 0.10976 = 0.03107 0.01141 -0.01289 -0.03119 C54 1 0.518927 0.325564 0.419849 11.00000 0.07037 0.10353 = 0.02797 0.01826 -0.01084 -0.03707 AFIX 43 H54 2 0.521033 0.385792 0.389667 11.00000 -1.20000 AFIX 0 C55 1 0.480496 0.320343 0.485684 11.00000 0.06082 0.09799 = 0.02641 0.02150 -0.01081 -0.03887 AFIX 43 H55 2 0.459165 0.377783 0.500067 11.00000 -1.20000 AFIX 0 C56 1 0.591659 0.232688 0.330892 11.00000 0.13127 0.12811 = 0.03562 0.00012 -0.01315 -0.02239 AFIX 137 H56A 2 0.659411 0.175465 0.326655 11.00000 -1.50000 H56B 2 0.613701 0.291731 0.306257 11.00000 -1.50000 H56C 2 0.525618 0.230275 0.313979 11.00000 -1.50000 AFIX 0 C57 1 0.197064 0.441048 0.647212 11.00000 0.05143 0.08464 = 0.02343 0.01892 -0.01791 -0.02240 C58 1 0.270931 0.511926 0.619051 11.00000 0.07685 0.09729 = 0.04497 0.02805 -0.00940 -0.03907 AFIX 137 H58A 2 0.340692 0.488326 0.640983 11.00000 -1.50000 H58B 2 0.223365 0.576143 0.625533 11.00000 -1.50000 H58C 2 0.296073 0.516729 0.572591 11.00000 -1.50000 AFIX 0 C59 1 0.115648 0.455550 0.599085 11.00000 0.05350 0.12176 = 0.04030 0.01285 -0.02783 -0.01508 AFIX 137 H59A 2 0.161624 0.456742 0.555801 11.00000 -1.50000 H59B 2 0.052718 0.517233 0.597918 11.00000 -1.50000 H59C 2 0.080626 0.401932 0.612814 11.00000 -1.50000 AFIX 0 C60 1 0.123402 0.457733 0.713203 11.00000 0.05449 0.07584 = 0.02822 0.02275 -0.01576 -0.01898 AFIX 137 H60A 2 0.105631 0.397686 0.739819 11.00000 -1.50000 H60B 2 0.049408 0.509771 0.705484 11.00000 -1.50000 H60C 2 0.168790 0.476247 0.735854 11.00000 -1.50000 AFIX 0 PART 1 S1 7 0.074391 0.144050 0.741608 21.00000 0.04196 0.11631 = 0.06263 -0.00586 -0.01454 -0.04127 PART 0 O1 6 0.123516 0.221498 0.740301 11.00000 0.04436 0.12329 = 0.05977 0.00648 -0.02135 -0.05373 PART 1 O2 6 0.087438 0.067700 0.803285 21.00000 0.04561 0.10640 = 0.06541 0.00053 -0.02043 -0.04084 PART 0 O3 6 -0.047801 0.179704 0.725966 11.00000 0.02850 0.12087 = 0.06781 0.00351 -0.01710 -0.04610 PART 1 C61 1 0.157414 0.080577 0.679499 21.00000 0.05002 0.11878 = 0.07414 -0.01026 -0.01243 -0.03962 F1 3 0.177656 0.148291 0.625030 21.00000 0.05515 0.12796 = 0.07303 -0.00553 -0.00221 -0.03336 F2 3 0.110415 0.025177 0.662637 21.00000 0.07192 0.12745 = 0.09147 -0.03161 -0.01324 -0.04138 F3 3 0.264511 0.023452 0.694772 21.00000 0.05447 0.11738 = 0.07683 -0.01757 -0.01828 -0.03006 PART 0 PART 2 S1A 7 0.074286 0.182794 0.699820 -21.00000 0.04422 0.11517 = 0.06873 -0.00516 -0.01331 -0.04210 O2A 6 0.086254 0.233597 0.630146 -21.00000 0.04684 0.11664 = 0.05197 -0.00435 -0.00589 -0.03982 C61A 1 0.158284 0.055157 0.704213 -21.00000 0.05017 0.11824 = 0.07437 -0.00941 -0.01128 -0.03986 F1A 3 0.176915 0.005260 0.765222 -21.00000 0.05867 0.12143 = 0.08392 0.00295 -0.01409 -0.02494 F2A 3 0.262530 0.048933 0.665016 -21.00000 0.05250 0.11549 = 0.07691 -0.01431 -0.00675 -0.03593 F3A 3 0.091920 0.018516 0.683698 -21.00000 0.06774 0.12036 = 0.09488 -0.02744 -0.00177 -0.05033 PART 0 PART 1 S4 7 0.478806 0.357843 0.759490 31.00000 0.05432 0.08063 = 0.04424 0.01292 -0.02066 -0.03025 O4 6 0.480792 0.430828 0.698766 31.00000 0.06329 0.08257 = 0.04761 0.02917 -0.02001 -0.03602 PART 0 O5 6 0.592715 0.279054 0.758505 11.00000 0.04375 0.07441 = 0.03878 0.02067 -0.01464 -0.02757 O6 6 0.372975 0.325350 0.774954 11.00000 0.04613 0.07697 = 0.04350 0.01863 -0.02641 -0.03501 PART 1 C62 1 0.462725 0.415832 0.823235 31.00000 0.06000 0.08309 = 0.05227 0.00691 -0.02051 -0.03038 F4 3 0.529048 0.476653 0.808164 31.00000 0.07128 0.08415 = 0.06211 0.00069 -0.01492 -0.03495 F5 3 0.350075 0.468666 0.836332 31.00000 0.06436 0.09166 = 0.06780 -0.00117 -0.00409 -0.02490 F6 3 0.492052 0.351167 0.878556 31.00000 0.08089 0.09958 = 0.04778 0.00433 -0.02615 -0.02879 PART 0 PART 2 S4A 7 0.477350 0.317331 0.799322 -31.00000 0.05292 0.07872 = 0.04555 0.01555 -0.02122 -0.02933 O4A 6 0.478894 0.260571 0.865743 -31.00000 0.06810 0.09251 = 0.02954 0.02368 -0.02171 -0.02786 C62A 1 0.460921 0.442916 0.796448 -31.00000 0.06002 0.08295 = 0.05156 0.00714 -0.02083 -0.03042 F4A 3 0.533088 0.446528 0.832820 -31.00000 0.07279 0.09404 = 0.05833 -0.00432 -0.02685 -0.02906 F5A 3 0.350598 0.491895 0.817845 -31.00000 0.06356 0.08994 = 0.07375 0.00649 -0.01520 -0.01925 F6A 3 0.489198 0.492478 0.735937 -31.00000 0.07953 0.08364 = 0.06044 0.01974 -0.01643 -0.03396 HKLF 4 REM 12_3_try_a.res in P-1 REM wR2 = 0.3534, GooF = S = 1.045, Restrained GooF = 0.917 for all data REM R1 = 0.1592 for 3820 Fo > 4sig(Fo) and 0.1917 for all 5349 data REM 883 parameters refined using 1703 restraints END WGHT 0.1756 130.6316 REM Highest difference peak 1.482, deepest hole -0.993, 1-sigma level 0.158 Q1 1 -0.0249 0.2387 0.7519 11.00000 0.05 1.48 Q2 1 0.4219 0.2425 0.7485 11.00000 0.05 1.36 Q3 1 0.4796 0.2547 0.7438 11.00000 0.05 1.32 Q4 1 0.4643 0.2378 0.7511 11.00000 0.05 1.30 Q5 1 0.1864 0.2539 0.7407 11.00000 0.05 1.30 Q6 1 0.1753 0.1587 0.7180 11.00000 0.05 1.12 Q7 1 0.6910 0.2608 0.7461 11.00000 0.05 1.08 Q8 1 0.7192 0.3355 0.7774 11.00000 0.05 1.06 ; _shelx_res_checksum 70514 _shelx_hkl_file ; -2 0 0 120.57 11.22 -2 0 0 128.44 11.21 2 0 0 140.72 11.22 2 0 0 140.18 11.21 2 0 0 127.87 11.22 -3 0 0 598.50 44.56 -3 0 0 521.11 44.55 3 0 0 527.58 44.55 3 0 0 445.56 44.56 -4 0 0 255.93 22.30 -4 0 0 266.68 22.30 -4 0 0 257.63 22.29 4 0 0 273.91 22.30 4 0 0 251.17 22.30 4 0 0 263.91 22.29 -5 0 0 5.45 0.95 -5 0 0 7.58 1.02 5 0 0 7.54 0.86 5 0 0 7.21 0.95 -6 0 0 29.93 2.35 -6 0 0 28.01 2.40 -6 0 0 21.72 2.31 6 0 0 24.15 2.31 6 0 0 25.33 2.32 -7 0 0 22.52 2.02 -7 0 0 21.76 2.11 7 0 0 22.98 2.11 7 0 0 18.67 2.03 -8 0 0 -0.05 0.60 -8 0 0 -0.75 0.50 8 0 0 0.32 0.65 8 0 0 0.58 0.49 -9 0 0 1.18 0.71 -9 0 0 -0.45 0.75 9 0 0 -0.70 0.76 -10 0 0 8.63 1.81 10 0 0 12.65 1.98 9 -1 0 0.50 0.79 -9 1 0 0.02 0.66 -9 1 0 0.26 0.83 8 -1 0 10.66 1.45 8 -1 0 10.20 1.39 -8 1 0 12.35 1.41 -8 1 0 8.37 1.47 7 -1 0 9.48 1.28 7 -1 0 12.60 1.33 -7 1 0 10.40 1.21 -7 1 0 9.82 1.33 6 -1 0 262.56 21.46 6 -1 0 235.08 21.42 -6 1 0 250.17 21.44 -6 1 0 241.47 21.41 -6 1 0 265.95 21.45 5 -1 0 14.29 1.46 5 -1 0 14.14 1.37 -5 1 0 15.11 1.36 -5 1 0 14.04 1.44 -5 1 0 12.81 1.46 4 -1 0 60.93 4.83 -4 1 0 57.44 4.85 -4 1 0 52.95 4.83 -4 1 0 52.94 4.86 3 -1 0 100.21 8.22 3 -1 0 110.01 8.22 3 -1 0 90.82 8.21 -3 1 0 82.60 8.21 -3 1 0 104.75 8.22 -3 1 0 88.93 8.22 1 -1 0 1.38 0.23 -1 1 0 1.91 0.23 -2 -1 0 73.90 6.17 -2 -1 0 74.56 6.17 2 1 0 70.11 6.17 2 1 0 70.81 6.17 -3 -1 0 73.16 6.68 -3 -1 0 73.68 6.68 -3 -1 0 89.77 6.67 3 1 0 83.62 6.67 3 1 0 75.06 6.67 3 1 0 73.44 6.68 -4 -1 0 146.32 12.95 -4 -1 0 172.17 12.96 -4 -1 0 129.78 12.95 4 1 0 155.35 12.94 4 1 0 145.42 12.96 4 1 0 161.33 12.94 -5 -1 0 4.03 0.79 -5 -1 0 2.64 0.76 -5 -1 0 1.31 0.44 5 1 0 2.42 0.55 5 1 0 3.40 0.72 5 1 0 2.21 0.54 -6 -1 0 80.01 6.77 -6 -1 0 82.45 6.79 -6 -1 0 78.14 6.77 6 1 0 84.64 6.80 6 1 0 71.89 6.74 6 1 0 74.64 6.75 -7 -1 0 1.35 0.51 -7 -1 0 1.42 0.61 7 1 0 1.57 0.41 7 1 0 1.22 0.52 7 1 0 1.50 0.42 -8 -1 0 33.29 3.09 -8 -1 0 34.28 3.15 8 1 0 35.80 3.08 8 1 0 31.43 3.14 -9 -1 0 1.20 0.78 -9 -1 0 0.61 0.67 9 1 0 1.85 0.77 -10 -1 0 42.39 4.06 -10 -1 0 37.57 3.91 10 1 0 48.43 4.14 9 -2 0 0.72 0.82 -9 2 0 1.01 0.71 -9 2 0 0.51 0.91 8 -2 0 -0.26 0.72 -8 2 0 0.07 0.75 7 -2 0 0.80 0.57 7 -2 0 0.21 0.56 -7 2 0 0.78 0.63 -7 2 0 -0.73 0.47 6 -2 0 35.60 3.26 6 -2 0 36.76 3.21 -6 2 0 35.24 3.25 5 -2 0 0.68 0.43 5 -2 0 -0.26 0.43 5 -2 0 -0.63 0.37 -5 2 0 0.69 0.33 -5 2 0 -0.08 0.48 -5 2 0 -0.09 0.40 4 -2 0 73.26 6.19 4 -2 0 70.92 6.19 4 -2 0 72.77 6.17 -4 2 0 79.16 6.20 -4 2 0 66.69 6.16 -4 2 0 68.24 6.19 3 -2 0 1.55 0.29 3 -2 0 2.74 0.51 -3 2 0 1.55 0.37 2 -2 0 65.85 6.15 2 -2 0 76.49 6.15 2 -2 0 81.12 6.16 -2 2 0 72.42 6.15 -2 2 0 60.97 6.14 -2 2 0 74.78 6.16 1 -2 0 66.10 5.31 1 -2 0 59.65 5.31 -1 2 0 58.64 5.30 -1 2 0 64.11 5.31 0 -2 0 438.09 38.56 0 -2 0 423.70 38.57 0 2 0 436.83 38.56 0 2 0 445.90 38.57 0 2 0 520.25 38.57 -1 -2 0 1.97 0.19 -1 -2 0 1.76 0.23 -1 -2 0 1.31 0.25 -1 -2 0 1.99 0.25 -2 -2 0 27.67 2.51 -2 -2 0 28.81 2.51 -2 -2 0 33.35 2.51 2 2 0 26.16 2.51 2 2 0 28.22 2.52 2 2 0 31.30 2.51 -3 -2 0 36.16 3.20 3 2 0 35.54 3.19 3 2 0 43.46 3.21 3 2 0 33.53 3.20 -4 -2 0 293.90 24.00 -4 -2 0 290.82 24.01 -4 -2 0 267.71 24.01 4 2 0 301.61 24.00 4 2 0 275.65 24.00 4 2 0 260.28 24.01 -5 -2 0 10.29 1.16 -5 -2 0 8.51 1.03 -5 -2 0 9.98 1.02 5 2 0 8.63 0.92 5 2 0 10.19 1.06 5 2 0 8.02 0.93 -6 -2 0 35.62 2.95 -6 -2 0 29.63 2.90 -6 -2 0 34.22 2.93 6 2 0 32.44 2.87 6 2 0 37.55 2.95 6 2 0 28.33 2.88 -7 -2 0 18.86 1.71 -7 -2 0 13.67 1.69 -7 -2 0 17.16 1.68 7 2 0 18.90 1.70 7 2 0 15.25 1.54 7 2 0 16.48 1.59 -8 -2 0 9.57 1.40 -8 -2 0 9.07 1.36 8 2 0 9.88 1.31 -9 -2 0 24.63 2.65 -9 -2 0 27.53 2.71 9 2 0 25.72 2.64 -10 -2 0 9.33 1.96 -10 -2 0 8.77 1.73 10 2 0 11.84 1.76 8 -3 0 0.84 0.81 -8 3 0 1.10 0.76 -8 3 0 1.66 0.84 7 -3 0 -0.04 0.61 -7 3 0 0.01 0.68 -7 3 0 0.29 0.58 6 -3 0 21.23 2.15 6 -3 0 21.47 2.21 -6 3 0 23.98 2.19 5 -3 0 0.94 0.47 5 -3 0 1.36 0.49 5 -3 0 0.88 0.40 -5 3 0 0.17 0.42 -5 3 0 1.70 0.54 4 -3 0 8.60 0.88 4 -3 0 6.99 1.06 4 -3 0 6.56 0.96 -4 3 0 6.88 1.03 -4 3 0 5.91 0.85 -4 3 0 6.56 1.05 3 -3 0 2.80 0.52 3 -3 0 2.69 0.58 -3 3 0 1.89 0.37 -3 3 0 3.86 0.71 2 -3 0 8.43 0.79 2 -3 0 6.32 0.89 2 -3 0 9.32 0.82 -2 3 0 8.28 0.88 -2 3 0 7.70 0.82 1 -3 0 9.01 0.86 1 -3 0 8.28 0.84 -1 3 0 9.68 0.92 -1 3 0 10.19 0.87 -1 3 0 9.69 0.86 0 -3 0 11.91 1.01 0 3 0 11.50 1.01 0 3 0 11.07 1.02 -1 -3 0 51.55 4.40 -1 -3 0 48.40 4.39 1 3 0 58.39 4.39 1 3 0 47.17 4.42 -2 -3 0 30.93 2.92 -2 -3 0 35.13 2.94 -2 -3 0 33.16 2.93 2 3 0 35.73 2.93 2 3 0 33.59 2.93 2 3 0 36.26 2.94 -3 -3 0 18.78 1.50 -3 -3 0 16.20 1.49 3 3 0 14.96 1.49 3 3 0 17.68 1.50 -4 -3 0 24.76 2.14 -4 -3 0 22.68 2.14 -4 -3 0 24.56 2.10 4 3 0 21.40 2.12 4 3 0 27.09 2.11 -5 -3 0 3.71 0.68 -5 -3 0 3.13 0.71 5 3 0 4.32 0.59 5 3 0 3.54 0.58 -6 -3 0 63.89 5.15 -6 -3 0 57.74 5.16 -6 -3 0 56.59 5.17 6 3 0 61.63 5.16 6 3 0 63.94 5.13 6 3 0 53.57 5.13 -7 -3 0 29.18 2.49 -7 -3 0 26.19 2.52 -7 -3 0 23.95 2.50 7 3 0 27.52 2.40 7 3 0 27.78 2.48 -8 -3 0 41.65 3.81 -8 -3 0 43.88 3.75 8 3 0 42.67 3.75 8 3 0 37.97 3.69 -9 -3 0 2.60 0.91 -9 -3 0 2.43 0.89 9 3 0 2.31 0.74 9 3 0 2.07 0.53 -10 -3 0 19.67 2.50 -10 -3 0 18.45 2.59 10 3 0 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-0.0734 8 6 12 0.4232 -0.0158 8 6 13 -0.6613 -0.0840 8 6 14 0.9207 -0.0078 8 6 15 -0.5844 0.0456 8 6 16 -1.5605 0.0226 8 7 0 -2.9404 -0.7634 8 7 1 -2.9455 -0.0076 8 7 2 1.7526 -0.2574 8 7 3 -0.6281 -0.0401 8 7 4 0.6924 -0.0833 8 7 5 0.3057 0.0577 8 7 6 -0.3670 -0.0894 8 7 7 2.2404 0.0784 8 7 8 1.9303 -0.0723 8 7 9 3.7031 0.0400 8 7 10 -1.0532 0.0685 8 7 11 1.9676 0.0805 8 7 12 4.0187 -0.0100 8 7 13 0.3251 0.0438 8 7 14 0.1552 -0.0049 8 7 15 -1.6563 -0.0057 8 7 16 -0.3661 -0.1912 8 8 0 1.2729 -0.1706 8 8 1 0.4524 0.1075 8 8 2 2.6706 -0.0268 8 8 3 0.5596 0.1436 8 8 4 1.5978 0.0522 8 8 5 1.6220 0.0237 8 8 6 0.9064 -0.0125 8 8 7 -0.3317 0.0993 8 8 8 0.5830 0.0096 8 8 9 0.3720 -0.0082 8 8 10 -2.4618 0.0406 8 8 11 0.3507 -0.0955 8 8 12 -3.6325 0.0168 8 8 13 -2.6976 0.0848 8 8 14 -0.8704 0.0139 8 8 15 0.3302 0.0664 8 9 0 2.1517 0.5782 8 9 1 -1.6057 -0.0311 8 9 2 0.9726 0.2158 8 9 3 -3.4944 -0.0077 8 9 4 -1.0103 0.1310 8 9 5 1.3573 -0.0131 8 9 6 -1.1056 0.0903 8 9 7 0.0753 -0.0019 8 9 8 1.5776 0.0271 8 9 9 -2.4124 -0.0469 8 9 10 -1.1512 0.0627 8 9 11 0.3847 -0.0417 8 9 12 -0.4659 0.0569 8 9 13 2.4125 -0.0717 8 9 14 0.4946 -0.1479 8 9 15 0.2743 -0.0207 8 10 0 1.9137 0.0914 8 10 1 -1.1301 -0.0675 8 10 2 0.7072 0.0516 8 10 3 0.0932 0.0059 8 10 4 5.4687 -0.0215 8 10 5 1.0404 -0.0698 8 10 6 -3.8358 -0.0623 8 10 7 -0.0319 -0.0130 8 10 8 -0.5902 -0.0165 8 10 9 -0.1752 -0.0953 8 10 10 0.3515 -0.0178 8 10 11 0.5783 0.0572 8 10 12 -0.3298 -0.0822 8 10 13 0.5371 0.1100 8 10 14 -0.2719 -0.0207 8 11 1 -1.3147 0.0708 8 11 2 -0.2906 -0.0566 8 11 3 1.1591 0.0106 8 11 4 -1.3775 -0.1400 8 11 5 -5.6922 0.0440 8 11 6 -0.6664 -0.1127 8 11 7 3.7081 0.0625 8 11 8 0.6107 -0.0587 8 11 9 -1.2981 -0.0322 8 11 10 -2.2828 0.1505 8 11 11 2.1952 0.0147 8 11 12 0.3868 -0.1589 8 12 4 -2.2914 -0.0050 8 12 5 1.3195 -0.0950 9 -3 1 -2.0276 0.0104 9 -3 2 -0.5534 0.0191 9 -3 3 -0.9394 0.1183 9 -3 4 0.8761 0.0800 9 -3 5 0.1755 -0.0129 9 -2 0 1.5773 0.0093 9 -2 1 0.2972 -0.2070 9 -2 2 1.5112 0.0638 9 -2 3 -0.7925 -0.1741 9 -2 4 -0.6522 -0.0274 9 -2 5 -0.5522 -0.2244 9 -2 6 -0.6298 0.0301 9 -2 7 0.8917 0.0486 9 -2 8 1.1380 0.0213 9 -1 0 2.6508 -0.4467 9 -1 1 -4.4926 0.0209 9 -1 2 -0.3174 0.0835 9 -1 3 -0.0602 -0.0496 9 -1 4 2.5168 0.0303 9 -1 5 0.9869 0.0037 9 -1 6 -0.8759 0.2387 9 -1 7 -1.7213 -0.0668 9 -1 8 -0.0608 -0.0323 9 -1 9 0.5885 0.0300 9 -1 10 -1.4925 -0.0313 9 0 0 1.3203 0.0080 9 0 1 -2.6405 0.5490 9 0 2 4.4894 -0.0764 9 0 3 2.0096 0.0222 9 0 4 -1.5718 0.0115 9 0 5 -3.1829 0.1761 9 0 6 -0.4830 -0.0615 9 0 7 1.1349 -0.1127 9 0 8 4.3297 0.0714 9 0 9 -0.8852 0.0307 9 0 10 -0.0896 -0.0612 9 0 11 1.2781 0.0340 9 1 0 -1.7347 0.2352 9 1 1 0.3314 -0.0240 9 1 2 2.3015 -0.2656 9 1 3 -3.0449 0.0389 9 1 4 -1.2456 0.1007 9 1 5 1.4525 -0.0816 9 1 6 3.1837 -0.1043 9 1 7 0.5122 0.0581 9 1 8 1.3987 0.0528 9 1 9 -3.1613 -0.0692 9 1 10 2.5928 -0.0073 9 1 11 -1.4981 0.0273 9 1 12 -0.2909 0.0545 9 2 0 -0.6302 -0.0386 9 2 1 1.8260 -0.6399 9 2 2 1.2374 0.0815 9 2 3 -1.0394 -0.0200 9 2 4 2.2958 -0.0251 9 2 5 -2.9406 -0.2161 9 2 6 0.9782 0.1413 9 2 7 -3.3595 -0.0732 9 2 8 -0.4044 -0.0075 9 2 9 -5.5973 -0.0631 9 2 10 -0.7323 0.0575 9 2 11 -3.8676 0.0042 9 2 12 1.5552 0.0034 9 2 13 -0.2049 -0.0628 9 3 0 0.3326 -0.2493 9 3 1 -1.7890 0.0489 9 3 2 -0.7702 0.3531 9 3 3 -1.8447 -0.0398 9 3 4 -0.9376 -0.0432 9 3 5 -0.3806 0.1342 9 3 6 5.7013 0.0813 9 3 7 -2.0832 -0.0487 9 3 8 2.3098 0.0135 9 3 9 0.0453 0.0393 9 3 10 8.3358 -0.0335 9 3 11 2.5634 -0.0086 9 3 12 3.2320 -0.0308 9 3 13 0.2449 0.0182 9 3 14 -0.6768 -0.0413 9 4 0 -0.4210 0.0079 9 4 1 1.3386 0.6647 9 4 2 2.6243 -0.0881 9 4 3 -1.2318 0.0284 9 4 4 0.5289 0.0147 9 4 5 0.9414 0.2146 9 4 6 -2.4596 -0.1770 9 4 7 -4.3431 0.0840 9 4 8 0.0790 -0.0267 9 4 9 0.4969 0.1365 9 4 10 -0.9695 -0.0985 9 4 11 -7.4517 0.1904 9 4 12 -0.9613 -0.0314 9 4 13 -1.3911 0.0107 9 4 14 -2.0052 -0.0350 9 5 0 -4.4484 0.4562 9 5 1 -0.0015 -0.0334 9 5 2 -2.7173 -0.4217 9 5 3 -2.3456 0.0361 9 5 4 2.3570 0.0496 9 5 5 0.4369 -0.1055 9 5 6 1.7897 -0.1531 9 5 7 2.5338 0.0441 9 5 8 1.8441 -0.0128 9 5 9 0.9337 -0.0779 9 5 10 -1.9093 -0.0340 9 5 11 2.4911 0.0487 9 5 12 4.0763 -0.1880 9 5 13 -1.2599 0.0025 9 5 14 0.1584 0.0636 9 6 0 0.7091 0.0788 9 6 1 0.0980 -0.7487 9 6 2 -0.6023 0.0957 9 6 3 1.8744 0.0184 9 6 4 0.6525 -0.0259 9 6 5 -2.0386 -0.2535 9 6 6 -0.9929 0.1499 9 6 7 -4.0433 -0.0067 9 6 8 -0.5336 0.0385 9 6 9 -0.9676 -0.1458 9 6 10 0.8473 0.1692 9 6 11 -0.1661 -0.2150 9 6 12 -2.3497 0.0316 9 6 13 -1.0646 0.0376 9 6 14 2.1378 0.0518 9 7 0 -0.8494 -0.3548 9 7 1 -2.2482 0.0208 9 7 2 1.2741 0.2914 9 7 3 0.1528 -0.0794 9 7 4 -0.2815 0.0376 9 7 5 1.5102 0.1285 9 7 6 1.8348 0.1077 9 7 7 1.3294 -0.0706 9 7 8 3.6273 0.0327 9 7 9 0.6346 0.0462 9 7 10 1.3301 0.1813 9 7 11 -0.8999 -0.0762 9 7 12 2.9966 0.2768 9 7 13 1.2688 -0.0022 9 7 14 -0.3332 0.0535 9 8 0 -0.4408 -0.1219 9 8 1 1.8472 0.4240 9 8 2 2.9893 -0.1277 9 8 3 0.4901 0.1841 9 8 4 0.6345 0.0906 9 8 5 0.0544 0.0381 9 8 6 -2.8106 -0.1748 9 8 7 -2.5569 0.1710 9 8 8 0.2081 0.0377 9 8 9 -2.0289 -0.0301 9 8 10 -2.2503 -0.0904 9 8 11 -1.9490 -0.1721 9 8 12 -2.3308 -0.0192 9 8 13 -3.2240 -0.1364 9 9 0 2.6041 0.5178 9 9 1 -0.0701 -0.0024 9 9 2 -1.1442 -0.0610 9 9 3 -3.2351 0.0832 9 9 4 -1.3833 -0.1381 9 9 5 0.1752 -0.1518 9 9 6 -0.7469 0.0429 9 9 7 3.2326 0.1004 9 9 8 2.7472 -0.1771 9 9 9 -2.8721 -0.0931 9 9 10 1.0262 0.1000 9 9 11 2.0008 0.0227 9 9 12 1.9979 0.1731 9 9 13 3.9202 -0.0189 9 10 1 -1.7924 -0.4094 9 10 2 1.7262 0.0860 9 10 3 0.7768 -0.0712 9 10 4 4.2908 -0.0324 9 10 5 0.1975 -0.0856 9 10 6 -1.9647 0.1202 9 10 7 1.0754 -0.0950 9 10 8 -2.6263 -0.0476 9 10 9 -1.0668 -0.0079 9 10 10 3.3837 0.0812 9 10 11 -0.8212 -0.0850 10 -1 2 -0.4032 -0.1768 10 -1 4 -0.2355 0.2686 10 0 0 5.7558 0.0025 10 0 1 -2.1603 0.1002 10 0 2 5.8703 0.0304 10 0 3 -0.0159 0.1320 10 0 4 -1.2220 -0.0292 10 0 5 -0.6158 -0.0531 10 0 6 -0.2435 0.0283 10 0 7 -0.1816 -0.2713 10 1 0 -0.4724 -0.8407 10 1 1 -3.1660 0.0629 10 1 2 2.3185 -0.1621 10 1 3 -5.2514 -0.0005 10 1 4 -0.0083 -0.0511 10 1 5 1.5656 0.0768 10 1 6 1.2997 -0.0948 10 1 7 -0.3214 0.0492 10 1 8 -1.1196 0.0808 10 1 9 -3.2509 -0.0016 10 2 0 -4.2565 0.0262 10 2 1 0.1931 0.2477 10 2 2 2.0767 -0.0375 10 2 3 -1.2227 -0.0110 10 2 4 3.8097 0.0369 10 2 5 -0.9725 -0.0858 10 2 6 1.1688 -0.0034 10 2 7 -2.5880 -0.0045 10 2 8 0.4139 -0.0015 10 2 9 0.7664 0.0156 10 2 10 1.3936 0.0054 10 3 0 0.2441 0.8087 10 3 1 -0.1859 -0.0296 10 3 2 0.5676 0.1735 10 3 3 -3.1901 -0.0146 10 3 4 -0.7245 0.1689 10 3 5 -2.6412 -0.0702 10 3 6 2.4324 0.1204 10 3 7 -4.7067 -0.0624 10 3 8 4.0730 0.1076 10 3 9 -0.7645 -0.0572 10 3 10 2.5043 -0.0223 10 3 11 1.5323 -0.0159 10 4 0 -1.2979 -0.0806 10 4 1 -0.9611 -0.3232 10 4 2 1.8231 -0.0093 10 4 3 -2.2626 -0.0577 10 4 4 3.1042 -0.0404 10 4 5 1.5471 -0.0604 10 4 6 1.0739 0.0036 10 4 7 -2.3643 0.0123 10 4 8 4.3381 -0.0011 10 4 9 -3.1982 -0.0048 10 4 10 0.2054 -0.0014 10 4 11 -5.4322 0.1461 10 5 0 -6.5991 -0.6828 10 5 1 -1.2264 0.0471 10 5 2 -0.8854 -0.1594 10 5 3 -1.0951 -0.0012 10 5 4 2.7266 -0.1358 10 5 5 -0.9755 0.1040 10 5 6 -0.1012 -0.1127 10 5 7 -0.2085 0.0482 10 5 8 1.1084 -0.1038 10 5 9 -0.9925 0.0545 10 5 10 0.1601 -0.0729 10 5 11 1.8328 0.0497 10 6 0 0.4364 0.1383 10 6 1 5.9493 0.1186 10 6 2 2.9993 0.0317 10 6 3 2.9456 0.1180 10 6 4 0.5327 0.0839 10 6 5 -1.1271 0.0103 10 6 6 -0.3987 -0.0535 10 6 7 -1.8779 0.0749 10 6 8 1.4905 0.0153 10 6 9 -0.3933 0.0144 10 6 10 -0.2056 0.0259 10 6 11 1.3357 -0.1080 10 7 0 1.6685 0.5642 10 7 1 -0.3054 -0.1059 10 7 2 -2.6546 0.1812 10 7 3 -2.5405 -0.0162 10 7 4 -1.6870 0.1288 10 7 5 -0.1813 -0.0783 10 7 6 0.1079 0.1164 10 7 7 -0.5530 -0.0087 10 7 8 2.5461 0.0700 10 7 9 -2.9467 -0.0621 10 7 10 0.5058 0.1083 10 7 11 -0.8902 -0.0879 10 8 1 -0.1956 -0.2165 10 8 2 0.9615 -0.0468 10 8 3 0.9904 0.0848 10 8 4 0.6891 -0.0686 10 8 5 -1.1610 -0.1776 10 8 6 -1.2344 -0.0329 10 8 7 -1.0401 0.0782 10 8 8 2.5585 -0.0009 10 8 10 2.0918 0.0109 10 9 4 -1.4926 -0.3610 10 9 5 0.7961 0.0380 10 9 6 1.9382 0.1490 10 9 7 3.0179 0.0603 11 5 6 -0.1563 0.0597 0 0 0 0.0 0.0 ; _shelx_fab_checksum 7106 _olex2_submission_special_instructions 'No special instructions were received' 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 Ni1 Ni 0.7739(2) 0.2551(2) 0.75171(13) 0.0504(10) Uani 1 1 d . U . . . Ni2 Ni 0.2799(2) 0.2449(2) 0.74808(12) 0.0502(10) Uani 1 1 d . U . . . N1 N 0.7720(15) 0.1641(14) 0.8388(8) 0.052(3) Uani 1 1 d . U . . . N2 N 0.7818(15) 0.1788(14) 0.8946(8) 0.055(3) Uani 1 1 d . U . . . N3 N 0.7900(15) 0.3549(14) 0.7834(8) 0.054(3) Uani 1 1 d . U . . . N4 N 0.7816(15) 0.4295(14) 0.6424(8) 0.053(3) Uani 1 1 d . U . . . N5 N 0.7749(14) 0.3398(14) 0.6620(8) 0.049(3) Uani 1 1 d . U . . . N6 N 0.2787(15) 0.1605(14) 0.8394(8) 0.049(4) Uani 1 1 d . U . . . N7 N 0.3390(16) 0.0717(15) 0.8575(8) 0.057(4) Uani 1 1 d . U . . . N8 N 0.4051(15) 0.1426(14) 0.7154(8) 0.052(3) Uani 1 1 d . U . . . N9 N 0.3419(16) 0.3193(15) 0.6058(8) 0.057(4) Uani 1 1 d . U . . . N10 N 0.2798(15) 0.3370(14) 0.6609(8) 0.053(3) Uani 1 1 d . U . . . C1 C 0.762(2) 0.0460(16) 0.7863(10) 0.055(5) Uani 1 1 d . U . . . H1A H 0.686809 0.088044 0.771405 0.083 Uiso 1 1 calc GR . . . . H1B H 0.768460 -0.021976 0.791069 0.083 Uiso 1 1 calc GR . . . . H1C H 0.827546 0.063434 0.754493 0.083 Uiso 1 1 calc GR . . . . C2 C 0.767(2) 0.0593(18) 0.8508(10) 0.058(4) Uani 1 1 d . U . . . C3 C 0.878(2) -0.011(2) 0.8796(12) 0.087(7) Uani 1 1 d . U . . . H3A H 0.948487 -0.001535 0.848707 0.130 Uiso 1 1 calc GR . . . . H3B H 0.876977 -0.077777 0.888321 0.130 Uiso 1 1 calc GR . . . . H3C H 0.879979 0.002830 0.920069 0.130 Uiso 1 1 calc GR . . . . C4 C 0.661(2) 0.046(2) 0.9015(12) 0.082(7) Uani 1 1 d . U . . . H4A H 0.679970 0.036349 0.944545 0.122 Uiso 1 1 calc GR . . . . H4B H 0.641082 -0.010168 0.900127 0.122 Uiso 1 1 calc GR . . . . H4C H 0.593472 0.104680 0.892636 0.122 Uiso 1 1 calc GR . . . . C5 C 0.768(3) 0.241(2) 1.1697(12) 0.099(8) Uani 1 1 d . U . . . H5A H 0.712680 0.204719 1.194239 0.148 Uiso 1 1 calc GR . . . . H5B H 0.740669 0.305888 1.178122 0.148 Uiso 1 1 calc GR . . . . H5C H 0.846483 0.206518 1.183268 0.148 Uiso 1 1 calc GR . . . . C6 C 0.776(2) 0.251(2) 1.1026(12) 0.079(5) Uani 1 1 d . U . . . C7 C 0.818(2) 0.171(2) 1.0784(11) 0.069(5) Uani 1 1 d . U . . . H7 H 0.843300 0.108612 1.106965 0.082 Uiso 1 1 calc R . . . . C8 C 0.825(2) 0.1787(19) 1.0143(10) 0.064(5) Uani 1 1 d . U . . . H8 H 0.861571 0.120475 1.000308 0.077 Uiso 1 1 calc R . . . . C9 C 0.785(2) 0.2619(19) 0.9680(11) 0.062(4) Uani 1 1 d . U . . . C10 C 0.728(2) 0.348(2) 0.9931(11) 0.074(5) Uani 1 1 d . U . . . H10 H 0.692354 0.408239 0.965462 0.088 Uiso 1 1 calc R . . . . C11 C 0.728(2) 0.340(2) 1.0605(11) 0.080(5) Uani 1 1 d . U . . . H11 H 0.692663 0.396130 1.076437 0.097 Uiso 1 1 calc R . . . . C12 C 0.7902(19) 0.2640(18) 0.8992(10) 0.056(4) Uani 1 1 d . U . . . C13 C 0.8044(19) 0.3490(18) 0.8474(10) 0.055(4) Uani 1 1 d . U . . . C14 C 0.8293(19) 0.4335(17) 0.8497(10) 0.056(4) Uani 1 1 d . U . . . H14 H 0.845512 0.444146 0.886545 0.067 Uiso 1 1 calc R . . . . C15 C 0.8257(19) 0.4940(18) 0.7914(10) 0.056(4) Uani 1 1 d . U . . . H15 H 0.836338 0.556778 0.778845 0.068 Uiso 1 1 calc R . . . . C16 C 0.8028(19) 0.4468(18) 0.7507(10) 0.054(4) Uani 1 1 d . U . . . C17 C 0.7872(19) 0.4825(17) 0.6833(10) 0.054(3) Uani 1 1 d . U . . . C18 C 0.783(2) 0.5815(19) 0.6463(11) 0.061(4) Uani 1 1 d . U . . . C19 C 0.727(2) 0.659(2) 0.6754(12) 0.072(5) Uani 1 1 d . U . . . H19 H 0.693439 0.643586 0.719828 0.086 Uiso 1 1 calc R . . . . C20 C 0.715(2) 0.761(2) 0.6425(12) 0.080(5) Uani 1 1 d . U . . . H20 H 0.679479 0.810822 0.664753 0.096 Uiso 1 1 calc R . . . . C21 C 0.760(2) 0.781(2) 0.5763(13) 0.082(5) Uani 1 1 d . U . . . C22 C 0.815(2) 0.703(2) 0.5448(12) 0.074(5) Uani 1 1 d . U . . . H22 H 0.844243 0.716414 0.499809 0.089 Uiso 1 1 calc R . . . . C23 C 0.824(2) 0.6056(19) 0.5827(11) 0.065(5) Uani 1 1 d . U . . . H23 H 0.861611 0.554594 0.561489 0.078 Uiso 1 1 calc R . . . . C24 C 0.757(3) 0.879(2) 0.5366(14) 0.101(8) Uani 1 1 d . U . . . H24A H 0.683138 0.909260 0.518263 0.152 Uiso 1 1 calc GR . . . . H24B H 0.824177 0.875333 0.501461 0.152 Uiso 1 1 calc GR . . . . H24C H 0.762309 0.917812 0.563450 0.152 Uiso 1 1 calc GR . . . . C25 C 0.767(2) 0.3071(18) 0.6036(10) 0.057(4) Uani 1 1 d . U . . . C26 C 0.766(2) 0.1990(17) 0.6293(10) 0.062(6) Uani 1 1 d . U . . . H26A H 0.840426 0.158950 0.646394 0.094 Uiso 1 1 calc GR . . . . H26B H 0.759159 0.176074 0.593875 0.094 Uiso 1 1 calc GR . . . . H26C H 0.699547 0.193960 0.663928 0.094 Uiso 1 1 calc GR . . . . C27 C 0.655(2) 0.374(2) 0.5740(13) 0.085(7) Uani 1 1 d . U . . . H27A H 0.585231 0.366358 0.605690 0.127 Uiso 1 1 calc GR . . . . H27B H 0.653237 0.356504 0.535081 0.127 Uiso 1 1 calc GR . . . . H27C H 0.655976 0.441651 0.562533 0.127 Uiso 1 1 calc GR . . . . C28 C 0.881(2) 0.312(2) 0.5526(11) 0.080(7) Uani 1 1 d . U . . . H28A H 0.879831 0.379807 0.533590 0.119 Uiso 1 1 calc GR . . . . H28B H 0.882730 0.282526 0.518272 0.119 Uiso 1 1 calc GR . . . . H28C H 0.951244 0.276077 0.573951 0.119 Uiso 1 1 calc GR . . . . C33 C 0.197(2) 0.1918(18) 0.8972(10) 0.060(4) Uani 1 1 d . U . . . C34 C 0.1226(19) 0.2988(16) 0.8732(10) 0.054(5) Uani 1 1 d . U . . . H34A H 0.165568 0.342401 0.873596 0.081 Uiso 1 1 calc GR . . . . H34B H 0.046831 0.311499 0.901764 0.081 Uiso 1 1 calc GR . . . . H34C H 0.108311 0.310014 0.828921 0.081 Uiso 1 1 calc GR . . . . C35 C 0.116(2) 0.126(2) 0.9282(13) 0.089(7) Uani 1 1 d . U . . . H35A H 0.068252 0.131285 0.896321 0.133 Uiso 1 1 calc GR . . . . H35B H 0.063064 0.147395 0.965658 0.133 Uiso 1 1 calc GR . . . . H35C H 0.163715 0.058800 0.942318 0.133 Uiso 1 1 calc GR . . . . C36 C 0.270(2) 0.183(2) 0.9476(11) 0.083(7) Uani 1 1 d . U . . . H36A H 0.328225 0.118141 0.955439 0.124 Uiso 1 1 calc GR . . . . H36B H 0.217758 0.191251 0.988158 0.124 Uiso 1 1 calc GR . . . . H36C H 0.311026 0.232619 0.931637 0.124 Uiso 1 1 calc GR . . . . C37 C 0.581(3) -0.389(2) 0.9552(15) 0.139(11) Uani 1 1 d . U . . . H37A H 0.661809 -0.419742 0.936617 0.208 Uiso 1 1 calc GR . . . . H37B H 0.526555 -0.418400 0.949101 0.208 Uiso 1 1 calc GR . . . . H37C H 0.578418 -0.396939 1.001552 0.208 Uiso 1 1 calc GR . . . . C38 C 0.546(3) -0.281(2) 0.9216(14) 0.091(5) Uani 1 1 d . U . . . C39 C 0.517(2) -0.204(2) 0.9515(13) 0.079(5) Uani 1 1 d . U . . . H39 H 0.525152 -0.219401 0.995908 0.095 Uiso 1 1 calc R . . . . C40 C 0.478(2) -0.1088(19) 0.9194(11) 0.068(5) Uani 1 1 d . U . . . H40 H 0.458815 -0.058942 0.941036 0.081 Uiso 1 1 calc R . . . . C41 C 0.468(2) -0.0856(19) 0.8530(11) 0.063(4) Uani 1 1 d . U . . . C42 C 0.499(2) -0.1650(19) 0.8230(12) 0.073(5) Uani 1 1 d . U . . . H42 H 0.497330 -0.153202 0.778021 0.087 Uiso 1 1 calc R . . . . C43 C 0.528(2) -0.253(2) 0.8597(13) 0.088(5) Uani 1 1 d . U . . . H43 H 0.537806 -0.303833 0.840201 0.105 Uiso 1 1 calc R . . . . C44 C 0.420(2) 0.0184(18) 0.8193(10) 0.055(4) Uani 1 1 d . U . . . C45 C 0.459(2) 0.0568(18) 0.7496(10) 0.054(4) Uani 1 1 d . U . . . C46 C 0.560(2) 0.0077(18) 0.7090(10) 0.060(5) Uani 1 1 d . U . . . H46 H 0.614774 -0.054175 0.722646 0.072 Uiso 1 1 calc R . . . . C47 C 0.560(2) 0.0664(17) 0.6486(10) 0.059(5) Uani 1 1 d . U . . . H47 H 0.614580 0.055305 0.610816 0.070 Uiso 1 1 calc R . . . . C48 C 0.458(2) 0.1514(18) 0.6545(10) 0.055(4) Uani 1 1 d . U . . . C49 C 0.422(2) 0.2356(19) 0.5994(10) 0.055(4) Uani 1 1 d . U . . . C50 C 0.472(2) 0.233(2) 0.5319(10) 0.063(4) Uani 1 1 d . U . . . C51 C 0.505(2) 0.148(2) 0.5083(11) 0.073(5) Uani 1 1 d . U . . . H51 H 0.497250 0.087866 0.537391 0.087 Uiso 1 1 calc R . . . . C52 C 0.548(2) 0.152(2) 0.4416(11) 0.080(5) Uani 1 1 d . U . . . H52 H 0.570999 0.093743 0.427691 0.096 Uiso 1 1 calc R . . . . C53 C 0.557(2) 0.234(2) 0.3978(12) 0.082(5) Uani 1 1 d . U . . . C54 C 0.519(2) 0.326(2) 0.4198(11) 0.072(5) Uani 1 1 d . U . . . H54 H 0.521033 0.385792 0.389667 0.086 Uiso 1 1 calc R . . . . C55 C 0.480(2) 0.3203(19) 0.4857(10) 0.066(5) Uani 1 1 d . U . . . H55 H 0.459165 0.377783 0.500067 0.079 Uiso 1 1 calc R . . . . C56 C 0.592(3) 0.233(2) 0.3309(12) 0.108(9) Uani 1 1 d . U . . . H56A H 0.659411 0.175465 0.326655 0.161 Uiso 1 1 calc GR . . . . H56B H 0.613701 0.291731 0.306257 0.161 Uiso 1 1 calc GR . . . . H56C H 0.525618 0.230275 0.313979 0.161 Uiso 1 1 calc GR . . . . C57 C 0.197(2) 0.4410(18) 0.6472(10) 0.058(4) Uani 1 1 d . U . . . C58 C 0.271(2) 0.5119(19) 0.6191(11) 0.081(7) Uani 1 1 d . U . . . H58A H 0.340692 0.488326 0.640983 0.121 Uiso 1 1 calc GR . . . . H58B H 0.223365 0.576143 0.625533 0.121 Uiso 1 1 calc GR . . . . H58C H 0.296073 0.516729 0.572591 0.121 Uiso 1 1 calc GR . . . . C59 C 0.116(2) 0.456(2) 0.5991(11) 0.079(7) Uani 1 1 d . U . . . H59A H 0.161624 0.456742 0.555801 0.119 Uiso 1 1 calc GR . . . . H59B H 0.052718 0.517233 0.597918 0.119 Uiso 1 1 calc GR . . . . H59C H 0.080626 0.401932 0.612814 0.119 Uiso 1 1 calc GR . . . . C60 C 0.1234(19) 0.4577(17) 0.7132(10) 0.060(6) Uani 1 1 d . U . . . H60A H 0.105631 0.397686 0.739819 0.090 Uiso 1 1 calc GR . . . . H60B H 0.049408 0.509771 0.705484 0.090 Uiso 1 1 calc GR . . . . H60C H 0.168790 0.476247 0.735854 0.090 Uiso 1 1 calc GR . . . . S1 S 0.0744(13) 0.1441(13) 0.7416(8) 0.072(3) Uani 0.466(10) 1 d D U P A 1 O1 O 0.1235(13) 0.2215(13) 0.7403(7) 0.073(3) Uani 1 1 d . U . . . O2 O 0.087(3) 0.068(3) 0.8033(15) 0.071(7) Uani 0.466(10) 1 d D U P A 1 O3 O -0.0478(12) 0.1797(13) 0.7260(7) 0.071(4) Uani 1 1 d . U . . . C61 C 0.1574(19) 0.0806(16) 0.6795(10) 0.080(4) Uani 0.466(10) 1 d D U P A 1 F1 F 0.178(2) 0.148(2) 0.6250(13) 0.090(6) Uani 0.466(10) 1 d D U P A 1 F2 F 0.110(3) 0.025(2) 0.6626(16) 0.092(6) Uani 0.466(10) 1 d D U P A 1 F3 F 0.265(2) 0.023(2) 0.6948(16) 0.082(6) Uani 0.466(10) 1 d D U P A 1 S1A S 0.0743(11) 0.1828(11) 0.6998(7) 0.074(3) Uani 0.534(10) 1 d D U P A 2 O2A O 0.086(3) 0.234(2) 0.6301(12) 0.072(6) Uani 0.534(10) 1 d D U P A 2 C61A C 0.1583(16) 0.0552(14) 0.7042(9) 0.080(4) Uani 0.534(10) 1 d D U P A 2 F1A F 0.177(2) 0.005(2) 0.7652(10) 0.095(6) Uani 0.534(10) 1 d D U P A 2 F2A F 0.2625(19) 0.049(2) 0.6650(11) 0.082(6) Uani 0.534(10) 1 d D U P A 2 F3A F 0.092(3) 0.019(3) 0.6837(12) 0.090(6) Uani 0.534(10) 1 d D U P A 2 S4 S 0.4788(12) 0.3578(11) 0.7595(7) 0.061(3) Uani 0.483(10) 1 d D U P B 1 O4 O 0.481(3) 0.431(2) 0.6988(14) 0.070(7) Uani 0.483(10) 1 d D U P B 1 O5 O 0.5927(12) 0.2791(11) 0.7585(6) 0.057(3) Uani 1 1 d . U . . . O6 O 0.3730(12) 0.3254(11) 0.7750(7) 0.056(3) Uani 1 1 d . U . . . C62 C 0.463(2) 0.4158(15) 0.8232(8) 0.066(4) Uani 0.483(10) 1 d D U P B 1 F4 F 0.529(3) 0.477(2) 0.8082(15) 0.073(5) Uani 0.483(10) 1 d D U P B 1 F5 F 0.350(2) 0.469(2) 0.8363(16) 0.080(7) Uani 0.483(10) 1 d D U P B 1 F6 F 0.492(2) 0.3512(19) 0.8786(11) 0.078(6) Uani 0.483(10) 1 d D U P B 1 S4A S 0.4773(11) 0.3173(10) 0.7993(6) 0.061(3) Uani 0.517(10) 1 d D U P B 2 O4A O 0.479(3) 0.261(2) 0.8657(12) 0.069(7) Uani 0.517(10) 1 d D U P B 2 C62A C 0.4609(19) 0.4429(12) 0.7964(10) 0.066(4) Uani 0.517(10) 1 d D U P B 2 F4A F 0.533(2) 0.447(2) 0.8328(11) 0.074(5) Uani 0.517(10) 1 d D U P B 2 F5A F 0.351(2) 0.492(3) 0.8178(13) 0.082(7) Uani 0.517(10) 1 d D U P B 2 F6A F 0.489(2) 0.492(2) 0.7359(10) 0.080(5) Uani 0.517(10) 1 d D U P B 2 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 Ni1 0.0387(18) 0.081(2) 0.0251(17) 0.0243(15) -0.0182(13) -0.0339(16) Ni2 0.0378(18) 0.083(2) 0.0215(17) 0.0254(15) -0.0165(13) -0.0345(16) N1 0.048(6) 0.078(6) 0.027(6) 0.020(6) -0.018(5) -0.037(5) N2 0.051(7) 0.083(7) 0.027(6) 0.021(6) -0.017(6) -0.038(6) N3 0.047(6) 0.080(6) 0.028(5) 0.015(5) -0.016(5) -0.029(5) N4 0.047(7) 0.079(7) 0.028(7) 0.019(6) -0.016(6) -0.035(6) N5 0.043(6) 0.077(6) 0.025(6) 0.021(5) -0.020(5) -0.037(6) N6 0.038(8) 0.071(8) 0.028(7) 0.022(6) -0.011(5) -0.031(6) N7 0.050(8) 0.077(8) 0.025(7) 0.024(6) -0.010(6) -0.022(6) N8 0.045(6) 0.082(6) 0.025(5) 0.021(5) -0.015(5) -0.039(5) N9 0.052(8) 0.083(8) 0.018(6) 0.023(6) -0.010(6) -0.027(6) N10 0.046(6) 0.082(6) 0.017(6) 0.021(6) -0.014(5) -0.025(5) C1 0.066(13) 0.054(12) 0.035(9) 0.029(9) -0.021(9) -0.030(11) C2 0.059(8) 0.077(8) 0.036(7) 0.022(7) -0.020(6) -0.039(7) C3 0.078(12) 0.104(14) 0.064(14) 0.026(13) -0.040(11) -0.032(11) C4 0.082(12) 0.108(15) 0.063(12) 0.003(12) -0.003(10) -0.065(11) C5 0.116(17) 0.131(18) 0.042(10) 0.008(11) -0.014(12) -0.053(15) C6 0.087(10) 0.104(11) 0.039(8) 0.011(7) -0.015(8) -0.043(9) C7 0.072(9) 0.097(10) 0.033(7) 0.020(8) -0.017(8) -0.045(9) C8 0.061(9) 0.093(10) 0.032(7) 0.024(7) -0.018(8) -0.045(8) C9 0.060(8) 0.089(9) 0.032(6) 0.020(6) -0.015(7) -0.043(7) C10 0.077(9) 0.096(10) 0.038(7) 0.016(7) -0.008(8) -0.042(8) C11 0.088(10) 0.103(10) 0.041(8) 0.008(8) -0.010(8) -0.041(9) C12 0.050(7) 0.084(7) 0.032(6) 0.017(6) -0.020(6) -0.038(6) C13 0.049(7) 0.082(7) 0.032(6) 0.014(6) -0.018(6) -0.032(6) C14 0.048(8) 0.081(8) 0.034(7) 0.013(7) -0.019(7) -0.031(7) C15 0.049(8) 0.082(8) 0.034(7) 0.013(6) -0.019(7) -0.030(7) C16 0.047(7) 0.081(7) 0.030(6) 0.012(6) -0.016(6) -0.031(6) C17 0.048(7) 0.079(7) 0.030(6) 0.018(5) -0.013(6) -0.038(6) C18 0.055(8) 0.083(8) 0.039(7) 0.022(6) -0.019(7) -0.037(7) C19 0.067(9) 0.088(9) 0.054(9) 0.016(7) -0.023(8) -0.034(8) C20 0.077(10) 0.088(9) 0.063(9) 0.018(8) -0.022(8) -0.035(9) C21 0.083(10) 0.089(9) 0.063(9) 0.021(7) -0.022(8) -0.038(9) C22 0.071(10) 0.088(9) 0.051(9) 0.025(7) -0.021(8) -0.040(9) C23 0.059(9) 0.088(9) 0.039(8) 0.025(7) -0.023(8) -0.039(8) C24 0.120(17) 0.091(12) 0.081(15) 0.020(11) -0.027(14) -0.046(13) C25 0.061(8) 0.079(8) 0.028(8) 0.019(7) -0.021(6) -0.038(7) C26 0.074(14) 0.078(11) 0.034(12) 0.009(10) -0.012(10) -0.041(10) C27 0.084(12) 0.100(14) 0.071(14) 0.009(12) -0.056(11) -0.028(12) C28 0.081(12) 0.099(15) 0.043(12) 0.019(11) -0.005(9) -0.045(12) C33 0.050(9) 0.081(8) 0.034(8) 0.016(7) -0.008(6) -0.026(7) C34 0.061(11) 0.076(10) 0.022(10) 0.011(8) -0.022(8) -0.028(8) C35 0.055(13) 0.104(14) 0.073(14) 0.028(13) 0.010(11) -0.039(11) C36 0.071(14) 0.112(16) 0.048(12) 0.005(12) -0.026(10) -0.017(12) C37 0.138(19) 0.084(12) 0.094(17) 0.044(13) 0.028(16) -0.001(15) C38 0.088(10) 0.079(9) 0.061(9) 0.029(8) -0.004(9) -0.017(9) C39 0.070(10) 0.081(9) 0.052(9) 0.031(7) -0.011(8) -0.021(9) C40 0.059(9) 0.079(9) 0.044(8) 0.027(7) -0.016(8) -0.027(8) C41 0.055(8) 0.076(8) 0.042(7) 0.022(6) -0.015(7) -0.028(7) C42 0.069(9) 0.076(9) 0.052(9) 0.022(7) -0.015(8) -0.026(9) C43 0.086(10) 0.077(9) 0.062(9) 0.027(8) -0.008(9) -0.019(9) C44 0.050(7) 0.076(7) 0.028(6) 0.017(6) -0.015(6) -0.027(6) C45 0.050(7) 0.081(7) 0.026(6) 0.013(6) -0.013(6) -0.034(6) C46 0.058(8) 0.083(9) 0.027(7) 0.016(7) -0.009(7) -0.030(7) C47 0.057(8) 0.080(9) 0.028(7) 0.016(7) -0.007(7) -0.034(7) C48 0.051(7) 0.080(7) 0.026(6) 0.018(6) -0.012(6) -0.035(6) C49 0.050(7) 0.083(7) 0.023(6) 0.018(6) -0.008(6) -0.034(6) C50 0.059(8) 0.093(8) 0.024(6) 0.018(6) -0.009(6) -0.034(7) C51 0.076(9) 0.100(10) 0.029(7) 0.011(7) -0.011(8) -0.032(9) C52 0.088(10) 0.106(10) 0.031(7) 0.006(7) -0.011(8) -0.030(9) C53 0.087(10) 0.110(10) 0.031(7) 0.011(7) -0.013(8) -0.031(9) C54 0.070(9) 0.104(10) 0.028(7) 0.018(7) -0.011(8) -0.037(9) C55 0.061(9) 0.098(9) 0.026(7) 0.022(7) -0.011(7) -0.039(8) C56 0.131(18) 0.128(18) 0.036(10) 0.000(11) -0.013(12) -0.022(16) C57 0.051(8) 0.085(8) 0.023(7) 0.019(7) -0.018(6) -0.022(6) C58 0.077(14) 0.097(13) 0.045(13) 0.028(12) -0.009(11) -0.039(11) C59 0.054(13) 0.122(16) 0.040(11) 0.013(12) -0.028(9) -0.015(11) C60 0.054(12) 0.076(13) 0.028(9) 0.023(9) -0.016(8) -0.019(10) S1 0.042(5) 0.116(7) 0.063(7) -0.006(6) -0.015(5) -0.041(5) O1 0.044(6) 0.123(8) 0.060(7) 0.006(6) -0.021(6) -0.054(6) O2 0.046(13) 0.106(14) 0.065(12) 0.001(11) -0.020(10) -0.041(11) O3 0.029(6) 0.121(8) 0.068(7) 0.004(7) -0.017(5) -0.046(6) C61 0.050(6) 0.119(8) 0.074(7) -0.010(6) -0.012(6) -0.040(6) F1 0.055(9) 0.128(11) 0.073(9) -0.006(9) -0.002(9) -0.033(8) F2 0.072(11) 0.127(11) 0.091(13) -0.032(10) -0.013(10) -0.041(9) F3 0.054(9) 0.117(12) 0.077(12) -0.018(10) -0.018(9) -0.030(8) S1A 0.044(5) 0.115(7) 0.069(6) -0.005(6) -0.013(5) -0.042(5) O2A 0.047(12) 0.117(14) 0.052(11) -0.004(11) -0.006(10) -0.040(11) C61A 0.050(6) 0.118(8) 0.074(8) -0.009(7) -0.011(6) -0.040(6) F1A 0.059(10) 0.121(11) 0.084(9) 0.003(9) -0.014(8) -0.025(9) F2A 0.052(8) 0.115(11) 0.077(11) -0.014(10) -0.007(8) -0.036(8) F3A 0.068(10) 0.120(11) 0.095(13) -0.027(10) -0.002(10) -0.050(9) S4 0.054(5) 0.081(6) 0.044(6) 0.013(5) -0.021(5) -0.030(5) O4 0.063(13) 0.083(13) 0.048(11) 0.029(11) -0.020(11) -0.036(10) O5 0.044(6) 0.074(7) 0.039(6) 0.021(6) -0.015(5) -0.028(5) O6 0.046(6) 0.077(7) 0.044(7) 0.019(6) -0.026(5) -0.035(5) C62 0.060(6) 0.083(7) 0.052(7) 0.007(6) -0.021(6) -0.030(6) F4 0.071(9) 0.084(11) 0.062(11) 0.001(9) -0.015(9) -0.035(8) F5 0.064(8) 0.092(13) 0.068(12) -0.001(10) -0.004(9) -0.025(8) F6 0.081(10) 0.100(11) 0.048(9) 0.004(8) -0.026(8) -0.029(9) S4A 0.053(5) 0.079(6) 0.046(6) 0.016(5) -0.021(5) -0.029(5) O4A 0.068(13) 0.093(13) 0.030(10) 0.024(11) -0.022(9) -0.028(12) C62A 0.060(6) 0.083(7) 0.052(7) 0.007(6) -0.021(6) -0.030(6) F4A 0.073(9) 0.094(11) 0.058(11) -0.004(9) -0.027(8) -0.029(9) F5A 0.064(9) 0.090(12) 0.074(12) 0.006(10) -0.015(8) -0.019(9) F6A 0.080(9) 0.084(10) 0.060(9) 0.020(8) -0.016(8) -0.034(8) 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 N1 Ni1 N5 176.2(8) . . ? N1 Ni1 O3 90.4(7) . 1_655 ? N1 Ni1 O5 89.5(6) . . ? N3 Ni1 N1 92.6(7) . . ? N3 Ni1 N5 91.1(7) . . ? N3 Ni1 O3 101.5(7) . 1_655 ? N3 Ni1 O5 106.2(7) . . ? N5 Ni1 O3 88.7(7) . 1_655 ? N5 Ni1 O5 89.5(6) . . ? O5 Ni1 O3 152.2(6) . 1_655 ? N6 Ni2 O1 91.1(6) . . ? N6 Ni2 O6 87.8(6) . . ? N8 Ni2 N6 91.4(7) . . ? N8 Ni2 N10 92.0(7) . . ? N8 Ni2 O1 103.7(7) . . ? N8 Ni2 O6 104.7(6) . . ? N10 Ni2 N6 175.4(8) . . ? N10 Ni2 O1 91.1(6) . . ? N10 Ni2 O6 88.3(6) . . ? O1 Ni2 O6 151.6(7) . . ? N2 N1 Ni1 127.5(14) . . ? N2 N1 C2 109.9(15) . . ? C2 N1 Ni1 122.5(13) . . ? N1 N2 C12 123.6(17) . . ? C13 N3 Ni1 128.1(15) . . ? C16 N3 Ni1 131.0(14) . . ? C16 N3 C13 100.7(18) . . ? N5 N4 C17 124.6(17) . . ? N4 N5 Ni1 127.3(14) . . ? N4 N5 C25 109.7(15) . . ? C25 N5 Ni1 123.1(14) . . ? N7 N6 Ni2 126.7(15) . . ? N7 N6 C33 109.0(16) . . ? C33 N6 Ni2 124.1(14) . . ? N6 N7 C44 126.2(18) . . ? C45 N8 Ni2 126.9(15) . . ? C45 N8 C48 108(2) . . ? C48 N8 Ni2 125.0(16) . . ? N10 N9 C49 125.3(18) . . ? N9 N10 Ni2 127.5(15) . . ? N9 N10 C57 108.9(15) . . ? C57 N10 Ni2 123.5(13) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C1 C2 N1 107.3(16) . . ? C1 C2 C3 112(2) . . ? C1 C2 C4 114.0(19) . . ? C3 C2 N1 107.5(18) . . ? C4 C2 N1 108(2) . . ? C4 C2 C3 107.5(19) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? C7 C6 C5 120(3) . . ? C7 C6 C11 117(3) . . ? C11 C6 C5 122(3) . . ? C6 C7 H7 119.2 . . ? C8 C7 C6 122(3) . . ? C8 C7 H7 119.2 . . ? C7 C8 H8 116.8 . . ? C7 C8 C9 126(3) . . ? C9 C8 H8 116.8 . . ? C8 C9 C10 114(2) . . ? C8 C9 C12 123(3) . . ? C10 C9 C12 123(2) . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119(2) . . ? C11 C10 H10 120.4 . . ? C6 C11 C10 122(3) . . ? C6 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? N2 C12 C9 110.9(19) . . ? N2 C12 C13 129(2) . . ? C13 C12 C9 120(2) . . ? N3 C13 C12 119(2) . . ? N3 C13 C14 111.3(18) . . ? C14 C13 C12 130(2) . . ? C13 C14 H14 126.0 . . ? C15 C14 C13 108(2) . . ? C15 C14 H14 126.0 . . ? C14 C15 H15 126.6 . . ? C14 C15 C16 107(2) . . ? C16 C15 H15 126.6 . . ? N3 C16 C15 113.2(18) . . ? N3 C16 C17 118(2) . . ? C15 C16 C17 129(2) . . ? N4 C17 C16 127(2) . . ? N4 C17 C18 109.7(18) . . ? C16 C17 C18 123(2) . . ? C19 C18 C17 120(2) . . ? C23 C18 C17 123(3) . . ? C23 C18 C19 116(2) . . ? C18 C19 H19 117.6 . . ? C18 C19 C20 125(2) . . ? C20 C19 H19 117.6 . . ? C19 C20 H20 121.8 . . ? C21 C20 C19 116(3) . . ? C21 C20 H20 121.8 . . ? C20 C21 C22 120(3) . . ? C20 C21 C24 123(3) . . ? C22 C21 C24 117(3) . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 119(2) . . ? C23 C22 H22 120.6 . . ? C18 C23 C22 124(3) . . ? C18 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 107.0(16) . . ? N5 C25 C28 108.6(17) . . ? C26 C25 C28 108(2) . . ? C27 C25 N5 109(2) . . ? C27 C25 C26 112.5(19) . . ? C27 C25 C28 110.9(19) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C33 C34 107.6(16) . . ? N6 C33 C35 110(2) . . ? N6 C33 C36 109.4(18) . . ? C35 C33 C34 110.3(19) . . ? C36 C33 C34 111(2) . . ? C36 C33 C35 108.5(19) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? C39 C38 C37 126(3) . . ? C43 C38 C37 119(3) . . ? C43 C38 C39 115(3) . . ? C38 C39 H39 118.5 . . ? C40 C39 C38 123(3) . . ? C40 C39 H39 118.5 . . ? C39 C40 H40 120.6 . . ? C39 C40 C41 119(3) . . ? C41 C40 H40 120.6 . . ? C40 C41 C42 118(2) . . ? C40 C41 C44 118(2) . . ? C42 C41 C44 124(2) . . ? C41 C42 H42 121.1 . . ? C43 C42 C41 118(3) . . ? C43 C42 H42 121.1 . . ? C38 C43 H43 116.1 . . ? C42 C43 C38 128(3) . . ? C42 C43 H43 116.1 . . ? N7 C44 C41 114.0(19) . . ? N7 C44 C45 125(2) . . ? C45 C44 C41 121(2) . . ? N8 C45 C44 123(2) . . ? N8 C45 C46 110.1(18) . . ? C46 C45 C44 127(2) . . ? C45 C46 H46 126.4 . . ? C47 C46 C45 107(2) . . ? C47 C46 H46 126.4 . . ? C46 C47 H47 128.0 . . ? C46 C47 C48 104(2) . . ? C48 C47 H47 128.0 . . ? N8 C48 C47 110.8(19) . . ? N8 C48 C49 126(2) . . ? C47 C48 C49 124(2) . . ? N9 C49 C48 124(2) . . ? N9 C49 C50 114(2) . . ? C50 C49 C48 122(2) . . ? C51 C50 C49 124(2) . . ? C55 C50 C49 119(2) . . ? C55 C50 C51 117(2) . . ? C50 C51 H51 119.7 . . ? C52 C51 C50 121(2) . . ? C52 C51 H51 119.7 . . ? C51 C52 H52 118.6 . . ? C53 C52 C51 123(3) . . ? C53 C52 H52 118.6 . . ? C52 C53 C54 118(2) . . ? C52 C53 C56 119(3) . . ? C56 C53 C54 122(2) . . ? C53 C54 H54 120.8 . . ? C55 C54 C53 118(2) . . ? C55 C54 H54 120.8 . . ? C50 C55 H55 118.7 . . ? C54 C55 C50 123(3) . . ? C54 C55 H55 118.7 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N10 C57 C58 109.1(18) . . ? N10 C57 C59 111(2) . . ? N10 C57 C60 107.0(16) . . ? C58 C57 C59 109.6(18) . . ? C58 C57 C60 110(2) . . ? C59 C57 C60 110.6(19) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O1 S1 O3 114.6(15) . . ? O1 S1 C61 111.1(13) . . ? O2 S1 O1 110.7(17) . . ? O2 S1 O3 112.5(16) . . ? O2 S1 C61 104(2) . . ? O3 S1 C61 102.8(13) . . ? S1 O1 Ni2 142.3(13) . . ? S1A O1 Ni2 141.8(11) . . ? S1 O3 Ni1 146.7(12) . 1_455 ? F1 C61 S1 107(2) . . ? F2 C61 S1 119(3) . . ? F2 C61 F1 106.0(13) . . ? F2 C61 F3 106.2(13) . . ? F3 C61 S1 111(2) . . ? F3 C61 F1 105.9(13) . . ? O1 S1A C61A 109.3(12) . . ? O3 S1A O1 112.7(13) . . ? O3 S1A O2A 111.7(15) . . ? O3 S1A C61A 103.7(12) . . ? O2A S1A O1 113.1(16) . . ? O2A S1A C61A 105.7(17) . . ? F1A C61A S1A 111(2) . . ? F1A C61A F2A 109.7(11) . . ? F1A C61A F3A 109.7(11) . . ? F2A C61A S1A 110(2) . . ? F3A C61A S1A 106(2) . . ? F3A C61A F2A 109.8(11) . . ? O4 S4 O5 108.7(17) . . ? O4 S4 O6 112.0(16) . . ? O4 S4 C62 107.3(19) . . ? O5 S4 C62 109.8(12) . . ? O6 S4 O5 114.9(12) . . ? O6 S4 C62 103.8(12) . . ? S4 O5 Ni1 141.1(11) . . ? S4A O5 Ni1 140.7(10) . . ? S4 O6 Ni2 145.3(11) . . ? S4A O6 Ni2 144.9(11) . . ? F4 C62 S4 113(2) . . ? F5 C62 S4 111(3) . . ? F5 C62 F4 106.7(13) . . ? F6 C62 S4 112.1(19) . . ? F6 C62 F4 106.7(13) . . ? F6 C62 F5 106.8(13) . . ? O5 S4A C62A 108.2(12) . . ? O6 S4A O5 114.6(12) . . ? O6 S4A C62A 103.3(11) . . ? O4A S4A O5 110.0(16) . . ? O4A S4A O6 111.7(15) . . ? O4A S4A C62A 108.7(17) . . ? F4A C62A S4A 111(2) . . ? F5A C62A S4A 113(2) . . ? F5A C62A F4A 107.0(13) . . ? F6A C62A S4A 110.9(19) . . ? F6A C62A F4A 107.1(13) . . ? F6A C62A F5A 107.0(13) . . ? 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 Ni1 N1 1.977(16) . ? Ni1 N3 1.94(2) . ? Ni1 N5 1.986(16) . ? Ni1 O3 2.109(16) 1_655 ? Ni1 O5 2.087(14) . ? Ni2 N6 2.012(16) . ? Ni2 N8 1.95(2) . ? Ni2 N10 1.984(16) . ? Ni2 O1 2.111(14) . ? Ni2 O6 2.205(14) . ? N1 N2 1.35(2) . ? N1 C2 1.55(3) . ? N2 C12 1.37(3) . ? N3 C13 1.43(3) . ? N3 C16 1.40(3) . ? N4 N5 1.32(2) . ? N4 C17 1.41(3) . ? N5 C25 1.55(3) . ? N6 N7 1.28(2) . ? N6 C33 1.51(3) . ? N7 C44 1.34(3) . ? N8 C45 1.31(3) . ? N8 C48 1.33(3) . ? N9 N10 1.32(2) . ? N9 C49 1.33(3) . ? N10 C57 1.53(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.51(3) . ? C2 C3 1.53(3) . ? C2 C4 1.52(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 C6 1.42(3) . ? C6 C7 1.37(4) . ? C6 C11 1.39(4) . ? C7 H7 0.9500 . ? C7 C8 1.36(3) . ? C8 H8 0.9500 . ? C8 C9 1.37(3) . ? C9 C10 1.45(3) . ? C9 C12 1.49(3) . ? C10 H10 0.9500 . ? C10 C11 1.44(3) . ? C11 H11 0.9500 . ? C12 C13 1.46(3) . ? C13 C14 1.43(3) . ? C14 H14 0.9500 . ? C14 C15 1.32(3) . ? C15 H15 0.9500 . ? C15 C16 1.43(3) . ? C16 C17 1.44(3) . ? C17 C18 1.45(3) . ? C18 C19 1.40(3) . ? C18 C23 1.35(3) . ? C19 H19 0.9500 . ? C19 C20 1.47(3) . ? C20 H20 0.9500 . ? C20 C21 1.40(4) . ? C21 C22 1.44(4) . ? C21 C24 1.46(3) . ? C22 H22 0.9500 . ? C22 C23 1.44(3) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.56(3) . ? C25 C27 1.54(3) . ? C25 C28 1.57(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C33 C34 1.55(3) . ? C33 C35 1.54(3) . ? C33 C36 1.53(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C37 C38 1.51(4) . ? C38 C39 1.42(4) . ? C38 C43 1.34(4) . ? C39 H39 0.9500 . ? C39 C40 1.36(3) . ? C40 H40 0.9500 . ? C40 C41 1.41(3) . ? C41 C42 1.45(3) . ? C41 C44 1.49(3) . ? C42 H42 0.9500 . ? C42 C43 1.30(3) . ? C43 H43 0.9500 . ? C44 C45 1.48(3) . ? C45 C46 1.45(3) . ? C46 H46 0.9500 . ? C46 C47 1.35(3) . ? C47 H47 0.9500 . ? C47 C48 1.47(3) . ? C48 C49 1.48(3) . ? C49 C50 1.47(3) . ? C50 C51 1.43(3) . ? C50 C55 1.42(3) . ? C51 H51 0.9500 . ? C51 C52 1.42(3) . ? C52 H52 0.9500 . ? C52 C53 1.33(3) . ? C53 C54 1.50(4) . ? C53 C56 1.43(3) . ? C54 H54 0.9500 . ? C54 C55 1.40(3) . ? C55 H55 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.53(3) . ? C57 C59 1.54(3) . ? C57 C60 1.56(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? S1 O1 1.48(2) . ? S1 O2 1.48(2) . ? S1 O3 1.48(2) . ? S1 C61 1.817(5) . ? O1 S1A 1.52(2) . ? O3 S1A 1.474(19) . ? C61 F1 1.346(9) . ? C61 F2 1.343(8) . ? C61 F3 1.345(9) . ? S1A O2A 1.48(2) . ? S1A C61A 1.833(12) . ? C61A F1A 1.345(9) . ? C61A F2A 1.346(9) . ? C61A F3A 1.346(9) . ? S4 O4 1.44(2) . ? S4 O5 1.49(2) . ? S4 O6 1.467(19) . ? S4 C62 1.815(5) . ? O5 S4A 1.509(19) . ? O6 S4A 1.449(18) . ? C62 F4 1.347(10) . ? C62 F5 1.343(10) . ? C62 F6 1.335(8) . ? S4A O4A 1.44(2) . ? S4A C62A 1.827(12) . ? C62A F4A 1.347(10) . ? C62A F5A 1.344(10) . ? C62A F6A 1.336(8) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.531 -0.031 697.7 10.6 ?