# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '1-2.txt' _publ_contact_author_name 'Dr Ashutosh Ghosh' _publ_contact_author_address ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; _publ_contact_author_email 'ghosh 59@yahoo.com' loop_ _publ_author_name _publ_author_address R.Biswas ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; P.Kar ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; Y.Song ; State Key Laboratory of Coordination Chemistry Nanjing National Laboratory of Microstructures School of Chemistry and Chemical Engineering Nanjing University Nanjing 210093, P. R. China ; A.Ghosh ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; data_1 _database_code_depnum_ccdc_archive 'CCDC 800753' #TrackingRef '1-2.txt' #TrackingRef '1-2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 N4 Ni2 O7' _chemical_formula_weight 788.21 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' N N 0.0061 0.0033 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4851(11) _cell_length_b 21.865(3) _cell_length_c 20.453(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.113(2) _cell_angle_gamma 90.00 _cell_volume 3756.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25199 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 24.55 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7933 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 25199 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 24.55 _reflns_number_total 6241 _reflns_number_gt 4745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+1.8691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6241 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.73074(4) 0.325211(15) 0.075118(18) 0.03655(12) Uani 1 1 d . . . Ni2 Ni 0.61709(4) 0.203113(15) 0.049231(18) 0.03622(12) Uani 1 1 d . . . O3 O 0.6896(2) 0.25224(8) 0.13699(9) 0.0401(5) Uani 1 1 d . . . H3A H 0.6054 0.2595 0.1636 0.048 Uiso 1 1 calc R . . H3B H 0.7847 0.2364 0.1634 0.048 Uiso 1 1 calc R . . O51 O 0.7666(2) 0.13129(8) 0.07956(10) 0.0428(5) Uani 1 1 d . . . O41 O 0.6010(2) 0.38310(9) 0.12420(10) 0.0474(5) Uani 1 1 d . . . O43 O 0.5163(3) 0.32139(10) 0.19967(11) 0.0595(6) Uani 1 1 d . . . O53 O 0.8893(3) 0.16779(10) 0.17549(11) 0.0571(6) Uani 1 1 d . . . O11 O 0.8178(2) 0.25591(8) 0.02637(9) 0.0395(5) Uani 1 1 d . . . O26 O 0.5122(2) 0.28445(8) 0.02550(10) 0.0425(5) Uani 1 1 d . . . N38 N 0.4202(3) 0.15543(11) 0.08098(14) 0.0523(7) Uani 1 1 d . . . N19 N 0.7736(3) 0.38519(10) 0.00570(12) 0.0437(6) Uani 1 1 d . . . N23 N 0.9470(3) 0.35967(11) 0.13160(12) 0.0485(6) Uani 1 1 d . . . N34 N 0.5450(3) 0.17032(11) -0.04121(13) 0.0455(6) Uani 1 1 d . . . C44 C 0.4435(3) 0.42593(13) 0.19825(14) 0.0390(7) Uani 1 1 d . . . C54 C 0.9717(3) 0.07220(12) 0.13899(14) 0.0373(7) Uani 1 1 d . . . C55 C 1.0784(4) 0.06389(14) 0.19597(16) 0.0485(8) Uani 1 1 d . . . H55 H 1.0871 0.0936 0.2288 0.058 Uiso 1 1 calc R . . C59 C 0.9595(4) 0.02729(13) 0.09080(16) 0.0483(8) Uani 1 1 d . . . H59 H 0.8883 0.0321 0.0522 0.058 Uiso 1 1 calc R . . C42 C 0.5256(3) 0.37227(13) 0.17194(15) 0.0419(7) Uani 1 1 d . . . C49 C 0.4404(4) 0.48241(14) 0.16727(16) 0.0510(8) Uani 1 1 d . . . H49 H 0.4877 0.4869 0.1292 0.061 Uiso 1 1 calc R . . C45 C 0.3715(4) 0.42089(16) 0.25468(15) 0.0552(9) Uani 1 1 d . . . H45 H 0.3727 0.3835 0.2765 0.066 Uiso 1 1 calc R . . C12 C 0.8637(3) 0.25711(14) -0.03228(15) 0.0420(7) Uani 1 1 d . . . C52 C 0.8690(3) 0.12853(13) 0.13089(15) 0.0394(7) Uani 1 1 d . . . C18 C 0.8311(4) 0.37148(16) -0.04703(17) 0.0517(8) Uani 1 1 d . . . C28 C 0.3991(4) 0.36411(15) -0.04290(19) 0.0618(10) Uani 1 1 d . . . H28 H 0.3960 0.3887 -0.0060 0.074 Uiso 1 1 calc R . . C32 C 0.4542(4) 0.26756(15) -0.09221(16) 0.0514(8) Uani 1 1 d . . . C13 C 0.9123(4) 0.20266(15) -0.06030(17) 0.0554(9) Uani 1 1 d . . . H13 H 0.9088 0.1662 -0.0372 0.066 Uiso 1 1 calc R . . C36 C 0.3988(4) 0.08022(15) -0.0152(2) 0.0693(11) Uani 1 1 d . . . H36A H 0.3021 0.1000 -0.0360 0.083 Uiso 1 1 calc R . . H36B H 0.3872 0.0367 -0.0237 0.083 Uiso 1 1 calc R . . C17 C 0.8694(4) 0.31160(15) -0.06953(15) 0.0493(8) Uani 1 1 d . . . C27 C 0.4575(3) 0.30366(14) -0.03469(16) 0.0461(8) Uani 1 1 d . . . C20 C 0.7733(4) 0.44976(13) 0.02441(17) 0.0555(9) Uani 1 1 d . . . H20A H 0.6795 0.4588 0.0448 0.067 Uiso 1 1 calc R . . H20B H 0.7715 0.4753 -0.0145 0.067 Uiso 1 1 calc R . . C29 C 0.3466(5) 0.38708(18) -0.1048(2) 0.0790(12) Uani 1 1 d . . . H29 H 0.3079 0.4269 -0.1089 0.095 Uiso 1 1 calc R . . C56 C 1.1723(4) 0.01215(17) 0.20493(19) 0.0630(10) Uani 1 1 d . . . H56 H 1.2439 0.0073 0.2434 0.076 Uiso 1 1 calc R . . C47 C 0.2974(4) 0.52624(17) 0.24801(19) 0.0658(10) Uani 1 1 d . . . H47 H 0.2493 0.5599 0.2648 0.079 Uiso 1 1 calc R . . C33 C 0.4896(4) 0.20295(16) -0.09102(19) 0.0567(9) Uani 1 1 d . . . C48 C 0.3681(4) 0.53193(15) 0.19205(19) 0.0637(10) Uani 1 1 d . . . H48 H 0.3673 0.5695 0.1707 0.076 Uiso 1 1 calc R . . C31 C 0.4011(5) 0.29331(19) -0.15451(19) 0.0761(12) Uani 1 1 d . . . H31 H 0.4008 0.2695 -0.1922 0.091 Uiso 1 1 calc R . . C57 C 1.1594(4) -0.03197(17) 0.1570(2) 0.0677(11) Uani 1 1 d . . . H57 H 1.2225 -0.0669 0.1630 0.081 Uiso 1 1 calc R . . C46 C 0.2979(4) 0.47069(18) 0.27910(18) 0.0677(10) Uani 1 1 d . . . H46 H 0.2487 0.4665 0.3167 0.081 Uiso 1 1 calc R . . C58 C 1.0533(4) -0.02481(15) 0.10002(19) 0.0631(10) Uani 1 1 d . . . H58 H 1.0446 -0.0550 0.0676 0.076 Uiso 1 1 calc R . . C35 C 0.5370(4) 0.10349(14) -0.04794(17) 0.0591(9) Uani 1 1 d . . . H35A H 0.6357 0.0853 -0.0270 0.071 Uiso 1 1 calc R . . H35B H 0.5217 0.0923 -0.0943 0.071 Uiso 1 1 calc R . . C21 C 0.9220(5) 0.46259(16) 0.0725(2) 0.0736(11) Uani 1 1 d . . . H21A H 1.0131 0.4553 0.0498 0.088 Uiso 1 1 calc R . . H21B H 0.9223 0.5058 0.0835 0.088 Uiso 1 1 calc R . . C39 C 0.2703(4) 0.18742(16) 0.0556(2) 0.0763(12) Uani 1 1 d . . . H39A H 0.2572 0.1882 0.0082 0.115 Uiso 1 1 calc R . . H39B H 0.2743 0.2286 0.0721 0.115 Uiso 1 1 calc R . . H39C H 0.1821 0.1663 0.0700 0.115 Uiso 1 1 calc R . . C22 C 0.9468(5) 0.42783(16) 0.1351(2) 0.0763(12) Uani 1 1 d . . . H22A H 0.8644 0.4400 0.1609 0.092 Uiso 1 1 calc R . . H22B H 1.0478 0.4406 0.1595 0.092 Uiso 1 1 calc R . . C40 C 0.4374(5) 0.15450(18) 0.15394(19) 0.0777(12) Uani 1 1 d . . . H40A H 0.4415 0.1957 0.1703 0.117 Uiso 1 1 calc R . . H40B H 0.5337 0.1335 0.1711 0.117 Uiso 1 1 calc R . . H40C H 0.3480 0.1337 0.1677 0.117 Uiso 1 1 calc R . . C14 C 0.9644(5) 0.20199(19) -0.1204(2) 0.0784(12) Uani 1 1 d . . . H14 H 0.9966 0.1652 -0.1372 0.094 Uiso 1 1 calc R . . C16 C 0.9236(5) 0.30868(19) -0.13131(19) 0.0785(12) Uani 1 1 d . . . H16 H 0.9278 0.3445 -0.1556 0.094 Uiso 1 1 calc R . . C37 C 0.4131(4) 0.09047(14) 0.05855(19) 0.0651(10) Uani 1 1 d . . . H37A H 0.3230 0.0711 0.0744 0.078 Uiso 1 1 calc R . . H37B H 0.5085 0.0699 0.0793 0.078 Uiso 1 1 calc R . . C24 C 0.9557(5) 0.3387(2) 0.20064(18) 0.0865(13) Uani 1 1 d . . . H24A H 0.8647 0.3534 0.2189 0.130 Uiso 1 1 calc R . . H24B H 1.0511 0.3542 0.2261 0.130 Uiso 1 1 calc R . . H24C H 0.9571 0.2948 0.2018 0.130 Uiso 1 1 calc R . . C25 C 1.0855(4) 0.3369(2) 0.1040(2) 0.0866(14) Uani 1 1 d . . . H25A H 1.0807 0.3508 0.0592 0.130 Uiso 1 1 calc R . . H25B H 1.0858 0.2930 0.1049 0.130 Uiso 1 1 calc R . . H25C H 1.1809 0.3520 0.1297 0.130 Uiso 1 1 calc R . . C30 C 0.3499(5) 0.3526(2) -0.1607(2) 0.0876(14) Uani 1 1 d . . . H30 H 0.3178 0.3693 -0.2022 0.105 Uiso 1 1 calc R . . C15 C 0.9703(6) 0.2551(2) -0.1568(2) 0.0948(15) Uani 1 1 d . . . H15 H 1.0054 0.2542 -0.1979 0.114 Uiso 1 1 calc R . . H18 H 0.854(4) 0.4044(14) -0.0756(15) 0.060(10) Uiso 1 1 d . . . H33 H 0.466(5) 0.1809(18) -0.132(2) 0.095(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0408(2) 0.0293(2) 0.0413(2) -0.00127(16) 0.01173(17) -0.00117(16) Ni2 0.0365(2) 0.0283(2) 0.0430(2) 0.00190(16) 0.00285(16) 0.00000(15) O3 0.0426(11) 0.0371(10) 0.0420(12) 0.0022(9) 0.0114(9) 0.0008(9) O51 0.0432(12) 0.0339(11) 0.0489(13) 0.0003(9) -0.0025(10) 0.0041(9) O41 0.0566(13) 0.0377(11) 0.0530(13) -0.0009(10) 0.0258(11) 0.0016(10) O43 0.0726(16) 0.0448(13) 0.0682(16) 0.0096(11) 0.0342(13) 0.0100(11) O53 0.0652(15) 0.0477(13) 0.0536(14) -0.0107(11) -0.0087(11) 0.0139(11) O11 0.0425(11) 0.0352(11) 0.0420(12) -0.0030(9) 0.0104(9) 0.0008(9) O26 0.0433(11) 0.0329(11) 0.0506(13) 0.0040(9) 0.0041(10) 0.0031(9) N38 0.0441(15) 0.0385(14) 0.075(2) 0.0081(13) 0.0117(14) -0.0021(12) N19 0.0501(16) 0.0346(14) 0.0479(16) 0.0013(11) 0.0125(13) -0.0065(11) N23 0.0499(16) 0.0449(15) 0.0507(16) -0.0091(12) 0.0067(13) -0.0050(12) N34 0.0439(15) 0.0388(14) 0.0502(16) -0.0029(12) -0.0057(12) -0.0024(11) C44 0.0346(16) 0.0434(17) 0.0390(17) -0.0070(13) 0.0049(13) -0.0004(13) C54 0.0329(16) 0.0357(16) 0.0441(18) 0.0073(13) 0.0081(13) -0.0026(12) C55 0.0409(18) 0.0479(19) 0.055(2) 0.0079(15) 0.0008(15) -0.0015(14) C59 0.0502(19) 0.0426(18) 0.052(2) 0.0061(15) 0.0076(15) 0.0051(15) C42 0.0403(17) 0.0377(17) 0.0481(19) -0.0031(14) 0.0080(15) 0.0009(13) C49 0.053(2) 0.0454(19) 0.058(2) -0.0038(16) 0.0198(16) 0.0038(15) C45 0.059(2) 0.064(2) 0.043(2) -0.0009(16) 0.0119(16) 0.0100(17) C12 0.0355(16) 0.0481(18) 0.0430(19) -0.0095(14) 0.0074(14) -0.0055(13) C52 0.0361(16) 0.0352(16) 0.0472(19) 0.0064(14) 0.0074(15) -0.0029(13) C18 0.060(2) 0.049(2) 0.048(2) 0.0061(17) 0.0133(17) -0.0118(16) C28 0.052(2) 0.0452(19) 0.087(3) 0.0180(19) 0.0060(19) 0.0064(16) C32 0.0481(19) 0.050(2) 0.052(2) 0.0088(16) -0.0064(16) -0.0051(15) C13 0.059(2) 0.053(2) 0.057(2) -0.0147(17) 0.0184(18) -0.0048(16) C36 0.059(2) 0.0371(18) 0.104(3) -0.004(2) -0.014(2) -0.0084(16) C17 0.057(2) 0.054(2) 0.0391(18) -0.0045(15) 0.0145(15) -0.0138(16) C27 0.0330(16) 0.0426(18) 0.061(2) 0.0119(16) 0.0017(15) -0.0028(13) C20 0.069(2) 0.0347(17) 0.066(2) 0.0095(16) 0.0209(19) -0.0048(16) C29 0.067(3) 0.058(2) 0.108(4) 0.039(3) 0.000(2) 0.009(2) C56 0.048(2) 0.064(2) 0.074(3) 0.025(2) 0.0009(18) 0.0077(18) C47 0.059(2) 0.061(2) 0.080(3) -0.028(2) 0.016(2) 0.0072(18) C33 0.058(2) 0.055(2) 0.052(2) -0.0053(19) -0.0071(18) -0.0061(17) C48 0.065(2) 0.042(2) 0.088(3) -0.0053(18) 0.023(2) 0.0059(17) C31 0.082(3) 0.079(3) 0.061(3) 0.017(2) -0.013(2) -0.010(2) C57 0.056(2) 0.056(2) 0.093(3) 0.025(2) 0.019(2) 0.0211(18) C46 0.070(3) 0.083(3) 0.055(2) -0.016(2) 0.0251(19) 0.013(2) C58 0.072(2) 0.0438(19) 0.076(3) 0.0001(18) 0.018(2) 0.0102(18) C35 0.065(2) 0.0408(18) 0.065(2) -0.0137(16) -0.0107(18) 0.0024(16) C21 0.091(3) 0.040(2) 0.091(3) -0.008(2) 0.014(2) -0.0209(19) C39 0.040(2) 0.061(2) 0.130(4) 0.016(2) 0.019(2) 0.0024(17) C22 0.082(3) 0.058(2) 0.085(3) -0.015(2) 0.000(2) -0.026(2) C40 0.085(3) 0.073(3) 0.082(3) 0.012(2) 0.037(2) -0.023(2) C14 0.096(3) 0.071(3) 0.076(3) -0.035(2) 0.038(2) -0.011(2) C16 0.111(3) 0.074(3) 0.056(2) -0.010(2) 0.032(2) -0.026(2) C37 0.055(2) 0.0414(19) 0.097(3) 0.0130(19) 0.005(2) -0.0124(16) C24 0.090(3) 0.108(3) 0.054(2) 0.000(2) -0.014(2) -0.033(3) C25 0.042(2) 0.103(3) 0.112(3) -0.044(3) 0.003(2) 0.000(2) C30 0.087(3) 0.084(3) 0.084(3) 0.041(3) -0.016(3) -0.001(2) C15 0.135(4) 0.094(3) 0.067(3) -0.032(3) 0.057(3) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N19 2.003(2) . ? Ni1 O11 2.0109(19) . ? Ni1 O41 2.0328(19) . ? Ni1 O3 2.0961(18) . ? Ni1 N23 2.161(2) . ? Ni1 O26 2.175(2) . ? Ni1 Ni2 2.8624(6) . ? Ni2 N34 1.998(2) . ? Ni2 O26 2.0170(18) . ? Ni2 O51 2.0588(19) . ? Ni2 O3 2.1078(19) . ? Ni2 N38 2.146(3) . ? Ni2 O11 2.1624(19) . ? O3 H3A 0.9700 . ? O3 H3B 0.9700 . ? O51 C52 1.266(3) . ? O41 C42 1.263(3) . ? O43 C42 1.256(3) . ? O53 C52 1.247(3) . ? O11 C12 1.313(3) . ? O26 C27 1.321(3) . ? N38 C40 1.479(4) . ? N38 C39 1.480(4) . ? N38 C37 1.491(4) . ? N19 C18 1.280(4) . ? N19 C20 1.463(4) . ? N23 C25 1.461(4) . ? N23 C24 1.477(4) . ? N23 C22 1.492(4) . ? N34 C33 1.278(4) . ? N34 C35 1.468(4) . ? C44 C45 1.384(4) . ? C44 C49 1.387(4) . ? C44 C42 1.502(4) . ? C54 C55 1.383(4) . ? C54 C59 1.385(4) . ? C54 C52 1.504(4) . ? C55 C56 1.381(4) . ? C55 H55 0.9300 . ? C59 C58 1.387(4) . ? C59 H59 0.9300 . ? C49 C48 1.376(4) . ? C49 H49 0.9300 . ? C45 C46 1.383(4) . ? C45 H45 0.9300 . ? C12 C13 1.408(4) . ? C12 C17 1.419(4) . ? C18 C17 1.440(4) . ? C18 H18 0.96(3) . ? C28 C29 1.377(5) . ? C28 C27 1.413(4) . ? C28 H28 0.9300 . ? C32 C31 1.408(5) . ? C32 C27 1.414(4) . ? C32 C33 1.444(5) . ? C13 C14 1.364(5) . ? C13 H13 0.9300 . ? C36 C37 1.514(5) . ? C36 C35 1.517(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C17 C16 1.406(5) . ? C20 C21 1.513(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C29 C30 1.373(6) . ? C29 H29 0.9300 . ? C56 C57 1.368(5) . ? C56 H56 0.9300 . ? C47 C46 1.371(5) . ? C47 C48 1.371(5) . ? C47 H47 0.9300 . ? C33 H33 0.97(4) . ? C48 H48 0.9300 . ? C31 C30 1.367(6) . ? C31 H31 0.9300 . ? C57 C58 1.378(5) . ? C57 H57 0.9300 . ? C46 H46 0.9300 . ? C58 H58 0.9300 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C21 C22 1.478(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C16 C15 1.364(5) . ? C16 H16 0.9300 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C30 H30 0.9300 . ? C15 H15 0.9300 . ? 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 N19 Ni1 O11 91.47(9) . . ? N19 Ni1 O41 96.18(9) . . ? O11 Ni1 O41 167.51(8) . . ? N19 Ni1 O3 171.29(9) . . ? O11 Ni1 O3 80.21(8) . . ? O41 Ni1 O3 91.59(8) . . ? N19 Ni1 N23 85.71(10) . . ? O11 Ni1 N23 100.62(9) . . ? O41 Ni1 N23 89.82(9) . . ? O3 Ni1 N23 98.27(9) . . ? N19 Ni1 O26 99.53(9) . . ? O11 Ni1 O26 78.96(7) . . ? O41 Ni1 O26 90.02(8) . . ? O3 Ni1 O26 76.48(7) . . ? N23 Ni1 O26 174.74(9) . . ? N19 Ni1 Ni2 124.72(7) . . ? O11 Ni1 Ni2 48.94(5) . . ? O41 Ni1 Ni2 118.71(6) . . ? O3 Ni1 Ni2 47.26(5) . . ? N23 Ni1 Ni2 131.49(7) . . ? O26 Ni1 Ni2 44.67(5) . . ? N34 Ni2 O26 91.52(9) . . ? N34 Ni2 O51 95.77(9) . . ? O26 Ni2 O51 167.76(8) . . ? N34 Ni2 O3 170.37(9) . . ? O26 Ni2 O3 79.71(7) . . ? O51 Ni2 O3 92.23(7) . . ? N34 Ni2 N38 87.48(11) . . ? O26 Ni2 N38 99.52(9) . . ? O51 Ni2 N38 90.64(9) . . ? O3 Ni2 N38 97.81(9) . . ? N34 Ni2 O11 97.99(9) . . ? O26 Ni2 O11 79.13(7) . . ? O51 Ni2 O11 90.10(7) . . ? O3 Ni2 O11 76.59(7) . . ? N38 Ni2 O11 174.38(9) . . ? N34 Ni2 Ni1 123.86(7) . . ? O26 Ni2 Ni1 49.29(6) . . ? O51 Ni2 Ni1 118.59(6) . . ? O3 Ni2 Ni1 46.92(5) . . ? N38 Ni2 Ni1 130.80(7) . . ? O11 Ni2 Ni1 44.53(5) . . ? Ni1 O3 Ni2 85.82(7) . . ? Ni1 O3 H3A 114.3 . . ? Ni2 O3 H3A 114.3 . . ? Ni1 O3 H3B 114.3 . . ? Ni2 O3 H3B 114.3 . . ? H3A O3 H3B 111.5 . . ? C52 O51 Ni2 127.42(18) . . ? C42 O41 Ni1 129.33(19) . . ? C12 O11 Ni1 127.97(18) . . ? C12 O11 Ni2 123.56(17) . . ? Ni1 O11 Ni2 86.53(7) . . ? C27 O26 Ni2 126.13(19) . . ? C27 O26 Ni1 117.96(17) . . ? Ni2 O26 Ni1 86.04(7) . . ? C40 N38 C39 108.5(3) . . ? C40 N38 C37 106.9(3) . . ? C39 N38 C37 110.3(3) . . ? C40 N38 Ni2 110.0(2) . . ? C39 N38 Ni2 109.4(2) . . ? C37 N38 Ni2 111.6(2) . . ? C18 N19 C20 117.5(3) . . ? C18 N19 Ni1 124.9(2) . . ? C20 N19 Ni1 116.0(2) . . ? C25 N23 C24 109.2(3) . . ? C25 N23 C22 111.4(3) . . ? C24 N23 C22 105.3(3) . . ? C25 N23 Ni1 110.1(2) . . ? C24 N23 Ni1 109.1(2) . . ? C22 N23 Ni1 111.6(2) . . ? C33 N34 C35 118.3(3) . . ? C33 N34 Ni2 124.6(2) . . ? C35 N34 Ni2 116.6(2) . . ? C45 C44 C49 118.0(3) . . ? C45 C44 C42 121.2(3) . . ? C49 C44 C42 120.8(3) . . ? C55 C54 C59 118.8(3) . . ? C55 C54 C52 120.0(3) . . ? C59 C54 C52 121.2(3) . . ? C54 C55 C56 121.1(3) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C54 C59 C58 120.1(3) . . ? C54 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? O43 C42 O41 125.9(3) . . ? O43 C42 C44 117.9(3) . . ? O41 C42 C44 116.2(3) . . ? C48 C49 C44 120.9(3) . . ? C48 C49 H49 119.6 . . ? C44 C49 H49 119.6 . . ? C44 C45 C46 120.9(3) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? O11 C12 C13 119.8(3) . . ? O11 C12 C17 123.0(3) . . ? C13 C12 C17 117.2(3) . . ? O53 C52 O51 125.6(3) . . ? O53 C52 C54 117.7(3) . . ? O51 C52 C54 116.7(3) . . ? N19 C18 C17 127.7(3) . . ? N19 C18 H18 118.0(19) . . ? C17 C18 H18 114.3(19) . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C31 C32 C27 119.7(3) . . ? C31 C32 C33 116.5(3) . . ? C27 C32 C33 123.6(3) . . ? C14 C13 C12 121.8(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C37 C36 C35 115.6(3) . . ? C37 C36 H36A 108.4 . . ? C35 C36 H36A 108.4 . . ? C37 C36 H36B 108.4 . . ? C35 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C16 C17 C12 119.0(3) . . ? C16 C17 C18 116.5(3) . . ? C12 C17 C18 124.5(3) . . ? O26 C27 C28 118.6(3) . . ? O26 C27 C32 124.1(3) . . ? C28 C27 C32 117.3(3) . . ? N19 C20 C21 108.5(3) . . ? N19 C20 H20A 110.0 . . ? C21 C20 H20A 110.0 . . ? N19 C20 H20B 110.0 . . ? C21 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? C30 C29 C28 121.6(4) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C57 C56 C55 119.8(3) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C46 C47 C48 119.6(3) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? N34 C33 C32 127.7(3) . . ? N34 C33 H33 115(2) . . ? C32 C33 H33 117(2) . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C30 C31 C32 121.3(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C56 C57 C58 120.2(3) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C47 C46 C45 120.1(3) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C57 C58 C59 120.1(3) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? N34 C35 C36 108.7(3) . . ? N34 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? N34 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C22 C21 C20 118.1(3) . . ? C22 C21 H21A 107.8 . . ? C20 C21 H21A 107.8 . . ? C22 C21 H21B 107.8 . . ? C20 C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? N38 C39 H39A 109.5 . . ? N38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C21 C22 N23 118.2(3) . . ? C21 C22 H22A 107.8 . . ? N23 C22 H22A 107.8 . . ? C21 C22 H22B 107.8 . . ? N23 C22 H22B 107.8 . . ? H22A C22 H22B 107.1 . . ? N38 C40 H40A 109.5 . . ? N38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C13 C14 C15 121.1(4) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C15 C16 C17 122.1(4) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? N38 C37 C36 116.2(3) . . ? N38 C37 H37A 108.2 . . ? C36 C37 H37A 108.2 . . ? N38 C37 H37B 108.2 . . ? C36 C37 H37B 108.2 . . ? H37A C37 H37B 107.4 . . ? N23 C24 H24A 109.5 . . ? N23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N23 C25 H25A 109.5 . . ? N23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C30 C29 119.2(4) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.443 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.050 data_2 _database_code_depnum_ccdc_archive 'CCDC 800754' #TrackingRef '1-2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H50 N4 Ni2 O7' _chemical_formula_weight 816.26 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' N N 0.0061 0.0033 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.351(3) _cell_length_b 18.545(5) _cell_length_c 22.502(6) _cell_angle_alpha 68.265(7) _cell_angle_beta 87.141(8) _cell_angle_gamma 83.820(7) _cell_volume 3989.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 43562 _cell_measurement_theta_min 0.97 _cell_measurement_theta_max 26.40 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8333 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 43562 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 26.40 _reflns_number_total 15762 _reflns_number_gt 11199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1331P)^2^+3.1168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15762 _refine_ls_number_parameters 971 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.2177 _refine_ls_wR_factor_gt 0.1972 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.005 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1A Ni -0.09604(6) 0.29773(3) 0.05686(3) 0.04015(17) Uani 1 1 d . . . Ni1B Ni 0.37256(6) 0.33478(3) 0.46302(3) 0.03934(17) Uani 1 1 d . . . Ni2B Ni 0.56110(5) 0.22124(3) 0.54549(3) 0.03832(16) Uani 1 1 d . . . Ni2A Ni 0.09177(6) 0.25660(4) -0.02605(3) 0.04197(17) Uani 1 1 d . . . O11B O 0.3467(3) 0.23675(18) 0.53985(14) 0.0418(7) Uani 1 1 d . . . O3B O 0.5131(3) 0.33889(18) 0.52600(15) 0.0424(7) Uani 1 1 d . . . H3B1 H 0.5819 0.3714 0.5051 0.051 Uiso 1 1 calc R . . H3B2 H 0.4771 0.3508 0.5623 0.051 Uiso 1 1 calc R . . O26A O 0.0602(3) 0.20665(19) 0.06879(15) 0.0459(8) Uani 1 1 d . . . O11A O -0.1220(3) 0.27183(19) -0.02083(15) 0.0456(8) Uani 1 1 d . . . O3A O 0.0497(3) 0.35651(19) -0.00424(16) 0.0483(8) Uani 1 1 d . . . H3A1 H 0.0175 0.4023 -0.0400 0.058 Uiso 1 1 calc R . . H3A2 H 0.1190 0.3678 0.0175 0.058 Uiso 1 1 calc R . . O26B O 0.5344(3) 0.25780(18) 0.45081(15) 0.0435(7) Uani 1 1 d . . . O41B O 0.4476(4) 0.4212(2) 0.38683(17) 0.0537(9) Uani 1 1 d . . . N34A N 0.1184(4) 0.1507(2) -0.03275(18) 0.0433(9) Uani 1 1 d . . . O41A O -0.0249(3) 0.3170(2) 0.13097(16) 0.0533(9) Uani 1 1 d . . . N34B N 0.6002(4) 0.1114(2) 0.55003(19) 0.0422(9) Uani 1 1 d . . . O51A O 0.0853(4) 0.3192(2) -0.12050(17) 0.0590(9) Uani 1 1 d . . . O51B O 0.5488(4) 0.1959(2) 0.64062(16) 0.0510(8) Uani 1 1 d . . . O53A O 0.0313(5) 0.4393(3) -0.1219(2) 0.0836(14) Uani 1 1 d . . . N38A N 0.2998(4) 0.2565(3) -0.0299(2) 0.0545(11) Uani 1 1 d . . . O53B O 0.4913(5) 0.3119(2) 0.6470(2) 0.0748(12) Uani 1 1 d . . . N19B N 0.2401(4) 0.3101(2) 0.41332(19) 0.0474(9) Uani 1 1 d . . . N19A N -0.2318(4) 0.2284(2) 0.1054(2) 0.0471(10) Uani 1 1 d . . . O43A O 0.1655(4) 0.3626(3) 0.0921(2) 0.0730(12) Uani 1 1 d . . . N23A N -0.2419(5) 0.3931(3) 0.0462(2) 0.0574(11) Uani 1 1 d . . . O43B O 0.6326(5) 0.4275(3) 0.4313(2) 0.0792(13) Uani 1 1 d . . . N23B N 0.2274(4) 0.4173(3) 0.4779(2) 0.0545(11) Uani 1 1 d . . . N38B N 0.7687(4) 0.2237(3) 0.5501(2) 0.0514(10) Uani 1 1 d . . . C18A C -0.2833(5) 0.1812(3) 0.0871(3) 0.0491(12) Uani 1 1 d . . . C32A C 0.0521(5) 0.0751(3) 0.0766(3) 0.0485(11) Uani 1 1 d . . . C12A C -0.1867(5) 0.2167(3) -0.0246(2) 0.0476(12) Uani 1 1 d . . . C17A C -0.2611(5) 0.1697(3) 0.0274(3) 0.0495(12) Uani 1 1 d . . . C12B C 0.2828(4) 0.1784(3) 0.5415(2) 0.0423(10) Uani 1 1 d . . . C13B C 0.2825(5) 0.1132(3) 0.5986(3) 0.0580(14) Uani 1 1 d . . . H13B H 0.3263 0.1125 0.6339 0.070 Uiso 1 1 calc R . . C32B C 0.5518(5) 0.1339(3) 0.4389(2) 0.0470(11) Uani 1 1 d . . . C55B C 0.5233(6) 0.1138(3) 0.7683(2) 0.0576(14) Uani 1 1 d . . . C27B C 0.5238(4) 0.2150(3) 0.4161(2) 0.0441(11) Uani 1 1 d . . . C17B C 0.2132(5) 0.1785(3) 0.4890(3) 0.0473(11) Uani 1 1 d . . . C28A C 0.0053(5) 0.1123(3) 0.1664(3) 0.0548(13) Uani 1 1 d . . . H28A H 0.0007 0.1498 0.1850 0.066 Uiso 1 1 calc R . . C28B C 0.4881(5) 0.2520(3) 0.3513(2) 0.0555(13) Uani 1 1 d . . . H28B H 0.4728 0.3060 0.3340 0.067 Uiso 1 1 calc R . . C27A C 0.0400(4) 0.1335(3) 0.1022(2) 0.0427(10) Uani 1 1 d . . . C45A C 0.0386(6) 0.2829(4) 0.2543(3) 0.0657(16) Uani 1 1 d . . . C33A C 0.0963(5) 0.0865(3) 0.0120(3) 0.0529(13) Uani 1 1 d . . . C33B C 0.5943(5) 0.0872(3) 0.5048(3) 0.0504(12) Uani 1 1 d . . . C15B C 0.1527(6) 0.0488(3) 0.5508(4) 0.0747(19) Uani 1 1 d . . . H15B H 0.1115 0.0054 0.5537 0.090 Uiso 1 1 calc R . . C42A C 0.0845(6) 0.3390(3) 0.1359(3) 0.0578(14) Uani 1 1 d . . . C13A C -0.1841(6) 0.2031(4) -0.0819(3) 0.0629(15) Uani 1 1 d . . . H13A H -0.1384 0.2340 -0.1170 0.075 Uiso 1 1 calc R . . C16A C -0.3230(6) 0.1090(3) 0.0199(4) 0.0686(17) Uani 1 1 d . . . H16A H -0.3684 0.0763 0.0542 0.082 Uiso 1 1 calc R . . C15A C -0.3170(7) 0.0977(4) -0.0374(4) 0.082(2) Uani 1 1 d . . . H15A H -0.3595 0.0584 -0.0421 0.098 Uiso 1 1 calc R . . C35A C 0.1875(6) 0.1465(4) -0.0900(3) 0.0611(14) Uani 1 1 d . . . H35A H 0.1516 0.1878 -0.1280 0.073 Uiso 1 1 calc R . . H35B H 0.1790 0.0968 -0.0937 0.073 Uiso 1 1 calc R . . C35B C 0.6665(6) 0.0571(3) 0.6085(3) 0.0591(14) Uani 1 1 d . . . H35C H 0.6625 0.0037 0.6117 0.071 Uiso 1 1 calc R . . H35D H 0.6237 0.0632 0.6459 0.071 Uiso 1 1 calc R . . C31B C 0.5413(6) 0.0920(4) 0.3993(3) 0.0645(15) Uani 1 1 d . . . H31B H 0.5593 0.0381 0.4155 0.077 Uiso 1 1 calc R . . C36A C 0.3291(6) 0.1556(4) -0.0833(3) 0.0735(17) Uani 1 1 d . . . H36A H 0.3608 0.1154 -0.0437 0.088 Uiso 1 1 calc R . . H36B H 0.3777 0.1460 -0.1181 0.088 Uiso 1 1 calc R . . C16B C 0.1500(5) 0.1116(3) 0.4957(3) 0.0653(16) Uani 1 1 d . . . H16B H 0.1054 0.1110 0.4610 0.078 Uiso 1 1 calc R . . C20B C 0.1880(6) 0.3749(4) 0.3570(3) 0.0644(15) Uani 1 1 d . . . H20A H 0.1392 0.3555 0.3313 0.077 Uiso 1 1 calc R . . H20B H 0.2584 0.4017 0.3310 0.077 Uiso 1 1 calc R . . C18B C 0.1912(5) 0.2446(3) 0.4301(3) 0.0514(12) Uani 1 1 d . . . C30B C 0.5041(6) 0.1303(4) 0.3361(3) 0.0719(17) Uani 1 1 d . . . H30B H 0.4986 0.1025 0.3095 0.086 Uiso 1 1 calc R . . C21A C -0.3682(6) 0.3165(4) 0.1447(3) 0.0726(18) Uani 1 1 d . . . H21A H -0.4067 0.3214 0.1834 0.087 Uiso 1 1 calc R . . H21B H -0.4385 0.3144 0.1186 0.087 Uiso 1 1 calc R . . C42B C 0.5619(6) 0.4397(3) 0.3849(3) 0.0616(15) Uani 1 1 d . . . C36B C 0.8069(6) 0.0742(4) 0.6057(4) 0.0719(17) Uani 1 1 d . . . H36C H 0.8475 0.0684 0.5677 0.086 Uiso 1 1 calc R . . H36D H 0.8514 0.0356 0.6426 0.086 Uiso 1 1 calc R . . C31A C 0.0239(6) -0.0008(3) 0.1156(3) 0.0619(14) Uani 1 1 d . . . H31A H 0.0304 -0.0392 0.0980 0.074 Uiso 1 1 calc R . . C52B C 0.5169(5) 0.2402(3) 0.6709(3) 0.0532(12) Uani 1 1 d . . . C37A C 0.3592(6) 0.2333(4) -0.0833(3) 0.0685(16) Uani 1 1 d . . . H37A H 0.3304 0.2732 -0.1236 0.082 Uiso 1 1 calc R . . H37B H 0.4528 0.2328 -0.0818 0.082 Uiso 1 1 calc R . . C29B C 0.4755(6) 0.2102(4) 0.3132(3) 0.0638(15) Uani 1 1 d . . . H29B H 0.4473 0.2360 0.2713 0.077 Uiso 1 1 calc R . . C55A C 0.0464(7) 0.3632(4) -0.2505(3) 0.0755(19) Uani 1 1 d . . . C54B C 0.5162(7) 0.2019(4) 0.7436(3) 0.0731(18) Uani 1 1 d . . . H54A H 0.5894 0.2171 0.7600 0.088 Uiso 1 1 calc R . . H54B H 0.4375 0.2215 0.7602 0.088 Uiso 1 1 calc R . . C14B C 0.2174(6) 0.0495(3) 0.6030(3) 0.0712(18) Uani 1 1 d . . . H14B H 0.2172 0.0070 0.6415 0.085 Uiso 1 1 calc R . . C14A C -0.2485(7) 0.1444(5) -0.0867(4) 0.082(2) Uani 1 1 d . . . H14A H -0.2447 0.1366 -0.1252 0.098 Uiso 1 1 calc R . . C20A C -0.2825(6) 0.2403(3) 0.1630(3) 0.0636(15) Uani 1 1 d . . . H20C H -0.2111 0.2414 0.1889 0.076 Uiso 1 1 calc R . . H20D H -0.3324 0.1975 0.1881 0.076 Uiso 1 1 calc R . . C45B C 0.5279(7) 0.5147(3) 0.2651(3) 0.0674(17) Uani 1 1 d . . . C29A C -0.0223(6) 0.0381(4) 0.2034(3) 0.0670(16) Uani 1 1 d . . . H29A H -0.0477 0.0268 0.2459 0.080 Uiso 1 1 calc R . . C57B C 0.4208(7) -0.0033(4) 0.7888(4) 0.086(2) Uani 1 1 d . . . H57B H 0.3459 -0.0273 0.7900 0.103 Uiso 1 1 calc R . . C21B C 0.0996(7) 0.4305(4) 0.3803(3) 0.0785(19) Uani 1 1 d . . . H21C H 0.0576 0.4707 0.3434 0.094 Uiso 1 1 calc R . . H21D H 0.0321 0.4018 0.4073 0.094 Uiso 1 1 calc R . . C22B C 0.1654(7) 0.4694(4) 0.4168(3) 0.0735(17) Uani 1 1 d . . . H22A H 0.2314 0.4990 0.3892 0.088 Uiso 1 1 calc R . . H22B H 0.1015 0.5062 0.4259 0.088 Uiso 1 1 calc R . . C56B C 0.4129(6) 0.0764(4) 0.7719(3) 0.0729(18) Uani 1 1 d . . . H56B H 0.3324 0.1054 0.7627 0.087 Uiso 1 1 calc R . . C37B C 0.8266(6) 0.1556(4) 0.6044(3) 0.0643(15) Uani 1 1 d . . . H37C H 0.7911 0.1597 0.6438 0.077 Uiso 1 1 calc R . . H37D H 0.9193 0.1595 0.6042 0.077 Uiso 1 1 calc R . . C40B C 0.7986(6) 0.2933(4) 0.5615(4) 0.0704(17) Uani 1 1 d . . . H40A H 0.7588 0.2930 0.6011 0.106 Uiso 1 1 calc R . . H40B H 0.7655 0.3393 0.5271 0.106 Uiso 1 1 calc R . . H40C H 0.8911 0.2928 0.5640 0.106 Uiso 1 1 calc R . . C22A C -0.3004(6) 0.3891(4) 0.1084(3) 0.0669(16) Uani 1 1 d . . . H22C H -0.3628 0.4344 0.1012 0.080 Uiso 1 1 calc R . . H22D H -0.2325 0.3924 0.1353 0.080 Uiso 1 1 calc R . . C60B C 0.6398(6) 0.0709(4) 0.7824(3) 0.0693(16) Uani 1 1 d . . . H60B H 0.7149 0.0955 0.7793 0.083 Uiso 1 1 calc R . . C44A C 0.1171(8) 0.3364(5) 0.2020(3) 0.094(3) Uani 1 1 d . . . H44A H 0.2087 0.3194 0.2100 0.113 Uiso 1 1 calc R . . H44B H 0.1017 0.3886 0.2027 0.113 Uiso 1 1 calc R . . C25B C 0.1303(6) 0.3755(4) 0.5242(3) 0.0790(19) Uani 1 1 d . . . H25A H 0.0903 0.3426 0.5076 0.119 Uiso 1 1 calc R . . H25B H 0.0651 0.4125 0.5313 0.119 Uiso 1 1 calc R . . H25C H 0.1720 0.3442 0.5639 0.119 Uiso 1 1 calc R . . C40A C 0.3386(6) 0.3353(4) -0.0424(4) 0.088(2) Uani 1 1 d . . . H40D H 0.3040 0.3708 -0.0826 0.132 Uiso 1 1 calc R . . H40E H 0.4317 0.3336 -0.0439 0.132 Uiso 1 1 calc R . . H40F H 0.3054 0.3526 -0.0088 0.132 Uiso 1 1 calc R . . C25A C -0.3426(7) 0.3943(5) 0.0019(4) 0.086(2) Uani 1 1 d . . . H25D H -0.3029 0.3966 -0.0381 0.129 Uiso 1 1 calc R . . H25E H -0.4039 0.4393 -0.0049 0.129 Uiso 1 1 calc R . . H25F H -0.3866 0.3479 0.0199 0.129 Uiso 1 1 calc R . . C39A C 0.3544(6) 0.2033(4) 0.0313(3) 0.0766(18) Uani 1 1 d . . . H39A H 0.3304 0.1517 0.0399 0.115 Uiso 1 1 calc R . . H39B H 0.3212 0.2207 0.0648 0.115 Uiso 1 1 calc R . . H39C H 0.4473 0.2025 0.0293 0.115 Uiso 1 1 calc R . . C39B C 0.8307(6) 0.2256(4) 0.4895(3) 0.0754(18) Uani 1 1 d . . . H39D H 0.8128 0.1804 0.4813 0.113 Uiso 1 1 calc R . . H39E H 0.9229 0.2259 0.4921 0.113 Uiso 1 1 calc R . . H39F H 0.7969 0.2718 0.4553 0.113 Uiso 1 1 calc R . . C58B C 0.5366(8) -0.0473(4) 0.8040(4) 0.088(2) Uani 1 1 d . . . H58B H 0.5421 -0.1012 0.8157 0.105 Uiso 1 1 calc R . . C24B C 0.2855(8) 0.4674(4) 0.5052(4) 0.085(2) Uani 1 1 d . . . H24A H 0.3497 0.4955 0.4760 0.127 Uiso 1 1 calc R . . H24B H 0.3257 0.4356 0.5452 0.127 Uiso 1 1 calc R . . H24C H 0.2188 0.5037 0.5122 0.127 Uiso 1 1 calc R . . C44B C 0.6210(8) 0.4808(5) 0.3199(4) 0.093(2) Uani 1 1 d . . . H44C H 0.6670 0.5226 0.3221 0.112 Uiso 1 1 calc R . . H44D H 0.6848 0.4441 0.3104 0.112 Uiso 1 1 calc R . . C48A C -0.1203(10) 0.1857(6) 0.3433(4) 0.101(3) Uani 1 1 d . . . H48A H -0.1754 0.1533 0.3726 0.122 Uiso 1 1 calc R . . C59B C 0.6476(7) -0.0091(4) 0.8013(4) 0.083(2) Uani 1 1 d . . . H59B H 0.7276 -0.0382 0.8125 0.100 Uiso 1 1 calc R . . C56A C 0.1583(8) 0.3328(5) -0.2718(4) 0.091(2) Uani 1 1 d . . . H56A H 0.2369 0.3508 -0.2683 0.109 Uiso 1 1 calc R . . C46A C 0.0750(8) 0.2034(6) 0.2823(4) 0.091(2) Uani 1 1 d . . . H46A H 0.1543 0.1824 0.2716 0.109 Uiso 1 1 calc R . . C24A C -0.1795(8) 0.4683(4) 0.0193(4) 0.096(3) Uani 1 1 d . . . H24D H -0.1133 0.4680 0.0478 0.143 Uiso 1 1 calc R . . H24E H -0.2441 0.5112 0.0146 0.143 Uiso 1 1 calc R . . H24F H -0.1413 0.4737 -0.0217 0.143 Uiso 1 1 calc R . . C30A C -0.0129(6) -0.0201(4) 0.1787(3) 0.0730(18) Uani 1 1 d . . . H30A H -0.0308 -0.0705 0.2038 0.088 Uiso 1 1 calc R . . C49A C -0.1547(8) 0.2627(6) 0.3183(4) 0.095(2) Uani 1 1 d . . . H49A H -0.2312 0.2838 0.3315 0.114 Uiso 1 1 calc R . . C46B C 0.4812(8) 0.5926(4) 0.2491(4) 0.084(2) Uani 1 1 d . . . H46B H 0.5088 0.6211 0.2716 0.101 Uiso 1 1 calc R . . C60A C -0.0624(9) 0.3309(8) -0.2548(4) 0.130(4) Uani 1 1 d . . . H60A H -0.1403 0.3474 -0.2392 0.156 Uiso 1 1 calc R . . C50A C -0.0765(7) 0.3099(5) 0.2733(3) 0.084(2) Uani 1 1 d . . . H50A H -0.1035 0.3628 0.2548 0.101 Uiso 1 1 calc R . . C47A C -0.0080(10) 0.1550(5) 0.3268(4) 0.098(3) Uani 1 1 d . . . H47A H 0.0150 0.1015 0.3448 0.117 Uiso 1 1 calc R . . C54A C 0.0461(11) 0.4221(5) -0.2207(3) 0.112(3) Uani 1 1 d . . . H54C H -0.0330 0.4569 -0.2331 0.134 Uiso 1 1 calc R . . H54D H 0.1185 0.4529 -0.2385 0.134 Uiso 1 1 calc R . . C47B C 0.3973(9) 0.6265(6) 0.2016(5) 0.103(3) Uani 1 1 d . . . H47B H 0.3681 0.6789 0.1909 0.123 Uiso 1 1 calc R . . C52A C 0.0551(6) 0.3914(4) -0.1480(3) 0.0664(16) Uani 1 1 d . . . C57A C 0.1577(10) 0.2768(6) -0.2978(4) 0.105(3) Uani 1 1 d . . . H57A H 0.2350 0.2591 -0.3131 0.126 Uiso 1 1 calc R . . C49B C 0.3951(13) 0.5107(7) 0.1808(4) 0.134(4) Uani 1 1 d . . . H49B H 0.3626 0.4839 0.1580 0.161 Uiso 1 1 calc R . . C48B C 0.3546(11) 0.5872(6) 0.1693(4) 0.114(3) Uani 1 1 d . . . H48B H 0.2941 0.6128 0.1373 0.136 Uiso 1 1 calc R . . C59A C -0.0626(12) 0.2745(9) -0.2812(5) 0.156(6) Uani 1 1 d . . . H59A H -0.1399 0.2554 -0.2850 0.188 Uiso 1 1 calc R . . C50B C 0.4911(10) 0.4735(5) 0.2301(4) 0.106(3) Uani 1 1 d . . . H50B H 0.5272 0.4227 0.2380 0.127 Uiso 1 1 calc R . . C58A C 0.0498(14) 0.2477(7) -0.3015(4) 0.125(4) Uani 1 1 d . . . H58A H 0.0512 0.2085 -0.3181 0.150 Uiso 1 1 calc R . . H33B H 0.620(4) 0.033(3) 0.516(2) 0.032(11) Uiso 1 1 d . . . H18B H 0.137(5) 0.233(3) 0.405(3) 0.051(14) Uiso 1 1 d . . . H33A H 0.119(5) 0.040(3) 0.008(3) 0.058(16) Uiso 1 1 d . . . H18A H -0.343(5) 0.146(3) 0.114(3) 0.054(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1A 0.0456(3) 0.0393(3) 0.0374(3) -0.0148(3) 0.0025(2) -0.0108(2) Ni1B 0.0447(3) 0.0350(3) 0.0380(3) -0.0118(2) -0.0029(2) -0.0074(2) Ni2B 0.0399(3) 0.0377(3) 0.0387(3) -0.0148(2) -0.0015(2) -0.0065(2) Ni2A 0.0447(3) 0.0434(4) 0.0366(3) -0.0128(3) 0.0017(2) -0.0069(3) O11B 0.0443(17) 0.0397(17) 0.0372(16) -0.0084(14) -0.0019(13) -0.0077(14) O3B 0.0517(19) 0.0395(17) 0.0361(16) -0.0125(14) -0.0048(14) -0.0087(14) O26A 0.0524(19) 0.0430(19) 0.0413(18) -0.0135(15) 0.0012(14) -0.0086(15) O11A 0.0507(19) 0.0473(19) 0.0384(17) -0.0150(15) -0.0029(14) -0.0056(15) O3A 0.053(2) 0.0396(18) 0.0480(19) -0.0097(15) 0.0041(15) -0.0126(15) O26B 0.0474(18) 0.0406(18) 0.0444(18) -0.0166(15) 0.0015(14) -0.0092(14) O41B 0.061(2) 0.046(2) 0.048(2) -0.0075(16) 0.0032(16) -0.0153(17) N34A 0.044(2) 0.046(2) 0.037(2) -0.0133(18) -0.0047(16) -0.0015(17) O41A 0.060(2) 0.064(2) 0.0463(19) -0.0287(17) 0.0031(16) -0.0214(18) N34B 0.038(2) 0.041(2) 0.049(2) -0.0165(18) -0.0045(17) -0.0036(16) O51A 0.070(2) 0.056(2) 0.0415(19) -0.0076(17) 0.0077(17) -0.0048(18) O51B 0.064(2) 0.048(2) 0.0405(18) -0.0165(16) -0.0049(15) -0.0012(16) O53A 0.124(4) 0.060(3) 0.052(2) -0.004(2) 0.000(2) -0.006(3) N38A 0.049(2) 0.055(3) 0.058(3) -0.020(2) 0.001(2) -0.004(2) O53B 0.124(4) 0.048(2) 0.055(2) -0.0236(19) 0.001(2) -0.002(2) N19B 0.050(2) 0.050(2) 0.045(2) -0.0189(19) -0.0069(18) -0.0077(19) N19A 0.047(2) 0.050(2) 0.046(2) -0.0176(19) 0.0062(18) -0.0124(18) O43A 0.076(3) 0.087(3) 0.062(3) -0.027(2) 0.012(2) -0.045(2) N23A 0.065(3) 0.043(2) 0.064(3) -0.020(2) 0.008(2) -0.005(2) O43B 0.086(3) 0.079(3) 0.073(3) -0.018(2) -0.001(2) -0.049(2) N23B 0.062(3) 0.050(3) 0.054(3) -0.023(2) -0.006(2) 0.002(2) N38B 0.045(2) 0.060(3) 0.048(2) -0.017(2) -0.0071(18) -0.0082(19) C18A 0.043(3) 0.042(3) 0.061(3) -0.016(2) 0.001(2) -0.009(2) C32A 0.043(3) 0.040(3) 0.057(3) -0.011(2) -0.005(2) -0.003(2) C12A 0.048(3) 0.048(3) 0.050(3) -0.024(2) -0.017(2) 0.009(2) C17A 0.039(3) 0.045(3) 0.071(3) -0.028(3) -0.008(2) -0.002(2) C12B 0.035(2) 0.039(3) 0.048(3) -0.011(2) 0.0074(19) -0.0034(19) C13B 0.058(3) 0.046(3) 0.056(3) -0.002(2) 0.006(2) -0.007(2) C32B 0.048(3) 0.049(3) 0.050(3) -0.024(2) 0.008(2) -0.013(2) C55B 0.076(4) 0.060(3) 0.034(3) -0.015(2) 0.002(2) -0.005(3) C27B 0.039(2) 0.057(3) 0.045(3) -0.026(2) 0.011(2) -0.014(2) C17B 0.038(2) 0.045(3) 0.062(3) -0.023(2) 0.003(2) -0.006(2) C28A 0.056(3) 0.057(3) 0.048(3) -0.016(3) -0.002(2) -0.002(2) C28B 0.065(3) 0.062(3) 0.039(3) -0.018(2) 0.008(2) -0.014(3) C27A 0.034(2) 0.041(3) 0.047(3) -0.010(2) -0.0043(19) -0.0008(19) C45A 0.065(4) 0.094(5) 0.051(3) -0.035(3) -0.002(3) -0.029(3) C33A 0.051(3) 0.052(3) 0.063(3) -0.029(3) -0.006(2) -0.005(2) C33B 0.048(3) 0.042(3) 0.065(3) -0.024(3) 0.001(2) -0.006(2) C15B 0.062(4) 0.045(3) 0.113(6) -0.021(4) 0.005(4) -0.016(3) C42A 0.065(3) 0.057(3) 0.055(3) -0.020(3) 0.000(3) -0.024(3) C13A 0.067(4) 0.072(4) 0.057(3) -0.035(3) -0.019(3) 0.015(3) C16A 0.055(3) 0.054(3) 0.110(5) -0.043(4) -0.015(3) -0.002(3) C15A 0.070(4) 0.067(4) 0.134(7) -0.067(5) -0.029(4) 0.007(3) C35A 0.068(4) 0.069(4) 0.053(3) -0.031(3) 0.007(3) -0.005(3) C35B 0.068(4) 0.044(3) 0.064(3) -0.018(3) -0.010(3) 0.000(2) C31B 0.076(4) 0.060(4) 0.072(4) -0.040(3) 0.016(3) -0.019(3) C36A 0.071(4) 0.090(5) 0.068(4) -0.042(4) 0.018(3) -0.004(3) C16B 0.047(3) 0.053(3) 0.100(5) -0.030(3) -0.002(3) -0.012(2) C20B 0.077(4) 0.070(4) 0.041(3) -0.010(3) -0.021(3) -0.011(3) C18B 0.043(3) 0.057(3) 0.062(3) -0.029(3) -0.006(2) -0.007(2) C30B 0.084(4) 0.091(5) 0.062(4) -0.050(4) 0.006(3) -0.024(4) C21A 0.070(4) 0.081(4) 0.073(4) -0.037(3) 0.031(3) -0.018(3) C42B 0.082(4) 0.041(3) 0.060(4) -0.014(3) 0.008(3) -0.023(3) C36B 0.063(4) 0.059(4) 0.090(5) -0.024(3) -0.024(3) 0.012(3) C31A 0.063(3) 0.041(3) 0.077(4) -0.015(3) -0.003(3) -0.006(2) C52B 0.061(3) 0.057(3) 0.045(3) -0.022(3) -0.001(2) -0.010(3) C37A 0.058(3) 0.085(4) 0.063(4) -0.029(3) 0.016(3) -0.013(3) C29B 0.073(4) 0.081(4) 0.043(3) -0.026(3) 0.009(3) -0.022(3) C55A 0.089(5) 0.092(5) 0.030(3) -0.002(3) -0.009(3) -0.015(4) C54B 0.109(5) 0.064(4) 0.051(3) -0.027(3) 0.006(3) -0.007(3) C14B 0.063(4) 0.045(3) 0.088(5) -0.004(3) 0.020(3) -0.010(3) C14A 0.072(4) 0.096(5) 0.105(6) -0.074(5) -0.038(4) 0.021(4) C20A 0.069(4) 0.069(4) 0.055(3) -0.023(3) 0.024(3) -0.027(3) C45B 0.087(4) 0.056(4) 0.044(3) -0.004(3) 0.022(3) -0.008(3) C29A 0.067(4) 0.068(4) 0.045(3) 0.002(3) 0.008(3) -0.006(3) C57B 0.076(5) 0.070(5) 0.090(5) 0.003(4) -0.011(4) -0.026(4) C21B 0.086(5) 0.066(4) 0.069(4) -0.011(3) -0.036(3) 0.021(3) C22B 0.085(4) 0.056(4) 0.071(4) -0.019(3) -0.016(3) 0.018(3) C56B 0.056(4) 0.080(5) 0.060(4) 0.001(3) -0.002(3) -0.005(3) C37B 0.047(3) 0.072(4) 0.079(4) -0.032(3) -0.014(3) -0.007(3) C40B 0.048(3) 0.075(4) 0.101(5) -0.042(4) -0.011(3) -0.020(3) C22A 0.071(4) 0.061(4) 0.076(4) -0.036(3) 0.012(3) -0.004(3) C60B 0.066(4) 0.082(5) 0.052(3) -0.013(3) -0.005(3) -0.018(3) C44A 0.103(6) 0.129(7) 0.065(4) -0.039(4) 0.000(4) -0.067(5) C25B 0.067(4) 0.079(4) 0.082(5) -0.027(4) 0.020(3) 0.010(3) C40A 0.055(4) 0.091(5) 0.133(7) -0.054(5) 0.017(4) -0.033(3) C25A 0.086(5) 0.091(5) 0.083(5) -0.039(4) -0.021(4) 0.022(4) C39A 0.053(3) 0.111(5) 0.069(4) -0.039(4) -0.012(3) 0.004(3) C39B 0.047(3) 0.099(5) 0.080(4) -0.033(4) 0.019(3) -0.014(3) C58B 0.092(5) 0.069(4) 0.084(5) -0.006(4) 0.006(4) -0.012(4) C24B 0.104(5) 0.064(4) 0.104(6) -0.055(4) -0.019(4) 0.012(4) C44B 0.095(5) 0.093(5) 0.075(5) -0.008(4) 0.019(4) -0.033(4) C48A 0.127(8) 0.126(8) 0.070(5) -0.047(5) 0.018(5) -0.061(6) C59B 0.068(4) 0.082(5) 0.080(5) -0.010(4) -0.010(3) 0.004(4) C56A 0.073(5) 0.103(6) 0.085(5) -0.013(4) -0.013(4) -0.027(4) C46A 0.097(5) 0.129(7) 0.066(4) -0.057(5) -0.006(4) -0.009(5) C24A 0.114(6) 0.042(4) 0.120(6) -0.022(4) 0.042(5) -0.012(3) C30A 0.073(4) 0.047(3) 0.079(4) 0.000(3) 0.006(3) -0.013(3) C49A 0.089(5) 0.133(8) 0.071(5) -0.045(5) 0.014(4) -0.028(5) C46B 0.086(5) 0.071(5) 0.090(5) -0.025(4) 0.014(4) -0.006(4) C60A 0.077(5) 0.248(13) 0.071(5) -0.060(7) 0.020(4) -0.044(7) C50A 0.087(5) 0.111(6) 0.062(4) -0.034(4) -0.006(4) -0.022(4) C47A 0.145(8) 0.090(6) 0.063(4) -0.029(4) 0.000(5) -0.028(5) C54A 0.194(10) 0.075(5) 0.044(4) 0.000(3) -0.017(5) 0.005(5) C47B 0.092(6) 0.111(7) 0.105(7) -0.045(6) -0.010(5) 0.013(5) C52A 0.078(4) 0.061(4) 0.047(3) -0.005(3) 0.002(3) -0.012(3) C57A 0.103(7) 0.109(7) 0.096(6) -0.029(5) -0.017(5) 0.000(5) C49B 0.231(13) 0.127(9) 0.058(5) -0.042(5) 0.011(6) -0.055(8) C48B 0.154(9) 0.104(7) 0.083(6) -0.038(5) -0.026(6) 0.010(6) C59A 0.144(10) 0.272(16) 0.086(7) -0.076(9) 0.017(6) -0.130(11) C50B 0.170(9) 0.080(5) 0.062(5) -0.023(4) 0.015(5) -0.009(5) C58A 0.167(11) 0.145(9) 0.066(5) -0.033(5) -0.003(6) -0.052(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1A N19A 2.004(4) . ? Ni1A O11A 2.014(3) . ? Ni1A O41A 2.018(3) . ? Ni1A O3A 2.096(3) . ? Ni1A N23A 2.148(4) . ? Ni1A O26A 2.158(3) . ? Ni1A Ni2A 2.8662(10) . ? Ni1B N19B 2.002(4) . ? Ni1B O11B 2.024(3) . ? Ni1B O41B 2.052(3) . ? Ni1B O3B 2.107(3) . ? Ni1B N23B 2.132(4) . ? Ni1B O26B 2.157(3) . ? Ni1B Ni2B 2.8756(10) . ? Ni2B N34B 1.999(4) . ? Ni2B O26B 2.006(3) . ? Ni2B O51B 2.015(3) . ? Ni2B O3B 2.069(3) . ? Ni2B N38B 2.163(4) . ? Ni2B O11B 2.210(3) . ? Ni2A O51A 2.010(4) . ? Ni2A O26A 2.013(3) . ? Ni2A N34A 2.014(4) . ? Ni2A O3A 2.084(3) . ? Ni2A N38A 2.150(4) . ? Ni2A O11A 2.204(3) . ? O11B C12B 1.316(6) . ? O3B H3B1 0.9700 . ? O3B H3B2 0.9700 . ? O26A C27A 1.319(6) . ? O11A C12A 1.310(6) . ? O3A H3A1 0.9700 . ? O3A H3A2 0.9700 . ? O26B C27B 1.319(5) . ? O41B C42B 1.262(7) . ? N34A C33A 1.277(7) . ? N34A C35A 1.465(6) . ? O41A C42A 1.267(6) . ? N34B C33B 1.262(6) . ? N34B C35B 1.475(7) . ? O51A C52A 1.260(7) . ? O51B C52B 1.257(6) . ? O53A C52A 1.234(8) . ? N38A C39A 1.463(8) . ? N38A C40A 1.479(8) . ? N38A C37A 1.503(7) . ? O53B C52B 1.240(7) . ? N19B C18B 1.283(7) . ? N19B C20B 1.463(7) . ? N19A C18A 1.270(6) . ? N19A C20A 1.457(7) . ? O43A C42A 1.243(7) . ? N23A C25A 1.470(9) . ? N23A C22A 1.477(7) . ? N23A C24A 1.503(8) . ? O43B C42B 1.241(8) . ? N23B C25B 1.471(8) . ? N23B C24B 1.477(8) . ? N23B C22B 1.486(8) . ? N38B C39B 1.468(7) . ? N38B C40B 1.472(7) . ? N38B C37B 1.488(7) . ? C18A C17A 1.440(8) . ? C18A H18A 0.96(5) . ? C32A C27A 1.395(7) . ? C32A C31A 1.409(7) . ? C32A C33A 1.447(8) . ? C12A C13A 1.402(7) . ? C12A C17A 1.422(8) . ? C17A C16A 1.417(7) . ? C12B C13B 1.400(7) . ? C12B C17B 1.414(7) . ? C13B C14B 1.391(8) . ? C13B H13B 0.9300 . ? C32B C27B 1.398(7) . ? C32B C31B 1.396(7) . ? C32B C33B 1.475(8) . ? C55B C60B 1.354(9) . ? C55B C56B 1.383(9) . ? C55B C54B 1.514(8) . ? C27B C28B 1.412(7) . ? C17B C16B 1.421(7) . ? C17B C18B 1.442(8) . ? C28A C29A 1.373(8) . ? C28A C27A 1.390(7) . ? C28A H28A 0.9300 . ? C28B C29B 1.371(8) . ? C28B H28B 0.9300 . ? C45A C50A 1.353(10) . ? C45A C46A 1.388(11) . ? C45A C44A 1.499(9) . ? C33A H33A 0.91(6) . ? C33B H33B 0.96(4) . ? C15B C16B 1.350(9) . ? C15B C14B 1.387(10) . ? C15B H15B 0.9300 . ? C42A C44A 1.525(8) . ? C13A C14A 1.374(9) . ? C13A H13A 0.9300 . ? C16A C15A 1.379(10) . ? C16A H16A 0.9300 . ? C15A C14A 1.350(11) . ? C15A H15A 0.9300 . ? C35A C36A 1.514(9) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C35B C36B 1.514(8) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C31B C30B 1.388(9) . ? C31B H31B 0.9300 . ? C36A C37A 1.506(9) . ? C36A H36A 0.9700 . ? C36A H36B 0.9700 . ? C16B H16B 0.9300 . ? C20B C21B 1.524(9) . ? C20B H20A 0.9700 . ? C20B H20B 0.9700 . ? C18B H18B 0.91(6) . ? C30B C29B 1.380(9) . ? C30B H30B 0.9300 . ? C21A C20A 1.513(9) . ? C21A C22A 1.518(8) . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C42B C44B 1.510(8) . ? C36B C37B 1.534(8) . ? C36B H36C 0.9700 . ? C36B H36D 0.9700 . ? C31A C30A 1.374(9) . ? C31A H31A 0.9300 . ? C52B C54B 1.524(8) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C29B H29B 0.9300 . ? C55A C60A 1.353(12) . ? C55A C56A 1.375(11) . ? C55A C54A 1.479(11) . ? C54B H54A 0.9700 . ? C54B H54B 0.9700 . ? C14B H14B 0.9300 . ? C14A H14A 0.9300 . ? C20A H20C 0.9700 . ? C20A H20D 0.9700 . ? C45B C50B 1.374(11) . ? C45B C46B 1.390(9) . ? C45B C44B 1.503(10) . ? C29A C30A 1.377(9) . ? C29A H29A 0.9300 . ? C57B C58B 1.357(10) . ? C57B C56B 1.378(10) . ? C57B H57B 0.9300 . ? C21B C22B 1.502(10) . ? C21B H21C 0.9700 . ? C21B H21D 0.9700 . ? C22B H22A 0.9700 . ? C22B H22B 0.9700 . ? C56B H56B 0.9300 . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C40B H40A 0.9600 . ? C40B H40B 0.9600 . ? C40B H40C 0.9600 . ? C22A H22C 0.9700 . ? C22A H22D 0.9700 . ? C60B C59B 1.377(9) . ? C60B H60B 0.9300 . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C25B H25A 0.9600 . ? C25B H25B 0.9600 . ? C25B H25C 0.9600 . ? C40A H40D 0.9600 . ? C40A H40E 0.9600 . ? C40A H40F 0.9600 . ? C25A H25D 0.9600 . ? C25A H25E 0.9600 . ? C25A H25F 0.9600 . ? C39A H39A 0.9600 . ? C39A H39B 0.9600 . ? C39A H39C 0.9600 . ? C39B H39D 0.9600 . ? C39B H39E 0.9600 . ? C39B H39F 0.9600 . ? C58B C59B 1.401(11) . ? C58B H58B 0.9300 . ? C24B H24A 0.9600 . ? C24B H24B 0.9600 . ? C24B H24C 0.9600 . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C48A C47A 1.336(12) . ? C48A C49A 1.341(12) . ? C48A H48A 0.9300 . ? C59B H59B 0.9300 . ? C56A C57A 1.368(12) . ? C56A H56A 0.9300 . ? C46A C47A 1.401(11) . ? C46A H46A 0.9300 . ? C24A H24D 0.9600 . ? C24A H24E 0.9600 . ? C24A H24F 0.9600 . ? C30A H30A 0.9300 . ? C49A C50A 1.363(10) . ? C49A H49A 0.9300 . ? C46B C47B 1.329(11) . ? C46B H46B 0.9300 . ? C60A C59A 1.382(16) . ? C60A H60A 0.9300 . ? C50A H50A 0.9300 . ? C47A H47A 0.9300 . ? C54A C52A 1.525(9) . ? C54A H54C 0.9700 . ? C54A H54D 0.9700 . ? C47B C48B 1.323(12) . ? C47B H47B 0.9300 . ? C57A C58A 1.311(13) . ? C57A H57A 0.9300 . ? C49B C48B 1.366(13) . ? C49B C50B 1.446(14) . ? C49B H49B 0.9300 . ? C48B H48B 0.9300 . ? C59A C58A 1.342(16) . ? C59A H59A 0.9300 . ? C50B H50B 0.9300 . ? C58A H58A 0.9300 . ? 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 N19A Ni1A O11A 90.85(15) . . ? N19A Ni1A O41A 97.86(16) . . ? O11A Ni1A O41A 166.30(14) . . ? N19A Ni1A O3A 169.03(15) . . ? O11A Ni1A O3A 79.21(13) . . ? O41A Ni1A O3A 91.10(14) . . ? N19A Ni1A N23A 86.13(17) . . ? O11A Ni1A N23A 102.89(16) . . ? O41A Ni1A N23A 88.30(17) . . ? O3A Ni1A N23A 100.52(15) . . ? N19A Ni1A O26A 96.87(15) . . ? O11A Ni1A O26A 79.75(13) . . ? O41A Ni1A O26A 88.68(14) . . ? O3A Ni1A O26A 76.94(13) . . ? N23A Ni1A O26A 176.01(16) . . ? N19A Ni1A Ni2A 122.99(12) . . ? O11A Ni1A Ni2A 50.03(10) . . ? O41A Ni1A Ni2A 116.30(11) . . ? O3A Ni1A Ni2A 46.53(9) . . ? N23A Ni1A Ni2A 135.36(13) . . ? O26A Ni1A Ni2A 44.51(9) . . ? N19B Ni1B O11B 91.37(15) . . ? N19B Ni1B O41B 96.36(16) . . ? O11B Ni1B O41B 165.05(14) . . ? N19B Ni1B O3B 169.48(15) . . ? O11B Ni1B O3B 78.69(12) . . ? O41B Ni1B O3B 92.61(14) . . ? N19B Ni1B N23B 87.28(17) . . ? O11B Ni1B N23B 102.48(15) . . ? O41B Ni1B N23B 90.69(16) . . ? O3B Ni1B N23B 98.14(15) . . ? N19B Ni1B O26B 98.59(15) . . ? O11B Ni1B O26B 79.37(12) . . ? O41B Ni1B O26B 86.82(14) . . ? O3B Ni1B O26B 76.36(12) . . ? N23B Ni1B O26B 173.84(15) . . ? N19B Ni1B Ni2B 124.38(12) . . ? O11B Ni1B Ni2B 50.02(9) . . ? O41B Ni1B Ni2B 115.44(11) . . ? O3B Ni1B Ni2B 45.92(9) . . ? N23B Ni1B Ni2B 133.07(12) . . ? O26B Ni1B Ni2B 44.17(9) . . ? N34B Ni2B O26B 90.45(15) . . ? N34B Ni2B O51B 96.53(15) . . ? O26B Ni2B O51B 167.57(14) . . ? N34B Ni2B O3B 170.99(14) . . ? O26B Ni2B O3B 80.61(12) . . ? O51B Ni2B O3B 92.06(13) . . ? N34B Ni2B N38B 86.62(16) . . ? O26B Ni2B N38B 101.52(15) . . ? O51B Ni2B N38B 89.19(16) . . ? O3B Ni2B N38B 96.22(15) . . ? N34B Ni2B O11B 101.82(13) . . ? O26B Ni2B O11B 78.46(12) . . ? O51B Ni2B O11B 90.02(13) . . ? O3B Ni2B O11B 75.42(12) . . ? N38B Ni2B O11B 171.57(15) . . ? N34B Ni2B Ni1B 125.24(11) . . ? O26B Ni2B Ni1B 48.51(9) . . ? O51B Ni2B Ni1B 119.43(10) . . ? O3B Ni2B Ni1B 47.04(9) . . ? N38B Ni2B Ni1B 129.69(12) . . ? O11B Ni2B Ni1B 44.55(8) . . ? O51A Ni2A O26A 167.51(15) . . ? O51A Ni2A N34A 96.75(16) . . ? O26A Ni2A N34A 90.28(14) . . ? O51A Ni2A O3A 91.84(15) . . ? O26A Ni2A O3A 80.49(13) . . ? N34A Ni2A O3A 170.34(14) . . ? O51A Ni2A N38A 89.40(17) . . ? O26A Ni2A N38A 101.26(16) . . ? N34A Ni2A N38A 87.34(16) . . ? O3A Ni2A N38A 97.17(15) . . ? O51A Ni2A O11A 89.88(14) . . ? O26A Ni2A O11A 78.69(13) . . ? N34A Ni2A O11A 100.24(14) . . ? O3A Ni2A O11A 75.31(13) . . ? N38A Ni2A O11A 172.42(15) . . ? O51A Ni2A Ni1A 119.06(11) . . ? O26A Ni2A Ni1A 48.75(10) . . ? N34A Ni2A Ni1A 124.16(11) . . ? O3A Ni2A Ni1A 46.88(9) . . ? N38A Ni2A Ni1A 130.36(12) . . ? O11A Ni2A Ni1A 44.46(8) . . ? C12B O11B Ni1B 126.8(3) . . ? C12B O11B Ni2B 119.8(3) . . ? Ni1B O11B Ni2B 85.43(11) . . ? Ni2B O3B Ni1B 87.03(12) . . ? Ni2B O3B H3B1 114.1 . . ? Ni1B O3B H3B1 114.1 . . ? Ni2B O3B H3B2 114.1 . . ? Ni1B O3B H3B2 114.1 . . ? H3B1 O3B H3B2 111.3 . . ? C27A O26A Ni2A 128.0(3) . . ? C27A O26A Ni1A 119.7(3) . . ? Ni2A O26A Ni1A 86.74(13) . . ? C12A O11A Ni1A 127.8(3) . . ? C12A O11A Ni2A 118.1(3) . . ? Ni1A O11A Ni2A 85.50(12) . . ? Ni2A O3A Ni1A 86.59(12) . . ? Ni2A O3A H3A1 114.2 . . ? Ni1A O3A H3A1 114.2 . . ? Ni2A O3A H3A2 114.2 . . ? Ni1A O3A H3A2 114.2 . . ? H3A1 O3A H3A2 111.4 . . ? C27B O26B Ni2B 127.9(3) . . ? C27B O26B Ni1B 121.1(3) . . ? Ni2B O26B Ni1B 87.31(12) . . ? C42B O41B Ni1B 123.6(4) . . ? C33A N34A C35A 117.7(4) . . ? C33A N34A Ni2A 125.3(4) . . ? C35A N34A Ni2A 116.3(3) . . ? C42A O41A Ni1A 128.9(3) . . ? C33B N34B C35B 116.6(4) . . ? C33B N34B Ni2B 126.7(4) . . ? C35B N34B Ni2B 115.5(3) . . ? C52A O51A Ni2A 127.9(4) . . ? C52B O51B Ni2B 129.5(4) . . ? C39A N38A C40A 108.5(5) . . ? C39A N38A C37A 109.8(5) . . ? C40A N38A C37A 105.8(5) . . ? C39A N38A Ni2A 109.4(4) . . ? C40A N38A Ni2A 111.2(4) . . ? C37A N38A Ni2A 112.0(4) . . ? C18B N19B C20B 118.6(5) . . ? C18B N19B Ni1B 125.0(4) . . ? C20B N19B Ni1B 116.1(3) . . ? C18A N19A C20A 118.8(4) . . ? C18A N19A Ni1A 125.3(4) . . ? C20A N19A Ni1A 115.6(3) . . ? C25A N23A C22A 110.6(5) . . ? C25A N23A C24A 108.8(6) . . ? C22A N23A C24A 106.6(5) . . ? C25A N23A Ni1A 110.1(4) . . ? C22A N23A Ni1A 111.6(4) . . ? C24A N23A Ni1A 109.0(4) . . ? C25B N23B C24B 107.5(5) . . ? C25B N23B C22B 111.0(5) . . ? C24B N23B C22B 107.3(5) . . ? C25B N23B Ni1B 109.2(3) . . ? C24B N23B Ni1B 110.5(4) . . ? C22B N23B Ni1B 111.3(4) . . ? C39B N38B C40B 108.3(5) . . ? C39B N38B C37B 110.3(5) . . ? C40B N38B C37B 105.8(4) . . ? C39B N38B Ni2B 110.0(3) . . ? C40B N38B Ni2B 110.9(3) . . ? C37B N38B Ni2B 111.4(3) . . ? N19A C18A C17A 127.4(5) . . ? N19A C18A H18A 122(3) . . ? C17A C18A H18A 110(3) . . ? C27A C32A C31A 119.2(5) . . ? C27A C32A C33A 124.1(5) . . ? C31A C32A C33A 116.7(5) . . ? O11A C12A C13A 119.5(5) . . ? O11A C12A C17A 122.7(4) . . ? C13A C12A C17A 117.8(5) . . ? C16A C17A C12A 118.7(5) . . ? C16A C17A C18A 116.8(5) . . ? C12A C17A C18A 124.4(4) . . ? O11B C12B C13B 118.3(5) . . ? O11B C12B C17B 123.4(4) . . ? C13B C12B C17B 118.3(5) . . ? C14B C13B C12B 120.8(6) . . ? C14B C13B H13B 119.6 . . ? C12B C13B H13B 119.6 . . ? C27B C32B C31B 121.1(5) . . ? C27B C32B C33B 123.4(4) . . ? C31B C32B C33B 115.6(5) . . ? C60B C55B C56B 119.2(6) . . ? C60B C55B C54B 120.0(6) . . ? C56B C55B C54B 120.6(6) . . ? O26B C27B C32B 123.8(5) . . ? O26B C27B C28B 119.3(5) . . ? C32B C27B C28B 116.9(5) . . ? C12B C17B C16B 118.7(5) . . ? C12B C17B C18B 124.8(4) . . ? C16B C17B C18B 116.3(5) . . ? C29A C28A C27A 122.2(5) . . ? C29A C28A H28A 118.9 . . ? C27A C28A H28A 118.9 . . ? C29B C28B C27B 121.6(6) . . ? C29B C28B H28B 119.2 . . ? C27B C28B H28B 119.2 . . ? O26A C27A C28A 119.1(5) . . ? O26A C27A C32A 123.4(4) . . ? C28A C27A C32A 117.5(5) . . ? C50A C45A C46A 117.0(7) . . ? C50A C45A C44A 120.6(8) . . ? C46A C45A C44A 122.2(7) . . ? N34A C33A C32A 127.4(5) . . ? N34A C33A H33A 121(4) . . ? C32A C33A H33A 111(4) . . ? N34B C33B C32B 126.6(5) . . ? N34B C33B H33B 114(3) . . ? C32B C33B H33B 119(3) . . ? C16B C15B C14B 119.4(6) . . ? C16B C15B H15B 120.3 . . ? C14B C15B H15B 120.3 . . ? O43A C42A O41A 126.1(5) . . ? O43A C42A C44A 117.9(5) . . ? O41A C42A C44A 116.0(5) . . ? C14A C13A C12A 120.7(7) . . ? C14A C13A H13A 119.6 . . ? C12A C13A H13A 119.6 . . ? C15A C16A C17A 121.2(7) . . ? C15A C16A H16A 119.4 . . ? C17A C16A H16A 119.4 . . ? C14A C15A C16A 119.0(6) . . ? C14A C15A H15A 120.5 . . ? C16A C15A H15A 120.5 . . ? N34A C35A C36A 107.6(5) . . ? N34A C35A H35A 110.2 . . ? C36A C35A H35A 110.2 . . ? N34A C35A H35B 110.2 . . ? C36A C35A H35B 110.2 . . ? H35A C35A H35B 108.5 . . ? N34B C35B C36B 109.1(5) . . ? N34B C35B H35C 109.9 . . ? C36B C35B H35C 109.9 . . ? N34B C35B H35D 109.9 . . ? C36B C35B H35D 109.9 . . ? H35C C35B H35D 108.3 . . ? C30B C31B C32B 120.4(6) . . ? C30B C31B H31B 119.8 . . ? C32B C31B H31B 119.8 . . ? C37A C36A C35A 116.4(5) . . ? C37A C36A H36A 108.2 . . ? C35A C36A H36A 108.2 . . ? C37A C36A H36B 108.2 . . ? C35A C36A H36B 108.2 . . ? H36A C36A H36B 107.4 . . ? C15B C16B C17B 122.0(6) . . ? C15B C16B H16B 119.0 . . ? C17B C16B H16B 119.0 . . ? N19B C20B C21B 107.9(5) . . ? N19B C20B H20A 110.1 . . ? C21B C20B H20A 110.1 . . ? N19B C20B H20B 110.1 . . ? C21B C20B H20B 110.1 . . ? H20A C20B H20B 108.4 . . ? N19B C18B C17B 127.0(5) . . ? N19B C18B H18B 123(3) . . ? C17B C18B H18B 110(3) . . ? C29B C30B C31B 119.1(5) . . ? C29B C30B H30B 120.5 . . ? C31B C30B H30B 120.5 . . ? C20A C21A C22A 115.4(5) . . ? C20A C21A H21A 108.4 . . ? C22A C21A H21A 108.4 . . ? C20A C21A H21B 108.4 . . ? C22A C21A H21B 108.4 . . ? H21A C21A H21B 107.5 . . ? O43B C42B O41B 126.7(5) . . ? O43B C42B C44B 115.7(6) . . ? O41B C42B C44B 117.6(6) . . ? C35B C36B C37B 115.0(5) . . ? C35B C36B H36C 108.5 . . ? C37B C36B H36C 108.5 . . ? C35B C36B H36D 108.5 . . ? C37B C36B H36D 108.5 . . ? H36C C36B H36D 107.5 . . ? C30A C31A C32A 122.4(6) . . ? C30A C31A H31A 118.8 . . ? C32A C31A H31A 118.8 . . ? O53B C52B O51B 126.0(5) . . ? O53B C52B C54B 117.6(5) . . ? O51B C52B C54B 116.3(5) . . ? C36A C37A N38A 116.4(5) . . ? C36A C37A H37A 108.2 . . ? N38A C37A H37A 108.2 . . ? C36A C37A H37B 108.2 . . ? N38A C37A H37B 108.2 . . ? H37A C37A H37B 107.3 . . ? C28B C29B C30B 120.8(6) . . ? C28B C29B H29B 119.6 . . ? C30B C29B H29B 119.6 . . ? C60A C55A C56A 114.8(8) . . ? C60A C55A C54A 122.4(9) . . ? C56A C55A C54A 122.7(8) . . ? C55B C54B C52B 113.9(5) . . ? C55B C54B H54A 108.8 . . ? C52B C54B H54A 108.8 . . ? C55B C54B H54B 108.8 . . ? C52B C54B H54B 108.8 . . ? H54A C54B H54B 107.7 . . ? C15B C14B C13B 120.7(6) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C15A C14A C13A 122.5(6) . . ? C15A C14A H14A 118.8 . . ? C13A C14A H14A 118.8 . . ? N19A C20A C21A 109.6(5) . . ? N19A C20A H20C 109.8 . . ? C21A C20A H20C 109.8 . . ? N19A C20A H20D 109.8 . . ? C21A C20A H20D 109.8 . . ? H20C C20A H20D 108.2 . . ? C50B C45B C46B 119.8(7) . . ? C50B C45B C44B 123.5(7) . . ? C46B C45B C44B 116.7(7) . . ? C28A C29A C30A 121.1(6) . . ? C28A C29A H29A 119.5 . . ? C30A C29A H29A 119.4 . . ? C58B C57B C56B 120.9(7) . . ? C58B C57B H57B 119.6 . . ? C56B C57B H57B 119.6 . . ? C22B C21B C20B 115.6(6) . . ? C22B C21B H21C 108.4 . . ? C20B C21B H21C 108.4 . . ? C22B C21B H21D 108.4 . . ? C20B C21B H21D 108.4 . . ? H21C C21B H21D 107.4 . . ? N23B C22B C21B 116.5(5) . . ? N23B C22B H22A 108.2 . . ? C21B C22B H22A 108.2 . . ? N23B C22B H22B 108.2 . . ? C21B C22B H22B 108.2 . . ? H22A C22B H22B 107.3 . . ? C57B C56B C55B 120.7(6) . . ? C57B C56B H56B 119.7 . . ? C55B C56B H56B 119.6 . . ? N38B C37B C36B 117.1(5) . . ? N38B C37B H37C 108.0 . . ? C36B C37B H37C 108.0 . . ? N38B C37B H37D 108.0 . . ? C36B C37B H37D 108.0 . . ? H37C C37B H37D 107.3 . . ? N38B C40B H40A 109.5 . . ? N38B C40B H40B 109.5 . . ? H40A C40B H40B 109.5 . . ? N38B C40B H40C 109.5 . . ? H40A C40B H40C 109.5 . . ? H40B C40B H40C 109.5 . . ? N23A C22A C21A 115.5(5) . . ? N23A C22A H22C 108.4 . . ? C21A C22A H22C 108.4 . . ? N23A C22A H22D 108.4 . . ? C21A C22A H22D 108.4 . . ? H22C C22A H22D 107.5 . . ? C55B C60B C59B 120.2(6) . . ? C55B C60B H60B 119.9 . . ? C59B C60B H60B 119.9 . . ? C45A C44A C42A 112.8(5) . . ? C45A C44A H44A 109.0 . . ? C42A C44A H44A 109.0 . . ? C45A C44A H44B 109.0 . . ? C42A C44A H44B 109.0 . . ? H44A C44A H44B 107.8 . . ? N23B C25B H25A 109.5 . . ? N23B C25B H25B 109.5 . . ? H25A C25B H25B 109.5 . . ? N23B C25B H25C 109.5 . . ? H25A C25B H25C 109.5 . . ? H25B C25B H25C 109.5 . . ? N38A C40A H40D 109.5 . . ? N38A C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? N38A C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? N23A C25A H25D 109.5 . . ? N23A C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? N23A C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? N38A C39A H39A 109.5 . . ? N38A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? N38A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? N38B C39B H39D 109.5 . . ? N38B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? N38B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C57B C58B C59B 118.0(7) . . ? C57B C58B H58B 121.0 . . ? C59B C58B H58B 121.0 . . ? N23B C24B H24A 109.5 . . ? N23B C24B H24B 109.5 . . ? H24A C24B H24B 109.5 . . ? N23B C24B H24C 109.5 . . ? H24A C24B H24C 109.5 . . ? H24B C24B H24C 109.5 . . ? C45B C44B C42B 116.1(6) . . ? C45B C44B H44C 108.2 . . ? C42B C44B H44C 108.3 . . ? C45B C44B H44D 108.3 . . ? C42B C44B H44D 108.3 . . ? H44C C44B H44D 107.4 . . ? C47A C48A C49A 121.0(8) . . ? C47A C48A H48A 119.5 . . ? C49A C48A H48A 119.5 . . ? C60B C59B C58B 121.0(7) . . ? C60B C59B H59B 119.5 . . ? C58B C59B H59B 119.5 . . ? C57A C56A C55A 122.1(8) . . ? C57A C56A H56A 118.9 . . ? C55A C56A H56A 119.0 . . ? C45A C46A C47A 119.8(8) . . ? C45A C46A H46A 120.1 . . ? C47A C46A H46A 120.1 . . ? N23A C24A H24D 109.5 . . ? N23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? N23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C31A C30A C29A 117.6(5) . . ? C31A C30A H30A 121.2 . . ? C29A C30A H30A 121.2 . . ? C48A C49A C50A 119.5(9) . . ? C48A C49A H49A 120.3 . . ? C50A C49A H49A 120.3 . . ? C47B C46B C45B 120.3(8) . . ? C47B C46B H46B 119.8 . . ? C45B C46B H46B 119.9 . . ? C55A C60A C59A 122.8(9) . . ? C55A C60A H60A 118.6 . . ? C59A C60A H60A 118.6 . . ? C45A C50A C49A 122.8(8) . . ? C45A C50A H50A 118.6 . . ? C49A C50A H50A 118.6 . . ? C48A C47A C46A 119.9(9) . . ? C48A C47A H47A 120.1 . . ? C46A C47A H47A 120.1 . . ? C55A C54A C52A 116.6(6) . . ? C55A C54A H54C 108.1 . . ? C52A C54A H54C 108.1 . . ? C55A C54A H54D 108.1 . . ? C52A C54A H54D 108.1 . . ? H54C C54A H54D 107.3 . . ? C48B C47B C46B 121.3(9) . . ? C48B C47B H47B 119.4 . . ? C46B C47B H47B 119.4 . . ? O53A C52A O51A 126.5(6) . . ? O53A C52A C54A 117.0(6) . . ? O51A C52A C54A 116.5(6) . . ? C58A C57A C56A 121.0(10) . . ? C58A C57A H57A 119.5 . . ? C56A C57A H57A 119.5 . . ? C48B C49B C50B 116.6(9) . . ? C48B C49B H49B 121.7 . . ? C50B C49B H49B 121.7 . . ? C47B C48B C49B 123.1(10) . . ? C47B C48B H48B 118.4 . . ? C49B C48B H48B 118.4 . . ? C58A C59A C60A 119.4(9) . . ? C58A C59A H59A 120.3 . . ? C60A C59A H59A 120.3 . . ? C45B C50B C49B 118.6(8) . . ? C45B C50B H50B 120.7 . . ? C49B C50B H50B 120.7 . . ? C57A C58A C59A 119.7(11) . . ? C57A C58A H58A 120.1 . . ? C59A C58A H58A 120.1 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.994 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.097 #END