# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C60 H60 N18 Ni O12, C60 H56 N18 Ni O12, 3(C12 H26 N6 Ni), C12 H26 N6 Ni O2 ; _chemical_formula_sum 'C168 H220 N60 Ni6 O26' _chemical_formula_weight 3848.30 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1401(14) _cell_length_b 18.984(3) _cell_length_c 35.484(6) _cell_angle_alpha 97.850(4) _cell_angle_beta 94.141(4) _cell_angle_gamma 97.048(4) _cell_volume 5368.9(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3430 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 19.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8817 _exptl_absorpt_correction_T_max 0.9276 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40554 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1602 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 0.58 _diffrn_reflns_theta_max 25.25 _reflns_number_total 18736 _reflns_number_gt 7957 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1025P)^2^+0.7000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18736 _refine_ls_number_parameters 1108 _refine_ls_number_restraints 1022 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2432 _refine_ls_wR_factor_gt 0.2149 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.000 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 Ni5 Ni 0.4860(4) 0.49348(16) 0.49458(7) 0.0788(5) Uiso 0.50 1 d PDU . . C82 C 0.6265(11) 0.3917(4) 0.53239(19) 0.177(3) Uiso 1 1 d DU . . H82A H 0.7434 0.4145 0.5340 0.213 Uiso 1 1 calc R . . H82B H 0.6275 0.3407 0.5354 0.213 Uiso 1 1 calc R . . N28 N 0.5472(10) 0.3953(5) 0.49503(18) 0.190(2) Uiso 1 1 d DU . . C79 C 0.6747(10) 0.3938(5) 0.4634(2) 0.182(2) Uiso 1 1 d DU . . H79A H 0.7502 0.4395 0.4654 0.219 Uiso 1 1 calc R . . H79B H 0.7398 0.3531 0.4632 0.219 Uiso 1 1 calc R . . N29 N 0.5461(11) 0.3839(5) 0.4304(2) 0.195(2) Uiso 1 1 d DU . . C80 C 0.3785(10) 0.3442(5) 0.4379(2) 0.202(3) Uiso 1 1 d DU . . H80A H 0.3545 0.2964 0.4220 0.242 Uiso 1 1 calc R . . H80B H 0.2866 0.3723 0.4329 0.242 Uiso 1 1 calc R . . C81 C 0.4044(10) 0.3373(5) 0.4809(2) 0.177(3) Uiso 1 1 d DU . . H81A H 0.3039 0.3458 0.4940 0.213 Uiso 1 1 calc R . . H81B H 0.4334 0.2894 0.4845 0.213 Uiso 1 1 calc R . . C83 C 0.5297(12) 0.4516(4) 0.4137(3) 0.184(3) Uiso 1 1 d DU . . H83A H 0.6399 0.4750 0.4087 0.220 Uiso 1 1 calc R . . H83B H 0.4570 0.4412 0.3894 0.220 Uiso 1 1 calc R . . N30 N 0.4565(11) 0.4969(4) 0.4423(2) 0.190(2) Uiso 1 1 d DU . . H30 H 0.3444 0.4791 0.4370 0.228 Uiso 1 1 calc R . . C84 C 0.4555(13) 0.5729(4) 0.4359(2) 0.178(3) Uiso 1 1 d DU . . H84A H 0.5705 0.5969 0.4358 0.214 Uiso 1 1 calc R . . H84B H 0.3935 0.5749 0.4111 0.214 Uiso 1 1 calc R . . O13 O 0.1977(13) 0.4892(9) 0.4911(4) 0.179(4) Uiso 0.50 1 d PDU . . O14 O 0.7488(14) 0.5371(7) 0.4907(4) 0.153(3) Uiso 0.50 1 d PDU . . C52 C 0.7277(9) 1.0010(3) 0.4440(2) 0.061(2) Uiso 0.672(4) 1 d PDU . 1 H52A H 0.6257 0.9819 0.4288 0.091 Uiso 0.672(4) 1 d PR . 1 H52B H 0.7135 1.0452 0.4595 0.091 Uiso 0.672(4) 1 d PR . 1 H52C H 0.8144 1.0099 0.4277 0.091 Uiso 0.672(4) 1 d PR . 1 N13 N 0.7706(8) 0.9502(3) 0.46842(16) 0.0478(15) Uiso 0.672(4) 1 d PDU . 1 C49 C 0.6516(8) 0.9382(3) 0.49756(17) 0.052(2) Uiso 0.672(4) 1 d PDU . 1 H49A H 0.5404 0.9263 0.4854 0.063 Uiso 0.672(4) 1 d PR . 1 H49B H 0.6571 0.9789 0.5171 0.063 Uiso 0.672(4) 1 d PR . 1 N14 N 0.7041(8) 0.8757(3) 0.51295(16) 0.0618(18) Uiso 0.672(4) 1 d PDU . 1 C50 C 0.7646(11) 0.8291(3) 0.47996(19) 0.068(2) Uiso 0.672(4) 1 d PDU . 1 H50A H 0.6885 0.7857 0.4725 0.081 Uiso 0.672(4) 1 d PR . 1 H50B H 0.8723 0.8168 0.4871 0.081 Uiso 0.672(4) 1 d PR . 1 C51 C 0.7780(10) 0.8767(3) 0.44736(18) 0.060(2) Uiso 0.672(4) 1 d PDU . 1 H51A H 0.8787 0.8745 0.4350 0.073 Uiso 0.672(4) 1 d PR . 1 H51B H 0.6840 0.8628 0.4287 0.073 Uiso 0.672(4) 1 d PR . 1 C53 C 0.8337(8) 0.8943(4) 0.54524(19) 0.064(2) Uiso 0.672(4) 1 d PDU . 1 H53A H 0.8486 0.8523 0.5567 0.077 Uiso 0.672(4) 1 d PR . 1 H53B H 0.7908 0.9274 0.5637 0.077 Uiso 0.672(4) 1 d PR . 1 N15 N 0.9947(7) 0.9303(4) 0.53570(18) 0.0512(18) Uiso 0.672(4) 1 d PDU . 1 H15X H 1.0462 0.8945 0.5248 0.061 Uiso 0.672(4) 1 d PR . 1 C54 C 1.1046(9) 0.9623(4) 0.5708(2) 0.072(3) Uiso 0.672(4) 1 d PDU . 1 H54A H 1.1081 0.9281 0.5883 0.108 Uiso 0.672(4) 1 d PR . 1 H54B H 1.2151 0.9769 0.5645 0.108 Uiso 0.672(4) 1 d PR . 1 H54C H 1.0591 1.0034 0.5824 0.108 Uiso 0.672(4) 1 d PR . 1 C152 C 0.7894(14) 0.8703(5) 0.4994(2) 0.068(3) Uiso 0.328(4) 1 d PDU . 2 H15A H 0.6973 0.8336 0.4907 0.101 Uiso 0.328(4) 1 d PR . 2 H15B H 0.8916 0.8511 0.4956 0.101 Uiso 0.328(4) 1 d PR . 2 H15C H 0.7854 0.8870 0.5260 0.101 Uiso 0.328(4) 1 d PR . 2 N113 N 0.7933(12) 0.9302(5) 0.4785(2) 0.051(3) Uiso 0.328(4) 1 d PDU . 2 C149 C 0.8078(13) 0.9075(4) 0.4359(2) 0.062(3) Uiso 0.328(4) 1 d PDU . 2 H14A H 0.7379 0.8640 0.4251 0.074 Uiso 0.328(4) 1 d PR . 2 H14B H 0.9213 0.9029 0.4316 0.074 Uiso 0.328(4) 1 d PR . 2 N114 N 0.7536(13) 0.9697(6) 0.4193(3) 0.070(3) Uiso 0.328(4) 1 d PDU . 2 C150 C 0.6252(11) 0.9998(6) 0.4427(3) 0.067(4) Uiso 0.328(4) 1 d PDU . 2 H15D H 0.5184 0.9884 0.4284 0.081 Uiso 0.328(4) 1 d PR . 2 H15E H 0.6483 1.0508 0.4501 0.081 Uiso 0.328(4) 1 d PR . 2 C151 C 0.6279(12) 0.9606(6) 0.4788(3) 0.062(3) Uiso 0.328(4) 1 d PDU . 2 H15F H 0.6289 0.9936 0.5019 0.074 Uiso 0.328(4) 1 d PR . 2 H15G H 0.5349 0.9237 0.4773 0.074 Uiso 0.328(4) 1 d PR . 2 C153 C 0.9009(11) 1.0273(6) 0.4208(3) 0.063(4) Uiso 0.328(4) 1 d PDU . 2 H15H H 0.8693 1.0574 0.4026 0.076 Uiso 0.328(4) 1 d PR . 2 H15W H 0.9902 1.0037 0.4111 0.076 Uiso 0.328(4) 1 d PR . 2 N115 N 0.9718(13) 1.0721(8) 0.4569(3) 0.053(4) Uiso 0.328(4) 1 d PDU . 2 H11C H 0.9068 1.1059 0.4638 0.064 Uiso 0.328(4) 1 d PR . 2 C154 C 1.1461(14) 1.1012(9) 0.4576(3) 0.066(5) Uiso 0.328(4) 1 d PDU . 2 H15I H 1.1611 1.1356 0.4403 0.099 Uiso 0.328(4) 1 d PR . 2 H15J H 1.1815 1.1242 0.4832 0.099 Uiso 0.328(4) 1 d PR . 2 H15K H 1.2110 1.0631 0.4509 0.099 Uiso 0.328(4) 1 d PR . 2 Ni2 Ni 0.29320(11) 0.29330(4) 0.21776(3) 0.0299(3) Uani 0.7847(14) 1 d PU A 5 C62 C -0.0288(7) 0.2283(3) 0.19200(14) 0.0456(16) Uiso 0.7847(14) 1 d PDU A 5 H62A H -0.0872 0.2691 0.1969 0.055 Uiso 0.7847(14) 1 d PR A 5 H62B H -0.1077 0.1854 0.1878 0.055 Uiso 0.7847(14) 1 d PR A 5 N16 N 0.0942(6) 0.2274(3) 0.22424(12) 0.0432(13) Uiso 0.7847(14) 1 d PDU A 5 C55 C 0.0235(7) 0.2499(3) 0.26066(14) 0.0503(17) Uiso 0.7847(14) 1 d PDU A 5 H55A H -0.0896 0.2282 0.2602 0.060 Uiso 0.7847(14) 1 d PR A 5 H55B H 0.0281 0.3011 0.2656 0.060 Uiso 0.7847(14) 1 d PR A 5 N17 N 0.1307(7) 0.2230(3) 0.28953(15) 0.0586(15) Uiso 0.7847(14) 1 d PDU A 5 C64 C 0.1683(9) 0.1530(3) 0.27127(17) 0.0602(19) Uiso 0.7847(14) 1 d PDU A 5 H64A H 0.0914 0.1156 0.2783 0.072 Uiso 0.7847(14) 1 d PR A 5 H64B H 0.2793 0.1451 0.2789 0.072 Uiso 0.7847(14) 1 d PR A 5 C63 C 0.1428(8) 0.1546(3) 0.22730(15) 0.0462(16) Uiso 0.7847(14) 1 d PDU A 5 H63A H 0.2447 0.1487 0.2159 0.055 Uiso 0.7847(14) 1 d PR A 5 H63B H 0.0575 0.1174 0.2151 0.055 Uiso 0.7847(14) 1 d PR A 5 C56 C 0.2841(7) 0.2750(3) 0.29981(18) 0.0583(18) Uiso 0.7847(14) 1 d PDU A 5 H56A H 0.3502 0.2599 0.3200 0.070 Uiso 0.7847(14) 1 d PR A 5 H56B H 0.2533 0.3208 0.3094 0.070 Uiso 0.7847(14) 1 d PR A 5 N18 N 0.3864(6) 0.2843(2) 0.26751(13) 0.0346(12) Uiso 0.7847(14) 1 d PDU A 5 H18A H 0.4387 0.2450 0.2641 0.042 Uiso 0.7847(14) 1 d PR A 5 C57 C 0.5231(8) 0.3459(4) 0.27996(17) 0.0583(17) Uiso 0.7847(14) 1 d PDU A 5 H57A H 0.5972 0.3362 0.3003 0.070 Uiso 0.7847(14) 1 d PR A 5 H57B H 0.4760 0.3887 0.2883 0.070 Uiso 0.7847(14) 1 d PR A 5 C58 C 0.6118(7) 0.3541(3) 0.24422(14) 0.0450(16) Uiso 0.7847(14) 1 d PDU A 5 H58A H 0.6714 0.3141 0.2382 0.054 Uiso 0.7847(14) 1 d PR A 5 H58B H 0.6892 0.3974 0.2479 0.054 Uiso 0.7847(14) 1 d PR A 5 N19 N 0.4855(6) 0.3562(2) 0.21291(12) 0.0383(12) Uiso 0.7847(14) 1 d PDU A 5 C59 C 0.5608(7) 0.3363(3) 0.17499(14) 0.0419(16) Uiso 0.7847(14) 1 d PDU A 5 H59A H 0.5631 0.2855 0.1693 0.050 Uiso 0.7847(14) 1 d PR A 5 H59B H 0.6710 0.3611 0.1751 0.050 Uiso 0.7847(14) 1 d PR A 5 N20 N 0.4449(6) 0.3607(3) 0.14785(14) 0.0494(14) Uiso 0.7847(14) 1 d PDU A 5 C66 C 0.4102(9) 0.4314(3) 0.16718(17) 0.0584(18) Uiso 0.7847(14) 1 d PDU A 5 H66A H 0.2966 0.4372 0.1607 0.070 Uiso 0.7847(14) 1 d PR A 5 H66B H 0.4814 0.4702 0.1596 0.070 Uiso 0.7847(14) 1 d PR A 5 C65 C 0.4393(8) 0.4278(3) 0.21054(15) 0.0454(16) Uiso 0.7847(14) 1 d PDU A 5 H65A H 0.5277 0.4644 0.2219 0.055 Uiso 0.7847(14) 1 d PR A 5 H65B H 0.3411 0.4345 0.2233 0.055 Uiso 0.7847(14) 1 d PR A 5 C60 C 0.3012(7) 0.3094(3) 0.13672(17) 0.0504(16) Uiso 0.7847(14) 1 d PDU A 5 H60A H 0.3362 0.2640 0.1277 0.060 Uiso 0.7847(14) 1 d PR A 5 H60B H 0.2374 0.3239 0.1160 0.060 Uiso 0.7847(14) 1 d PR A 5 N21 N 0.1945(6) 0.2990(3) 0.16861(13) 0.0370(12) Uiso 0.7847(14) 1 d PDU A 5 H21A H 0.1368 0.3367 0.1712 0.044 Uiso 0.7847(14) 1 d PR A 5 C61 C 0.0703(8) 0.2355(3) 0.15750(16) 0.0493(16) Uiso 0.7847(14) 1 d PDU A 5 H61A H 0.0002 0.2400 0.1353 0.059 Uiso 0.7847(14) 1 d PR A 5 H61B H 0.1254 0.1938 0.1521 0.059 Uiso 0.7847(14) 1 d PR A 5 Ni2' Ni 0.2906(5) 0.28384(19) 0.22768(11) 0.0322(10) Uani 0.2153(14) 1 d PDU A 6 C162 C 0.1159(16) 0.1710(6) 0.2480(2) 0.054(3) Uiso 0.2153(14) 1 d PDU A 6 H16A H 0.1926 0.1367 0.2441 0.065 Uiso 0.2153(14) 1 d PR A 6 H16B H 0.0080 0.1459 0.2502 0.065 Uiso 0.2153(14) 1 d PR A 6 N116 N 0.1186(14) 0.2159(7) 0.2165(2) 0.046(3) Uiso 0.2153(14) 1 d PDU A 6 C155 C 0.1353(13) 0.1684(5) 0.1800(2) 0.055(4) Uiso 0.2153(14) 1 d PDU A 6 H15L H 0.0776 0.1208 0.1789 0.066 Uiso 0.2153(14) 1 d PR A 6 H15M H 0.2501 0.1657 0.1762 0.066 Uiso 0.2153(14) 1 d PR A 6 N117 N 0.0573(14) 0.2073(7) 0.1514(3) 0.050(3) Uiso 0.2153(14) 1 d PDU A 6 C164 C -0.0818(11) 0.2398(8) 0.1686(3) 0.046(3) Uiso 0.2153(14) 1 d PDU A 6 H16C H -0.1844 0.2089 0.1606 0.055 Uiso 0.2153(14) 1 d PR A 6 H16D H -0.0917 0.2864 0.1618 0.055 Uiso 0.2153(14) 1 d PR A 6 C163 C -0.0388(14) 0.2456(7) 0.2124(3) 0.042(3) Uiso 0.2153(14) 1 d PDU A 6 H16E H -0.0263 0.2945 0.2247 0.051 Uiso 0.2153(14) 1 d PR A 6 H16F H -0.1232 0.2178 0.2237 0.051 Uiso 0.2153(14) 1 d PR A 6 C156 C 0.1820(13) 0.2647(6) 0.1426(3) 0.049(3) Uiso 0.2153(14) 1 d PDU A 6 H15N H 0.1312 0.2880 0.1233 0.059 Uiso 0.2153(14) 1 d PR A 6 H15O H 0.2744 0.2444 0.1323 0.059 Uiso 0.2153(14) 1 d PR A 6 N118 N 0.2447(16) 0.3197(7) 0.1759(4) 0.039(3) Uiso 0.2153(14) 1 d PDU A 6 H11B H 0.1673 0.3495 0.1792 0.046 Uiso 0.2153(14) 1 d PR A 6 C157 C 0.3951(18) 0.3649(8) 0.1650(3) 0.046(3) Uiso 0.2153(14) 1 d PDU A 6 H15P H 0.3713 0.3899 0.1439 0.055 Uiso 0.2153(14) 1 d PR A 6 H15Q H 0.4796 0.3352 0.1589 0.055 Uiso 0.2153(14) 1 d PR A 6 C158 C 0.4481(17) 0.4200(5) 0.2012(2) 0.038(3) Uiso 0.2153(14) 1 d PDU A 6 H15R H 0.3691 0.4532 0.2058 0.046 Uiso 0.2153(14) 1 d PR A 6 H15S H 0.5547 0.4466 0.1994 0.046 Uiso 0.2153(14) 1 d PR A 6 N119 N 0.4576(13) 0.3750(7) 0.2328(2) 0.036(3) Uiso 0.2153(14) 1 d PDU A 6 C159 C 0.4616(14) 0.4237(5) 0.2696(2) 0.050(4) Uiso 0.2153(14) 1 d PDU A 6 H15T H 0.3505 0.4308 0.2751 0.060 Uiso 0.2153(14) 1 d PR A 6 H15U H 0.5279 0.4694 0.2704 0.060 Uiso 0.2153(14) 1 d PR A 6 N120 N 0.5367(15) 0.3788(7) 0.2956(3) 0.057(3) Uiso 0.2153(14) 1 d PDU A 6 C166 C 0.6696(11) 0.3451(8) 0.2757(3) 0.054(4) Uiso 0.2153(14) 1 d PDU A 6 H16G H 0.6672 0.2965 0.2806 0.065 Uiso 0.2153(14) 1 d PR A 6 H16H H 0.7773 0.3710 0.2844 0.065 Uiso 0.2153(14) 1 d PR A 6 C165 C 0.6181(15) 0.3446(8) 0.2326(3) 0.042(3) Uiso 0.2153(14) 1 d PDU A 6 H16I H 0.7021 0.3753 0.2228 0.050 Uiso 0.2153(14) 1 d PR A 6 H16J H 0.6069 0.2975 0.2181 0.050 Uiso 0.2153(14) 1 d PR A 6 C160 C 0.4051(13) 0.3212(5) 0.3017(3) 0.058(3) Uiso 0.2153(14) 1 d PDU A 6 H16K H 0.3092 0.3434 0.3084 0.070 Uiso 0.2153(14) 1 d PR A 6 H16L H 0.4478 0.3030 0.3239 0.070 Uiso 0.2153(14) 1 d PR A 6 N121 N 0.3464(15) 0.2568(8) 0.2758(5) 0.053(3) Uiso 0.2153(14) 1 d PDU A 6 H12D H 0.4233 0.2265 0.2746 0.063 Uiso 0.2153(14) 1 d PR A 6 C161 C 0.1735(16) 0.2260(8) 0.2851(3) 0.058(3) Uiso 0.2153(14) 1 d PDU A 6 H16M H 0.1793 0.2024 0.3074 0.069 Uiso 0.2153(14) 1 d PR A 6 H16O H 0.0988 0.2612 0.2886 0.069 Uiso 0.2153(14) 1 d PR A 6 N12 N -0.0452(5) 0.7929(2) 0.31073(11) 0.0446(11) Uani 0.396(4) 1 d PDU B 3 H12A H -0.0804 0.8334 0.3216 0.054 Uiso 0.396(4) 1 d PR B 3 C42 C -0.0208(14) 0.7398(5) 0.3359(3) 0.044(2) Uiso 0.396(4) 1 d PDU B 3 C43 C -0.0786(16) 0.7546(6) 0.3716(3) 0.053(3) Uiso 0.396(4) 1 d PDU B 3 H43A H -0.1138 0.8007 0.3786 0.063 Uiso 0.396(4) 1 d PR B 3 C44 C -0.0926(16) 0.7076(5) 0.3974(3) 0.063(3) Uiso 0.396(4) 1 d PDU B 3 H44A H -0.1529 0.7169 0.4194 0.075 Uiso 0.396(4) 1 d PR B 3 C45 C -0.0191(14) 0.6457(5) 0.3914(2) 0.065(3) Uiso 0.396(4) 1 d PDU B 3 C46 C 0.0622(16) 0.6344(6) 0.3583(2) 0.059(3) Uiso 0.396(4) 1 d PDU B 3 H46A H 0.1241 0.5945 0.3547 0.070 Uiso 0.396(4) 1 d PR B 3 C47 C 0.0547(16) 0.6765(5) 0.3301(3) 0.049(3) Uiso 0.396(4) 1 d PDU B 3 H47A H 0.1018 0.6638 0.3065 0.059 Uiso 0.396(4) 1 d PR B 3 C48 C -0.0071(16) 0.5979(5) 0.4208(3) 0.086(4) Uiso 0.396(4) 1 d PDU B 3 O11 O -0.0684(14) 0.6112(6) 0.4531(2) 0.086(3) Uiso 0.396(4) 1 d PDU B 3 O12 O 0.0490(16) 0.5378(5) 0.4118(3) 0.118(4) Uiso 0.396(4) 1 d PDU B 3 N12' N -0.0452(5) 0.7929(2) 0.31073(11) 0.0446(11) Uani 0.604(4) 1 d PDU B 4 H12B H -0.0616 0.8399 0.3196 0.054 Uiso 0.604(4) 1 d PR B 4 C42' C -0.0537(10) 0.7439(4) 0.3344(2) 0.0404(17) Uiso 0.604(4) 1 d PDU B 4 C43' C -0.1294(12) 0.7580(4) 0.3671(2) 0.055(2) Uiso 0.604(4) 1 d PDU B 4 H43B H -0.1739 0.8026 0.3720 0.067 Uiso 0.604(4) 1 d PR B 4 C44' C -0.1399(12) 0.7118(4) 0.3929(2) 0.060(2) Uiso 0.604(4) 1 d PDU B 4 H44B H -0.1930 0.7232 0.4158 0.072 Uiso 0.604(4) 1 d PR B 4 C45' C -0.0747(11) 0.6480(4) 0.3866(2) 0.058(2) Uiso 0.604(4) 1 d PDU B 4 C46' C 0.0011(11) 0.6334(4) 0.35293(19) 0.049(2) Uiso 0.604(4) 1 d PDU B 4 H46B H 0.0404 0.5877 0.3475 0.058 Uiso 0.604(4) 1 d PR B 4 C47' C 0.0164(11) 0.6805(4) 0.3273(2) 0.050(2) Uiso 0.604(4) 1 d PDU B 4 H47B H 0.0760 0.6709 0.3051 0.059 Uiso 0.604(4) 1 d PR B 4 C48' C -0.0911(12) 0.5951(4) 0.4136(2) 0.072(3) Uiso 0.604(4) 1 d PDU B 4 O11' O -0.1452(10) 0.6139(4) 0.44633(19) 0.092(3) Uiso 0.604(4) 1 d PDU B 4 O12' O -0.0765(10) 0.5292(3) 0.4019(2) 0.089(2) Uiso 0.604(4) 1 d PDU B 4 C1 C 1.4849(6) 0.7642(3) 0.29511(13) 0.0398(14) Uani 1 1 d . . . C2 C 1.5590(6) 0.7273(2) 0.23748(13) 0.0344(13) Uani 1 1 d . . . C3 C 1.4537(6) 0.8290(2) 0.24902(13) 0.0350(13) Uani 1 1 d . . . C4 C 1.4004(6) 0.7855(3) 0.36199(14) 0.0423(15) Uani 1 1 d . . . C5 C 1.3372(6) 0.8492(3) 0.36320(15) 0.0452(15) Uani 1 1 d . . . H5A H 1.3393 0.8732 0.3414 0.054 Uiso 1 1 calc R . . C6 C 1.2697(7) 0.8798(3) 0.39563(14) 0.0472(16) Uani 1 1 d . . . H6A H 1.2247 0.9236 0.3951 0.057 Uiso 1 1 calc R . . C7 C 1.2663(7) 0.8487(3) 0.42804(14) 0.0467(16) Uani 1 1 d . . . C8 C 1.3297(8) 0.7850(3) 0.42685(15) 0.0636(19) Uani 1 1 d D . . H8A H 1.3271 0.7619 0.4490 0.076 Uiso 1 1 calc R . . C9 C 1.3976(7) 0.7520(3) 0.39529(15) 0.0549(17) Uani 1 1 d . . . H9A H 1.4412 0.7080 0.3960 0.066 Uiso 1 1 calc R . . C10 C 1.1912(7) 0.8786(3) 0.46257(14) 0.0495(16) Uani 1 1 d . . . C11 C 1.7032(6) 0.6220(2) 0.21293(14) 0.0367(14) Uani 1 1 d . . . C12 C 1.7595(6) 0.5994(3) 0.24671(15) 0.0404(14) Uani 1 1 d . . . H12C H 1.7354 0.6235 0.2705 0.048 Uiso 1 1 calc R . . C13 C 1.8497(6) 0.5425(2) 0.24600(15) 0.0409(15) Uani 1 1 d . . . H13B H 1.8865 0.5276 0.2693 0.049 Uiso 1 1 calc R . . C14 C 1.8878(6) 0.5062(2) 0.21116(15) 0.0392(14) Uani 1 1 d . . . C15 C 1.8279(6) 0.5287(3) 0.17810(15) 0.0449(15) Uani 1 1 d . . . H15V H 1.8483 0.5035 0.1542 0.054 Uiso 1 1 calc R . . C16 C 1.7389(6) 0.5866(2) 0.17822(14) 0.0391(14) Uani 1 1 d . . . H16N H 1.7031 0.6018 0.1549 0.047 Uiso 1 1 calc R . . C17 C 1.9862(6) 0.4433(3) 0.21086(19) 0.0565(18) Uani 1 1 d . . . C18 C 1.3760(6) 0.9092(3) 0.20212(14) 0.0401(15) Uani 1 1 d . . . C19 C 1.4229(8) 0.8724(3) 0.16911(15) 0.0587(18) Uani 1 1 d . . . H19A H 1.4713 0.8297 0.1706 0.070 Uiso 1 1 calc R . . C20 C 1.4014(7) 0.8959(3) 0.13375(16) 0.0539(17) Uani 1 1 d . . . H20A H 1.4341 0.8688 0.1117 0.065 Uiso 1 1 calc R . . C21 C 1.3327(6) 0.9585(3) 0.13039(14) 0.0419(15) Uani 1 1 d . . . C22 C 1.2827(7) 0.9953(3) 0.16337(16) 0.0531(17) Uani 1 1 d . . . H22A H 1.2336 1.0379 0.1619 0.064 Uiso 1 1 calc R . . C23 C 1.3029(6) 0.9714(3) 0.19793(15) 0.0452(16) Uani 1 1 d . . . H23A H 1.2664 0.9978 0.2198 0.054 Uiso 1 1 calc R . . C24 C 1.3150(6) 0.9832(3) 0.09312(16) 0.0511(17) Uani 1 1 d . . . C25 C 0.0600(6) 0.7367(3) 0.21844(14) 0.0404(15) Uani 1 1 d . . . C26 C -0.0551(6) 0.8381(2) 0.22011(13) 0.0324(13) Uani 1 1 d . . . C27 C -0.0190(6) 0.7905(3) 0.27365(14) 0.0418(15) Uani 1 1 d . . . C28 C 0.1719(6) 0.6648(2) 0.16326(13) 0.0353(14) Uani 1 1 d . . . C29 C 0.1632(7) 0.7130(3) 0.13773(15) 0.0520(16) Uani 1 1 d . . . H29A H 0.1274 0.7584 0.1449 0.062 Uiso 1 1 calc R . . C30 C 0.2098(7) 0.6925(3) 0.10013(14) 0.0489(15) Uani 1 1 d . . . H30A H 0.2046 0.7244 0.0818 0.059 Uiso 1 1 calc R . . C31 C 0.2622(5) 0.6268(2) 0.09039(13) 0.0335(13) Uani 1 1 d . . . C32 C 0.2651(6) 0.5808(3) 0.11614(14) 0.0422(15) Uani 1 1 d . . . H32A H 0.2978 0.5350 0.1087 0.051 Uiso 1 1 calc R . . C33 C 0.2222(6) 0.5978(2) 0.15314(14) 0.0414(14) Uani 1 1 d . . . H33A H 0.2269 0.5648 0.1709 0.050 Uiso 1 1 calc R . . C34 C 0.3225(6) 0.6089(3) 0.05039(14) 0.0451(15) Uani 1 1 d . . . C35 C -0.1721(6) 0.9521(2) 0.20933(14) 0.0347(13) Uani 1 1 d . . . C36 C -0.2114(7) 0.9888(2) 0.18070(15) 0.0446(15) Uani 1 1 d . . . H36A H -0.1854 0.9726 0.1556 0.053 Uiso 1 1 calc R . . C37 C -0.2889(6) 1.0496(3) 0.18739(15) 0.0393(14) Uani 1 1 d . . . H37A H -0.3195 1.0736 0.1667 0.047 Uiso 1 1 calc R . . C38 C -0.3222(6) 1.0760(2) 0.22402(14) 0.0377(14) Uani 1 1 d . . . C39 C -0.2775(6) 1.0375(3) 0.25379(14) 0.0444(15) Uani 1 1 d . . . H39A H -0.2990 1.0546 0.2791 0.053 Uiso 1 1 calc R . . C40 C -0.2038(6) 0.9759(3) 0.24712(14) 0.0434(15) Uani 1 1 d . . . H40A H -0.1753 0.9505 0.2674 0.052 Uiso 1 1 calc R . . C41 C -0.4083(6) 1.1423(3) 0.23096(16) 0.0423(15) Uani 1 1 d . . . C67 C 0.7600(7) 0.0817(3) 0.03325(17) 0.0600(18) Uani 1 1 d . . . H67A H 0.7626 0.1018 0.0090 0.072 Uiso 1 1 calc R . . H67B H 0.6475 0.0818 0.0421 0.072 Uiso 1 1 calc R . . C68 C 0.9010(8) 0.0726(3) 0.09141(15) 0.0637(19) Uani 1 1 d . . . H68A H 0.8249 0.0823 0.1115 0.076 Uiso 1 1 calc R . . H68B H 1.0161 0.0782 0.1036 0.076 Uiso 1 1 calc R . . C69 C 0.8530(7) -0.0014(3) 0.06936(14) 0.0569(18) Uani 1 1 d . . . H69A H 0.9468 -0.0298 0.0709 0.068 Uiso 1 1 calc R . . H69B H 0.7567 -0.0267 0.0798 0.068 Uiso 1 1 calc R . . C70 C 0.6719(8) -0.0446(3) 0.00877(17) 0.067(2) Uani 1 1 d . . . H70A H 0.6173 -0.0248 -0.0125 0.080 Uiso 1 1 calc R . . H70B H 0.5879 -0.0561 0.0266 0.080 Uiso 1 1 calc R . . C71 C 1.0408(7) 0.1450(3) 0.04677(15) 0.0568(18) Uani 1 1 d . . . H71A H 1.1179 0.1746 0.0674 0.068 Uiso 1 1 calc R . . H71B H 1.0178 0.1755 0.0270 0.068 Uiso 1 1 calc R . . C72 C 1.2559(8) 0.1127(3) 0.00670(16) 0.0622(19) Uani 1 1 d . . . H72A H 1.3412 0.1477 0.0229 0.075 Uiso 1 1 calc R . . H72B H 1.2092 0.1356 -0.0143 0.075 Uiso 1 1 calc R . . C73 C 0.1521(6) 0.4360(3) -0.00779(14) 0.0421(15) Uani 1 1 d . . . H73A H 0.1548 0.4711 0.0157 0.051 Uiso 1 1 calc R . . H73B H 0.0384 0.4281 -0.0209 0.051 Uiso 1 1 calc R . . C74 C 0.2577(7) 0.3365(3) -0.03559(15) 0.0585(17) Uani 1 1 d . . . H74A H 0.1760 0.2952 -0.0477 0.070 Uiso 1 1 calc R . . H74B H 0.3665 0.3194 -0.0310 0.070 Uiso 1 1 calc R . . C75 C 0.2720(7) 0.3944(3) -0.06104(14) 0.0541(17) Uani 1 1 d . . . H75A H 0.3749 0.3944 -0.0743 0.065 Uiso 1 1 calc R . . H75B H 0.1750 0.3879 -0.0803 0.065 Uiso 1 1 calc R . . C76 C 0.2405(6) 0.5224(3) -0.05234(14) 0.0442(15) Uani 1 1 d . . . H76A H 0.1867 0.5559 -0.0349 0.053 Uiso 1 1 calc R . . H76B H 0.1624 0.5050 -0.0754 0.053 Uiso 1 1 calc R . . C77 C 0.3214(6) 0.3770(3) 0.03343(15) 0.0515(16) Uani 1 1 d . . . H77A H 0.3329 0.3286 0.0399 0.062 Uiso 1 1 calc R . . H77B H 0.2777 0.4042 0.0555 0.062 Uiso 1 1 calc R . . C78 C 0.6013(7) 0.4386(3) 0.06372(14) 0.0487(16) Uani 1 1 d . . . H78A H 0.6259 0.3972 0.0764 0.058 Uiso 1 1 calc R . . H78B H 0.5472 0.4713 0.0816 0.058 Uiso 1 1 calc R . . N1 N 1.4430(5) 0.8256(2) 0.28625(11) 0.0409(12) Uani 1 1 d . . . N2 N 1.5414(5) 0.7112(2) 0.27192(11) 0.0370(11) Uani 1 1 d . . . N3 N 1.5098(5) 0.7846(2) 0.22333(11) 0.0337(11) Uani 1 1 d . . . N4 N 1.4679(5) 0.7484(2) 0.33080(11) 0.0471(13) Uani 1 1 d . . . H4A H 1.5049 0.7084 0.3353 0.057 Uiso 1 1 calc R . . N5 N 1.6214(5) 0.6818(2) 0.21066(11) 0.0372(11) Uani 1 1 d . . . H5B H 1.6072 0.6923 0.1873 0.045 Uiso 1 1 calc R . . N6 N 1.3950(5) 0.8892(2) 0.23775(11) 0.0380(12) Uani 1 1 d . . . H6B H 1.3652 0.9192 0.2564 0.046 Uiso 1 1 calc R . . N7 N 0.0511(5) 0.7346(2) 0.25606(11) 0.0403(12) Uani 1 1 d . B . N8 N 0.0048(5) 0.7832(2) 0.19819(11) 0.0361(11) Uani 1 1 d . . . N9 N -0.0624(5) 0.8453(2) 0.25681(11) 0.0380(11) Uani 1 1 d . B . N10 N 0.1308(5) 0.67944(19) 0.20114(11) 0.0350(11) Uani 1 1 d . . . H10A H 0.1533 0.6476 0.2159 0.042 Uiso 1 1 calc R . . N11 N -0.0999(5) 0.8871(2) 0.19940(12) 0.0461(13) Uani 1 1 d . . . H11A H -0.0823 0.8781 0.1751 0.055 Uiso 1 1 calc R . . N22 N 0.8086(5) 0.0083(2) 0.02875(13) 0.0514(13) Uani 1 1 d . . . N23 N 0.8871(6) 0.1220(2) 0.06224(13) 0.0575(14) Uani 1 1 d . . . N24 N 1.1224(5) 0.0843(2) 0.02970(12) 0.0485(13) Uani 1 1 d . . . H24 H 1.1793 0.0699 0.0504 0.058 Uiso 1 1 d R . . N25 N 0.2765(5) 0.4622(2) -0.03350(11) 0.0446(12) Uani 1 1 d . . . N26 N 0.2016(6) 0.3693(2) 0.00124(12) 0.0515(14) Uani 1 1 d . . . N27 N 0.4932(5) 0.4141(2) 0.02857(11) 0.0424(12) Uani 1 1 d . . . H27 H 0.5451 0.3792 0.0148 0.051 Uiso 1 1 d R . . Ni1 Ni 0.9851(3) 1.0013(2) 0.49812(10) 0.0429(4) Uani 0.50 1 d P . . Ni3 Ni 1.0000 0.0000 0.0000 0.0464(3) Uani 1 2 d S . . Ni4 Ni 0.5000 0.5000 0.0000 0.0366(2) Uani 1 2 d S . . O1 O 1.1408(4) 0.9370(2) 0.46241(10) 0.0536(11) Uani 1 1 d . . . O2 O 1.1963(5) 0.8450(2) 0.49120(11) 0.0679(13) Uani 1 1 d . . . O3 O 2.0463(5) 0.4275(2) 0.24070(13) 0.0803(15) Uani 1 1 d . . . O4 O 2.0018(5) 0.40892(19) 0.17835(13) 0.0655(13) Uani 1 1 d . . . O5 O 1.3223(5) 0.9409(2) 0.06300(10) 0.0617(13) Uani 1 1 d . . . O6 O 1.2926(6) 1.0483(2) 0.09256(11) 0.0741(14) Uani 1 1 d . . . O7 O 0.3236(5) 0.6565(2) 0.02845(10) 0.0617(11) Uani 1 1 d . . . O8 O 0.3655(4) 0.54767(17) 0.04319(9) 0.0423(10) Uani 1 1 d . . . O9 O -0.4547(4) 1.17257(18) 0.20392(11) 0.0520(11) Uani 1 1 d . . . O10 O -0.4295(5) 1.1649(2) 0.26580(11) 0.0690(13) Uani 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 Ni2 0.0289(4) 0.0224(4) 0.0416(5) 0.0111(4) 0.0128(4) 0.0033(3) Ni2' 0.0328(17) 0.0241(16) 0.0453(19) 0.0209(14) 0.0213(14) -0.0018(14) N12 0.045(2) 0.0418(19) 0.046(2) -0.0090(18) 0.0114(18) 0.0139(18) N12' 0.045(2) 0.0418(19) 0.046(2) -0.0090(18) 0.0114(18) 0.0139(18) C1 0.039(3) 0.049(3) 0.030(3) -0.003(2) 0.014(2) 0.004(3) C2 0.030(3) 0.035(3) 0.034(3) -0.010(2) 0.008(2) 0.003(2) C3 0.042(3) 0.025(2) 0.034(3) -0.005(2) 0.010(2) -0.007(2) C4 0.037(3) 0.042(3) 0.047(3) -0.005(3) 0.016(2) 0.009(2) C5 0.045(3) 0.046(3) 0.043(3) -0.009(3) 0.011(3) 0.016(3) C6 0.052(3) 0.047(3) 0.041(3) -0.005(3) 0.021(3) 0.005(3) C7 0.054(3) 0.039(3) 0.042(3) -0.013(3) 0.018(3) 0.001(3) C8 0.090(4) 0.071(4) 0.035(3) 0.008(3) 0.028(3) 0.018(4) C9 0.066(4) 0.049(3) 0.055(3) 0.003(3) 0.022(3) 0.027(3) C10 0.061(3) 0.050(3) 0.035(3) -0.004(3) 0.022(3) -0.001(3) C11 0.033(3) 0.023(2) 0.052(3) -0.002(2) 0.016(2) -0.002(2) C12 0.034(3) 0.034(3) 0.051(3) -0.005(2) 0.012(2) 0.005(2) C13 0.031(3) 0.030(3) 0.059(3) 0.005(3) 0.007(3) -0.005(2) C14 0.021(2) 0.029(3) 0.066(3) -0.002(2) 0.016(2) -0.004(2) C15 0.041(3) 0.041(3) 0.050(3) -0.006(3) 0.021(3) -0.003(3) C16 0.048(3) 0.026(2) 0.046(3) 0.001(2) 0.014(3) 0.013(2) C17 0.015(2) 0.056(3) 0.100(5) 0.000(3) 0.008(3) 0.018(2) C18 0.040(3) 0.031(3) 0.046(3) -0.002(2) -0.001(3) 0.003(2) C19 0.088(4) 0.043(3) 0.050(3) 0.000(3) 0.016(3) 0.027(3) C20 0.065(4) 0.050(3) 0.053(3) 0.005(3) 0.012(3) 0.027(3) C21 0.039(3) 0.042(3) 0.042(3) 0.003(3) -0.008(3) 0.006(3) C22 0.052(3) 0.049(3) 0.056(4) -0.006(3) -0.004(3) 0.017(3) C23 0.039(3) 0.043(3) 0.049(3) -0.009(3) -0.001(3) 0.006(3) C24 0.039(3) 0.057(3) 0.054(3) -0.007(3) -0.012(3) 0.016(3) C25 0.035(3) 0.033(3) 0.046(3) -0.016(2) 0.011(2) -0.005(2) C26 0.029(2) 0.030(2) 0.040(3) -0.001(2) 0.008(2) 0.013(2) C27 0.048(3) 0.038(3) 0.032(3) -0.013(2) 0.005(2) -0.004(3) C28 0.034(3) 0.032(3) 0.038(3) -0.005(2) 0.010(2) 0.001(2) C29 0.084(4) 0.028(3) 0.054(3) 0.004(2) 0.034(3) 0.031(3) C30 0.068(3) 0.047(3) 0.043(3) 0.015(2) 0.024(3) 0.035(3) C31 0.029(2) 0.037(3) 0.040(3) 0.001(2) 0.009(2) 0.027(2) C32 0.049(3) 0.040(3) 0.037(3) -0.006(2) 0.008(3) 0.017(3) C33 0.057(3) 0.028(2) 0.047(3) 0.008(2) 0.025(3) 0.021(2) C34 0.045(3) 0.060(3) 0.033(3) -0.001(3) 0.010(2) 0.021(3) C35 0.031(3) 0.027(2) 0.046(3) -0.007(2) 0.013(2) 0.008(2) C36 0.062(3) 0.028(3) 0.046(3) 0.001(2) 0.019(3) 0.012(3) C37 0.032(3) 0.037(3) 0.048(3) -0.002(2) 0.006(2) 0.010(2) C38 0.027(3) 0.030(2) 0.053(3) -0.012(2) 0.000(2) 0.012(2) C39 0.048(3) 0.047(3) 0.036(3) -0.009(3) 0.013(3) 0.009(3) C40 0.057(3) 0.032(3) 0.042(3) -0.001(2) 0.009(3) 0.015(3) C41 0.023(3) 0.036(3) 0.064(4) -0.008(3) 0.004(3) 0.007(2) C67 0.069(4) 0.059(3) 0.063(4) 0.008(3) 0.007(3) 0.053(3) C68 0.093(4) 0.066(4) 0.038(3) 0.000(3) 0.007(3) 0.044(3) C69 0.064(4) 0.071(4) 0.041(3) 0.011(3) 0.013(3) 0.021(3) C70 0.073(4) 0.073(4) 0.058(4) 0.007(3) 0.012(3) 0.024(4) C71 0.081(4) 0.050(3) 0.042(3) 0.000(3) 0.016(3) 0.022(3) C72 0.070(4) 0.059(4) 0.053(4) 0.006(3) -0.008(3) 0.003(3) C73 0.040(3) 0.050(3) 0.039(3) 0.000(2) 0.014(2) 0.019(3) C74 0.062(3) 0.060(3) 0.054(4) -0.014(3) -0.003(3) 0.041(3) C75 0.041(3) 0.074(4) 0.040(3) -0.024(3) -0.006(3) 0.020(3) C76 0.043(3) 0.063(3) 0.032(3) -0.001(3) 0.001(2) 0.035(3) C77 0.051(3) 0.053(3) 0.059(3) 0.010(3) 0.018(3) 0.028(3) C78 0.070(4) 0.054(3) 0.027(3) 0.011(2) -0.002(3) 0.027(3) N1 0.048(3) 0.035(2) 0.039(2) -0.002(2) 0.013(2) 0.007(2) N2 0.049(2) 0.035(2) 0.028(2) 0.0008(18) 0.0086(19) 0.008(2) N3 0.028(2) 0.030(2) 0.043(2) -0.0010(19) 0.0114(19) 0.0056(18) N4 0.066(3) 0.043(2) 0.036(2) -0.003(2) 0.017(2) 0.026(2) N5 0.047(2) 0.033(2) 0.030(2) -0.0014(18) 0.0076(19) 0.004(2) N6 0.042(2) 0.031(2) 0.038(2) -0.0079(19) 0.009(2) 0.003(2) N7 0.046(2) 0.032(2) 0.041(2) -0.0012(19) 0.010(2) -0.003(2) N8 0.033(2) 0.031(2) 0.046(2) -0.0035(19) 0.0150(19) 0.0166(18) N9 0.039(2) 0.033(2) 0.045(2) 0.000(2) 0.010(2) 0.0182(19) N10 0.041(2) 0.0209(19) 0.044(2) -0.0011(18) 0.017(2) 0.0059(18) N11 0.054(3) 0.040(2) 0.046(3) -0.009(2) 0.015(2) 0.020(2) N22 0.042(2) 0.059(3) 0.058(3) 0.001(2) 0.003(2) 0.031(2) N23 0.073(3) 0.058(3) 0.047(3) 0.001(2) 0.003(3) 0.039(3) N24 0.059(3) 0.053(3) 0.037(2) 0.004(2) -0.002(2) 0.030(2) N25 0.056(3) 0.041(2) 0.038(2) -0.002(2) -0.004(2) 0.030(2) N26 0.056(3) 0.052(3) 0.047(3) -0.004(2) 0.002(2) 0.023(2) N27 0.045(2) 0.053(2) 0.036(2) 0.001(2) 0.004(2) 0.039(2) Ni1 0.0429(8) 0.0510(6) 0.0337(6) -0.0074(5) 0.0168(6) 0.0090(7) Ni3 0.0584(6) 0.0529(6) 0.0315(5) -0.0012(4) 0.0020(5) 0.0319(5) Ni4 0.0429(5) 0.0423(5) 0.0276(5) -0.0030(4) 0.0030(4) 0.0269(4) O1 0.057(2) 0.052(2) 0.052(2) -0.0059(19) 0.0273(18) 0.0107(19) O2 0.095(3) 0.061(2) 0.053(2) 0.001(2) 0.036(2) 0.022(2) O3 0.059(3) 0.101(3) 0.095(3) 0.032(3) 0.014(2) 0.042(2) O4 0.050(2) 0.042(2) 0.104(3) -0.010(2) 0.012(2) 0.0220(19) O5 0.071(3) 0.058(2) 0.051(2) 0.002(2) 0.006(2) -0.005(2) O6 0.111(3) 0.059(2) 0.054(2) 0.001(2) -0.024(2) 0.042(2) O7 0.087(2) 0.072(2) 0.044(2) 0.0152(19) 0.028(2) 0.061(2) O8 0.0404(19) 0.0443(19) 0.043(2) -0.0091(16) 0.0066(16) 0.0236(16) O9 0.053(2) 0.0384(19) 0.064(2) 0.0006(19) -0.002(2) 0.0162(18) O10 0.081(3) 0.068(2) 0.061(3) -0.015(2) 0.009(2) 0.047(2) _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 Ni5 Ni5 0.457(5) 2_666 ? Ni5 N30 1.864(9) . ? Ni5 N28 1.989(10) . ? Ni5 O14 2.054(12) 2_666 ? Ni5 N28 2.146(10) 2_666 ? Ni5 O14 2.218(11) . ? Ni5 N30 2.232(9) 2_666 ? Ni5 O13 2.332(11) . ? C82 N28 1.446(9) . ? C82 C84 1.474(10) 2_666 ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? N28 C81 1.506(10) . ? N28 C79 1.583(10) . ? N28 Ni5 2.146(10) 2_666 ? C79 N29 1.489(10) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? N29 C83 1.503(10) . ? N29 C80 1.536(10) . ? C80 C81 1.549(10) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C83 N30 1.451(10) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? N30 C84 1.491(10) . ? N30 Ni5 2.232(9) 2_666 ? N30 H30 0.9300 . ? C84 C82 1.474(10) 2_666 ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? O13 O14 0.977(19) 2_666 ? O14 O13 0.977(19) 2_666 ? O14 Ni5 2.054(12) 2_666 ? C52 N13 1.439(8) . ? C52 C54 1.612(9) 2_776 ? C52 H52A 0.9599 . ? C52 H52B 0.9599 . ? C52 H52C 0.9599 . ? C52 H15E 1.2133 . ? N13 C49 1.488(8) . ? N13 C51 1.501(8) . ? N13 Ni1 2.035(6) . ? N13 Ni1 2.263(6) 2_776 ? C49 N14 1.469(8) . ? C49 H49A 0.9601 . ? C49 H49B 0.9599 . ? C49 H15F 1.0826 . ? C49 H15G 1.1307 . ? N14 C53 1.475(8) . ? N14 C50 1.518(8) . ? N14 H15A 1.0364 . ? N14 H15C 0.7701 . ? C50 C51 1.564(9) . ? C50 H50A 0.9600 . ? C50 H50B 0.9601 . ? C50 H15A 0.6968 . ? C50 H15B 1.1405 . ? C51 H51A 0.9599 . ? C51 H51B 0.9599 . ? C51 H14A 0.8252 . ? C53 N15 1.486(9) . ? C53 H53A 0.9599 . ? C53 H53B 0.9599 . ? C53 H15C 0.7488 . ? N15 C54 1.490(9) . ? N15 Ni1 1.884(8) 2_776 ? N15 Ni1 2.025(8) . ? N15 H15X 0.9001 . ? C54 C52 1.612(9) 2_776 ? C54 H54A 0.9599 . ? C54 H54B 0.9600 . ? C54 H54C 0.9599 . ? C152 N113 1.439(12) . ? C152 C154 1.578(12) 2_776 ? C152 H15A 0.9599 . ? C152 H15B 0.9600 . ? C152 H15C 0.9600 . ? N113 C151 1.528(12) . ? N113 C149 1.529(11) . ? N113 Ni1 1.953(10) . ? N113 Ni1 2.132(10) 2_776 ? C149 N114 1.488(12) . ? C149 H51A 0.9017 . ? C149 H51B 1.2224 . ? C149 H14A 0.9600 . ? C149 H14B 0.9600 . ? N114 C150 1.501(12) . ? N114 C153 1.513(12) . ? N114 H52A 1.1577 . ? N114 H52C 0.8607 . ? C150 C151 1.567(13) . ? C150 H52A 0.5612 . ? C150 H52B 1.1213 . ? C150 H15D 0.9601 . ? C150 H15E 0.9599 . ? C151 H49A 0.9690 . ? C151 H15F 0.9600 . ? C151 H15G 0.9599 . ? C153 N115 1.475(13) . ? C153 H52C 0.8087 . ? C153 H15H 0.9600 . ? C153 H15W 0.9599 . ? N115 C154 1.455(13) . ? N115 Ni1 2.123(15) . ? N115 Ni1 2.293(15) 2_776 ? N115 H11C 0.8999 . ? C154 C152 1.578(12) 2_776 ? C154 H15I 0.9600 . ? C154 H15J 0.9601 . ? C154 H15K 0.9598 . ? Ni2 N19 1.883(5) . ? Ni2 N21 1.890(5) . ? Ni2 N18 1.908(5) . ? Ni2 N16 1.969(5) . ? C62 N16 1.468(7) . ? C62 C61 1.527(7) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? N16 C55 1.484(7) . ? N16 C63 1.500(7) . ? C55 N17 1.481(7) . ? C55 H55A 0.9599 . ? C55 H55B 0.9599 . ? C55 H16O 1.1074 . ? N17 C64 1.474(7) . ? N17 C56 1.483(7) . ? N17 H16M 0.8825 . ? N17 H16O 0.8039 . ? C64 C63 1.564(8) . ? C64 H64A 0.9601 . ? C64 H64B 0.9601 . ? C64 H16A 1.0136 . ? C63 H63A 0.9599 . ? C63 H63B 0.9600 . ? C63 H16A 0.8294 . ? C56 N18 1.482(7) . ? C56 H56A 0.9599 . ? C56 H56B 0.9601 . ? C56 H16K 1.2804 . ? N18 C57 1.506(7) . ? N18 H18A 0.9000 . ? N18 H12D 1.2253 . ? C57 C58 1.521(8) . ? C57 H57A 0.9599 . ? C57 H57B 0.9600 . ? C58 N19 1.466(7) . ? C58 H58A 0.9599 . ? C58 H58B 0.9601 . ? C58 H16I 1.1723 . ? N19 C65 1.465(7) . ? N19 C59 1.538(7) . ? C59 N20 1.460(7) . ? C59 H59A 0.9602 . ? C59 H59B 0.9601 . ? C59 H15Q 0.8394 . ? N20 C60 1.422(7) . ? N20 C66 1.490(7) . ? N20 H15P 0.8801 . ? N20 H15Q 0.7315 . ? C66 C65 1.552(8) . ? C66 H66A 0.9600 . ? C66 H66B 0.9601 . ? C66 H15P 1.0608 . ? C65 H65A 0.9600 . ? C65 H65B 0.9599 . ? C65 H15R 0.8133 . ? C65 H15S 1.0848 . ? C60 N21 1.495(7) . ? C60 H60A 0.9599 . ? C60 H60B 0.9600 . ? C60 H15O 1.2124 . ? N21 C61 1.464(7) . ? N21 H21A 0.9002 . ? N21 H11B 1.0368 . ? C61 H61A 0.9600 . ? C61 H61B 0.9599 . ? Ni2' N116 1.766(13) . ? Ni2' N121 1.889(18) . ? Ni2' N119 2.044(13) . ? Ni2' N118 2.069(16) . ? Ni2' H18A 1.9805 . ? C162 N116 1.496(13) . ? C162 C161 1.566(12) . ? C162 H16A 0.9600 . ? C162 H16B 0.9599 . ? N116 C163 1.469(13) . ? N116 C155 1.497(12) . ? C155 N117 1.486(13) . ? C155 H61B 1.1625 . ? C155 H15L 0.9600 . ? C155 H15M 0.9600 . ? N117 C156 1.477(13) . ? N117 C164 1.486(13) . ? N117 H61A 1.0298 . ? N117 H61B 0.6379 . ? C164 C163 1.551(12) . ? C164 H62A 1.0831 . ? C164 H16C 0.9600 . ? C164 H16D 0.9602 . ? C163 H62A 0.8574 . ? C163 H16E 0.9600 . ? C163 H16F 0.9602 . ? C156 N118 1.481(14) . ? C156 H15N 0.9598 . ? C156 H15O 0.9601 . ? N118 C157 1.512(14) . ? N118 H21A 0.9822 . ? N118 H11B 0.9000 . ? C157 C158 1.540(12) . ? C157 H15P 0.9601 . ? C157 H15Q 0.9600 . ? C158 N119 1.502(12) . ? C158 H65A 1.1385 . ? C158 H65B 1.2435 . ? C158 H15R 0.9600 . ? C158 H15S 0.9601 . ? N119 C159 1.490(12) . ? N119 C165 1.491(13) . ? C159 N120 1.487(13) . ? C159 H57B 1.0117 . ? C159 H15T 0.9599 . ? C159 H15U 0.9601 . ? N120 C160 1.484(13) . ? N120 C166 1.495(13) . ? N120 H57A 1.0238 . ? N120 H57B 0.6028 . ? C166 C165 1.553(13) . ? C166 H57A 1.1106 . ? C166 H16G 0.9600 . ? C166 H16H 0.9600 . ? C165 H58A 0.8035 . ? C165 H58B 1.1396 . ? C165 H16I 0.9601 . ? C165 H16J 0.9601 . ? C160 N121 1.433(14) . ? C160 H56B 1.2838 . ? C160 H16K 0.9600 . ? C160 H16L 0.9601 . ? N121 C161 1.533(14) . ? N121 H18A 0.9199 . ? N121 H12D 0.9001 . ? C161 H16M 0.9601 . ? C161 H16O 0.9600 . ? N12 C27 1.343(6) . ? N12 C42 1.458(10) . ? N12 H12A 0.8999 . ? N12 H12B 0.9328 . ? C42 C43 1.389(11) . ? C42 C47 1.413(11) . ? C43 C44 1.364(12) . ? C43 H43A 0.9599 . ? C43 H43B 1.2654 . ? C44 C45 1.381(11) . ? C44 H44A 0.9598 . ? C44 H44B 1.1250 . ? C45 C46 1.394(11) . ? C45 C48 1.480(11) . ? C46 C47 1.365(12) . ? C46 H46A 0.9599 . ? C46 H46B 0.9065 . ? C47 H47A 0.9600 . ? C47 H47B 0.9089 . ? C48 O11 1.287(10) . ? C48 O12 1.289(11) . ? C42' C43' 1.363(9) . ? C42' C47' 1.395(9) . ? C43' C44' 1.351(10) . ? C43' H43A 0.8469 . ? C43' H43B 0.9600 . ? C44' C45' 1.378(9) . ? C44' H44A 0.9483 . ? C44' H44B 0.9601 . ? C45' C46' 1.395(9) . ? C45' C48' 1.481(10) . ? C46' C47' 1.362(10) . ? C46' H46B 0.9601 . ? C47' H47A 1.0917 . ? C47' H47B 0.9601 . ? C48' O12' 1.285(9) . ? C48' O11' 1.292(9) . ? C1 N1 1.325(6) . ? C1 N4 1.354(6) . ? C1 N2 1.358(6) . ? C2 N2 1.313(6) . ? C2 N3 1.351(6) . ? C2 N5 1.365(6) . ? C3 N3 1.302(6) . ? C3 N1 1.340(6) . ? C3 N6 1.387(6) . ? C4 C5 1.366(7) . ? C4 N4 1.413(6) . ? C4 C9 1.417(8) . ? C5 C6 1.397(7) . ? C5 H5A 0.9500 . ? C6 C7 1.363(7) . ? C6 H6A 0.9500 . ? C7 C8 1.369(8) . ? C7 C10 1.484(7) . ? C8 C9 1.391(7) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 O1 1.229(6) . ? C10 O2 1.273(6) . ? C11 C16 1.388(7) . ? C11 C12 1.393(7) . ? C11 N5 1.393(6) . ? C12 C13 1.377(7) . ? C12 H12C 0.9500 . ? C13 C14 1.405(7) . ? C13 H13B 0.9500 . ? C14 C15 1.379(7) . ? C14 C17 1.516(7) . ? C15 C16 1.389(7) . ? C15 H15V 0.9500 . ? C16 H16N 0.9500 . ? C17 O3 1.225(7) . ? C17 O4 1.269(7) . ? C18 N6 1.372(6) . ? C18 C19 1.383(7) . ? C18 C23 1.408(7) . ? C19 C20 1.394(8) . ? C19 H19A 0.9500 . ? C20 C21 1.389(7) . ? C20 H20A 0.9500 . ? C21 C22 1.393(7) . ? C21 C24 1.465(8) . ? C22 C23 1.371(8) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 O5 1.256(6) . ? C24 O6 1.274(7) . ? C25 N8 1.312(6) . ? C25 N7 1.348(6) . ? C25 N10 1.384(6) . ? C26 N9 1.297(6) . ? C26 N11 1.329(6) . ? C26 N8 1.374(6) . ? C27 N9 1.339(6) . ? C27 N7 1.364(6) . ? C28 C29 1.378(7) . ? C28 C33 1.392(6) . ? C28 N10 1.408(6) . ? C29 C30 1.429(7) . ? C29 H29A 0.9500 . ? C30 C31 1.376(7) . ? C30 H30A 0.9500 . ? C31 C32 1.347(7) . ? C31 C34 1.543(7) . ? C32 C33 1.389(7) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 O8 1.252(6) . ? C34 O7 1.272(6) . ? C35 C36 1.349(7) . ? C35 C40 1.408(7) . ? C35 N11 1.443(6) . ? C36 C37 1.383(7) . ? C36 H36A 0.9500 . ? C37 C38 1.385(7) . ? C37 H37A 0.9500 . ? C38 C39 1.415(7) . ? C38 C41 1.515(7) . ? C39 C40 1.378(7) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 O9 1.242(6) . ? C41 O10 1.283(6) . ? C67 N23 1.466(7) . ? C67 N22 1.486(7) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N23 1.495(7) . ? C68 C69 1.503(7) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 N22 1.501(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 N22 1.473(7) . ? C70 C72 1.534(8) 2_755 ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N23 1.445(7) . ? C71 N24 1.480(7) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 N24 1.498(7) . ? C72 C70 1.534(8) 2_755 ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 N26 1.444(7) . ? C73 N25 1.496(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 N26 1.496(7) . ? C74 C75 1.514(8) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 N25 1.501(6) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 N25 1.451(6) . ? C76 C78 1.515(7) 2_665 ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 N26 1.427(7) . ? C77 N27 1.519(6) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 N27 1.459(6) . ? C78 C76 1.515(7) 2_665 ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? N4 H4A 0.8800 . ? N5 H5B 0.8800 . ? N6 H6B 0.8800 . ? N10 H10A 0.8800 . ? N11 H11A 0.8800 . ? N22 Ni3 1.933(4) . ? N24 Ni3 1.913(4) . ? N24 H24 0.9300 . ? N25 Ni4 2.091(4) . ? N27 Ni4 2.032(4) . ? N27 H27 0.9299 . ? Ni1 Ni1 0.281(6) 2_776 ? Ni1 N15 1.884(8) 2_776 ? Ni1 O1 2.106(5) 2_776 ? Ni1 N113 2.132(10) 2_776 ? Ni1 O1 2.211(5) . ? Ni1 N13 2.263(7) 2_776 ? Ni1 N115 2.293(15) 2_776 ? Ni3 N24 1.913(4) 2_755 ? Ni3 N22 1.933(4) 2_755 ? Ni4 N27 2.032(4) 2_665 ? Ni4 N25 2.091(4) 2_665 ? Ni4 O8 2.115(3) . ? Ni4 O8 2.115(3) 2_665 ? O1 Ni1 2.106(5) 2_776 ? 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 Ni5 Ni5 N30 139.7(9) 2_666 . ? Ni5 Ni5 N28 104.1(9) 2_666 . ? N30 Ni5 N28 101.4(3) . . ? Ni5 Ni5 O14 105.3(9) 2_666 2_666 ? N30 Ni5 O14 104.3(5) . 2_666 ? N28 Ni5 O14 92.1(5) . 2_666 ? Ni5 Ni5 N28 64.0(8) 2_666 2_666 ? N30 Ni5 N28 88.8(3) . 2_666 ? N28 Ni5 N28 168.09(15) . 2_666 ? O14 Ni5 N28 91.3(5) 2_666 2_666 ? Ni5 Ni5 O14 63.3(8) 2_666 . ? N30 Ni5 O14 85.9(5) . . ? N28 Ni5 O14 91.0(5) . . ? O14 Ni5 O14 168.54(15) 2_666 . ? N28 Ni5 O14 83.6(4) 2_666 . ? Ni5 Ni5 N30 32.7(8) 2_666 2_666 ? N30 Ni5 N30 172.40(17) . 2_666 ? N28 Ni5 N30 83.4(3) . 2_666 ? O14 Ni5 N30 81.2(5) 2_666 2_666 ? N28 Ni5 N30 85.9(3) 2_666 2_666 ? O14 Ni5 N30 88.2(4) . 2_666 ? Ni5 Ni5 O13 115.2(9) 2_666 . ? N30 Ni5 O13 83.8(4) . . ? N28 Ni5 O13 109.9(5) . . ? O14 Ni5 O13 24.7(5) 2_666 . ? N28 Ni5 O13 77.0(5) 2_666 . ? O14 Ni5 O13 158.2(6) . . ? N30 Ni5 O13 100.2(4) 2_666 . ? N28 C82 C84 113.7(7) . 2_666 ? N28 C82 H82A 108.8 . . ? C84 C82 H82A 108.8 2_666 . ? N28 C82 H82B 108.8 . . ? C84 C82 H82B 108.8 2_666 . ? H82A C82 H82B 107.7 . . ? C82 N28 C81 115.4(8) . . ? C82 N28 C79 112.0(7) . . ? C81 N28 C79 107.2(6) . . ? C82 N28 Ni5 108.5(6) . . ? C81 N28 Ni5 112.8(7) . . ? C79 N28 Ni5 100.0(6) . . ? C82 N28 Ni5 96.8(5) . 2_666 ? C81 N28 Ni5 122.0(7) . 2_666 ? C79 N28 Ni5 102.7(6) . 2_666 ? Ni5 N28 Ni5 11.91(15) . 2_666 ? N29 C79 N28 95.5(6) . . ? N29 C79 H79A 112.6 . . ? N28 C79 H79A 112.6 . . ? N29 C79 H79B 112.6 . . ? N28 C79 H79B 112.6 . . ? H79A C79 H79B 110.1 . . ? C79 N29 C83 113.3(7) . . ? C79 N29 C80 113.7(6) . . ? C83 N29 C80 113.1(7) . . ? N29 C80 C81 102.8(6) . . ? N29 C80 H80A 111.2 . . ? C81 C80 H80A 111.2 . . ? N29 C80 H80B 111.2 . . ? C81 C80 H80B 111.2 . . ? H80A C80 H80B 109.1 . . ? N28 C81 C80 102.3(6) . . ? N28 C81 H81A 111.3 . . ? C80 C81 H81A 111.3 . . ? N28 C81 H81B 111.3 . . ? C80 C81 H81B 111.3 . . ? H81A C81 H81B 109.2 . . ? N30 C83 N29 105.1(7) . . ? N30 C83 H83A 110.7 . . ? N29 C83 H83A 110.7 . . ? N30 C83 H83B 110.7 . . ? N29 C83 H83B 110.7 . . ? H83A C83 H83B 108.8 . . ? C83 N30 C84 115.7(7) . . ? C83 N30 Ni5 123.9(6) . . ? C84 N30 Ni5 109.4(5) . . ? C83 N30 Ni5 125.7(6) . 2_666 ? C84 N30 Ni5 103.2(5) . 2_666 ? Ni5 N30 Ni5 7.60(17) . 2_666 ? C83 N30 H30 101.1 . . ? C84 N30 H30 101.1 . . ? Ni5 N30 H30 101.1 . . ? Ni5 N30 H30 107.0 2_666 . ? C82 C84 N30 106.5(7) 2_666 . ? C82 C84 H84A 110.4 2_666 . ? N30 C84 H84A 110.4 . . ? C82 C84 H84B 110.4 2_666 . ? N30 C84 H84B 110.4 . . ? H84A C84 H84B 108.6 . . ? O14 O13 Ni5 61.5(9) 2_666 . ? O13 O14 Ni5 93.8(11) 2_666 2_666 ? O13 O14 Ni5 99.0(11) 2_666 . ? Ni5 O14 Ni5 11.46(14) 2_666 . ? N13 C52 C54 108.7(6) . 2_776 ? N13 C52 H52A 109.1 . . ? C54 C52 H52A 126.6 2_776 . ? N13 C52 H52B 109.4 . . ? C54 C52 H52B 91.6 2_776 . ? H52A C52 H52B 109.5 . . ? N13 C52 H52C 109.8 . . ? C54 C52 H52C 20.3 2_776 . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N13 C52 H15E 129.9 . . ? C54 C52 H15E 103.0 2_776 . ? H52A C52 H15E 79.5 . . ? H52B C52 H15E 31.3 . . ? H52C C52 H15E 113.1 . . ? C52 N13 C49 113.9(5) . . ? C52 N13 C51 113.8(5) . . ? C49 N13 C51 104.5(5) . . ? C52 N13 Ni1 102.6(4) . . ? C49 N13 Ni1 105.7(4) . . ? C51 N13 Ni1 116.4(5) . . ? C52 N13 Ni1 106.5(4) . 2_776 ? C49 N13 Ni1 105.5(4) . 2_776 ? C51 N13 Ni1 112.4(5) . 2_776 ? Ni1 N13 Ni1 4.4(2) . 2_776 ? N14 C49 N13 102.7(5) . . ? N14 C49 H49A 109.8 . . ? N13 C49 H49A 109.9 . . ? N14 C49 H49B 111.8 . . ? N13 C49 H49B 112.5 . . ? H49A C49 H49B 109.9 . . ? N14 C49 H15F 150.0 . . ? N13 C49 H15F 93.5 . . ? H49A C49 H15F 87.5 . . ? H49B C49 H15F 38.2 . . ? N14 C49 H15G 112.4 . . ? N13 C49 H15G 97.4 . . ? H49A C49 H15G 12.6 . . ? H49B C49 H15G 118.1 . . ? H15F C49 H15G 90.0 . . ? C49 N14 C53 113.8(6) . . ? C49 N14 C50 106.5(5) . . ? C53 N14 C50 110.9(6) . . ? C49 N14 H15A 108.6 . . ? C53 N14 H15A 126.6 . . ? C50 N14 H15A 23.2 . . ? C49 N14 H15C 109.9 . . ? C53 N14 H15C 13.6 . . ? C50 N14 H15C 100.8 . . ? H15A N14 H15C 119.7 . . ? N14 C50 C51 105.2(5) . . ? N14 C50 H50A 110.4 . . ? C51 C50 H50A 112.4 . . ? N14 C50 H50B 110.5 . . ? C51 C50 H50B 109.3 . . ? H50A C50 H50B 109.0 . . ? N14 C50 H15A 35.8 . . ? C51 C50 H15A 114.2 . . ? H50A C50 H15A 75.2 . . ? H50B C50 H15A 130.4 . . ? N14 C50 H15B 82.6 . . ? C51 C50 H15B 96.2 . . ? H50A C50 H15B 142.9 . . ? H50B C50 H15B 36.2 . . ? H15A C50 H15B 115.0 . . ? N13 C51 C50 102.2(5) . . ? N13 C51 H51A 111.8 . . ? C50 C51 H51A 113.1 . . ? N13 C51 H51B 110.1 . . ? C50 C51 H51B 110.0 . . ? H51A C51 H51B 109.5 . . ? N13 C51 H14A 122.4 . . ? C50 C51 H14A 124.9 . . ? H51A C51 H14A 80.6 . . ? H51B C51 H14A 28.9 . . ? N13 C51 H14B 90.0 . . ? C50 C51 H14B 127.8 . . ? H51A C51 H14B 23.0 . . ? H51B C51 H14B 112.8 . . ? H14A C51 H14B 85.8 . . ? N14 C53 N15 114.8(6) . . ? N14 C53 H53A 109.6 . . ? N15 C53 H53A 111.2 . . ? N14 C53 H53B 105.9 . . ? N15 C53 H53B 107.3 . . ? H53A C53 H53B 107.6 . . ? N14 C53 H15C 14.0 . . ? N15 C53 H15C 101.0 . . ? H53A C53 H15C 114.7 . . ? H53B C53 H15C 114.7 . . ? C53 N15 C54 111.4(5) . . ? C53 N15 Ni1 124.3(5) . 2_776 ? C54 N15 Ni1 106.0(5) . 2_776 ? C53 N15 Ni1 117.1(5) . . ? C54 N15 Ni1 111.0(5) . . ? Ni1 N15 Ni1 7.14(16) 2_776 . ? C53 N15 H15X 104.8 . . ? C54 N15 H15X 104.8 . . ? Ni1 N15 H15X 103.8 2_776 . ? Ni1 N15 H15X 106.6 . . ? N15 C54 C52 105.6(6) . 2_776 ? N15 C54 H54A 110.1 . . ? C52 C54 H54A 121.1 2_776 . ? N15 C54 H54B 110.5 . . ? C52 C54 H54B 11.8 2_776 . ? H54A C54 H54B 109.5 . . ? N15 C54 H54C 107.9 . . ? C52 C54 H54C 101.8 2_776 . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N113 C152 C154 108.9(9) . 2_776 ? N113 C152 H50B 118.0 . . ? C154 C152 H50B 108.2 2_776 . ? N113 C152 H15A 113.2 . . ? C154 C152 H15A 125.7 2_776 . ? H50B C152 H15A 80.6 . . ? N113 C152 H15B 105.8 . . ? C154 C152 H15B 89.9 2_776 . ? H50B C152 H15B 28.9 . . ? H15A C152 H15B 109.5 . . ? N113 C152 H15C 109.4 . . ? C154 C152 H15C 21.2 2_776 . ? H50B C152 H15C 122.4 . . ? H15A C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? C152 N113 C151 110.6(9) . . ? C152 N113 C149 111.9(8) . . ? C151 N113 C149 103.2(7) . . ? C152 N113 Ni1 109.9(6) . . ? C151 N113 Ni1 113.6(7) . . ? C149 N113 Ni1 107.6(7) . . ? C152 N113 Ni1 104.3(6) . 2_776 ? C151 N113 Ni1 118.8(7) . 2_776 ? C149 N113 Ni1 108.2(7) . 2_776 ? Ni1 N113 Ni1 6.1(2) . 2_776 ? N114 C149 N113 101.5(7) . . ? N114 C149 H51A 146.1 . . ? N113 C149 H51A 105.1 . . ? N114 C149 H51B 102.2 . . ? N113 C149 H51B 99.0 . . ? H51A C149 H51B 93.9 . . ? N114 C149 H14A 110.5 . . ? N113 C149 H14A 114.1 . . ? H51A C149 H14A 76.9 . . ? H51B C149 H14A 20.4 . . ? N114 C149 H14B 110.8 . . ? N113 C149 H14B 110.0 . . ? H51A C149 H14B 39.7 . . ? H51B C149 H14B 129.5 . . ? H14A C149 H14B 109.6 . . ? C149 N114 C150 108.8(7) . . ? C149 N114 C153 109.4(9) . . ? C150 N114 C153 108.6(8) . . ? C149 N114 H52A 111.4 . . ? C150 N114 H52A 19.4 . . ? C153 N114 H52A 122.8 . . ? C149 N114 H52C 114.0 . . ? C150 N114 H52C 85.0 . . ? C153 N114 H52C 24.2 . . ? H52A N114 H52C 100.9 . . ? N114 C150 C151 104.7(7) . . ? N114 C150 H52A 43.2 . . ? C151 C150 H52A 114.8 . . ? N114 C150 H52B 95.2 . . ? C151 C150 H52B 88.7 . . ? H52A C150 H52B 134.7 . . ? N114 C150 H15D 109.2 . . ? C151 C150 H15D 110.3 . . ? H52A C150 H15D 66.3 . . ? H52B C150 H15D 143.1 . . ? N114 C150 H15E 113.0 . . ? C151 C150 H15E 110.7 . . ? H52A C150 H15E 132.8 . . ? H52B C150 H15E 34.4 . . ? H15D C150 H15E 108.8 . . ? N113 C151 C150 103.1(7) . . ? N113 C151 H49A 111.2 . . ? C150 C151 H49A 126.8 . . ? N113 C151 H49B 89.0 . . ? C150 C151 H49B 137.4 . . ? H49A C151 H49B 83.5 . . ? N113 C151 H15F 109.0 . . ? C150 C151 H15F 111.5 . . ? H49A C151 H15F 94.4 . . ? H49B C151 H15F 28.1 . . ? N113 C151 H15G 112.2 . . ? C150 C151 H15G 111.7 . . ? H49A C151 H15G 17.0 . . ? H49B C151 H15G 100.5 . . ? H15F C151 H15G 109.2 . . ? N115 C153 N114 121.8(10) . . ? N115 C153 H52C 99.3 . . ? N114 C153 H52C 25.8 . . ? N115 C153 H15H 109.7 . . ? N114 C153 H15H 105.3 . . ? H52C C153 H15H 105.1 . . ? N115 C153 H15W 105.7 . . ? N114 C153 H15W 106.6 . . ? H52C C153 H15W 129.0 . . ? H15H C153 H15W 107.1 . . ? C154 N115 C153 114.8(10) . . ? C154 N115 Ni1 100.8(8) . . ? C153 N115 Ni1 106.2(9) . . ? C154 N115 Ni1 95.0(8) . 2_776 ? C153 N115 Ni1 108.7(9) . 2_776 ? Ni1 N115 Ni1 5.80(15) . 2_776 ? C154 N115 H11C 113.0 . . ? C153 N115 H11C 110.5 . . ? Ni1 N115 H11C 111.0 . . ? Ni1 N115 H11C 114.1 2_776 . ? N115 C154 C152 107.2(9) . 2_776 ? N115 C154 H15I 111.1 . . ? C152 C154 H15I 115.5 2_776 . ? N115 C154 H15J 107.2 . . ? C152 C154 H15J 7.1 2_776 . ? H15I C154 H15J 109.5 . . ? N115 C154 H15K 110.1 . . ? C152 C154 H15K 103.2 2_776 . ? H15I C154 H15K 109.5 . . ? H15J C154 H15K 109.5 . . ? N19 Ni2 N21 94.13(19) . . ? N19 Ni2 N18 88.11(19) . . ? N21 Ni2 N18 177.7(2) . . ? N19 Ni2 N16 178.50(19) . . ? N21 Ni2 N16 87.37(19) . . ? N18 Ni2 N16 90.39(19) . . ? N16 C62 C61 105.8(5) . . ? N16 C62 H62A 110.0 . . ? C61 C62 H62A 109.2 . . ? N16 C62 H62B 111.2 . . ? C61 C62 H62B 111.6 . . ? H62A C62 H62B 108.9 . . ? N16 C62 H16E 67.5 . . ? C61 C62 H16E 120.6 . . ? H62A C62 H16E 42.6 . . ? H62B C62 H16E 126.1 . . ? N16 C62 H16F 74.5 . . ? C61 C62 H16F 177.3 . . ? H62A C62 H16F 73.0 . . ? H62B C62 H16F 65.9 . . ? H16E C62 H16F 62.1 . . ? C62 N16 C55 109.6(4) . . ? C62 N16 C63 113.8(4) . . ? C55 N16 C63 105.4(4) . . ? C62 N16 Ni2 107.6(3) . . ? C55 N16 Ni2 111.3(3) . . ? C63 N16 Ni2 109.1(4) . . ? N17 C55 N16 103.5(4) . . ? N17 C55 H55A 110.5 . . ? N16 C55 H55A 111.0 . . ? N17 C55 H55B 111.7 . . ? N16 C55 H55B 110.9 . . ? H55A C55 H55B 109.2 . . ? N17 C55 H16O 32.3 . . ? N16 C55 H16O 122.9 . . ? H55A C55 H16O 117.5 . . ? H55B C55 H16O 80.1 . . ? C64 N17 C55 106.0(4) . . ? C64 N17 C56 111.3(5) . . ? C55 N17 C56 108.7(5) . . ? C64 N17 H16M 72.3 . . ? C55 N17 H16M 170.4 . . ? C56 N17 H16M 80.4 . . ? C64 N17 H16O 151.9 . . ? C55 N17 H16O 47.3 . . ? C56 N17 H16O 76.6 . . ? H16M N17 H16O 135.5 . . ? N17 C64 C63 105.6(4) . . ? N17 C64 H64A 109.2 . . ? C63 C64 H64A 110.0 . . ? N17 C64 H64B 111.9 . . ? C63 C64 H64B 111.5 . . ? H64A C64 H64B 108.7 . . ? N17 C64 H16A 130.5 . . ? C63 C64 H16A 28.5 . . ? H64A C64 H16A 106.7 . . ? H64B C64 H16A 86.9 . . ? N17 C64 H16B 86.3 . . ? C63 C64 H16B 56.2 . . ? H64A C64 H16B 67.6 . . ? H64B C64 H16B 161.1 . . ? H16A C64 H16B 77.0 . . ? N17 C64 H16M 34.9 . . ? C63 C64 H16M 139.2 . . ? H64A C64 H16M 97.2 . . ? H64B C64 H16M 86.3 . . ? H16A C64 H16M 156.1 . . ? H16B C64 H16M 112.3 . . ? N16 C63 C64 104.2(4) . . ? N16 C63 H63A 110.9 . . ? C64 C63 H63A 110.0 . . ? N16 C63 H63B 111.1 . . ? C64 C63 H63B 111.6 . . ? H63A C63 H63B 109.0 . . ? N16 C63 H16A 134.8 . . ? C64 C63 H16A 35.7 . . ? H63A C63 H16A 79.9 . . ? H63B C63 H16A 105.6 . . ? N16 C63 H16B 85.8 . . ? C64 C63 H16B 57.4 . . ? H63A C63 H16B 162.0 . . ? H63B C63 H16B 68.9 . . ? H16A C63 H16B 83.5 . . ? N18 C56 N17 114.0(5) . . ? N18 C56 H56A 109.2 . . ? N17 C56 H56A 109.2 . . ? N18 C56 H56B 108.1 . . ? N17 C56 H56B 108.5 . . ? H56A C56 H56B 107.6 . . ? N18 C56 H16K 86.7 . . ? N17 C56 H16K 132.6 . . ? H56A C56 H16K 102.2 . . ? H56B C56 H16K 26.0 . . ? N18 C56 H16L 83.3 . . ? N17 C56 H16L 152.4 . . ? H56A C56 H16L 43.2 . . ? H56B C56 H16L 84.2 . . ? H16K C56 H16L 66.4 . . ? N18 C56 H16O 114.2 . . ? N17 C56 H16O 31.1 . . ? H56A C56 H16O 131.0 . . ? H56B C56 H16O 79.7 . . ? H16K C56 H16O 101.9 . . ? H16L C56 H16O 159.1 . . ? C56 N18 C57 108.8(4) . . ? C56 N18 Ni2 122.8(4) . . ? C57 N18 Ni2 108.2(4) . . ? C56 N18 H18A 105.4 . . ? C57 N18 H18A 105.0 . . ? Ni2 N18 H18A 105.1 . . ? C56 N18 H12D 80.6 . . ? C57 N18 H12D 113.5 . . ? Ni2 N18 H12D 120.5 . . ? H18A N18 H12D 24.8 . . ? N18 C57 C58 104.5(4) . . ? N18 C57 H57A 111.6 . . ? C58 C57 H57A 111.5 . . ? N18 C57 H57B 109.9 . . ? C58 C57 H57B 110.2 . . ? H57A C57 H57B 109.0 . . ? N18 C57 H16G 94.6 . . ? C58 C57 H16G 73.8 . . ? H57A C57 H16G 47.9 . . ? H57B C57 H16G 152.5 . . ? N19 C58 C57 107.9(5) . . ? N19 C58 H58A 110.0 . . ? C57 C58 H58A 109.6 . . ? N19 C58 H58B 109.8 . . ? C57 C58 H58B 110.9 . . ? H58A C58 H58B 108.6 . . ? N19 C58 H16I 82.6 . . ? C57 C58 H16I 162.8 . . ? H58A C58 H16I 78.3 . . ? H58B C58 H16I 51.9 . . ? N19 C58 H16J 69.9 . . ? C57 C58 H16J 118.4 . . ? H58A C58 H16J 40.3 . . ? H58B C58 H16J 128.1 . . ? H16I C58 H16J 77.7 . . ? C65 N19 C58 114.1(4) . . ? C65 N19 C59 103.9(4) . . ? C58 N19 C59 108.0(4) . . ? C65 N19 Ni2 108.9(4) . . ? C58 N19 Ni2 109.7(3) . . ? C59 N19 Ni2 112.1(3) . . ? N20 C59 N19 101.5(4) . . ? N20 C59 H59A 111.3 . . ? N19 C59 H59A 111.7 . . ? N20 C59 H59B 111.1 . . ? N19 C59 H59B 111.6 . . ? H59A C59 H59B 109.4 . . ? N20 C59 H15Q 20.2 . . ? N19 C59 H15Q 102.1 . . ? H59A C59 H15Q 92.9 . . ? H59B C59 H15Q 127.5 . . ? C60 N20 C59 111.9(5) . . ? C60 N20 C66 114.4(5) . . ? C59 N20 C66 104.9(4) . . ? C60 N20 H15P 80.5 . . ? C59 N20 H15P 147.6 . . ? C66 N20 H15P 44.5 . . ? C60 N20 H15Q 89.0 . . ? C59 N20 H15Q 23.3 . . ? C66 N20 H15Q 120.7 . . ? H15P N20 H15Q 151.3 . . ? N20 C66 C65 105.0(4) . . ? N20 C66 H66A 109.6 . . ? C65 C66 H66A 110.1 . . ? N20 C66 H66B 111.1 . . ? C65 C66 H66B 112.0 . . ? H66A C66 H66B 108.9 . . ? N20 C66 H15P 35.6 . . ? C65 C66 H15P 130.2 . . ? H66A C66 H15P 76.5 . . ? H66B C66 H15P 111.6 . . ? N20 C66 H15R 130.8 . . ? C65 C66 H15R 31.2 . . ? H66A C66 H15R 83.1 . . ? H66B C66 H15R 108.5 . . ? H15P C66 H15R 139.0 . . ? N20 C66 H15S 99.6 . . ? C65 C66 H15S 40.9 . . ? H66A C66 H15S 144.7 . . ? H66B C66 H15S 77.1 . . ? H15P C66 H15S 135.1 . . ? H15R C66 H15S 62.6 . . ? N19 C65 C66 105.2(4) . . ? N19 C65 H65A 110.9 . . ? C66 C65 H65A 109.6 . . ? N19 C65 H65B 110.7 . . ? C66 C65 H65B 111.5 . . ? H65A C65 H65B 108.9 . . ? N19 C65 H15R 149.7 . . ? C66 C65 H15R 67.6 . . ? H65A C65 H15R 99.0 . . ? H65B C65 H15R 52.1 . . ? N19 C65 H15S 93.5 . . ? C66 C65 H15S 69.5 . . ? H65A C65 H15S 50.4 . . ? H65B C65 H15S 153.7 . . ? H15R C65 H15S 109.9 . . ? N20 C60 N21 113.3(5) . . ? N20 C60 H60A 108.6 . . ? N21 C60 H60A 108.0 . . ? N20 C60 H60B 109.0 . . ? N21 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? N20 C60 H15N 153.8 . . ? N21 C60 H15N 67.9 . . ? H60A C60 H15N 95.1 . . ? H60B C60 H15N 50.8 . . ? N20 C60 H15O 134.6 . . ? N21 C60 H15O 80.1 . . ? H60A C60 H15O 31.2 . . ? H60B C60 H15O 105.9 . . ? H15N C60 H15O 71.6 . . ? N20 C60 H15P 34.2 . . ? N21 C60 H15P 104.8 . . ? H60A C60 H15P 139.3 . . ? H60B C60 H15P 82.2 . . ? H15N C60 H15P 119.6 . . ? H15O C60 H15P 168.7 . . ? N20 C60 H15Q 27.4 . . ? N21 C60 H15Q 102.3 . . ? H60A C60 H15Q 89.7 . . ? H60B C60 H15Q 135.5 . . ? H15N C60 H15Q 170.0 . . ? H15O C60 H15Q 109.5 . . ? H15P C60 H15Q 59.8 . . ? C61 N21 C60 110.0(4) . . ? C61 N21 Ni2 107.5(4) . . ? C60 N21 Ni2 120.0(4) . . ? C61 N21 H21A 105.7 . . ? C60 N21 H21A 106.1 . . ? Ni2 N21 H21A 106.6 . . ? C61 N21 H11B 124.4 . . ? C60 N21 H11B 106.2 . . ? Ni2 N21 H11B 88.2 . . ? H21A N21 H11B 22.3 . . ? N21 C61 C62 106.2(4) . . ? N21 C61 H61A 111.3 . . ? C62 C61 H61A 111.8 . . ? N21 C61 H61B 109.5 . . ? C62 C61 H61B 109.1 . . ? H61A C61 H61B 108.9 . . ? N116 Ni2' N121 93.6(5) . . ? N116 Ni2' N119 166.7(5) . . ? N121 Ni2' N119 98.0(4) . . ? N116 Ni2' N118 90.8(4) . . ? N121 Ni2' N118 175.6(5) . . ? N119 Ni2' N118 77.6(4) . . ? N116 Ni2' H18A 103.8 . . ? N121 Ni2' H18A 27.4 . . ? N119 Ni2' H18A 89.5 . . ? N118 Ni2' H18A 150.7 . . ? N116 C162 C161 104.4(8) . . ? N116 C162 H63B 78.6 . . ? C161 C162 H63B 176.7 . . ? N116 C162 H16A 109.5 . . ? C161 C162 H16A 110.7 . . ? H63B C162 H16A 69.2 . . ? N116 C162 H16B 113.5 . . ? C161 C162 H16B 109.9 . . ? H63B C162 H16B 67.3 . . ? H16A C162 H16B 108.8 . . ? C163 N116 C162 109.9(9) . . ? C163 N116 C155 108.1(7) . . ? C162 N116 C155 108.2(9) . . ? C163 N116 Ni2' 112.0(10) . . ? C162 N116 Ni2' 107.6(7) . . ? C155 N116 Ni2' 111.0(8) . . ? N117 C155 N116 101.4(7) . . ? N117 C155 H61B 24.1 . . ? N116 C155 H61B 116.8 . . ? N117 C155 H15L 111.1 . . ? N116 C155 H15L 112.7 . . ? H61B C155 H15L 116.3 . . ? N117 C155 H15M 111.0 . . ? N116 C155 H15M 111.1 . . ? H61B C155 H15M 87.5 . . ? H15L C155 H15M 109.4 . . ? C156 N117 C164 109.4(10) . . ? C156 N117 C155 108.9(9) . . ? C164 N117 C155 107.7(8) . . ? C156 N117 H61A 70.3 . . ? C164 N117 H61A 64.8 . . ? C155 N117 H61A 170.7 . . ? C156 N117 H61B 75.8 . . ? C164 N117 H61B 153.7 . . ? C155 N117 H61B 48.2 . . ? H61A N117 H61B 137.7 . . ? N117 C164 C163 104.7(7) . . ? N117 C164 H62A 130.3 . . ? C163 C164 H62A 32.2 . . ? N117 C164 H62B 89.6 . . ? C163 C164 H62B 56.4 . . ? H62A C164 H62B 80.6 . . ? N117 C164 H61A 41.7 . . ? C163 C164 H61A 139.0 . . ? H62A C164 H61A 143.5 . . ? H62B C164 H61A 126.1 . . ? N117 C164 H16C 109.6 . . ? C163 C164 H16C 110.9 . . ? H62A C164 H16C 110.2 . . ? H62B C164 H16C 65.8 . . ? H61A C164 H16C 104.1 . . ? N117 C164 H16D 112.6 . . ? C163 C164 H16D 110.1 . . ? H62A C164 H16D 80.8 . . ? H62B C164 H16D 157.2 . . ? H61A C164 H16D 76.5 . . ? H16C C164 H16D 109.0 . . ? N116 C163 C164 105.0(7) . . ? N116 C163 H62A 137.6 . . ? C164 C163 H62A 42.3 . . ? N116 C163 H62B 90.5 . . ? C164 C163 H62B 53.1 . . ? H62A C163 H62B 85.7 . . ? N116 C163 H16E 110.5 . . ? C164 C163 H16E 111.7 . . ? H62A C163 H16E 73.8 . . ? H62B C163 H16E 157.7 . . ? N116 C163 H16F 109.8 . . ? C164 C163 H16F 110.9 . . ? H62A C163 H16F 108.0 . . ? H62B C163 H16F 68.7 . . ? H16E C163 H16F 108.9 . . ? N117 C156 N118 113.8(10) . . ? N117 C156 H60A 132.8 . . ? N118 C156 H60A 94.7 . . ? N117 C156 H61A 40.6 . . ? N118 C156 H61A 119.4 . . ? H60A C156 H61A 145.3 . . ? N117 C156 H61B 25.1 . . ? N118 C156 H61B 114.7 . . ? H60A C156 H61B 109.4 . . ? H61A C156 H61B 64.0 . . ? N117 C156 H15N 107.9 . . ? N118 C156 H15N 108.3 . . ? H60A C156 H15N 96.7 . . ? H61A C156 H15N 68.2 . . ? H61B C156 H15N 126.7 . . ? N117 C156 H15O 110.1 . . ? N118 C156 H15O 108.9 . . ? H60A C156 H15O 22.8 . . ? H61A C156 H15O 130.4 . . ? H61B C156 H15O 87.1 . . ? H15N C156 H15O 107.6 . . ? C156 N118 C157 107.6(10) . . ? C156 N118 Ni2' 117.1(9) . . ? C157 N118 Ni2' 112.1(9) . . ? C156 N118 H21A 83.5 . . ? C157 N118 H21A 116.5 . . ? Ni2' N118 H21A 116.9 . . ? C156 N118 H11B 107.2 . . ? C157 N118 H11B 105.4 . . ? Ni2' N118 H11B 106.7 . . ? H21A N118 H11B 23.9 . . ? N118 C157 C158 103.2(9) . . ? N118 C157 H15P 113.7 . . ? C158 C157 H15P 109.1 . . ? N118 C157 H15Q 109.8 . . ? C158 C157 H15Q 112.2 . . ? H15P C157 H15Q 108.8 . . ? N119 C158 C157 104.0(8) . . ? N119 C158 H65A 86.3 . . ? C157 C158 H65A 159.3 . . ? N119 C158 H65B 71.3 . . ? C157 C158 H65B 118.4 . . ? H65A C158 H65B 81.8 . . ? N119 C158 H15R 110.5 . . ? C157 C158 H15R 112.3 . . ? H65A C158 H15R 79.7 . . ? H65B C158 H15R 39.4 . . ? N119 C158 H15S 110.5 . . ? C157 C158 H15S 110.8 . . ? H65A C158 H15S 48.5 . . ? H65B C158 H15S 128.8 . . ? H15R C158 H15S 108.8 . . ? C159 N119 C165 107.4(7) . . ? C159 N119 C158 107.5(9) . . ? C165 N119 C158 108.5(9) . . ? C159 N119 Ni2' 114.4(7) . . ? C165 N119 Ni2' 101.2(9) . . ? C158 N119 Ni2' 117.1(7) . . ? N120 C159 N119 98.9(7) . . ? N120 C159 H57B 17.4 . . ? N119 C159 H57B 100.2 . . ? N120 C159 H15T 112.1 . . ? N119 C159 H15T 109.9 . . ? H57B C159 H15T 95.7 . . ? N120 C159 H15U 112.0 . . ? N119 C159 H15U 114.0 . . ? H57B C159 H15U 125.6 . . ? H15T C159 H15U 109.6 . . ? C160 N120 C159 107.8(9) . . ? C160 N120 C166 108.6(10) . . ? C159 N120 C166 107.7(8) . . ? C160 N120 H57A 74.4 . . ? C159 N120 H57A 151.7 . . ? C166 N120 H57A 48.0 . . ? C160 N120 H57B 79.1 . . ? C159 N120 H57B 30.1 . . ? C166 N120 H57B 127.2 . . ? H57A N120 H57B 146.8 . . ? N120 C166 C165 104.0(7) . . ? N120 C166 H57A 43.2 . . ? C165 C166 H57A 132.8 . . ? N120 C166 H58A 130.6 . . ? C165 C166 H58A 31.1 . . ? H57A C166 H58A 137.7 . . ? N120 C166 H58B 95.3 . . ? C165 C166 H58B 43.9 . . ? H57A C166 H58B 138.4 . . ? H58A C166 H58B 65.6 . . ? N120 C166 H16G 109.4 . . ? C165 C166 H16G 109.2 . . ? H57A C166 H16G 69.3 . . ? H58A C166 H16G 83.4 . . ? H58B C166 H16G 148.6 . . ? N120 C166 H16H 111.0 . . ? C165 C166 H16H 114.1 . . ? H57A C166 H16H 110.3 . . ? H58A C166 H16H 108.8 . . ? H58B C166 H16H 78.2 . . ? H16G C166 H16H 109.0 . . ? N119 C165 C166 103.4(7) . . ? N119 C165 H58A 148.5 . . ? C166 C165 H58A 62.5 . . ? N119 C165 H58B 91.6 . . ? C166 C165 H58B 65.3 . . ? H58A C165 H58B 105.4 . . ? N119 C165 H16I 111.3 . . ? C166 C165 H16I 108.0 . . ? H58A C165 H16I 100.1 . . ? H58B C165 H16I 53.1 . . ? N119 C165 H16J 112.4 . . ? C166 C165 H16J 112.5 . . ? H58A C165 H16J 56.9 . . ? H58B C165 H16J 155.1 . . ? H16I C165 H16J 109.1 . . ? N121 C160 N120 126.3(10) . . ? N121 C160 H56A 65.5 . . ? N120 C160 H56A 150.5 . . ? N121 C160 H56B 85.8 . . ? N120 C160 H56B 133.3 . . ? H56A C160 H56B 68.8 . . ? N121 C160 H57A 107.4 . . ? N120 C160 H57A 39.2 . . ? H56A C160 H57A 114.4 . . ? H56B C160 H57A 166.7 . . ? N121 C160 H57B 122.1 . . ? N120 C160 H57B 23.4 . . ? H56A C160 H57B 171.7 . . ? H56B C160 H57B 113.3 . . ? H57A C160 H57B 61.6 . . ? N121 C160 H16K 107.0 . . ? N120 C160 H16K 107.6 . . ? H56A C160 H16K 91.3 . . ? H56B C160 H16K 25.8 . . ? H57A C160 H16K 143.3 . . ? H57B C160 H16K 89.2 . . ? N121 C160 H16L 102.5 . . ? N120 C160 H16L 104.7 . . ? H56A C160 H16L 46.8 . . ? H56B C160 H16L 98.8 . . ? H57A C160 H16L 76.8 . . ? H57B C160 H16L 125.3 . . ? H16K C160 H16L 107.6 . . ? C160 N121 C161 109.7(11) . . ? C160 N121 Ni2' 107.5(11) . . ? C161 N121 Ni2' 99.7(9) . . ? C160 N121 H18A 104.6 . . ? C161 N121 H18A 143.3 . . ? Ni2' N121 H18A 81.8 . . ? C160 N121 H12D 111.1 . . ? C161 N121 H12D 116.2 . . ? Ni2' N121 H12D 111.9 . . ? H18A N121 H12D 35.6 . . ? N121 C161 C162 100.6(9) . . ? N121 C161 H16M 111.7 . . ? C162 C161 H16M 111.5 . . ? N121 C161 H16O 113.4 . . ? C162 C161 H16O 110.7 . . ? H16M C161 H16O 108.8 . . ? C27 N12 C42 128.8(5) . . ? C27 N12 H12A 115.5 . . ? C42 N12 H12A 115.6 . . ? C27 N12 H12B 106.9 . . ? C42 N12 H12B 123.2 . . ? H12A N12 H12B 12.9 . . ? C43 C42 C47 114.9(9) . . ? C43 C42 N12 114.6(8) . . ? C47 C42 N12 130.5(8) . . ? C44 C43 C42 124.6(10) . . ? C44 C43 H43A 117.1 . . ? C42 C43 H43A 118.2 . . ? C44 C43 H43B 119.3 . . ? C42 C43 H43B 111.0 . . ? H43A C43 H43B 23.0 . . ? C43 C44 C45 119.0(10) . . ? C43 C44 H44A 121.0 . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44B 106.8 . . ? C45 C44 H44B 132.2 . . ? H44A C44 H44B 19.0 . . ? C44 C45 C46 117.1(9) . . ? C44 C45 C48 121.8(8) . . ? C46 C45 C48 120.6(8) . . ? C47 C46 C45 123.1(10) . . ? C47 C46 H46A 118.1 . . ? C45 C46 H46A 118.8 . . ? C47 C46 H46B 108.7 . . ? C45 C46 H46B 110.3 . . ? H46A C46 H46B 44.0 . . ? C46 C47 C42 119.8(10) . . ? C46 C47 H47A 120.5 . . ? C42 C47 H47A 119.7 . . ? C46 C47 H47B 134.1 . . ? C42 C47 H47B 105.5 . . ? H47A C47 H47B 16.2 . . ? O11 C48 O12 119.9(10) . . ? O11 C48 C45 121.5(9) . . ? O12 C48 C45 118.1(9) . . ? C43' C42' C47' 119.6(7) . . ? C44' C43' C42' 121.8(8) . . ? C44' C43' H43A 109.6 . . ? C42' C43' H43A 117.6 . . ? C44' C43' H43B 119.7 . . ? C42' C43' H43B 118.5 . . ? H43A C43' H43B 33.7 . . ? C43' C44' C45' 120.5(8) . . ? C43' C44' H44A 133.9 . . ? C45' C44' H44A 102.6 . . ? C43' C44' H44B 120.1 . . ? C45' C44' H44B 119.4 . . ? H44A C44' H44B 23.0 . . ? C44' C45' C46' 117.5(7) . . ? C44' C45' C48' 121.5(7) . . ? C46' C45' C48' 120.9(6) . . ? C47' C46' C45' 122.4(8) . . ? C47' C46' H46A 113.8 . . ? C45' C46' H46A 115.9 . . ? C47' C46' H46B 119.4 . . ? C45' C46' H46B 118.1 . . ? H46A C46' H46B 31.0 . . ? C46' C47' C42' 118.1(8) . . ? C46' C47' H47A 110.0 . . ? C42' C47' H47A 131.1 . . ? C46' C47' H47B 121.1 . . ? C42' C47' H47B 120.7 . . ? H47A C47' H47B 13.1 . . ? O12' C48' O11' 121.2(8) . . ? O12' C48' C45' 119.2(7) . . ? O11' C48' C45' 118.6(7) . . ? N1 C1 N4 119.4(4) . . ? N1 C1 N2 127.7(4) . . ? N4 C1 N2 112.8(5) . . ? N2 C2 N3 126.6(4) . . ? N2 C2 N5 120.8(4) . . ? N3 C2 N5 112.4(4) . . ? N3 C3 N1 129.1(5) . . ? N3 C3 N6 118.1(4) . . ? N1 C3 N6 112.7(4) . . ? C5 C4 N4 127.1(5) . . ? C5 C4 C9 117.4(5) . . ? N4 C4 C9 115.5(5) . . ? C4 C5 C6 121.7(5) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 121.9(5) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 116.4(5) . . ? C6 C7 C10 123.3(5) . . ? C8 C7 C10 120.2(5) . . ? C7 C8 C9 124.1(5) . . ? C7 C8 H8A 118.0 . . ? C9 C8 H8A 118.0 . . ? C8 C9 C4 118.5(5) . . ? C8 C9 H9A 120.7 . . ? C4 C9 H9A 120.7 . . ? O1 C10 O2 124.8(5) . . ? O1 C10 C7 117.3(5) . . ? O2 C10 C7 117.6(5) . . ? C16 C11 C12 119.4(5) . . ? C16 C11 N5 115.3(5) . . ? C12 C11 N5 125.2(4) . . ? C13 C12 C11 120.8(5) . . ? C13 C12 H12C 119.6 . . ? C11 C12 H12C 119.6 . . ? C12 C13 C14 120.7(5) . . ? C12 C13 H13B 119.7 . . ? C14 C13 H13B 119.7 . . ? C15 C14 C13 117.4(5) . . ? C15 C14 C17 122.5(5) . . ? C13 C14 C17 120.0(5) . . ? C14 C15 C16 122.7(5) . . ? C14 C15 H15V 118.6 . . ? C16 C15 H15V 118.6 . . ? C11 C16 C15 118.9(5) . . ? C11 C16 H16N 120.5 . . ? C15 C16 H16N 120.5 . . ? O3 C17 O4 122.7(5) . . ? O3 C17 C14 120.9(5) . . ? O4 C17 C14 116.4(5) . . ? N6 C18 C19 125.0(5) . . ? N6 C18 C23 118.9(4) . . ? C19 C18 C23 116.1(5) . . ? C18 C19 C20 122.2(5) . . ? C18 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 117.4(5) . . ? C20 C21 C24 119.9(5) . . ? C22 C21 C24 122.6(5) . . ? C23 C22 C21 121.3(5) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C18 122.1(5) . . ? C22 C23 H23A 118.9 . . ? C18 C23 H23A 118.9 . . ? O5 C24 O6 121.9(5) . . ? O5 C24 C21 120.3(5) . . ? O6 C24 C21 117.8(5) . . ? N8 C25 N7 127.8(4) . . ? N8 C25 N10 120.6(4) . . ? N7 C25 N10 111.6(4) . . ? N9 C26 N11 122.1(4) . . ? N9 C26 N8 126.0(4) . . ? N11 C26 N8 111.8(4) . . ? N9 C27 N12 116.1(4) . . ? N9 C27 N7 124.7(4) . . ? N12 C27 N7 119.2(5) . . ? C29 C28 C33 121.9(4) . . ? C29 C28 N10 122.7(4) . . ? C33 C28 N10 115.4(4) . . ? C28 C29 C30 117.7(4) . . ? C28 C29 H29A 121.2 . . ? C30 C29 H29A 121.2 . . ? C31 C30 C29 120.3(5) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 119.7(5) . . ? C32 C31 C34 121.7(4) . . ? C30 C31 C34 118.6(5) . . ? C31 C32 C33 122.6(5) . . ? C31 C32 H32A 118.7 . . ? C33 C32 H32A 118.7 . . ? C32 C33 C28 117.7(5) . . ? C32 C33 H33A 121.1 . . ? C28 C33 H33A 121.1 . . ? O8 C34 O7 127.0(5) . . ? O8 C34 C31 115.2(5) . . ? O7 C34 C31 117.8(4) . . ? C36 C35 C40 120.9(4) . . ? C36 C35 N11 117.3(4) . . ? C40 C35 N11 121.8(5) . . ? C35 C36 C37 121.0(5) . . ? C35 C36 H36A 119.5 . . ? C37 C36 H36A 119.5 . . ? C36 C37 C38 120.6(5) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C37 C38 C39 117.5(4) . . ? C37 C38 C41 120.2(5) . . ? C39 C38 C41 122.3(4) . . ? C40 C39 C38 122.0(5) . . ? C40 C39 H39A 119.0 . . ? C38 C39 H39A 119.0 . . ? C39 C40 C35 117.8(5) . . ? C39 C40 H40A 121.1 . . ? C35 C40 H40A 121.1 . . ? O9 C41 O10 122.8(5) . . ? O9 C41 C38 120.8(5) . . ? O10 C41 C38 116.5(5) . . ? N23 C67 N22 102.9(4) . . ? N23 C67 H67A 111.2 . . ? N22 C67 H67A 111.2 . . ? N23 C67 H67B 111.2 . . ? N22 C67 H67B 111.2 . . ? H67A C67 H67B 109.1 . . ? N23 C68 C69 104.7(4) . . ? N23 C68 H68A 110.8 . . ? C69 C68 H68A 110.8 . . ? N23 C68 H68B 110.8 . . ? C69 C68 H68B 110.8 . . ? H68A C68 H68B 108.9 . . ? N22 C69 C68 106.5(5) . . ? N22 C69 H69A 110.4 . . ? C68 C69 H69A 110.4 . . ? N22 C69 H69B 110.4 . . ? C68 C69 H69B 110.4 . . ? H69A C69 H69B 108.6 . . ? N22 C70 C72 108.4(5) . 2_755 ? N22 C70 H70A 110.0 . . ? C72 C70 H70A 110.0 2_755 . ? N22 C70 H70B 110.0 . . ? C72 C70 H70B 110.0 2_755 . ? H70A C70 H70B 108.4 . . ? N23 C71 N24 112.9(4) . . ? N23 C71 H71A 109.0 . . ? N24 C71 H71A 109.0 . . ? N23 C71 H71B 109.0 . . ? N24 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? N24 C72 C70 102.6(5) . 2_755 ? N24 C72 H72A 111.3 . . ? C70 C72 H72A 111.3 2_755 . ? N24 C72 H72B 111.3 . . ? C70 C72 H72B 111.3 2_755 . ? H72A C72 H72B 109.2 . . ? N26 C73 N25 104.9(4) . . ? N26 C73 H73A 110.8 . . ? N25 C73 H73A 110.8 . . ? N26 C73 H73B 110.8 . . ? N25 C73 H73B 110.8 . . ? H73A C73 H73B 108.8 . . ? N26 C74 C75 106.8(4) . . ? N26 C74 H74A 110.4 . . ? C75 C74 H74A 110.4 . . ? N26 C74 H74B 110.4 . . ? C75 C74 H74B 110.4 . . ? H74A C74 H74B 108.6 . . ? N25 C75 C74 103.2(4) . . ? N25 C75 H75A 111.1 . . ? C74 C75 H75A 111.1 . . ? N25 C75 H75B 111.1 . . ? C74 C75 H75B 111.1 . . ? H75A C75 H75B 109.1 . . ? N25 C76 C78 110.5(4) . 2_665 ? N25 C76 H76A 109.5 . . ? C78 C76 H76A 109.5 2_665 . ? N25 C76 H76B 109.5 . . ? C78 C76 H76B 109.5 2_665 . ? H76A C76 H76B 108.1 . . ? N26 C77 N27 116.0(4) . . ? N26 C77 H77A 108.3 . . ? N27 C77 H77A 108.3 . . ? N26 C77 H77B 108.3 . . ? N27 C77 H77B 108.3 . . ? H77A C77 H77B 107.4 . . ? N27 C78 C76 106.6(4) . 2_665 ? N27 C78 H78A 110.4 . . ? C76 C78 H78A 110.4 2_665 . ? N27 C78 H78B 110.4 . . ? C76 C78 H78B 110.4 2_665 . ? H78A C78 H78B 108.6 . . ? C1 N1 C3 110.9(4) . . ? C2 N2 C1 112.4(4) . . ? C3 N3 C2 112.6(4) . . ? C1 N4 C4 130.5(5) . . ? C1 N4 H4A 114.8 . . ? C4 N4 H4A 114.8 . . ? C2 N5 C11 132.7(4) . . ? C2 N5 H5B 113.7 . . ? C11 N5 H5B 113.7 . . ? C18 N6 C3 130.1(4) . . ? C18 N6 H6B 114.9 . . ? C3 N6 H6B 114.9 . . ? C25 N7 C27 112.6(4) . . ? C25 N8 C26 112.8(4) . . ? C26 N9 C27 115.4(4) . . ? C25 N10 C28 129.2(4) . . ? C25 N10 H10A 115.4 . . ? C28 N10 H10A 115.4 . . ? C26 N11 C35 131.9(4) . . ? C26 N11 H11A 114.0 . . ? C35 N11 H11A 114.0 . . ? C70 N22 C67 110.9(4) . . ? C70 N22 C69 114.1(5) . . ? C67 N22 C69 102.2(4) . . ? C70 N22 Ni3 107.2(3) . . ? C67 N22 Ni3 113.0(4) . . ? C69 N22 Ni3 109.5(3) . . ? C71 N23 C67 113.2(4) . . ? C71 N23 C68 115.2(5) . . ? C67 N23 C68 103.5(4) . . ? C71 N24 C72 108.6(4) . . ? C71 N24 Ni3 122.4(3) . . ? C72 N24 Ni3 107.9(3) . . ? C71 N24 H24 104.4 . . ? C72 N24 H24 104.6 . . ? Ni3 N24 H24 107.4 . . ? C76 N25 C73 116.7(4) . . ? C76 N25 C75 112.6(4) . . ? C73 N25 C75 99.0(4) . . ? C76 N25 Ni4 104.2(3) . . ? C73 N25 Ni4 107.8(3) . . ? C75 N25 Ni4 117.0(3) . . ? C77 N26 C73 114.5(4) . . ? C77 N26 C74 114.7(4) . . ? C73 N26 C74 103.0(4) . . ? C78 N27 C77 115.8(4) . . ? C78 N27 Ni4 105.4(3) . . ? C77 N27 Ni4 116.1(3) . . ? C78 N27 H27 105.4 . . ? C77 N27 H27 105.3 . . ? Ni4 N27 H27 108.2 . . ? Ni1 Ni1 N15 116.4(17) 2_776 2_776 ? Ni1 Ni1 N113 126.4(18) 2_776 . ? N15 Ni1 N113 107.7(3) 2_776 . ? Ni1 Ni1 N15 56.5(16) 2_776 . ? N15 Ni1 N15 172.86(16) 2_776 . ? N113 Ni1 N15 78.4(3) . . ? Ni1 Ni1 N13 142.0(18) 2_776 . ? N15 Ni1 N13 91.4(3) 2_776 . ? N113 Ni1 N13 16.9(3) . . ? N15 Ni1 N13 95.0(3) . . ? Ni1 Ni1 O1 108.4(15) 2_776 2_776 ? N15 Ni1 O1 95.1(3) 2_776 2_776 ? N113 Ni1 O1 96.0(3) . 2_776 ? N15 Ni1 O1 87.8(3) . 2_776 ? N13 Ni1 O1 93.2(2) . 2_776 ? Ni1 Ni1 N115 124.4(17) 2_776 . ? N15 Ni1 N115 8.3(3) 2_776 . ? N113 Ni1 N115 99.7(4) . . ? N15 Ni1 N115 177.6(4) . . ? N13 Ni1 N115 83.2(3) . . ? O1 Ni1 N115 93.8(4) 2_776 . ? Ni1 Ni1 N113 47.5(16) 2_776 2_776 ? N15 Ni1 N113 77.3(3) 2_776 2_776 ? N113 Ni1 N113 173.9(2) . 2_776 ? N15 Ni1 N113 96.4(3) . 2_776 ? N13 Ni1 N113 168.7(4) . 2_776 ? O1 Ni1 N113 86.9(3) 2_776 2_776 ? N115 Ni1 N113 85.4(4) . 2_776 ? Ni1 Ni1 O1 64.7(15) 2_776 . ? N15 Ni1 O1 88.4(3) 2_776 . ? N113 Ni1 O1 88.7(3) . . ? N15 Ni1 O1 88.1(3) . . ? N13 Ni1 O1 92.7(2) . . ? O1 Ni1 O1 173.07(16) 2_776 . ? N115 Ni1 O1 90.5(4) . . ? N113 Ni1 O1 88.0(3) 2_776 . ? Ni1 Ni1 N13 33.6(16) 2_776 2_776 ? N15 Ni1 N13 91.9(3) 2_776 2_776 ? N113 Ni1 N13 159.1(4) . 2_776 ? N15 Ni1 N13 81.6(2) . 2_776 ? N13 Ni1 N13 175.6(2) . 2_776 ? O1 Ni1 N13 89.3(2) 2_776 2_776 ? N115 Ni1 N13 100.1(3) . 2_776 ? N113 Ni1 N13 15.1(3) 2_776 2_776 ? O1 Ni1 N13 84.5(2) . 2_776 ? Ni1 Ni1 N115 49.8(16) 2_776 2_776 ? N15 Ni1 N115 166.0(4) 2_776 2_776 ? N113 Ni1 N115 85.3(4) . 2_776 ? N15 Ni1 N115 7.0(3) . 2_776 ? N13 Ni1 N115 101.9(3) . 2_776 ? O1 Ni1 N115 88.7(4) 2_776 2_776 ? N115 Ni1 N115 174.20(15) . 2_776 ? N113 Ni1 N115 89.5(4) 2_776 2_776 ? O1 Ni1 N115 86.6(4) . 2_776 ? N13 Ni1 N115 74.6(3) 2_776 2_776 ? N24 Ni3 N24 179.996(1) . 2_755 ? N24 Ni3 N22 87.86(18) . 2_755 ? N24 Ni3 N22 92.14(18) 2_755 2_755 ? N24 Ni3 N22 92.14(18) . . ? N24 Ni3 N22 87.87(18) 2_755 . ? N22 Ni3 N22 179.998(1) 2_755 . ? N27 Ni4 N27 179.999(1) 2_665 . ? N27 Ni4 N25 94.56(16) 2_665 2_665 ? N27 Ni4 N25 85.44(16) . 2_665 ? N27 Ni4 N25 85.44(16) 2_665 . ? N27 Ni4 N25 94.56(16) . . ? N25 Ni4 N25 179.998(1) 2_665 . ? N27 Ni4 O8 93.04(14) 2_665 . ? N27 Ni4 O8 86.96(14) . . ? N25 Ni4 O8 90.39(14) 2_665 . ? N25 Ni4 O8 89.61(14) . . ? N27 Ni4 O8 86.96(14) 2_665 2_665 ? N27 Ni4 O8 93.04(14) . 2_665 ? N25 Ni4 O8 89.61(14) 2_665 2_665 ? N25 Ni4 O8 90.39(14) . 2_665 ? O8 Ni4 O8 179.997(1) . 2_665 ? C10 O1 Ni1 132.2(4) . 2_776 ? C10 O1 Ni1 135.7(4) . . ? Ni1 O1 Ni1 6.93(16) 2_776 . ? C34 O8 Ni4 133.0(3) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.269 0.238 -0.006 206 88 ' ' 2 0.069 0.762 0.006 206 84 ' ' 3 -0.039 0.248 0.358 413 147 ' ' 4 0.036 0.752 0.642 413 148 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.061 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 963330' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef 'web_deposit_cif_file_1_XiangJiang_1366094804.2-ok.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C84 H108 N30 Ni3 O12), 4(C3 H7 N O)' _chemical_formula_sum 'C180 H244 N64 Ni6 O28' _chemical_formula_weight 4104.53 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.537(5) _cell_length_b 20.222(5) _cell_length_c 18.930(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.102(4) _cell_angle_gamma 90.00 _cell_volume 10444(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2354 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 18.78 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4327 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8626 _exptl_absorpt_correction_T_max 0.9142 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34303 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.1438 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9583 _reflns_number_gt 3517 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0600P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9583 _refine_ls_number_parameters 616 _refine_ls_number_restraints 214 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 O7 O 0.0091(4) 0.1389(3) 0.2503(8) 0.057(3) Uiso 0.50 1 d P . . C43 C 0.0236(5) 0.1918(7) 0.2495(9) 0.070(4) Uiso 0.50 1 d P . . H43A H 0.0503 0.1950 0.2389 0.084 Uiso 0.50 1 d PR . . N16 N 0.0065(6) 0.2479(4) 0.2620(10) 0.049(3) Uiso 0.50 1 d P . . C44 C 0.0259(6) 0.3079(8) 0.2613(12) 0.119(7) Uiso 0.50 1 d P . . H44A H 0.0533 0.3036 0.2527 0.178 Uiso 0.50 1 d PR . . H44B H 0.0012 0.3349 0.2189 0.178 Uiso 0.50 1 d PR . . H44C H 0.0365 0.3282 0.3133 0.178 Uiso 0.50 1 d PR . . C45 C -0.0363(5) 0.2483(8) 0.2736(10) 0.085(5) Uiso 0.50 1 d P . . H45A H -0.0478 0.2041 0.2718 0.127 Uiso 0.50 1 d PR . . H45B H -0.0267 0.2676 0.3258 0.127 Uiso 0.50 1 d PR . . H45C H -0.0619 0.2743 0.2314 0.127 Uiso 0.50 1 d PR . . O8 O 0.4678(4) 0.2686(5) 0.1135(6) 0.081(3) Uiso 0.50 1 d PDU . . C46 C 0.4891(7) 0.2955(10) 0.1817(9) 0.064(5) Uiso 0.50 1 d PDU . . H46A H 0.4819 0.3416 0.1819 0.077 Uiso 0.50 1 d PR . . N17 N 0.5000 0.2591(5) 0.2500 0.080(3) Uiso 1 2 d SDU . . C47 C 0.5000 0.1885(7) 0.2500 0.193(7) Uiso 1 2 d SDU . . H47A H 0.4907 0.1727 0.1963 0.289 Uiso 0.50 1 d PR . . H47B H 0.5322 0.1727 0.2883 0.289 Uiso 0.50 1 d PR . . H47C H 0.4771 0.1727 0.2654 0.289 Uiso 0.50 1 d PR . . C48 C 0.5250(7) 0.2844(10) 0.3327(10) 0.080(6) Uiso 0.50 1 d PDU . . H48A H 0.5222 0.3299 0.3165 0.119 Uiso 0.50 1 d PR . . H48B H 0.5028 0.2756 0.3524 0.119 Uiso 0.50 1 d PR . . H48C H 0.5579 0.2756 0.3752 0.119 Uiso 0.50 1 d PR . . C25 C 0.5668(4) 0.0829(5) 0.4710(6) 0.129(4) Uiso 0.753(5) 1 d PDU A 1 H25A H 0.5822 0.0984 0.4414 0.154 Uiso 0.753(5) 1 d PR A 1 H25B H 0.5412 0.1128 0.4635 0.154 Uiso 0.753(5) 1 d PR A 1 N8 N 0.6020(4) 0.0724(5) 0.5608(6) 0.121(3) Uiso 0.753(5) 1 d PDU A 1 C26 C 0.6269(4) 0.0062(5) 0.5694(6) 0.143(4) Uiso 0.753(5) 1 d PDU A 1 H26A H 0.6291 -0.0180 0.6147 0.172 Uiso 0.753(5) 1 d PR A 1 H26B H 0.6593 0.0121 0.5776 0.172 Uiso 0.753(5) 1 d PR A 1 C27 C 0.5937(4) -0.0284(5) 0.4881(7) 0.120(4) Uiso 0.753(5) 1 d PDU A 1 H27A H 0.5862 -0.0724 0.4975 0.144 Uiso 0.753(5) 1 d PR A 1 H27B H 0.6086 -0.0304 0.4547 0.144 Uiso 0.753(5) 1 d PR A 1 N7 N 0.5471(3) 0.0144(4) 0.4513(5) 0.099(3) Uiso 0.753(5) 1 d PDU A 1 C28 C 0.5199(4) -0.0047(6) 0.3637(7) 0.133(4) Uiso 0.753(5) 1 d PDU A 1 H28A H 0.5411 -0.0238 0.3465 0.160 Uiso 0.753(5) 1 d PR A 1 H28B H 0.5067 0.0355 0.3337 0.160 Uiso 0.753(5) 1 d PR A 1 C29 C 0.4768(5) -0.0441(7) 0.3441(9) 0.118(4) Uiso 0.753(5) 1 d PDU A 1 H29A H 0.4900 -0.0880 0.3591 0.142 Uiso 0.753(5) 1 d PR A 1 H29B H 0.4540 -0.0440 0.2864 0.142 Uiso 0.753(5) 1 d PR A 1 C30 C 0.5836(4) 0.0770(6) 0.6134(7) 0.111(4) Uiso 0.753(5) 1 d PDU . 1 H30A H 0.5687 0.1200 0.6037 0.133 Uiso 0.753(5) 1 d PR A 1 H30B H 0.6111 0.0775 0.6680 0.133 Uiso 0.753(5) 1 d PR A 1 N9 N 0.4520(3) -0.0314(4) 0.3853(5) 0.082(3) Uiso 0.753(5) 1 d PDU . 1 H9A H 0.4336 0.0039 0.3582 0.098 Uiso 0.753(5) 1 d PR A 1 C25' C 0.5626(9) -0.0379(10) 0.4306(17) 0.119(5) Uiso 0.247(5) 1 d PDU A 2 H25C H 0.5688 -0.0688 0.4732 0.142 Uiso 0.247(5) 1 d PR A 2 H25D H 0.5752 -0.0551 0.3973 0.142 Uiso 0.247(5) 1 d PR A 2 N8' N 0.5852(8) 0.0281(12) 0.4663(14) 0.133(5) Uiso 0.247(5) 1 d PDU A 2 C26' C 0.5551(11) 0.0797(11) 0.4026(17) 0.129(7) Uiso 0.247(5) 1 d PDU A 2 H26C H 0.5718 0.0889 0.3730 0.155 Uiso 0.247(5) 1 d PR A 2 H26D H 0.5513 0.1202 0.4253 0.155 Uiso 0.247(5) 1 d PR A 2 C27' C 0.5049(9) 0.0504(13) 0.3549(19) 0.134(7) Uiso 0.247(5) 1 d PDU A 2 H27C H 0.4989 0.0455 0.3002 0.161 Uiso 0.247(5) 1 d PR A 2 H27D H 0.4787 0.0756 0.3537 0.161 Uiso 0.247(5) 1 d PR A 2 N7' N 0.5104(8) -0.0162(12) 0.3958(13) 0.132(5) Uiso 0.247(5) 1 d PDU A 2 C28' C 0.4761(10) -0.0633(17) 0.340(2) 0.118(5) Uiso 0.247(5) 1 d PDU A 2 H28C H 0.4924 -0.1053 0.3558 0.142 Uiso 0.247(5) 1 d PR A 2 H28D H 0.4693 -0.0541 0.2850 0.142 Uiso 0.247(5) 1 d PR A 2 C29' C 0.4349(9) -0.0742(15) 0.3541(17) 0.093(6) Uiso 0.247(5) 1 d PDU A 2 H29C H 0.4306 -0.1179 0.3694 0.111 Uiso 0.247(5) 1 d PR A 2 H29D H 0.4080 -0.0653 0.3003 0.111 Uiso 0.247(5) 1 d PR A 2 C30' C 0.5911(8) 0.0443(16) 0.5452(14) 0.131(5) Uiso 0.247(5) 1 d PDU . 2 H30C H 0.5865 0.0913 0.5409 0.157 Uiso 0.247(5) 1 d PR A 2 H30D H 0.6253 0.0382 0.5840 0.157 Uiso 0.247(5) 1 d PR A 2 N9' N 0.4337(6) -0.0293(12) 0.4104(12) 0.080(6) Uiso 0.247(5) 1 d PDU . 2 H9'A H 0.4188 0.0075 0.3822 0.096 Uiso 0.247(5) 1 d PR A 2 C1 C 0.4399(2) 0.4542(3) 0.4932(4) 0.0368(16) Uani 1 1 d . . . C2 C 0.4510(2) 0.5634(3) 0.5132(4) 0.0425(17) Uani 1 1 d . . . C3 C 0.49650(19) 0.4938(3) 0.6152(3) 0.0355(14) Uani 1 1 d . . . C4 C 0.4237(2) 0.3367(3) 0.4373(4) 0.0388(16) Uani 1 1 d . . . C5 C 0.4603(2) 0.3035(3) 0.5029(4) 0.0433(17) Uani 1 1 d . . . H5 H 0.4812 0.3262 0.5523 0.052 Uiso 1 1 calc R . . C6 C 0.4664(2) 0.2362(3) 0.4960(4) 0.0518(19) Uani 1 1 d . . . H6 H 0.4913 0.2129 0.5416 0.062 Uiso 1 1 calc R . . C7 C 0.4369(2) 0.2023(3) 0.4239(4) 0.0490(18) Uani 1 1 d . . . C8 C 0.4004(2) 0.2371(3) 0.3584(4) 0.0523(19) Uani 1 1 d . . . H8 H 0.3802 0.2148 0.3083 0.063 Uiso 1 1 calc R . . C9 C 0.3928(2) 0.3035(3) 0.3647(4) 0.0470(18) Uani 1 1 d . . . H9 H 0.3669 0.3264 0.3201 0.056 Uiso 1 1 calc R . . C10 C 0.4432(3) 0.1296(3) 0.4150(5) 0.063(2) Uani 1 1 d . . . C11 C 0.4105(2) 0.6552(3) 0.4135(4) 0.0430(17) Uani 1 1 d . . . C12 C 0.3876(2) 0.6219(3) 0.3395(4) 0.0505(18) Uani 1 1 d . . . H12 H 0.3909 0.5753 0.3383 0.061 Uiso 1 1 calc R . . C13 C 0.3601(2) 0.6561(3) 0.2682(4) 0.0519(19) Uani 1 1 d . . . H13 H 0.3446 0.6322 0.2182 0.062 Uiso 1 1 calc R . . C14 C 0.3541(2) 0.7239(3) 0.2659(4) 0.0523(19) Uani 1 1 d . . . C15 C 0.3777(3) 0.7556(3) 0.3388(5) 0.072(2) Uani 1 1 d . . . H15 H 0.3748 0.8023 0.3395 0.087 Uiso 1 1 calc R . . C16 C 0.4051(2) 0.7237(3) 0.4106(4) 0.055(2) Uani 1 1 d . . . H16 H 0.4209 0.7485 0.4599 0.065 Uiso 1 1 calc R . . C17 C 0.3239(3) 0.7608(4) 0.1886(5) 0.076(3) Uani 1 1 d . . . C18 C 0.5651(2) 0.5173(3) 0.7579(4) 0.0444(17) Uani 1 1 d . . . C19 C 0.5765(2) 0.5813(3) 0.7456(4) 0.060(2) Uani 1 1 d . . . H19 H 0.5595 0.6008 0.6929 0.072 Uiso 1 1 calc R . . C20 C 0.6130(2) 0.6164(3) 0.8114(4) 0.059(2) Uani 1 1 d . . . H20 H 0.6211 0.6596 0.8024 0.071 Uiso 1 1 calc R . . C21 C 0.6380(2) 0.5900(3) 0.8899(4) 0.0494(18) Uani 1 1 d . . . C22 C 0.6262(2) 0.5260(3) 0.9003(4) 0.0528(19) Uani 1 1 d . . . H22 H 0.6427 0.5063 0.9529 0.063 Uiso 1 1 calc R . . C23 C 0.5908(2) 0.4908(3) 0.8351(4) 0.0528(18) Uani 1 1 d . . . H23 H 0.5838 0.4468 0.8437 0.063 Uiso 1 1 calc R . . C24 C 0.6785(3) 0.6303(4) 0.9604(6) 0.078(3) Uani 1 1 d . . . C31 C 0.1980(4) 0.7223(7) 0.0860(7) 0.135(4) Uani 1 1 d . . . H31A H 0.1775 0.7360 0.1095 0.162 Uiso 1 1 calc R . . H31B H 0.2322 0.7169 0.1308 0.162 Uiso 1 1 calc R . . C32 C 0.1377(4) 0.6824(6) -0.0420(9) 0.157(5) Uani 1 1 d . . . H32A H 0.1057 0.6698 -0.0481 0.188 Uiso 1 1 calc R . . H32B H 0.1405 0.6630 -0.0874 0.188 Uiso 1 1 calc R . . C33 C 0.1435(3) 0.7571(6) -0.0393(7) 0.125(4) Uani 1 1 d . . . H33A H 0.1386 0.7739 -0.0920 0.150 Uiso 1 1 calc R . . H33B H 0.1197 0.7788 -0.0275 0.150 Uiso 1 1 calc R . . C34 C 0.2022(3) 0.8427(5) 0.0522(6) 0.104(3) Uani 1 1 d . . . H34A H 0.1705 0.8618 0.0408 0.125 Uiso 1 1 calc R . . H34B H 0.2255 0.8466 0.1116 0.125 Uiso 1 1 calc R . . C35 C 0.2212(3) 0.8803(4) 0.0069(5) 0.085(3) Uani 1 1 d . . . H35A H 0.1960 0.8826 -0.0517 0.102 Uiso 1 1 calc R . . H35B H 0.2295 0.9260 0.0283 0.102 Uiso 1 1 calc R . . C36 C 0.2162(4) 0.6196(4) 0.0302(6) 0.098(3) Uani 1 1 d . . . H36A H 0.2436 0.6084 0.0852 0.117 Uiso 1 1 calc R . . H36B H 0.2003 0.5777 0.0026 0.117 Uiso 1 1 calc R . . C37 C 0.8398(3) 0.6924(5) 1.0173(5) 0.087(3) Uani 1 1 d . . . H37A H 0.8609 0.6778 0.9953 0.105 Uiso 1 1 calc R . . H37B H 0.8517 0.7356 1.0449 0.105 Uiso 1 1 calc R . . C38 C 0.8006(3) 0.5927(4) 1.0179(6) 0.107(3) Uani 1 1 d . . . H38A H 0.7772 0.5833 1.0372 0.128 Uiso 1 1 calc R . . H38B H 0.8164 0.5508 1.0164 0.128 Uiso 1 1 calc R . . C39 C 0.7739(3) 0.6263(4) 0.9319(5) 0.095(3) Uani 1 1 d . . . H39A H 0.7859 0.6085 0.8963 0.114 Uiso 1 1 calc R . . H39B H 0.7380 0.6200 0.9047 0.114 Uiso 1 1 calc R . . C40 C 0.7773(3) 0.7369(4) 0.8789(6) 0.098(3) Uani 1 1 d . . . H40A H 0.8003 0.7748 0.8970 0.117 Uiso 1 1 calc R . . H40B H 0.7834 0.7097 0.8414 0.117 Uiso 1 1 calc R . . C41 C 0.7263(3) 0.7621(4) 0.8341(4) 0.076(2) Uani 1 1 d . . . H41A H 0.7209 0.7896 0.7870 0.092 Uiso 1 1 calc R . . H41B H 0.7025 0.7252 0.8140 0.092 Uiso 1 1 calc R . . C42 C 0.8284(3) 0.6715(4) 1.1341(5) 0.095(3) Uani 1 1 d . . . H42A H 0.8521 0.7077 1.1622 0.114 Uiso 1 1 calc R . . H42B H 0.8349 0.6370 1.1755 0.114 Uiso 1 1 calc R . . N1 N 0.47455(17) 0.4394(2) 0.5687(3) 0.0387(13) Uani 1 1 d . . . N2 N 0.42505(17) 0.51577(19) 0.4613(3) 0.0377(13) Uani 1 1 d . . . N3 N 0.48777(18) 0.5556(2) 0.5921(3) 0.0407(13) Uani 1 1 d . . . N4 N 0.41429(16) 0.4044(2) 0.4376(3) 0.0437(14) Uani 1 1 d . . . H4 H 0.3870 0.4178 0.3945 0.052 Uiso 1 1 calc R . . N5 N 0.44058(17) 0.6271(2) 0.4895(3) 0.0422(14) Uani 1 1 d . . . H5A H 0.4555 0.6559 0.5294 0.051 Uiso 1 1 calc R . . N6 N 0.53100(17) 0.4775(2) 0.6936(3) 0.0393(13) Uani 1 1 d . . . H6A H 0.5319 0.4353 0.7057 0.047 Uiso 1 1 calc R . . N10 N 0.1951(3) 0.7696(4) 0.0282(4) 0.093(2) Uani 1 1 d . . . N11 N 0.1795(4) 0.6607(5) 0.0397(7) 0.135(4) Uani 1 1 d . . . N12 N 0.2636(2) 0.8480(3) 0.0167(4) 0.0699(19) Uani 1 1 d . . . H12A H 0.2873 0.8531 0.0714 0.084 Uiso 1 1 calc R . . N13 N 0.7872(2) 0.6962(4) 0.9513(4) 0.083(2) Uani 1 1 d . . . N14 N 0.8386(2) 0.6430(4) 1.0727(5) 0.092(2) Uani 1 1 d . . . N15 N 0.7212(2) 0.8023(3) 0.8948(4) 0.081(2) Uani 1 1 d . . . H15A H 0.7414 0.8389 0.9056 0.098 Uiso 1 1 calc R . . Ni1 Ni 0.5000 0.0000 0.5000 0.0487(3) Uani 1 2 d SD . . Ni2 Ni 0.2500 0.7500 0.0000 0.0469(4) Uani 1 2 d S . . Ni3 Ni 0.7500 0.7500 1.0000 0.0581(4) Uani 1 2 d S . . O1 O 0.47720(16) 0.10037(19) 0.4746(3) 0.0566(13) Uani 1 1 d . A . O2 O 0.4152(2) 0.1029(2) 0.3457(3) 0.099(2) Uani 1 1 d . . . O3 O 0.29900(16) 0.7270(2) 0.1238(3) 0.0593(13) Uani 1 1 d . . . O4 O 0.3268(2) 0.8227(2) 0.1907(3) 0.129(3) Uani 1 1 d . . . O5 O 0.68944(16) 0.6847(3) 0.9403(3) 0.0682(15) Uani 1 1 d . . . O6 O 0.69896(19) 0.6038(3) 1.0300(3) 0.098(2) Uani 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 C1 0.037(4) 0.036(4) 0.038(4) -0.012(3) 0.019(3) -0.010(3) C2 0.053(4) 0.036(4) 0.040(4) -0.004(3) 0.024(4) -0.006(3) C3 0.030(3) 0.038(4) 0.028(3) 0.001(4) 0.007(3) 0.002(3) C4 0.038(4) 0.024(4) 0.044(4) 0.001(3) 0.013(3) -0.001(3) C5 0.050(4) 0.025(4) 0.038(4) -0.009(3) 0.009(3) -0.007(3) C6 0.045(4) 0.028(4) 0.060(5) 0.000(3) 0.009(4) 0.000(3) C7 0.060(5) 0.035(4) 0.043(4) 0.006(3) 0.020(4) 0.001(4) C8 0.062(5) 0.039(4) 0.035(4) -0.004(3) 0.009(4) 0.001(4) C9 0.044(4) 0.032(4) 0.038(4) 0.002(3) 0.000(3) 0.003(3) C10 0.077(6) 0.040(5) 0.058(5) -0.002(4) 0.022(5) 0.005(4) C11 0.047(4) 0.029(4) 0.043(4) 0.005(3) 0.015(4) -0.001(3) C12 0.064(5) 0.029(4) 0.036(4) -0.006(3) 0.008(4) -0.001(3) C13 0.055(4) 0.039(4) 0.037(4) -0.004(3) 0.004(4) 0.001(3) C14 0.051(4) 0.028(4) 0.051(5) -0.003(4) 0.006(4) 0.001(3) C15 0.082(6) 0.026(4) 0.069(6) 0.007(4) 0.008(5) 0.009(4) C16 0.066(5) 0.036(4) 0.031(4) -0.004(3) 0.002(4) -0.003(4) C17 0.085(6) 0.045(5) 0.057(6) -0.007(4) 0.004(5) 0.013(5) C18 0.032(4) 0.040(5) 0.048(4) 0.005(3) 0.010(3) 0.006(3) C19 0.055(4) 0.052(5) 0.042(5) 0.000(4) 0.001(4) -0.013(4) C20 0.068(5) 0.052(5) 0.031(4) -0.004(4) 0.005(4) -0.020(4) C21 0.043(4) 0.058(5) 0.037(4) -0.006(4) 0.013(4) -0.009(4) C22 0.047(4) 0.051(4) 0.038(4) 0.002(3) 0.005(4) 0.000(3) C23 0.049(4) 0.035(4) 0.056(5) -0.003(4) 0.013(4) -0.011(3) C24 0.052(5) 0.074(6) 0.073(7) -0.005(5) 0.005(5) -0.018(5) C31 0.133(10) 0.173(13) 0.143(11) 0.043(10) 0.102(9) -0.012(9) C32 0.088(9) 0.138(12) 0.193(14) 0.022(10) 0.032(9) -0.027(8) C33 0.062(7) 0.161(12) 0.142(10) 0.008(9) 0.044(7) 0.013(7) C34 0.107(8) 0.087(8) 0.123(9) -0.025(7) 0.062(7) 0.026(6) C35 0.089(7) 0.075(6) 0.064(6) -0.014(5) 0.018(5) 0.020(5) C36 0.113(8) 0.062(6) 0.106(8) 0.019(5) 0.046(7) -0.013(6) C37 0.067(6) 0.112(8) 0.078(7) -0.012(6) 0.032(5) -0.002(5) C38 0.091(7) 0.071(7) 0.123(9) -0.020(6) 0.027(7) -0.007(6) C39 0.074(6) 0.074(7) 0.108(8) -0.013(6) 0.025(6) 0.006(5) C40 0.081(7) 0.098(8) 0.082(7) -0.017(6) 0.016(6) -0.008(6) C41 0.087(6) 0.079(6) 0.039(5) -0.011(4) 0.013(5) -0.020(5) C42 0.088(7) 0.072(6) 0.070(7) -0.005(5) -0.001(6) -0.017(5) N1 0.034(3) 0.031(3) 0.035(3) 0.003(3) 0.005(3) 0.001(2) N2 0.043(3) 0.012(3) 0.036(3) 0.001(2) 0.004(3) -0.002(2) N3 0.041(3) 0.026(3) 0.036(3) 0.004(3) 0.005(3) -0.002(2) N4 0.041(3) 0.025(3) 0.045(3) -0.001(3) 0.007(3) -0.002(3) N5 0.052(3) 0.016(3) 0.033(3) -0.003(2) 0.002(3) -0.006(2) N6 0.050(3) 0.027(3) 0.029(3) 0.001(2) 0.011(3) -0.006(2) N10 0.077(5) 0.133(7) 0.073(5) 0.013(5) 0.039(5) 0.012(5) N11 0.139(10) 0.110(8) 0.173(11) 0.012(8) 0.089(9) -0.044(7) N12 0.067(4) 0.059(4) 0.055(4) 0.009(3) 0.009(4) 0.013(3) N13 0.061(5) 0.079(5) 0.080(5) -0.011(4) 0.015(4) -0.005(4) N14 0.081(5) 0.090(6) 0.074(5) -0.002(5) 0.015(5) 0.000(4) N15 0.057(4) 0.080(5) 0.071(5) -0.002(4) 0.005(4) -0.024(4) Ni1 0.0657(8) 0.0284(6) 0.0436(7) -0.0045(6) 0.0210(6) -0.0011(7) Ni2 0.0440(7) 0.0428(8) 0.0426(8) 0.0079(6) 0.0132(6) 0.0067(6) Ni3 0.0471(8) 0.0607(9) 0.0432(9) -0.0125(7) 0.0053(7) -0.0130(7) O1 0.069(3) 0.022(2) 0.053(3) -0.002(2) 0.011(3) 0.005(2) O2 0.128(5) 0.041(3) 0.058(4) -0.014(3) -0.006(3) 0.016(3) O3 0.070(3) 0.039(3) 0.039(3) 0.008(2) 0.005(3) 0.012(2) O4 0.185(6) 0.035(3) 0.065(4) 0.010(3) -0.014(4) 0.023(4) O5 0.061(3) 0.071(4) 0.041(3) -0.010(3) 0.003(3) -0.025(3) O6 0.079(4) 0.100(5) 0.057(4) 0.009(3) -0.010(3) -0.042(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 O7 O7 0.57(2) 2 ? O7 C43 1.165(14) . ? O7 C43 1.486(16) 2 ? C43 N16 1.328(16) . ? C43 C45 1.353(18) 2 ? C43 N16 1.426(17) 2 ? C43 O7 1.486(15) 2 ? C43 C43 1.50(3) 2 ? C43 H43A 0.9599 . ? N16 N16 0.44(3) 2 ? N16 C44 1.362(17) . ? N16 C45 1.40(2) 2 ? N16 C43 1.426(17) 2 ? N16 C45 1.47(2) . ? N16 C44 1.504(18) 2 ? C44 C44 1.47(3) 2 ? C44 C45 1.49(2) 2 ? C44 N16 1.504(18) 2 ? C44 H44A 0.9599 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C43 1.353(18) 2 ? C45 N16 1.40(2) 2 ? C45 C44 1.49(2) 2 ? C45 H45A 0.9601 . ? C45 H45B 0.9599 . ? C45 H45C 0.9600 . ? O8 C48 0.979(19) 2_655 ? O8 C46 1.242(15) . ? C46 C48 0.45(3) 2_655 ? C46 N17 1.374(18) . ? C46 H46A 0.9600 . ? N17 C46 1.374(18) 2_655 ? N17 C47 1.428(13) . ? N17 C48 1.447(16) . ? N17 C48 1.447(15) 2_655 ? C47 H47A 0.9600 . ? C47 H47B 0.9601 . ? C47 H47C 0.9600 . ? C48 C46 0.45(3) 2_655 ? C48 O8 0.979(19) 2_655 ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C25 N7 1.487(10) . ? C25 N8 1.507(10) . ? C25 H25A 0.9599 . ? C25 H25B 0.9596 . ? C25 H26D 1.0647 . ? C25 H30C 1.1579 . ? N8 C30 1.384(10) . ? N8 C26 1.520(10) . ? N8 H30C 0.5841 . ? N8 H30D 0.9424 . ? C26 C27 1.528(10) . ? C26 H26A 0.9599 . ? C26 H26B 0.9603 . ? C26 H30D 0.7152 . ? C27 N7 1.539(9) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H25C 1.0685 . ? N7 C28 1.485(11) . ? N7 Ni1 2.124(9) . ? C28 C29 1.453(11) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C29 N9 1.380(11) . ? C29 H29A 0.9600 . ? C29 H29B 0.9601 . ? C29 H28D 1.0392 . ? C30 N9 1.462(11) 5_656 ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? N9 C30 1.462(11) 5_656 ? N9 Ni1 2.029(8) . ? N9 H9A 0.9000 . ? N9 H9'A 1.2880 . ? C25' N7' 1.501(13) . ? C25' N8' 1.505(13) . ? C25' H27B 1.2911 . ? C25' H25C 0.9600 . ? C25' H25D 0.9601 . ? N8' C30' 1.446(18) . ? N8' C26' 1.516(13) . ? C26' C27' 1.497(18) . ? C26' H25A 0.8842 . ? C26' H26C 0.9597 . ? C26' H26D 0.9602 . ? C27' N7' 1.520(13) . ? C27' H28B 0.5266 . ? C27' H27C 0.9601 . ? C27' H27D 0.9601 . ? N7' C28' 1.434(16) . ? N7' Ni1 2.180(18) . ? C28' C29' 1.476(17) . ? C28' H29A 0.6451 . ? C28' H29B 0.9725 . ? C28' H28C 0.9599 . ? C28' H28D 0.9602 . ? C29' N9' 1.413(18) . ? C29' H29C 0.9598 . ? C29' H29D 0.9600 . ? C30' N9' 1.439(17) 5_656 ? C30' H30C 0.9599 . ? C30' H30D 0.9598 . ? N9' C30' 1.439(17) 5_656 ? N9' Ni1 2.011(16) . ? N9' H9A 1.1947 . ? N9' H9'A 0.8998 . ? C1 N1 1.326(7) . ? C1 N2 1.361(7) . ? C1 N4 1.385(6) . ? C2 N2 1.326(7) . ? C2 N5 1.348(6) . ? C2 N3 1.365(7) . ? C3 N3 1.305(6) . ? C3 N1 1.362(7) . ? C3 N6 1.370(6) . ? C4 C5 1.374(7) . ? C4 C9 1.395(7) . ? C4 N4 1.403(7) . ? C5 C6 1.390(7) . ? C5 H5 0.9500 . ? C6 C7 1.387(8) . ? C6 H6 0.9500 . ? C7 C8 1.388(8) . ? C7 C10 1.506(8) . ? C8 C9 1.379(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 O1 1.248(7) . ? C10 O2 1.277(8) . ? C11 C12 1.386(8) . ? C11 N5 1.388(7) . ? C11 C16 1.393(8) . ? C12 C13 1.372(8) . ? C12 H12 0.9500 . ? C13 C14 1.380(8) . ? C13 H13 0.9500 . ? C14 C15 1.357(9) . ? C14 C17 1.486(9) . ? C15 C16 1.353(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O4 1.255(8) . ? C17 O3 1.273(7) . ? C18 C23 1.376(8) . ? C18 C19 1.392(8) . ? C18 N6 1.405(7) . ? C19 C20 1.393(8) . ? C19 H19 0.9500 . ? C20 C21 1.394(8) . ? C20 H20 0.9500 . ? C21 C22 1.387(8) . ? C21 C24 1.539(9) . ? C22 C23 1.376(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O6 1.260(9) . ? C24 O5 1.266(8) . ? C31 N10 1.423(11) . ? C31 N11 1.466(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N11 1.509(12) . ? C32 C33 1.519(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N10 1.503(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.480(11) . ? C34 N10 1.528(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N12 1.414(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N12 1.480(9) 7_565 ? C36 N11 1.507(11) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N14 1.463(9) . ? C37 N13 1.497(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N14 1.517(9) . ? C38 C39 1.565(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N13 1.469(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.483(10) . ? C40 N13 1.491(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N15 1.480(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N14 1.470(10) . ? C42 N15 1.472(9) 7_667 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N4 H4 0.8800 . ? N5 H5A 0.8800 . ? N6 H6A 0.8800 . ? N10 Ni2 2.088(7) . ? N12 C36 1.480(9) 7_565 ? N12 Ni2 2.018(6) . ? N12 H12A 0.9300 . ? N13 Ni3 2.120(7) . ? N15 C42 1.472(9) 7_667 ? N15 Ni3 2.024(6) . ? N15 H15A 0.9300 . ? Ni1 N9' 2.011(16) 5_656 ? Ni1 N9 2.029(8) 5_656 ? Ni1 N7 2.124(9) 5_656 ? Ni1 O1 2.126(4) 5_656 ? Ni1 O1 2.126(4) . ? Ni1 N7' 2.180(18) 5_656 ? Ni2 N12 2.018(6) 7_565 ? Ni2 N10 2.088(7) 7_565 ? Ni2 O3 2.113(4) . ? Ni2 O3 2.113(4) 7_565 ? Ni3 N15 2.024(6) 7_667 ? Ni3 N13 2.120(7) 7_667 ? Ni3 O5 2.122(5) . ? Ni3 O5 2.123(5) 7_667 ? 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 O7 O7 C43 113.5(9) 2 . ? O7 O7 C43 46.0(6) 2 2 ? C43 O7 C43 67.6(14) . 2 ? O7 C43 N16 125.8(16) . . ? O7 C43 C45 163.7(18) . 2 ? N16 C43 C45 63.1(11) . 2 ? O7 C43 N16 119.7(15) . 2 ? N16 C43 N16 17.7(13) . 2 ? C45 C43 N16 63.9(11) 2 2 ? O7 C43 O7 20.5(8) . 2 ? N16 C43 O7 105.7(13) . 2 ? C45 C43 O7 157.7(14) 2 2 ? N16 C43 O7 99.4(12) 2 2 ? O7 C43 C43 66.5(9) . 2 ? N16 C43 C43 60.2(10) . 2 ? C45 C43 C43 117.4(10) 2 2 ? N16 C43 C43 53.9(9) 2 2 ? O7 C43 C43 46.0(6) 2 2 ? O7 C43 H43A 117.2 . . ? N16 C43 H43A 117.1 . . ? C45 C43 H43A 56.2 2 . ? N16 C43 H43A 120.0 2 . ? O7 C43 H43A 137.0 2 . ? C43 C43 H43A 169.4 2 . ? N16 N16 C43 94(3) 2 . ? N16 N16 C44 101(2) 2 . ? C43 N16 C44 122.4(18) . . ? N16 N16 C45 91(5) 2 2 ? C43 N16 C45 59.3(11) . 2 ? C44 N16 C45 65.1(12) . 2 ? N16 N16 C43 68(3) 2 2 ? C43 N16 C43 65.8(14) . 2 ? C44 N16 C43 167.5(15) . 2 ? C45 N16 C43 119.0(14) 2 2 ? N16 N16 C45 72(5) 2 . ? C43 N16 C45 121.0(14) . . ? C44 N16 C45 116.6(14) . . ? C45 N16 C45 162.8(13) 2 . ? C43 N16 C45 55.6(9) 2 . ? N16 N16 C44 63(2) 2 2 ? C43 N16 C44 156.2(16) . 2 ? C44 N16 C44 61.4(13) . 2 ? C45 N16 C44 112.1(14) 2 2 ? C43 N16 C44 107.1(13) 2 2 ? C45 N16 C44 60.0(10) . 2 ? N16 C44 C44 64.1(10) . 2 ? N16 C44 C45 58.8(11) . 2 ? C44 C44 C45 109.3(12) 2 2 ? N16 C44 N16 16.5(12) . 2 ? C44 C44 N16 54.5(8) 2 2 ? C45 C44 N16 59.0(10) 2 2 ? N16 C44 H44A 111.6 . . ? C44 C44 H44A 156.5 2 . ? C45 C44 H44A 55.6 2 . ? N16 C44 H44A 114.6 2 . ? N16 C44 H44B 109.5 . . ? C44 C44 H44B 55.8 2 . ? C45 C44 H44B 110.9 2 . ? N16 C44 H44B 93.7 2 . ? H44A C44 H44B 109.5 . . ? N16 C44 H44C 107.3 . . ? C44 C44 H44C 93.5 2 . ? C45 C44 H44C 139.6 2 . ? N16 C44 H44C 118.7 2 . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 N16 57.6(9) 2 2 ? C43 C45 N16 60.5(9) 2 . ? N16 C45 N16 17.2(13) 2 . ? C43 C45 C44 112.1(14) 2 2 ? N16 C45 C44 56.1(9) 2 2 ? N16 C45 C44 61.1(9) . 2 ? C43 C45 H45A 51.0 2 . ? N16 C45 H45A 108.2 2 . ? N16 C45 H45A 110.6 . . ? C44 C45 H45A 154.7 2 . ? C43 C45 H45B 133.2 2 . ? N16 C45 H45B 123.7 2 . ? N16 C45 H45B 108.4 . . ? C44 C45 H45B 95.8 2 . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 117.1 2 . ? N16 C45 H45C 95.2 2 . ? N16 C45 H45C 109.4 . . ? C44 C45 H45C 57.9 2 . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 O8 C46 18.9(19) 2_655 . ? C48 C46 O8 45(4) 2_655 . ? C48 C46 N17 90(4) 2_655 . ? O8 C46 N17 119.5(15) . . ? C48 C46 H46A 108.8 2_655 . ? O8 C46 H46A 115.1 . . ? N17 C46 H46A 117.6 . . ? C46 N17 C46 115.2(16) . 2_655 ? C46 N17 C47 122.4(8) . . ? C46 N17 C47 122.4(8) 2_655 . ? C46 N17 C48 124.9(12) . . ? C46 N17 C48 18.0(13) 2_655 . ? C47 N17 C48 110.7(10) . . ? C46 N17 C48 18.0(13) . 2_655 ? C46 N17 C48 124.9(12) 2_655 2_655 ? C47 N17 C48 110.7(10) . 2_655 ? C48 N17 C48 138.6(19) . 2_655 ? N17 C47 H47A 109.5 . . ? N17 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N17 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 O8 116(5) 2_655 2_655 ? C46 C48 N17 72(4) 2_655 . ? O8 C48 N17 137(2) 2_655 . ? C46 C48 H48A 54.7 2_655 . ? O8 C48 H48A 125.5 2_655 . ? N17 C48 H48A 94.6 . . ? C46 C48 H48B 68.5 2_655 . ? O8 C48 H48B 50.9 2_655 . ? N17 C48 H48B 104.3 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 158.4 2_655 . ? O8 C48 H48C 58.5 2_655 . ? N17 C48 H48C 127.9 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N7 C25 N8 97.6(7) . . ? N7 C25 H25A 115.3 . . ? N8 C25 H25A 113.7 . . ? N7 C25 H25B 109.7 . . ? N8 C25 H25B 110.2 . . ? H25A C25 H25B 109.9 . . ? N7 C25 H26D 119.4 . . ? N8 C25 H26D 142.6 . . ? H25A C25 H26D 56.9 . . ? H25B C25 H26D 54.8 . . ? N7 C25 H30C 110.0 . . ? N8 C25 H30C 20.4 . . ? H25A C25 H30C 118.7 . . ? H25B C25 H30C 90.4 . . ? H26D C25 H30C 126.1 . . ? C30 N8 C25 117.7(9) . . ? C30 N8 C26 111.3(9) . . ? C25 N8 C26 107.0(7) . . ? C30 N8 H30C 84.5 . . ? C25 N8 H30C 43.7 . . ? C26 N8 H30C 149.9 . . ? C30 N8 H30D 102.9 . . ? C25 N8 H30D 126.1 . . ? C26 N8 H30D 20.3 . . ? H30C N8 H30D 169.8 . . ? N8 C26 C27 103.8(6) . . ? N8 C26 H26A 110.3 . . ? C27 C26 H26A 111.8 . . ? N8 C26 H26B 111.2 . . ? C27 C26 H26B 110.9 . . ? H26A C26 H26B 108.8 . . ? N8 C26 H30D 27.2 . . ? C27 C26 H30D 131.0 . . ? H26A C26 H30D 95.8 . . ? H26B C26 H30D 96.1 . . ? C26 C27 N7 102.5(6) . . ? C26 C27 H27A 110.3 . . ? N7 C27 H27A 109.7 . . ? C26 C27 H27B 111.5 . . ? N7 C27 H27B 113.4 . . ? H27A C27 H27B 109.3 . . ? C26 C27 H25C 131.2 . . ? N7 C27 H25C 84.4 . . ? H27A C27 H25C 28.8 . . ? H27B C27 H25C 109.3 . . ? C28 N7 C25 117.3(8) . . ? C28 N7 C27 104.2(8) . . ? C25 N7 C27 103.0(7) . . ? C28 N7 Ni1 108.1(6) . . ? C25 N7 Ni1 108.3(7) . . ? C27 N7 Ni1 116.3(7) . . ? C29 C28 N7 111.8(9) . . ? C29 C28 H28A 114.4 . . ? N7 C28 H28A 112.0 . . ? C29 C28 H28B 103.8 . . ? N7 C28 H28B 106.0 . . ? H28A C28 H28B 108.1 . . ? C29 C28 H27C 101.0 . . ? N7 C28 H27C 120.6 . . ? H28A C28 H27C 96.1 . . ? H28B C28 H27C 15.5 . . ? N9 C29 C28 118.5(9) . . ? N9 C29 H29A 106.7 . . ? C28 C29 H29A 102.8 . . ? N9 C29 H29B 109.2 . . ? C28 C29 H29B 111.1 . . ? H29A C29 H29B 107.8 . . ? N9 C29 H28C 110.5 . . ? C28 C29 H28C 104.6 . . ? H29A C29 H28C 6.4 . . ? H29B C29 H28C 101.5 . . ? N9 C29 H28D 139.1 . . ? C28 C29 H28D 93.6 . . ? H29A C29 H28D 88.3 . . ? H29B C29 H28D 30.8 . . ? H28C C29 H28D 82.1 . . ? N8 C30 N9 124.9(10) . 5_656 ? N8 C30 H30A 105.3 . . ? N9 C30 H30A 105.6 5_656 . ? N8 C30 H30B 107.2 . . ? N9 C30 H30B 106.0 5_656 . ? H30A C30 H30B 106.8 . . ? N8 C30 H30C 23.6 . . ? N9 C30 H30C 123.8 5_656 . ? H30A C30 H30C 84.0 . . ? H30B C30 H30C 124.3 . . ? C29 N9 C30 123.5(9) . 5_656 ? C29 N9 Ni1 109.4(7) . . ? C30 N9 Ni1 110.3(6) 5_656 . ? C29 N9 H9A 102.2 . . ? C30 N9 H9A 103.4 5_656 . ? Ni1 N9 H9A 106.4 . . ? C29 N9 H9'A 140.2 . . ? C30 N9 H9'A 76.9 5_656 . ? Ni1 N9 H9'A 90.6 . . ? H9A N9 H9'A 38.2 . . ? N7' C25' N8' 96.0(11) . . ? N7' C25' H27A 123.2 . . ? N8' C25' H27A 97.3 . . ? N7' C25' H27B 155.6 . . ? N8' C25' H27B 62.8 . . ? H27A C25' H27B 74.2 . . ? N7' C25' H28A 69.2 . . ? N8' C25' H28A 100.3 . . ? H27A C25' H28A 157.2 . . ? H27B C25' H28A 101.2 . . ? N7' C25' H25C 105.8 . . ? N8' C25' H25C 110.4 . . ? H27A C25' H25C 19.7 . . ? H27B C25' H25C 93.6 . . ? H28A C25' H25C 149.3 . . ? N7' C25' H25D 122.7 . . ? N8' C25' H25D 111.0 . . ? H27A C25' H25D 102.9 . . ? H27B C25' H25D 61.1 . . ? H28A C25' H25D 57.1 . . ? H25C C25' H25D 109.9 . . ? C30' N8' C25' 116.9(15) . . ? C30' N8' C26' 111.8(14) . . ? C25' N8' C26' 106.7(10) . . ? C30' N8' H25A 93.8 . . ? C25' N8' H25A 140.0 . . ? C26' N8' H25A 34.3 . . ? C30' N8' H27B 121.5 . . ? C25' N8' H27B 51.5 . . ? C26' N8' H27B 126.6 . . ? H25A N8' H27B 132.9 . . ? C27' C26' N8' 105.0(9) . . ? C27' C26' H25A 163.4 . . ? N8' C26' H25A 71.0 . . ? C27' C26' H26C 116.7 . . ? N8' C26' H26C 106.9 . . ? H25A C26' H26C 79.6 . . ? C27' C26' H26D 106.0 . . ? N8' C26' H26D 113.5 . . ? H25A C26' H26D 63.2 . . ? H26C C26' H26D 109.0 . . ? C26' C27' N7' 103.1(8) . . ? C26' C27' H28B 101.6 . . ? N7' C27' H28B 81.5 . . ? C26' C27' H27C 105.6 . . ? N7' C27' H27C 111.7 . . ? H28B C27' H27C 32.6 . . ? C26' C27' H27D 116.2 . . ? N7' C27' H27D 111.0 . . ? H28B C27' H27D 134.7 . . ? H27C C27' H27D 109.1 . . ? C28' N7' C25' 112.6(12) . . ? C28' N7' C27' 111.0(13) . . ? C25' N7' C27' 107.6(11) . . ? C28' N7' Ni1 111.9(12) . . ? C25' N7' Ni1 106.1(16) . . ? C27' N7' Ni1 107.3(19) . . ? N7' C28' C29' 111.5(13) . . ? N7' C28' H29A 92.6 . . ? C29' C28' H29A 100.6 . . ? N7' C28' H29B 112.6 . . ? C29' C28' H29B 90.8 . . ? H29A C28' H29B 146.3 . . ? N7' C28' H28C 105.4 . . ? C29' C28' H28C 100.8 . . ? H29A C28' H28C 14.1 . . ? H29B C28' H28C 132.6 . . ? N7' C28' H28D 110.4 . . ? C29' C28' H28D 119.2 . . ? H29A C28' H28D 119.2 . . ? H29B C28' H28D 32.2 . . ? H28C C28' H28D 108.1 . . ? N9' C29' C28' 113.8(14) . . ? N9' C29' H29C 107.6 . . ? C28' C29' H29C 117.6 . . ? N9' C29' H29D 109.7 . . ? C28' C29' H29D 99.5 . . ? H29C C29' H29D 108.0 . . ? N9' C30' N8' 136.8(17) 5_656 . ? N9' C30' H30C 98.8 5_656 . ? N8' C30' H30C 101.7 . . ? N9' C30' H30D 104.8 5_656 . ? N8' C30' H30D 106.0 . . ? H30C C30' H30D 104.8 . . ? C29' N9' C30' 122.2(18) . 5_656 ? C29' N9' Ni1 114.6(14) . . ? C30' N9' Ni1 102.1(13) 5_656 . ? C29' N9' H9A 74.2 . . ? C30' N9' H9A 145.7 5_656 . ? Ni1 N9' H9A 95.8 . . ? C29' N9' H9'A 106.7 . . ? C30' N9' H9'A 104.1 5_656 . ? Ni1 N9' H9'A 105.6 . . ? H9A N9' H9'A 42.3 . . ? N1 C1 N2 126.7(5) . . ? N1 C1 N4 120.4(5) . . ? N2 C1 N4 112.8(5) . . ? N2 C2 N5 119.4(6) . . ? N2 C2 N3 126.6(6) . . ? N5 C2 N3 114.0(5) . . ? N3 C3 N1 127.2(5) . . ? N3 C3 N6 120.8(5) . . ? N1 C3 N6 112.1(5) . . ? C5 C4 C9 120.8(6) . . ? C5 C4 N4 123.9(5) . . ? C9 C4 N4 115.4(5) . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 121.3(6) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 118.4(6) . . ? C6 C7 C10 122.0(6) . . ? C8 C7 C10 119.6(6) . . ? C9 C8 C7 121.2(6) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C4 119.1(6) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? O1 C10 O2 124.6(6) . . ? O1 C10 C7 117.6(7) . . ? O2 C10 C7 117.7(7) . . ? C12 C11 N5 125.9(6) . . ? C12 C11 C16 116.9(6) . . ? N5 C11 C16 117.1(6) . . ? C13 C12 C11 120.0(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 122.7(6) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 116.2(6) . . ? C15 C14 C17 121.2(6) . . ? C13 C14 C17 122.6(6) . . ? C16 C15 C14 123.0(7) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 C16 C11 121.1(6) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? O4 C17 O3 124.4(7) . . ? O4 C17 C14 118.1(7) . . ? O3 C17 C14 117.4(7) . . ? C23 C18 C19 118.5(6) . . ? C23 C18 N6 118.9(6) . . ? C19 C18 N6 122.5(6) . . ? C18 C19 C20 119.3(6) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 122.0(6) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 117.4(6) . . ? C22 C21 C24 122.5(7) . . ? C20 C21 C24 120.1(7) . . ? C23 C22 C21 120.7(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C18 C23 C22 122.0(6) . . ? C18 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? O6 C24 O5 127.6(7) . . ? O6 C24 C21 116.6(7) . . ? O5 C24 C21 115.7(8) . . ? N10 C31 N11 105.0(10) . . ? N10 C31 H31A 110.7 . . ? N11 C31 H31A 110.7 . . ? N10 C31 H31B 110.7 . . ? N11 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? N11 C32 C33 103.1(9) . . ? N11 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? N11 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? N10 C33 C32 104.9(8) . . ? N10 C33 H33A 110.8 . . ? C32 C33 H33A 110.8 . . ? N10 C33 H33B 110.8 . . ? C32 C33 H33B 110.8 . . ? H33A C33 H33B 108.8 . . ? C35 C34 N10 111.5(7) . . ? C35 C34 H34A 109.3 . . ? N10 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? N10 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? N12 C35 C34 108.4(7) . . ? N12 C35 H35A 110.0 . . ? C34 C35 H35A 110.0 . . ? N12 C35 H35B 110.0 . . ? C34 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? N12 C36 N11 114.5(7) 7_565 . ? N12 C36 H36A 108.6 7_565 . ? N11 C36 H36A 108.6 . . ? N12 C36 H36B 108.6 7_565 . ? N11 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? N14 C37 N13 102.5(7) . . ? N14 C37 H37A 111.3 . . ? N13 C37 H37A 111.3 . . ? N14 C37 H37B 111.3 . . ? N13 C37 H37B 111.3 . . ? H37A C37 H37B 109.2 . . ? N14 C38 C39 104.3(7) . . ? N14 C38 H38A 110.9 . . ? C39 C38 H38A 110.9 . . ? N14 C38 H38B 110.9 . . ? C39 C38 H38B 110.9 . . ? H38A C38 H38B 108.9 . . ? N13 C39 C38 102.7(7) . . ? N13 C39 H39A 111.2 . . ? C38 C39 H39A 111.2 . . ? N13 C39 H39B 111.2 . . ? C38 C39 H39B 111.2 . . ? H39A C39 H39B 109.1 . . ? C41 C40 N13 112.5(8) . . ? C41 C40 H40A 109.1 . . ? N13 C40 H40A 109.1 . . ? C41 C40 H40B 109.1 . . ? N13 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? N15 C41 C40 104.7(6) . . ? N15 C41 H41A 110.8 . . ? C40 C41 H41A 110.8 . . ? N15 C41 H41B 110.8 . . ? C40 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? N14 C42 N15 117.4(7) . 7_667 ? N14 C42 H42A 108.0 . . ? N15 C42 H42A 108.0 7_667 . ? N14 C42 H42B 108.0 . . ? N15 C42 H42B 108.0 7_667 . ? H42A C42 H42B 107.2 . . ? C1 N1 C3 113.0(5) . . ? C2 N2 C1 112.9(5) . . ? C3 N3 C2 113.4(5) . . ? C1 N4 C4 132.0(5) . . ? C1 N4 H4 114.0 . . ? C4 N4 H4 114.0 . . ? C2 N5 C11 131.5(5) . . ? C2 N5 H5A 114.3 . . ? C11 N5 H5A 114.3 . . ? C3 N6 C18 130.4(5) . . ? C3 N6 H6A 114.8 . . ? C18 N6 H6A 114.8 . . ? C31 N10 C33 99.4(8) . . ? C31 N10 C34 118.5(9) . . ? C33 N10 C34 110.6(8) . . ? C31 N10 Ni2 109.2(6) . . ? C33 N10 Ni2 115.7(6) . . ? C34 N10 Ni2 104.1(5) . . ? C31 N11 C36 116.2(9) . . ? C31 N11 C32 104.2(10) . . ? C36 N11 C32 111.5(10) . . ? C35 N12 C36 112.2(7) . 7_565 ? C35 N12 Ni2 108.8(5) . . ? C36 N12 Ni2 117.6(5) 7_565 . ? C35 N12 H12A 105.8 . . ? C36 N12 H12A 105.8 7_565 . ? Ni2 N12 H12A 105.8 . . ? C39 N13 C40 113.5(7) . . ? C39 N13 C37 102.5(6) . . ? C40 N13 C37 115.4(7) . . ? C39 N13 Ni3 116.9(5) . . ? C40 N13 Ni3 102.2(5) . . ? C37 N13 Ni3 106.7(5) . . ? C37 N14 C42 113.3(7) . . ? C37 N14 C38 105.3(7) . . ? C42 N14 C38 113.1(7) . . ? C42 N15 C41 114.7(6) 7_667 . ? C42 N15 Ni3 115.1(6) 7_667 . ? C41 N15 Ni3 107.9(5) . . ? C42 N15 H15A 106.2 7_667 . ? C41 N15 H15A 106.2 . . ? Ni3 N15 H15A 106.2 . . ? N9' Ni1 N9' 179.997(3) 5_656 . ? N9' Ni1 N9 153.9(6) 5_656 . ? N9' Ni1 N9 26.1(6) . . ? N9' Ni1 N9 26.1(6) 5_656 5_656 ? N9' Ni1 N9 153.9(6) . 5_656 ? N9 Ni1 N9 179.999(2) . 5_656 ? N9' Ni1 N7 109.4(6) 5_656 5_656 ? N9' Ni1 N7 70.6(6) . 5_656 ? N9 Ni1 N7 96.5(3) . 5_656 ? N9 Ni1 N7 83.5(3) 5_656 5_656 ? N9' Ni1 N7 70.6(6) 5_656 . ? N9' Ni1 N7 109.4(6) . . ? N9 Ni1 N7 83.5(3) . . ? N9 Ni1 N7 96.5(3) 5_656 . ? N7 Ni1 N7 179.998(1) 5_656 . ? N9' Ni1 O1 90.0(7) 5_656 5_656 ? N9' Ni1 O1 90.0(7) . 5_656 ? N9 Ni1 O1 85.9(3) . 5_656 ? N9 Ni1 O1 94.1(3) 5_656 5_656 ? N7 Ni1 O1 90.1(3) 5_656 5_656 ? N7 Ni1 O1 89.9(3) . 5_656 ? N9' Ni1 O1 90.0(7) 5_656 . ? N9' Ni1 O1 90.0(7) . . ? N9 Ni1 O1 94.1(3) . . ? N9 Ni1 O1 85.9(3) 5_656 . ? N7 Ni1 O1 89.9(3) 5_656 . ? N7 Ni1 O1 90.1(3) . . ? O1 Ni1 O1 179.997(1) 5_656 . ? N9' Ni1 N7' 104.0(8) 5_656 . ? N9' Ni1 N7' 76.0(8) . . ? N9 Ni1 N7' 49.8(6) . . ? N9 Ni1 N7' 130.2(6) 5_656 . ? N7 Ni1 N7' 145.8(5) 5_656 . ? N7 Ni1 N7' 34.2(5) . . ? O1 Ni1 N7' 82.7(7) 5_656 . ? O1 Ni1 N7' 97.3(7) . . ? N9' Ni1 N7' 76.0(8) 5_656 5_656 ? N9' Ni1 N7' 104.0(8) . 5_656 ? N9 Ni1 N7' 130.2(6) . 5_656 ? N9 Ni1 N7' 49.8(6) 5_656 5_656 ? N7 Ni1 N7' 34.2(5) 5_656 5_656 ? N7 Ni1 N7' 145.8(5) . 5_656 ? O1 Ni1 N7' 97.3(7) 5_656 5_656 ? O1 Ni1 N7' 82.7(7) . 5_656 ? N7' Ni1 N7' 179.998(3) . 5_656 ? N12 Ni2 N12 179.998(1) . 7_565 ? N12 Ni2 N10 95.1(3) . 7_565 ? N12 Ni2 N10 84.9(3) 7_565 7_565 ? N12 Ni2 N10 84.9(3) . . ? N12 Ni2 N10 95.1(3) 7_565 . ? N10 Ni2 N10 180.0 7_565 . ? N12 Ni2 O3 93.6(2) . . ? N12 Ni2 O3 86.4(2) 7_565 . ? N10 Ni2 O3 90.2(2) 7_565 . ? N10 Ni2 O3 89.8(2) . . ? N12 Ni2 O3 86.4(2) . 7_565 ? N12 Ni2 O3 93.6(2) 7_565 7_565 ? N10 Ni2 O3 89.8(2) 7_565 7_565 ? N10 Ni2 O3 90.2(2) . 7_565 ? O3 Ni2 O3 180.0 . 7_565 ? N15 Ni3 N15 179.999(1) 7_667 . ? N15 Ni3 N13 85.0(3) 7_667 7_667 ? N15 Ni3 N13 95.0(3) . 7_667 ? N15 Ni3 N13 95.0(3) 7_667 . ? N15 Ni3 N13 85.0(3) . . ? N13 Ni3 N13 179.998(2) 7_667 . ? N15 Ni3 O5 92.2(2) 7_667 . ? N15 Ni3 O5 87.8(2) . . ? N13 Ni3 O5 90.2(2) 7_667 . ? N13 Ni3 O5 89.8(2) . . ? N15 Ni3 O5 87.8(2) 7_667 7_667 ? N15 Ni3 O5 92.2(2) . 7_667 ? N13 Ni3 O5 89.8(2) 7_667 7_667 ? N13 Ni3 O5 90.2(2) . 7_667 ? O5 Ni3 O5 179.998(1) . 7_667 ? C10 O1 Ni1 134.1(4) . . ? C17 O3 Ni2 134.9(4) . . ? C24 O5 Ni3 133.5(5) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.261 1.003 0.226 183 64 ' ' 2 0.761 0.503 0.226 183 64 ' ' 3 0.239 0.503 0.273 183 67 ' ' 4 0.739 0.003 0.273 183 67 ' ' 5 0.261 -0.003 0.726 183 65 ' ' 6 0.761 0.497 0.726 183 65 ' ' 7 0.239 0.497 0.773 183 67 ' ' 8 0.739 -0.003 0.773 183 67 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.639 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 934236' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '15848_web_deposit_cif_file_0_XiangJiang_1354511394.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H114 N24 Ni3 O18' _chemical_formula_weight 2068.24 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.589(4) _cell_length_b 17.784(9) _cell_length_c 38.729(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.629(11) _cell_angle_gamma 90.00 _cell_volume 5773(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1149 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 19.49 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9610 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20808 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.1688 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10183 _reflns_number_gt 4149 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0405P)^2^+1.0000P] 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 9766 _refine_ls_number_parameters 600 _refine_ls_number_restraints 375 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 N4 N 0.0313(6) 0.4774(3) 0.05257(13) 0.0443(15) Uiso 0.674(9) 1 d PD . 1 H4A H -0.0319 0.5091 0.0614 0.053 Uiso 0.674(9) 1 d PR . 1 C32 C 0.1922(12) 0.4964(7) 0.0706(2) 0.048(9) Uiso 0.674(9) 1 d PD . 1 H32B H 0.2637 0.4604 0.0640 0.058 Uiso 0.674(9) 1 d PR . 1 H32D H 0.2070 0.4963 0.0959 0.058 Uiso 0.674(9) 1 d PR . 1 C33 C 0.2277(15) 0.5729(6) 0.0557(2) 0.071(4) Uiso 0.674(9) 1 d PD . 1 H33A H 0.3358 0.5879 0.0655 0.086 Uiso 0.674(9) 1 d PR . 1 H33B H 0.1578 0.6087 0.0631 0.086 Uiso 0.674(9) 1 d PR . 1 N5 N 0.1986(8) 0.5729(4) 0.0176(2) 0.040(3) Uiso 0.674(9) 1 d PD . 1 C34 C 0.1524(12) 0.6462(5) -0.0001(2) 0.056(4) Uiso 0.674(9) 1 d PD . 1 H34A H 0.2190 0.6869 0.0108 0.067 Uiso 0.674(9) 1 d PR . 1 H34B H 0.0431 0.6571 0.0001 0.067 Uiso 0.674(9) 1 d PR . 1 C35 C 0.3064(12) 0.5798(6) -0.0340(2) 0.074(4) Uiso 0.674(9) 1 d PD . 1 H35A H 0.2815 0.5398 -0.0510 0.088 Uiso 0.674(9) 1 d PR . 1 H35B H 0.3968 0.6071 -0.0383 0.088 Uiso 0.674(9) 1 d PR . 1 C36 C 0.3423(10) 0.5517(6) 0.0048(2) 0.057(4) Uiso 0.674(9) 1 d PD . 1 H36A H 0.3586 0.4966 0.0059 0.068 Uiso 0.674(9) 1 calc PR . 1 H36B H 0.4385 0.5766 0.0189 0.068 Uiso 0.674(9) 1 calc PR . 1 N6 N 0.1683(9) 0.6312(5) -0.0368(2) 0.055(3) Uiso 0.674(9) 1 d PD . 1 C37 C 0.0230(13) 0.5981(5) -0.0586(2) 0.044(8) Uiso 0.674(9) 1 d PD . 1 H37A H 0.0340 0.6016 -0.0827 0.053 Uiso 0.674(9) 1 d PR . 1 H37B H -0.0634 0.6308 -0.0565 0.053 Uiso 0.674(9) 1 d PR . 1 C32' C 0.037(3) 0.5949(12) -0.0577(4) 0.10(3) Uiso 0.326(9) 1 d PD . 2 H32A H 0.0428 0.6049 -0.0818 0.151 Uiso 0.326(9) 1 d PR . 2 H32C H -0.0226 0.6340 -0.0495 0.151 Uiso 0.326(9) 1 d PR . 2 C33' C 0.2073(18) 0.5934(12) -0.0336(3) 0.093(11) Uiso 0.326(9) 1 d PD . 2 H33C H 0.2601 0.6406 -0.0347 0.111 Uiso 0.326(9) 1 d PR . 2 H33D H 0.2684 0.5546 -0.0416 0.111 Uiso 0.326(9) 1 d PR . 2 N5' N 0.1910(12) 0.5767(6) 0.0024(3) 0.032(5) Uiso 0.326(9) 1 d PD . 2 C34' C 0.3346(12) 0.5428(9) 0.0254(3) 0.045(7) Uiso 0.326(9) 1 d PD . 2 H34C H 0.4311 0.5688 0.0242 0.054 Uiso 0.326(9) 1 d PR . 2 H34D H 0.3433 0.4908 0.0193 0.054 Uiso 0.326(9) 1 d PR . 2 C35' C 0.210(3) 0.6232(11) 0.0607(4) 0.080(8) Uiso 0.326(9) 1 d PDU . 2 H35C H 0.1204 0.6164 0.0715 0.096 Uiso 0.326(9) 1 d PR . 2 H35D H 0.2795 0.6606 0.0737 0.096 Uiso 0.326(9) 1 d PR . 2 C36' C 0.1633(19) 0.6455(6) 0.0209(4) 0.056(7) Uiso 0.326(9) 1 d PDU . 2 H36C H 0.0508 0.6556 0.0150 0.067 Uiso 0.326(9) 1 d PR . 2 H36D H 0.2199 0.6889 0.0155 0.067 Uiso 0.326(9) 1 d PR . 2 N6' N 0.298(2) 0.5512(9) 0.0603(4) 0.083(9) Uiso 0.326(9) 1 d PD . 2 C37' C 0.1996(17) 0.4892(13) 0.0695(4) 0.09(3) Uiso 0.326(9) 1 d PD . 2 H37C H 0.2109 0.4902 0.0947 0.104 Uiso 0.326(9) 1 d PR . 2 H37D H 0.2516 0.4443 0.0641 0.104 Uiso 0.326(9) 1 d PR . 2 N4' N 0.0313(6) 0.4774(3) 0.05257(13) 0.0443(15) Uiso 0.326(9) 1 d PD . 2 H4'A H -0.0272 0.5190 0.0639 0.053 Uiso 0.326(9) 1 d PR . 2 N7 N 0.3969(6) -0.1524(3) 0.34741(13) 0.0439(15) Uiso 0.521(6) 1 d PD A 3 H7A H 0.4489 -0.1191 0.3365 0.053 Uiso 0.521(6) 1 d PR A 3 C38 C 0.2502(13) -0.1143(11) 0.3513(3) 0.060(8) Uiso 0.521(6) 1 d PD A 3 H38A H 0.2759 -0.0647 0.3606 0.072 Uiso 0.521(6) 1 d PR A 3 H38B H 0.2097 -0.1417 0.3688 0.072 Uiso 0.521(6) 1 d PR A 3 N8 N 0.1188(12) -0.1073(6) 0.3205(3) 0.056(4) Uiso 0.521(6) 1 d PD A 3 C39 C 0.0436(14) -0.1799(6) 0.3082(3) 0.050(4) Uiso 0.521(6) 1 d PD A 3 H39A H -0.0665 -0.1741 0.2966 0.060 Uiso 0.521(6) 1 d PR A 3 H39B H 0.0534 -0.2148 0.3275 0.060 Uiso 0.521(6) 1 d PR A 3 C40 C 0.1624(16) -0.1377(6) 0.2624(3) 0.052(4) Uiso 0.521(6) 1 d PD A 3 H40A H 0.2589 -0.1422 0.2539 0.063 Uiso 0.521(6) 1 d PR A 3 H40B H 0.0732 -0.1309 0.2429 0.063 Uiso 0.521(6) 1 d PR A 3 C41 C 0.1710(16) -0.0744(7) 0.2898(3) 0.058(4) Uiso 0.521(6) 1 d PD A 3 H41A H 0.2791 -0.0572 0.2973 0.069 Uiso 0.521(6) 1 d PR A 3 H41B H 0.1052 -0.0324 0.2802 0.069 Uiso 0.521(6) 1 d PR A 3 N9 N 0.1493(17) -0.2032(7) 0.2845(3) 0.044(10) Uiso 0.521(6) 1 d PD A 3 C42 C 0.0898(14) -0.2699(6) 0.2633(4) 0.049(4) Uiso 0.521(6) 1 d PD A 3 H42A H 0.0101 -0.2575 0.2426 0.058 Uiso 0.521(6) 1 d PR A 3 H42B H 0.0407 -0.3020 0.2778 0.058 Uiso 0.521(6) 1 d PR A 3 C43 C 0.2221(17) -0.3176(12) 0.2521(3) 0.041(8) Uiso 0.521(6) 1 d PD A 3 H43A H 0.2819 -0.2857 0.2398 0.050 Uiso 0.521(6) 1 d PR A 3 H43B H 0.1791 -0.3588 0.2369 0.050 Uiso 0.521(6) 1 d PR A 3 N10 N 0.3282(6) -0.3392(3) 0.28516(12) 0.0410(15) Uiso 0.521(6) 1 d PD A 3 H10A H 0.2743 -0.3735 0.2951 0.049 Uiso 0.521(6) 1 d PR A 3 C44 C 0.4801(13) -0.3730(12) 0.2829(3) 0.042(8) Uiso 0.521(6) 1 d PD A 3 H44A H 0.5188 -0.3429 0.2660 0.050 Uiso 0.521(6) 1 d PR A 3 H44B H 0.4617 -0.4226 0.2731 0.050 Uiso 0.521(6) 1 d PR A 3 N11 N 0.6125(13) -0.3810(6) 0.3135(3) 0.062(4) Uiso 0.521(6) 1 d PD A 3 C45 C 0.6863(15) -0.3081(6) 0.3259(3) 0.057(4) Uiso 0.521(6) 1 d PD A 3 H45A H 0.6742 -0.2733 0.3066 0.069 Uiso 0.521(6) 1 d PR A 3 H45B H 0.7969 -0.3126 0.3374 0.069 Uiso 0.521(6) 1 d PR A 3 C46 C 0.5643(15) -0.3522(6) 0.3700(3) 0.050(4) Uiso 0.521(6) 1 d PD A 3 H46A H 0.6523 -0.3580 0.3899 0.060 Uiso 0.521(6) 1 d PR A 3 H46B H 0.4665 -0.3499 0.3781 0.060 Uiso 0.521(6) 1 d PR A 3 C47 C 0.5602(17) -0.4169(7) 0.3433(3) 0.066(5) Uiso 0.521(6) 1 d PD A 3 H47A H 0.6324 -0.4567 0.3528 0.079 Uiso 0.521(6) 1 d PR A 3 H47B H 0.4547 -0.4373 0.3358 0.079 Uiso 0.521(6) 1 d PR A 3 N12 N 0.5756(17) -0.2845(7) 0.3489(4) 0.055(7) Uiso 0.521(6) 1 d PD A 3 C48 C 0.6369(18) -0.2203(7) 0.3713(4) 0.073(6) Uiso 0.521(6) 1 d PD A 3 H48A H 0.6997 -0.1898 0.3590 0.088 Uiso 0.521(6) 1 d PR A 3 H48B H 0.7057 -0.2370 0.3929 0.088 Uiso 0.521(6) 1 d PR A 3 C49 C 0.5029(18) -0.1730(12) 0.3810(3) 0.051(5) Uiso 0.521(6) 1 d PDU A 3 H49A H 0.4466 -0.2000 0.3960 0.061 Uiso 0.521(6) 1 d PR A 3 H49B H 0.5477 -0.1283 0.3932 0.061 Uiso 0.521(6) 1 d PR A 3 N7' N 0.3282(6) -0.3392(3) 0.28516(12) 0.0410(15) Uiso 0.479(6) 1 d PD A 4 H7'A H 0.2664 -0.3738 0.2970 0.049 Uiso 0.479(6) 1 d PR A 4 C38' C 0.2291(19) -0.3297(11) 0.2498(3) 0.063(12) Uiso 0.479(6) 1 d PD A 4 H38C H 0.1909 -0.3781 0.2407 0.076 Uiso 0.479(6) 1 d PR A 4 H38D H 0.2973 -0.3112 0.2351 0.076 Uiso 0.479(6) 1 d PR A 4 N8' N 0.0913(13) -0.2790(6) 0.2443(3) 0.065(4) Uiso 0.479(6) 1 d PD A 4 C39' C 0.1350(16) -0.1988(7) 0.2494(3) 0.056(5) Uiso 0.479(6) 1 d PD A 4 H39C H 0.0550 -0.1661 0.2360 0.067 Uiso 0.479(6) 1 d PR A 4 H39D H 0.2369 -0.1888 0.2439 0.067 Uiso 0.479(6) 1 d PR A 4 C40' C -0.0011(17) -0.2327(8) 0.2935(4) 0.072(6) Uiso 0.479(6) 1 d PD A 4 H40C H 0.0203 -0.2506 0.3175 0.087 Uiso 0.479(6) 1 d PR A 4 H40D H -0.0933 -0.2006 0.2894 0.087 Uiso 0.479(6) 1 d PR A 4 C41' C -0.0190(17) -0.2987(8) 0.2674(4) 0.071(5) Uiso 0.479(6) 1 d PD A 4 H41C H 0.0124 -0.3457 0.2790 0.085 Uiso 0.479(6) 1 d PR A 4 H41D H -0.1272 -0.3028 0.2542 0.085 Uiso 0.479(6) 1 d PR A 4 N9' N 0.146(2) -0.1945(9) 0.2875(4) 0.056(12) Uiso 0.479(6) 1 d PD A 4 C42' C 0.161(2) -0.1190(9) 0.3029(4) 0.081(6) Uiso 0.479(6) 1 d PD A 4 H42C H 0.0600 -0.0932 0.2985 0.097 Uiso 0.479(6) 1 d PR A 4 H42D H 0.2277 -0.0921 0.2903 0.097 Uiso 0.479(6) 1 d PR A 4 C43' C 0.2406(18) -0.1143(15) 0.3432(4) 0.076(10) Uiso 0.479(6) 1 d PD A 4 H43C H 0.1774 -0.1392 0.3573 0.091 Uiso 0.479(6) 1 d PR A 4 H43D H 0.2515 -0.0622 0.3498 0.091 Uiso 0.479(6) 1 d PR A 4 N10' N 0.3969(6) -0.1524(3) 0.34741(13) 0.0439(15) Uiso 0.479(6) 1 d PD A 4 H10B H 0.4586 -0.1186 0.3379 0.053 Uiso 0.479(6) 1 d PR A 4 C44' C 0.4844(19) -0.1652(12) 0.3831(3) 0.059(6) Uiso 0.479(6) 1 d PDU A 4 H44C H 0.4097 -0.1893 0.3946 0.071 Uiso 0.479(6) 1 d PR A 4 H44D H 0.5161 -0.1188 0.3954 0.071 Uiso 0.479(6) 1 d PR A 4 N11' N 0.6206(13) -0.2157(6) 0.3869(3) 0.054(4) Uiso 0.479(6) 1 d PD A 4 C45' C 0.5750(16) -0.2956(7) 0.3807(3) 0.054(5) Uiso 0.479(6) 1 d PD A 4 H45C H 0.4722 -0.3070 0.3853 0.065 Uiso 0.479(6) 1 d PR A 4 H45D H 0.6543 -0.3290 0.3937 0.065 Uiso 0.479(6) 1 d PR A 4 C46' C 0.7237(16) -0.2612(8) 0.3389(4) 0.069(5) Uiso 0.479(6) 1 d PD A 4 H46C H 0.8168 -0.2926 0.3428 0.083 Uiso 0.479(6) 1 d PR A 4 H46D H 0.7044 -0.2404 0.3155 0.083 Uiso 0.479(6) 1 d PR A 4 C47' C 0.7361(15) -0.1968(7) 0.3662(3) 0.053(5) Uiso 0.479(6) 1 d PD A 4 H47C H 0.8434 -0.1932 0.3799 0.064 Uiso 0.479(6) 1 d PR A 4 H47D H 0.7047 -0.1488 0.3556 0.064 Uiso 0.479(6) 1 d PR A 4 N12' N 0.5747(16) -0.2984(8) 0.3430(3) 0.043(6) Uiso 0.479(6) 1 d PD A 4 C48' C 0.555(2) -0.3736(8) 0.3277(4) 0.075(6) Uiso 0.479(6) 1 d PD A 4 H48C H 0.4963 -0.4033 0.3412 0.090 Uiso 0.479(6) 1 d PR A 4 H48D H 0.6595 -0.3958 0.3312 0.090 Uiso 0.479(6) 1 d PR A 4 C49' C 0.477(2) -0.3795(16) 0.2881(4) 0.076(13) Uiso 0.479(6) 1 d PD A 4 H49C H 0.5378 -0.3573 0.2728 0.091 Uiso 0.479(6) 1 d PR A 4 H49D H 0.4596 -0.4318 0.2823 0.091 Uiso 0.479(6) 1 d PR A 4 C1 C 0.6772(6) 0.0050(4) 0.04857(14) 0.0261(15) Uani 1 1 d U . . C2 C 0.6946(7) -0.0289(4) 0.08093(15) 0.0310(17) Uani 1 1 d . . . H2 H 0.6316 -0.0118 0.0967 0.037 Uiso 1 1 calc R . . C3 C 0.8017(7) -0.0876(4) 0.09139(16) 0.0311(17) Uani 1 1 d . . . C4 C 0.8917(7) -0.1145(4) 0.06870(16) 0.0338(17) Uani 1 1 d . . . H4 H 0.9642 -0.1548 0.0759 0.041 Uiso 1 1 calc R . . C5 C 0.8765(7) -0.0829(4) 0.03529(16) 0.0280(16) Uani 1 1 d . . . C6 C 0.7718(7) -0.0224(3) 0.02591(15) 0.0292(16) Uani 1 1 d U . . H6 H 0.7643 0.0010 0.0035 0.035 Uiso 1 1 calc R . . C7 C 0.5622(8) 0.0670(4) 0.03793(17) 0.0323(17) Uani 1 1 d . . . C8 C 0.4958(8) 0.1831(4) 0.00351(17) 0.0341(17) Uani 1 1 d . . . C9 C 0.4344(8) 0.2239(4) 0.02818(18) 0.051(2) Uani 1 1 d . . . H9 H 0.4568 0.2089 0.0523 0.061 Uiso 1 1 calc R . . C10 C 0.3417(7) 0.2857(4) 0.01749(17) 0.0386(18) Uani 1 1 d . . . H10 H 0.2961 0.3125 0.0341 0.046 Uiso 1 1 calc R . . C11 C 0.3133(8) 0.3101(4) -0.01803(17) 0.0360(17) Uani 1 1 d . . . C12 C 0.3785(8) 0.2704(4) -0.04187(19) 0.0440(19) Uani 1 1 d . . . H12 H 0.3617 0.2862 -0.0658 0.053 Uiso 1 1 calc R . . C13 C 0.4688(8) 0.2071(4) -0.03057(17) 0.0395(18) Uani 1 1 d . . . H13 H 0.5132 0.1797 -0.0471 0.047 Uiso 1 1 calc R . . C14 C 0.2075(8) 0.3797(4) -0.0279(2) 0.049(2) Uani 1 1 d U . . C16 C 0.8051(8) -0.1272(5) 0.12682(18) 0.0423(19) Uani 1 1 d . . . C17 C 0.7455(8) -0.0999(4) 0.18547(19) 0.044(2) Uani 1 1 d . . . C18 C 0.6637(9) -0.1667(5) 0.18920(19) 0.061(2) Uani 1 1 d . . . H18 H 0.6459 -0.2029 0.1707 0.073 Uiso 1 1 calc R . . C19 C 0.6101(8) -0.1800(5) 0.21897(19) 0.056(2) Uani 1 1 d . . . H19 H 0.5570 -0.2260 0.2213 0.068 Uiso 1 1 calc R . . C20 C 0.6311(8) -0.1278(4) 0.24612(18) 0.0416(19) Uani 1 1 d . . . C21 C 0.7187(9) -0.0627(4) 0.24349(18) 0.051(2) Uani 1 1 d . . . H21 H 0.7382 -0.0274 0.2624 0.061 Uiso 1 1 calc R . . C22 C 0.7776(8) -0.0492(4) 0.21336(17) 0.0421(19) Uani 1 1 d . . . H22 H 0.8396 -0.0056 0.2119 0.051 Uiso 1 1 calc R . . C23 C 0.5640(9) -0.1401(5) 0.2776(2) 0.055(2) Uani 1 1 d . . . C24 C 0.9716(8) -0.1108(4) 0.01038(17) 0.0355(18) Uani 1 1 d . . . C25 C 0.9602(7) -0.1223(4) -0.05427(15) 0.0267(16) Uani 1 1 d . . . C26 C 1.0597(7) -0.1824(4) -0.05599(17) 0.0348(17) Uani 1 1 d . . . H26 H 1.0836 -0.2178 -0.0372 0.042 Uiso 1 1 calc R . . C27 C 1.1252(7) -0.1902(4) -0.08613(16) 0.0315(17) Uani 1 1 d . . . H27 H 1.1927 -0.2318 -0.0877 0.038 Uiso 1 1 calc R . . C28 C 1.0932(7) -0.1390(4) -0.11310(16) 0.0283(16) Uani 1 1 d . . . C29 C 0.9922(7) -0.0784(4) -0.11107(16) 0.0321(17) Uani 1 1 d . . . H29 H 0.9705 -0.0425 -0.1297 0.038 Uiso 1 1 calc R . . C30 C 0.9231(7) -0.0705(4) -0.08208(16) 0.0330(17) Uani 1 1 d . . . H30 H 0.8514 -0.0303 -0.0811 0.040 Uiso 1 1 calc R . . C31 C 1.1721(8) -0.1437(5) -0.14404(17) 0.043(2) Uani 1 1 d . . . N1 N 0.5888(6) 0.1176(3) 0.01400(13) 0.0311(13) Uani 1 1 d . . . H1 H 0.6702 0.1094 0.0041 0.037 Uiso 1 1 calc R . . N2 N 0.7889(6) -0.0786(3) 0.15337(14) 0.0417(15) Uani 1 1 d . . . H2A H 0.8067 -0.0306 0.1503 0.050 Uiso 1 1 calc R . . N3 N 0.8940(6) -0.1082(3) -0.02407(13) 0.0365(15) Uani 1 1 d . . . H3 H 0.7920 -0.0967 -0.0283 0.044 Uiso 1 1 calc R . . Ni2 Ni 0.36180(9) -0.24523(6) 0.31608(2) 0.0365(3) Uani 1 1 d . . . Ni1 Ni 0.0000 0.5000 0.0000 0.0339(3) Uani 1 2 d SD . . O1 O 0.4429(5) 0.0702(3) 0.05168(11) 0.0451(13) Uani 1 1 d . . . O2 O 0.1545(5) 0.4104(2) -0.00375(12) 0.0376(12) Uani 1 1 d U . . O3 O 0.1830(6) 0.4012(3) -0.06030(13) 0.0642(16) Uani 1 1 d . . . O4 O 0.8207(6) -0.1944(3) 0.12940(12) 0.0609(15) Uani 1 1 d . . . O5 O 0.4844(5) -0.1995(3) 0.27965(11) 0.0447(13) Uani 1 1 d . A . O6 O 0.5833(7) -0.0884(3) 0.30227(14) 0.0717(17) Uani 1 1 d . . . O7 O 1.1146(6) -0.1295(3) 0.01971(12) 0.0563(15) Uani 1 1 d . . . O8 O 1.2350(5) -0.2078(3) -0.14779(10) 0.0383(12) Uani 1 1 d . . . O9 O 1.1698(6) -0.0879(3) -0.16312(13) 0.0615(16) Uani 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 C1 0.023(3) 0.039(4) 0.017(3) 0.000(3) 0.008(3) 0.010(3) C2 0.034(4) 0.039(5) 0.022(4) 0.000(3) 0.010(3) 0.002(3) C3 0.031(4) 0.034(4) 0.030(4) 0.008(3) 0.010(3) 0.009(3) C4 0.038(4) 0.034(4) 0.030(4) 0.010(3) 0.007(3) 0.005(3) C5 0.029(4) 0.035(4) 0.025(4) -0.003(3) 0.016(3) 0.012(3) C6 0.029(4) 0.030(4) 0.023(4) 0.005(3) -0.005(3) 0.002(3) C7 0.042(4) 0.025(4) 0.029(4) -0.003(3) 0.008(3) 0.006(4) C8 0.038(4) 0.031(4) 0.032(4) -0.001(4) 0.005(3) 0.014(4) C9 0.065(5) 0.040(5) 0.036(4) -0.009(4) -0.011(4) 0.019(4) C10 0.037(4) 0.048(5) 0.034(4) -0.012(4) 0.016(3) 0.006(4) C11 0.044(4) 0.031(4) 0.033(4) 0.003(3) 0.006(3) 0.000(4) C12 0.052(5) 0.041(5) 0.042(4) -0.005(4) 0.018(4) 0.005(4) C13 0.047(4) 0.038(5) 0.039(4) 0.000(4) 0.021(4) 0.013(4) C14 0.043(5) 0.028(5) 0.074(6) 0.001(4) 0.006(4) 0.012(4) C16 0.052(5) 0.036(5) 0.038(5) 0.000(4) 0.005(4) -0.001(4) C17 0.040(4) 0.047(5) 0.043(5) 0.009(4) 0.003(4) 0.016(4) C18 0.086(6) 0.060(6) 0.039(5) -0.002(4) 0.019(5) -0.021(5) C19 0.066(6) 0.066(6) 0.039(5) 0.004(5) 0.016(4) -0.021(5) C20 0.043(4) 0.043(5) 0.040(5) 0.013(4) 0.011(4) 0.003(4) C21 0.074(6) 0.049(6) 0.035(4) 0.003(4) 0.023(4) -0.002(5) C22 0.057(5) 0.040(5) 0.033(4) 0.007(4) 0.020(4) 0.000(4) C23 0.056(5) 0.062(7) 0.050(5) 0.002(5) 0.016(4) -0.005(5) C24 0.042(4) 0.037(5) 0.031(4) 0.003(3) 0.015(4) 0.011(4) C25 0.017(3) 0.046(5) 0.022(4) -0.002(3) 0.015(3) -0.005(3) C26 0.033(4) 0.028(4) 0.040(4) 0.006(3) 0.000(3) 0.000(3) C27 0.026(4) 0.042(5) 0.030(4) 0.000(4) 0.014(3) 0.003(3) C28 0.020(3) 0.032(4) 0.035(4) -0.003(3) 0.012(3) 0.001(3) C29 0.030(4) 0.041(5) 0.031(4) 0.003(3) 0.017(3) 0.002(3) C30 0.029(4) 0.032(4) 0.040(4) -0.002(3) 0.013(3) 0.008(3) C31 0.053(5) 0.055(6) 0.026(4) -0.004(4) 0.018(4) 0.016(4) N1 0.029(3) 0.030(4) 0.038(3) 0.003(3) 0.015(3) 0.013(3) N2 0.056(4) 0.039(4) 0.034(3) 0.012(3) 0.018(3) 0.000(3) N3 0.035(3) 0.046(4) 0.027(3) 0.000(3) 0.001(3) 0.014(3) Ni2 0.0341(5) 0.0486(6) 0.0280(4) 0.0046(5) 0.0095(3) -0.0027(5) Ni1 0.0326(7) 0.0282(8) 0.0412(7) 0.0066(6) 0.0085(6) 0.0079(6) O1 0.048(3) 0.047(3) 0.040(3) 0.008(2) 0.009(2) 0.014(3) O2 0.036(3) 0.034(3) 0.049(3) 0.004(2) 0.021(2) 0.017(2) O3 0.084(4) 0.059(4) 0.053(4) 0.017(3) 0.021(3) 0.040(3) O4 0.112(5) 0.033(3) 0.045(3) 0.011(3) 0.032(3) 0.008(3) O5 0.047(3) 0.054(4) 0.037(3) 0.008(3) 0.019(2) -0.007(3) O6 0.102(4) 0.070(4) 0.055(4) 0.003(3) 0.045(3) -0.020(4) O7 0.057(3) 0.061(4) 0.048(3) 0.003(3) 0.005(3) 0.030(3) O8 0.037(3) 0.053(4) 0.035(3) -0.006(2) 0.029(2) 0.001(3) O9 0.092(4) 0.050(4) 0.061(3) 0.028(3) 0.057(3) 0.028(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 N4 C32 1.446(7) . ? N4 C37 1.456(7) 3_565 ? N4 Ni1 2.035(5) . ? N4 H4A 0.9000 . ? N4 H4'A 1.0426 . ? C32 C33 1.534(9) . ? C32 H32B 0.9599 . ? C32 H32D 0.9601 . ? C32 H37C 0.9195 . ? C32 H37D 1.1132 . ? C33 N5 1.443(8) . ? C33 H33A 0.9600 . ? C33 H33B 0.9601 . ? N5 C36 1.476(8) . ? N5 C34 1.485(8) . ? N5 Ni1 2.132(6) . ? C34 N6 1.483(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9601 . ? C34 H36C 1.1632 . ? C34 H36D 1.0608 . ? C35 N6 1.482(9) . ? C35 C36 1.551(9) . ? C35 H35A 0.9599 . ? C35 H35B 0.9598 . ? C35 H33C 1.1512 . ? C35 H33D 0.5930 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 H34C 0.9928 . ? C36 H34D 1.2197 . ? N6 C37 1.468(8) . ? N6 H33C 0.7927 . ? C37 N4 1.456(7) 3_565 ? C37 H37A 0.9601 . ? C37 H37B 0.9600 . ? C37 H32A 0.9578 . ? C37 H32C 0.8647 . ? C32' N4' 1.447(10) 3_565 ? C32' C33' 1.552(11) . ? C32' H37A 0.9685 . ? C32' H37B 1.0835 . ? C32' H32A 0.9602 . ? C32' H32C 0.9599 . ? C33' N5' 1.460(10) . ? C33' H33C 0.9600 . ? C33' H33D 0.9602 . ? N5' C36' 1.466(10) . ? N5' C34' 1.483(10) . ? N5' Ni1 2.120(9) . ? C34' N6' 1.463(10) . ? C34' H34C 0.9600 . ? C34' H34D 0.9600 . ? C35' N6' 1.488(10) . ? C35' C36' 1.554(10) . ? C35' H33A 1.2299 . ? C35' H33B 0.5422 . ? C35' H35C 0.9600 . ? C35' H35D 0.9599 . ? C36' H34A 1.0039 . ? C36' H34B 1.1808 . ? C36' H36C 0.9600 . ? C36' H36D 0.9601 . ? N6' C37' 1.478(11) . ? N6' H33A 0.7368 . ? C37' H32B 0.8136 . ? C37' H32D 1.0178 . ? C37' H37C 0.9601 . ? C37' H37D 0.9598 . ? N7 C49 1.464(9) . ? N7 C38 1.467(9) . ? N7 Ni2 2.032(5) . ? N7 H7A 0.8999 . ? N7 H10B 0.9297 . ? C38 N8 1.457(9) . ? C38 H38A 0.9599 . ? C38 H38B 0.9598 . ? C38 H43C 0.8386 . ? C38 H43D 0.9287 . ? N8 C39 1.474(9) . ? N8 C41 1.481(10) . ? N8 H42C 0.9253 . ? C39 N9 1.485(10) . ? C39 H39A 0.9600 . ? C39 H39B 0.9601 . ? C39 H40D 1.2950 . ? C40 N9 1.465(10) . ? C40 C41 1.538(10) . ? C40 H40A 0.9599 . ? C40 H40B 0.9599 . ? C41 H41A 0.9600 . ? C41 H41B 0.9599 . ? C41 H42C 1.1295 . ? C41 H42D 0.5763 . ? N9 C42 1.468(10) . ? N9 Ni2 2.099(16) . ? C42 C43 1.555(10) . ? C42 H42A 0.9599 . ? C42 H42B 0.9601 . ? C43 N10 1.451(9) . ? C43 H43A 0.9599 . ? C43 H43B 0.9600 . ? C43 H38C 1.1709 . ? C43 H38D 1.0258 . ? N10 C44 1.456(9) . ? N10 Ni2 2.040(5) . ? N10 H10A 0.9000 . ? N10 H7'A 0.9887 . ? C44 N11 1.459(9) . ? C44 H44A 0.9598 . ? C44 H44B 0.9601 . ? C44 H49C 0.7524 . ? C44 H49D 1.0601 . ? N11 C47 1.472(10) . ? N11 C45 1.478(9) . ? N11 H48D 0.7606 . ? C45 N12 1.499(10) . ? C45 H45A 0.9599 . ? C45 H45B 0.9601 . ? C45 H46C 1.1992 . ? C45 H46D 1.2886 . ? C46 N12 1.468(10) . ? C46 C47 1.540(10) . ? C46 H46A 0.9599 . ? C46 H46B 0.9600 . ? C46 H45D 1.1407 . ? C47 H47A 0.9599 . ? C47 H47B 0.9600 . ? C47 H48C 0.5891 . ? C47 H48D 1.1248 . ? N12 C48 1.460(10) . ? N12 Ni2 2.111(15) . ? C48 C49 1.538(10) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C49 H49A 0.9598 . ? C49 H49B 0.9601 . ? C49 H44C 1.0896 . ? C49 H44D 1.1057 . ? C38' N8' 1.466(9) . ? C38' H43A 1.0221 . ? C38' H43B 0.7780 . ? C38' H38C 0.9598 . ? C38' H38D 0.9599 . ? N8' C39' 1.477(10) . ? N8' C41' 1.482(10) . ? N8' H42A 0.7853 . ? C39' N9' 1.461(10) . ? C39' H39C 0.9600 . ? C39' H39D 0.9599 . ? C40' N9' 1.495(11) . ? C40' C41' 1.536(10) . ? C40' H39A 1.2014 . ? C40' H40C 0.9601 . ? C40' H40D 0.9600 . ? C41' H42A 1.2758 . ? C41' H42B 0.5818 . ? C41' H41C 0.9600 . ? C41' H41D 0.9600 . ? N9' C42' 1.465(10) . ? N9' Ni2 2.141(19) . ? C42' C43' 1.562(11) . ? C42' H42C 0.9600 . ? C42' H42D 0.9601 . ? C43' H38A 1.1113 . ? C43' H38B 1.1892 . ? C43' H43C 0.9600 . ? C43' H43D 0.9600 . ? C44' N11' 1.457(9) . ? C44' H49A 0.8998 . ? C44' H49B 0.8853 . ? C44' H44C 0.9599 . ? C44' H44D 0.9600 . ? N11' C47' 1.445(10) . ? N11' C45' 1.480(10) . ? N11' H48B 0.8105 . ? C45' N12' 1.457(10) . ? C45' H45C 0.9601 . ? C45' H45D 0.9600 . ? C46' N12' 1.480(10) . ? C46' C47' 1.545(10) . ? C46' H45A 1.2520 . ? C46' H45B 1.1190 . ? C46' H46C 0.9600 . ? C46' H46D 0.9598 . ? C47' H48A 0.3899 . ? C47' H47C 0.9599 . ? C47' H47D 0.9601 . ? N12' C48' 1.457(10) . ? N12' Ni2 2.120(15) . ? C48' C49' 1.541(11) . ? C48' H48C 0.9598 . ? C48' H48D 0.9600 . ? C49' H44A 1.1909 . ? C49' H44B 0.9520 . ? C49' H49C 0.9599 . ? C49' H49D 0.9600 . ? C1 C2 1.369(7) . ? C1 C6 1.407(8) . ? C1 C7 1.477(8) . ? C2 C3 1.392(8) . ? C2 H2 0.9500 . ? C3 C4 1.377(8) . ? C3 C16 1.537(9) . ? C4 C5 1.391(8) . ? C4 H4 0.9500 . ? C5 C6 1.398(8) . ? C5 C24 1.479(8) . ? C6 H6 0.9500 . ? C7 O1 1.255(7) . ? C7 N1 1.346(8) . ? C8 C13 1.358(8) . ? C8 C9 1.391(9) . ? C8 N1 1.421(7) . ? C9 C10 1.368(8) . ? C9 H9 0.9500 . ? C10 C11 1.412(8) . ? C10 H10 0.9500 . ? C11 C12 1.375(8) . ? C11 C14 1.533(9) . ? C12 C13 1.381(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O2 1.252(8) . ? C14 O3 1.284(8) . ? C16 O4 1.203(8) . ? C16 N2 1.374(8) . ? C17 C22 1.387(9) . ? C17 C18 1.404(9) . ? C17 N2 1.425(8) . ? C18 C19 1.353(9) . ? C18 H18 0.9500 . ? C19 C20 1.385(9) . ? C19 H19 0.9500 . ? C20 C21 1.396(9) . ? C20 C23 1.475(10) . ? C21 C22 1.391(8) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O5 1.269(8) . ? C23 O6 1.310(9) . ? C24 O7 1.248(7) . ? C24 N3 1.355(7) . ? C25 C26 1.379(8) . ? C25 C30 1.399(8) . ? C25 N3 1.430(7) . ? C26 C27 1.409(8) . ? C26 H26 0.9500 . ? C27 C28 1.368(8) . ? C27 H27 0.9500 . ? C28 C29 1.396(8) . ? C28 C31 1.502(8) . ? C29 C30 1.387(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O9 1.235(8) . ? C31 O8 1.282(8) . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N3 H3 0.8800 . ? Ni2 O5 2.100(5) . ? Ni2 O8 2.124(4) 4_456 ? Ni1 N4' 2.035(5) 3_565 ? Ni1 N4 2.035(5) 3_565 ? Ni1 O2 2.099(4) 3_565 ? Ni1 O2 2.099(4) . ? Ni1 N5' 2.120(9) 3_565 ? Ni1 N5 2.132(6) 3_565 ? O8 Ni2 2.124(4) 4_655 ? 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 C32 N4 C37 116.4(7) . 3_565 ? C32 N4 Ni1 109.9(5) . . ? C37 N4 Ni1 111.4(4) 3_565 . ? C32 N4 H4A 105.2 . . ? C37 N4 H4A 106.0 3_565 . ? Ni1 N4 H4A 107.3 . . ? C32 N4 H4'A 97.4 . . ? C37 N4 H4'A 112.7 3_565 . ? Ni1 N4 H4'A 108.1 . . ? H4A N4 H4'A 8.3 . . ? N4 C32 C33 105.9(7) . . ? N4 C32 H32B 108.3 . . ? C33 C32 H32B 107.5 . . ? N4 C32 H32D 113.1 . . ? C33 C32 H32D 113.0 . . ? H32B C32 H32D 108.8 . . ? N4 C32 H37C 113.5 . . ? C33 C32 H37C 118.8 . . ? H32B C32 H37C 102.2 . . ? H32D C32 H37C 7.2 . . ? N4 C32 H37D 97.7 . . ? C33 C32 H37D 121.1 . . ? H32B C32 H37D 14.7 . . ? H32D C32 H37D 105.2 . . ? H37C C32 H37D 98.2 . . ? N5 C33 C32 112.3(7) . . ? N5 C33 H33A 109.9 . . ? C32 C33 H33A 110.6 . . ? N5 C33 H33B 109.0 . . ? C32 C33 H33B 106.7 . . ? H33A C33 H33B 108.3 . . ? N5 C33 H35C 116.8 . . ? C32 C33 H35C 96.8 . . ? H33A C33 H35C 109.8 . . ? H33B C33 H35C 10.4 . . ? C33 N5 C36 111.9(8) . . ? C33 N5 C34 116.1(7) . . ? C36 N5 C34 103.2(6) . . ? C33 N5 Ni1 106.0(5) . . ? C36 N5 Ni1 114.0(6) . . ? C34 N5 Ni1 105.8(5) . . ? N6 C34 N5 102.3(7) . . ? N6 C34 H34A 112.6 . . ? N5 C34 H34A 112.7 . . ? N6 C34 H34B 109.9 . . ? N5 C34 H34B 109.7 . . ? H34A C34 H34B 109.5 . . ? N6 C34 H36C 138.1 . . ? N5 C34 H36C 92.8 . . ? H34A C34 H36C 96.5 . . ? H34B C34 H36C 28.9 . . ? N6 C34 H36D 121.4 . . ? N5 C34 H36D 108.0 . . ? H34A C34 H36D 8.9 . . ? H34B C34 H36D 105.3 . . ? H36C C34 H36D 89.3 . . ? N6 C35 C36 104.8(6) . . ? N6 C35 H35A 110.6 . . ? C36 C35 H35A 113.1 . . ? N6 C35 H35B 109.9 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.9 . . ? N6 C35 H33C 32.0 . . ? C36 C35 H33C 108.5 . . ? H35A C35 H33C 131.2 . . ? H35B C35 H33C 79.0 . . ? N6 C35 H33D 94.9 . . ? C36 C35 H33D 102.0 . . ? H35A C35 H33D 23.7 . . ? H35B C35 H33D 132.4 . . ? H33C C35 H33D 123.4 . . ? N5 C36 C35 103.9(6) . . ? N5 C36 H36A 111.0 . . ? C35 C36 H36A 111.0 . . ? N5 C36 H36B 111.0 . . ? C35 C36 H36B 111.0 . . ? H36A C36 H36B 109.0 . . ? N5 C36 H34C 103.2 . . ? C35 C36 H34C 126.2 . . ? H36A C36 H34C 101.1 . . ? H36B C36 H34C 15.3 . . ? N5 C36 H34D 89.6 . . ? C35 C36 H34D 135.5 . . ? H36A C36 H34D 27.6 . . ? H36B C36 H34D 102.7 . . ? H34C C36 H34D 89.8 . . ? C37 N6 C34 112.2(7) . . ? C37 N6 C35 111.1(8) . . ? C34 N6 C35 106.3(6) . . ? C37 N6 H33C 147.9 . . ? C34 N6 H33C 99.2 . . ? C35 N6 H33C 50.3 . . ? N4 C37 N6 122.7(7) 3_565 . ? N4 C37 H37A 108.6 3_565 . ? N6 C37 H37A 106.2 . . ? N4 C37 H37B 105.4 3_565 . ? N6 C37 H37B 106.5 . . ? H37A C37 H37B 106.5 . . ? N4 C37 H32A 113.3 3_565 . ? N6 C37 H32A 100.6 . . ? H37A C37 H32A 5.8 . . ? H37B C37 H32A 107.5 . . ? N4 C37 H32C 115.3 3_565 . ? N6 C37 H32C 82.7 . . ? H37A C37 H32C 119.9 . . ? H37B C37 H32C 24.5 . . ? H32A C37 H32C 118.6 . . ? N4' C32' C33' 105.0(11) 3_565 . ? N4' C32' H37A 108.8 3_565 . ? C33' C32' H37A 115.0 . . ? N4' C32' H37B 99.4 3_565 . ? C33' C32' H37B 129.7 . . ? H37A C32' H37B 97.0 . . ? N4' C32' H32A 113.9 3_565 . ? C33' C32' H32A 110.4 . . ? H37A C32' H32A 5.7 . . ? H37B C32' H32A 98.2 . . ? N4' C32' H32C 109.5 3_565 . ? C33' C32' H32C 108.3 . . ? H37A C32' H32C 110.0 . . ? H37B C32' H32C 21.4 . . ? H32A C32' H32C 109.5 . . ? N5' C33' C32' 107.7(9) . . ? N5' C33' H35A 117.9 . . ? C32' C33' H35A 100.9 . . ? N5' C33' H33C 111.4 . . ? C32' C33' H33C 110.5 . . ? H35A C33' H33C 107.8 . . ? N5' C33' H33D 109.6 . . ? C32' C33' H33D 109.1 . . ? H35A C33' H33D 9.6 . . ? H33C C33' H33D 108.5 . . ? C33' N5' C36' 111.0(11) . . ? C33' N5' C34' 114.6(9) . . ? C36' N5' C34' 104.3(8) . . ? C33' N5' Ni1 108.9(6) . . ? C36' N5' Ni1 110.5(7) . . ? C34' N5' Ni1 107.4(7) . . ? N6' C34' N5' 101.3(9) . . ? N6' C34' H34C 111.1 . . ? N5' C34' H34C 112.8 . . ? N6' C34' H34D 111.6 . . ? N5' C34' H34D 110.1 . . ? H34C C34' H34D 109.8 . . ? N6' C35' C36' 103.4(8) . . ? N6' C35' H33A 29.6 . . ? C36' C35' H33A 108.0 . . ? N6' C35' H33B 91.8 . . ? C36' C35' H33B 104.6 . . ? H33A C35' H33B 117.4 . . ? N6' C35' H35C 110.6 . . ? C36' C35' H35C 114.0 . . ? H33A C35' H35C 129.1 . . ? H33B C35' H35C 25.1 . . ? N6' C35' H35D 109.9 . . ? C36' C35' H35D 109.7 . . ? H33A C35' H35D 81.2 . . ? H33B C35' H35D 133.0 . . ? H35C C35' H35D 109.0 . . ? N5' C36' C35' 103.8(7) . . ? N5' C36' H34A 106.0 . . ? C35' C36' H34A 122.3 . . ? N5' C36' H34B 91.3 . . ? C35' C36' H34B 135.9 . . ? H34A C36' H34B 91.4 . . ? N5' C36' H36C 107.6 . . ? C35' C36' H36C 108.3 . . ? H34A C36' H36C 108.1 . . ? H34B C36' H36C 28.3 . . ? N5' C36' H36D 114.8 . . ? C35' C36' H36D 112.9 . . ? H34A C36' H36D 10.6 . . ? H34B C36' H36D 96.8 . . ? H36C C36' H36D 109.2 . . ? C34' N6' C37' 113.3(11) . . ? C34' N6' C35' 108.0(9) . . ? C37' N6' C35' 108.8(12) . . ? C34' N6' H33A 99.7 . . ? C37' N6' H33A 146.9 . . ? C35' N6' H33A 55.4 . . ? N6' C37' H32B 87.3 . . ? N6' C37' H32D 103.5 . . ? H32B C37' H32D 116.5 . . ? N6' C37' H37C 107.1 . . ? H32B C37' H37C 110.9 . . ? H32D C37' H37C 6.4 . . ? N6' C37' H37D 104.6 . . ? H32B C37' H37D 17.5 . . ? H32D C37' H37D 113.1 . . ? H37C C37' H37D 106.8 . . ? C49 N7 C38 113.9(8) . . ? C49 N7 Ni2 108.1(8) . . ? C38 N7 Ni2 114.7(7) . . ? C49 N7 H7A 107.8 . . ? C38 N7 H7A 105.7 . . ? Ni2 N7 H7A 106.2 . . ? C49 N7 H10B 102.5 . . ? C38 N7 H10B 108.6 . . ? Ni2 N7 H10B 108.2 . . ? H7A N7 H10B 5.3 . . ? N8 C38 N7 118.9(10) . . ? N8 C38 H38A 107.5 . . ? N7 C38 H38A 109.3 . . ? N8 C38 H38B 106.6 . . ? N7 C38 H38B 106.9 . . ? H38A C38 H38B 107.0 . . ? N8 C38 H43C 77.3 . . ? N7 C38 H43C 119.6 . . ? H38A C38 H43C 120.5 . . ? H38B C38 H43C 29.6 . . ? N8 C38 H43D 83.2 . . ? N7 C38 H43D 115.5 . . ? H38A C38 H43D 26.0 . . ? H38B C38 H43D 124.2 . . ? H43C C38 H43D 124.4 . . ? C38 N8 C39 113.3(10) . . ? C38 N8 C41 112.0(9) . . ? C39 N8 C41 106.0(8) . . ? C38 N8 H42C 161.1 . . ? C39 N8 H42C 80.1 . . ? C41 N8 H42C 49.6 . . ? C38 N8 H43C 32.7 . . ? C39 N8 H43C 90.5 . . ? C41 N8 H43C 143.9 . . ? H42C N8 H43C 166.2 . . ? N8 C39 N9 99.2(9) . . ? N8 C39 H39A 112.0 . . ? N9 C39 H39A 114.4 . . ? N8 C39 H39B 110.9 . . ? N9 C39 H39B 109.8 . . ? H39A C39 H39B 110.1 . . ? N8 C39 H40C 145.0 . . ? N9 C39 H40C 92.9 . . ? H39A C39 H40C 92.1 . . ? H39B C39 H40C 34.4 . . ? N8 C39 H40D 135.3 . . ? N9 C39 H40D 100.0 . . ? H39A C39 H40D 23.9 . . ? H39B C39 H40D 99.7 . . ? H40C C39 H40D 73.3 . . ? N9 C40 C41 100.2(9) . . ? N9 C40 H40A 108.4 . . ? C41 C40 H40A 112.6 . . ? N9 C40 H40B 114.2 . . ? C41 C40 H40B 111.2 . . ? H40A C40 H40B 109.9 . . ? N9 C40 H39C 91.0 . . ? C41 C40 H39C 137.3 . . ? H40A C40 H39C 102.2 . . ? H40B C40 H39C 30.0 . . ? N9 C40 H39D 83.3 . . ? C41 C40 H39D 150.7 . . ? H40A C40 H39D 40.7 . . ? H40B C40 H39D 93.1 . . ? H39C C40 H39D 71.0 . . ? N9 C40 H42D 94.6 . . ? C41 C40 H42D 21.9 . . ? H40A C40 H42D 95.0 . . ? H40B C40 H42D 131.8 . . ? H39C C40 H42D 159.2 . . ? H39D C40 H42D 129.5 . . ? N8 C41 C40 106.7(8) . . ? N8 C41 H41A 108.9 . . ? C40 C41 H41A 109.9 . . ? N8 C41 H41B 111.2 . . ? C40 C41 H41B 111.6 . . ? H41A C41 H41B 108.6 . . ? N8 C41 H42C 38.6 . . ? C40 C41 H42C 94.2 . . ? H41A C41 H42C 145.7 . . ? H41B C41 H42C 83.2 . . ? N8 C41 H42D 99.0 . . ? C40 C41 H42D 62.5 . . ? H41A C41 H42D 53.8 . . ? H41B C41 H42D 149.3 . . ? H42C C41 H42D 126.1 . . ? C40 N9 C42 112.2(10) . . ? C40 N9 C39 106.0(10) . . ? C42 N9 C39 112.7(10) . . ? C40 N9 Ni2 117.1(9) . . ? C42 N9 Ni2 101.0(9) . . ? C39 N9 Ni2 108.1(9) . . ? N9 C42 C43 114.3(12) . . ? N9 C42 H42A 112.3 . . ? C43 C42 H42A 108.9 . . ? N9 C42 H42B 107.3 . . ? C43 C42 H42B 106.2 . . ? H42A C42 H42B 107.5 . . ? N10 C43 C42 104.8(10) . . ? N10 C43 H43A 107.1 . . ? C42 C43 H43A 108.5 . . ? N10 C43 H43B 114.9 . . ? C42 C43 H43B 112.4 . . ? H43A C43 H43B 108.9 . . ? N10 C43 H38C 98.0 . . ? C42 C43 H38C 119.1 . . ? H43A C43 H38C 117.3 . . ? H43B C43 H38C 17.0 . . ? N10 C43 H38D 103.6 . . ? C42 C43 H38D 136.0 . . ? H43A C43 H38D 30.0 . . ? H43B C43 H38D 84.4 . . ? H38C C43 H38D 89.0 . . ? C43 N10 C44 117.1(8) . . ? C43 N10 Ni2 106.4(8) . . ? C44 N10 Ni2 111.0(7) . . ? C43 N10 H10A 105.9 . . ? C44 N10 H10A 107.3 . . ? Ni2 N10 H10A 108.9 . . ? C43 N10 H7'A 106.1 . . ? C44 N10 H7'A 110.5 . . ? Ni2 N10 H7'A 104.9 . . ? H10A N10 H7'A 4.2 . . ? N10 C44 N11 122.9(10) . . ? N10 C44 H44A 105.0 . . ? N11 C44 H44A 106.5 . . ? N10 C44 H44B 109.3 . . ? N11 C44 H44B 105.3 . . ? H44A C44 H44B 106.9 . . ? N10 C44 H49C 125.4 . . ? N11 C44 H49C 88.6 . . ? H44A C44 H49C 21.2 . . ? H44B C44 H49C 101.7 . . ? N10 C44 H49D 105.2 . . ? N11 C44 H49D 91.1 . . ? H44A C44 H49D 127.9 . . ? H44B C44 H49D 22.0 . . ? H49C C44 H49D 118.7 . . ? C44 N11 C47 111.2(10) . . ? C44 N11 C45 112.4(10) . . ? C47 N11 C45 108.0(9) . . ? C44 N11 H48D 158.5 . . ? C47 N11 H48D 48.6 . . ? C45 N11 H48D 84.5 . . ? N11 C45 N12 98.9(9) . . ? N11 C45 H45A 110.3 . . ? N12 C45 H45A 108.1 . . ? N11 C45 H45B 112.8 . . ? N12 C45 H45B 116.0 . . ? H45A C45 H45B 110.1 . . ? N11 C45 H46C 131.5 . . ? N12 C45 H46C 104.5 . . ? H45A C45 H46C 101.9 . . ? H45B C45 H46C 19.1 . . ? N11 C45 H46D 142.3 . . ? N12 C45 H46D 93.5 . . ? H45A C45 H46D 32.2 . . ? H45B C45 H46D 92.8 . . ? H46C C45 H46D 78.1 . . ? N12 C46 C47 103.6(9) . . ? N12 C46 H46A 113.4 . . ? C47 C46 H46A 111.0 . . ? N12 C46 H46B 108.3 . . ? C47 C46 H46B 111.0 . . ? H46A C46 H46B 109.5 . . ? N12 C46 H45C 82.6 . . ? C47 C46 H45C 143.9 . . ? H46A C46 H45C 98.3 . . ? H46B C46 H45C 36.2 . . ? N12 C46 H45D 92.0 . . ? C47 C46 H45D 136.3 . . ? H46A C46 H45D 27.9 . . ? H46B C46 H45D 102.0 . . ? H45C C46 H45D 77.8 . . ? N12 C46 H48C 98.6 . . ? C47 C46 H48C 22.4 . . ? H46A C46 H48C 131.5 . . ? H46B C46 H48C 92.5 . . ? H45C C46 H48C 122.1 . . ? H45D C46 H48C 158.4 . . ? N11 C47 C46 103.6(9) . . ? N11 C47 H47A 109.7 . . ? C46 C47 H47A 112.0 . . ? N11 C47 H47B 110.9 . . ? C46 C47 H47B 111.5 . . ? H47A C47 H47B 109.0 . . ? N11 C47 H48C 98.3 . . ? C46 C47 H48C 70.9 . . ? H47A C47 H48C 149.5 . . ? H47B C47 H48C 47.4 . . ? N11 C47 H48D 30.5 . . ? C46 C47 H48D 97.0 . . ? H47A C47 H48D 85.5 . . ? H47B C47 H48D 138.7 . . ? H48C C47 H48D 124.8 . . ? C48 N12 C46 111.8(11) . . ? C48 N12 C45 112.2(10) . . ? C46 N12 C45 103.2(9) . . ? C48 N12 Ni2 104.6(9) . . ? C46 N12 Ni2 116.9(9) . . ? C45 N12 Ni2 108.4(9) . . ? N12 C48 C49 112.4(13) . . ? N12 C48 H48A 108.5 . . ? C49 C48 H48A 110.2 . . ? N12 C48 H48B 110.4 . . ? C49 C48 H48B 107.8 . . ? H48A C48 H48B 107.5 . . ? N12 C48 H47D 121.3 . . ? C49 C48 H47D 90.8 . . ? H48A C48 H47D 19.7 . . ? H48B C48 H47D 112.2 . . ? N7 C49 C48 105.8(11) . . ? N7 C49 H49A 111.4 . . ? C48 C49 H49A 112.2 . . ? N7 C49 H49B 109.4 . . ? C48 C49 H49B 109.3 . . ? H49A C49 H49B 108.7 . . ? N7 C49 H44C 96.7 . . ? C48 C49 H44C 130.0 . . ? H49A C49 H44C 19.2 . . ? H49B C49 H44C 103.9 . . ? N7 C49 H44D 101.8 . . ? C48 C49 H44D 126.9 . . ? H49A C49 H44D 98.2 . . ? H49B C49 H44D 17.5 . . ? H44C C49 H44D 89.6 . . ? N8' C38' H43A 83.3 . . ? N8' C38' H43B 90.1 . . ? H43A C38' H43B 119.8 . . ? N8' C38' H38C 107.3 . . ? H43A C38' H38C 133.8 . . ? H43B C38' H38C 22.0 . . ? N8' C38' H38D 106.3 . . ? H43A C38' H38D 30.1 . . ? H43B C38' H38D 99.9 . . ? H38C C38' H38D 107.0 . . ? C38' N8' C39' 113.7(11) . . ? C38' N8' C41' 111.6(10) . . ? C39' N8' C41' 109.0(9) . . ? C38' N8' H42A 170.1 . . ? C39' N8' H42A 74.8 . . ? C41' N8' H42A 59.4 . . ? C38' N8' H42B 94.7 . . ? C39' N8' H42B 105.0 . . ? C41' N8' H42B 22.4 . . ? H42A N8' H42B 77.6 . . ? N9' C39' N8' 98.2(10) . . ? N9' C39' H40A 87.7 . . ? N8' C39' H40A 147.8 . . ? N9' C39' H40B 94.5 . . ? N8' C39' H40B 141.0 . . ? H40A C39' H40B 69.1 . . ? N9' C39' H42A 95.6 . . ? N8' C39' H42A 30.8 . . ? H40A C39' H42A 176.6 . . ? H40B C39' H42A 111.4 . . ? N9' C39' H39C 113.2 . . ? N8' C39' H39C 112.4 . . ? H40A C39' H39C 93.8 . . ? H40B C39' H39C 30.0 . . ? H42A C39' H39C 85.7 . . ? N9' C39' H39D 110.6 . . ? N8' C39' H39D 111.5 . . ? H40A C39' H39D 38.4 . . ? H40B C39' H39D 97.9 . . ? H42A C39' H39D 138.8 . . ? H39C C39' H39D 110.4 . . ? N9' C40' C41' 102.1(10) . . ? N9' C40' H39A 92.9 . . ? C41' C40' H39A 138.3 . . ? N9' C40' H39B 85.4 . . ? C41' C40' H39B 142.6 . . ? H39A C40' H39B 76.5 . . ? N9' C40' H42B 91.4 . . ? C41' C40' H42B 22.2 . . ? H39A C40' H42B 160.1 . . ? H39B C40' H42B 123.3 . . ? N9' C40' H40C 108.2 . . ? C41' C40' H40C 110.6 . . ? H39A C40' H40C 100.8 . . ? H39B C40' H40C 34.4 . . ? H42B C40' H40C 96.3 . . ? N9' C40' H40D 113.4 . . ? C41' C40' H40D 112.5 . . ? H39A C40' H40D 27.9 . . ? H39B C40' H40D 97.1 . . ? H42B C40' H40D 134.7 . . ? H40C C40' H40D 109.7 . . ? N8' C41' C40' 103.4(9) . . ? N8' C41' H42A 32.0 . . ? C40' C41' H42A 92.8 . . ? N8' C41' H42B 81.9 . . ? C40' C41' H42B 71.0 . . ? H42A C41' H42B 106.9 . . ? N8' C41' H41C 109.8 . . ? C40' C41' H41C 112.3 . . ? H42A C41' H41C 140.6 . . ? H42B C41' H41C 58.2 . . ? N8' C41' H41D 111.6 . . ? C40' C41' H41D 110.7 . . ? H42A C41' H41D 88.2 . . ? H42B C41' H41D 164.9 . . ? H41C C41' H41D 109.0 . . ? C39' N9' C42' 116.1(11) . . ? C39' N9' C40' 105.4(10) . . ? C42' N9' C40' 110.7(12) . . ? C39' N9' Ni2 110.9(11) . . ? C42' N9' Ni2 100.7(11) . . ? C40' N9' Ni2 113.2(11) . . ? N9' C42' C43' 115.9(16) . . ? N9' C42' H41A 126.6 . . ? C43' C42' H41A 86.6 . . ? N9' C42' H42C 111.8 . . ? C43' C42' H42C 109.5 . . ? H41A C42' H42C 103.3 . . ? N9' C42' H42D 105.0 . . ? C43' C42' H42D 107.3 . . ? H41A C42' H42D 24.1 . . ? H42C C42' H42D 106.7 . . ? C42' C43' H38A 130.6 . . ? C42' C43' H38B 133.0 . . ? H38A C43' H38B 84.2 . . ? C42' C43' H43C 111.3 . . ? H38A C43' H43C 97.7 . . ? H38B C43' H43C 22.4 . . ? C42' C43' H43D 108.5 . . ? H38A C43' H43D 22.2 . . ? H38B C43' H43D 101.4 . . ? H43C C43' H43D 109.1 . . ? N11' C44' H49A 84.1 . . ? N11' C44' H49B 90.5 . . ? H49A C44' H49B 121.8 . . ? N11' C44' H44C 106.4 . . ? H49A C44' H44C 22.3 . . ? H49B C44' H44C 122.3 . . ? N11' C44' H44D 110.1 . . ? H49A C44' H44D 114.5 . . ? H49B C44' H44D 21.1 . . ? H44C C44' H44D 107.4 . . ? C47' N11' C44' 115.7(10) . . ? C47' N11' C45' 108.8(9) . . ? C44' N11' C45' 113.4(11) . . ? C47' N11' H48A 15.3 . . ? C44' N11' H48A 102.9 . . ? C45' N11' H48A 109.2 . . ? C47' N11' H48B 65.3 . . ? C44' N11' H48B 166.1 . . ? C45' N11' H48B 77.8 . . ? H48A N11' H48B 79.9 . . ? N12' C45' N11' 98.0(10) . . ? N12' C45' H46A 97.7 . . ? N11' C45' H46A 132.3 . . ? N12' C45' H46B 92.9 . . ? N11' C45' H46B 150.0 . . ? H46A C45' H46B 73.1 . . ? N12' C45' H48B 100.0 . . ? N11' C45' H48B 31.2 . . ? H46A C45' H48B 101.5 . . ? H46B C45' H48B 166.6 . . ? N12' C45' H45C 112.2 . . ? N11' C45' H45C 113.3 . . ? H46A C45' H45C 101.7 . . ? H46B C45' H45C 37.1 . . ? H48B C45' H45C 136.8 . . ? N12' C45' H45D 110.5 . . ? N11' C45' H45D 112.1 . . ? H46A C45' H45D 21.2 . . ? H46B C45' H45D 89.7 . . ? H48B C45' H45D 82.6 . . ? H45C C45' H45D 110.2 . . ? N12' C46' C47' 101.0(9) . . ? N12' C46' H45A 85.3 . . ? C47' C46' H45A 140.3 . . ? N12' C46' H45B 98.6 . . ? C47' C46' H45B 133.3 . . ? H45A C46' H45B 83.0 . . ? N12' C46' H48A 95.8 . . ? C47' C46' H48A 14.6 . . ? H45A C46' H48A 126.9 . . ? H45B C46' H48A 147.9 . . ? N12' C46' H46C 115.7 . . ? C47' C46' H46C 113.2 . . ? H45A C46' H46C 98.2 . . ? H45B C46' H46C 22.1 . . ? H48A C46' H46C 127.3 . . ? N12' C46' H46D 107.4 . . ? C47' C46' H46D 109.4 . . ? H45A C46' H46D 33.7 . . ? H45B C46' H46D 104.3 . . ? H48A C46' H46D 98.5 . . ? H46C C46' H46D 109.6 . . ? N11' C47' C46' 104.7(9) . . ? N11' C47' H48A 85.9 . . ? C46' C47' H48A 79.8 . . ? N11' C47' H48B 33.6 . . ? C46' C47' H48B 97.8 . . ? H48A C47' H48B 117.4 . . ? N11' C47' H47C 113.6 . . ? C46' C47' H47C 110.0 . . ? H48A C47' H47C 153.7 . . ? H48B C47' H47C 86.2 . . ? N11' C47' H47D 106.4 . . ? C46' C47' H47D 113.3 . . ? H48A C47' H47D 46.2 . . ? H48B C47' H47D 136.6 . . ? H47C C47' H47D 108.9 . . ? C48' N12' C45' 114.5(10) . . ? C48' N12' C46' 113.0(11) . . ? C45' N12' C46' 106.2(9) . . ? C48' N12' Ni2 101.5(10) . . ? C45' N12' Ni2 106.9(9) . . ? C46' N12' Ni2 114.8(10) . . ? N12' C48' C49' 117.1(17) . . ? N12' C48' H47B 128.9 . . ? C49' C48' H47B 90.5 . . ? N12' C48' H48C 108.1 . . ? C49' C48' H48C 109.4 . . ? H47B C48' H48C 22.2 . . ? N12' C48' H48D 107.5 . . ? C49' C48' H48D 107.6 . . ? H47B C48' H48D 102.9 . . ? H48C C48' H48D 106.6 . . ? C48' C49' H44A 122.7 . . ? C48' C49' H44B 129.3 . . ? H44A C49' H44B 91.4 . . ? C48' C49' H49C 114.0 . . ? H44A C49' H49C 15.9 . . ? H44B C49' H49C 88.5 . . ? C48' C49' H49D 108.1 . . ? H44A C49' H49D 114.7 . . ? H44B C49' H49D 24.0 . . ? H49C C49' H49D 109.4 . . ? C2 C1 C6 117.2(6) . . ? C2 C1 C7 121.1(6) . . ? C6 C1 C7 121.8(5) . . ? C1 C2 C3 122.0(6) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 120.2(6) . . ? C4 C3 C16 120.4(6) . . ? C2 C3 C16 119.1(6) . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 118.5(6) . . ? C4 C5 C24 121.2(6) . . ? C6 C5 C24 120.3(6) . . ? C5 C6 C1 122.0(6) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? O1 C7 N1 122.6(6) . . ? O1 C7 C1 118.3(6) . . ? N1 C7 C1 119.1(6) . . ? C13 C8 C9 119.6(6) . . ? C13 C8 N1 120.1(6) . . ? C9 C8 N1 120.3(6) . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.5(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 C14 123.6(7) . . ? C10 C11 C14 117.2(7) . . ? C11 C12 C13 119.2(7) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C8 C13 C12 121.9(6) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? O2 C14 O3 126.2(7) . . ? O2 C14 C11 117.3(7) . . ? O3 C14 C11 116.5(7) . . ? O4 C16 N2 126.2(7) . . ? O4 C16 C3 120.6(7) . . ? N2 C16 C3 113.2(6) . . ? C22 C17 C18 119.2(7) . . ? C22 C17 N2 117.5(7) . . ? C18 C17 N2 123.1(7) . . ? C19 C18 C17 120.5(8) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.2(8) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C21 118.9(7) . . ? C19 C20 C23 121.2(7) . . ? C21 C20 C23 119.9(7) . . ? C22 C21 C20 120.3(7) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C17 C22 C21 119.7(7) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? O5 C23 O6 121.5(7) . . ? O5 C23 C20 119.3(8) . . ? O6 C23 C20 119.2(8) . . ? O7 C24 N3 122.3(6) . . ? O7 C24 C5 123.4(6) . . ? N3 C24 C5 114.1(6) . . ? C26 C25 C30 120.8(6) . . ? C26 C25 N3 122.4(6) . . ? C30 C25 N3 116.8(6) . . ? C25 C26 C27 118.7(6) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 121.1(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.6(6) . . ? C27 C28 C31 121.4(6) . . ? C29 C28 C31 118.9(6) . . ? C30 C29 C28 120.3(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 119.4(6) . . ? C29 C30 H30 120.3 . . ? C25 C30 H30 120.3 . . ? O9 C31 O8 126.7(7) . . ? O9 C31 C28 118.8(7) . . ? O8 C31 C28 114.5(7) . . ? C7 N1 C8 125.1(5) . . ? C7 N1 H1 117.5 . . ? C8 N1 H1 117.5 . . ? C16 N2 C17 125.1(6) . . ? C16 N2 H2A 117.5 . . ? C17 N2 H2A 117.5 . . ? C24 N3 C25 127.0(5) . . ? C24 N3 H3 116.5 . . ? C25 N3 H3 116.5 . . ? N7 Ni2 N10 179.3(2) . . ? N7 Ni2 O5 93.2(2) . . ? N10 Ni2 O5 87.2(2) . . ? N7 Ni2 N9 93.2(4) . . ? N10 Ni2 N9 87.5(4) . . ? O5 Ni2 N9 88.3(3) . . ? N7 Ni2 N12 85.0(4) . . ? N10 Ni2 N12 94.3(4) . . ? O5 Ni2 N12 92.0(3) . . ? N9 Ni2 N12 178.2(5) . . ? N7 Ni2 N12' 94.0(4) . . ? N10 Ni2 N12' 85.4(4) . . ? O5 Ni2 N12' 89.9(3) . . ? N9 Ni2 N12' 172.7(5) . . ? N12 Ni2 N12' 9.1(5) . . ? N7 Ni2 O8 87.5(2) . 4_456 ? N10 Ni2 O8 92.1(2) . 4_456 ? O5 Ni2 O8 179.06(18) . 4_456 ? N9 Ni2 O8 91.0(3) . 4_456 ? N12 Ni2 O8 88.6(3) . 4_456 ? N12' Ni2 O8 90.6(3) . 4_456 ? N7 Ni2 N9' 88.0(4) . . ? N10 Ni2 N9' 92.6(4) . . ? O5 Ni2 N9' 89.7(4) . . ? N9 Ni2 N9' 5.3(6) . . ? N12 Ni2 N9' 172.9(5) . . ? N12' Ni2 N9' 178.0(6) . . ? O8 Ni2 N9' 89.7(4) 4_456 . ? N4' Ni1 N4 180.0(3) 3_565 . ? N4' Ni1 N4 0.002(1) 3_565 3_565 ? N4 Ni1 N4 179.998(1) . 3_565 ? N4' Ni1 O2 88.40(19) 3_565 3_565 ? N4 Ni1 O2 91.60(19) . 3_565 ? N4 Ni1 O2 88.40(19) 3_565 3_565 ? N4' Ni1 O2 91.60(19) 3_565 . ? N4 Ni1 O2 88.40(19) . . ? N4 Ni1 O2 91.59(19) 3_565 . ? O2 Ni1 O2 180.0 3_565 . ? N4' Ni1 N5' 98.8(3) 3_565 3_565 ? N4 Ni1 N5' 81.2(3) . 3_565 ? N4 Ni1 N5' 98.8(3) 3_565 3_565 ? O2 Ni1 N5' 89.8(3) 3_565 3_565 ? O2 Ni1 N5' 90.2(3) . 3_565 ? N4' Ni1 N5' 81.2(3) 3_565 . ? N4 Ni1 N5' 98.8(3) . . ? N4 Ni1 N5' 81.2(3) 3_565 . ? O2 Ni1 N5' 90.2(3) 3_565 . ? O2 Ni1 N5' 89.8(3) . . ? N5' Ni1 N5' 179.998(1) 3_565 . ? N4' Ni1 N5 83.0(2) 3_565 3_565 ? N4 Ni1 N5 97.0(2) . 3_565 ? N4 Ni1 N5 83.0(2) 3_565 3_565 ? O2 Ni1 N5 90.6(2) 3_565 3_565 ? O2 Ni1 N5 89.4(2) . 3_565 ? N5' Ni1 N5 15.8(3) 3_565 3_565 ? N5' Ni1 N5 164.2(3) . 3_565 ? N4' Ni1 N5 97.0(2) 3_565 . ? N4 Ni1 N5 83.0(2) . . ? N4 Ni1 N5 97.0(2) 3_565 . ? O2 Ni1 N5 89.4(2) 3_565 . ? O2 Ni1 N5 90.6(2) . . ? N5' Ni1 N5 164.2(3) 3_565 . ? N5' Ni1 N5 15.8(3) . . ? N5 Ni1 N5 180.0(2) 3_565 . ? C14 O2 Ni1 136.2(5) . . ? C23 O5 Ni2 136.1(5) . . ? C31 O8 Ni2 135.5(4) . 4_655 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.469 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.079 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.091 0.734 0.250 684 260 ' ' 2 0.093 0.763 0.750 684 255 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 913627'