# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Miaoli Zhu' _publ_contact_author_email MIAOLI@SXU.EDU.CN _publ_section_title ; Rationally Designed Chiral Ni5L6 Clusters with the in Situ Generated Tridentate Ligand. Hydrothermal Synthesis, Crystal Structures, Morphology and Magnetic Properties ; loop_ _publ_author_name 'Miaoli Zhu' 'Lei Du' 'Sisi Feng' 'Liping Lu' 'Tianwei Wang' 'Yunbo Zhang' # Attachment '5_CCDC676416.cif' data_fwno3b-s _database_code_depnum_ccdc_archive 'CCDC 676416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C96 H66 N24 Ni5 O6, N O3, 3(H O), 2(H2 O)' _chemical_formula_sum 'C96 H73 N25 Ni5 O14' _chemical_formula_weight 2094.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.267(4) _cell_length_b 26.128(7) _cell_length_c 29.054(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.509(11) _cell_angle_gamma 90.00 _cell_volume 9656(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11273 _cell_measurement_theta_min 2.0895 _cell_measurement_theta_max 27.4487 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.9406 _exptl_absorpt_process_details ; (HIGASHI, T. (1995). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60801 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16705 _reflns_number_gt 10432 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material ; SHELXTL/PC Mercury Ver. 1.3 (Bruno et al., 2002) ; _publ_section_references ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _refine_special_details ; Structure was phased by direct methods. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. There were disorder and partially occupied sites for the antiparticles, O11A and O11B as well as O14A, O14B and O14C. The occupancies of these sites were freely refined with PART and SUMP instruction. ISOR instruction was employed to have ellipsoids of sites (O14A, O14B, O14C and O11B) be restraint to more appropriate values. So, 25 restraints were used for refinement anisotropically. Non H-atoms were refined anisotropically. H-atoms of OH and water have been located from Fourier difference maps and fixed to its position. The remaining H-atoms were included in calculated positions and treated as riding atoms using the SHELXL default parameters. ; _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^)+(0.1463P)^2^] 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 16705 _refine_ls_number_parameters 1292 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.2695 _refine_ls_wR_factor_gt 0.2322 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.067 _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 Ni1 Ni 0.83095(6) 0.08888(3) 0.35278(3) 0.0439(2) Uani 1 1 d . . . Ni2 Ni 0.64912(7) 0.19240(4) 0.18397(3) 0.0604(3) Uani 1 1 d . . . Ni3 Ni 0.72426(7) 0.07069(4) 0.22809(3) 0.0575(3) Uani 1 1 d . . . Ni4 Ni 0.89034(7) 0.17946(4) 0.27437(4) 0.0633(3) Uani 1 1 d . . . Ni5 Ni 0.61848(7) 0.17145(4) 0.29713(3) 0.0618(3) Uani 1 1 d . . . O1 O 0.7105(3) 0.06227(18) 0.29258(14) 0.0478(10) Uani 1 1 d . . . O2 O 0.9104(3) 0.11069(18) 0.30171(16) 0.0541(11) Uani 1 1 d . . . O3 O 0.7545(3) 0.16209(18) 0.34421(16) 0.0551(12) Uani 1 1 d . . . O4 O 0.7482(4) 0.1276(2) 0.18928(16) 0.0609(13) Uani 1 1 d . . . O5 O 0.7623(4) 0.2196(2) 0.24701(17) 0.0625(13) Uani 1 1 d . . . O6 O 0.5716(4) 0.1557(2) 0.22888(18) 0.0680(14) Uani 1 1 d . . . N1 N 0.7295(4) 0.0561(2) 0.38506(17) 0.0439(12) Uani 1 1 d . . . N2 N 0.5879(4) 0.0080(2) 0.37833(18) 0.0501(13) Uani 1 1 d . . . H2 H 0.5313 -0.0100 0.3646 0.060 Uiso 1 1 calc R . . N3 N 0.5991(4) 0.0316(2) 0.19781(18) 0.0566(15) Uani 1 1 d . . . N4 N 0.4589(5) -0.0180(3) 0.1914(2) 0.078(2) Uani 1 1 d . . . H4 H 0.4103 -0.0355 0.1998 0.094 Uiso 1 1 calc R . . N5 N 0.9260(4) 0.0272(2) 0.35545(18) 0.0470(13) Uani 1 1 d . . . N6 N 1.0573(4) -0.0082(2) 0.3339(2) 0.0554(15) Uani 1 1 d . . . H6 H 1.1073 -0.0120 0.3197 0.067 Uiso 1 1 calc R . . N7 N 0.9923(5) 0.1685(3) 0.2392(2) 0.0669(17) Uani 1 1 d . . . N8 N 1.1122(6) 0.1300(4) 0.2105(4) 0.111(3) Uani 1 1 d . . . H8 H 1.1550 0.1065 0.2050 0.133 Uiso 1 1 calc R . . N9 N 0.9315(4) 0.1297(2) 0.40661(18) 0.0491(13) Uani 1 1 d . . . N10 N 0.9737(5) 0.2064(2) 0.4415(2) 0.0590(15) Uani 1 1 d . . . H10 H 0.9685 0.2388 0.4489 0.071 Uiso 1 1 calc R . . N11 N 0.5921(5) 0.2379(3) 0.3228(2) 0.0679(17) Uani 1 1 d . . . N12 N 0.6146(6) 0.3033(3) 0.3745(3) 0.082(2) Uani 1 1 d . . . H12 H 0.6444 0.3241 0.3983 0.098 Uiso 1 1 calc R . . N13 N 0.7332(5) 0.2119(3) 0.1379(2) 0.0699(18) Uani 1 1 d . . . N14 N 0.8266(6) 0.1838(3) 0.0909(3) 0.086(2) Uani 1 1 d . . . H14 H 0.8657 0.1634 0.0790 0.103 Uiso 1 1 calc R . . N15 N 0.8277(4) 0.0281(2) 0.2097(2) 0.0585(15) Uani 1 1 d . . . N16 N 0.9455(6) 0.0035(3) 0.1749(3) 0.086(2) Uani 1 1 d . . . H16 H 0.9893 0.0047 0.1571 0.103 Uiso 1 1 calc R . . N17 N 0.5840(5) 0.2614(3) 0.1927(2) 0.0657(17) Uani 1 1 d . . . N18 N 0.6031(5) 0.3342(3) 0.2337(3) 0.0734(18) Uani 1 1 d . . . H18 H 0.6321 0.3582 0.2544 0.088 Uiso 1 1 calc R . . N19 N 0.9593(5) 0.2339(3) 0.3170(2) 0.0655(17) Uani 1 1 d . . . N20 N 0.9817(6) 0.3103(3) 0.3530(3) 0.079(2) Uani 1 1 d . . . H20 H 0.9674 0.3411 0.3618 0.095 Uiso 1 1 calc R . . N21 N 0.5278(5) 0.1579(3) 0.1336(2) 0.077(2) Uani 1 1 d . . . N22 N 0.3762(6) 0.1158(4) 0.1192(3) 0.101(3) Uani 1 1 d . . . H22 H 0.3210 0.1007 0.1243 0.121 Uiso 1 1 calc R . . N23 N 0.5027(4) 0.1342(3) 0.3103(2) 0.0634(16) Uani 1 1 d . . . N24 N 0.3499(6) 0.0920(4) 0.2959(3) 0.104(3) Uani 1 1 d . . . H24 H 0.2917 0.0764 0.2801 0.125 Uiso 1 1 calc R . . C1 C 0.6364(5) 0.0346(3) 0.3033(2) 0.0517(16) Uani 1 1 d . . . C2 C 0.6493(5) 0.0328(3) 0.3559(2) 0.0449(15) Uani 1 1 d . . . C3 C 0.7192(5) 0.0476(3) 0.4309(2) 0.0449(15) Uani 1 1 d . . . C4 C 0.7816(5) 0.0623(3) 0.4759(2) 0.0562(18) Uani 1 1 d . . . H4A H 0.8441 0.0817 0.4800 0.067 Uiso 1 1 calc R . . C5 C 0.7464(6) 0.0467(3) 0.5152(3) 0.067(2) Uani 1 1 d . . . H5 H 0.7863 0.0564 0.5466 0.081 Uiso 1 1 calc R . . C6 C 0.6580(6) 0.0182(3) 0.5102(3) 0.065(2) Uani 1 1 d . . . H6A H 0.6379 0.0094 0.5380 0.078 Uiso 1 1 calc R . . C7 C 0.5967(5) 0.0019(3) 0.4661(2) 0.0579(19) Uani 1 1 d . . . H7 H 0.5351 -0.0179 0.4630 0.069 Uiso 1 1 calc R . . C8 C 0.6294(5) 0.0159(3) 0.4257(2) 0.0519(16) Uani 1 1 d . . . C9 C 0.5540(5) 0.0098(3) 0.2716(2) 0.0575(18) Uani 1 1 d . . . H9 H 0.5055 -0.0080 0.2843 0.069 Uiso 1 1 calc R . . C10 C 0.5367(5) 0.0090(3) 0.2216(3) 0.0614(19) Uani 1 1 d . . . C11 C 0.5555(6) 0.0175(4) 0.1497(3) 0.073(2) Uani 1 1 d . . . C12 C 0.5919(8) 0.0279(5) 0.1101(3) 0.101(3) Uani 1 1 d . . . H12C H 0.6544 0.0469 0.1128 0.121 Uiso 1 1 calc R . . C13 C 0.5306(11) 0.0087(6) 0.0663(4) 0.141(6) Uani 1 1 d . . . H13 H 0.5486 0.0172 0.0378 0.169 Uiso 1 1 calc R . . C14 C 0.4458(10) -0.0220(5) 0.0631(3) 0.125(5) Uani 1 1 d . . . H14D H 0.4098 -0.0359 0.0326 0.150 Uiso 1 1 calc R . . C15 C 0.4095(10) -0.0338(5) 0.1017(3) 0.133(5) Uani 1 1 d . . . H15 H 0.3486 -0.0542 0.0985 0.159 Uiso 1 1 calc R . . C16 C 0.4677(7) -0.0139(4) 0.1460(3) 0.083(3) Uani 1 1 d . . . C17 C 0.9889(5) 0.0789(3) 0.3002(2) 0.0544(17) Uani 1 1 d . . . C18 C 0.9924(5) 0.0330(3) 0.3294(2) 0.0506(16) Uani 1 1 d . . . C19 C 0.9467(5) -0.0199(3) 0.3780(2) 0.0524(17) Uani 1 1 d . . . C20 C 0.9042(5) -0.0453(3) 0.4098(2) 0.0559(17) Uani 1 1 d . . . H20A H 0.8493 -0.0303 0.4203 0.067 Uiso 1 1 calc R . . C21 C 0.9436(6) -0.0929(3) 0.4259(3) 0.067(2) Uani 1 1 d . . . H21 H 0.9139 -0.1111 0.4473 0.080 Uiso 1 1 calc R . . C22 C 1.0245(6) -0.1149(3) 0.4120(3) 0.069(2) Uani 1 1 d . . . H22A H 1.0491 -0.1477 0.4243 0.083 Uiso 1 1 calc R . . C23 C 1.0704(5) -0.0917(3) 0.3816(3) 0.064(2) Uani 1 1 d . . . H23 H 1.1260 -0.1074 0.3722 0.077 Uiso 1 1 calc R . . C24 C 1.0314(5) -0.0431(3) 0.3646(2) 0.0549(17) Uani 1 1 d . . . C25 C 1.0534(6) 0.0836(3) 0.2708(3) 0.072(2) Uani 1 1 d . . . H25 H 1.1007 0.0564 0.2704 0.086 Uiso 1 1 calc R . . C26 C 1.0534(6) 0.1259(4) 0.2418(3) 0.073(2) Uani 1 1 d . . . C27 C 1.0190(7) 0.2018(4) 0.2075(3) 0.074(2) Uani 1 1 d . . . C28 C 0.9821(7) 0.2507(4) 0.1929(3) 0.083(3) Uani 1 1 d . . . H28 H 0.9314 0.2675 0.2050 0.100 Uiso 1 1 calc R . . C29 C 1.0248(11) 0.2736(5) 0.1591(5) 0.118(4) Uani 1 1 d . . . H29 H 1.0027 0.3071 0.1479 0.141 Uiso 1 1 calc R . . C30 C 1.0980(13) 0.2489(7) 0.1417(6) 0.147(6) Uani 1 1 d . . . H30 H 1.1245 0.2662 0.1188 0.176 Uiso 1 1 calc R . . C31 C 1.1346(12) 0.2011(7) 0.1556(6) 0.154(6) Uani 1 1 d . . . H31 H 1.1855 0.1849 0.1432 0.185 Uiso 1 1 calc R . . C32 C 1.0930(9) 0.1771(5) 0.1890(5) 0.107(4) Uani 1 1 d . . . C33 C 0.7994(5) 0.1955(3) 0.3796(2) 0.0531(16) Uani 1 1 d . . . C34 C 0.9004(5) 0.1782(3) 0.4091(2) 0.0506(16) Uani 1 1 d . . . C35 C 1.0305(5) 0.1271(3) 0.4391(2) 0.0475(15) Uani 1 1 d . . . C36 C 1.0980(5) 0.0858(3) 0.4519(2) 0.0590(19) Uani 1 1 d . . . H36 H 1.0794 0.0526 0.4389 0.071 Uiso 1 1 calc R . . C37 C 1.1957(6) 0.0959(4) 0.4852(3) 0.072(2) Uani 1 1 d . . . H37 H 1.2446 0.0687 0.4945 0.086 Uiso 1 1 calc R . . C38 C 1.2237(6) 0.1432(4) 0.5049(3) 0.074(2) Uani 1 1 d . . . H38 H 1.2919 0.1475 0.5265 0.089 Uiso 1 1 calc R . . C39 C 1.1565(6) 0.1851(3) 0.4946(3) 0.067(2) Uani 1 1 d . . . H39 H 1.1746 0.2178 0.5090 0.080 Uiso 1 1 calc R . . C40 C 1.0571(5) 0.1744(3) 0.4603(2) 0.0561(18) Uani 1 1 d . . . C41 C 0.7586(6) 0.2409(3) 0.3877(3) 0.065(2) Uani 1 1 d . . . H41 H 0.8004 0.2616 0.4128 0.078 Uiso 1 1 calc R . . C42 C 0.6579(6) 0.2605(3) 0.3617(3) 0.068(2) Uani 1 1 d . . . C43 C 0.5005(6) 0.2671(4) 0.3110(3) 0.071(2) Uani 1 1 d . . . C44 C 0.4040(6) 0.2596(4) 0.2757(3) 0.087(3) Uani 1 1 d . . . H44 H 0.3927 0.2321 0.2534 0.104 Uiso 1 1 calc R . . C45 C 0.3242(8) 0.2962(5) 0.2760(4) 0.110(4) Uani 1 1 d . . . H45 H 0.2562 0.2918 0.2542 0.132 Uiso 1 1 calc R . . C46 C 0.3424(10) 0.3383(5) 0.3071(5) 0.116(4) Uani 1 1 d . . . H46 H 0.2884 0.3631 0.3037 0.139 Uiso 1 1 calc R . . C47 C 0.4345(9) 0.3449(4) 0.3420(4) 0.105(3) Uani 1 1 d . . . H47 H 0.4446 0.3723 0.3644 0.126 Uiso 1 1 calc R . . C48 C 0.5155(7) 0.3081(4) 0.3433(3) 0.084(3) Uani 1 1 d . . . C49 C 0.8031(7) 0.1256(3) 0.1577(3) 0.070(2) Uani 1 1 d . . . C50 C 0.7904(7) 0.1739(4) 0.1282(3) 0.068(2) Uani 1 1 d . . . C51 C 0.7352(7) 0.2497(3) 0.1044(3) 0.071(2) Uani 1 1 d . . . C52 C 0.6862(7) 0.2974(4) 0.0984(3) 0.085(3) Uani 1 1 d . . . H52 H 0.6473 0.3092 0.1192 0.102 Uiso 1 1 calc R . . C53 C 0.6979(9) 0.3278(5) 0.0590(4) 0.103(4) Uani 1 1 d . . . H53 H 0.6680 0.3610 0.0535 0.124 Uiso 1 1 calc R . . C54 C 0.7531(10) 0.3081(5) 0.0291(4) 0.107(4) Uani 1 1 d . . . H54 H 0.7567 0.3278 0.0022 0.128 Uiso 1 1 calc R . . C55 C 0.8030(9) 0.2613(5) 0.0366(4) 0.106(4) Uani 1 1 d . . . H55 H 0.8437 0.2497 0.0165 0.127 Uiso 1 1 calc R . . C56 C 0.7915(8) 0.2316(4) 0.0746(3) 0.084(3) Uani 1 1 d . . . C57 C 0.8638(7) 0.0870(4) 0.1512(3) 0.074(2) Uani 1 1 d . . . H57 H 0.8993 0.0908 0.1272 0.089 Uiso 1 1 calc R . . C58 C 0.8785(6) 0.0403(3) 0.1780(3) 0.066(2) Uani 1 1 d . . . C59 C 0.8603(5) -0.0211(3) 0.2261(3) 0.0591(18) Uani 1 1 d . . . C60 C 0.8334(6) -0.0534(3) 0.2577(2) 0.0616(19) Uani 1 1 d . . . H60 H 0.7818 -0.0434 0.2729 0.074 Uiso 1 1 calc R . . C61 C 0.8817(7) -0.1008(3) 0.2675(3) 0.073(2) Uani 1 1 d . . . H61 H 0.8616 -0.1234 0.2889 0.088 Uiso 1 1 calc R . . C62 C 0.9583(8) -0.1156(4) 0.2467(4) 0.091(3) Uani 1 1 d . . . H62 H 0.9906 -0.1481 0.2542 0.110 Uiso 1 1 calc R . . C63 C 0.9884(9) -0.0846(4) 0.2157(4) 0.105(3) Uani 1 1 d . . . H63 H 1.0429 -0.0945 0.2022 0.126 Uiso 1 1 calc R . . C64 C 0.9358(8) -0.0368(4) 0.2039(3) 0.081(2) Uani 1 1 d . . . C65 C 0.7477(5) 0.2676(3) 0.2574(3) 0.0604(19) Uani 1 1 d . . . C66 C 0.6456(6) 0.2887(3) 0.2281(3) 0.064(2) Uani 1 1 d . . . C67 C 0.4953(6) 0.2900(3) 0.1747(3) 0.067(2) Uani 1 1 d . . . C68 C 0.4043(6) 0.2783(4) 0.1375(3) 0.085(3) Uani 1 1 d . . . H68 H 0.3955 0.2468 0.1205 0.102 Uiso 1 1 calc R . . C69 C 0.3272(8) 0.3168(6) 0.1274(4) 0.116(4) Uani 1 1 d . . . H69 H 0.2654 0.3119 0.1015 0.139 Uiso 1 1 calc R . . C70 C 0.3384(8) 0.3627(5) 0.1544(5) 0.102(4) Uani 1 1 d . . . H70 H 0.2829 0.3870 0.1469 0.122 Uiso 1 1 calc R . . C71 C 0.4264(7) 0.3728(4) 0.1907(4) 0.093(3) Uani 1 1 d . . . H71 H 0.4341 0.4037 0.2086 0.112 Uiso 1 1 calc R . . C72 C 0.5035(7) 0.3361(4) 0.1999(3) 0.079(3) Uani 1 1 d . . . C73 C 0.8153(7) 0.2967(4) 0.2920(3) 0.075(2) Uani 1 1 d . . . H73 H 0.7933 0.3303 0.2972 0.090 Uiso 1 1 calc R . . C74 C 0.9159(6) 0.2805(3) 0.3207(3) 0.0626(19) Uani 1 1 d . . . C75 C 1.0614(6) 0.2370(3) 0.3480(2) 0.0603(18) Uani 1 1 d . . . C76 C 1.1447(6) 0.2015(4) 0.3580(3) 0.072(2) Uani 1 1 d . . . H76 H 1.1370 0.1686 0.3435 0.086 Uiso 1 1 calc R . . C77 C 1.2370(7) 0.2170(5) 0.3895(4) 0.093(3) Uani 1 1 d . . . H77 H 1.2959 0.1948 0.3952 0.111 Uiso 1 1 calc R . . C78 C 1.2492(9) 0.2630(5) 0.4136(4) 0.108(4) Uani 1 1 d . . . H78 H 1.3140 0.2700 0.4370 0.129 Uiso 1 1 calc R . . C79 C 1.1697(8) 0.2996(4) 0.4047(4) 0.096(3) Uani 1 1 d . . . H79 H 1.1779 0.3318 0.4205 0.115 Uiso 1 1 calc R . . C80 C 1.0757(7) 0.2846(4) 0.3704(3) 0.078(2) Uani 1 1 d . . . C81 C 0.4781(6) 0.1356(3) 0.2065(3) 0.070(2) Uani 1 1 d . . . C82 C 0.4591(6) 0.1366(4) 0.1538(3) 0.077(2) Uani 1 1 d . . . C83 C 0.4892(7) 0.1494(4) 0.0836(3) 0.090(3) Uani 1 1 d . . . C84 C 0.5303(8) 0.1642(4) 0.0466(3) 0.092(3) Uani 1 1 d . . . H84 H 0.5925 0.1842 0.0524 0.111 Uiso 1 1 calc R . . C85 C 0.4740(9) 0.1477(5) -0.0001(3) 0.109(4) Uani 1 1 d . . . H85 H 0.5008 0.1550 -0.0264 0.131 Uiso 1 1 calc R . . C86 C 0.3793(11) 0.1207(6) -0.0079(5) 0.134(5) Uani 1 1 d . . . H86 H 0.3413 0.1118 -0.0398 0.161 Uiso 1 1 calc R . . C87 C 0.3386(10) 0.1064(6) 0.0301(5) 0.121(4) Uani 1 1 d . . . H87 H 0.2762 0.0866 0.0247 0.145 Uiso 1 1 calc R . . C88 C 0.3938(8) 0.1225(5) 0.0754(4) 0.104(4) Uani 1 1 d . . . C89 C 0.4097(6) 0.1157(4) 0.2263(3) 0.084(3) Uani 1 1 d . . . H89 H 0.3475 0.1015 0.2054 0.101 Uiso 1 1 calc R . . C90 C 0.4208(7) 0.1136(4) 0.2770(3) 0.078(2) Uani 1 1 d . . . C91 C 0.4803(6) 0.1260(4) 0.3540(3) 0.073(2) Uani 1 1 d . . . C92 C 0.5363(6) 0.1414(4) 0.4004(3) 0.073(2) Uani 1 1 d . . . H92 H 0.5999 0.1603 0.4060 0.088 Uiso 1 1 calc R . . C93 C 0.4971(7) 0.1286(4) 0.4368(4) 0.090(3) Uani 1 1 d . . . H93 H 0.5341 0.1380 0.4687 0.108 Uiso 1 1 calc R . . C94 C 0.4026(10) 0.1017(5) 0.4282(5) 0.114(4) Uani 1 1 d . . . H94 H 0.3770 0.0939 0.4548 0.137 Uiso 1 1 calc R . . C95 C 0.3434(8) 0.0854(5) 0.3823(5) 0.104(3) Uani 1 1 d . . . H95 H 0.2796 0.0668 0.3766 0.125 Uiso 1 1 calc R . . C96 C 0.3870(8) 0.0993(4) 0.3465(4) 0.089(3) Uani 1 1 d . . . O7 O 0.6018(4) 0.4568(3) 0.1737(3) 0.095(2) Uani 1 1 d . . . O8 O 0.7681(4) 0.4741(4) 0.2042(3) 0.120(3) Uani 1 1 d . . . O9 O 0.6941(7) 0.4621(5) 0.1262(3) 0.155(4) Uani 1 1 d . . . N25 N 0.6867(7) 0.4628(4) 0.1670(3) 0.100(3) Uani 1 1 d . . . O10 O 0.7086(6) 0.4238(3) 0.2874(3) 0.119(3) Uani 1 1 d . . . H10A H 0.6897 0.4350 0.2630 0.178 Uiso 1 1 d R . . O11A O 0.9738(9) 0.3093(3) 0.4694(3) 0.099(4) Uani 0.683(16) 1 d P A 1 H11A H 0.9703 0.3222 0.4940 0.099 Uiso 0.683(16) 1 d PR A 1 O11B O 1.082(3) 0.3118(14) 0.5186(12) 0.168(15) Uani 0.317(16) 1 d PU A 2 H11B H 1.1365 0.2972 0.5333 0.168 Uiso 0.317(16) 1 d PR A 2 O12 O 0.7569(9) 0.3616(4) 0.4496(4) 0.230(7) Uani 1 1 d . . . H12A H 0.8012 0.3377 0.4626 0.345 Uiso 1 1 d R . . H12B H 0.7647 0.3804 0.4331 0.345 Uiso 1 1 d R . . O13 O 0.8693(15) 0.4004(6) 0.3749(6) 0.259(8) Uani 1 1 d . . . H13A H 0.8547 0.4338 0.3805 0.389 Uiso 1 1 d R . . H13B H 0.8387 0.3969 0.3439 0.389 Uiso 1 1 d R . . O14A O 0.1896(14) 0.0667(8) 0.1435(7) 0.117(7) Uani 0.408(15) 1 d PU . . H14A H 0.1576 0.0789 0.1184 0.117 Uiso 0.408(15) 1 d PR . . O14B O 0.9726(15) 0.1313(9) 0.0525(7) 0.114(8) Uani 0.373(16) 1 d PU . . H14B H 1.0156 0.1137 0.0718 0.114 Uiso 0.373(16) 1 d PR . . O14C O 0.0658(14) 0.0137(9) 0.1089(6) 0.052(7) Uani 0.219(14) 1 d PU . . H14C H 0.0422 0.0424 0.1038 0.052 Uiso 0.219(14) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0431(4) 0.0450(5) 0.0424(4) 0.0022(4) 0.0099(3) -0.0007(4) Ni2 0.0637(6) 0.0641(7) 0.0454(5) 0.0103(4) 0.0024(4) -0.0072(5) Ni3 0.0634(6) 0.0620(6) 0.0492(5) -0.0015(4) 0.0191(4) -0.0121(5) Ni4 0.0661(6) 0.0547(6) 0.0649(6) 0.0036(5) 0.0117(5) -0.0024(5) Ni5 0.0558(5) 0.0642(7) 0.0600(6) 0.0058(5) 0.0080(4) 0.0022(5) O1 0.047(2) 0.056(3) 0.040(2) 0.002(2) 0.0116(18) -0.006(2) O2 0.063(3) 0.046(3) 0.054(3) 0.005(2) 0.018(2) 0.000(2) O3 0.052(2) 0.049(3) 0.059(3) 0.004(2) 0.006(2) 0.011(2) O4 0.066(3) 0.070(4) 0.049(3) 0.006(2) 0.020(2) -0.006(3) O5 0.067(3) 0.054(3) 0.054(3) -0.002(2) -0.002(2) 0.005(2) O6 0.066(3) 0.070(4) 0.062(3) 0.004(3) 0.007(2) -0.013(3) N1 0.040(3) 0.051(3) 0.039(3) 0.004(2) 0.008(2) 0.010(2) N2 0.046(3) 0.060(4) 0.044(3) 0.007(3) 0.013(2) 0.005(3) N3 0.065(3) 0.064(4) 0.039(3) -0.003(3) 0.011(3) -0.012(3) N4 0.084(4) 0.098(6) 0.049(3) -0.013(4) 0.012(3) -0.040(4) N5 0.047(3) 0.046(3) 0.048(3) -0.006(2) 0.012(2) -0.010(2) N6 0.040(3) 0.060(4) 0.065(4) -0.011(3) 0.011(3) -0.001(3) N7 0.073(4) 0.060(4) 0.060(4) 0.009(3) 0.007(3) -0.018(3) N8 0.099(6) 0.106(7) 0.157(8) 0.014(7) 0.083(6) -0.006(5) N9 0.055(3) 0.047(4) 0.046(3) 0.004(3) 0.016(2) 0.003(3) N10 0.070(4) 0.048(4) 0.056(3) -0.006(3) 0.014(3) -0.008(3) N11 0.073(4) 0.058(4) 0.072(4) 0.022(3) 0.019(3) 0.019(3) N12 0.100(5) 0.068(5) 0.080(5) 0.001(4) 0.031(4) 0.026(4) N13 0.084(4) 0.075(5) 0.046(3) 0.019(3) 0.010(3) -0.019(4) N14 0.109(6) 0.083(6) 0.072(5) 0.001(4) 0.038(4) -0.031(5) N15 0.056(3) 0.063(4) 0.059(3) -0.017(3) 0.021(3) -0.012(3) N16 0.117(6) 0.077(5) 0.086(5) 0.003(4) 0.066(4) 0.005(5) N17 0.059(3) 0.065(4) 0.063(4) 0.017(3) 0.003(3) -0.002(3) N18 0.070(4) 0.063(5) 0.084(5) 0.007(4) 0.018(4) -0.003(3) N19 0.062(4) 0.069(5) 0.062(4) 0.007(3) 0.014(3) -0.003(3) N20 0.090(5) 0.058(4) 0.079(5) -0.003(4) 0.008(4) -0.008(4) N21 0.073(4) 0.096(6) 0.054(4) 0.009(4) 0.006(3) -0.016(4) N22 0.078(5) 0.119(7) 0.090(6) -0.009(5) 0.001(4) -0.027(5) N23 0.055(3) 0.061(4) 0.072(4) 0.011(3) 0.015(3) 0.006(3) N24 0.060(4) 0.140(8) 0.117(7) -0.001(6) 0.035(4) -0.025(5) C1 0.051(4) 0.055(4) 0.047(3) -0.001(3) 0.012(3) -0.002(3) C2 0.040(3) 0.052(4) 0.042(3) 0.014(3) 0.011(3) 0.009(3) C3 0.047(3) 0.046(4) 0.042(3) 0.005(3) 0.014(3) 0.009(3) C4 0.056(4) 0.056(5) 0.056(4) -0.007(3) 0.015(3) 0.011(3) C5 0.077(5) 0.078(6) 0.043(4) -0.001(4) 0.011(3) 0.012(4) C6 0.067(5) 0.079(6) 0.056(4) 0.015(4) 0.029(4) 0.013(4) C7 0.049(4) 0.080(6) 0.050(4) 0.012(4) 0.023(3) 0.006(4) C8 0.043(3) 0.053(4) 0.060(4) 0.002(3) 0.016(3) 0.010(3) C9 0.056(4) 0.067(5) 0.049(4) -0.001(3) 0.014(3) -0.014(4) C10 0.054(4) 0.063(5) 0.064(4) 0.000(4) 0.013(3) -0.004(4) C11 0.072(5) 0.081(6) 0.058(4) -0.009(4) 0.005(4) -0.016(4) C12 0.117(7) 0.135(10) 0.048(4) -0.013(5) 0.019(5) -0.045(7) C13 0.153(10) 0.205(16) 0.061(6) -0.030(8) 0.028(6) -0.085(11) C14 0.150(10) 0.169(13) 0.051(5) -0.032(6) 0.019(6) -0.077(9) C15 0.162(10) 0.165(12) 0.054(5) -0.028(6) 0.003(6) -0.105(10) C16 0.091(6) 0.084(7) 0.067(5) -0.006(5) 0.013(4) -0.031(5) C17 0.040(3) 0.060(5) 0.055(4) -0.003(3) 0.002(3) -0.009(3) C18 0.043(3) 0.056(4) 0.051(4) -0.005(3) 0.010(3) -0.012(3) C19 0.043(3) 0.048(4) 0.056(4) -0.004(3) -0.002(3) 0.004(3) C20 0.055(4) 0.052(5) 0.058(4) 0.003(3) 0.013(3) -0.008(3) C21 0.067(5) 0.056(5) 0.071(5) 0.009(4) 0.008(4) -0.004(4) C22 0.070(5) 0.047(5) 0.083(5) 0.005(4) 0.010(4) 0.002(4) C23 0.047(4) 0.065(5) 0.074(5) -0.015(4) 0.007(3) 0.008(4) C24 0.050(4) 0.055(5) 0.057(4) -0.013(4) 0.010(3) -0.008(3) C25 0.066(5) 0.065(5) 0.089(6) 0.006(5) 0.030(4) -0.004(4) C26 0.064(5) 0.075(6) 0.083(5) 0.005(5) 0.028(4) -0.006(4) C27 0.073(5) 0.086(7) 0.060(5) 0.005(5) 0.016(4) -0.029(5) C28 0.092(6) 0.068(6) 0.078(5) 0.018(5) 0.005(5) -0.025(5) C29 0.141(10) 0.093(9) 0.120(9) 0.032(7) 0.040(8) -0.028(8) C30 0.179(14) 0.128(13) 0.162(13) 0.059(11) 0.094(11) -0.024(11) C31 0.155(12) 0.131(12) 0.224(17) 0.025(12) 0.128(12) -0.028(10) C32 0.123(8) 0.090(8) 0.130(9) 0.026(7) 0.069(8) -0.015(7) C33 0.060(4) 0.047(4) 0.054(4) -0.005(3) 0.020(3) -0.002(3) C34 0.057(4) 0.059(5) 0.040(3) -0.002(3) 0.019(3) -0.012(3) C35 0.042(3) 0.047(4) 0.051(4) 0.001(3) 0.009(3) -0.002(3) C36 0.051(4) 0.072(5) 0.048(4) -0.004(4) 0.006(3) 0.003(4) C37 0.050(4) 0.094(7) 0.064(5) -0.009(5) 0.004(3) 0.017(4) C38 0.054(4) 0.098(7) 0.061(5) -0.006(5) -0.001(4) -0.003(5) C39 0.061(4) 0.076(6) 0.056(4) 0.001(4) 0.005(3) -0.013(4) C40 0.051(4) 0.064(5) 0.052(4) -0.001(4) 0.012(3) -0.011(4) C41 0.071(5) 0.068(5) 0.050(4) 0.010(4) 0.007(3) 0.010(4) C42 0.083(5) 0.065(5) 0.056(4) 0.009(4) 0.018(4) 0.019(4) C43 0.073(5) 0.070(6) 0.071(5) 0.023(5) 0.022(4) 0.015(4) C44 0.071(5) 0.098(7) 0.085(6) 0.035(5) 0.011(5) 0.023(5) C45 0.089(7) 0.124(10) 0.114(9) 0.059(8) 0.025(6) 0.041(7) C46 0.119(9) 0.107(10) 0.121(9) 0.029(8) 0.035(8) 0.058(8) C47 0.121(8) 0.095(8) 0.090(7) 0.012(6) 0.014(6) 0.051(7) C48 0.086(6) 0.087(7) 0.074(5) 0.016(5) 0.016(5) 0.032(5) C49 0.083(5) 0.063(5) 0.057(4) 0.001(4) 0.010(4) -0.020(4) C50 0.084(5) 0.075(6) 0.044(4) -0.007(4) 0.019(4) -0.019(5) C51 0.091(5) 0.066(6) 0.048(4) 0.005(4) 0.007(4) -0.031(5) C52 0.093(6) 0.080(7) 0.068(5) 0.015(5) -0.001(4) -0.033(5) C53 0.115(8) 0.100(8) 0.070(6) 0.038(6) -0.011(6) -0.026(6) C54 0.130(9) 0.117(10) 0.063(6) 0.023(6) 0.010(6) -0.065(8) C55 0.118(8) 0.121(10) 0.074(6) 0.012(6) 0.019(5) -0.058(8) C56 0.111(7) 0.086(7) 0.050(4) 0.006(5) 0.013(5) -0.043(6) C57 0.081(5) 0.075(6) 0.072(5) -0.008(5) 0.033(4) -0.016(5) C58 0.075(5) 0.069(6) 0.058(4) -0.011(4) 0.027(4) -0.008(4) C59 0.062(4) 0.054(5) 0.058(4) -0.006(4) 0.013(3) -0.004(4) C60 0.060(4) 0.076(6) 0.046(4) -0.012(4) 0.011(3) -0.014(4) C61 0.089(6) 0.050(5) 0.071(5) -0.006(4) 0.006(4) 0.001(4) C62 0.119(8) 0.058(6) 0.096(7) -0.006(5) 0.028(6) 0.023(6) C63 0.132(9) 0.085(8) 0.117(8) -0.012(7) 0.067(7) 0.022(7) C64 0.104(6) 0.065(6) 0.086(6) 0.001(5) 0.045(5) -0.001(5) C65 0.055(4) 0.066(5) 0.058(4) 0.010(4) 0.012(3) 0.005(4) C66 0.072(5) 0.056(5) 0.059(4) 0.005(4) 0.007(4) -0.008(4) C67 0.057(4) 0.074(6) 0.060(4) 0.026(4) -0.001(4) -0.001(4) C68 0.065(5) 0.085(7) 0.096(6) 0.032(5) 0.009(5) 0.007(5) C69 0.079(7) 0.162(13) 0.090(7) 0.054(8) -0.005(5) 0.012(8) C70 0.079(7) 0.097(9) 0.126(9) 0.054(8) 0.023(6) 0.034(6) C71 0.067(5) 0.091(7) 0.120(8) 0.036(6) 0.024(5) 0.019(5) C72 0.076(5) 0.073(6) 0.092(6) 0.036(5) 0.030(5) 0.013(5) C73 0.087(6) 0.065(6) 0.076(5) 0.011(4) 0.025(5) 0.008(5) C74 0.070(5) 0.056(5) 0.055(4) 0.008(4) 0.008(4) 0.009(4) C75 0.064(4) 0.055(5) 0.054(4) -0.001(4) 0.004(3) -0.006(4) C76 0.062(5) 0.075(6) 0.071(5) 0.010(4) 0.007(4) 0.003(4) C77 0.058(5) 0.097(8) 0.109(7) 0.008(6) 0.003(5) 0.003(5) C78 0.082(7) 0.113(10) 0.111(8) 0.004(7) 0.000(6) -0.014(7) C79 0.097(7) 0.081(7) 0.091(7) -0.006(5) -0.001(5) -0.037(6) C80 0.078(5) 0.073(6) 0.076(5) 0.005(5) 0.012(4) -0.001(5) C81 0.058(5) 0.079(6) 0.066(5) 0.009(4) 0.004(4) -0.003(4) C82 0.057(4) 0.075(6) 0.086(6) -0.005(5) -0.001(4) -0.004(4) C83 0.082(6) 0.109(8) 0.062(5) 0.008(5) -0.010(4) -0.007(5) C84 0.090(6) 0.108(8) 0.064(5) 0.002(5) -0.002(5) -0.003(6) C85 0.117(8) 0.139(10) 0.054(5) -0.012(6) -0.004(5) 0.008(8) C86 0.114(9) 0.139(12) 0.103(9) -0.031(8) -0.043(8) 0.001(8) C87 0.109(8) 0.131(11) 0.100(8) -0.028(8) -0.006(7) -0.011(7) C88 0.087(6) 0.123(10) 0.077(6) -0.005(6) -0.018(5) -0.033(6) C89 0.053(5) 0.095(7) 0.093(7) 0.002(5) 0.004(4) -0.007(5) C90 0.066(5) 0.086(7) 0.074(5) 0.007(5) 0.010(4) -0.002(5) C91 0.053(4) 0.084(6) 0.081(6) 0.028(5) 0.019(4) 0.018(4) C92 0.063(5) 0.077(6) 0.084(6) 0.024(5) 0.029(4) 0.017(4) C93 0.086(6) 0.090(7) 0.103(7) 0.033(6) 0.043(5) 0.022(5) C94 0.120(9) 0.108(9) 0.146(11) 0.043(8) 0.088(9) 0.031(8) C95 0.071(6) 0.120(10) 0.135(10) 0.008(8) 0.051(7) 0.003(6) C96 0.084(6) 0.083(7) 0.112(8) 0.020(6) 0.046(6) 0.010(5) O7 0.053(3) 0.104(5) 0.130(5) -0.006(4) 0.030(3) 0.010(3) O8 0.048(3) 0.192(9) 0.116(5) 0.045(6) 0.016(3) -0.005(4) O9 0.146(7) 0.234(12) 0.090(6) -0.003(7) 0.042(5) -0.007(7) N25 0.079(6) 0.137(8) 0.082(6) 0.014(5) 0.021(5) 0.004(5) O10 0.122(5) 0.104(6) 0.153(7) -0.046(5) 0.075(5) 0.008(4) O11A 0.158(10) 0.054(6) 0.081(6) -0.033(5) 0.027(6) 0.006(6) O11B 0.180(17) 0.170(18) 0.161(17) -0.015(9) 0.062(10) -0.005(9) O12 0.236(11) 0.141(9) 0.208(11) -0.051(8) -0.107(9) 0.102(9) O13 0.42(2) 0.181(13) 0.244(15) -0.017(12) 0.201(17) 0.030(14) O14A 0.104(10) 0.127(11) 0.125(10) -0.033(8) 0.042(7) -0.003(7) O14B 0.123(11) 0.132(12) 0.110(11) -0.015(8) 0.071(8) 0.007(8) O14C 0.051(10) 0.078(11) 0.037(9) -0.011(7) 0.028(7) -0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.034(6) . y Ni1 N1 2.035(5) . y Ni1 N9 2.044(5) . y Ni1 O1 2.123(4) . y Ni1 O2 2.128(5) . y Ni1 O3 2.146(5) . y Ni2 N13 2.035(6) . y Ni2 N17 2.045(7) . y Ni2 N21 2.050(7) . y Ni2 O6 2.108(5) . y Ni2 O4 2.122(5) . y Ni2 O5 2.133(5) . y Ni3 N3 1.935(6) . y Ni3 O1 1.946(4) . y Ni3 O4 1.946(5) . y Ni3 N15 1.955(6) . y Ni4 N7 1.934(7) . y Ni4 N19 1.938(7) . y Ni4 O2 1.952(5) . y Ni4 O5 1.961(5) . y Ni5 O3 1.945(4) . y Ni5 N23 1.946(6) . y Ni5 O6 1.947(5) . y Ni5 N11 1.959(7) . y O1 C1 1.328(8) . ? O2 C17 1.343(8) . ? O3 C33 1.351(8) . ? O4 C49 1.325(10) . ? O5 C65 1.318(9) . ? O6 C81 1.333(9) . ? N1 C2 1.307(8) . ? N1 C3 1.395(8) . ? N2 C2 1.345(8) . ? N2 C8 1.346(8) . ? N2 H2 0.8800 . ? N3 C10 1.354(9) . ? N3 C11 1.403(9) . ? N4 C10 1.347(9) . ? N4 C16 1.362(10) . ? N4 H4 0.8800 . ? N5 C18 1.323(8) . ? N5 C19 1.385(9) . ? N6 C18 1.361(9) . ? N6 C24 1.385(9) . ? N6 H6 0.8800 . ? N7 C26 1.366(11) . ? N7 C27 1.385(10) . ? N8 C26 1.358(11) . ? N8 C32 1.373(14) . ? N8 H8 0.8800 . ? N9 C34 1.340(9) . ? N9 C35 1.384(8) . ? N10 C34 1.362(8) . ? N10 C40 1.371(9) . ? N10 H10 0.8800 . ? N11 C42 1.353(10) . ? N11 C43 1.392(10) . ? N12 C42 1.356(10) . ? N12 C48 1.375(11) . ? N12 H12 0.8800 . ? N13 C50 1.327(11) . ? N13 C51 1.393(10) . ? N14 C50 1.329(10) . ? N14 C56 1.371(12) . ? N14 H14 0.8800 . ? N15 C58 1.326(9) . ? N15 C59 1.396(10) . ? N16 C58 1.330(11) . ? N16 C64 1.379(11) . ? N16 H16 0.8800 . ? N17 C66 1.325(9) . ? N17 C67 1.367(9) . ? N18 C66 1.345(11) . ? N18 C72 1.405(11) . ? N18 H18 0.8800 . ? N19 C74 1.363(10) . ? N19 C75 1.399(9) . ? N20 C74 1.337(10) . ? N20 C80 1.380(11) . ? N20 H20 0.8800 . ? N21 C82 1.337(11) . ? N21 C83 1.416(11) . ? N22 C88 1.366(13) . ? N22 C82 1.374(10) . ? N22 H22 0.8800 . ? N23 C90 1.345(10) . ? N23 C91 1.400(10) . ? N24 C90 1.341(11) . ? N24 C96 1.425(13) . ? N24 H24 0.8800 . ? C1 C9 1.375(9) . ? C1 C2 1.489(9) . ? C3 C4 1.389(9) . ? C3 C8 1.423(9) . ? C4 C5 1.410(11) . ? C4 H4A 0.9500 . ? C5 C6 1.361(11) . ? C5 H5 0.9500 . ? C6 C7 1.376(10) . ? C6 H6A 0.9500 . ? C7 C8 1.409(9) . ? C7 H7 0.9500 . ? C9 C10 1.406(10) . ? C9 H9 0.9500 . ? C11 C12 1.394(12) . ? C11 C16 1.404(12) . ? C12 C13 1.395(13) . ? C12 H12C 0.9500 . ? C13 C14 1.363(15) . ? C13 H13 0.9500 . ? C14 C15 1.376(15) . ? C14 H14D 0.9500 . ? C15 C16 1.397(11) . ? C15 H15 0.9500 . ? C17 C25 1.374(11) . ? C17 C18 1.463(10) . ? C19 C20 1.381(10) . ? C19 C24 1.424(10) . ? C20 C21 1.379(10) . ? C20 H20A 0.9500 . ? C21 C22 1.376(12) . ? C21 H21 0.9500 . ? C22 C23 1.348(11) . ? C22 H22A 0.9500 . ? C23 C24 1.408(11) . ? C23 H23 0.9500 . ? C25 C26 1.393(12) . ? C25 H25 0.9500 . ? C27 C28 1.391(13) . ? C27 C32 1.403(14) . ? C28 C29 1.399(14) . ? C28 H28 0.9500 . ? C29 C30 1.376(19) . ? C29 H29 0.9500 . ? C30 C31 1.36(2) . ? C30 H30 0.9500 . ? C31 C32 1.395(16) . ? C31 H31 0.9500 . ? C33 C41 1.354(10) . ? C33 C34 1.443(10) . ? C35 C40 1.382(10) . ? C35 C36 1.385(10) . ? C36 C37 1.406(10) . ? C36 H36 0.9500 . ? C37 C38 1.366(12) . ? C37 H37 0.9500 . ? C38 C39 1.391(12) . ? C38 H38 0.9500 . ? C39 C40 1.436(10) . ? C39 H39 0.9500 . ? C41 C42 1.429(10) . ? C41 H41 0.9500 . ? C43 C48 1.400(13) . ? C43 C44 1.409(12) . ? C44 C45 1.428(14) . ? C44 H44 0.9500 . ? C45 C46 1.401(17) . ? C45 H45 0.9500 . ? C46 C47 1.359(16) . ? C46 H46 0.9500 . ? C47 C48 1.434(13) . ? C47 H47 0.9500 . ? C49 C57 1.337(12) . ? C49 C50 1.508(12) . ? C51 C56 1.377(13) . ? C51 C52 1.395(13) . ? C52 C53 1.437(13) . ? C52 H52 0.9500 . ? C53 C54 1.384(17) . ? C53 H53 0.9500 . ? C54 C55 1.377(17) . ? C54 H54 0.9500 . ? C55 C56 1.393(13) . ? C55 H55 0.9500 . ? C57 C58 1.431(12) . ? C57 H57 0.9500 . ? C59 C60 1.368(10) . ? C59 C64 1.397(11) . ? C60 C61 1.385(11) . ? C60 H60 0.9500 . ? C61 C62 1.377(13) . ? C61 H61 0.9500 . ? C62 C63 1.352(15) . ? C62 H62 0.9500 . ? C63 C64 1.424(14) . ? C63 H63 0.9500 . ? C65 C73 1.372(11) . ? C65 C66 1.486(10) . ? C67 C72 1.399(13) . ? C67 C68 1.406(11) . ? C68 C69 1.404(15) . ? C68 H68 0.9500 . ? C69 C70 1.417(17) . ? C69 H69 0.9500 . ? C70 C71 1.359(15) . ? C70 H70 0.9500 . ? C71 C72 1.373(13) . ? C71 H71 0.9500 . ? C73 C74 1.422(11) . ? C73 H73 0.9500 . ? C75 C80 1.392(12) . ? C75 C76 1.407(11) . ? C76 C77 1.366(12) . ? C76 H76 0.9500 . ? C77 C78 1.378(15) . ? C77 H77 0.9500 . ? C78 C79 1.392(15) . ? C78 H78 0.9500 . ? C79 C80 1.413(12) . ? C79 H79 0.9500 . ? C81 C89 1.312(12) . ? C81 C82 1.479(12) . ? C83 C84 1.390(14) . ? C83 C88 1.408(14) . ? C84 C85 1.418(13) . ? C84 H84 0.9500 . ? C85 C86 1.403(17) . ? C85 H85 0.9500 . ? C86 C87 1.408(19) . ? C86 H86 0.9500 . ? C87 C88 1.380(14) . ? C87 H87 0.9500 . ? C89 C90 1.440(12) . ? C89 H89 0.9500 . ? C91 C96 1.383(13) . ? C91 C92 1.400(12) . ? C92 C93 1.348(12) . ? C92 H92 0.9500 . ? C93 C94 1.396(16) . ? C93 H93 0.9500 . ? C94 C95 1.408(17) . ? C94 H94 0.9500 . ? C95 C96 1.374(14) . ? C95 H95 0.9500 . ? O7 N25 1.207(9) . ? O8 N25 1.326(10) . ? O9 N25 1.215(10) . ? O10 H10A 0.7414 . ? O11A H11A 0.8026 . ? O11B H11B 0.8264 . ? O12 H12A 0.8682 . ? O12 H12B 0.7152 . ? O13 H13A 0.9192 . ? O13 H13B 0.8830 . ? O14A H14A 0.7996 . ? O14B H14B 0.8178 . ? O14C H14C 0.8097 . ? 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 N5 Ni1 N1 97.6(2) . . y N5 Ni1 N9 97.0(2) . . y N1 Ni1 N9 103.9(2) . . y N5 Ni1 O1 94.9(2) . . y N1 Ni1 O1 78.5(2) . . y N9 Ni1 O1 167.4(2) . . y N5 Ni1 O2 79.3(2) . . y N1 Ni1 O2 163.3(2) . . y N9 Ni1 O2 92.8(2) . . y O1 Ni1 O2 85.4(2) . . y N5 Ni1 O3 168.0(2) . . y N1 Ni1 O3 94.4(2) . . y N9 Ni1 O3 78.9(2) . . y O1 Ni1 O3 88.6(2) . . y O2 Ni1 O3 89.6(2) . . y N13 Ni2 N17 101.0(3) . . y N13 Ni2 N21 96.1(3) . . y N17 Ni2 N21 101.7(3) . . y N13 Ni2 O6 167.4(3) . . y N17 Ni2 O6 91.5(2) . . y N21 Ni2 O6 79.6(2) . . y N13 Ni2 O4 78.7(3) . . y N17 Ni2 O4 165.6(2) . . y N21 Ni2 O4 92.6(3) . . y O6 Ni2 O4 89.6(2) . . y N13 Ni2 O5 95.6(2) . . y N17 Ni2 O5 79.6(2) . . y N21 Ni2 O5 167.7(2) . . y O6 Ni2 O5 88.2(2) . . y O4 Ni2 O5 86.1(2) . . y N3 Ni3 O1 94.3(2) . . y N3 Ni3 O4 113.6(2) . . y O1 Ni3 O4 136.0(2) . . y N3 Ni3 N15 98.9(2) . . y O1 Ni3 N15 117.6(2) . . y O4 Ni3 N15 91.9(2) . . y N7 Ni4 N19 100.0(3) . . y N7 Ni4 O2 92.5(2) . . y N19 Ni4 O2 115.5(2) . . y N7 Ni4 O5 121.3(2) . . y N19 Ni4 O5 93.7(2) . . y O2 Ni4 O5 131.2(2) . . y O3 Ni5 N23 115.2(2) . . y O3 Ni5 O6 130.8(2) . . y N23 Ni5 O6 93.0(2) . . y O3 Ni5 N11 94.3(2) . . y N23 Ni5 N11 97.5(3) . . y O6 Ni5 N11 122.4(3) . . y C1 O1 Ni3 124.5(4) . . ? C1 O1 Ni1 114.8(4) . . ? Ni3 O1 Ni1 120.1(2) . . y C17 O2 Ni4 125.0(4) . . ? C17 O2 Ni1 113.6(4) . . ? Ni4 O2 Ni1 119.5(2) . . y C33 O3 Ni5 125.1(4) . . ? C33 O3 Ni1 113.3(4) . . ? Ni5 O3 Ni1 120.5(2) . . y C49 O4 Ni3 125.7(5) . . ? C49 O4 Ni2 115.6(5) . . ? Ni3 O4 Ni2 116.9(2) . . y C65 O5 Ni4 125.7(4) . . ? C65 O5 Ni2 113.6(4) . . ? Ni4 O5 Ni2 119.2(3) . . y C81 O6 Ni5 124.4(5) . . ? C81 O6 Ni2 115.3(5) . . ? Ni5 O6 Ni2 117.6(2) . . y C2 N1 C3 105.1(5) . . ? C2 N1 Ni1 114.9(4) . . ? C3 N1 Ni1 139.8(4) . . ? C2 N2 C8 107.1(6) . . ? C2 N2 H2 126.5 . . ? C8 N2 H2 126.5 . . ? C10 N3 C11 104.8(6) . . ? C10 N3 Ni3 124.6(5) . . ? C11 N3 Ni3 130.5(5) . . ? C10 N4 C16 109.2(7) . . ? C10 N4 H4 125.4 . . ? C16 N4 H4 125.4 . . ? C18 N5 C19 107.2(6) . . ? C18 N5 Ni1 113.2(5) . . ? C19 N5 Ni1 139.5(4) . . ? C18 N6 C24 108.4(6) . . ? C18 N6 H6 125.8 . . ? C24 N6 H6 125.8 . . ? C26 N7 C27 106.7(7) . . ? C26 N7 Ni4 125.9(5) . . ? C27 N7 Ni4 127.4(6) . . ? C26 N8 C32 107.8(9) . . ? C26 N8 H8 126.1 . . ? C32 N8 H8 126.1 . . ? C34 N9 C35 104.9(6) . . ? C34 N9 Ni1 113.0(4) . . ? C35 N9 Ni1 141.5(5) . . ? C34 N10 C40 106.4(6) . . ? C34 N10 H10 126.8 . . ? C40 N10 H10 126.8 . . ? C42 N11 C43 106.0(7) . . ? C42 N11 Ni5 124.2(5) . . ? C43 N11 Ni5 129.1(6) . . ? C42 N12 C48 107.2(8) . . ? C42 N12 H12 126.4 . . ? C48 N12 H12 126.4 . . ? C50 N13 C51 104.8(7) . . ? C50 N13 Ni2 114.0(5) . . ? C51 N13 Ni2 139.5(7) . . ? C50 N14 C56 107.0(8) . . ? C50 N14 H14 126.5 . . ? C56 N14 H14 126.5 . . ? C58 N15 C59 106.8(6) . . ? C58 N15 Ni3 126.0(6) . . ? C59 N15 Ni3 127.2(5) . . ? C58 N16 C64 109.3(7) . . ? C58 N16 H16 125.4 . . ? C64 N16 H16 125.4 . . ? C66 N17 C67 106.1(7) . . ? C66 N17 Ni2 112.5(5) . . ? C67 N17 Ni2 141.5(6) . . ? C66 N18 C72 106.9(7) . . ? C66 N18 H18 126.6 . . ? C72 N18 H18 126.6 . . ? C74 N19 C75 104.6(6) . . ? C74 N19 Ni4 124.9(5) . . ? C75 N19 Ni4 130.4(6) . . ? C74 N20 C80 108.3(7) . . ? C74 N20 H20 125.8 . . ? C80 N20 H20 125.8 . . ? C82 N21 C83 107.0(7) . . ? C82 N21 Ni2 111.4(5) . . ? C83 N21 Ni2 141.6(6) . . ? C88 N22 C82 108.5(8) . . ? C88 N22 H22 125.7 . . ? C82 N22 H22 125.7 . . ? C90 N23 C91 104.8(7) . . ? C90 N23 Ni5 125.4(6) . . ? C91 N23 Ni5 129.6(6) . . ? C90 N24 C96 106.9(8) . . ? C90 N24 H24 126.6 . . ? C96 N24 H24 126.6 . . ? O1 C1 C9 126.8(6) . . ? O1 C1 C2 112.4(5) . . ? C9 C1 C2 120.8(6) . . ? N1 C2 N2 113.9(5) . . ? N1 C2 C1 119.0(5) . . ? N2 C2 C1 127.0(6) . . ? C4 C3 N1 131.4(6) . . ? C4 C3 C8 121.2(6) . . ? N1 C3 C8 107.4(5) . . ? C3 C4 C5 115.9(7) . . ? C3 C4 H4A 122.1 . . ? C5 C4 H4A 122.1 . . ? C6 C5 C4 123.0(7) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C7 122.2(7) . . ? C5 C6 H6A 118.9 . . ? C7 C6 H6A 118.9 . . ? C6 C7 C8 117.0(7) . . ? C6 C7 H7 121.5 . . ? C8 C7 H7 121.5 . . ? N2 C8 C7 132.7(6) . . ? N2 C8 C3 106.5(6) . . ? C7 C8 C3 120.7(6) . . ? C1 C9 C10 124.5(7) . . ? C1 C9 H9 117.8 . . ? C10 C9 H9 117.8 . . ? N4 C10 N3 111.3(6) . . ? N4 C10 C9 123.3(7) . . ? N3 C10 C9 125.2(6) . . ? C12 C11 N3 129.0(7) . . ? C12 C11 C16 121.7(7) . . ? N3 C11 C16 109.1(7) . . ? C11 C12 C13 115.7(9) . . ? C11 C12 H12C 122.2 . . ? C13 C12 H12C 122.2 . . ? C14 C13 C12 122.0(10) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 123.3(9) . . ? C13 C14 H14D 118.3 . . ? C15 C14 H14D 118.3 . . ? C14 C15 C16 115.9(9) . . ? C14 C15 H15 122.0 . . ? C16 C15 H15 122.0 . . ? N4 C16 C15 133.3(9) . . ? N4 C16 C11 105.6(7) . . ? C15 C16 C11 121.1(9) . . ? O2 C17 C25 126.2(7) . . ? O2 C17 C18 112.7(6) . . ? C25 C17 C18 120.7(7) . . ? N5 C18 N6 111.2(6) . . ? N5 C18 C17 120.6(6) . . ? N6 C18 C17 128.2(6) . . ? C20 C19 N5 132.8(6) . . ? C20 C19 C24 118.8(7) . . ? N5 C19 C24 108.4(6) . . ? C21 C20 C19 118.2(7) . . ? C21 C20 H20A 120.9 . . ? C19 C20 H20A 120.9 . . ? C22 C21 C20 121.9(8) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C23 C22 C21 122.7(8) . . ? C23 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? C22 C23 C24 116.5(7) . . ? C22 C23 H23 121.8 . . ? C24 C23 H23 121.8 . . ? N6 C24 C23 133.4(7) . . ? N6 C24 C19 104.8(6) . . ? C23 C24 C19 121.9(7) . . ? C17 C25 C26 123.7(8) . . ? C17 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? N8 C26 N7 110.2(8) . . ? N8 C26 C25 124.5(9) . . ? N7 C26 C25 125.3(7) . . ? N7 C27 C28 130.3(9) . . ? N7 C27 C32 107.7(9) . . ? C28 C27 C32 122.0(9) . . ? C27 C28 C29 115.4(11) . . ? C27 C28 H28 122.3 . . ? C29 C28 H28 122.3 . . ? C30 C29 C28 121.7(12) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C31 C30 C29 123.5(12) . . ? C31 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? C30 C31 C32 116.1(14) . . ? C30 C31 H31 121.9 . . ? C32 C31 H31 121.9 . . ? N8 C32 C31 131.4(13) . . ? N8 C32 C27 107.3(8) . . ? C31 C32 C27 121.2(12) . . ? O3 C33 C41 125.9(6) . . ? O3 C33 C34 112.7(6) . . ? C41 C33 C34 121.4(6) . . ? N9 C34 N10 112.2(6) . . ? N9 C34 C33 120.8(6) . . ? N10 C34 C33 127.0(7) . . ? C40 C35 N9 109.5(6) . . ? C40 C35 C36 120.9(6) . . ? N9 C35 C36 129.6(6) . . ? C35 C36 C37 115.9(7) . . ? C35 C36 H36 122.0 . . ? C37 C36 H36 122.0 . . ? C38 C37 C36 123.2(8) . . ? C38 C37 H37 118.4 . . ? C36 C37 H37 118.4 . . ? C37 C38 C39 122.7(7) . . ? C37 C38 H38 118.7 . . ? C39 C38 H38 118.7 . . ? C38 C39 C40 113.7(8) . . ? C38 C39 H39 123.1 . . ? C40 C39 H39 123.1 . . ? N10 C40 C35 107.0(6) . . ? N10 C40 C39 129.5(7) . . ? C35 C40 C39 123.5(7) . . ? C33 C41 C42 125.7(7) . . ? C33 C41 H41 117.2 . . ? C42 C41 H41 117.2 . . ? N11 C42 N12 111.5(7) . . ? N11 C42 C41 124.7(7) . . ? N12 C42 C41 123.8(8) . . ? N11 C43 C48 107.9(7) . . ? N11 C43 C44 130.6(9) . . ? C48 C43 C44 121.4(8) . . ? C43 C44 C45 115.1(11) . . ? C43 C44 H44 122.4 . . ? C45 C44 H44 122.4 . . ? C46 C45 C44 122.5(11) . . ? C46 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C47 C46 C45 122.4(10) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C46 C47 C48 116.2(11) . . ? C46 C47 H47 121.9 . . ? C48 C47 H47 121.9 . . ? N12 C48 C43 107.3(8) . . ? N12 C48 C47 130.4(10) . . ? C43 C48 C47 122.2(9) . . ? O4 C49 C57 126.8(8) . . ? O4 C49 C50 111.5(8) . . ? C57 C49 C50 121.7(8) . . ? N13 C50 N14 113.0(8) . . ? N13 C50 C49 118.9(7) . . ? N14 C50 C49 128.1(9) . . ? C56 C51 N13 108.6(9) . . ? C56 C51 C52 123.1(8) . . ? N13 C51 C52 128.3(9) . . ? C51 C52 C53 116.1(11) . . ? C51 C52 H52 122.0 . . ? C53 C52 H52 122.0 . . ? C54 C53 C52 119.4(11) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 123.2(10) . . ? C55 C54 H54 118.4 . . ? C53 C54 H54 118.4 . . ? C54 C55 C56 117.6(12) . . ? C54 C55 H55 121.2 . . ? C56 C55 H55 121.2 . . ? N14 C56 C51 106.7(7) . . ? N14 C56 C55 132.8(11) . . ? C51 C56 C55 120.5(11) . . ? C49 C57 C58 124.1(8) . . ? C49 C57 H57 118.0 . . ? C58 C57 H57 118.0 . . ? N15 C58 N16 110.8(8) . . ? N15 C58 C57 124.5(8) . . ? N16 C58 C57 124.7(7) . . ? C60 C59 N15 133.0(7) . . ? C60 C59 C64 119.1(8) . . ? N15 C59 C64 107.9(7) . . ? C59 C60 C61 119.7(8) . . ? C59 C60 H60 120.1 . . ? C61 C60 H60 120.1 . . ? C62 C61 C60 121.1(9) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C63 C62 C61 121.3(9) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C62 C63 C64 117.8(9) . . ? C62 C63 H63 121.1 . . ? C64 C63 H63 121.1 . . ? N16 C64 C59 105.2(8) . . ? N16 C64 C63 133.8(9) . . ? C59 C64 C63 120.9(9) . . ? O5 C65 C73 126.0(7) . . ? O5 C65 C66 113.1(7) . . ? C73 C65 C66 120.9(8) . . ? N17 C66 N18 112.5(7) . . ? N17 C66 C65 120.3(7) . . ? N18 C66 C65 127.2(7) . . ? N17 C67 C72 109.8(7) . . ? N17 C67 C68 129.4(9) . . ? C72 C67 C68 120.8(8) . . ? C69 C68 C67 114.9(11) . . ? C69 C68 H68 122.6 . . ? C67 C68 H68 122.6 . . ? C68 C69 C70 122.3(10) . . ? C68 C69 H69 118.8 . . ? C70 C69 H69 118.8 . . ? C71 C70 C69 121.8(10) . . ? C71 C70 H70 119.1 . . ? C69 C70 H70 119.1 . . ? C70 C71 C72 116.3(11) . . ? C70 C71 H71 121.9 . . ? C72 C71 H71 121.9 . . ? C71 C72 C67 123.9(9) . . ? C71 C72 N18 131.4(10) . . ? C67 C72 N18 104.7(7) . . ? C65 C73 C74 125.0(8) . . ? C65 C73 H73 117.5 . . ? C74 C73 H73 117.5 . . ? N20 C74 N19 111.7(7) . . ? N20 C74 C73 123.7(8) . . ? N19 C74 C73 124.6(7) . . ? C80 C75 N19 109.3(7) . . ? C80 C75 C76 119.8(7) . . ? N19 C75 C76 130.9(7) . . ? C77 C76 C75 116.4(9) . . ? C77 C76 H76 121.8 . . ? C75 C76 H76 121.8 . . ? C76 C77 C78 123.6(10) . . ? C76 C77 H77 118.2 . . ? C78 C77 H77 118.2 . . ? C77 C78 C79 122.1(10) . . ? C77 C78 H78 119.0 . . ? C79 C78 H78 119.0 . . ? C78 C79 C80 114.3(10) . . ? C78 C79 H79 122.8 . . ? C80 C79 H79 122.8 . . ? N20 C80 C75 106.0(7) . . ? N20 C80 C79 130.4(9) . . ? C75 C80 C79 123.6(9) . . ? C89 C81 O6 127.2(8) . . ? C89 C81 C82 121.7(8) . . ? O6 C81 C82 111.1(7) . . ? N21 C82 N22 110.3(8) . . ? N21 C82 C81 121.6(7) . . ? N22 C82 C81 128.1(8) . . ? C84 C83 C88 122.8(9) . . ? C84 C83 N21 130.0(9) . . ? C88 C83 N21 107.2(9) . . ? C83 C84 C85 116.0(10) . . ? C83 C84 H84 122.0 . . ? C85 C84 H84 122.0 . . ? C86 C85 C84 120.7(11) . . ? C86 C85 H85 119.6 . . ? C84 C85 H85 119.6 . . ? C85 C86 C87 122.2(10) . . ? C85 C86 H86 118.9 . . ? C87 C86 H86 118.9 . . ? C88 C87 C86 116.7(12) . . ? C88 C87 H87 121.7 . . ? C86 C87 H87 121.7 . . ? N22 C88 C87 131.7(11) . . ? N22 C88 C83 106.9(8) . . ? C87 C88 C83 121.4(12) . . ? C81 C89 C90 125.6(8) . . ? C81 C89 H89 117.2 . . ? C90 C89 H89 117.2 . . ? N24 C90 N23 113.0(8) . . ? N24 C90 C89 123.7(8) . . ? N23 C90 C89 123.2(8) . . ? C96 C91 N23 110.2(8) . . ? C96 C91 C92 120.2(9) . . ? N23 C91 C92 129.6(8) . . ? C93 C92 C91 117.8(9) . . ? C93 C92 H92 121.1 . . ? C91 C92 H92 121.1 . . ? C92 C93 C94 120.8(11) . . ? C92 C93 H93 119.6 . . ? C94 C93 H93 119.6 . . ? C93 C94 C95 123.5(10) . . ? C93 C94 H94 118.2 . . ? C95 C94 H94 118.2 . . ? C96 C95 C94 113.3(10) . . ? C96 C95 H95 123.3 . . ? C94 C95 H95 123.3 . . ? C95 C96 C91 124.3(11) . . ? C95 C96 N24 130.6(10) . . ? C91 C96 N24 105.1(8) . . ? O7 N25 O9 119.5(9) . . ? O7 N25 O8 118.6(9) . . ? O9 N25 O8 121.6(9) . . ? H11A O11B H11B 162.3 . . ? H12A O12 H12B 125.3 . . ? H13A O13 H13B 102.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni3 O1 C1 3.3(5) . . . . ? O4 Ni3 O1 C1 134.2(5) . . . . ? N15 Ni3 O1 C1 -99.1(5) . . . . ? N3 Ni3 O1 Ni1 173.8(3) . . . . ? O4 Ni3 O1 Ni1 -55.3(4) . . . . ? N15 Ni3 O1 Ni1 71.4(3) . . . . ? N5 Ni1 O1 C1 91.0(5) . . . . ? N1 Ni1 O1 C1 -5.8(4) . . . . ? N9 Ni1 O1 C1 -108.2(9) . . . . ? O2 Ni1 O1 C1 169.8(5) . . . . ? O3 Ni1 O1 C1 -100.6(5) . . . . ? N5 Ni1 O1 Ni3 -80.4(3) . . . . ? N1 Ni1 O1 Ni3 -177.2(3) . . . . ? N9 Ni1 O1 Ni3 80.4(9) . . . . ? O2 Ni1 O1 Ni3 -1.6(3) . . . . ? O3 Ni1 O1 Ni3 88.0(3) . . . . ? N7 Ni4 O2 C17 12.3(5) . . . . ? N19 Ni4 O2 C17 -90.0(5) . . . . ? O5 Ni4 O2 C17 149.2(5) . . . . ? N7 Ni4 O2 Ni1 175.7(3) . . . . ? N19 Ni4 O2 Ni1 73.4(3) . . . . ? O5 Ni4 O2 Ni1 -47.4(4) . . . . ? N5 Ni1 O2 C17 -7.5(4) . . . . ? N1 Ni1 O2 C17 -88.2(8) . . . . ? N9 Ni1 O2 C17 89.1(4) . . . . ? O1 Ni1 O2 C17 -103.3(4) . . . . ? O3 Ni1 O2 C17 168.0(4) . . . . ? N5 Ni1 O2 Ni4 -172.7(3) . . . . ? N1 Ni1 O2 Ni4 106.6(7) . . . . ? N9 Ni1 O2 Ni4 -76.1(3) . . . . ? O1 Ni1 O2 Ni4 91.5(3) . . . . ? O3 Ni1 O2 Ni4 2.8(3) . . . . ? N23 Ni5 O3 C33 -100.2(5) . . . . ? O6 Ni5 O3 C33 140.9(5) . . . . ? N11 Ni5 O3 C33 0.2(5) . . . . ? N23 Ni5 O3 Ni1 66.6(3) . . . . ? O6 Ni5 O3 Ni1 -52.3(4) . . . . ? N11 Ni5 O3 Ni1 167.0(3) . . . . ? N5 Ni1 O3 C33 -78.3(10) . . . . ? N1 Ni1 O3 C33 96.2(4) . . . . ? N9 Ni1 O3 C33 -7.2(4) . . . . ? O1 Ni1 O3 C33 174.5(4) . . . . ? O2 Ni1 O3 C33 -100.1(4) . . . . ? N5 Ni1 O3 Ni5 113.5(9) . . . . ? N1 Ni1 O3 Ni5 -72.1(3) . . . . ? N9 Ni1 O3 Ni5 -175.5(3) . . . . ? O1 Ni1 O3 Ni5 6.2(3) . . . . ? O2 Ni1 O3 Ni5 91.6(3) . . . . ? N3 Ni3 O4 C49 -90.1(6) . . . . ? O1 Ni3 O4 C49 145.2(5) . . . . ? N15 Ni3 O4 C49 10.5(6) . . . . ? N3 Ni3 O4 Ni2 73.9(3) . . . . ? O1 Ni3 O4 Ni2 -50.8(4) . . . . ? N15 Ni3 O4 Ni2 174.4(3) . . . . ? N13 Ni2 O4 C49 -9.3(5) . . . . ? N17 Ni2 O4 C49 -99.5(10) . . . . ? N21 Ni2 O4 C49 86.4(5) . . . . ? O6 Ni2 O4 C49 166.0(5) . . . . ? O5 Ni2 O4 C49 -105.8(5) . . . . ? N13 Ni2 O4 Ni3 -174.9(3) . . . . ? N17 Ni2 O4 Ni3 94.9(9) . . . . ? N21 Ni2 O4 Ni3 -79.2(3) . . . . ? O6 Ni2 O4 Ni3 0.4(3) . . . . ? O5 Ni2 O4 Ni3 88.6(3) . . . . ? N7 Ni4 O5 C65 -100.8(6) . . . . ? N19 Ni4 O5 C65 3.2(6) . . . . ? O2 Ni4 O5 C65 132.3(6) . . . . ? N7 Ni4 O5 Ni2 63.8(4) . . . . ? N19 Ni4 O5 Ni2 167.8(3) . . . . ? O2 Ni4 O5 Ni2 -63.1(4) . . . . ? N13 Ni2 O5 C65 91.1(5) . . . . ? N17 Ni2 O5 C65 -9.1(5) . . . . ? N21 Ni2 O5 C65 -106.2(13) . . . . ? O6 Ni2 O5 C65 -101.0(5) . . . . ? O4 Ni2 O5 C65 169.3(5) . . . . ? N13 Ni2 O5 Ni4 -75.3(3) . . . . ? N17 Ni2 O5 Ni4 -175.5(3) . . . . ? N21 Ni2 O5 Ni4 87.4(13) . . . . ? O6 Ni2 O5 Ni4 92.6(3) . . . . ? O4 Ni2 O5 Ni4 2.9(3) . . . . ? O3 Ni5 O6 C81 139.2(6) . . . . ? N23 Ni5 O6 C81 11.8(6) . . . . ? N11 Ni5 O6 C81 -89.1(6) . . . . ? O3 Ni5 O6 Ni2 -60.7(4) . . . . ? N23 Ni5 O6 Ni2 171.9(3) . . . . ? N11 Ni5 O6 Ni2 70.9(4) . . . . ? N13 Ni2 O6 C81 -80.9(11) . . . . ? N17 Ni2 O6 C81 91.8(6) . . . . ? N21 Ni2 O6 C81 -9.8(6) . . . . ? O4 Ni2 O6 C81 -102.5(6) . . . . ? O5 Ni2 O6 C81 171.3(6) . . . . ? N13 Ni2 O6 Ni5 117.2(9) . . . . ? N17 Ni2 O6 Ni5 -70.1(3) . . . . ? N21 Ni2 O6 Ni5 -171.7(4) . . . . ? O4 Ni2 O6 Ni5 95.6(3) . . . . ? O5 Ni2 O6 Ni5 9.5(3) . . . . ? N5 Ni1 N1 C2 -88.8(5) . . . . ? N9 Ni1 N1 C2 172.0(4) . . . . ? O1 Ni1 N1 C2 4.7(4) . . . . ? O2 Ni1 N1 C2 -10.7(9) . . . . ? O3 Ni1 N1 C2 92.4(5) . . . . ? N5 Ni1 N1 C3 86.7(7) . . . . ? N9 Ni1 N1 C3 -12.5(7) . . . . ? O1 Ni1 N1 C3 -179.8(7) . . . . ? O2 Ni1 N1 C3 164.8(6) . . . . ? O3 Ni1 N1 C3 -92.1(7) . . . . ? O1 Ni3 N3 C10 -0.9(6) . . . . ? O4 Ni3 N3 C10 -145.9(6) . . . . ? N15 Ni3 N3 C10 118.0(6) . . . . ? O1 Ni3 N3 C11 -176.7(7) . . . . ? O4 Ni3 N3 C11 38.3(8) . . . . ? N15 Ni3 N3 C11 -57.8(8) . . . . ? N1 Ni1 N5 C18 169.0(4) . . . . ? N9 Ni1 N5 C18 -85.9(4) . . . . ? O1 Ni1 N5 C18 90.0(4) . . . . ? O2 Ni1 N5 C18 5.7(4) . . . . ? O3 Ni1 N5 C18 -16.6(11) . . . . ? N1 Ni1 N5 C19 -14.1(6) . . . . ? N9 Ni1 N5 C19 91.0(6) . . . . ? O1 Ni1 N5 C19 -93.1(6) . . . . ? O2 Ni1 N5 C19 -177.5(6) . . . . ? O3 Ni1 N5 C19 160.3(8) . . . . ? N19 Ni4 N7 C26 111.8(7) . . . . ? O2 Ni4 N7 C26 -4.6(6) . . . . ? O5 Ni4 N7 C26 -147.6(6) . . . . ? N19 Ni4 N7 C27 -67.1(6) . . . . ? O2 Ni4 N7 C27 176.5(6) . . . . ? O5 Ni4 N7 C27 33.4(7) . . . . ? N5 Ni1 N9 C34 168.8(4) . . . . ? N1 Ni1 N9 C34 -91.6(4) . . . . ? O1 Ni1 N9 C34 8.0(11) . . . . ? O2 Ni1 N9 C34 89.2(4) . . . . ? O3 Ni1 N9 C34 0.2(4) . . . . ? N5 Ni1 N9 C35 -0.1(7) . . . . ? N1 Ni1 N9 C35 99.5(7) . . . . ? O1 Ni1 N9 C35 -160.9(7) . . . . ? O2 Ni1 N9 C35 -79.7(7) . . . . ? O3 Ni1 N9 C35 -168.7(7) . . . . ? O3 Ni5 N11 C42 -1.7(6) . . . . ? N23 Ni5 N11 C42 114.4(6) . . . . ? O6 Ni5 N11 C42 -147.2(6) . . . . ? O3 Ni5 N11 C43 -171.0(6) . . . . ? N23 Ni5 N11 C43 -54.9(7) . . . . ? O6 Ni5 N11 C43 43.5(7) . . . . ? N17 Ni2 N13 C50 175.9(5) . . . . ? N21 Ni2 N13 C50 -80.9(6) . . . . ? O6 Ni2 N13 C50 -11.5(13) . . . . ? O4 Ni2 N13 C50 10.5(5) . . . . ? O5 Ni2 N13 C50 95.4(5) . . . . ? N17 Ni2 N13 C51 -22.3(8) . . . . ? N21 Ni2 N13 C51 80.9(8) . . . . ? O6 Ni2 N13 C51 150.3(9) . . . . ? O4 Ni2 N13 C51 172.3(8) . . . . ? O5 Ni2 N13 C51 -102.7(8) . . . . ? N3 Ni3 N15 C58 108.9(6) . . . . ? O1 Ni3 N15 C58 -151.4(5) . . . . ? O4 Ni3 N15 C58 -5.3(6) . . . . ? N3 Ni3 N15 C59 -69.0(6) . . . . ? O1 Ni3 N15 C59 30.6(6) . . . . ? O4 Ni3 N15 C59 176.7(5) . . . . ? N13 Ni2 N17 C66 -88.0(5) . . . . ? N21 Ni2 N17 C66 173.3(5) . . . . ? O6 Ni2 N17 C66 93.6(5) . . . . ? O4 Ni2 N17 C66 -0.7(12) . . . . ? O5 Ni2 N17 C66 5.7(5) . . . . ? N13 Ni2 N17 C67 93.2(8) . . . . ? N21 Ni2 N17 C67 -5.5(9) . . . . ? O6 Ni2 N17 C67 -85.1(8) . . . . ? O5 Ni2 N17 C67 -173.0(9) . . . . ? N7 Ni4 N19 C74 123.7(6) . . . . ? O2 Ni4 N19 C74 -138.7(6) . . . . ? O5 Ni4 N19 C74 1.0(6) . . . . ? N7 Ni4 N19 C75 -52.2(7) . . . . ? O2 Ni4 N19 C75 45.4(7) . . . . ? O5 Ni4 N19 C75 -174.9(6) . . . . ? N13 Ni2 N21 C82 175.3(7) . . . . ? N17 Ni2 N21 C82 -82.1(7) . . . . ? O6 Ni2 N21 C82 7.3(6) . . . . ? O4 Ni2 N21 C82 96.4(6) . . . . ? O5 Ni2 N21 C82 12.6(17) . . . . ? N13 Ni2 N21 C83 -6.5(11) . . . . ? N17 Ni2 N21 C83 96.1(11) . . . . ? O6 Ni2 N21 C83 -174.5(11) . . . . ? O4 Ni2 N21 C83 -85.4(11) . . . . ? O5 Ni2 N21 C83 -169.2(10) . . . . ? O3 Ni5 N23 C90 -145.4(7) . . . . ? O6 Ni5 N23 C90 -7.0(7) . . . . ? N11 Ni5 N23 C90 116.2(7) . . . . ? O3 Ni5 N23 C91 40.0(7) . . . . ? O6 Ni5 N23 C91 178.4(7) . . . . ? N11 Ni5 N23 C91 -58.4(7) . . . . ? Ni3 O1 C1 C9 -4.2(10) . . . . ? Ni1 O1 C1 C9 -175.1(6) . . . . ? Ni3 O1 C1 C2 176.7(4) . . . . ? Ni1 O1 C1 C2 5.7(7) . . . . ? C3 N1 C2 N2 -2.0(7) . . . . ? Ni1 N1 C2 N2 175.0(4) . . . . ? C3 N1 C2 C1 179.8(6) . . . . ? Ni1 N1 C2 C1 -3.2(7) . . . . ? C8 N2 C2 N1 0.9(8) . . . . ? C8 N2 C2 C1 178.9(6) . . . . ? O1 C1 C2 N1 -1.9(9) . . . . ? C9 C1 C2 N1 178.9(7) . . . . ? O1 C1 C2 N2 -179.8(6) . . . . ? C9 C1 C2 N2 1.0(11) . . . . ? C2 N1 C3 C4 178.9(7) . . . . ? Ni1 N1 C3 C4 3.1(12) . . . . ? C2 N1 C3 C8 2.2(7) . . . . ? Ni1 N1 C3 C8 -173.6(5) . . . . ? N1 C3 C4 C5 179.9(7) . . . . ? C8 C3 C4 C5 -3.8(10) . . . . ? C3 C4 C5 C6 1.0(11) . . . . ? C4 C5 C6 C7 0.9(13) . . . . ? C5 C6 C7 C8 0.0(12) . . . . ? C2 N2 C8 C7 176.2(7) . . . . ? C2 N2 C8 C3 0.6(7) . . . . ? C6 C7 C8 N2 -177.9(7) . . . . ? C6 C7 C8 C3 -2.8(10) . . . . ? C4 C3 C8 N2 -178.9(6) . . . . ? N1 C3 C8 N2 -1.8(7) . . . . ? C4 C3 C8 C7 4.9(10) . . . . ? N1 C3 C8 C7 -178.0(6) . . . . ? O1 C1 C9 C10 1.7(13) . . . . ? C2 C1 C9 C10 -179.2(7) . . . . ? C16 N4 C10 N3 -0.1(10) . . . . ? C16 N4 C10 C9 -175.5(8) . . . . ? C11 N3 C10 N4 0.4(9) . . . . ? Ni3 N3 C10 N4 -176.3(5) . . . . ? C11 N3 C10 C9 175.7(8) . . . . ? Ni3 N3 C10 C9 -1.0(11) . . . . ? C1 C9 C10 N4 175.9(8) . . . . ? C1 C9 C10 N3 1.1(13) . . . . ? C10 N3 C11 C12 -176.2(11) . . . . ? Ni3 N3 C11 C12 0.2(15) . . . . ? C10 N3 C11 C16 -0.5(10) . . . . ? Ni3 N3 C11 C16 175.9(6) . . . . ? N3 C11 C12 C13 -179.7(11) . . . . ? C16 C11 C12 C13 5.0(17) . . . . ? C11 C12 C13 C14 -5(2) . . . . ? C12 C13 C14 C15 4(3) . . . . ? C13 C14 C15 C16 -2(2) . . . . ? C10 N4 C16 C15 179.9(13) . . . . ? C10 N4 C16 C11 -0.2(11) . . . . ? C14 C15 C16 N4 -178.1(13) . . . . ? C14 C15 C16 C11 2(2) . . . . ? C12 C11 C16 N4 176.5(10) . . . . ? N3 C11 C16 N4 0.4(11) . . . . ? C12 C11 C16 C15 -3.6(17) . . . . ? N3 C11 C16 C15 -179.7(11) . . . . ? Ni4 O2 C17 C25 -15.5(9) . . . . ? Ni1 O2 C17 C25 -179.8(6) . . . . ? Ni4 O2 C17 C18 171.8(4) . . . . ? Ni1 O2 C17 C18 7.6(6) . . . . ? C19 N5 C18 N6 -0.5(7) . . . . ? Ni1 N5 C18 N6 177.3(4) . . . . ? C19 N5 C18 C17 178.6(5) . . . . ? Ni1 N5 C18 C17 -3.5(7) . . . . ? C24 N6 C18 N5 0.3(7) . . . . ? C24 N6 C18 C17 -178.8(6) . . . . ? O2 C17 C18 N5 -3.0(8) . . . . ? C25 C17 C18 N5 -176.1(6) . . . . ? O2 C17 C18 N6 176.0(6) . . . . ? C25 C17 C18 N6 2.9(10) . . . . ? C18 N5 C19 C20 178.4(7) . . . . ? Ni1 N5 C19 C20 1.4(11) . . . . ? C18 N5 C19 C24 0.6(7) . . . . ? Ni1 N5 C19 C24 -176.4(5) . . . . ? N5 C19 C20 C21 -179.9(7) . . . . ? C24 C19 C20 C21 -2.2(10) . . . . ? C19 C20 C21 C22 1.4(11) . . . . ? C20 C21 C22 C23 -0.4(12) . . . . ? C21 C22 C23 C24 0.3(11) . . . . ? C18 N6 C24 C23 179.1(7) . . . . ? C18 N6 C24 C19 0.1(7) . . . . ? C22 C23 C24 N6 179.9(7) . . . . ? C22 C23 C24 C19 -1.2(10) . . . . ? C20 C19 C24 N6 -178.6(6) . . . . ? N5 C19 C24 N6 -0.4(7) . . . . ? C20 C19 C24 C23 2.2(10) . . . . ? N5 C19 C24 C23 -179.6(6) . . . . ? O2 C17 C25 C26 7.3(13) . . . . ? C18 C17 C25 C26 179.4(7) . . . . ? C32 N8 C26 N7 3.1(12) . . . . ? C32 N8 C26 C25 -179.0(10) . . . . ? C27 N7 C26 N8 -4.0(9) . . . . ? Ni4 N7 C26 N8 176.9(6) . . . . ? C27 N7 C26 C25 178.1(8) . . . . ? Ni4 N7 C26 C25 -1.1(12) . . . . ? C17 C25 C26 N8 -176.0(8) . . . . ? C17 C25 C26 N7 1.7(14) . . . . ? C26 N7 C27 C28 -178.5(9) . . . . ? Ni4 N7 C27 C28 0.6(12) . . . . ? C26 N7 C27 C32 3.4(10) . . . . ? Ni4 N7 C27 C32 -177.5(7) . . . . ? N7 C27 C28 C29 -178.7(9) . . . . ? C32 C27 C28 C29 -0.8(14) . . . . ? C27 C28 C29 C30 0.2(17) . . . . ? C28 C29 C30 C31 0(2) . . . . ? C29 C30 C31 C32 0(3) . . . . ? C26 N8 C32 C31 177.9(14) . . . . ? C26 N8 C32 C27 -0.9(13) . . . . ? C30 C31 C32 N8 -179.6(15) . . . . ? C30 C31 C32 C27 -1(2) . . . . ? N7 C27 C32 N8 -1.6(12) . . . . ? C28 C27 C32 N8 -179.9(9) . . . . ? N7 C27 C32 C31 179.5(12) . . . . ? C28 C27 C32 C31 1.2(17) . . . . ? Ni5 O3 C33 C41 -1.1(10) . . . . ? Ni1 O3 C33 C41 -168.7(6) . . . . ? Ni5 O3 C33 C34 179.8(4) . . . . ? Ni1 O3 C33 C34 12.2(7) . . . . ? C35 N9 C34 N10 -0.3(7) . . . . ? Ni1 N9 C34 N10 -173.2(4) . . . . ? C35 N9 C34 C33 179.6(6) . . . . ? Ni1 N9 C34 C33 6.8(7) . . . . ? C40 N10 C34 N9 0.9(7) . . . . ? C40 N10 C34 C33 -179.1(6) . . . . ? O3 C33 C34 N9 -13.1(9) . . . . ? C41 C33 C34 N9 167.7(7) . . . . ? O3 C33 C34 N10 166.9(6) . . . . ? C41 C33 C34 N10 -12.3(11) . . . . ? C34 N9 C35 C40 -0.3(7) . . . . ? Ni1 N9 C35 C40 169.1(5) . . . . ? C34 N9 C35 C36 178.3(7) . . . . ? Ni1 N9 C35 C36 -12.2(12) . . . . ? C40 C35 C36 C37 -3.5(10) . . . . ? N9 C35 C36 C37 178.0(7) . . . . ? C35 C36 C37 C38 1.0(12) . . . . ? C36 C37 C38 C39 1.9(14) . . . . ? C37 C38 C39 C40 -2.1(12) . . . . ? C34 N10 C40 C35 -1.0(7) . . . . ? C34 N10 C40 C39 177.6(7) . . . . ? N9 C35 C40 N10 0.9(8) . . . . ? C36 C35 C40 N10 -177.9(6) . . . . ? N9 C35 C40 C39 -177.8(6) . . . . ? C36 C35 C40 C39 3.4(11) . . . . ? C38 C39 C40 N10 -178.9(7) . . . . ? C38 C39 C40 C35 -0.5(11) . . . . ? O3 C33 C41 C42 3.4(12) . . . . ? C34 C33 C41 C42 -177.5(7) . . . . ? C43 N11 C42 N12 -1.8(9) . . . . ? Ni5 N11 C42 N12 -173.2(5) . . . . ? C43 N11 C42 C41 175.6(7) . . . . ? Ni5 N11 C42 C41 4.2(11) . . . . ? C48 N12 C42 N11 1.4(10) . . . . ? C48 N12 C42 C41 -176.0(8) . . . . ? C33 C41 C42 N11 -5.2(13) . . . . ? C33 C41 C42 N12 171.9(8) . . . . ? C42 N11 C43 C48 1.5(9) . . . . ? Ni5 N11 C43 C48 172.3(6) . . . . ? C42 N11 C43 C44 -175.6(9) . . . . ? Ni5 N11 C43 C44 -4.8(13) . . . . ? N11 C43 C44 C45 176.1(8) . . . . ? C48 C43 C44 C45 -0.6(13) . . . . ? C43 C44 C45 C46 3.7(15) . . . . ? C44 C45 C46 C47 -5.7(19) . . . . ? C45 C46 C47 C48 4.2(18) . . . . ? C42 N12 C48 C43 -0.4(10) . . . . ? C42 N12 C48 C47 176.6(11) . . . . ? N11 C43 C48 N12 -0.7(10) . . . . ? C44 C43 C48 N12 176.7(8) . . . . ? N11 C43 C48 C47 -178.0(9) . . . . ? C44 C43 C48 C47 -0.6(14) . . . . ? C46 C47 C48 N12 -177.7(11) . . . . ? C46 C47 C48 C43 -1.1(16) . . . . ? Ni3 O4 C49 C57 -9.9(11) . . . . ? Ni2 O4 C49 C57 -174.0(7) . . . . ? Ni3 O4 C49 C50 170.4(4) . . . . ? Ni2 O4 C49 C50 6.2(7) . . . . ? C51 N13 C50 N14 -1.3(9) . . . . ? Ni2 N13 C50 N14 166.6(5) . . . . ? C51 N13 C50 C49 -178.8(6) . . . . ? Ni2 N13 C50 C49 -10.9(9) . . . . ? C56 N14 C50 N13 0.1(10) . . . . ? C56 N14 C50 C49 177.3(7) . . . . ? O4 C49 C50 N13 3.0(10) . . . . ? C57 C49 C50 N13 -176.8(8) . . . . ? O4 C49 C50 N14 -174.1(7) . . . . ? C57 C49 C50 N14 6.2(13) . . . . ? C50 N13 C51 C56 2.0(8) . . . . ? Ni2 N13 C51 C56 -160.8(7) . . . . ? C50 N13 C51 C52 179.2(8) . . . . ? Ni2 N13 C51 C52 16.3(13) . . . . ? C56 C51 C52 C53 -0.4(12) . . . . ? N13 C51 C52 C53 -177.1(7) . . . . ? C51 C52 C53 C54 1.7(12) . . . . ? C52 C53 C54 C55 -3.5(15) . . . . ? C53 C54 C55 C56 3.8(15) . . . . ? C50 N14 C56 C51 1.2(9) . . . . ? C50 N14 C56 C55 -178.8(9) . . . . ? N13 C51 C56 N14 -2.0(9) . . . . ? C52 C51 C56 N14 -179.3(7) . . . . ? N13 C51 C56 C55 178.0(7) . . . . ? C52 C51 C56 C55 0.7(13) . . . . ? C54 C55 C56 N14 177.7(9) . . . . ? C54 C55 C56 C51 -2.3(13) . . . . ? O4 C49 C57 C58 0.4(14) . . . . ? C50 C49 C57 C58 -179.8(7) . . . . ? C59 N15 C58 N16 -3.5(9) . . . . ? Ni3 N15 C58 N16 178.2(5) . . . . ? C59 N15 C58 C57 177.2(7) . . . . ? Ni3 N15 C58 C57 -1.1(11) . . . . ? C64 N16 C58 N15 3.5(10) . . . . ? C64 N16 C58 C57 -177.2(8) . . . . ? C49 C57 C58 N15 5.5(13) . . . . ? C49 C57 C58 N16 -173.8(8) . . . . ? C58 N15 C59 C60 -178.3(8) . . . . ? Ni3 N15 C59 C60 0.0(11) . . . . ? C58 N15 C59 C64 2.2(8) . . . . ? Ni3 N15 C59 C64 -179.5(5) . . . . ? N15 C59 C60 C61 -179.0(7) . . . . ? C64 C59 C60 C61 0.5(11) . . . . ? C59 C60 C61 C62 1.4(12) . . . . ? C60 C61 C62 C63 -0.6(14) . . . . ? C61 C62 C63 C64 -2.1(16) . . . . ? C58 N16 C64 C59 -1.9(10) . . . . ? C58 N16 C64 C63 -177.7(11) . . . . ? C60 C59 C64 N16 -179.8(7) . . . . ? N15 C59 C64 N16 -0.2(9) . . . . ? C60 C59 C64 C63 -3.3(13) . . . . ? N15 C59 C64 C63 176.3(9) . . . . ? C62 C63 C64 N16 179.4(10) . . . . ? C62 C63 C64 C59 4.1(16) . . . . ? Ni4 O5 C65 C73 -5.9(11) . . . . ? Ni2 O5 C65 C73 -171.2(6) . . . . ? Ni4 O5 C65 C66 175.6(5) . . . . ? Ni2 O5 C65 C66 10.2(8) . . . . ? C67 N17 C66 N18 -1.2(9) . . . . ? Ni2 N17 C66 N18 179.6(5) . . . . ? C67 N17 C66 C65 177.0(7) . . . . ? Ni2 N17 C66 C65 -2.2(9) . . . . ? C72 N18 C66 N17 1.9(9) . . . . ? C72 N18 C66 C65 -176.1(7) . . . . ? O5 C65 C66 N17 -5.7(10) . . . . ? C73 C65 C66 N17 175.7(7) . . . . ? O5 C65 C66 N18 172.2(7) . . . . ? C73 C65 C66 N18 -6.4(13) . . . . ? C66 N17 C67 C72 -0.1(9) . . . . ? Ni2 N17 C67 C72 178.7(6) . . . . ? C66 N17 C67 C68 -178.6(8) . . . . ? Ni2 N17 C67 C68 0.2(14) . . . . ? N17 C67 C68 C69 -179.3(8) . . . . ? C72 C67 C68 C69 2.4(12) . . . . ? C67 C68 C69 C70 -3.2(15) . . . . ? C68 C69 C70 C71 2.4(18) . . . . ? C69 C70 C71 C72 -0.4(15) . . . . ? C70 C71 C72 C67 -0.4(14) . . . . ? C70 C71 C72 N18 179.0(9) . . . . ? N17 C67 C72 C71 -179.3(8) . . . . ? C68 C67 C72 C71 -0.6(13) . . . . ? N17 C67 C72 N18 1.2(9) . . . . ? C68 C67 C72 N18 179.8(7) . . . . ? C66 N18 C72 C71 178.7(9) . . . . ? C66 N18 C72 C67 -1.8(9) . . . . ? O5 C65 C73 C74 3.8(13) . . . . ? C66 C65 C73 C74 -177.8(7) . . . . ? C80 N20 C74 N19 3.5(9) . . . . ? C80 N20 C74 C73 -173.6(8) . . . . ? C75 N19 C74 N20 -3.2(9) . . . . ? Ni4 N19 C74 N20 -180.0(5) . . . . ? C75 N19 C74 C73 173.8(7) . . . . ? Ni4 N19 C74 C73 -3.0(11) . . . . ? C65 C73 C74 N20 177.7(8) . . . . ? C65 C73 C74 N19 1.1(13) . . . . ? C74 N19 C75 C80 1.7(9) . . . . ? Ni4 N19 C75 C80 178.3(6) . . . . ? C74 N19 C75 C76 -177.4(8) . . . . ? Ni4 N19 C75 C76 -0.8(12) . . . . ? C80 C75 C76 C77 -0.8(12) . . . . ? N19 C75 C76 C77 178.3(8) . . . . ? C75 C76 C77 C78 4.5(15) . . . . ? C76 C77 C78 C79 -5.2(18) . . . . ? C77 C78 C79 C80 1.8(16) . . . . ? C74 N20 C80 C75 -2.2(9) . . . . ? C74 N20 C80 C79 179.8(10) . . . . ? N19 C75 C80 N20 0.2(9) . . . . ? C76 C75 C80 N20 179.4(7) . . . . ? N19 C75 C80 C79 178.4(8) . . . . ? C76 C75 C80 C79 -2.4(13) . . . . ? C78 C79 C80 N20 179.5(10) . . . . ? C78 C79 C80 C75 1.9(15) . . . . ? Ni5 O6 C81 C89 -11.7(13) . . . . ? Ni2 O6 C81 C89 -172.2(8) . . . . ? Ni5 O6 C81 C82 170.1(6) . . . . ? Ni2 O6 C81 C82 9.6(9) . . . . ? C83 N21 C82 N22 -1.6(11) . . . . ? Ni2 N21 C82 N22 177.2(6) . . . . ? C83 N21 C82 C81 176.4(8) . . . . ? Ni2 N21 C82 C81 -4.8(11) . . . . ? C88 N22 C82 N21 2.1(12) . . . . ? C88 N22 C82 C81 -175.8(10) . . . . ? C89 C81 C82 N21 178.4(9) . . . . ? O6 C81 C82 N21 -3.3(12) . . . . ? C89 C81 C82 N22 -4.0(16) . . . . ? O6 C81 C82 N22 174.3(9) . . . . ? C82 N21 C83 C84 179.3(11) . . . . ? Ni2 N21 C83 C84 1.1(19) . . . . ? C82 N21 C83 C88 0.6(12) . . . . ? Ni2 N21 C83 C88 -177.7(9) . . . . ? C88 C83 C84 C85 -4.0(17) . . . . ? N21 C83 C84 C85 177.5(11) . . . . ? C83 C84 C85 C86 3.7(17) . . . . ? C84 C85 C86 C87 -3(2) . . . . ? C85 C86 C87 C88 3(2) . . . . ? C82 N22 C88 C87 175.8(14) . . . . ? C82 N22 C88 C83 -1.6(13) . . . . ? C86 C87 C88 N22 179.4(14) . . . . ? C86 C87 C88 C83 -3(2) . . . . ? C84 C83 C88 N22 -178.2(11) . . . . ? N21 C83 C88 N22 0.7(13) . . . . ? C84 C83 C88 C87 4.0(19) . . . . ? N21 C83 C88 C87 -177.1(11) . . . . ? O6 C81 C89 C90 2.7(17) . . . . ? C82 C81 C89 C90 -179.3(9) . . . . ? C96 N24 C90 N23 0.7(12) . . . . ? C96 N24 C90 C89 -177.9(9) . . . . ? C91 N23 C90 N24 -1.6(10) . . . . ? Ni5 N23 C90 N24 -177.3(6) . . . . ? C91 N23 C90 C89 177.0(9) . . . . ? Ni5 N23 C90 C89 1.3(13) . . . . ? C81 C89 C90 N24 -178.6(10) . . . . ? C81 C89 C90 N23 3.0(16) . . . . ? C90 N23 C91 C96 1.9(9) . . . . ? Ni5 N23 C91 C96 177.3(6) . . . . ? C90 N23 C91 C92 -177.1(9) . . . . ? Ni5 N23 C91 C92 -1.6(13) . . . . ? C96 C91 C92 C93 0.9(13) . . . . ? N23 C91 C92 C93 179.8(8) . . . . ? C91 C92 C93 C94 -1.1(14) . . . . ? C92 C93 C94 C95 1.1(17) . . . . ? C93 C94 C95 C96 -0.8(17) . . . . ? C94 C95 C96 C91 0.6(16) . . . . ? C94 C95 C96 N24 -177.2(11) . . . . ? N23 C91 C96 C95 -179.8(9) . . . . ? C92 C91 C96 C95 -0.7(15) . . . . ? N23 C91 C96 N24 -1.5(10) . . . . ? C92 C91 C96 N24 177.6(8) . . . . ? C90 N24 C96 C95 178.6(11) . . . . ? C90 N24 C96 C91 0.5(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O13 H13A O14C 0.92 2.32 3.08(3) 140.1 2_655 y O13 H13B O10 0.88 2.13 2.88(2) 142.0 . y O12 H12B O13 0.72 2.53 3.13(2) 143.5 . y O12 H12A O11A 0.87 2.36 3.090(15) 141.5 . y O11A H11A O14B 0.80 2.08 2.87(2) 168.5 4_566 y O10 H10A O7 0.74 2.59 3.317(12) 168.3 . y O10 H10A O8 0.74 2.46 3.046(11) 137.1 . y N22 H22 O14A 0.88 2.17 3.04(2) 174.7 . y N20 H20 O13 0.88 2.13 2.950(16) 155.5 . y N18 H18 O10 0.88 2.08 2.939(11) 164.5 . y N16 H16 O14C 0.88 1.96 2.835(17) 169.6 1_655 y N14 H14 O14B 0.88 1.98 2.847(19) 167.4 . y N12 H12 O12 0.88 2.04 2.883(13) 160.9 . y N10 H10 O11A 0.88 1.93 2.807(10) 173.4 . y N8 H8 O14A 0.88 2.23 2.95(2) 139.6 1_655 y N6 H6 O8 0.88 2.00 2.874(8) 172.0 2_745 y N4 H4 O10 0.88 2.02 2.900(9) 174.8 2_645 y N2 H2 O7 0.88 2.00 2.871(8) 171.9 2_645 y _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.942 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.097 # SQUEEZE RESULTS 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 0.000 0.000 0.000 273 33 ' ' 2 0.489 0.116 0.577 26 4 ' ' 3 0.799 0.140 0.698 15 2 ' ' 4 0.467 0.241 0.494 58 8 ' ' 5 0.467 0.261 -0.004 59 8 ' ' 6 0.799 0.360 0.198 15 2 ' ' 7 0.490 0.388 0.079 25 3 ' ' 8 0.000 0.500 0.500 273 32 ' ' 9 0.511 0.616 0.923 26 3 ' ' 10 0.201 0.640 0.802 15 3 ' ' 11 0.533 0.741 1.006 59 8 ' ' 12 0.533 0.761 0.504 60 8 ' ' 13 0.201 0.859 0.302 15 2 ' ' 14 0.510 0.888 0.421 25 3 ' ' _platon_squeeze_details ; The crystal structure contains voids (950.6 A3/per unit cell, i.e. some 9.84% of the unit cell volume) filled with a disordered solvent molecule (water). Attempts to refine peaks of residual electron density as solvent O atom (water) and NO3 anion were unsuccessful. Derived values (formula weight, density, absorption coefficient) do not contain the contribution of the disordered solvent molecule. R factors before data are squeezed: _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2694 _refine_ls_wR_factor_gt 0.2294 ; # start Validation Reply Form _vrf_PLAT420_fwno3b-s ; PROBLEM: D-H Without Acceptor >O11A - >H11A ... ?, O13 - H13A ... ?, N8 - H8 ... ?, N14 - H14 ... ?, N16 - H16 ... ?, N22 - H22 ... ?, N24 - H24 ... ? RESPONSE: The possible acceptors are solvent molecules (water). They are disordered and squeezed by PLATON without refinment. ; _vrf_PLAT241_fwno3b-s ; PROBLEM: Check High Ueq as Compared to Neighbors for N8, N24, C13, C15, C31, C63, C69, C86, C94 RESPONSE: these atoms are also disordered. ; _vrf_PLAT234_fwno3b-s ; PROBLEM: Large Hirshfeld Difference N8 -- C32 Large Hirshfeld Difference N21 -- C82 Large Hirshfeld Difference C15 -- C16 Large Hirshfeld Difference C45 -- C46 Large Hirshfeld Difference C46 -- C47 Large Hirshfeld Difference C60 -- C61 Large Hirshfeld Difference C67 -- C68 Large Hirshfeld Difference C68 -- C69 Large Hirshfeld Difference C69 -- C70 Large Hirshfeld Difference C73 -- C74 Large Hirshfeld Difference C75 -- C80 Large Hirshfeld Difference C81 -- C82 Large Hirshfeld Difference C86 -- C87 Large Hirshfeld Difference C89 -- C90 Large Hirshfeld Difference C93 -- C94 Large Hirshfeld Difference C94 -- C95 RESPONSE: these atoms are also disordered. ; # end Validation Reply Form # Attachment '6_CCDC676417.cif' data_fwbr-14 _database_code_depnum_ccdc_archive 'CCDC 676417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H66 N24 Ni5 O6, Br0.70, Br0.60, Br0.45, 2.25Br' _chemical_formula_sum 'C96 H66 Br4 N24 Ni5 O6' _chemical_formula_weight 2264.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 13.146(4) _cell_length_b 26.711(9) _cell_length_c 29.026(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.353(13) _cell_angle_gamma 90.00 _cell_volume 9829(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16459 _cell_measurement_theta_min 2.0760 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4552 _exptl_absorpt_coefficient_mu 2.632 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6485 _exptl_absorpt_correction_T_max 0.7093 _exptl_absorpt_process_details ; (HIGASHI, T. (1995). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60407 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17074 _reflns_number_gt 11736 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material ; SHELXTL/PC Mercury Ver. 1.3 (Bruno et al., 2002) ; _refine_special_details ; Structure was phased by direct methods. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. There were partial occupancies for all four Br anions. The occupancies of these sites were freely refined with PART and SUMP instruction firstly until convergence, and then fixed at final refine with partial occupancies for Br1 0.75, Br2 0.70, Br3 0.50, Br4 0.40, Br5 0.20, Br6 0.20, Br7 0.45, Br8 0.23, Br9 0.22, Br10 0.20, Br11 0.15. Diffaction data were well observed at high resolution but fit poorly at low resolution suggesting limitations in the proposed disorder model. All efforts to identify a super-lattice or refine an ordered model in all possible non-isomorphic sub-groups failed to eliminate the ambiguities in the ligand and anions. The residual electron density had a maximum located 1.32 A from atom Br1. Non H-atoms were refined anisotropically. H-atoms were included in calculated positions and treated as riding atoms using the SHELXL default parameters. ISOR instruction was employed to have ellipsoids of sites (All partially occupied Br anions) be restraint to more appropriate values. So, 66 restraints were used for refinement anisotropically. ; _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^)+(0.1225P)^2^+22.1431P] 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 17074 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2011 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _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 Ni1 Ni 0.16800(6) 0.41128(3) 0.14643(3) 0.0381(2) Uani 1 1 d . . . Ni2 Ni 0.35218(7) 0.30966(3) 0.31339(3) 0.0485(2) Uani 1 1 d . . . Ni3 Ni 0.27474(7) 0.42947(3) 0.27013(3) 0.0455(2) Uani 1 1 d . . . Ni4 Ni 0.38178(7) 0.32975(3) 0.19965(3) 0.0475(2) Uani 1 1 d . . . Ni5 Ni 0.11225(7) 0.32051(3) 0.22355(3) 0.0497(2) Uani 1 1 d . . . O1 O 0.2890(3) 0.43836(15) 0.20561(14) 0.0422(9) Uani 1 1 d . . . O2 O 0.2439(3) 0.33954(15) 0.15433(14) 0.0428(10) Uani 1 1 d . . . O3 O 0.0891(3) 0.38841(16) 0.19799(14) 0.0446(10) Uani 1 1 d . . . O4 O 0.2505(4) 0.37259(17) 0.30748(16) 0.0505(11) Uani 1 1 d . . . O5 O 0.4285(3) 0.34636(18) 0.26722(15) 0.0507(11) Uani 1 1 d . . . O6 O 0.2396(4) 0.28245(16) 0.25087(15) 0.0484(10) Uani 1 1 d . . . N1 N 0.2683(4) 0.44338(18) 0.11317(17) 0.0381(11) Uani 1 1 d . . . N2 N 0.4078(4) 0.4927(2) 0.11773(17) 0.0420(12) Uani 1 1 d . . . H2 H 0.4634 0.5114 0.1303 0.050 Uiso 1 1 calc R . . N3 N 0.4002(4) 0.4695(2) 0.29933(18) 0.0496(13) Uani 1 1 d . . . N4 N 0.5346(5) 0.5213(2) 0.30468(19) 0.0603(16) Uani 1 1 d . . . H4 H 0.5822 0.5395 0.2961 0.072 Uiso 1 1 calc R . . N5 N 0.0693(4) 0.37169(18) 0.09275(17) 0.0397(11) Uani 1 1 d . . . N6 N 0.0263(4) 0.2976(2) 0.05660(18) 0.0463(12) Uani 1 1 d . . . H6 H 0.0311 0.2659 0.0492 0.056 Uiso 1 1 calc R . . N7 N 0.4075(4) 0.2647(2) 0.1748(2) 0.0541(14) Uani 1 1 d . . . N8 N 0.3841(6) 0.2006(3) 0.1237(2) 0.075(2) Uani 1 1 d . . . H8 H 0.3538 0.1802 0.1003 0.089 Uiso 1 1 calc R . . N9 N 0.0733(4) 0.47163(18) 0.14682(18) 0.0419(11) Uani 1 1 d . . . N10 N -0.0590(4) 0.50430(19) 0.17200(19) 0.0465(12) Uani 1 1 d . . . H10 H -0.1081 0.5072 0.1874 0.056 Uiso 1 1 calc R . . N11 N 0.0094(5) 0.3280(2) 0.2608(2) 0.0544(14) Uani 1 1 d . . . N12 N -0.1149(6) 0.3619(3) 0.2896(3) 0.081(2) Uani 1 1 d . . . H12 H -0.1610 0.3834 0.2951 0.097 Uiso 1 1 calc R . . N13 N 0.2669(4) 0.2902(2) 0.35984(18) 0.0507(14) Uani 1 1 d . . . N14 N 0.1635(5) 0.3160(2) 0.4047(2) 0.0598(16) Uani 1 1 d . . . H14 H 0.1211 0.3352 0.4159 0.072 Uiso 1 1 calc R . . N15 N 0.1715(4) 0.4708(2) 0.28876(18) 0.0476(13) Uani 1 1 d . . . N16 N 0.0545(6) 0.4954(3) 0.3275(2) 0.0721(19) Uani 1 1 d . . . H16 H 0.0128 0.4947 0.3467 0.086 Uiso 1 1 calc R . . N17 N 0.4744(5) 0.3443(3) 0.36132(19) 0.0600(16) Uani 1 1 d . . . N18 N 0.6201(5) 0.3904(3) 0.3741(2) 0.077(2) Uani 1 1 d . . . H18 H 0.6721 0.4076 0.3680 0.092 Uiso 1 1 calc R . . N19 N 0.4963(4) 0.3668(2) 0.18453(19) 0.0507(13) Uani 1 1 d . . . N20 N 0.6418(5) 0.4137(2) 0.1945(2) 0.0620(16) Uani 1 1 d . . . H20 H 0.6976 0.4315 0.2086 0.074 Uiso 1 1 calc R . . N21 N 0.4163(4) 0.2426(2) 0.3043(2) 0.0538(14) Uani 1 1 d . . . N22 N 0.3998(5) 0.1697(2) 0.2641(2) 0.0653(17) Uani 1 1 d . . . H22 H 0.3721 0.1461 0.2434 0.078 Uiso 1 1 calc R . . N23 N 0.0430(5) 0.2674(2) 0.1806(2) 0.0513(13) Uani 1 1 d . . . N24 N 0.0204(6) 0.1918(2) 0.1473(2) 0.073(2) Uani 1 1 d . . . H24 H 0.0344 0.1612 0.1395 0.087 Uiso 1 1 calc R . . C1 C 0.3626(5) 0.4671(2) 0.1940(2) 0.0415(14) Uani 1 1 d . . . C2 C 0.3470(5) 0.4687(2) 0.1414(2) 0.0408(14) Uani 1 1 d . . . C3 C 0.2774(5) 0.4517(2) 0.0668(2) 0.0398(13) Uani 1 1 d . . . C4 C 0.2154(5) 0.4348(2) 0.0223(2) 0.0461(15) Uani 1 1 d . . . H4A H 0.1539 0.4152 0.0194 0.055 Uiso 1 1 calc R . . C5 C 0.2495(6) 0.4486(3) -0.0171(2) 0.0530(17) Uani 1 1 d . . . H5 H 0.2109 0.4374 -0.0478 0.064 Uiso 1 1 calc R . . C6 C 0.3379(5) 0.4783(3) -0.0136(2) 0.0497(16) Uani 1 1 d . . . H6A H 0.3579 0.4861 -0.0419 0.060 Uiso 1 1 calc R . . C7 C 0.3980(6) 0.4968(3) 0.0295(2) 0.0508(16) Uani 1 1 d . . . H7 H 0.4572 0.5179 0.0317 0.061 Uiso 1 1 calc R . . C8 C 0.3657(5) 0.4824(2) 0.0699(2) 0.0434(14) Uani 1 1 d . . . C9 C 0.4402(5) 0.4923(2) 0.2237(2) 0.0467(15) Uani 1 1 d . . . H9 H 0.4874 0.5108 0.2104 0.056 Uiso 1 1 calc R . . C10 C 0.4571(6) 0.4932(3) 0.2753(2) 0.0503(16) Uani 1 1 d . . . C11 C 0.4399(6) 0.4829(3) 0.3471(2) 0.0541(17) Uani 1 1 d . . . C12 C 0.4044(7) 0.4713(3) 0.3878(3) 0.074(2) Uani 1 1 d . . . H12A H 0.3454 0.4501 0.3859 0.089 Uiso 1 1 calc R . . C13 C 0.4597(9) 0.4921(4) 0.4301(3) 0.094(3) Uani 1 1 d . . . H13 H 0.4396 0.4843 0.4584 0.113 Uiso 1 1 calc R . . C14 C 0.5445(9) 0.5246(5) 0.4331(3) 0.104(4) Uani 1 1 d . . . H14A H 0.5794 0.5388 0.4631 0.124 Uiso 1 1 calc R . . C15 C 0.5784(8) 0.5364(4) 0.3937(3) 0.089(3) Uani 1 1 d . . . H15 H 0.6370 0.5580 0.3960 0.107 Uiso 1 1 calc R . . C16 C 0.5239(6) 0.5158(3) 0.3503(2) 0.0624(19) Uani 1 1 d . . . C17 C 0.2006(5) 0.3066(2) 0.1192(2) 0.0459(15) Uani 1 1 d . . . C18 C 0.0993(5) 0.3245(2) 0.0896(2) 0.0426(14) Uani 1 1 d . . . C19 C -0.0291(5) 0.3758(2) 0.0598(2) 0.0429(14) Uani 1 1 d . . . C20 C -0.0947(5) 0.4178(3) 0.0468(2) 0.0472(15) Uani 1 1 d . . . H20A H -0.0753 0.4499 0.0604 0.057 Uiso 1 1 calc R . . C21 C -0.1899(6) 0.4095(3) 0.0126(3) 0.0577(18) Uani 1 1 d . . . H21 H -0.2371 0.4367 0.0028 0.069 Uiso 1 1 calc R . . C22 C -0.2188(6) 0.3616(3) -0.0079(3) 0.0592(18) Uani 1 1 d . . . H22A H -0.2853 0.3574 -0.0305 0.071 Uiso 1 1 calc R . . C23 C -0.1529(5) 0.3212(3) 0.0042(2) 0.0527(17) Uani 1 1 d . . . H23 H -0.1725 0.2891 -0.0094 0.063 Uiso 1 1 calc R . . C24 C -0.0552(5) 0.3292(2) 0.0373(2) 0.0463(15) Uani 1 1 d . . . C25 C 0.2405(6) 0.2625(3) 0.1103(2) 0.0535(17) Uani 1 1 d . . . H25 H 0.1994 0.2428 0.0848 0.064 Uiso 1 1 calc R . . C26 C 0.3416(6) 0.2426(3) 0.1366(2) 0.0579(18) Uani 1 1 d . . . C27 C 0.4996(6) 0.2356(3) 0.1860(3) 0.063(2) Uani 1 1 d . . . C28 C 0.5931(7) 0.2418(3) 0.2204(3) 0.071(2) Uani 1 1 d . . . H28 H 0.6034 0.2689 0.2424 0.086 Uiso 1 1 calc R . . C29 C 0.6732(8) 0.2063(4) 0.2217(3) 0.082(3) Uani 1 1 d . . . H29 H 0.7396 0.2099 0.2445 0.098 Uiso 1 1 calc R . . C30 C 0.6570(8) 0.1674(4) 0.1911(4) 0.094(3) Uani 1 1 d . . . H30 H 0.7125 0.1438 0.1940 0.113 Uiso 1 1 calc R . . C31 C 0.5649(9) 0.1595(4) 0.1559(4) 0.092(3) Uani 1 1 d . . . H31 H 0.5557 0.1321 0.1344 0.110 Uiso 1 1 calc R . . C32 C 0.4853(7) 0.1955(3) 0.1545(3) 0.073(2) Uani 1 1 d . . . C33 C 0.0117(5) 0.4192(2) 0.2030(2) 0.0420(14) Uani 1 1 d . . . C34 C 0.0063(5) 0.4652(2) 0.1738(2) 0.0441(14) Uani 1 1 d . . . C35 C 0.0484(5) 0.5182(2) 0.1250(2) 0.0442(14) Uani 1 1 d . . . C36 C 0.0904(5) 0.5443(2) 0.0931(2) 0.0486(15) Uani 1 1 d . . . H36 H 0.1455 0.5303 0.0816 0.058 Uiso 1 1 calc R . . C37 C 0.0510(6) 0.5907(3) 0.0783(3) 0.0569(18) Uani 1 1 d . . . H37 H 0.0790 0.6091 0.0565 0.068 Uiso 1 1 calc R . . C38 C -0.0315(6) 0.6117(3) 0.0954(3) 0.062(2) Uani 1 1 d . . . H38 H -0.0573 0.6440 0.0848 0.075 Uiso 1 1 calc R . . C39 C -0.0748(6) 0.5864(3) 0.1268(2) 0.0561(18) Uani 1 1 d . . . H39 H -0.1298 0.6006 0.1382 0.067 Uiso 1 1 calc R . . C40 C -0.0346(5) 0.5393(2) 0.1412(2) 0.0476(15) Uani 1 1 d . . . C41 C -0.0536(6) 0.4128(3) 0.2309(3) 0.0560(17) Uani 1 1 d . . . H41 H -0.1034 0.4384 0.2318 0.067 Uiso 1 1 calc R . . C42 C -0.0514(6) 0.3688(3) 0.2596(3) 0.0568(18) Uani 1 1 d . . . C43 C -0.0168(6) 0.2936(3) 0.2904(3) 0.0606(19) Uani 1 1 d . . . C44 C 0.0211(7) 0.2461(3) 0.3026(3) 0.072(2) Uani 1 1 d . . . H44 H 0.0724 0.2318 0.2888 0.087 Uiso 1 1 calc R . . C45 C -0.0174(10) 0.2196(5) 0.3353(4) 0.102(4) Uani 1 1 d . . . H45 H 0.0076 0.1866 0.3442 0.122 Uiso 1 1 calc R . . C46 C -0.0919(11) 0.2409(5) 0.3549(5) 0.126(5) Uani 1 1 d . . . H46 H -0.1160 0.2219 0.3776 0.151 Uiso 1 1 calc R . . C47 C -0.1343(9) 0.2886(5) 0.3435(4) 0.113(4) Uani 1 1 d . . . H47 H -0.1861 0.3025 0.3572 0.135 Uiso 1 1 calc R . . C48 C -0.0930(8) 0.3145(4) 0.3097(4) 0.083(3) Uani 1 1 d . . . C49 C 0.1945(6) 0.3729(3) 0.3404(2) 0.0512(16) Uani 1 1 d . . . C50 C 0.2060(6) 0.3268(3) 0.3680(2) 0.0513(16) Uani 1 1 d . . . C51 C 0.2645(5) 0.2528(3) 0.3926(2) 0.0504(16) Uani 1 1 d . . . C52 C 0.3134(6) 0.2064(3) 0.3993(2) 0.0583(18) Uani 1 1 d . . . H52 H 0.3556 0.1952 0.3793 0.070 Uiso 1 1 calc R . . C53 C 0.2977(6) 0.1768(3) 0.4366(3) 0.062(2) Uani 1 1 d . . . H53 H 0.3289 0.1445 0.4420 0.074 Uiso 1 1 calc R . . C54 C 0.2372(7) 0.1942(3) 0.4660(3) 0.073(2) Uani 1 1 d . . . H54 H 0.2310 0.1738 0.4919 0.088 Uiso 1 1 calc R . . C55 C 0.1845(8) 0.2406(3) 0.4590(3) 0.072(2) Uani 1 1 d . . . H55 H 0.1417 0.2517 0.4787 0.086 Uiso 1 1 calc R . . C56 C 0.1998(6) 0.2692(3) 0.4210(2) 0.0582(18) Uani 1 1 d . . . C57 C 0.1331(6) 0.4121(3) 0.3476(3) 0.0605(19) Uani 1 1 d . . . H57 H 0.0971 0.4082 0.3718 0.073 Uiso 1 1 calc R . . C58 C 0.1184(6) 0.4584(3) 0.3218(3) 0.0573(18) Uani 1 1 d . . . C59 C 0.1388(5) 0.5202(2) 0.2748(2) 0.0480(15) Uani 1 1 d . . . C60 C 0.1706(6) 0.5515(3) 0.2426(2) 0.0511(16) Uani 1 1 d . . . H60 H 0.2212 0.5411 0.2265 0.061 Uiso 1 1 calc R . . C61 C 0.1237(6) 0.5988(3) 0.2354(3) 0.0587(18) Uani 1 1 d . . . H61 H 0.1439 0.6217 0.2145 0.070 Uiso 1 1 calc R . . C62 C 0.0472(7) 0.6129(3) 0.2588(3) 0.074(2) Uani 1 1 d . . . H62 H 0.0151 0.6449 0.2525 0.088 Uiso 1 1 calc R . . C63 C 0.0178(8) 0.5819(3) 0.2901(4) 0.079(3) Uani 1 1 d . . . H63 H -0.0334 0.5919 0.3060 0.095 Uiso 1 1 calc R . . C64 C 0.0648(7) 0.5356(3) 0.2980(3) 0.068(2) Uani 1 1 d . . . C65 C 0.5201(6) 0.3688(3) 0.2889(3) 0.0552(17) Uani 1 1 d . . . C66 C 0.5396(6) 0.3679(3) 0.3411(3) 0.0597(18) Uani 1 1 d . . . C67 C 0.5140(6) 0.3526(3) 0.4116(2) 0.065(2) Uani 1 1 d . . . C68 C 0.4760(7) 0.3374(4) 0.4497(3) 0.082(3) Uani 1 1 d . . . H68 H 0.4149 0.3170 0.4446 0.098 Uiso 1 1 calc R . . C69 C 0.5293(9) 0.3527(4) 0.4950(3) 0.090(3) Uani 1 1 d . . . H69 H 0.5034 0.3441 0.5216 0.109 Uiso 1 1 calc R . . C70 C 0.6227(8) 0.3814(5) 0.5018(3) 0.093(3) Uani 1 1 d . . . H70 H 0.6586 0.3914 0.5334 0.112 Uiso 1 1 calc R . . C71 C 0.6635(8) 0.3954(5) 0.4653(4) 0.102(3) Uani 1 1 d . . . H71 H 0.7276 0.4137 0.4708 0.122 Uiso 1 1 calc R . . C72 C 0.6058(7) 0.3815(4) 0.4190(3) 0.076(2) Uani 1 1 d . . . C73 C 0.5886(6) 0.3902(3) 0.2670(3) 0.0587(18) Uani 1 1 d . . . H73 H 0.6501 0.4057 0.2866 0.070 Uiso 1 1 calc R . . C74 C 0.5742(6) 0.3909(3) 0.2166(3) 0.0550(17) Uani 1 1 d . . . C75 C 0.5167(5) 0.3743(3) 0.1400(3) 0.0539(17) Uani 1 1 d . . . C76 C 0.4626(6) 0.3573(3) 0.0950(3) 0.0583(18) Uani 1 1 d . . . H76 H 0.4007 0.3375 0.0907 0.070 Uiso 1 1 calc R . . C77 C 0.5012(7) 0.3698(3) 0.0566(3) 0.068(2) Uani 1 1 d . . . H77 H 0.4678 0.3572 0.0257 0.081 Uiso 1 1 calc R . . C78 C 0.5896(7) 0.4009(4) 0.0634(3) 0.074(2) Uani 1 1 d . . . H78 H 0.6126 0.4106 0.0363 0.089 Uiso 1 1 calc R . . C79 C 0.6450(7) 0.4183(3) 0.1081(3) 0.070(2) Uani 1 1 d . . . H79 H 0.7056 0.4389 0.1122 0.084 Uiso 1 1 calc R . . C80 C 0.6075(6) 0.4039(3) 0.1462(3) 0.0600(19) Uani 1 1 d . . . C81 C 0.2546(6) 0.2344(3) 0.2406(2) 0.0546(17) Uani 1 1 d . . . C82 C 0.3566(6) 0.2144(3) 0.2693(3) 0.0546(17) Uani 1 1 d . . . C83 C 0.5050(6) 0.2139(3) 0.3233(3) 0.061(2) Uani 1 1 d . . . C84 C 0.5954(6) 0.2242(4) 0.3614(3) 0.074(2) Uani 1 1 d . . . H84 H 0.6027 0.2546 0.3790 0.089 Uiso 1 1 calc R . . C85 C 0.6736(7) 0.1867(5) 0.3716(4) 0.094(3) Uani 1 1 d . . . H85 H 0.7360 0.1917 0.3966 0.113 Uiso 1 1 calc R . . C86 C 0.6604(8) 0.1421(5) 0.3453(5) 0.098(4) Uani 1 1 d . . . H86 H 0.7143 0.1175 0.3538 0.118 Uiso 1 1 calc R . . C87 C 0.5744(8) 0.1317(4) 0.3080(4) 0.089(3) Uani 1 1 d . . . H87 H 0.5688 0.1015 0.2903 0.107 Uiso 1 1 calc R . . C88 C 0.4954(6) 0.1684(3) 0.2975(3) 0.067(2) Uani 1 1 d . . . C89 C 0.1885(6) 0.2066(3) 0.2069(3) 0.0563(17) Uani 1 1 d . . . H89 H 0.2114 0.1740 0.2011 0.068 Uiso 1 1 calc R . . C90 C 0.0869(6) 0.2221(3) 0.1790(2) 0.0565(18) Uani 1 1 d . . . C91 C -0.0589(6) 0.2650(3) 0.1509(2) 0.0542(17) Uani 1 1 d . . . C92 C -0.1402(6) 0.3004(3) 0.1406(3) 0.0621(19) Uani 1 1 d . . . H92 H -0.1315 0.3328 0.1546 0.075 Uiso 1 1 calc R . . C93 C -0.2332(7) 0.2861(4) 0.1091(3) 0.079(3) Uani 1 1 d . . . H93 H -0.2897 0.3094 0.1014 0.095 Uiso 1 1 calc R . . C94 C -0.2483(8) 0.2393(4) 0.0882(4) 0.093(3) Uani 1 1 d . . . H94 H -0.3153 0.2312 0.0675 0.111 Uiso 1 1 calc R . . C95 C -0.1688(8) 0.2040(4) 0.0966(3) 0.089(3) Uani 1 1 d . . . H95 H -0.1780 0.1724 0.0810 0.107 Uiso 1 1 calc R . . C96 C -0.0739(7) 0.2175(3) 0.1294(3) 0.070(2) Uani 1 1 d . . . Br1 Br 0.61669(12) 0.56246(6) 0.13817(6) 0.0918(4) Uani 0.75 1 d PU . . Br2 Br 0.82712(13) 0.45164(8) 0.35758(7) 0.1134(6) Uani 0.70 1 d PU . . Br3 Br 0.24759(18) 0.36429(8) 0.53355(7) 0.0904(6) Uani 0.50 1 d PU . . Br4 Br 0.2625(2) 0.08015(9) 0.19542(12) 0.0959(8) Uani 0.40 1 d PU . . Br5 Br 0.2005(9) 0.4479(4) 0.4757(4) 0.176(4) Uani 0.20 1 d PU . . Br6 Br 0.1401(9) 0.1024(4) 0.1216(4) 0.163(3) Uani 0.20 1 d PU . . Br7 Br 0.7578(2) 0.51807(14) 0.21892(14) 0.1345(12) Uani 0.45 1 d PU . . Br8 Br 0.9859(6) 0.1862(2) 0.0168(2) 0.0890(17) Uani 0.23 1 d PU . . Br9 Br 1.0324(8) 0.1946(5) 0.0297(4) 0.146(4) Uani 0.22 1 d PU . . Br10 Br 0.9875(7) 0.3763(3) 0.4360(3) 0.132(2) Uani 0.20 1 d PU . . Br11 Br 0.0788(8) 0.5601(5) 0.4385(3) 0.136(3) Uani 0.15 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0447(4) 0.0365(4) 0.0322(4) 0.0016(3) 0.0085(3) -0.0019(3) Ni2 0.0533(5) 0.0536(5) 0.0348(4) 0.0076(3) 0.0052(3) -0.0055(4) Ni3 0.0554(5) 0.0468(5) 0.0353(4) 0.0007(3) 0.0139(3) -0.0083(4) Ni4 0.0498(5) 0.0499(5) 0.0393(4) 0.0043(4) 0.0058(4) 0.0004(4) Ni5 0.0556(5) 0.0407(5) 0.0486(5) 0.0035(4) 0.0064(4) -0.0011(4) O1 0.047(2) 0.043(2) 0.037(2) 0.0014(18) 0.0119(18) -0.0050(19) O2 0.048(2) 0.040(2) 0.038(2) -0.0005(18) 0.0063(18) 0.0002(18) O3 0.054(3) 0.040(2) 0.039(2) 0.0031(18) 0.0109(19) -0.0029(19) O4 0.058(3) 0.055(3) 0.042(2) 0.004(2) 0.020(2) -0.007(2) O5 0.048(3) 0.059(3) 0.041(2) 0.009(2) 0.0036(19) -0.009(2) O6 0.060(3) 0.038(2) 0.043(2) 0.0025(18) 0.006(2) 0.006(2) N1 0.042(3) 0.040(3) 0.033(2) 0.002(2) 0.011(2) 0.004(2) N2 0.041(3) 0.051(3) 0.034(3) 0.005(2) 0.010(2) -0.002(2) N3 0.060(3) 0.057(3) 0.031(3) 0.002(2) 0.012(2) -0.011(3) N4 0.077(4) 0.065(4) 0.035(3) -0.007(3) 0.010(3) -0.028(3) N5 0.044(3) 0.037(3) 0.037(3) 0.002(2) 0.009(2) 0.002(2) N6 0.060(3) 0.037(3) 0.038(3) -0.001(2) 0.006(2) -0.002(2) N7 0.057(3) 0.053(3) 0.049(3) 0.011(3) 0.008(3) 0.009(3) N8 0.098(5) 0.058(4) 0.059(4) -0.001(3) 0.005(4) 0.032(4) N9 0.046(3) 0.036(3) 0.042(3) 0.004(2) 0.008(2) -0.004(2) N10 0.051(3) 0.040(3) 0.049(3) -0.001(2) 0.015(2) 0.004(2) N11 0.058(3) 0.054(3) 0.048(3) 0.007(3) 0.008(3) -0.012(3) N12 0.067(4) 0.107(6) 0.081(5) 0.020(4) 0.041(4) 0.000(4) N13 0.058(3) 0.053(3) 0.038(3) 0.006(2) 0.006(2) -0.021(3) N14 0.081(4) 0.057(4) 0.048(3) 0.004(3) 0.028(3) -0.013(3) N15 0.057(3) 0.044(3) 0.040(3) -0.002(2) 0.012(2) -0.009(2) N16 0.099(5) 0.064(4) 0.068(4) 0.003(3) 0.047(4) 0.010(4) N17 0.062(4) 0.077(4) 0.033(3) 0.011(3) -0.001(3) -0.010(3) N18 0.065(4) 0.098(5) 0.058(4) -0.001(4) -0.001(3) -0.023(4) N19 0.050(3) 0.059(3) 0.043(3) 0.006(3) 0.013(2) 0.007(3) N20 0.051(3) 0.070(4) 0.068(4) 0.008(3) 0.021(3) -0.004(3) N21 0.052(3) 0.060(4) 0.046(3) 0.013(3) 0.008(3) 0.002(3) N22 0.066(4) 0.057(4) 0.070(4) 0.011(3) 0.012(3) 0.010(3) N23 0.065(4) 0.042(3) 0.045(3) 0.005(2) 0.011(3) -0.001(3) N24 0.094(5) 0.040(3) 0.071(4) -0.005(3) -0.001(4) -0.014(3) C1 0.048(3) 0.048(4) 0.027(3) 0.003(2) 0.007(2) 0.001(3) C2 0.045(3) 0.043(3) 0.032(3) -0.002(2) 0.007(3) 0.006(3) C3 0.043(3) 0.043(3) 0.035(3) 0.001(2) 0.012(2) 0.006(3) C4 0.051(4) 0.048(4) 0.037(3) -0.003(3) 0.007(3) 0.004(3) C5 0.068(5) 0.059(4) 0.031(3) -0.001(3) 0.013(3) 0.004(4) C6 0.055(4) 0.062(4) 0.033(3) 0.007(3) 0.013(3) 0.009(3) C7 0.054(4) 0.064(4) 0.038(3) 0.005(3) 0.018(3) 0.007(3) C8 0.048(4) 0.049(4) 0.034(3) 0.002(3) 0.013(3) 0.006(3) C9 0.057(4) 0.049(4) 0.035(3) 0.002(3) 0.015(3) -0.013(3) C10 0.062(4) 0.050(4) 0.035(3) 0.001(3) 0.006(3) -0.017(3) C11 0.065(4) 0.063(4) 0.033(3) -0.004(3) 0.011(3) -0.020(4) C12 0.100(6) 0.084(6) 0.041(4) -0.006(4) 0.023(4) -0.030(5) C13 0.122(8) 0.122(8) 0.040(4) -0.012(5) 0.022(5) -0.050(7) C14 0.133(9) 0.139(9) 0.036(4) -0.017(5) 0.018(5) -0.065(8) C15 0.097(7) 0.117(8) 0.044(4) -0.013(5) 0.003(4) -0.050(6) C16 0.076(5) 0.069(5) 0.041(4) -0.005(3) 0.013(3) -0.021(4) C17 0.056(4) 0.041(3) 0.039(3) 0.003(3) 0.010(3) -0.001(3) C18 0.058(4) 0.034(3) 0.033(3) -0.003(2) 0.007(3) -0.005(3) C19 0.042(3) 0.052(4) 0.035(3) 0.003(3) 0.011(3) -0.002(3) C20 0.046(4) 0.053(4) 0.042(3) -0.004(3) 0.010(3) 0.004(3) C21 0.052(4) 0.066(5) 0.052(4) 0.000(3) 0.009(3) 0.010(3) C22 0.048(4) 0.072(5) 0.052(4) -0.004(4) 0.004(3) -0.004(4) C23 0.056(4) 0.053(4) 0.042(4) 0.002(3) 0.000(3) -0.011(3) C24 0.052(4) 0.047(4) 0.038(3) -0.001(3) 0.009(3) -0.009(3) C25 0.068(4) 0.043(4) 0.042(4) 0.004(3) 0.001(3) 0.005(3) C26 0.074(5) 0.053(4) 0.044(4) 0.008(3) 0.011(3) 0.010(4) C27 0.062(4) 0.066(5) 0.060(5) 0.027(4) 0.014(4) 0.021(4) C28 0.075(5) 0.077(6) 0.062(5) 0.023(4) 0.018(4) 0.014(4) C29 0.079(6) 0.089(7) 0.075(6) 0.025(5) 0.014(5) 0.034(5) C30 0.091(7) 0.101(8) 0.094(7) 0.030(6) 0.028(6) 0.053(6) C31 0.109(8) 0.084(7) 0.081(6) 0.022(5) 0.020(6) 0.047(6) C32 0.093(6) 0.062(5) 0.061(5) 0.007(4) 0.015(4) 0.036(4) C33 0.042(3) 0.040(3) 0.045(3) -0.003(3) 0.013(3) -0.001(3) C34 0.047(3) 0.041(3) 0.045(3) -0.005(3) 0.011(3) -0.004(3) C35 0.058(4) 0.031(3) 0.037(3) -0.001(2) 0.003(3) -0.005(3) C36 0.053(4) 0.036(3) 0.054(4) 0.002(3) 0.009(3) 0.000(3) C37 0.071(5) 0.045(4) 0.048(4) 0.010(3) 0.004(3) -0.003(3) C38 0.078(5) 0.035(4) 0.060(4) 0.003(3) -0.007(4) 0.002(3) C39 0.065(4) 0.049(4) 0.049(4) -0.003(3) 0.005(3) 0.014(3) C40 0.049(4) 0.038(3) 0.051(4) -0.011(3) 0.005(3) -0.005(3) C41 0.056(4) 0.052(4) 0.061(4) 0.004(3) 0.016(3) 0.001(3) C42 0.058(4) 0.062(5) 0.053(4) 0.010(3) 0.018(3) -0.010(4) C43 0.057(4) 0.063(5) 0.055(4) 0.013(4) 0.004(3) -0.021(4) C44 0.086(6) 0.065(5) 0.059(5) 0.014(4) 0.007(4) -0.023(4) C45 0.119(9) 0.095(8) 0.086(7) 0.036(6) 0.017(6) -0.031(7) C46 0.134(10) 0.130(11) 0.124(10) 0.070(9) 0.049(9) -0.016(9) C47 0.088(7) 0.151(11) 0.108(9) 0.056(8) 0.042(6) 0.004(7) C48 0.079(6) 0.092(7) 0.082(6) 0.033(5) 0.028(5) -0.017(5) C49 0.065(4) 0.044(4) 0.043(4) -0.002(3) 0.012(3) -0.015(3) C50 0.058(4) 0.054(4) 0.041(4) -0.002(3) 0.012(3) -0.011(3) C51 0.063(4) 0.052(4) 0.029(3) 0.007(3) 0.001(3) -0.013(3) C52 0.066(4) 0.059(4) 0.044(4) 0.010(3) 0.005(3) -0.007(4) C53 0.072(5) 0.061(5) 0.049(4) 0.009(3) 0.010(4) -0.019(4) C54 0.099(6) 0.065(5) 0.051(4) 0.013(4) 0.012(4) -0.037(5) C55 0.107(6) 0.059(5) 0.055(5) 0.007(4) 0.033(4) -0.016(5) C56 0.083(5) 0.049(4) 0.042(4) 0.002(3) 0.013(3) -0.015(4) C57 0.078(5) 0.063(5) 0.049(4) 0.003(3) 0.031(4) -0.006(4) C58 0.078(5) 0.052(4) 0.048(4) 0.002(3) 0.027(4) -0.004(4) C59 0.059(4) 0.043(4) 0.041(3) -0.003(3) 0.013(3) -0.005(3) C60 0.056(4) 0.049(4) 0.044(4) -0.003(3) 0.006(3) -0.011(3) C61 0.065(5) 0.051(4) 0.055(4) -0.001(3) 0.006(3) -0.010(3) C62 0.094(6) 0.057(5) 0.074(6) -0.003(4) 0.029(5) 0.006(4) C63 0.104(7) 0.062(5) 0.089(6) 0.002(5) 0.055(5) 0.013(5) C64 0.097(6) 0.055(5) 0.063(5) -0.012(4) 0.038(4) -0.002(4) C65 0.055(4) 0.056(4) 0.051(4) 0.009(3) 0.008(3) -0.004(3) C66 0.059(4) 0.065(5) 0.051(4) 0.004(3) 0.007(3) -0.008(4) C67 0.062(4) 0.088(6) 0.037(4) 0.006(4) 0.001(3) -0.016(4) C68 0.082(6) 0.103(7) 0.052(5) -0.001(5) 0.006(4) -0.014(5) C69 0.106(7) 0.107(8) 0.048(5) -0.006(5) 0.001(5) -0.009(6) C70 0.094(7) 0.133(9) 0.045(5) -0.007(5) 0.004(4) -0.014(6) C71 0.089(7) 0.137(10) 0.068(6) -0.022(6) -0.001(5) -0.035(7) C72 0.069(5) 0.104(7) 0.048(4) -0.007(4) 0.003(4) -0.019(5) C73 0.052(4) 0.066(5) 0.051(4) 0.004(3) 0.002(3) -0.003(3) C74 0.053(4) 0.051(4) 0.060(4) 0.007(3) 0.014(3) -0.002(3) C75 0.051(4) 0.051(4) 0.063(4) 0.011(3) 0.020(3) 0.010(3) C76 0.058(4) 0.068(5) 0.049(4) 0.016(3) 0.014(3) 0.016(4) C77 0.075(5) 0.076(5) 0.058(5) 0.009(4) 0.029(4) 0.026(4) C78 0.082(6) 0.085(6) 0.066(5) 0.021(4) 0.040(5) 0.015(5) C79 0.066(5) 0.077(5) 0.078(6) 0.013(4) 0.039(4) 0.000(4) C80 0.056(4) 0.062(5) 0.068(5) 0.015(4) 0.027(4) 0.013(4) C81 0.066(4) 0.052(4) 0.043(4) 0.007(3) 0.010(3) 0.004(3) C82 0.055(4) 0.055(4) 0.051(4) 0.017(3) 0.008(3) 0.005(3) C83 0.055(4) 0.071(5) 0.054(4) 0.029(4) 0.010(3) 0.004(4) C84 0.056(4) 0.091(6) 0.070(5) 0.035(5) 0.007(4) -0.001(4) C85 0.060(5) 0.123(10) 0.094(7) 0.055(7) 0.008(5) 0.007(6) C86 0.065(6) 0.106(9) 0.130(10) 0.065(8) 0.036(6) 0.021(6) C87 0.075(6) 0.068(6) 0.127(9) 0.034(6) 0.029(6) 0.020(5) C88 0.065(5) 0.058(5) 0.079(5) 0.031(4) 0.023(4) 0.007(4) C89 0.074(5) 0.042(4) 0.050(4) 0.003(3) 0.012(3) 0.005(3) C90 0.072(5) 0.042(4) 0.047(4) 0.007(3) 0.001(3) -0.003(3) C91 0.058(4) 0.052(4) 0.045(4) 0.009(3) 0.001(3) -0.011(3) C92 0.059(4) 0.066(5) 0.056(4) 0.007(4) 0.006(3) -0.006(4) C93 0.060(5) 0.093(7) 0.075(6) 0.023(5) 0.002(4) -0.006(5) C94 0.081(6) 0.094(7) 0.084(6) 0.007(6) -0.011(5) -0.037(6) C95 0.102(7) 0.067(6) 0.070(6) 0.004(4) -0.026(5) -0.033(5) C96 0.082(6) 0.057(5) 0.058(5) 0.007(4) -0.004(4) -0.011(4) Br1 0.0916(9) 0.0874(9) 0.0992(10) -0.0082(7) 0.0301(7) -0.0154(7) Br2 0.0787(9) 0.1600(17) 0.1124(13) -0.0333(11) 0.0448(9) -0.0377(10) Br3 0.1059(14) 0.0819(13) 0.0779(12) -0.0080(10) 0.0146(10) -0.0253(11) Br4 0.1048(18) 0.0679(14) 0.132(2) 0.0009(14) 0.0611(17) 0.0214(13) Br5 0.172(7) 0.184(7) 0.153(6) -0.004(6) 0.010(5) -0.032(6) Br6 0.193(7) 0.144(6) 0.167(7) -0.002(5) 0.076(6) 0.027(5) Br7 0.1034(19) 0.149(3) 0.171(3) -0.048(2) 0.071(2) -0.0309(18) Br8 0.113(4) 0.077(3) 0.089(4) -0.030(3) 0.047(3) -0.018(3) Br9 0.142(7) 0.142(7) 0.146(7) 0.001(5) 0.024(5) -0.005(5) Br10 0.182(6) 0.117(5) 0.103(4) 0.001(4) 0.049(4) 0.008(4) Br11 0.125(6) 0.192(8) 0.095(5) -0.027(5) 0.033(4) -0.040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.020(5) . y Ni1 N9 2.039(5) . y Ni1 N5 2.039(5) . y Ni1 O3 2.124(4) . y Ni1 O1 2.134(4) . y Ni1 O2 2.145(4) . y Ni2 N21 2.027(6) . y Ni2 N13 2.036(6) . y Ni2 N17 2.047(6) . y Ni2 O5 2.115(5) . y Ni2 O4 2.126(5) . y Ni2 O6 2.143(4) . y Ni3 N15 1.934(6) . y Ni3 O4 1.941(4) . y Ni3 O1 1.945(4) . y Ni3 N3 1.960(5) . y Ni4 O5 1.945(4) . y Ni4 N7 1.945(6) . y Ni4 N19 1.947(6) . y Ni4 O2 1.955(4) . y Ni5 O6 1.939(4) . y Ni5 N23 1.948(6) . y Ni5 N11 1.951(6) . y Ni5 O3 1.953(4) . y O1 C1 1.346(7) . ? O2 C17 1.352(7) . ? O3 C33 1.346(7) . ? O4 C49 1.352(8) . ? O5 C65 1.344(8) . ? O6 C81 1.344(8) . ? N1 C2 1.321(8) . ? N1 C3 1.402(7) . ? N2 C2 1.347(8) . ? N2 C8 1.380(8) . ? N2 H2 0.8800 . ? N3 C10 1.313(8) . ? N3 C11 1.394(8) . ? N4 C10 1.367(8) . ? N4 C16 1.376(9) . ? N4 H4 0.8800 . ? N5 C18 1.332(8) . ? N5 C19 1.394(8) . ? N6 C24 1.364(9) . ? N6 C18 1.366(8) . ? N6 H6 0.8800 . ? N7 C26 1.348(9) . ? N7 C27 1.402(9) . ? N8 C26 1.351(10) . ? N8 C32 1.398(11) . ? N8 H8 0.8800 . ? N9 C34 1.335(8) . ? N9 C35 1.394(8) . ? N10 C34 1.345(8) . ? N10 C40 1.388(9) . ? N10 H10 0.8800 . ? N11 C42 1.348(10) . ? N11 C43 1.362(9) . ? N12 C42 1.368(9) . ? N12 C48 1.392(12) . ? N12 H12 0.8800 . ? N13 C50 1.324(9) . ? N13 C51 1.384(8) . ? N14 C50 1.358(9) . ? N14 C56 1.377(10) . ? N14 H14 0.8800 . ? N15 C58 1.367(9) . ? N15 C59 1.414(9) . ? N16 C58 1.337(10) . ? N16 C64 1.401(10) . ? N16 H16 0.8800 . ? N17 C66 1.319(9) . ? N17 C67 1.429(9) . ? N18 C66 1.366(10) . ? N18 C72 1.386(11) . ? N18 H18 0.8800 . ? N19 C74 1.351(9) . ? N19 C75 1.402(9) . ? N20 C74 1.370(9) . ? N20 C80 1.378(10) . ? N20 H20 0.8800 . ? N21 C82 1.338(9) . ? N21 C83 1.383(9) . ? N22 C82 1.349(10) . ? N22 C88 1.369(10) . ? N22 H22 0.8800 . ? N23 C90 1.347(9) . ? N23 C91 1.388(9) . ? N24 C90 1.357(9) . ? N24 C96 1.392(11) . ? N24 H24 0.8800 . ? C1 C9 1.331(9) . ? C1 C2 1.488(8) . ? C3 C8 1.405(9) . ? C3 C4 1.406(9) . ? C4 C5 1.383(9) . ? C4 H4A 0.9500 . ? C5 C6 1.387(10) . ? C5 H5 0.9500 . ? C6 C7 1.382(9) . ? C6 H6A 0.9500 . ? C7 C8 1.401(9) . ? C7 H7 0.9500 . ? C9 C10 1.455(9) . ? C9 H9 0.9500 . ? C11 C16 1.396(10) . ? C11 C12 1.414(10) . ? C12 C13 1.367(11) . ? C12 H12A 0.9500 . ? C13 C14 1.398(13) . ? C13 H13 0.9500 . ? C14 C15 1.368(13) . ? C14 H14A 0.9500 . ? C15 C16 1.389(10) . ? C15 H15 0.9500 . ? C17 C25 1.345(9) . ? C17 C18 1.461(9) . ? C19 C24 1.404(9) . ? C19 C20 1.406(9) . ? C20 C21 1.394(9) . ? C20 H20A 0.9500 . ? C21 C22 1.420(11) . ? C21 H21 0.9500 . ? C22 C23 1.370(10) . ? C22 H22A 0.9500 . ? C23 C24 1.402(9) . ? C23 H23 0.9500 . ? C25 C26 1.447(10) . ? C25 H25 0.9500 . ? C27 C28 1.373(11) . ? C27 C32 1.391(12) . ? C28 C29 1.410(12) . ? C28 H28 0.9500 . ? C29 C30 1.347(15) . ? C29 H29 0.9500 . ? C30 C31 1.377(15) . ? C30 H30 0.9500 . ? C31 C32 1.412(12) . ? C31 H31 0.9500 . ? C33 C41 1.337(9) . ? C33 C34 1.484(9) . ? C35 C36 1.387(9) . ? C35 C40 1.414(9) . ? C36 C37 1.367(9) . ? C36 H36 0.9500 . ? C37 C38 1.421(11) . ? C37 H37 0.9500 . ? C38 C39 1.373(11) . ? C38 H38 0.9500 . ? C39 C40 1.386(9) . ? C39 H39 0.9500 . ? C41 C42 1.437(10) . ? C41 H41 0.9500 . ? C43 C44 1.375(12) . ? C43 C48 1.388(13) . ? C44 C45 1.384(13) . ? C44 H44 0.9500 . ? C45 C46 1.381(18) . ? C45 H45 0.9500 . ? C46 C47 1.395(18) . ? C46 H46 0.9500 . ? C47 C48 1.421(13) . ? C47 H47 0.9500 . ? C49 C57 1.370(10) . ? C49 C50 1.456(10) . ? C51 C52 1.386(10) . ? C51 C56 1.401(10) . ? C52 C53 1.401(10) . ? C52 H52 0.9500 . ? C53 C54 1.391(12) . ? C53 H53 0.9500 . ? C54 C55 1.408(13) . ? C54 H54 0.9500 . ? C55 C56 1.401(10) . ? C55 H55 0.9500 . ? C57 C58 1.432(10) . ? C57 H57 0.9500 . ? C59 C64 1.385(10) . ? C59 C60 1.396(9) . ? C60 C61 1.397(10) . ? C60 H60 0.9500 . ? C61 C62 1.405(11) . ? C61 H61 0.9500 . ? C62 C63 1.358(12) . ? C62 H62 0.9500 . ? C63 C64 1.374(12) . ? C63 H63 0.9500 . ? C65 C73 1.358(10) . ? C65 C66 1.469(10) . ? C67 C68 1.389(12) . ? C67 C72 1.400(11) . ? C68 C69 1.380(12) . ? C68 H68 0.9500 . ? C69 C70 1.416(14) . ? C69 H69 0.9500 . ? C70 C71 1.360(14) . ? C70 H70 0.9500 . ? C71 C72 1.406(12) . ? C71 H71 0.9500 . ? C73 C74 1.425(10) . ? C73 H73 0.9500 . ? C75 C76 1.388(11) . ? C75 C80 1.403(11) . ? C76 C77 1.383(11) . ? C76 H76 0.9500 . ? C77 C78 1.401(13) . ? C77 H77 0.9500 . ? C78 C79 1.390(13) . ? C78 H78 0.9500 . ? C79 C80 1.379(11) . ? C79 H79 0.9500 . ? C81 C89 1.348(10) . ? C81 C82 1.478(10) . ? C83 C88 1.415(12) . ? C83 C84 1.421(11) . ? C84 C85 1.410(14) . ? C84 H84 0.9500 . ? C85 C86 1.402(17) . ? C85 H85 0.9500 . ? C86 C87 1.369(16) . ? C86 H86 0.9500 . ? C87 C88 1.400(12) . ? C87 H87 0.9500 . ? C89 C90 1.428(10) . ? C89 H89 0.9500 . ? C91 C92 1.398(11) . ? C91 C96 1.406(11) . ? C92 C93 1.372(11) . ? C92 H92 0.9500 . ? C93 C94 1.379(14) . ? C93 H93 0.9500 . ? C94 C95 1.382(15) . ? C94 H94 0.9500 . ? C95 C96 1.402(11) . ? C95 H95 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N9 98.3(2) . . y N1 Ni1 N5 102.6(2) . . y N9 Ni1 N5 98.5(2) . . y N1 Ni1 O3 164.0(2) . . y N9 Ni1 O3 79.1(2) . . y N5 Ni1 O3 93.4(2) . . y N1 Ni1 O1 78.4(2) . . y N9 Ni1 O1 93.1(2) . . y N5 Ni1 O1 168.0(2) . . y O3 Ni1 O1 85.9(2) . . y N1 Ni1 O2 94.9(2) . . y N9 Ni1 O2 166.8(2) . . y N5 Ni1 O2 78.6(2) . . y O3 Ni1 O2 88.2(2) . . y O1 Ni1 O2 89.5(2) . . y N21 Ni2 N13 100.4(2) . . y N21 Ni2 N17 102.1(3) . . y N13 Ni2 N17 97.8(2) . . y N21 Ni2 O5 92.5(2) . . y N13 Ni2 O5 167.0(2) . . y N17 Ni2 O5 78.6(2) . . y N21 Ni2 O4 164.3(2) . . y N13 Ni2 O4 79.1(2) . . y N17 Ni2 O4 93.5(2) . . y O5 Ni2 O4 88.6(2) . . y N21 Ni2 O6 78.9(2) . . y N13 Ni2 O6 95.5(2) . . y N17 Ni2 O6 166.2(2) . . y O5 Ni2 O6 87.6(2) . . y O4 Ni2 O6 85.5(2) . . y N15 Ni3 O4 93.4(2) . . y N15 Ni3 O1 116.9(2) . . y O4 Ni3 O1 134.8(2) . . y N15 Ni3 N3 98.1(2) . . y O4 Ni3 N3 115.4(2) . . y O1 Ni3 N3 93.8(2) . . y O5 Ni4 N7 122.6(2) . . y O5 Ni4 N19 93.1(2) . . y N7 Ni4 N19 98.6(2) . . y O5 Ni4 O2 129.6(2) . . y N7 Ni4 O2 95.2(2) . . y N19 Ni4 O2 114.5(2) . . y O6 Ni5 N23 95.0(2) . . y O6 Ni5 N11 118.5(2) . . y N23 Ni5 N11 98.8(2) . . y O6 Ni5 O3 132.3(2) . . y N23 Ni5 O3 115.7(2) . . y N11 Ni5 O3 93.1(2) . . y C1 O1 Ni3 124.7(4) . . ? C1 O1 Ni1 115.1(3) . . ? Ni3 O1 Ni1 119.5(2) . . y C17 O2 Ni4 123.4(4) . . ? C17 O2 Ni1 114.1(4) . . ? Ni4 O2 Ni1 120.9(2) . . y C33 O3 Ni5 124.9(4) . . ? C33 O3 Ni1 115.2(4) . . ? Ni5 O3 Ni1 118.6(2) . . y C49 O4 Ni3 126.2(4) . . ? C49 O4 Ni2 113.4(4) . . ? Ni3 O4 Ni2 118.1(2) . . y C65 O5 Ni4 125.3(4) . . ? C65 O5 Ni2 115.3(4) . . ? Ni4 O5 Ni2 117.2(2) . . y C81 O6 Ni5 124.9(4) . . ? C81 O6 Ni2 113.7(4) . . ? Ni5 O6 Ni2 119.8(2) . . y C2 N1 C3 105.2(5) . . ? C2 N1 Ni1 115.1(4) . . ? C3 N1 Ni1 139.4(4) . . ? C2 N2 C8 106.5(5) . . ? C2 N2 H2 126.7 . . ? C8 N2 H2 126.7 . . ? C10 N3 C11 106.8(5) . . ? C10 N3 Ni3 124.5(4) . . ? C11 N3 Ni3 128.4(4) . . ? C10 N4 C16 107.0(6) . . ? C10 N4 H4 126.5 . . ? C16 N4 H4 126.5 . . ? C18 N5 C19 105.4(5) . . ? C18 N5 Ni1 113.8(4) . . ? C19 N5 Ni1 140.4(4) . . ? C24 N6 C18 107.0(5) . . ? C24 N6 H6 126.5 . . ? C18 N6 H6 126.5 . . ? C26 N7 C27 106.1(6) . . ? C26 N7 Ni4 123.9(5) . . ? C27 N7 Ni4 129.2(5) . . ? C26 N8 C32 107.3(7) . . ? C26 N8 H8 126.3 . . ? C32 N8 H8 126.3 . . ? C34 N9 C35 105.6(5) . . ? C34 N9 Ni1 113.5(4) . . ? C35 N9 Ni1 140.6(4) . . ? C34 N10 C40 107.1(5) . . ? C34 N10 H10 126.5 . . ? C40 N10 H10 126.5 . . ? C42 N11 C43 108.2(6) . . ? C42 N11 Ni5 124.2(5) . . ? C43 N11 Ni5 127.5(6) . . ? C42 N12 C48 107.2(8) . . ? C42 N12 H12 126.4 . . ? C48 N12 H12 126.4 . . ? C50 N13 C51 106.5(6) . . ? C50 N13 Ni2 113.3(4) . . ? C51 N13 Ni2 139.1(5) . . ? C50 N14 C56 106.5(6) . . ? C50 N14 H14 126.7 . . ? C56 N14 H14 126.7 . . ? C58 N15 C59 104.8(6) . . ? C58 N15 Ni3 125.7(5) . . ? C59 N15 Ni3 129.4(4) . . ? C58 N16 C64 109.1(6) . . ? C58 N16 H16 125.5 . . ? C64 N16 H16 125.5 . . ? C66 N17 C67 106.0(6) . . ? C66 N17 Ni2 113.5(5) . . ? C67 N17 Ni2 140.5(5) . . ? C66 N18 C72 108.2(7) . . ? C66 N18 H18 125.9 . . ? C72 N18 H18 125.9 . . ? C74 N19 C75 105.8(6) . . ? C74 N19 Ni4 125.3(5) . . ? C75 N19 Ni4 128.9(5) . . ? C74 N20 C80 108.3(6) . . ? C74 N20 H20 125.8 . . ? C80 N20 H20 125.8 . . ? C82 N21 C83 104.7(6) . . ? C82 N21 Ni2 114.5(4) . . ? C83 N21 Ni2 140.8(5) . . ? C82 N22 C88 106.2(7) . . ? C82 N22 H22 126.9 . . ? C88 N22 H22 126.9 . . ? C90 N23 C91 106.8(6) . . ? C90 N23 Ni5 123.0(5) . . ? C91 N23 Ni5 129.8(5) . . ? C90 N24 C96 108.0(7) . . ? C90 N24 H24 126.0 . . ? C96 N24 H24 126.0 . . ? C9 C1 O1 127.3(5) . . ? C9 C1 C2 121.6(6) . . ? O1 C1 C2 111.1(5) . . ? N1 C2 N2 113.6(5) . . ? N1 C2 C1 119.7(6) . . ? N2 C2 C1 126.7(5) . . ? N1 C3 C8 108.1(5) . . ? N1 C3 C4 131.0(6) . . ? C8 C3 C4 121.0(6) . . ? C5 C4 C3 115.9(6) . . ? C5 C4 H4A 122.0 . . ? C3 C4 H4A 122.0 . . ? C4 C5 C6 122.7(6) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 122.5(6) . . ? C7 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? C6 C7 C8 115.6(6) . . ? C6 C7 H7 122.2 . . ? C8 C7 H7 122.2 . . ? N2 C8 C7 131.1(6) . . ? N2 C8 C3 106.6(5) . . ? C7 C8 C3 122.3(6) . . ? C1 C9 C10 123.8(6) . . ? C1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? N3 C10 N4 111.7(6) . . ? N3 C10 C9 125.8(6) . . ? N4 C10 C9 122.4(6) . . ? N3 C11 C16 107.9(6) . . ? N3 C11 C12 131.0(6) . . ? C16 C11 C12 120.9(6) . . ? C13 C12 C11 116.4(8) . . ? C13 C12 H12A 121.8 . . ? C11 C12 H12A 121.8 . . ? C12 C13 C14 122.4(8) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 121.4(8) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 117.6(8) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? N4 C16 C15 132.2(7) . . ? N4 C16 C11 106.6(6) . . ? C15 C16 C11 121.2(7) . . ? C25 C17 O2 127.5(6) . . ? C25 C17 C18 120.9(6) . . ? O2 C17 C18 111.6(5) . . ? N5 C18 N6 112.3(5) . . ? N5 C18 C17 120.6(5) . . ? N6 C18 C17 127.1(5) . . ? N5 C19 C24 108.5(5) . . ? N5 C19 C20 129.7(6) . . ? C24 C19 C20 121.7(6) . . ? C21 C20 C19 115.8(6) . . ? C21 C20 H20A 122.1 . . ? C19 C20 H20A 122.1 . . ? C20 C21 C22 122.2(7) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 121.4(6) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 117.2(6) . . ? C22 C23 H23 121.4 . . ? C24 C23 H23 121.4 . . ? N6 C24 C23 131.6(6) . . ? N6 C24 C19 106.8(5) . . ? C23 C24 C19 121.5(6) . . ? C17 C25 C26 124.7(6) . . ? C17 C25 H25 117.6 . . ? C26 C25 H25 117.6 . . ? N7 C26 N8 111.6(6) . . ? N7 C26 C25 125.1(7) . . ? N8 C26 C25 123.2(7) . . ? C28 C27 C32 120.6(7) . . ? C28 C27 N7 130.9(8) . . ? C32 C27 N7 108.4(7) . . ? C27 C28 C29 117.3(9) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C30 C29 C28 121.0(9) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 124.1(9) . . ? C29 C30 H30 117.9 . . ? C31 C30 H30 117.9 . . ? C30 C31 C32 114.7(10) . . ? C30 C31 H31 122.7 . . ? C32 C31 H31 122.7 . . ? C27 C32 N8 106.5(6) . . ? C27 C32 C31 122.3(9) . . ? N8 C32 C31 131.1(9) . . ? C41 C33 O3 127.8(6) . . ? C41 C33 C34 120.7(6) . . ? O3 C33 C34 111.5(5) . . ? N9 C34 N10 113.0(6) . . ? N9 C34 C33 120.2(6) . . ? N10 C34 C33 126.8(6) . . ? C36 C35 N9 131.7(6) . . ? C36 C35 C40 120.0(6) . . ? N9 C35 C40 108.3(6) . . ? C37 C36 C35 118.7(7) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 120.6(7) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 121.8(6) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 117.0(7) . . ? C38 C39 H39 121.5 . . ? C40 C39 H39 121.5 . . ? C39 C40 N10 132.1(7) . . ? C39 C40 C35 121.9(7) . . ? N10 C40 C35 106.0(5) . . ? C33 C41 C42 122.5(7) . . ? C33 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? N11 C42 N12 109.5(7) . . ? N11 C42 C41 126.6(7) . . ? N12 C42 C41 123.9(7) . . ? N11 C43 C44 130.4(8) . . ? N11 C43 C48 108.4(7) . . ? C44 C43 C48 121.2(8) . . ? C43 C44 C45 118.4(10) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? C46 C45 C44 120.0(11) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 124.1(10) . . ? C45 C46 H46 117.9 . . ? C47 C46 H46 117.9 . . ? C46 C47 C48 114.1(11) . . ? C46 C47 H47 123.0 . . ? C48 C47 H47 123.0 . . ? C43 C48 N12 106.7(7) . . ? C43 C48 C47 122.1(10) . . ? N12 C48 C47 131.2(11) . . ? O4 C49 C57 124.5(6) . . ? O4 C49 C50 112.8(6) . . ? C57 C49 C50 122.8(7) . . ? N13 C50 N14 112.2(6) . . ? N13 C50 C49 120.4(6) . . ? N14 C50 C49 127.4(7) . . ? N13 C51 C52 130.3(7) . . ? N13 C51 C56 107.9(6) . . ? C52 C51 C56 121.8(6) . . ? C51 C52 C53 117.1(8) . . ? C51 C52 H52 121.5 . . ? C53 C52 H52 121.5 . . ? C54 C53 C52 120.8(8) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 123.1(7) . . ? C53 C54 H54 118.5 . . ? C55 C54 H54 118.5 . . ? C56 C55 C54 115.2(8) . . ? C56 C55 H55 122.4 . . ? C54 C55 H55 122.4 . . ? N14 C56 C55 131.1(8) . . ? N14 C56 C51 106.9(6) . . ? C55 C56 C51 122.0(7) . . ? C49 C57 C58 125.6(7) . . ? C49 C57 H57 117.2 . . ? C58 C57 H57 117.2 . . ? N16 C58 N15 111.1(6) . . ? N16 C58 C57 125.2(7) . . ? N15 C58 C57 123.6(7) . . ? C64 C59 C60 121.4(7) . . ? C64 C59 N15 109.7(6) . . ? C60 C59 N15 128.9(6) . . ? C61 C60 C59 116.3(7) . . ? C61 C60 H60 121.9 . . ? C59 C60 H60 121.9 . . ? C60 C61 C62 121.0(7) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C63 C62 C61 121.7(8) . . ? C63 C62 H62 119.1 . . ? C61 C62 H62 119.1 . . ? C62 C63 C64 117.7(8) . . ? C62 C63 H63 121.2 . . ? C64 C63 H63 121.2 . . ? C63 C64 C59 121.9(8) . . ? C63 C64 N16 132.8(8) . . ? C59 C64 N16 105.3(7) . . ? O5 C65 C73 126.4(7) . . ? O5 C65 C66 111.4(6) . . ? C73 C65 C66 122.3(7) . . ? N17 C66 N18 111.8(7) . . ? N17 C66 C65 120.8(6) . . ? N18 C66 C65 127.4(7) . . ? C68 C67 C72 120.9(7) . . ? C68 C67 N17 131.0(7) . . ? C72 C67 N17 108.0(7) . . ? C69 C68 C67 118.4(9) . . ? C69 C68 H68 120.8 . . ? C67 C68 H68 120.8 . . ? C68 C69 C70 119.7(9) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C71 C70 C69 123.1(8) . . ? C71 C70 H70 118.5 . . ? C69 C70 H70 118.5 . . ? C70 C71 C72 116.6(9) . . ? C70 C71 H71 121.7 . . ? C72 C71 H71 121.7 . . ? N18 C72 C67 105.9(6) . . ? N18 C72 C71 132.8(9) . . ? C67 C72 C71 121.2(9) . . ? C65 C73 C74 124.1(7) . . ? C65 C73 H73 117.9 . . ? C74 C73 H73 117.9 . . ? N19 C74 N20 110.8(7) . . ? N19 C74 C73 124.9(6) . . ? N20 C74 C73 124.2(7) . . ? C76 C75 N19 130.2(7) . . ? C76 C75 C80 120.8(7) . . ? N19 C75 C80 109.0(7) . . ? C77 C76 C75 118.3(8) . . ? C77 C76 H76 120.9 . . ? C75 C76 H76 120.9 . . ? C76 C77 C78 119.9(8) . . ? C76 C77 H77 120.1 . . ? C78 C77 H77 120.1 . . ? C79 C78 C77 122.6(7) . . ? C79 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C80 C79 C78 116.5(8) . . ? C80 C79 H79 121.7 . . ? C78 C79 H79 121.7 . . ? N20 C80 C79 132.2(8) . . ? N20 C80 C75 106.0(6) . . ? C79 C80 C75 121.8(8) . . ? O6 C81 C89 125.7(6) . . ? O6 C81 C82 112.6(6) . . ? C89 C81 C82 121.6(7) . . ? N21 C82 N22 113.8(6) . . ? N21 C82 C81 119.1(7) . . ? N22 C82 C81 127.1(7) . . ? N21 C83 C88 108.5(7) . . ? N21 C83 C84 130.2(8) . . ? C88 C83 C84 121.2(7) . . ? C85 C84 C83 115.9(10) . . ? C85 C84 H84 122.0 . . ? C83 C84 H84 122.0 . . ? C86 C85 C84 120.8(10) . . ? C86 C85 H85 119.6 . . ? C84 C85 H85 119.6 . . ? C87 C86 C85 124.0(9) . . ? C87 C86 H86 118.0 . . ? C85 C86 H86 118.0 . . ? C86 C87 C88 116.1(11) . . ? C86 C87 H87 121.9 . . ? C88 C87 H87 121.9 . . ? N22 C88 C87 131.4(9) . . ? N22 C88 C83 106.8(7) . . ? C87 C88 C83 121.8(9) . . ? C81 C89 C90 125.3(7) . . ? C81 C89 H89 117.4 . . ? C90 C89 H89 117.4 . . ? N23 C90 N24 110.8(6) . . ? N23 C90 C89 125.9(6) . . ? N24 C90 C89 123.3(7) . . ? N23 C91 C92 131.3(7) . . ? N23 C91 C96 108.4(6) . . ? C92 C91 C96 120.3(7) . . ? C93 C92 C91 116.8(8) . . ? C93 C92 H92 121.6 . . ? C91 C92 H92 121.6 . . ? C92 C93 C94 123.0(9) . . ? C92 C93 H93 118.5 . . ? C94 C93 H93 118.5 . . ? C93 C94 C95 121.8(8) . . ? C93 C94 H94 119.1 . . ? C95 C94 H94 119.1 . . ? C94 C95 C96 116.1(9) . . ? C94 C95 H95 122.0 . . ? C96 C95 H95 122.0 . . ? N24 C96 C95 132.1(8) . . ? N24 C96 C91 105.9(6) . . ? C95 C96 C91 122.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N15 Ni3 O1 C1 97.1(5) . . . . ? O4 Ni3 O1 C1 -136.1(4) . . . . ? N3 Ni3 O1 C1 -3.9(5) . . . . ? N15 Ni3 O1 Ni1 -72.5(3) . . . . ? O4 Ni3 O1 Ni1 54.2(4) . . . . ? N3 Ni3 O1 Ni1 -173.6(3) . . . . ? N1 Ni1 O1 C1 7.3(4) . . . . ? N9 Ni1 O1 C1 -90.5(4) . . . . ? N5 Ni1 O1 C1 103.6(9) . . . . ? O3 Ni1 O1 C1 -169.4(4) . . . . ? O2 Ni1 O1 C1 102.5(4) . . . . ? N1 Ni1 O1 Ni3 177.9(3) . . . . ? N9 Ni1 O1 Ni3 80.1(3) . . . . ? N5 Ni1 O1 Ni3 -85.8(9) . . . . ? O3 Ni1 O1 Ni3 1.3(2) . . . . ? O2 Ni1 O1 Ni3 -86.9(2) . . . . ? O5 Ni4 O2 C17 -143.1(4) . . . . ? N7 Ni4 O2 C17 -2.1(5) . . . . ? N19 Ni4 O2 C17 99.8(5) . . . . ? O5 Ni4 O2 Ni1 51.8(3) . . . . ? N7 Ni4 O2 Ni1 -167.3(3) . . . . ? N19 Ni4 O2 Ni1 -65.3(3) . . . . ? N1 Ni1 O2 C17 -95.0(4) . . . . ? N9 Ni1 O2 C17 85.5(9) . . . . ? N5 Ni1 O2 C17 6.9(4) . . . . ? O3 Ni1 O2 C17 100.8(4) . . . . ? O1 Ni1 O2 C17 -173.3(4) . . . . ? N1 Ni1 O2 Ni4 71.4(3) . . . . ? N9 Ni1 O2 Ni4 -108.0(8) . . . . ? N5 Ni1 O2 Ni4 173.3(3) . . . . ? O3 Ni1 O2 Ni4 -92.8(2) . . . . ? O1 Ni1 O2 Ni4 -6.9(2) . . . . ? O6 Ni5 O3 C33 -143.3(4) . . . . ? N23 Ni5 O3 C33 92.1(5) . . . . ? N11 Ni5 O3 C33 -9.3(5) . . . . ? O6 Ni5 O3 Ni1 50.5(3) . . . . ? N23 Ni5 O3 Ni1 -74.1(3) . . . . ? N11 Ni5 O3 Ni1 -175.5(2) . . . . ? N1 Ni1 O3 C33 88.2(7) . . . . ? N9 Ni1 O3 C33 6.3(4) . . . . ? N5 Ni1 O3 C33 -91.8(4) . . . . ? O1 Ni1 O3 C33 100.2(4) . . . . ? O2 Ni1 O3 C33 -170.2(4) . . . . ? N1 Ni1 O3 Ni5 -104.3(6) . . . . ? N9 Ni1 O3 Ni5 173.8(3) . . . . ? N5 Ni1 O3 Ni5 75.7(2) . . . . ? O1 Ni1 O3 Ni5 -92.3(2) . . . . ? O2 Ni1 O3 Ni5 -2.7(2) . . . . ? N15 Ni3 O4 C49 -11.4(5) . . . . ? O1 Ni3 O4 C49 -145.7(5) . . . . ? N3 Ni3 O4 C49 89.3(5) . . . . ? N15 Ni3 O4 Ni2 -172.7(3) . . . . ? O1 Ni3 O4 Ni2 53.0(4) . . . . ? N3 Ni3 O4 Ni2 -72.0(3) . . . . ? N21 Ni2 O4 C49 99.1(8) . . . . ? N13 Ni2 O4 C49 9.3(4) . . . . ? N17 Ni2 O4 C49 -88.0(4) . . . . ? O5 Ni2 O4 C49 -166.5(4) . . . . ? O6 Ni2 O4 C49 105.8(4) . . . . ? N21 Ni2 O4 Ni3 -97.3(8) . . . . ? N13 Ni2 O4 Ni3 172.9(3) . . . . ? N17 Ni2 O4 Ni3 75.6(3) . . . . ? O5 Ni2 O4 Ni3 -2.9(2) . . . . ? O6 Ni2 O4 Ni3 -90.6(3) . . . . ? N7 Ni4 O5 C65 93.2(6) . . . . ? N19 Ni4 O5 C65 -9.1(5) . . . . ? O2 Ni4 O5 C65 -134.9(5) . . . . ? N7 Ni4 O5 Ni2 -69.2(3) . . . . ? N19 Ni4 O5 Ni2 -171.5(3) . . . . ? O2 Ni4 O5 Ni2 62.8(3) . . . . ? N21 Ni2 O5 C65 -95.3(5) . . . . ? N13 Ni2 O5 C65 81.7(10) . . . . ? N17 Ni2 O5 C65 6.5(5) . . . . ? O4 Ni2 O5 C65 100.3(5) . . . . ? O6 Ni2 O5 C65 -174.1(5) . . . . ? N21 Ni2 O5 Ni4 68.8(3) . . . . ? N13 Ni2 O5 Ni4 -114.2(8) . . . . ? N17 Ni2 O5 Ni4 170.6(3) . . . . ? O4 Ni2 O5 Ni4 -95.6(3) . . . . ? O6 Ni2 O5 Ni4 -10.0(3) . . . . ? N23 Ni5 O6 C81 -3.9(5) . . . . ? N11 Ni5 O6 C81 98.9(5) . . . . ? O3 Ni5 O6 C81 -135.8(5) . . . . ? N23 Ni5 O6 Ni2 -168.4(3) . . . . ? N11 Ni5 O6 Ni2 -65.6(3) . . . . ? O3 Ni5 O6 Ni2 59.7(4) . . . . ? N21 Ni2 O6 C81 9.4(5) . . . . ? N13 Ni2 O6 C81 -90.2(5) . . . . ? N17 Ni2 O6 C81 105.1(10) . . . . ? O5 Ni2 O6 C81 102.4(5) . . . . ? O4 Ni2 O6 C81 -168.8(5) . . . . ? N21 Ni2 O6 Ni5 175.5(3) . . . . ? N13 Ni2 O6 Ni5 75.9(3) . . . . ? N17 Ni2 O6 Ni5 -88.8(10) . . . . ? O5 Ni2 O6 Ni5 -91.4(3) . . . . ? O4 Ni2 O6 Ni5 -2.6(2) . . . . ? N9 Ni1 N1 C2 84.3(4) . . . . ? N5 Ni1 N1 C2 -175.0(4) . . . . ? O3 Ni1 N1 C2 5.0(9) . . . . ? O1 Ni1 N1 C2 -7.2(4) . . . . ? O2 Ni1 N1 C2 -95.6(4) . . . . ? N9 Ni1 N1 C3 -88.0(6) . . . . ? N5 Ni1 N1 C3 12.7(6) . . . . ? O3 Ni1 N1 C3 -167.3(6) . . . . ? O1 Ni1 N1 C3 -179.5(6) . . . . ? O2 Ni1 N1 C3 92.1(6) . . . . ? N15 Ni3 N3 C10 -114.1(6) . . . . ? O4 Ni3 N3 C10 148.2(6) . . . . ? O1 Ni3 N3 C10 3.8(6) . . . . ? N15 Ni3 N3 C11 58.4(7) . . . . ? O4 Ni3 N3 C11 -39.3(7) . . . . ? O1 Ni3 N3 C11 176.2(6) . . . . ? N1 Ni1 N5 C18 92.4(4) . . . . ? N9 Ni1 N5 C18 -167.1(4) . . . . ? O3 Ni1 N5 C18 -87.6(4) . . . . ? O1 Ni1 N5 C18 -1.3(12) . . . . ? O2 Ni1 N5 C18 -0.2(4) . . . . ? N1 Ni1 N5 C19 -96.9(6) . . . . ? N9 Ni1 N5 C19 3.6(7) . . . . ? O3 Ni1 N5 C19 83.1(6) . . . . ? O1 Ni1 N5 C19 169.3(7) . . . . ? O2 Ni1 N5 C19 170.5(7) . . . . ? O5 Ni4 N7 C26 147.6(5) . . . . ? N19 Ni4 N7 C26 -113.1(6) . . . . ? O2 Ni4 N7 C26 2.7(6) . . . . ? O5 Ni4 N7 C27 -43.7(7) . . . . ? N19 Ni4 N7 C27 55.7(6) . . . . ? O2 Ni4 N7 C27 171.5(6) . . . . ? N1 Ni1 N9 C34 -169.8(4) . . . . ? N5 Ni1 N9 C34 86.0(4) . . . . ? O3 Ni1 N9 C34 -5.8(4) . . . . ? O1 Ni1 N9 C34 -91.1(4) . . . . ? O2 Ni1 N9 C34 9.7(10) . . . . ? N1 Ni1 N9 C35 16.4(6) . . . . ? N5 Ni1 N9 C35 -87.8(6) . . . . ? O3 Ni1 N9 C35 -179.6(6) . . . . ? O1 Ni1 N9 C35 95.1(6) . . . . ? O2 Ni1 N9 C35 -164.2(6) . . . . ? O6 Ni5 N11 C42 146.8(5) . . . . ? N23 Ni5 N11 C42 -112.6(6) . . . . ? O3 Ni5 N11 C42 4.0(6) . . . . ? O6 Ni5 N11 C43 -35.7(6) . . . . ? N23 Ni5 N11 C43 64.9(6) . . . . ? O3 Ni5 N11 C43 -178.5(6) . . . . ? N21 Ni2 N13 C50 -172.8(4) . . . . ? N17 Ni2 N13 C50 83.3(5) . . . . ? O5 Ni2 N13 C50 10.2(11) . . . . ? O4 Ni2 N13 C50 -8.8(4) . . . . ? O6 Ni2 N13 C50 -93.1(5) . . . . ? N21 Ni2 N13 C51 21.7(7) . . . . ? N17 Ni2 N13 C51 -82.3(7) . . . . ? O5 Ni2 N13 C51 -155.4(7) . . . . ? O4 Ni2 N13 C51 -174.3(7) . . . . ? O6 Ni2 N13 C51 101.4(6) . . . . ? O4 Ni3 N15 C58 6.3(6) . . . . ? O1 Ni3 N15 C58 151.6(5) . . . . ? N3 Ni3 N15 C58 -110.0(6) . . . . ? O4 Ni3 N15 C59 -178.2(5) . . . . ? O1 Ni3 N15 C59 -32.9(6) . . . . ? N3 Ni3 N15 C59 65.5(5) . . . . ? N21 Ni2 N17 C66 86.0(6) . . . . ? N13 Ni2 N17 C66 -171.5(6) . . . . ? O5 Ni2 N17 C66 -4.1(5) . . . . ? O4 Ni2 N17 C66 -92.0(6) . . . . ? O6 Ni2 N17 C66 -6.8(14) . . . . ? N21 Ni2 N17 C67 -95.1(9) . . . . ? N13 Ni2 N17 C67 7.4(9) . . . . ? O5 Ni2 N17 C67 174.8(9) . . . . ? O4 Ni2 N17 C67 86.9(9) . . . . ? O6 Ni2 N17 C67 172.1(8) . . . . ? O5 Ni4 N19 C74 2.3(6) . . . . ? N7 Ni4 N19 C74 -121.4(6) . . . . ? O2 Ni4 N19 C74 138.8(5) . . . . ? O5 Ni4 N19 C75 -178.0(6) . . . . ? N7 Ni4 N19 C75 58.4(6) . . . . ? O2 Ni4 N19 C75 -41.5(6) . . . . ? N13 Ni2 N21 C82 88.0(5) . . . . ? N17 Ni2 N21 C82 -171.6(5) . . . . ? O5 Ni2 N21 C82 -92.7(5) . . . . ? O4 Ni2 N21 C82 1.2(11) . . . . ? O6 Ni2 N21 C82 -5.7(5) . . . . ? N13 Ni2 N21 C83 -90.8(8) . . . . ? N17 Ni2 N21 C83 9.6(8) . . . . ? O5 Ni2 N21 C83 88.5(7) . . . . ? O4 Ni2 N21 C83 -177.6(6) . . . . ? O6 Ni2 N21 C83 175.5(8) . . . . ? O6 Ni5 N23 C90 1.6(6) . . . . ? N11 Ni5 N23 C90 -118.3(6) . . . . ? O3 Ni5 N23 C90 143.9(5) . . . . ? O6 Ni5 N23 C91 173.9(6) . . . . ? N11 Ni5 N23 C91 54.0(6) . . . . ? O3 Ni5 N23 C91 -43.8(6) . . . . ? Ni3 O1 C1 C9 3.2(9) . . . . ? Ni1 O1 C1 C9 173.3(6) . . . . ? Ni3 O1 C1 C2 -175.9(4) . . . . ? Ni1 O1 C1 C2 -5.9(6) . . . . ? C3 N1 C2 N2 -0.4(7) . . . . ? Ni1 N1 C2 N2 -175.2(4) . . . . ? C3 N1 C2 C1 -178.6(5) . . . . ? Ni1 N1 C2 C1 6.6(7) . . . . ? C8 N2 C2 N1 0.0(7) . . . . ? C8 N2 C2 C1 178.0(6) . . . . ? C9 C1 C2 N1 -179.5(6) . . . . ? O1 C1 C2 N1 -0.2(8) . . . . ? C9 C1 C2 N2 2.6(10) . . . . ? O1 C1 C2 N2 -178.2(6) . . . . ? C2 N1 C3 C8 0.7(6) . . . . ? Ni1 N1 C3 C8 173.5(5) . . . . ? C2 N1 C3 C4 -179.3(6) . . . . ? Ni1 N1 C3 C4 -6.5(11) . . . . ? N1 C3 C4 C5 -177.5(6) . . . . ? C8 C3 C4 C5 2.6(9) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? C4 C5 C6 C7 -0.8(11) . . . . ? C5 C6 C7 C8 1.9(10) . . . . ? C2 N2 C8 C7 -178.7(7) . . . . ? C2 N2 C8 C3 0.5(7) . . . . ? C6 C7 C8 N2 178.3(6) . . . . ? C6 C7 C8 C3 -0.8(10) . . . . ? N1 C3 C8 N2 -0.7(7) . . . . ? C4 C3 C8 N2 179.2(5) . . . . ? N1 C3 C8 C7 178.5(6) . . . . ? C4 C3 C8 C7 -1.5(10) . . . . ? O1 C1 C9 C10 -0.9(11) . . . . ? C2 C1 C9 C10 178.2(6) . . . . ? C11 N3 C10 N4 1.1(9) . . . . ? Ni3 N3 C10 N4 175.0(5) . . . . ? C11 N3 C10 C9 -176.7(7) . . . . ? Ni3 N3 C10 C9 -2.9(11) . . . . ? C16 N4 C10 N3 -1.6(9) . . . . ? C16 N4 C10 C9 176.3(7) . . . . ? C1 C9 C10 N3 0.8(12) . . . . ? C1 C9 C10 N4 -176.8(7) . . . . ? C10 N3 C11 C16 -0.2(9) . . . . ? Ni3 N3 C11 C16 -173.7(5) . . . . ? C10 N3 C11 C12 175.1(9) . . . . ? Ni3 N3 C11 C12 1.6(13) . . . . ? N3 C11 C12 C13 -177.7(9) . . . . ? C16 C11 C12 C13 -2.8(14) . . . . ? C11 C12 C13 C14 2.1(17) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C16 1.4(19) . . . . ? C10 N4 C16 C15 -178.2(11) . . . . ? C10 N4 C16 C11 1.3(9) . . . . ? C14 C15 C16 N4 177.3(11) . . . . ? C14 C15 C16 C11 -2.2(16) . . . . ? N3 C11 C16 N4 -0.7(9) . . . . ? C12 C11 C16 N4 -176.6(8) . . . . ? N3 C11 C16 C15 178.9(9) . . . . ? C12 C11 C16 C15 3.0(14) . . . . ? Ni4 O2 C17 C25 2.2(9) . . . . ? Ni1 O2 C17 C25 168.2(6) . . . . ? Ni4 O2 C17 C18 -177.6(4) . . . . ? Ni1 O2 C17 C18 -11.6(6) . . . . ? C19 N5 C18 N6 -0.1(7) . . . . ? Ni1 N5 C18 N6 173.8(4) . . . . ? C19 N5 C18 C17 179.7(6) . . . . ? Ni1 N5 C18 C17 -6.5(8) . . . . ? C24 N6 C18 N5 0.1(7) . . . . ? C24 N6 C18 C17 -179.6(6) . . . . ? C25 C17 C18 N5 -167.4(6) . . . . ? O2 C17 C18 N5 12.4(9) . . . . ? C25 C17 C18 N6 12.3(11) . . . . ? O2 C17 C18 N6 -167.9(6) . . . . ? C18 N5 C19 C24 0.0(7) . . . . ? Ni1 N5 C19 C24 -171.1(5) . . . . ? C18 N5 C19 C20 -176.9(6) . . . . ? Ni1 N5 C19 C20 12.0(11) . . . . ? N5 C19 C20 C21 -179.4(6) . . . . ? C24 C19 C20 C21 4.1(9) . . . . ? C19 C20 C21 C22 -0.2(10) . . . . ? C20 C21 C22 C23 -1.5(12) . . . . ? C21 C22 C23 C24 -0.5(11) . . . . ? C18 N6 C24 C23 -176.0(7) . . . . ? C18 N6 C24 C19 -0.1(7) . . . . ? C22 C23 C24 N6 179.7(7) . . . . ? C22 C23 C24 C19 4.4(10) . . . . ? N5 C19 C24 N6 0.1(7) . . . . ? C20 C19 C24 N6 177.3(6) . . . . ? N5 C19 C24 C23 176.4(6) . . . . ? C20 C19 C24 C23 -6.4(10) . . . . ? O2 C17 C25 C26 -2.0(12) . . . . ? C18 C17 C25 C26 177.7(7) . . . . ? C27 N7 C26 N8 1.9(9) . . . . ? Ni4 N7 C26 N8 172.9(5) . . . . ? C27 N7 C26 C25 -174.3(7) . . . . ? Ni4 N7 C26 C25 -3.3(10) . . . . ? C32 N8 C26 N7 -1.7(9) . . . . ? C32 N8 C26 C25 174.6(7) . . . . ? C17 C25 C26 N7 2.7(12) . . . . ? C17 C25 C26 N8 -173.1(8) . . . . ? C26 N7 C27 C28 177.5(8) . . . . ? Ni4 N7 C27 C28 7.2(12) . . . . ? C26 N7 C27 C32 -1.4(9) . . . . ? Ni4 N7 C27 C32 -171.7(6) . . . . ? C32 C27 C28 C29 0.8(12) . . . . ? N7 C27 C28 C29 -178.0(8) . . . . ? C27 C28 C29 C30 -1.6(14) . . . . ? C28 C29 C30 C31 1.9(17) . . . . ? C29 C30 C31 C32 -1.2(16) . . . . ? C28 C27 C32 N8 -178.6(7) . . . . ? N7 C27 C32 N8 0.4(9) . . . . ? C28 C27 C32 C31 -0.2(14) . . . . ? N7 C27 C32 C31 178.9(8) . . . . ? C26 N8 C32 C27 0.7(10) . . . . ? C26 N8 C32 C31 -177.5(10) . . . . ? C30 C31 C32 C27 0.3(14) . . . . ? C30 C31 C32 N8 178.3(10) . . . . ? Ni5 O3 C33 C41 9.9(9) . . . . ? Ni1 O3 C33 C41 176.5(6) . . . . ? Ni5 O3 C33 C34 -171.9(4) . . . . ? Ni1 O3 C33 C34 -5.3(6) . . . . ? C35 N9 C34 N10 -1.1(7) . . . . ? Ni1 N9 C34 N10 -177.1(4) . . . . ? C35 N9 C34 C33 -179.0(5) . . . . ? Ni1 N9 C34 C33 5.0(7) . . . . ? C40 N10 C34 N9 0.6(7) . . . . ? C40 N10 C34 C33 178.3(6) . . . . ? C41 C33 C34 N9 178.6(6) . . . . ? O3 C33 C34 N9 0.3(8) . . . . ? C41 C33 C34 N10 1.0(10) . . . . ? O3 C33 C34 N10 -177.3(6) . . . . ? C34 N9 C35 C36 -179.3(7) . . . . ? Ni1 N9 C35 C36 -5.1(11) . . . . ? C34 N9 C35 C40 1.3(6) . . . . ? Ni1 N9 C35 C40 175.4(5) . . . . ? N9 C35 C36 C37 -178.5(6) . . . . ? C40 C35 C36 C37 0.9(9) . . . . ? C35 C36 C37 C38 -0.1(10) . . . . ? C36 C37 C38 C39 -0.3(11) . . . . ? C37 C38 C39 C40 -0.2(10) . . . . ? C38 C39 C40 N10 179.8(7) . . . . ? C38 C39 C40 C35 1.0(10) . . . . ? C34 N10 C40 C39 -178.7(7) . . . . ? C34 N10 C40 C35 0.2(7) . . . . ? C36 C35 C40 C39 -1.4(9) . . . . ? N9 C35 C40 C39 178.1(6) . . . . ? C36 C35 C40 N10 179.5(5) . . . . ? N9 C35 C40 N10 -0.9(7) . . . . ? O3 C33 C41 C42 -2.2(11) . . . . ? C34 C33 C41 C42 179.8(6) . . . . ? C43 N11 C42 N12 1.8(8) . . . . ? Ni5 N11 C42 N12 179.7(5) . . . . ? C43 N11 C42 C41 -176.4(7) . . . . ? Ni5 N11 C42 C41 1.5(10) . . . . ? C48 N12 C42 N11 -0.6(9) . . . . ? C48 N12 C42 C41 177.7(8) . . . . ? C33 C41 C42 N11 -4.0(12) . . . . ? C33 C41 C42 N12 178.0(7) . . . . ? C42 N11 C43 C44 178.7(8) . . . . ? Ni5 N11 C43 C44 0.9(11) . . . . ? C42 N11 C43 C48 -2.3(9) . . . . ? Ni5 N11 C43 C48 179.8(6) . . . . ? N11 C43 C44 C45 177.8(8) . . . . ? C48 C43 C44 C45 -1.1(12) . . . . ? C43 C44 C45 C46 0.0(15) . . . . ? C44 C45 C46 C47 1(2) . . . . ? C45 C46 C47 C48 -1(2) . . . . ? N11 C43 C48 N12 2.0(10) . . . . ? C44 C43 C48 N12 -178.9(7) . . . . ? N11 C43 C48 C47 -177.7(9) . . . . ? C44 C43 C48 C47 1.4(14) . . . . ? C42 N12 C48 C43 -0.9(10) . . . . ? C42 N12 C48 C47 178.8(11) . . . . ? C46 C47 C48 C43 -0.5(17) . . . . ? C46 C47 C48 N12 179.9(12) . . . . ? Ni3 O4 C49 C57 10.1(9) . . . . ? Ni2 O4 C49 C57 172.1(6) . . . . ? Ni3 O4 C49 C50 -170.0(4) . . . . ? Ni2 O4 C49 C50 -8.0(7) . . . . ? C51 N13 C50 N14 0.4(7) . . . . ? Ni2 N13 C50 N14 -169.8(4) . . . . ? C51 N13 C50 C49 177.8(6) . . . . ? Ni2 N13 C50 C49 7.6(8) . . . . ? C56 N14 C50 N13 -0.1(8) . . . . ? C56 N14 C50 C49 -177.3(7) . . . . ? O4 C49 C50 N13 0.5(9) . . . . ? C57 C49 C50 N13 -179.6(7) . . . . ? O4 C49 C50 N14 177.4(6) . . . . ? C57 C49 C50 N14 -2.6(11) . . . . ? C50 N13 C51 C52 179.2(7) . . . . ? Ni2 N13 C51 C52 -14.6(11) . . . . ? C50 N13 C51 C56 -0.5(7) . . . . ? Ni2 N13 C51 C56 165.7(5) . . . . ? N13 C51 C52 C53 178.6(6) . . . . ? C56 C51 C52 C53 -1.8(10) . . . . ? C51 C52 C53 C54 -1.1(10) . . . . ? C52 C53 C54 C55 3.0(12) . . . . ? C53 C54 C55 C56 -1.8(12) . . . . ? C50 N14 C56 C55 177.2(8) . . . . ? C50 N14 C56 C51 -0.1(8) . . . . ? C54 C55 C56 N14 -178.2(8) . . . . ? C54 C55 C56 C51 -1.1(11) . . . . ? N13 C51 C56 N14 0.4(7) . . . . ? C52 C51 C56 N14 -179.3(6) . . . . ? N13 C51 C56 C55 -177.3(7) . . . . ? C52 C51 C56 C55 3.0(11) . . . . ? O4 C49 C57 C58 -0.1(12) . . . . ? C50 C49 C57 C58 -180.0(7) . . . . ? C64 N16 C58 N15 -1.0(9) . . . . ? C64 N16 C58 C57 177.0(8) . . . . ? C59 N15 C58 N16 1.9(8) . . . . ? Ni3 N15 C58 N16 178.4(5) . . . . ? C59 N15 C58 C57 -176.1(7) . . . . ? Ni3 N15 C58 C57 0.3(10) . . . . ? C49 C57 C58 N16 176.8(8) . . . . ? C49 C57 C58 N15 -5.4(12) . . . . ? C58 N15 C59 C64 -2.2(8) . . . . ? Ni3 N15 C59 C64 -178.4(5) . . . . ? C58 N15 C59 C60 178.4(7) . . . . ? Ni3 N15 C59 C60 2.2(10) . . . . ? C64 C59 C60 C61 0.2(10) . . . . ? N15 C59 C60 C61 179.5(6) . . . . ? C59 C60 C61 C62 -1.5(10) . . . . ? C60 C61 C62 C63 1.9(13) . . . . ? C61 C62 C63 C64 -0.7(14) . . . . ? C62 C63 C64 C59 -0.7(14) . . . . ? C62 C63 C64 N16 179.3(9) . . . . ? C60 C59 C64 C63 1.0(12) . . . . ? N15 C59 C64 C63 -178.5(8) . . . . ? C60 C59 C64 N16 -179.0(6) . . . . ? N15 C59 C64 N16 1.6(8) . . . . ? C58 N16 C64 C63 179.7(10) . . . . ? C58 N16 C64 C59 -0.4(9) . . . . ? Ni4 O5 C65 C73 10.2(11) . . . . ? Ni2 O5 C65 C73 172.9(6) . . . . ? Ni4 O5 C65 C66 -169.9(5) . . . . ? Ni2 O5 C65 C66 -7.3(8) . . . . ? C67 N17 C66 N18 0.9(9) . . . . ? Ni2 N17 C66 N18 -179.8(6) . . . . ? C67 N17 C66 C65 -177.7(7) . . . . ? Ni2 N17 C66 C65 1.6(10) . . . . ? C72 N18 C66 N17 -0.8(10) . . . . ? C72 N18 C66 C65 177.7(8) . . . . ? O5 C65 C66 N17 3.9(11) . . . . ? C73 C65 C66 N17 -176.2(8) . . . . ? O5 C65 C66 N18 -174.4(8) . . . . ? C73 C65 C66 N18 5.4(13) . . . . ? C66 N17 C67 C68 178.7(10) . . . . ? Ni2 N17 C67 C68 -0.3(16) . . . . ? C66 N17 C67 C72 -0.7(10) . . . . ? Ni2 N17 C67 C72 -179.6(7) . . . . ? C72 C67 C68 C69 1.8(15) . . . . ? N17 C67 C68 C69 -177.5(10) . . . . ? C67 C68 C69 C70 -2.6(16) . . . . ? C68 C69 C70 C71 0.5(18) . . . . ? C69 C70 C71 C72 2.3(19) . . . . ? C66 N18 C72 C67 0.3(11) . . . . ? C66 N18 C72 C71 179.9(12) . . . . ? C68 C67 C72 N18 -179.2(9) . . . . ? N17 C67 C72 N18 0.2(10) . . . . ? C68 C67 C72 C71 1.1(16) . . . . ? N17 C67 C72 C71 -179.5(10) . . . . ? C70 C71 C72 N18 177.4(11) . . . . ? C70 C71 C72 C67 -3.1(17) . . . . ? O5 C65 C73 C74 -1.7(13) . . . . ? C66 C65 C73 C74 178.5(7) . . . . ? C75 N19 C74 N20 0.7(8) . . . . ? Ni4 N19 C74 N20 -179.5(5) . . . . ? C75 N19 C74 C73 -175.4(7) . . . . ? Ni4 N19 C74 C73 4.4(10) . . . . ? C80 N20 C74 N19 -0.4(8) . . . . ? C80 N20 C74 C73 175.7(7) . . . . ? C65 C73 C74 N19 -6.2(12) . . . . ? C65 C73 C74 N20 178.2(7) . . . . ? C74 N19 C75 C76 179.0(7) . . . . ? Ni4 N19 C75 C76 -0.8(11) . . . . ? C74 N19 C75 C80 -0.7(8) . . . . ? Ni4 N19 C75 C80 179.5(5) . . . . ? N19 C75 C76 C77 -179.1(7) . . . . ? C80 C75 C76 C77 0.6(11) . . . . ? C75 C76 C77 C78 -3.1(11) . . . . ? C76 C77 C78 C79 3.5(13) . . . . ? C77 C78 C79 C80 -1.1(13) . . . . ? C74 N20 C80 C79 178.8(8) . . . . ? C74 N20 C80 C75 0.0(8) . . . . ? C78 C79 C80 N20 179.8(8) . . . . ? C78 C79 C80 C75 -1.5(12) . . . . ? C76 C75 C80 N20 -179.3(6) . . . . ? N19 C75 C80 N20 0.5(8) . . . . ? C76 C75 C80 C79 1.7(11) . . . . ? N19 C75 C80 C79 -178.5(7) . . . . ? Ni5 O6 C81 C89 6.4(10) . . . . ? Ni2 O6 C81 C89 171.8(6) . . . . ? Ni5 O6 C81 C82 -176.2(4) . . . . ? Ni2 O6 C81 C82 -10.8(7) . . . . ? C83 N21 C82 N22 -0.1(8) . . . . ? Ni2 N21 C82 N22 -179.3(5) . . . . ? C83 N21 C82 C81 -179.1(6) . . . . ? Ni2 N21 C82 C81 1.7(8) . . . . ? C88 N22 C82 N21 -0.9(9) . . . . ? C88 N22 C82 C81 178.1(7) . . . . ? O6 C81 C82 N21 6.5(9) . . . . ? C89 C81 C82 N21 -176.0(7) . . . . ? O6 C81 C82 N22 -172.4(7) . . . . ? C89 C81 C82 N22 5.1(12) . . . . ? C82 N21 C83 C88 0.9(8) . . . . ? Ni2 N21 C83 C88 179.8(6) . . . . ? C82 N21 C83 C84 -179.6(8) . . . . ? Ni2 N21 C83 C84 -0.7(13) . . . . ? N21 C83 C84 C85 -179.3(8) . . . . ? C88 C83 C84 C85 0.1(11) . . . . ? C83 C84 C85 C86 -0.5(13) . . . . ? C84 C85 C86 C87 1.3(16) . . . . ? C85 C86 C87 C88 -1.7(15) . . . . ? C82 N22 C88 C87 -179.1(9) . . . . ? C82 N22 C88 C83 1.4(8) . . . . ? C86 C87 C88 N22 -178.1(9) . . . . ? C86 C87 C88 C83 1.3(13) . . . . ? N21 C83 C88 N22 -1.5(8) . . . . ? C84 C83 C88 N22 179.0(7) . . . . ? N21 C83 C88 C87 179.0(7) . . . . ? C84 C83 C88 C87 -0.5(12) . . . . ? O6 C81 C89 C90 -5.7(13) . . . . ? C82 C81 C89 C90 177.1(7) . . . . ? C91 N23 C90 N24 4.0(8) . . . . ? Ni5 N23 C90 N24 177.8(5) . . . . ? C91 N23 C90 C89 -175.2(7) . . . . ? Ni5 N23 C90 C89 -1.4(10) . . . . ? C96 N24 C90 N23 -3.6(9) . . . . ? C96 N24 C90 C89 175.6(7) . . . . ? C81 C89 C90 N23 3.0(13) . . . . ? C81 C89 C90 N24 -176.1(8) . . . . ? C90 N23 C91 C92 177.5(8) . . . . ? Ni5 N23 C91 C92 4.2(12) . . . . ? C90 N23 C91 C96 -2.8(8) . . . . ? Ni5 N23 C91 C96 -176.1(5) . . . . ? N23 C91 C92 C93 -180.0(8) . . . . ? C96 C91 C92 C93 0.4(11) . . . . ? C91 C92 C93 C94 0.1(13) . . . . ? C92 C93 C94 C95 -2.0(16) . . . . ? C93 C94 C95 C96 3.1(15) . . . . ? C90 N24 C96 C95 -178.9(10) . . . . ? C90 N24 C96 C91 1.7(9) . . . . ? C94 C95 C96 N24 178.0(9) . . . . ? C94 C95 C96 C91 -2.6(14) . . . . ? N23 C91 C96 N24 0.7(9) . . . . ? C92 C91 C96 N24 -179.6(7) . . . . ? N23 C91 C96 C95 -178.8(8) . . . . ? C92 C91 C96 C95 0.9(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N24 H24 Br6 0.88 2.25 3.059(12) 153.2 . y N22 H22 Br4 0.88 2.46 3.324(8) 166.7 . y N20 H20 Br7 0.88 2.44 3.166(7) 140.8 . y N18 H18 Br2 0.88 2.44 3.318(7) 174.6 . y N16 H16 Br2 0.88 2.79 3.529(7) 143.3 1_455 y N14 H14 Br10 0.88 2.27 3.144(11) 169.5 1_455 y N12 H12 Br2 0.88 2.61 3.320(9) 139.0 1_455 y N10 H10 Br7 0.88 2.21 3.086(6) 173.7 1_455 y N8 H8 Br3 0.88 2.38 3.254(7) 169.9 4_565 y N6 H6 Br8 0.88 2.34 3.186(8) 161.0 1_455 y N6 H6 Br9 0.88 1.99 2.866(13) 176.3 1_455 y N4 H4 Br4 0.88 2.27 3.097(7) 157.2 2_655 y N2 H2 Br1 0.88 2.39 3.241(5) 161.4 . y _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.597 _refine_diff_density_min -1.372 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) 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 0.000 0.000 0.500 7 1 ' ' 2 0.736 0.081 0.127 21 1 ' ' 3 0.193 0.143 0.296 16 1 ' ' 4 0.524 0.224 0.495 67 7 ' ' 5 0.524 0.275 -0.005 67 7 ' ' 6 0.193 0.357 0.796 16 1 ' ' 7 0.736 0.419 0.627 21 1 ' ' 8 0.000 0.500 0.000 7 1 ' ' 9 0.264 0.581 0.373 21 1 ' ' 10 0.807 0.643 0.204 16 1 ' ' 11 0.476 0.724 0.005 67 7 ' ' 12 0.476 0.776 0.505 67 7 ' ' 13 0.807 0.857 0.704 16 1 ' ' 14 0.264 0.919 0.872 21 1 ' ' _platon_squeeze_details ; Structure contains solvent accessible voids of 521.4 A3/per unit cell, i.e. some 5.3% of the total volume. Data were also corrected for disordered electron density through use of the SQUEEZE procedure. Attempts to refine peaks of residual electron density as solvent water molecules were unsuccessful. Derived values (formula weight, density, absorption coefficient) do not contain the contribution of the disordered solvent molecule. ; _vrf_PLAT431_fwbr-14 ; PROBLEM: Short Inter HL..A Contact Br2 .. Br10 .. 3.34 Ang. Short Inter HL..A Contact Br5 .. Br10 .. 3.33 Ang. RESPONSE: these atoms are disordered. ; _vrf_PLAT241_fwbr-14 ; PROBLEM: High Ueq as Compared to Neighbors for C46 High Ueq as Compared to Neighbors for C71 RESPONSE: these atoms are also disordered. ; _vrf_PLAT420_fwbr-14 ; PROBLEM: D-H Without Acceptor N4 - H4 ... ? D-H Without Acceptor N6 - H6 ... ? D-H Without Acceptor N10 - H10 ... ? D-H Without Acceptor N14 - H14 ... ? D-H Without Acceptor N20 - H20 ... ? D-H Without Acceptor N22 - H22 ... ? D-H Without Acceptor N24 - H24 ... ? RESPONSE: The possible acceptors are solvent molecules (water). They are disordered without refinment. ; _vrf_PLAT234_fwno3b-s ; PROBLEM: Large Hirshfeld Difference C27 -- C32 Large Hirshfeld Difference C53 -- C54 Large Hirshfeld Difference C70 -- C71 RESPONSE: these atoms are also disordered. ; # end Validation Reply Form # Attachment '7_CCDC676418.cif' data_fwi-14 _database_code_depnum_ccdc_archive 'CCDC 676418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H66 I4 N24 Ni5 O6' _chemical_formula_weight 2452.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.239(2) _cell_length_b 26.690(4) _cell_length_c 28.981(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.749(6) _cell_angle_gamma 90.00 _cell_volume 9856(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17261 _cell_measurement_theta_min 2.1119 _cell_measurement_theta_max 27.4719 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4840 _exptl_absorpt_coefficient_mu 2.256 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6869 _exptl_absorpt_correction_T_max 0.7581 _exptl_absorpt_process_details ; (HIGASHI, T. (1995). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61653 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16928 _reflns_number_gt 13041 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material ; SHELXTL/PC Mercury Ver. 1.3 (Bruno et al., 2002) ; _refine_special_details ; Structure was phased by direct methods. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. Fourier maps show that there were severe partial occupancies for all four I anions. The occupancies of these sites were freely refined with PART or SUMP instruction firstly, and then the assigned occupancies of many sites were fixed in the process of refinement except I1A and I1B. The final occupancies of all I anions from the refinement were I1A 0.60, I1B 0.40; I2A 0.75, I2B 0.15, I2C 0.10; I3A 0.45, I3B 0.25, I3C 0.18, I3D 0.12; I4A 0.70, I4B 0.20, I4C 0.10, respectively. The anions had still large Ueq values. This should be results of disordered anions. We also note several distances in range of 2.85~3.02 A between N atoms and I anions with partial occupacies, I3B 0.25, I3C 0.18, I3D 0.12, I4C 0.10. We considered that these I anions of less occupacies could be O atoms (water molecules), but failed convergence in the process of refinement and these sites were very closed each other and to other I anions. So, we think these situations should be also results of severe disordered anions. The residual electron density had a maximum located 1.98 A from atom I1B. H-atoms were included in calculated positions and treated as riding atoms using the SHELXL default parameters. Displacement parameters for the proposed model converged with an unusually large Ueq(max)/Ueq(min) ratio 3.55 to 4.10. This large range may be attributed to the basic structural network which might best be described as systematic disorder for I anions. Diffaction data were well observed at high resolution but fit poorly at low resolution suggesting limitations in the proposed disorder model. All efforts to identify a super-lattice or refine an ordered model in all possible non-isomorphic sub-groups failed to eliminate the ambiguities in the ligand and solvate molecules. ; _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^)+(0.2000P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16928 _refine_ls_number_parameters 1290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.1017 _refine_ls_wR_factor_ref 0.3154 _refine_ls_wR_factor_gt 0.2781 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max 0.001 _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 Ni1 Ni 0.16933(6) 0.91149(3) 0.64551(2) 0.0322(2) Uani 1 1 d . . . Ni2 Ni 0.35145(8) 0.81020(4) 0.81330(3) 0.0485(3) Uani 1 1 d . . . Ni3 Ni 0.11414(7) 0.82057(3) 0.72267(3) 0.0430(3) Uani 1 1 d . . . Ni4 Ni 0.27636(7) 0.92945(3) 0.76932(3) 0.0447(3) Uani 1 1 d . . . Ni5 Ni 0.38031(7) 0.83002(4) 0.69914(3) 0.0460(3) Uani 1 1 d . . . O1 O 0.0914(4) 0.88836(16) 0.69713(15) 0.0410(10) Uani 1 1 d . . . O2 O 0.2915(3) 0.93735(17) 0.70488(14) 0.0389(9) Uani 1 1 d . . . O3 O 0.2447(4) 0.83961(16) 0.65299(14) 0.0408(10) Uani 1 1 d . . . O4 O 0.2411(4) 0.78295(18) 0.74975(16) 0.0489(11) Uani 1 1 d . . . O5 O 0.2512(4) 0.87320(18) 0.80704(15) 0.0469(11) Uani 1 1 d . . . O6 O 0.4273(4) 0.8464(2) 0.76644(16) 0.0521(12) Uani 1 1 d . . . N1 N 0.0751(4) 0.97166(18) 0.64576(18) 0.0364(11) Uani 1 1 d . . . N2 N -0.0543(5) 1.0047(2) 0.6702(2) 0.0499(14) Uani 1 1 d . . . H2 H -0.1040 1.0077 0.6850 0.060 Uiso 1 1 calc R . . N3 N 0.0122(5) 0.8287(2) 0.7585(2) 0.0496(14) Uani 1 1 d . . . N4 N -0.1120(8) 0.8609(3) 0.7874(4) 0.088(3) Uani 1 1 d . . . H4 H -0.1588 0.8823 0.7921 0.105 Uiso 1 1 calc R . . N5 N 0.2689(4) 0.94361(18) 0.61205(17) 0.0350(11) Uani 1 1 d . . . N6 N 0.4108(4) 0.9914(2) 0.61772(18) 0.0399(12) Uani 1 1 d . . . H6 H 0.4668 1.0096 0.6304 0.048 Uiso 1 1 calc R . . N7 N 0.4017(5) 0.9687(2) 0.7989(2) 0.0537(15) Uani 1 1 d . . . N8 N 0.5343(6) 1.0203(3) 0.8040(2) 0.072(2) Uani 1 1 d . . . H8 H 0.5803 1.0390 0.7950 0.087 Uiso 1 1 calc R . . N9 N 0.0704(4) 0.87229(18) 0.59180(17) 0.0347(10) Uani 1 1 d . . . N10 N 0.0271(5) 0.7981(2) 0.55606(17) 0.0444(13) Uani 1 1 d . . . H10 H 0.0329 0.7666 0.5483 0.053 Uiso 1 1 calc R . . N11 N 0.4070(5) 0.7650(2) 0.6736(2) 0.0562(16) Uani 1 1 d . . . N12 N 0.3813(7) 0.7007(3) 0.6231(2) 0.068(2) Uani 1 1 d . . . H12 H 0.3500 0.6802 0.5999 0.081 Uiso 1 1 calc R . . N13 N 0.4180(5) 0.7431(3) 0.8055(2) 0.0590(17) Uani 1 1 d . . . N14 N 0.4033(7) 0.6708(3) 0.7647(3) 0.070(2) Uani 1 1 d . . . H14 H 0.3775 0.6477 0.7431 0.084 Uiso 1 1 calc R . . N15 N 0.0466(5) 0.7666(2) 0.6807(2) 0.0456(13) Uani 1 1 d . . . N16 N 0.0251(7) 0.6908(2) 0.6475(2) 0.0633(18) Uani 1 1 d . . . H16 H 0.0391 0.6601 0.6400 0.076 Uiso 1 1 calc R . . N17 N 0.2644(5) 0.7911(2) 0.85904(18) 0.0477(14) Uani 1 1 d . . . N18 N 0.1594(7) 0.8175(2) 0.9026(2) 0.065(2) Uani 1 1 d . . . H18 H 0.1157 0.8368 0.9126 0.078 Uiso 1 1 calc R . . N19 N 0.1743(5) 0.9716(2) 0.7874(2) 0.0536(15) Uani 1 1 d . . . N20 N 0.0619(11) 0.9977(3) 0.8261(4) 0.111(4) Uani 1 1 d . . . H20 H 0.0212 0.9976 0.8456 0.133 Uiso 1 1 calc R . . N21 N 0.4727(6) 0.8447(3) 0.8619(2) 0.0613(17) Uani 1 1 d . . . N22 N 0.6193(6) 0.8901(4) 0.8748(2) 0.079(2) Uani 1 1 d . . . H22 H 0.6716 0.9068 0.8687 0.095 Uiso 1 1 calc R . . N23 N 0.4961(5) 0.8663(3) 0.6844(2) 0.0535(15) Uani 1 1 d . . . N24 N 0.6429(6) 0.9114(4) 0.6946(3) 0.082(2) Uani 1 1 d . . . H24 H 0.6992 0.9289 0.7086 0.098 Uiso 1 1 calc R . . C1 C 0.0153(5) 0.9195(2) 0.7018(2) 0.0421(14) Uani 1 1 d . . . C2 C 0.0100(5) 0.9650(2) 0.6729(2) 0.0413(14) Uani 1 1 d . . . C3 C 0.0520(5) 1.0184(2) 0.6243(2) 0.0382(13) Uani 1 1 d . . . C4 C 0.0961(6) 1.0440(2) 0.5926(2) 0.0429(14) Uani 1 1 d . . . H4A H 0.1513 1.0302 0.5815 0.051 Uiso 1 1 calc R . . C5 C 0.0541(6) 1.0910(3) 0.5785(3) 0.0499(16) Uani 1 1 d . . . H5 H 0.0816 1.1096 0.5567 0.060 Uiso 1 1 calc R . . C6 C -0.0247(7) 1.1119(3) 0.5942(3) 0.060(2) Uani 1 1 d . . . H6A H -0.0494 1.1444 0.5832 0.072 Uiso 1 1 calc R . . C7 C -0.0707(6) 1.0869(3) 0.6263(3) 0.0564(19) Uani 1 1 d . . . H7 H -0.1256 1.1009 0.6374 0.068 Uiso 1 1 calc R . . C8 C -0.0286(5) 1.0401(2) 0.6400(3) 0.0477(16) Uani 1 1 d . . . C9 C -0.0504(6) 0.9127(3) 0.7300(3) 0.0544(19) Uani 1 1 d . . . H9 H -0.0989 0.9386 0.7312 0.065 Uiso 1 1 calc R . . C10 C -0.0506(7) 0.8683(3) 0.7583(3) 0.058(2) Uani 1 1 d . . . C11 C -0.0135(7) 0.7935(3) 0.7893(3) 0.0583(19) Uani 1 1 d . . . C12 C 0.0237(8) 0.7459(3) 0.8020(3) 0.064(2) Uani 1 1 d . . . H12A H 0.0770 0.7313 0.7901 0.077 Uiso 1 1 calc R . . C13 C -0.0200(11) 0.7212(4) 0.8326(5) 0.096(4) Uani 1 1 d . . . H13 H 0.0033 0.6880 0.8415 0.116 Uiso 1 1 calc R . . C14 C -0.0950(14) 0.7407(5) 0.8515(6) 0.128(6) Uani 1 1 d . . . H14A H -0.1221 0.7207 0.8725 0.153 Uiso 1 1 calc R . . C15 C -0.1314(12) 0.7873(6) 0.8412(6) 0.118(5) Uani 1 1 d . . . H15 H -0.1823 0.8012 0.8552 0.141 Uiso 1 1 calc R . . C16 C -0.0911(10) 0.8153(4) 0.8085(4) 0.082(3) Uani 1 1 d . . . C17 C 0.3635(5) 0.9661(3) 0.6930(2) 0.0415(14) Uani 1 1 d . . . C18 C 0.3489(5) 0.9674(2) 0.6413(2) 0.0362(13) Uani 1 1 d . . . C19 C 0.2781(5) 0.9518(2) 0.5659(2) 0.0378(13) Uani 1 1 d . . . C20 C 0.2162(5) 0.9360(2) 0.5214(2) 0.0402(14) Uani 1 1 d . . . H20A H 0.1547 0.9166 0.5185 0.048 Uiso 1 1 calc R . . C21 C 0.2479(6) 0.9496(3) 0.4818(2) 0.0468(16) Uani 1 1 d . . . H21 H 0.2079 0.9388 0.4511 0.056 Uiso 1 1 calc R . . C22 C 0.3380(6) 0.9792(3) 0.4853(2) 0.0521(18) Uani 1 1 d . . . H22A H 0.3567 0.9878 0.4569 0.063 Uiso 1 1 calc R . . C23 C 0.3995(6) 0.9960(3) 0.5289(2) 0.0466(15) Uani 1 1 d . . . H23 H 0.4598 1.0163 0.5316 0.056 Uiso 1 1 calc R . . C24 C 0.3665(5) 0.9808(2) 0.5690(2) 0.0385(13) Uani 1 1 d . . . C25 C 0.4406(6) 0.9917(3) 0.7233(2) 0.0503(17) Uani 1 1 d . . . H25 H 0.4858 1.0109 0.7098 0.060 Uiso 1 1 calc R . . C26 C 0.4605(6) 0.9924(3) 0.7747(2) 0.0525(18) Uani 1 1 d . . . C27 C 0.4418(7) 0.9833(3) 0.8468(2) 0.063(2) Uani 1 1 d . . . C28 C 0.4093(9) 0.9706(4) 0.8871(3) 0.082(3) Uani 1 1 d . . . H28 H 0.3515 0.9489 0.8854 0.099 Uiso 1 1 calc R . . C29 C 0.4675(12) 0.9917(4) 0.9300(3) 0.097(4) Uani 1 1 d . . . H29 H 0.4486 0.9832 0.9584 0.117 Uiso 1 1 calc R . . C30 C 0.5472(11) 1.0228(5) 0.9340(3) 0.102(4) Uani 1 1 d . . . H30 H 0.5792 1.0374 0.9644 0.122 Uiso 1 1 calc R . . C31 C 0.5878(11) 1.0356(5) 0.8934(3) 0.102(4) Uani 1 1 d . . . H31 H 0.6487 1.0555 0.8962 0.122 Uiso 1 1 calc R . . C32 C 0.5281(8) 1.0156(4) 0.8500(3) 0.067(2) Uani 1 1 d . . . C33 C 0.2017(6) 0.8073(2) 0.6181(2) 0.0462(16) Uani 1 1 d . . . C34 C 0.0989(5) 0.8247(2) 0.5887(2) 0.0390(13) Uani 1 1 d . . . C35 C -0.0284(5) 0.8765(2) 0.5593(2) 0.0365(12) Uani 1 1 d . . . C36 C -0.0948(5) 0.9176(2) 0.5474(2) 0.0417(14) Uani 1 1 d . . . H36 H -0.0763 0.9496 0.5615 0.050 Uiso 1 1 calc R . . C37 C -0.1917(6) 0.9088(3) 0.5130(3) 0.0542(18) Uani 1 1 d . . . H37 H -0.2393 0.9359 0.5031 0.065 Uiso 1 1 calc R . . C38 C -0.2188(6) 0.8620(3) 0.4934(3) 0.0553(18) Uani 1 1 d . . . H38 H -0.2859 0.8577 0.4714 0.066 Uiso 1 1 calc R . . C39 C -0.1526(6) 0.8211(3) 0.5045(2) 0.0513(17) Uani 1 1 d . . . H39 H -0.1720 0.7892 0.4904 0.062 Uiso 1 1 calc R . . C40 C -0.0576(6) 0.8292(2) 0.5369(2) 0.0425(14) Uani 1 1 d . . . C41 C 0.2407(6) 0.7628(3) 0.6091(2) 0.0484(16) Uani 1 1 d . . . H41 H 0.1992 0.7431 0.5836 0.058 Uiso 1 1 calc R . . C42 C 0.3402(7) 0.7432(3) 0.6354(2) 0.058(2) Uani 1 1 d . . . C43 C 0.4976(7) 0.7366(4) 0.6849(3) 0.066(2) Uani 1 1 d . . . C44 C 0.5908(7) 0.7410(4) 0.7201(3) 0.075(3) Uani 1 1 d . . . H44 H 0.5991 0.7681 0.7421 0.091 Uiso 1 1 calc R . . C45 C 0.6719(9) 0.7082(6) 0.7246(4) 0.103(4) Uani 1 1 d . . . H45 H 0.7379 0.7124 0.7476 0.123 Uiso 1 1 calc R . . C46 C 0.6481(11) 0.6644(6) 0.6900(5) 0.102(4) Uani 1 1 d . . . H46 H 0.7005 0.6394 0.6931 0.122 Uiso 1 1 calc R . . C47 C 0.5599(12) 0.6587(5) 0.6560(5) 0.109(5) Uani 1 1 d . . . H47 H 0.5496 0.6314 0.6342 0.131 Uiso 1 1 calc R . . C48 C 0.4816(8) 0.6950(4) 0.6534(3) 0.074(3) Uani 1 1 d . . . C49 C 0.2576(6) 0.7347(3) 0.7404(2) 0.0486(16) Uani 1 1 d . . . C50 C 0.3575(7) 0.7151(3) 0.7699(3) 0.059(2) Uani 1 1 d . . . C51 C 0.5054(7) 0.7158(5) 0.8247(3) 0.080(3) Uani 1 1 d . . . C52 C 0.5931(8) 0.7275(5) 0.8634(4) 0.091(4) Uani 1 1 d . . . H52 H 0.6002 0.7577 0.8813 0.109 Uiso 1 1 calc R . . C53 C 0.6723(10) 0.6871(8) 0.8728(6) 0.126(7) Uani 1 1 d . . . H53 H 0.7345 0.6914 0.8981 0.151 Uiso 1 1 calc R . . C54 C 0.6599(12) 0.6434(7) 0.8462(6) 0.116(6) Uani 1 1 d . . . H54 H 0.7143 0.6191 0.8541 0.139 Uiso 1 1 calc R . . C55 C 0.5775(10) 0.6338(5) 0.8108(5) 0.105(4) Uani 1 1 d . . . H55 H 0.5729 0.6034 0.7933 0.126 Uiso 1 1 calc R . . C56 C 0.4962(9) 0.6687(5) 0.7990(4) 0.083(3) Uani 1 1 d . . . C57 C 0.1899(6) 0.7058(3) 0.7063(2) 0.0501(16) Uani 1 1 d . . . H57 H 0.2113 0.6727 0.7015 0.060 Uiso 1 1 calc R . . C58 C 0.0921(7) 0.7217(3) 0.6784(2) 0.0549(18) Uani 1 1 d . . . C59 C -0.0535(6) 0.7640(3) 0.6507(2) 0.0465(15) Uani 1 1 d . . . C60 C -0.1356(6) 0.7982(3) 0.6404(3) 0.0526(17) Uani 1 1 d . . . H60 H -0.1273 0.8306 0.6545 0.063 Uiso 1 1 calc R . . C61 C -0.2309(8) 0.7837(4) 0.6088(3) 0.077(3) Uani 1 1 d . . . H61 H -0.2876 0.8068 0.6010 0.092 Uiso 1 1 calc R . . C62 C -0.2438(9) 0.7370(5) 0.5888(4) 0.092(3) Uani 1 1 d . . . H62 H -0.3094 0.7280 0.5674 0.110 Uiso 1 1 calc R . . C63 C -0.1639(10) 0.7029(4) 0.5992(4) 0.089(4) Uani 1 1 d . . . H63 H -0.1741 0.6704 0.5853 0.106 Uiso 1 1 calc R . . C64 C -0.0689(7) 0.7156(3) 0.6297(3) 0.061(2) Uani 1 1 d . . . C65 C 0.1949(7) 0.8742(3) 0.8388(2) 0.0539(18) Uani 1 1 d . . . C66 C 0.2068(6) 0.8280(3) 0.8671(2) 0.0519(18) Uani 1 1 d . . . C67 C 0.2616(6) 0.7536(3) 0.8912(2) 0.0525(17) Uani 1 1 d . . . C68 C 0.3093(6) 0.7082(3) 0.8997(2) 0.0554(18) Uani 1 1 d . . . H68 H 0.3543 0.6966 0.8814 0.067 Uiso 1 1 calc R . . C69 C 0.2893(7) 0.6790(3) 0.9367(3) 0.064(2) Uani 1 1 d . . . H69 H 0.3187 0.6464 0.9422 0.077 Uiso 1 1 calc R . . C70 C 0.2294(8) 0.6960(4) 0.9649(3) 0.069(3) Uani 1 1 d . . . H70 H 0.2222 0.6759 0.9909 0.083 Uiso 1 1 calc R . . C71 C 0.1785(9) 0.7419(3) 0.9565(3) 0.069(2) Uani 1 1 d . . . H71 H 0.1347 0.7531 0.9755 0.082 Uiso 1 1 calc R . . C72 C 0.1941(7) 0.7707(3) 0.9195(3) 0.062(2) Uani 1 1 d . . . C73 C 0.1347(9) 0.9123(3) 0.8462(3) 0.070(3) Uani 1 1 d . . . H73 H 0.0985 0.9085 0.8702 0.084 Uiso 1 1 calc R . . C74 C 0.1219(9) 0.9597(3) 0.8193(3) 0.070(3) Uani 1 1 d . . . C75 C 0.1425(7) 1.0207(3) 0.7733(3) 0.0564(19) Uani 1 1 d . . . C76 C 0.1753(6) 1.0519(3) 0.7410(2) 0.0516(17) Uani 1 1 d . . . H76 H 0.2251 1.0411 0.7249 0.062 Uiso 1 1 calc R . . C77 C 0.1305(8) 1.0997(3) 0.7339(3) 0.062(2) Uani 1 1 d . . . H77 H 0.1509 1.1224 0.7128 0.075 Uiso 1 1 calc R . . C78 C 0.0566(12) 1.1144(4) 0.7572(4) 0.095(4) Uani 1 1 d . . . H78 H 0.0257 1.1467 0.7511 0.114 Uiso 1 1 calc R . . C79 C 0.0274(15) 1.0832(4) 0.7889(6) 0.130(7) Uani 1 1 d . . . H79 H -0.0239 1.0932 0.8045 0.155 Uiso 1 1 calc R . . C80 C 0.0746(11) 1.0373(3) 0.7974(4) 0.089(4) Uani 1 1 d . . . C81 C 0.5201(7) 0.8670(4) 0.7892(3) 0.067(2) Uani 1 1 d . . . C82 C 0.5384(7) 0.8678(4) 0.8411(3) 0.069(2) Uani 1 1 d . . . C83 C 0.5106(8) 0.8530(4) 0.9109(3) 0.071(2) Uani 1 1 d . . . C84 C 0.4749(9) 0.8377(4) 0.9490(3) 0.080(3) Uani 1 1 d . . . H84 H 0.4130 0.8182 0.9445 0.096 Uiso 1 1 calc R . . C85 C 0.5346(10) 0.8525(5) 0.9947(3) 0.094(4) Uani 1 1 d . . . H85 H 0.5118 0.8428 1.0218 0.113 Uiso 1 1 calc R . . C86 C 0.6225(12) 0.8798(6) 1.0017(3) 0.116(5) Uani 1 1 d . . . H86 H 0.6599 0.8885 1.0335 0.139 Uiso 1 1 calc R . . C87 C 0.6601(10) 0.8954(6) 0.9645(3) 0.102(4) Uani 1 1 d . . . H87 H 0.7223 0.9150 0.9702 0.122 Uiso 1 1 calc R . . C88 C 0.6056(8) 0.8821(5) 0.9187(3) 0.084(3) Uani 1 1 d . . . C89 C 0.5865(7) 0.8888(4) 0.7670(3) 0.073(3) Uani 1 1 d . . . H89 H 0.6462 0.9054 0.7866 0.088 Uiso 1 1 calc R . . C90 C 0.5742(6) 0.8888(4) 0.7172(3) 0.062(2) Uani 1 1 d . . . C91 C 0.5139(6) 0.8730(3) 0.6398(3) 0.0563(19) Uani 1 1 d . . . C92 C 0.4577(8) 0.8575(4) 0.5943(3) 0.066(2) Uani 1 1 d . . . H92 H 0.3936 0.8396 0.5893 0.079 Uiso 1 1 calc R . . C93 C 0.4981(7) 0.8690(4) 0.5570(3) 0.068(2) Uani 1 1 d . . . H93 H 0.4631 0.8572 0.5259 0.081 Uiso 1 1 calc R . . C94 C 0.5912(9) 0.8983(5) 0.5632(4) 0.091(4) Uani 1 1 d . . . H94 H 0.6145 0.9073 0.5361 0.109 Uiso 1 1 calc R . . C95 C 0.6446(9) 0.9127(5) 0.6062(5) 0.096(4) Uani 1 1 d . . . H95 H 0.7084 0.9306 0.6104 0.115 Uiso 1 1 calc R . . C96 C 0.6067(8) 0.9014(4) 0.6463(4) 0.078(3) Uani 1 1 d . . . I1A I 0.37295(9) 0.57118(4) 0.85795(5) 0.0817(5) Uani 0.605(3) 1 d P A 1 I1B I 0.31777(12) 0.53641(7) 0.83114(7) 0.0783(7) Uani 0.395(3) 1 d P A 2 I2A I 0.0837(2) 0.44164(11) 0.44225(7) 0.1847(10) Uani 0.75 1 d P . . I2B I 0.1793(12) 0.5341(6) 0.4731(4) 0.237(9) Uani 0.15 1 d P . . I2C I 0.107(3) 0.4820(6) 0.4566(9) 0.32(2) Uani 0.10 1 d P . . I3A I 0.24180(14) 0.63100(6) 0.52522(5) 0.0838(5) Uani 0.45 1 d P . . I3B I 0.2904(7) 0.5833(2) 0.7073(3) 0.202(4) Uani 0.25 1 d P . . I3C I 0.1423(11) 0.6022(3) 0.6288(5) 0.203(5) Uani 0.18 1 d P . . I3D I 0.2265(16) 0.6413(6) 0.5584(5) 0.193(6) Uani 0.12 1 d P . . I4A I 0.82827(10) 0.53707(5) 0.35665(7) 0.1234(6) Uani 0.70 1 d P . . I4B I -0.0497(5) 0.68333(18) 0.5052(2) 0.1158(19) Uani 0.20 1 d P . . I4C I 0.0200(14) 0.6952(5) 0.5286(5) 0.130(4) Uani 0.10 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0337(4) 0.0333(4) 0.0298(4) -0.0002(3) 0.0089(3) -0.0005(3) Ni2 0.0478(6) 0.0667(6) 0.0291(4) 0.0057(4) 0.0069(4) -0.0092(4) Ni3 0.0493(6) 0.0372(5) 0.0422(5) -0.0009(3) 0.0120(4) -0.0024(3) Ni4 0.0528(6) 0.0518(5) 0.0333(4) -0.0045(3) 0.0179(4) -0.0155(4) Ni5 0.0433(5) 0.0582(6) 0.0352(4) 0.0092(4) 0.0087(4) 0.0073(4) O1 0.048(3) 0.034(2) 0.045(2) -0.0001(18) 0.019(2) 0.0001(18) O2 0.039(2) 0.050(2) 0.0295(19) -0.0028(17) 0.0121(17) -0.0114(19) O3 0.045(3) 0.042(2) 0.0305(19) -0.0056(17) 0.0032(18) 0.0081(19) O4 0.052(3) 0.050(3) 0.039(2) -0.001(2) 0.004(2) 0.009(2) O5 0.060(3) 0.050(3) 0.036(2) -0.0029(19) 0.020(2) -0.012(2) O6 0.041(3) 0.076(3) 0.037(2) 0.008(2) 0.008(2) -0.013(2) N1 0.035(3) 0.034(2) 0.040(2) -0.004(2) 0.009(2) -0.005(2) N2 0.047(3) 0.038(3) 0.074(4) -0.008(3) 0.031(3) -0.002(2) N3 0.058(4) 0.043(3) 0.056(3) -0.002(3) 0.029(3) -0.018(3) N4 0.103(7) 0.064(5) 0.126(7) -0.015(5) 0.082(6) -0.020(4) N5 0.038(3) 0.037(3) 0.031(2) 0.0054(19) 0.011(2) 0.005(2) N6 0.031(3) 0.055(3) 0.035(2) 0.003(2) 0.012(2) -0.011(2) N7 0.065(4) 0.065(4) 0.036(3) -0.010(3) 0.021(3) -0.023(3) N8 0.076(5) 0.096(5) 0.041(3) -0.011(3) 0.011(3) -0.049(4) N9 0.036(3) 0.034(2) 0.035(2) 0.0007(19) 0.011(2) 0.006(2) N10 0.065(4) 0.034(3) 0.031(2) 0.005(2) 0.006(2) -0.002(2) N11 0.060(4) 0.059(4) 0.048(3) 0.017(3) 0.014(3) 0.024(3) N12 0.092(6) 0.057(4) 0.057(4) 0.010(3) 0.027(4) 0.037(4) N13 0.058(4) 0.079(4) 0.038(3) 0.027(3) 0.010(3) 0.014(3) N14 0.077(5) 0.074(5) 0.061(4) 0.023(3) 0.020(4) 0.030(4) N15 0.051(3) 0.038(3) 0.045(3) 0.008(2) 0.008(2) 0.000(2) N16 0.087(5) 0.036(3) 0.059(4) -0.003(3) 0.006(4) -0.005(3) N17 0.050(3) 0.065(4) 0.029(2) 0.004(2) 0.012(2) -0.014(3) N18 0.106(6) 0.051(4) 0.049(3) 0.000(3) 0.040(4) -0.012(4) N19 0.061(4) 0.060(4) 0.044(3) -0.012(3) 0.020(3) -0.018(3) N20 0.206(12) 0.059(5) 0.118(7) 0.005(5) 0.129(9) 0.019(6) N21 0.058(4) 0.081(5) 0.038(3) 0.009(3) 0.001(3) -0.021(3) N22 0.057(4) 0.119(7) 0.053(4) 0.008(4) 0.000(3) -0.030(4) N23 0.044(3) 0.072(4) 0.045(3) 0.019(3) 0.015(3) 0.013(3) N24 0.041(4) 0.121(7) 0.087(5) 0.027(5) 0.022(4) -0.012(4) C1 0.041(4) 0.041(3) 0.050(3) -0.012(3) 0.021(3) -0.005(3) C2 0.035(3) 0.034(3) 0.057(4) -0.012(3) 0.017(3) -0.008(2) C3 0.039(3) 0.030(3) 0.041(3) -0.008(2) 0.003(3) -0.001(2) C4 0.047(4) 0.035(3) 0.044(3) 0.003(3) 0.009(3) -0.003(3) C5 0.056(4) 0.038(3) 0.055(4) 0.004(3) 0.014(3) -0.001(3) C6 0.060(5) 0.037(3) 0.073(5) 0.004(3) 0.000(4) 0.008(3) C7 0.045(4) 0.041(4) 0.081(5) -0.004(4) 0.014(4) 0.006(3) C8 0.037(4) 0.038(3) 0.065(4) -0.014(3) 0.009(3) -0.001(3) C9 0.055(5) 0.042(4) 0.079(5) 0.000(3) 0.040(4) -0.006(3) C10 0.073(5) 0.043(4) 0.073(5) -0.007(3) 0.043(4) -0.013(4) C11 0.066(5) 0.047(4) 0.067(5) 0.003(3) 0.027(4) -0.019(4) C12 0.088(6) 0.045(4) 0.061(4) 0.001(3) 0.021(4) -0.022(4) C13 0.123(10) 0.058(5) 0.107(8) 0.027(6) 0.030(7) -0.018(6) C14 0.170(15) 0.091(9) 0.171(14) 0.022(9) 0.129(13) -0.026(9) C15 0.122(11) 0.104(10) 0.164(13) 0.015(9) 0.099(11) -0.029(8) C16 0.108(8) 0.063(5) 0.095(7) 0.010(5) 0.065(7) -0.024(5) C17 0.042(4) 0.056(4) 0.027(3) -0.004(3) 0.010(3) -0.006(3) C18 0.035(3) 0.048(3) 0.030(3) -0.007(2) 0.016(2) -0.009(3) C19 0.041(3) 0.044(3) 0.029(3) 0.000(2) 0.010(2) 0.007(3) C20 0.044(4) 0.047(3) 0.029(3) 0.001(2) 0.008(3) 0.005(3) C21 0.055(4) 0.055(4) 0.028(3) 0.000(3) 0.008(3) 0.008(3) C22 0.060(5) 0.069(5) 0.031(3) 0.007(3) 0.019(3) 0.019(4) C23 0.041(4) 0.062(4) 0.041(3) 0.005(3) 0.018(3) 0.008(3) C24 0.039(3) 0.047(3) 0.032(3) 0.007(2) 0.014(2) 0.008(3) C25 0.049(4) 0.063(4) 0.040(3) -0.001(3) 0.015(3) -0.019(3) C26 0.061(5) 0.067(5) 0.031(3) -0.008(3) 0.015(3) -0.031(4) C27 0.080(6) 0.076(5) 0.033(3) -0.010(3) 0.015(3) -0.038(4) C28 0.109(8) 0.099(7) 0.044(4) -0.018(4) 0.029(5) -0.053(6) C29 0.162(12) 0.102(8) 0.040(4) -0.012(4) 0.047(6) -0.052(8) C30 0.128(10) 0.132(10) 0.044(4) -0.033(5) 0.021(5) -0.075(8) C31 0.143(11) 0.115(9) 0.039(4) -0.011(5) 0.011(5) -0.071(8) C32 0.083(6) 0.081(6) 0.036(3) -0.011(4) 0.014(4) -0.025(5) C33 0.066(5) 0.033(3) 0.036(3) 0.008(2) 0.009(3) 0.012(3) C34 0.047(4) 0.034(3) 0.032(3) 0.005(2) 0.005(3) 0.005(3) C35 0.034(3) 0.041(3) 0.036(3) 0.006(2) 0.011(2) -0.004(2) C36 0.034(3) 0.043(3) 0.047(3) -0.002(3) 0.010(3) 0.002(3) C37 0.042(4) 0.070(5) 0.049(4) -0.009(3) 0.011(3) 0.011(3) C38 0.040(4) 0.078(5) 0.046(4) -0.004(4) 0.008(3) -0.011(4) C39 0.050(4) 0.055(4) 0.044(3) -0.007(3) 0.005(3) -0.018(3) C40 0.047(4) 0.047(3) 0.036(3) -0.003(3) 0.015(3) -0.011(3) C41 0.068(5) 0.040(3) 0.036(3) -0.002(3) 0.012(3) 0.016(3) C42 0.079(6) 0.057(4) 0.038(3) 0.008(3) 0.016(4) 0.025(4) C43 0.066(5) 0.088(6) 0.050(4) 0.021(4) 0.027(4) 0.029(5) C44 0.062(5) 0.105(7) 0.067(5) 0.034(5) 0.030(4) 0.032(5) C45 0.072(7) 0.150(12) 0.085(7) 0.053(8) 0.020(6) 0.057(7) C46 0.098(9) 0.122(10) 0.088(7) 0.035(7) 0.031(7) 0.057(8) C47 0.123(11) 0.108(9) 0.108(9) 0.051(7) 0.054(9) 0.080(8) C48 0.078(6) 0.090(6) 0.060(5) 0.027(5) 0.028(5) 0.045(5) C49 0.063(5) 0.045(4) 0.038(3) 0.005(3) 0.014(3) 0.008(3) C50 0.061(5) 0.072(5) 0.045(4) 0.014(4) 0.013(4) 0.019(4) C51 0.053(5) 0.133(9) 0.055(4) 0.057(6) 0.017(4) 0.029(5) C52 0.061(6) 0.144(10) 0.065(5) 0.049(6) 0.010(4) 0.002(6) C53 0.055(7) 0.210(19) 0.112(10) 0.108(12) 0.021(7) 0.030(9) C54 0.077(9) 0.146(13) 0.130(12) 0.081(11) 0.038(9) 0.048(9) C55 0.087(8) 0.126(10) 0.113(9) 0.066(8) 0.048(8) 0.060(7) C56 0.080(7) 0.103(8) 0.076(6) 0.045(6) 0.038(5) 0.035(6) C57 0.060(5) 0.045(4) 0.048(4) 0.004(3) 0.019(3) 0.012(3) C58 0.084(6) 0.039(3) 0.042(3) 0.004(3) 0.018(4) 0.003(3) C59 0.050(4) 0.043(3) 0.042(3) 0.003(3) 0.006(3) -0.016(3) C60 0.059(5) 0.042(3) 0.048(4) 0.008(3) 0.002(3) -0.008(3) C61 0.056(5) 0.095(7) 0.071(5) 0.020(5) 0.003(4) -0.013(5) C62 0.077(7) 0.096(8) 0.082(6) 0.011(6) -0.012(5) -0.032(6) C63 0.119(9) 0.056(5) 0.069(5) 0.006(4) -0.012(6) -0.037(6) C64 0.078(6) 0.042(4) 0.056(4) 0.001(3) 0.007(4) -0.013(4) C65 0.078(5) 0.050(4) 0.042(3) -0.006(3) 0.029(4) -0.020(4) C66 0.064(5) 0.060(4) 0.038(3) -0.008(3) 0.024(3) -0.025(4) C67 0.058(4) 0.059(4) 0.039(3) -0.001(3) 0.011(3) -0.022(3) C68 0.057(5) 0.067(5) 0.039(3) 0.007(3) 0.008(3) -0.017(4) C69 0.069(6) 0.065(5) 0.052(4) 0.011(4) 0.005(4) -0.020(4) C70 0.089(7) 0.078(6) 0.045(4) 0.006(4) 0.025(4) -0.037(5) C71 0.108(7) 0.053(5) 0.058(4) -0.002(4) 0.044(5) -0.021(5) C72 0.077(6) 0.062(5) 0.048(4) -0.004(3) 0.019(4) -0.021(4) C73 0.113(8) 0.054(4) 0.061(5) -0.015(4) 0.057(5) -0.019(5) C74 0.115(8) 0.045(4) 0.072(5) -0.003(4) 0.061(6) -0.003(4) C75 0.076(5) 0.044(4) 0.055(4) -0.010(3) 0.028(4) -0.012(4) C76 0.058(5) 0.056(4) 0.039(3) -0.007(3) 0.012(3) -0.009(3) C77 0.083(6) 0.048(4) 0.058(4) -0.005(3) 0.023(4) -0.014(4) C78 0.172(12) 0.047(5) 0.090(7) 0.007(5) 0.076(8) 0.018(6) C79 0.230(18) 0.056(6) 0.162(13) 0.003(7) 0.155(14) 0.028(8) C80 0.162(11) 0.048(5) 0.087(6) -0.006(4) 0.085(8) -0.007(6) C81 0.052(5) 0.098(7) 0.044(4) 0.022(4) 0.003(3) -0.005(4) C82 0.050(5) 0.106(7) 0.045(4) 0.010(4) 0.002(3) -0.027(4) C83 0.072(6) 0.096(7) 0.035(3) 0.006(4) -0.003(3) -0.013(5) C84 0.097(8) 0.093(7) 0.041(4) -0.004(4) 0.004(4) -0.020(6) C85 0.094(8) 0.141(10) 0.037(4) 0.007(5) 0.001(4) -0.030(7) C86 0.133(12) 0.148(12) 0.042(5) -0.019(6) -0.019(6) -0.023(9) C87 0.088(8) 0.150(11) 0.051(5) -0.011(6) -0.010(5) -0.048(8) C88 0.071(6) 0.113(8) 0.058(5) 0.003(5) 0.001(4) -0.030(6) C89 0.044(5) 0.111(7) 0.060(5) 0.016(5) 0.005(4) -0.018(5) C90 0.043(4) 0.094(6) 0.053(4) 0.020(4) 0.019(3) 0.015(4) C91 0.041(4) 0.079(5) 0.054(4) 0.015(4) 0.021(3) 0.020(4) C92 0.071(5) 0.080(6) 0.051(4) 0.026(4) 0.024(4) 0.036(5) C93 0.072(6) 0.087(6) 0.057(4) 0.026(4) 0.037(4) 0.030(5) C94 0.085(8) 0.128(9) 0.075(6) 0.039(6) 0.050(6) 0.037(7) C95 0.073(7) 0.136(10) 0.099(9) 0.035(7) 0.058(7) 0.011(6) C96 0.070(6) 0.103(7) 0.072(6) 0.030(5) 0.040(5) 0.018(5) I1A 0.0693(8) 0.0618(7) 0.1294(11) 0.0052(6) 0.0530(7) 0.0117(5) I1B 0.0473(9) 0.0880(13) 0.1109(14) 0.0081(9) 0.0409(9) 0.0078(7) I2A 0.188(2) 0.211(2) 0.1282(13) 0.0216(14) -0.0020(13) 0.0685(18) I2B 0.273(15) 0.320(17) 0.135(7) 0.113(10) 0.087(9) 0.206(15) I2C 0.52(5) 0.094(8) 0.24(2) -0.099(12) -0.10(3) 0.036(16) I3A 0.1107(12) 0.0770(9) 0.0659(8) 0.0174(7) 0.0278(8) 0.0389(8) I3B 0.272(9) 0.111(3) 0.297(9) 0.035(4) 0.205(8) 0.061(4) I3C 0.281(13) 0.113(5) 0.265(12) 0.010(6) 0.159(11) 0.021(6) I3D 0.249(17) 0.203(14) 0.115(7) -0.013(8) 0.031(9) 0.059(12) I4A 0.0773(8) 0.1075(9) 0.1986(16) 0.0558(9) 0.0598(9) 0.0264(6) I4B 0.125(4) 0.094(3) 0.152(4) -0.072(3) 0.078(4) -0.047(3) I4C 0.190(14) 0.104(7) 0.122(8) -0.009(6) 0.087(9) 0.008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.027(5) . y Ni1 N9 2.032(5) . y Ni1 N1 2.035(5) . y Ni1 O1 2.126(4) . y Ni1 O2 2.131(4) . y Ni1 O3 2.146(4) . y Ni2 N13 2.035(7) . y Ni2 N17 2.043(5) . y Ni2 N21 2.045(7) . y Ni2 O5 2.119(5) . y Ni2 O6 2.128(5) . y Ni2 O4 2.144(5) . y Ni3 N3 1.926(6) . y Ni3 O4 1.932(5) . y Ni3 N15 1.941(6) . y Ni3 O1 1.947(4) . y Ni4 N19 1.937(7) . y Ni4 O5 1.938(4) . y Ni4 O2 1.943(4) . y Ni4 N7 1.953(6) . y Ni5 O6 1.929(5) . y Ni5 O3 1.942(4) . y Ni5 N23 1.955(7) . y Ni5 N11 1.956(7) . y Ni1 Ni3 3.509(1) . Y Ni1 Ni4 3.515(1) . Y Ni1 Ni5 3.548(1) . Y Ni1 Ni2 5.514(1) . Y Ni2 Ni4 3.472(1) . Y Ni2 Ni5 3.473(1) . Y Ni2 Ni3 3.517(1) . Y Ni3 Ni4 3.648(1) . Y Ni3 Ni5 3.775(1) . Y Ni4 Ni5 3.820(1) . Y O1 C1 1.342(8) . ? O2 C17 1.339(8) . ? O3 C33 1.333(8) . ? O4 C49 1.345(8) . ? O5 C65 1.332(8) . ? O6 C81 1.344(10) . ? N1 C2 1.326(8) . ? N1 C3 1.391(8) . ? N2 C2 1.349(9) . ? N2 C8 1.391(10) . ? N2 H2 0.8800 . ? N3 C10 1.345(11) . ? N3 C11 1.398(9) . ? N4 C10 1.335(10) . ? N4 C16 1.357(14) . ? N4 H4 0.8800 . ? N5 C18 1.325(8) . ? N5 C19 1.392(7) . ? N6 C18 1.361(8) . ? N6 C24 1.403(8) . ? N6 H6 0.8800 . ? N7 C26 1.339(9) . ? N7 C27 1.401(9) . ? N8 C26 1.335(10) . ? N8 C32 1.363(10) . ? N8 H8 0.8800 . ? N9 C34 1.335(8) . ? N9 C35 1.393(8) . ? N10 C34 1.348(9) . ? N10 C40 1.382(9) . ? N10 H10 0.8800 . ? N11 C42 1.348(11) . ? N11 C43 1.381(10) . ? N12 C42 1.347(10) . ? N12 C48 1.388(13) . ? N12 H12 0.8800 . ? N13 C50 1.347(12) . ? N13 C51 1.353(11) . ? N14 C56 1.355(14) . ? N14 C50 1.357(11) . ? N14 H14 0.8800 . ? N15 C58 1.351(9) . ? N15 C59 1.375(9) . ? N16 C58 1.356(11) . ? N16 C64 1.381(12) . ? N16 H16 0.8800 . ? N17 C66 1.306(11) . ? N17 C67 1.375(9) . ? N18 C66 1.371(9) . ? N18 C72 1.375(12) . ? N18 H18 0.8800 . ? N19 C74 1.336(10) . ? N19 C75 1.404(11) . ? N20 C74 1.336(13) . ? N20 C80 1.383(12) . ? N20 H20 0.8800 . ? N21 C82 1.337(11) . ? N21 C83 1.390(10) . ? N22 C88 1.351(12) . ? N22 C82 1.374(11) . ? N22 H22 0.8800 . ? N23 C90 1.342(12) . ? N23 C91 1.387(9) . ? N24 C96 1.376(14) . ? N24 C90 1.394(11) . ? N24 H24 0.8800 . ? C1 C9 1.358(10) . ? C1 C2 1.466(10) . ? C3 C4 1.393(10) . ? C3 C8 1.394(10) . ? C4 C5 1.390(10) . ? C4 H4A 0.9500 . ? C5 C6 1.366(12) . ? C5 H5 0.9500 . ? C6 C7 1.410(12) . ? C6 H6A 0.9500 . ? C7 C8 1.382(10) . ? C7 H7 0.9500 . ? C9 C10 1.442(11) . ? C9 H9 0.9500 . ? C11 C12 1.375(12) . ? C11 C16 1.420(14) . ? C12 C13 1.354(14) . ? C12 H12A 0.9500 . ? C13 C14 1.361(19) . ? C13 H13 0.9500 . ? C14 C15 1.34(2) . ? C14 H14A 0.9500 . ? C15 C16 1.418(14) . ? C15 H15 0.9500 . ? C17 C25 1.339(10) . ? C17 C18 1.458(8) . ? C19 C24 1.387(10) . ? C19 C20 1.394(9) . ? C20 C21 1.372(9) . ? C20 H20A 0.9500 . ? C21 C22 1.410(12) . ? C21 H21 0.9500 . ? C22 C23 1.377(11) . ? C22 H22A 0.9500 . ? C23 C24 1.408(9) . ? C23 H23 0.9500 . ? C25 C26 1.440(9) . ? C25 H25 0.9500 . ? C27 C28 1.392(11) . ? C27 C32 1.415(12) . ? C28 C29 1.392(13) . ? C28 H28 0.9500 . ? C29 C30 1.323(15) . ? C29 H29 0.9500 . ? C30 C31 1.461(14) . ? C30 H30 0.9500 . ? C31 C32 1.398(12) . ? C31 H31 0.9500 . ? C33 C41 1.349(9) . ? C33 C34 1.471(10) . ? C35 C36 1.388(9) . ? C35 C40 1.425(9) . ? C36 C37 1.415(10) . ? C36 H36 0.9500 . ? C37 C38 1.378(12) . ? C37 H37 0.9500 . ? C38 C39 1.382(12) . ? C38 H38 0.9500 . ? C39 C40 1.367(10) . ? C39 H39 0.9500 . ? C41 C42 1.429(11) . ? C41 H41 0.9500 . ? C43 C44 1.376(14) . ? C43 C48 1.416(15) . ? C44 C45 1.365(14) . ? C44 H44 0.9500 . ? C45 C46 1.52(2) . ? C45 H45 0.9500 . ? C46 C47 1.32(2) . ? C46 H46 0.9500 . ? C47 C48 1.405(13) . ? C47 H47 0.9500 . ? C49 C57 1.376(11) . ? C49 C50 1.462(11) . ? C51 C52 1.413(16) . ? C51 C56 1.451(18) . ? C52 C53 1.48(2) . ? C52 H52 0.9500 . ? C53 C54 1.38(2) . ? C53 H53 0.9500 . ? C54 C55 1.30(2) . ? C54 H54 0.9500 . ? C55 C56 1.394(14) . ? C55 H55 0.9500 . ? C57 C58 1.393(11) . ? C57 H57 0.9500 . ? C59 C60 1.387(11) . ? C59 C64 1.418(10) . ? C60 C61 1.397(12) . ? C60 H60 0.9500 . ? C61 C62 1.366(16) . ? C61 H61 0.9500 . ? C62 C63 1.366(18) . ? C62 H62 0.9500 . ? C63 C64 1.370(14) . ? C63 H63 0.9500 . ? C65 C73 1.345(13) . ? C65 C66 1.466(11) . ? C67 C68 1.358(12) . ? C67 C72 1.441(12) . ? C68 C69 1.407(11) . ? C68 H68 0.9500 . ? C69 C70 1.362(14) . ? C69 H69 0.9500 . ? C70 C71 1.387(14) . ? C70 H70 0.9500 . ? C71 C72 1.378(11) . ? C71 H71 0.9500 . ? C73 C74 1.470(12) . ? C73 H73 0.9500 . ? C75 C80 1.353(13) . ? C75 C76 1.407(11) . ? C76 C77 1.397(12) . ? C76 H76 0.9500 . ? C77 C78 1.389(14) . ? C77 H77 0.9500 . ? C78 C79 1.370(15) . ? C78 H78 0.9500 . ? C79 C80 1.366(16) . ? C79 H79 0.9500 . ? C81 C89 1.353(12) . ? C81 C82 1.456(11) . ? C83 C84 1.375(13) . ? C83 C88 1.443(14) . ? C84 C85 1.403(13) . ? C84 H84 0.9500 . ? C85 C86 1.341(18) . ? C85 H85 0.9500 . ? C86 C87 1.371(18) . ? C86 H86 0.9500 . ? C87 C88 1.374(13) . ? C87 H87 0.9500 . ? C89 C90 1.408(12) . ? C89 H89 0.9500 . ? C91 C92 1.389(13) . ? C91 C96 1.414(14) . ? C92 C93 1.363(11) . ? C92 H92 0.9500 . ? C93 C94 1.428(17) . ? C93 H93 0.9500 . ? C94 C95 1.313(19) . ? C94 H94 0.9500 . ? C95 C96 1.417(13) . ? C95 H95 0.9500 . ? 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 N5 Ni1 N9 102.7(2) . . y N5 Ni1 N1 98.5(2) . . y N9 Ni1 N1 98.1(2) . . y N5 Ni1 O1 164.2(2) . . y N9 Ni1 O1 93.1(2) . . y N1 Ni1 O1 79.1(2) . . y N5 Ni1 O2 78.4(2) . . y N9 Ni1 O2 167.3(2) . . y N1 Ni1 O2 94.2(2) . . y O1 Ni1 O2 86.2(2) . . y N5 Ni1 O3 94.7(2) . . y N9 Ni1 O3 78.6(2) . . y N1 Ni1 O3 166.9(2) . . y O1 Ni1 O3 88.3(2) . . y O2 Ni1 O3 88.7(2) . . y N13 Ni2 N17 101.0(3) . . y N13 Ni2 N21 101.0(3) . . y N17 Ni2 N21 98.1(2) . . y N13 Ni2 O5 165.6(2) . . y N17 Ni2 O5 78.7(2) . . y N21 Ni2 O5 93.3(3) . . y N13 Ni2 O6 92.0(2) . . y N17 Ni2 O6 167.1(3) . . y N21 Ni2 O6 79.5(2) . . y O5 Ni2 O6 88.76(19) . . y N13 Ni2 O4 79.7(2) . . y N17 Ni2 O4 95.7(2) . . y N21 Ni2 O4 165.7(2) . . y O5 Ni2 O4 86.04(18) . . y O6 Ni2 O4 86.29(19) . . y N3 Ni3 O4 119.9(2) . . y N3 Ni3 N15 98.7(3) . . y O4 Ni3 N15 94.1(2) . . y N3 Ni3 O1 92.4(2) . . y O4 Ni3 O1 131.7(2) . . y N15 Ni3 O1 117.0(2) . . y N19 Ni4 O5 93.3(2) . . y N19 Ni4 O2 117.3(2) . . y O5 Ni4 O2 134.78(19) . . y N19 Ni4 N7 98.1(3) . . y O5 Ni4 N7 115.1(2) . . y O2 Ni4 N7 93.8(2) . . y O6 Ni5 O3 130.6(2) . . y O6 Ni5 N23 93.0(2) . . y O3 Ni5 N23 114.7(2) . . y O6 Ni5 N11 122.8(2) . . y O3 Ni5 N11 94.8(2) . . y N23 Ni5 N11 97.1(3) . . y C1 O1 Ni3 125.5(4) . . ? C1 O1 Ni1 114.4(4) . . ? Ni3 O1 Ni1 118.9(2) . . y C17 O2 Ni4 125.1(4) . . ? C17 O2 Ni1 114.5(3) . . ? Ni4 O2 Ni1 119.2(2) . . y C33 O3 Ni5 124.2(4) . . ? C33 O3 Ni1 114.2(4) . . ? Ni5 O3 Ni1 120.3(2) . . y C49 O4 Ni3 125.9(5) . . ? C49 O4 Ni2 112.8(4) . . ? Ni3 O4 Ni2 119.2(2) . . y C65 O5 Ni4 126.0(5) . . ? C65 O5 Ni2 114.3(5) . . ? Ni4 O5 Ni2 117.6(2) . . y C81 O6 Ni5 126.2(4) . . ? C81 O6 Ni2 113.6(4) . . ? Ni5 O6 Ni2 117.6(2) . . y C2 N1 C3 106.7(5) . . ? C2 N1 Ni1 113.2(4) . . ? C3 N1 Ni1 140.1(4) . . ? C2 N2 C8 108.1(6) . . ? C2 N2 H2 125.9 . . ? C8 N2 H2 125.9 . . ? C10 N3 C11 105.9(6) . . ? C10 N3 Ni3 127.5(5) . . ? C11 N3 Ni3 126.5(5) . . ? C10 N4 C16 109.4(8) . . ? C10 N4 H4 125.3 . . ? C16 N4 H4 125.3 . . ? C18 N5 C19 106.1(5) . . ? C18 N5 Ni1 114.0(4) . . ? C19 N5 Ni1 139.8(4) . . ? C18 N6 C24 105.6(5) . . ? C18 N6 H6 127.2 . . ? C24 N6 H6 127.2 . . ? C26 N7 C27 105.7(6) . . ? C26 N7 Ni4 124.7(5) . . ? C27 N7 Ni4 129.2(5) . . ? C26 N8 C32 110.1(6) . . ? C26 N8 H8 125.0 . . ? C32 N8 H8 125.0 . . ? C34 N9 C35 105.3(5) . . ? C34 N9 Ni1 113.9(4) . . ? C35 N9 Ni1 140.2(4) . . ? C34 N10 C40 107.9(5) . . ? C34 N10 H10 126.1 . . ? C40 N10 H10 126.1 . . ? C42 N11 C43 107.0(7) . . ? C42 N11 Ni5 123.3(5) . . ? C43 N11 Ni5 129.2(6) . . ? C42 N12 C48 108.1(8) . . ? C42 N12 H12 125.9 . . ? C48 N12 H12 125.9 . . ? C50 N13 C51 106.3(9) . . ? C50 N13 Ni2 112.8(5) . . ? C51 N13 Ni2 140.9(8) . . ? C56 N14 C50 107.4(9) . . ? C56 N14 H14 126.3 . . ? C50 N14 H14 126.3 . . ? C58 N15 C59 106.9(6) . . ? C58 N15 Ni3 123.6(5) . . ? C59 N15 Ni3 129.3(5) . . ? C58 N16 C64 108.4(6) . . ? C58 N16 H16 125.8 . . ? C64 N16 H16 125.8 . . ? C66 N17 C67 107.6(6) . . ? C66 N17 Ni2 112.8(5) . . ? C67 N17 Ni2 138.2(6) . . ? C66 N18 C72 106.1(7) . . ? C66 N18 H18 127.0 . . ? C72 N18 H18 127.0 . . ? C74 N19 C75 104.6(7) . . ? C74 N19 Ni4 125.5(6) . . ? C75 N19 Ni4 129.8(5) . . ? C74 N20 C80 108.6(8) . . ? C74 N20 H20 125.7 . . ? C80 N20 H20 125.7 . . ? C82 N21 C83 106.8(7) . . ? C82 N21 Ni2 112.4(5) . . ? C83 N21 Ni2 140.7(6) . . ? C88 N22 C82 108.9(7) . . ? C88 N22 H22 125.5 . . ? C82 N22 H22 125.5 . . ? C90 N23 C91 108.0(7) . . ? C90 N23 Ni5 124.5(5) . . ? C91 N23 Ni5 127.5(6) . . ? C96 N24 C90 107.6(8) . . ? C96 N24 H24 126.2 . . ? C90 N24 H24 126.2 . . ? O1 C1 C9 126.9(7) . . ? O1 C1 C2 112.0(5) . . ? C9 C1 C2 121.1(6) . . ? N1 C2 N2 111.2(6) . . ? N1 C2 C1 120.8(6) . . ? N2 C2 C1 127.9(6) . . ? N1 C3 C4 130.8(6) . . ? N1 C3 C8 108.7(6) . . ? C4 C3 C8 120.5(6) . . ? C5 C4 C3 115.5(6) . . ? C5 C4 H4A 122.2 . . ? C3 C4 H4A 122.2 . . ? C6 C5 C4 123.5(7) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C7 122.1(7) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C8 C7 C6 114.0(7) . . ? C8 C7 H7 123.0 . . ? C6 C7 H7 123.0 . . ? C7 C8 N2 130.3(7) . . ? C7 C8 C3 124.4(7) . . ? N2 C8 C3 105.3(6) . . ? C1 C9 C10 123.5(7) . . ? C1 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? N4 C10 N3 111.3(7) . . ? N4 C10 C9 125.2(8) . . ? N3 C10 C9 123.6(6) . . ? C12 C11 N3 131.3(8) . . ? C12 C11 C16 121.1(7) . . ? N3 C11 C16 107.6(7) . . ? C13 C12 C11 116.2(10) . . ? C13 C12 H12A 121.9 . . ? C11 C12 H12A 121.9 . . ? C12 C13 C14 124.4(11) . . ? C12 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C15 C14 C13 121.5(10) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C14 C15 C16 117.4(12) . . ? C14 C15 H15 121.3 . . ? C16 C15 H15 121.3 . . ? N4 C16 C15 134.8(11) . . ? N4 C16 C11 105.7(7) . . ? C15 C16 C11 119.4(10) . . ? C25 C17 O2 126.4(6) . . ? C25 C17 C18 121.8(6) . . ? O2 C17 C18 111.8(5) . . ? N5 C18 N6 112.9(5) . . ? N5 C18 C17 120.5(5) . . ? N6 C18 C17 126.7(6) . . ? C24 C19 N5 108.6(5) . . ? C24 C19 C20 120.1(6) . . ? N5 C19 C20 131.3(6) . . ? C21 C20 C19 117.2(7) . . ? C21 C20 H20A 121.4 . . ? C19 C20 H20A 121.4 . . ? C20 C21 C22 122.2(6) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 121.7(6) . . ? C23 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C22 C23 C24 115.1(7) . . ? C22 C23 H23 122.4 . . ? C24 C23 H23 122.4 . . ? C19 C24 N6 106.9(5) . . ? C19 C24 C23 123.6(6) . . ? N6 C24 C23 129.5(6) . . ? C17 C25 C26 125.3(6) . . ? C17 C25 H25 117.4 . . ? C26 C25 H25 117.4 . . ? N8 C26 N7 111.0(6) . . ? N8 C26 C25 124.3(6) . . ? N7 C26 C25 124.5(6) . . ? C28 C27 N7 130.1(7) . . ? C28 C27 C32 121.5(7) . . ? N7 C27 C32 108.4(6) . . ? C27 C28 C29 115.4(8) . . ? C27 C28 H28 122.3 . . ? C29 C28 H28 122.3 . . ? C30 C29 C28 124.6(8) . . ? C30 C29 H29 117.7 . . ? C28 C29 H29 117.7 . . ? C29 C30 C31 122.4(8) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C32 C31 C30 113.2(9) . . ? C32 C31 H31 123.4 . . ? C30 C31 H31 123.4 . . ? N8 C32 C31 132.5(9) . . ? N8 C32 C27 104.7(6) . . ? C31 C32 C27 122.8(8) . . ? O3 C33 C41 127.6(7) . . ? O3 C33 C34 111.8(5) . . ? C41 C33 C34 120.6(6) . . ? N9 C34 N10 112.9(6) . . ? N9 C34 C33 119.8(6) . . ? N10 C34 C33 127.3(6) . . ? C36 C35 N9 130.3(6) . . ? C36 C35 C40 120.8(6) . . ? N9 C35 C40 108.9(5) . . ? C35 C36 C37 115.9(6) . . ? C35 C36 H36 122.0 . . ? C37 C36 H36 122.0 . . ? C38 C37 C36 121.6(7) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C39 122.8(7) . . ? C37 C38 H38 118.6 . . ? C39 C38 H38 118.6 . . ? C40 C39 C38 116.3(7) . . ? C40 C39 H39 121.9 . . ? C38 C39 H39 121.9 . . ? C39 C40 N10 132.5(7) . . ? C39 C40 C35 122.5(7) . . ? N10 C40 C35 105.0(6) . . ? C33 C41 C42 124.3(7) . . ? C33 C41 H41 117.8 . . ? C42 C41 H41 117.8 . . ? N12 C42 N11 111.0(7) . . ? N12 C42 C41 123.1(7) . . ? N11 C42 C41 125.8(7) . . ? C44 C43 N11 132.5(9) . . ? C44 C43 C48 119.4(8) . . ? N11 C43 C48 108.0(8) . . ? C45 C44 C43 122.7(12) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C44 C45 C46 114.5(12) . . ? C44 C45 H45 122.8 . . ? C46 C45 H45 122.8 . . ? C47 C46 C45 124.6(11) . . ? C47 C46 H46 117.7 . . ? C45 C46 H46 117.7 . . ? C46 C47 C48 116.8(14) . . ? C46 C47 H47 121.6 . . ? C48 C47 H47 121.6 . . ? N12 C48 C47 132.4(12) . . ? N12 C48 C43 105.8(7) . . ? C47 C48 C43 121.8(11) . . ? O4 C49 C57 124.8(7) . . ? O4 C49 C50 113.2(7) . . ? C57 C49 C50 121.9(7) . . ? N13 C50 N14 112.2(7) . . ? N13 C50 C49 120.3(7) . . ? N14 C50 C49 127.4(8) . . ? N13 C51 C52 129.4(12) . . ? N13 C51 C56 108.2(9) . . ? C52 C51 C56 122.3(10) . . ? C51 C52 C53 112.1(14) . . ? C51 C52 H52 123.9 . . ? C53 C52 H52 123.9 . . ? C54 C53 C52 122.8(14) . . ? C54 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? C55 C54 C53 123.4(13) . . ? C55 C54 H54 118.3 . . ? C53 C54 H54 118.3 . . ? C54 C55 C56 119.2(16) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? N14 C56 C55 134.0(14) . . ? N14 C56 C51 105.8(8) . . ? C55 C56 C51 120.1(12) . . ? C49 C57 C58 124.6(7) . . ? C49 C57 H57 117.7 . . ? C58 C57 H57 117.7 . . ? N15 C58 N16 110.6(7) . . ? N15 C58 C57 126.7(7) . . ? N16 C58 C57 122.5(7) . . ? N15 C59 C60 131.9(6) . . ? N15 C59 C64 108.5(7) . . ? C60 C59 C64 119.5(7) . . ? C59 C60 C61 118.4(8) . . ? C59 C60 H60 120.8 . . ? C61 C60 H60 120.8 . . ? C62 C61 C60 121.1(10) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C63 C62 C61 121.0(10) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 119.8(9) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C63 C64 N16 134.2(8) . . ? C63 C64 C59 120.3(9) . . ? N16 C64 C59 105.5(7) . . ? O5 C65 C73 126.4(7) . . ? O5 C65 C66 112.0(7) . . ? C73 C65 C66 121.6(6) . . ? N17 C66 N18 112.9(7) . . ? N17 C66 C65 120.8(6) . . ? N18 C66 C65 126.3(8) . . ? C68 C67 N17 132.5(7) . . ? C68 C67 C72 120.5(7) . . ? N17 C67 C72 107.0(7) . . ? C67 C68 C69 117.3(8) . . ? C67 C68 H68 121.4 . . ? C69 C68 H68 121.4 . . ? C70 C69 C68 122.2(9) . . ? C70 C69 H69 118.9 . . ? C68 C69 H69 118.9 . . ? C69 C70 C71 121.5(7) . . ? C69 C70 H70 119.3 . . ? C71 C70 H70 119.3 . . ? C72 C71 C70 117.5(8) . . ? C72 C71 H71 121.3 . . ? C70 C71 H71 121.3 . . ? N18 C72 C71 132.6(9) . . ? N18 C72 C67 106.4(7) . . ? C71 C72 C67 120.9(9) . . ? C65 C73 C74 123.6(7) . . ? C65 C73 H73 118.2 . . ? C74 C73 H73 118.2 . . ? N19 C74 N20 111.2(7) . . ? N19 C74 C73 124.4(8) . . ? N20 C74 C73 124.3(7) . . ? C80 C75 N19 110.2(7) . . ? C80 C75 C76 121.2(8) . . ? N19 C75 C76 128.6(7) . . ? C77 C76 C75 116.3(7) . . ? C77 C76 H76 121.9 . . ? C75 C76 H76 121.9 . . ? C78 C77 C76 120.9(8) . . ? C78 C77 H77 119.6 . . ? C76 C77 H77 119.6 . . ? C79 C78 C77 121.3(9) . . ? C79 C78 H78 119.4 . . ? C77 C78 H78 119.4 . . ? C80 C79 C78 117.8(10) . . ? C80 C79 H79 121.1 . . ? C78 C79 H79 121.1 . . ? C75 C80 C79 122.4(9) . . ? C75 C80 N20 105.4(8) . . ? C79 C80 N20 132.0(10) . . ? O6 C81 C89 124.6(7) . . ? O6 C81 C82 112.7(7) . . ? C89 C81 C82 122.5(8) . . ? N21 C82 N22 110.8(7) . . ? N21 C82 C81 120.9(7) . . ? N22 C82 C81 128.3(8) . . ? C84 C83 N21 131.7(9) . . ? C84 C83 C88 120.6(8) . . ? N21 C83 C88 107.7(7) . . ? C83 C84 C85 116.5(10) . . ? C83 C84 H84 121.7 . . ? C85 C84 H84 121.7 . . ? C86 C85 C84 122.6(10) . . ? C86 C85 H85 118.7 . . ? C84 C85 H85 118.7 . . ? C85 C86 C87 122.2(9) . . ? C85 C86 H86 118.9 . . ? C87 C86 H86 118.9 . . ? C86 C87 C88 118.3(10) . . ? C86 C87 H87 120.9 . . ? C88 C87 H87 120.9 . . ? N22 C88 C87 134.4(10) . . ? N22 C88 C83 105.7(8) . . ? C87 C88 C83 119.9(9) . . ? C81 C89 C90 125.4(9) . . ? C81 C89 H89 117.3 . . ? C90 C89 H89 117.3 . . ? N23 C90 N24 109.7(7) . . ? N23 C90 C89 125.3(7) . . ? N24 C90 C89 125.0(9) . . ? N23 C91 C92 131.6(8) . . ? N23 C91 C96 107.9(8) . . ? C92 C91 C96 120.5(7) . . ? C93 C92 C91 117.5(10) . . ? C93 C92 H92 121.3 . . ? C91 C92 H92 121.3 . . ? C92 C93 C94 122.3(10) . . ? C92 C93 H93 118.9 . . ? C94 C93 H93 118.9 . . ? C95 C94 C93 120.2(9) . . ? C95 C94 H94 119.9 . . ? C93 C94 H94 119.9 . . ? C94 C95 C96 119.8(12) . . ? C94 C95 H95 120.1 . . ? C96 C95 H95 120.1 . . ? N24 C96 C91 106.8(7) . . ? N24 C96 C95 133.6(11) . . ? C91 C96 C95 119.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni3 O1 C1 -8.6(5) . . . . ? O4 Ni3 O1 C1 -143.6(5) . . . . ? N15 Ni3 O1 C1 92.4(5) . . . . ? N3 Ni3 O1 Ni1 -174.9(3) . . . . ? O4 Ni3 O1 Ni1 50.1(4) . . . . ? N15 Ni3 O1 Ni1 -73.9(3) . . . . ? N5 Ni1 O1 C1 88.5(8) . . . . ? N9 Ni1 O1 C1 -91.8(4) . . . . ? N1 Ni1 O1 C1 5.8(4) . . . . ? O2 Ni1 O1 C1 100.8(4) . . . . ? O3 Ni1 O1 C1 -170.3(4) . . . . ? N5 Ni1 O1 Ni3 -103.8(7) . . . . ? N9 Ni1 O1 Ni3 75.9(3) . . . . ? N1 Ni1 O1 Ni3 173.6(3) . . . . ? O2 Ni1 O1 Ni3 -91.4(3) . . . . ? O3 Ni1 O1 Ni3 -2.6(3) . . . . ? N19 Ni4 O2 C17 95.5(5) . . . . ? O5 Ni4 O2 C17 -137.3(5) . . . . ? N7 Ni4 O2 C17 -5.6(6) . . . . ? N19 Ni4 O2 Ni1 -71.3(3) . . . . ? O5 Ni4 O2 Ni1 55.9(4) . . . . ? N7 Ni4 O2 Ni1 -172.4(3) . . . . ? N5 Ni1 O2 C17 7.9(4) . . . . ? N9 Ni1 O2 C17 104.3(9) . . . . ? N1 Ni1 O2 C17 -89.9(4) . . . . ? O1 Ni1 O2 C17 -168.7(4) . . . . ? O3 Ni1 O2 C17 102.9(4) . . . . ? N5 Ni1 O2 Ni4 176.1(3) . . . . ? N9 Ni1 O2 Ni4 -87.5(8) . . . . ? N1 Ni1 O2 Ni4 78.3(3) . . . . ? O1 Ni1 O2 Ni4 -0.5(2) . . . . ? O3 Ni1 O2 Ni4 -88.9(3) . . . . ? O6 Ni5 O3 C33 -143.0(5) . . . . ? N23 Ni5 O3 C33 99.1(5) . . . . ? N11 Ni5 O3 C33 -1.0(5) . . . . ? O6 Ni5 O3 Ni1 50.7(4) . . . . ? N23 Ni5 O3 Ni1 -67.2(3) . . . . ? N11 Ni5 O3 Ni1 -167.3(3) . . . . ? N5 Ni1 O3 C33 -94.8(5) . . . . ? N9 Ni1 O3 C33 7.2(4) . . . . ? N1 Ni1 O3 C33 83.7(9) . . . . ? O1 Ni1 O3 C33 100.7(5) . . . . ? O2 Ni1 O3 C33 -173.1(5) . . . . ? N5 Ni1 O3 Ni5 72.7(3) . . . . ? N9 Ni1 O3 Ni5 174.7(3) . . . . ? N1 Ni1 O3 Ni5 -108.7(8) . . . . ? O1 Ni1 O3 Ni5 -91.7(3) . . . . ? O2 Ni1 O3 Ni5 -5.6(2) . . . . ? N3 Ni3 O4 C49 98.1(5) . . . . ? N15 Ni3 O4 C49 -4.3(5) . . . . ? O1 Ni3 O4 C49 -136.6(5) . . . . ? N3 Ni3 O4 Ni2 -64.1(4) . . . . ? N15 Ni3 O4 Ni2 -166.5(3) . . . . ? O1 Ni3 O4 Ni2 61.2(4) . . . . ? N13 Ni2 O4 C49 9.9(5) . . . . ? N17 Ni2 O4 C49 -90.3(5) . . . . ? N21 Ni2 O4 C49 103.8(12) . . . . ? O5 Ni2 O4 C49 -168.4(5) . . . . ? O6 Ni2 O4 C49 102.6(5) . . . . ? N13 Ni2 O4 Ni3 174.3(3) . . . . ? N17 Ni2 O4 Ni3 74.2(3) . . . . ? N21 Ni2 O4 Ni3 -91.8(11) . . . . ? O5 Ni2 O4 Ni3 -4.0(3) . . . . ? O6 Ni2 O4 Ni3 -93.0(3) . . . . ? N19 Ni4 O5 C65 -10.1(6) . . . . ? O2 Ni4 O5 C65 -145.0(5) . . . . ? N7 Ni4 O5 C65 90.4(6) . . . . ? N19 Ni4 O5 Ni2 -172.7(3) . . . . ? O2 Ni4 O5 Ni2 52.4(4) . . . . ? N7 Ni4 O5 Ni2 -72.2(3) . . . . ? N13 Ni2 O5 C65 99.2(9) . . . . ? N17 Ni2 O5 C65 9.3(5) . . . . ? N21 Ni2 O5 C65 -88.3(5) . . . . ? O6 Ni2 O5 C65 -167.7(5) . . . . ? O4 Ni2 O5 C65 106.0(5) . . . . ? N13 Ni2 O5 Ni4 -96.2(8) . . . . ? N17 Ni2 O5 Ni4 173.9(3) . . . . ? N21 Ni2 O5 Ni4 76.3(3) . . . . ? O6 Ni2 O5 Ni4 -3.1(3) . . . . ? O4 Ni2 O5 Ni4 -89.4(3) . . . . ? O3 Ni5 O6 C81 -137.2(7) . . . . ? N23 Ni5 O6 C81 -10.8(7) . . . . ? N11 Ni5 O6 C81 89.6(7) . . . . ? O3 Ni5 O6 Ni2 62.5(4) . . . . ? N23 Ni5 O6 Ni2 -171.0(3) . . . . ? N11 Ni5 O6 Ni2 -70.6(4) . . . . ? N13 Ni2 O6 C81 -92.3(6) . . . . ? N17 Ni2 O6 C81 88.7(11) . . . . ? N21 Ni2 O6 C81 8.5(6) . . . . ? O5 Ni2 O6 C81 102.1(6) . . . . ? O4 Ni2 O6 C81 -171.8(6) . . . . ? N13 Ni2 O6 Ni5 70.4(3) . . . . ? N17 Ni2 O6 Ni5 -108.6(9) . . . . ? N21 Ni2 O6 Ni5 171.2(4) . . . . ? O5 Ni2 O6 Ni5 -95.2(3) . . . . ? O4 Ni2 O6 Ni5 -9.1(3) . . . . ? N5 Ni1 N1 C2 -169.5(4) . . . . ? N9 Ni1 N1 C2 86.3(4) . . . . ? O1 Ni1 N1 C2 -5.3(4) . . . . ? O2 Ni1 N1 C2 -90.6(4) . . . . ? O3 Ni1 N1 C2 11.9(11) . . . . ? N5 Ni1 N1 C3 14.7(6) . . . . ? N9 Ni1 N1 C3 -89.5(6) . . . . ? O1 Ni1 N1 C3 178.9(6) . . . . ? O2 Ni1 N1 C3 93.6(6) . . . . ? O3 Ni1 N1 C3 -163.9(7) . . . . ? O4 Ni3 N3 C10 146.9(7) . . . . ? N15 Ni3 N3 C10 -113.3(7) . . . . ? O1 Ni3 N3 C10 4.5(7) . . . . ? O4 Ni3 N3 C11 -35.1(7) . . . . ? N15 Ni3 N3 C11 64.7(7) . . . . ? O1 Ni3 N3 C11 -177.5(7) . . . . ? N9 Ni1 N5 C18 -173.2(4) . . . . ? N1 Ni1 N5 C18 86.5(5) . . . . ? O1 Ni1 N5 C18 6.5(10) . . . . ? O2 Ni1 N5 C18 -6.1(4) . . . . ? O3 Ni1 N5 C18 -93.9(4) . . . . ? N9 Ni1 N5 C19 12.1(7) . . . . ? N1 Ni1 N5 C19 -88.2(6) . . . . ? O1 Ni1 N5 C19 -168.2(6) . . . . ? O2 Ni1 N5 C19 179.2(7) . . . . ? O3 Ni1 N5 C19 91.5(6) . . . . ? N19 Ni4 N7 C26 -114.3(7) . . . . ? O5 Ni4 N7 C26 148.1(7) . . . . ? O2 Ni4 N7 C26 4.0(7) . . . . ? N19 Ni4 N7 C27 57.3(8) . . . . ? O5 Ni4 N7 C27 -40.3(9) . . . . ? O2 Ni4 N7 C27 175.6(8) . . . . ? N5 Ni1 N9 C34 93.1(4) . . . . ? N1 Ni1 N9 C34 -166.2(4) . . . . ? O1 Ni1 N9 C34 -86.8(4) . . . . ? O2 Ni1 N9 C34 -0.5(11) . . . . ? O3 Ni1 N9 C34 0.9(4) . . . . ? N5 Ni1 N9 C35 -98.0(6) . . . . ? N1 Ni1 N9 C35 2.6(6) . . . . ? O1 Ni1 N9 C35 82.1(6) . . . . ? O2 Ni1 N9 C35 168.4(6) . . . . ? O3 Ni1 N9 C35 169.7(6) . . . . ? O6 Ni5 N11 C42 147.3(6) . . . . ? O3 Ni5 N11 C42 1.1(7) . . . . ? N23 Ni5 N11 C42 -114.6(6) . . . . ? O6 Ni5 N11 C43 -42.7(7) . . . . ? O3 Ni5 N11 C43 171.1(6) . . . . ? N23 Ni5 N11 C43 55.5(7) . . . . ? N17 Ni2 N13 C50 87.6(5) . . . . ? N21 Ni2 N13 C50 -171.9(5) . . . . ? O5 Ni2 N13 C50 0.5(12) . . . . ? O6 Ni2 N13 C50 -92.2(5) . . . . ? O4 Ni2 N13 C50 -6.4(5) . . . . ? N17 Ni2 N13 C51 -92.0(8) . . . . ? N21 Ni2 N13 C51 8.6(9) . . . . ? O6 Ni2 N13 C51 88.3(8) . . . . ? O4 Ni2 N13 C51 174.1(9) . . . . ? N3 Ni3 N15 C58 -121.4(6) . . . . ? O4 Ni3 N15 C58 -0.3(6) . . . . ? O1 Ni3 N15 C58 141.4(5) . . . . ? N3 Ni3 N15 C59 54.4(6) . . . . ? O4 Ni3 N15 C59 175.5(6) . . . . ? O1 Ni3 N15 C59 -42.9(6) . . . . ? N13 Ni2 N17 C66 -175.3(5) . . . . ? N21 Ni2 N17 C66 81.8(5) . . . . ? O5 Ni2 N17 C66 -10.0(5) . . . . ? O6 Ni2 N17 C66 3.7(12) . . . . ? O4 Ni2 N17 C66 -94.8(5) . . . . ? N13 Ni2 N17 C67 20.2(7) . . . . ? N21 Ni2 N17 C67 -82.7(7) . . . . ? O5 Ni2 N17 C67 -174.5(7) . . . . ? O6 Ni2 N17 C67 -160.8(8) . . . . ? O4 Ni2 N17 C67 100.7(7) . . . . ? O5 Ni4 N19 C74 5.4(7) . . . . ? O2 Ni4 N19 C74 151.0(7) . . . . ? N7 Ni4 N19 C74 -110.5(7) . . . . ? O5 Ni4 N19 C75 -178.3(7) . . . . ? O2 Ni4 N19 C75 -32.8(7) . . . . ? N7 Ni4 N19 C75 65.8(7) . . . . ? N13 Ni2 N21 C82 85.4(7) . . . . ? N17 Ni2 N21 C82 -171.7(7) . . . . ? O5 Ni2 N21 C82 -92.7(7) . . . . ? O6 Ni2 N21 C82 -4.6(7) . . . . ? O4 Ni2 N21 C82 -5.8(16) . . . . ? N13 Ni2 N21 C83 -95.5(11) . . . . ? N17 Ni2 N21 C83 7.4(11) . . . . ? O5 Ni2 N21 C83 86.4(11) . . . . ? O6 Ni2 N21 C83 174.5(11) . . . . ? O4 Ni2 N21 C83 173.3(9) . . . . ? O6 Ni5 N23 C90 3.3(7) . . . . ? O3 Ni5 N23 C90 141.1(6) . . . . ? N11 Ni5 N23 C90 -120.2(7) . . . . ? O6 Ni5 N23 C91 -177.6(6) . . . . ? O3 Ni5 N23 C91 -39.8(7) . . . . ? N11 Ni5 N23 C91 58.8(6) . . . . ? Ni3 O1 C1 C9 9.4(10) . . . . ? Ni1 O1 C1 C9 176.2(6) . . . . ? Ni3 O1 C1 C2 -171.8(4) . . . . ? Ni1 O1 C1 C2 -5.0(7) . . . . ? C3 N1 C2 N2 0.1(7) . . . . ? Ni1 N1 C2 N2 -177.0(4) . . . . ? C3 N1 C2 C1 -178.3(6) . . . . ? Ni1 N1 C2 C1 4.5(7) . . . . ? C8 N2 C2 N1 -1.0(8) . . . . ? C8 N2 C2 C1 177.2(6) . . . . ? O1 C1 C2 N1 0.4(9) . . . . ? C9 C1 C2 N1 179.3(7) . . . . ? O1 C1 C2 N2 -177.7(6) . . . . ? C9 C1 C2 N2 1.2(11) . . . . ? C2 N1 C3 C4 -180.0(7) . . . . ? Ni1 N1 C3 C4 -4.0(11) . . . . ? C2 N1 C3 C8 0.8(7) . . . . ? Ni1 N1 C3 C8 176.8(5) . . . . ? N1 C3 C4 C5 -179.4(6) . . . . ? C8 C3 C4 C5 -0.2(9) . . . . ? C3 C4 C5 C6 0.4(11) . . . . ? C4 C5 C6 C7 -0.4(12) . . . . ? C5 C6 C7 C8 0.1(12) . . . . ? C6 C7 C8 N2 -179.1(7) . . . . ? C6 C7 C8 C3 0.0(11) . . . . ? C2 N2 C8 C7 -179.3(8) . . . . ? C2 N2 C8 C3 1.5(7) . . . . ? N1 C3 C8 C7 179.3(7) . . . . ? C4 C3 C8 C7 0.0(10) . . . . ? N1 C3 C8 N2 -1.4(7) . . . . ? C4 C3 C8 N2 179.3(6) . . . . ? O1 C1 C9 C10 -2.9(13) . . . . ? C2 C1 C9 C10 178.4(7) . . . . ? C16 N4 C10 N3 0.4(12) . . . . ? C16 N4 C10 C9 -179.7(10) . . . . ? C11 N3 C10 N4 1.3(10) . . . . ? Ni3 N3 C10 N4 179.7(6) . . . . ? C11 N3 C10 C9 -178.7(8) . . . . ? Ni3 N3 C10 C9 -0.3(12) . . . . ? C1 C9 C10 N4 178.1(9) . . . . ? C1 C9 C10 N3 -2.0(14) . . . . ? C10 N3 C11 C12 178.2(9) . . . . ? Ni3 N3 C11 C12 -0.2(13) . . . . ? C10 N3 C11 C16 -2.3(10) . . . . ? Ni3 N3 C11 C16 179.2(7) . . . . ? N3 C11 C12 C13 -178.9(10) . . . . ? C16 C11 C12 C13 1.7(14) . . . . ? C11 C12 C13 C14 -1.3(19) . . . . ? C12 C13 C14 C15 -1(3) . . . . ? C13 C14 C15 C16 2(3) . . . . ? C10 N4 C16 C15 -178.8(16) . . . . ? C10 N4 C16 C11 -1.8(13) . . . . ? C14 C15 C16 N4 175.3(16) . . . . ? C14 C15 C16 C11 -1(2) . . . . ? C12 C11 C16 N4 -178.0(9) . . . . ? N3 C11 C16 N4 2.6(12) . . . . ? C12 C11 C16 C15 -0.4(17) . . . . ? N3 C11 C16 C15 -179.9(12) . . . . ? Ni4 O2 C17 C25 4.3(10) . . . . ? Ni1 O2 C17 C25 171.7(7) . . . . ? Ni4 O2 C17 C18 -175.2(4) . . . . ? Ni1 O2 C17 C18 -7.8(7) . . . . ? C19 N5 C18 N6 0.4(7) . . . . ? Ni1 N5 C18 N6 -176.0(4) . . . . ? C19 N5 C18 C17 -179.5(6) . . . . ? Ni1 N5 C18 C17 4.1(8) . . . . ? C24 N6 C18 N5 -1.2(7) . . . . ? C24 N6 C18 C17 178.8(6) . . . . ? C25 C17 C18 N5 -176.8(7) . . . . ? O2 C17 C18 N5 2.7(9) . . . . ? C25 C17 C18 N6 3.3(12) . . . . ? O2 C17 C18 N6 -177.2(6) . . . . ? C18 N5 C19 C24 0.5(7) . . . . ? Ni1 N5 C19 C24 175.4(5) . . . . ? C18 N5 C19 C20 -179.8(7) . . . . ? Ni1 N5 C19 C20 -4.9(11) . . . . ? C24 C19 C20 C21 1.1(9) . . . . ? N5 C19 C20 C21 -178.5(6) . . . . ? C19 C20 C21 C22 -1.2(10) . . . . ? C20 C21 C22 C23 0.2(11) . . . . ? C21 C22 C23 C24 0.8(10) . . . . ? N5 C19 C24 N6 -1.2(7) . . . . ? C20 C19 C24 N6 179.1(6) . . . . ? N5 C19 C24 C23 179.7(6) . . . . ? C20 C19 C24 C23 0.0(10) . . . . ? C18 N6 C24 C19 1.4(7) . . . . ? C18 N6 C24 C23 -179.5(7) . . . . ? C22 C23 C24 C19 -0.9(10) . . . . ? C22 C23 C24 N6 -179.8(7) . . . . ? O2 C17 C25 C26 0.7(13) . . . . ? C18 C17 C25 C26 -179.9(8) . . . . ? C32 N8 C26 N7 0.9(12) . . . . ? C32 N8 C26 C25 175.3(9) . . . . ? C27 N7 C26 N8 0.3(11) . . . . ? Ni4 N7 C26 N8 173.6(7) . . . . ? C27 N7 C26 C25 -174.2(9) . . . . ? Ni4 N7 C26 C25 -0.9(13) . . . . ? C17 C25 C26 N8 -176.2(9) . . . . ? C17 C25 C26 N7 -2.5(14) . . . . ? C26 N7 C27 C28 178.9(12) . . . . ? Ni4 N7 C27 C28 6.1(17) . . . . ? C26 N7 C27 C32 -1.3(11) . . . . ? Ni4 N7 C27 C32 -174.2(7) . . . . ? N7 C27 C28 C29 179.7(11) . . . . ? C32 C27 C28 C29 0.0(18) . . . . ? C27 C28 C29 C30 1(2) . . . . ? C28 C29 C30 C31 -5(3) . . . . ? C29 C30 C31 C32 6(2) . . . . ? C26 N8 C32 C31 178.2(13) . . . . ? C26 N8 C32 C27 -1.6(12) . . . . ? C30 C31 C32 N8 175.9(13) . . . . ? C30 C31 C32 C27 -4.2(19) . . . . ? C28 C27 C32 N8 -178.4(11) . . . . ? N7 C27 C32 N8 1.8(12) . . . . ? C28 C27 C32 C31 1.7(18) . . . . ? N7 C27 C32 C31 -178.1(11) . . . . ? Ni5 O3 C33 C41 1.9(10) . . . . ? Ni1 O3 C33 C41 169.0(6) . . . . ? Ni5 O3 C33 C34 -179.8(4) . . . . ? Ni1 O3 C33 C34 -12.8(7) . . . . ? C35 N9 C34 N10 1.2(7) . . . . ? Ni1 N9 C34 N10 173.9(4) . . . . ? C35 N9 C34 C33 178.9(5) . . . . ? Ni1 N9 C34 C33 -8.4(7) . . . . ? C40 N10 C34 N9 -2.3(7) . . . . ? C40 N10 C34 C33 -179.8(6) . . . . ? O3 C33 C34 N9 14.5(9) . . . . ? C41 C33 C34 N9 -167.1(6) . . . . ? O3 C33 C34 N10 -168.2(6) . . . . ? C41 C33 C34 N10 10.2(11) . . . . ? C34 N9 C35 C36 -179.6(6) . . . . ? Ni1 N9 C35 C36 10.9(10) . . . . ? C34 N9 C35 C40 0.3(6) . . . . ? Ni1 N9 C35 C40 -169.2(5) . . . . ? N9 C35 C36 C37 -179.1(6) . . . . ? C40 C35 C36 C37 1.0(9) . . . . ? C35 C36 C37 C38 1.4(10) . . . . ? C36 C37 C38 C39 -2.5(12) . . . . ? C37 C38 C39 C40 0.9(11) . . . . ? C38 C39 C40 N10 -179.6(7) . . . . ? C38 C39 C40 C35 1.6(10) . . . . ? C34 N10 C40 C39 -176.7(7) . . . . ? C34 N10 C40 C35 2.3(7) . . . . ? C36 C35 C40 C39 -2.6(9) . . . . ? N9 C35 C40 C39 177.5(6) . . . . ? C36 C35 C40 N10 178.3(5) . . . . ? N9 C35 C40 N10 -1.6(6) . . . . ? O3 C33 C41 C42 -2.7(13) . . . . ? C34 C33 C41 C42 179.2(7) . . . . ? C48 N12 C42 N11 -2.3(10) . . . . ? C48 N12 C42 C41 175.0(8) . . . . ? C43 N11 C42 N12 3.2(9) . . . . ? Ni5 N11 C42 N12 175.1(5) . . . . ? C43 N11 C42 C41 -174.0(8) . . . . ? Ni5 N11 C42 C41 -2.0(12) . . . . ? C33 C41 C42 N12 -174.1(8) . . . . ? C33 C41 C42 N11 2.7(13) . . . . ? C42 N11 C43 C44 179.9(9) . . . . ? Ni5 N11 C43 C44 8.6(13) . . . . ? C42 N11 C43 C48 -2.8(9) . . . . ? Ni5 N11 C43 C48 -174.1(6) . . . . ? N11 C43 C44 C45 -179.5(10) . . . . ? C48 C43 C44 C45 3.5(14) . . . . ? C43 C44 C45 C46 -4.1(15) . . . . ? C44 C45 C46 C47 3.9(18) . . . . ? C45 C46 C47 C48 -2.8(19) . . . . ? C42 N12 C48 C47 -178.1(11) . . . . ? C42 N12 C48 C43 0.5(10) . . . . ? C46 C47 C48 N12 -179.8(11) . . . . ? C46 C47 C48 C43 1.8(17) . . . . ? C44 C43 C48 N12 179.1(8) . . . . ? N11 C43 C48 N12 1.5(9) . . . . ? C44 C43 C48 C47 -2.1(14) . . . . ? N11 C43 C48 C47 -179.8(9) . . . . ? Ni3 O4 C49 C57 6.7(10) . . . . ? Ni2 O4 C49 C57 169.8(6) . . . . ? Ni3 O4 C49 C50 -174.2(5) . . . . ? Ni2 O4 C49 C50 -11.1(7) . . . . ? C51 N13 C50 N14 -1.1(9) . . . . ? Ni2 N13 C50 N14 179.2(5) . . . . ? C51 N13 C50 C49 -177.8(7) . . . . ? Ni2 N13 C50 C49 2.5(9) . . . . ? C56 N14 C50 N13 1.8(10) . . . . ? C56 N14 C50 C49 178.3(8) . . . . ? O4 C49 C50 N13 6.1(10) . . . . ? C57 C49 C50 N13 -174.7(7) . . . . ? O4 C49 C50 N14 -170.1(7) . . . . ? C57 C49 C50 N14 9.1(13) . . . . ? C50 N13 C51 C52 -178.9(9) . . . . ? Ni2 N13 C51 C52 0.6(14) . . . . ? C50 N13 C51 C56 0.0(9) . . . . ? Ni2 N13 C51 C56 179.5(6) . . . . ? N13 C51 C52 C53 -179.7(9) . . . . ? C56 C51 C52 C53 1.5(12) . . . . ? C51 C52 C53 C54 -0.1(15) . . . . ? C52 C53 C54 C55 0(2) . . . . ? C53 C54 C55 C56 -1(2) . . . . ? C50 N14 C56 C55 -178.4(11) . . . . ? C50 N14 C56 C51 -1.7(9) . . . . ? C54 C55 C56 N14 178.5(11) . . . . ? C54 C55 C56 C51 2.2(16) . . . . ? N13 C51 C56 N14 1.1(10) . . . . ? C52 C51 C56 N14 -179.9(8) . . . . ? N13 C51 C56 C55 178.3(8) . . . . ? C52 C51 C56 C55 -2.7(14) . . . . ? O4 C49 C57 C58 -3.5(12) . . . . ? C50 C49 C57 C58 177.5(7) . . . . ? C59 N15 C58 N16 0.9(8) . . . . ? Ni3 N15 C58 N16 177.5(5) . . . . ? C59 N15 C58 C57 -173.5(7) . . . . ? Ni3 N15 C58 C57 3.1(10) . . . . ? C64 N16 C58 N15 -1.7(9) . . . . ? C64 N16 C58 C57 172.9(7) . . . . ? C49 C57 C58 N15 -1.8(12) . . . . ? C49 C57 C58 N16 -175.5(7) . . . . ? C58 N15 C59 C60 177.4(7) . . . . ? Ni3 N15 C59 C60 1.1(11) . . . . ? C58 N15 C59 C64 0.3(8) . . . . ? Ni3 N15 C59 C64 -176.1(5) . . . . ? N15 C59 C60 C61 -178.1(7) . . . . ? C64 C59 C60 C61 -1.2(11) . . . . ? C59 C60 C61 C62 0.9(13) . . . . ? C60 C61 C62 C63 -0.1(17) . . . . ? C61 C62 C63 C64 -0.5(18) . . . . ? C62 C63 C64 N16 179.5(10) . . . . ? C62 C63 C64 C59 0.2(15) . . . . ? C58 N16 C64 C63 -177.6(10) . . . . ? C58 N16 C64 C59 1.8(9) . . . . ? N15 C59 C64 C63 178.2(8) . . . . ? C60 C59 C64 C63 0.7(12) . . . . ? N15 C59 C64 N16 -1.3(8) . . . . ? C60 C59 C64 N16 -178.8(7) . . . . ? Ni4 O5 C65 C73 8.9(12) . . . . ? Ni2 O5 C65 C73 172.0(7) . . . . ? Ni4 O5 C65 C66 -169.8(5) . . . . ? Ni2 O5 C65 C66 -6.7(8) . . . . ? C67 N17 C66 N18 -2.5(9) . . . . ? Ni2 N17 C66 N18 -171.7(5) . . . . ? C67 N17 C66 C65 179.3(7) . . . . ? Ni2 N17 C66 C65 10.1(9) . . . . ? C72 N18 C66 N17 2.7(9) . . . . ? C72 N18 C66 C65 -179.2(8) . . . . ? O5 C65 C66 N17 -2.1(10) . . . . ? C73 C65 C66 N17 179.1(8) . . . . ? O5 C65 C66 N18 179.9(7) . . . . ? C73 C65 C66 N18 1.1(13) . . . . ? C66 N17 C67 C68 -177.6(8) . . . . ? Ni2 N17 C67 C68 -12.6(13) . . . . ? C66 N17 C67 C72 1.3(8) . . . . ? Ni2 N17 C67 C72 166.3(6) . . . . ? N17 C67 C68 C69 179.1(8) . . . . ? C72 C67 C68 C69 0.4(11) . . . . ? C67 C68 C69 C70 -3.4(12) . . . . ? C68 C69 C70 C71 4.5(14) . . . . ? C69 C70 C71 C72 -2.3(14) . . . . ? C66 N18 C72 C71 175.7(10) . . . . ? C66 N18 C72 C67 -1.7(9) . . . . ? C70 C71 C72 N18 -177.7(9) . . . . ? C70 C71 C72 C67 -0.6(13) . . . . ? C68 C67 C72 N18 179.4(7) . . . . ? N17 C67 C72 N18 0.3(8) . . . . ? C68 C67 C72 C71 1.6(12) . . . . ? N17 C67 C72 C71 -177.4(8) . . . . ? O5 C65 C73 C74 0.3(15) . . . . ? C66 C65 C73 C74 178.9(9) . . . . ? C75 N19 C74 N20 -0.8(12) . . . . ? Ni4 N19 C74 N20 176.3(8) . . . . ? C75 N19 C74 C73 -176.3(9) . . . . ? Ni4 N19 C74 C73 0.7(14) . . . . ? C80 N20 C74 N19 0.0(15) . . . . ? C80 N20 C74 C73 175.5(11) . . . . ? C65 C73 C74 N19 -5.4(16) . . . . ? C65 C73 C74 N20 179.6(11) . . . . ? C74 N19 C75 C80 1.3(11) . . . . ? Ni4 N19 C75 C80 -175.5(7) . . . . ? C74 N19 C75 C76 178.6(9) . . . . ? Ni4 N19 C75 C76 1.7(12) . . . . ? C80 C75 C76 C77 -2.6(13) . . . . ? N19 C75 C76 C77 -179.6(8) . . . . ? C75 C76 C77 C78 -1.0(13) . . . . ? C76 C77 C78 C79 2(2) . . . . ? C77 C78 C79 C80 1(2) . . . . ? N19 C75 C80 C79 -176.9(13) . . . . ? C76 C75 C80 C79 5.7(19) . . . . ? N19 C75 C80 N20 -1.3(13) . . . . ? C76 C75 C80 N20 -178.8(10) . . . . ? C78 C79 C80 C75 -5(2) . . . . ? C78 C79 C80 N20 -178.9(16) . . . . ? C74 N20 C80 C75 0.8(15) . . . . ? C74 N20 C80 C79 175.8(17) . . . . ? Ni5 O6 C81 C89 13.9(14) . . . . ? Ni2 O6 C81 C89 174.9(9) . . . . ? Ni5 O6 C81 C82 -171.3(6) . . . . ? Ni2 O6 C81 C82 -10.4(10) . . . . ? C83 N21 C82 N22 1.2(12) . . . . ? Ni2 N21 C82 N22 -179.4(7) . . . . ? C83 N21 C82 C81 -179.0(10) . . . . ? Ni2 N21 C82 C81 0.4(12) . . . . ? C88 N22 C82 N21 -0.9(14) . . . . ? C88 N22 C82 C81 179.3(11) . . . . ? O6 C81 C82 N21 6.9(14) . . . . ? C89 C81 C82 N21 -178.2(10) . . . . ? O6 C81 C82 N22 -173.3(10) . . . . ? C89 C81 C82 N22 1.6(18) . . . . ? C82 N21 C83 C84 -179.3(12) . . . . ? Ni2 N21 C83 C84 2(2) . . . . ? C82 N21 C83 C88 -1.0(12) . . . . ? Ni2 N21 C83 C88 179.8(9) . . . . ? N21 C83 C84 C85 178.9(12) . . . . ? C88 C83 C84 C85 0.8(18) . . . . ? C83 C84 C85 C86 0(2) . . . . ? C84 C85 C86 C87 0(3) . . . . ? C85 C86 C87 C88 -1(2) . . . . ? C82 N22 C88 C87 -179.7(16) . . . . ? C82 N22 C88 C83 0.3(14) . . . . ? C86 C87 C88 N22 -179.2(15) . . . . ? C86 C87 C88 C83 1(2) . . . . ? C84 C83 C88 N22 179.0(11) . . . . ? N21 C83 C88 N22 0.5(13) . . . . ? C84 C83 C88 C87 -1.0(19) . . . . ? N21 C83 C88 C87 -179.6(12) . . . . ? O6 C81 C89 C90 -6.7(18) . . . . ? C82 C81 C89 C90 179.0(10) . . . . ? C91 N23 C90 N24 1.2(10) . . . . ? Ni5 N23 C90 N24 -179.5(6) . . . . ? C91 N23 C90 C89 -177.5(9) . . . . ? Ni5 N23 C90 C89 1.7(13) . . . . ? C96 N24 C90 N23 -1.3(11) . . . . ? C96 N24 C90 C89 177.5(10) . . . . ? C81 C89 C90 N23 -1.5(17) . . . . ? C81 C89 C90 N24 179.9(10) . . . . ? C90 N23 C91 C92 -179.9(8) . . . . ? Ni5 N23 C91 C92 0.9(12) . . . . ? C90 N23 C91 C96 -0.7(9) . . . . ? Ni5 N23 C91 C96 -179.9(6) . . . . ? N23 C91 C92 C93 -178.1(8) . . . . ? C96 C91 C92 C93 2.7(12) . . . . ? C91 C92 C93 C94 -3.6(13) . . . . ? C92 C93 C94 C95 4.0(16) . . . . ? C93 C94 C95 C96 -3.3(18) . . . . ? C90 N24 C96 C91 0.9(11) . . . . ? C90 N24 C96 C95 -177.4(12) . . . . ? N23 C91 C96 N24 -0.2(10) . . . . ? C92 C91 C96 N24 179.2(8) . . . . ? N23 C91 C96 C95 178.4(9) . . . . ? C92 C91 C96 C95 -2.2(14) . . . . ? C94 C95 C96 N24 -179.4(12) . . . . ? C94 C95 C96 C91 2.5(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N24 H24 I1B 0.88 3.08 3.488(9) 110.8 2_656 y N22 H22 I4A 0.88 2.66 3.536(8) 174.9 4_576 y N20 H20 I4A 0.88 2.82 3.564(11) 143.8 4_476 y N20 H20 I2A 0.88 3.15 3.675(9) 120.7 4_576 y N20 H20 I2C 0.88 3.16 3.71(3) 122.7 4_576 y N16 H16 I3C 0.88 2.14 2.958(11) 153.3 . y N14 H14 I3B 0.88 2.17 3.018(13) 161.6 . y N12 H12 I3A 0.88 2.60 3.475(9) 171.5 . y N12 H12 I3D 0.88 2.03 2.85(2) 155.1 . y N10 H10 I4C 0.88 1.98 2.856(14) 170.3 . y N10 H10 I4B 0.88 2.64 3.432(7) 150.8 . y N8 H8 I3B 0.88 2.10 2.955(9) 165.0 2_656 y N6 H6 I1B 0.88 2.86 3.697(5) 160.1 2_656 y N6 H6 I1A 0.88 2.63 3.484(5) 163.4 2_656 y N4 H4 I4A 0.88 2.89 3.596(8) 138.8 4_476 y N2 H2 I1B 0.88 2.85 3.579(6) 141.7 2_556 y _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.211 _refine_diff_density_min -2.775 _refine_diff_density_rms 0.177 # SQUEEZE RESULTS (APPEND TO CIF) 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 0.271 0.078 0.877 21 3 ' ' 2 0.475 0.221 0.506 73 6 ' ' 3 0.819 0.144 0.706 14 2 ' ' 4 0.475 0.279 1.006 73 6 ' ' 5 0.819 0.356 0.206 14 2 ' ' 6 0.271 0.422 0.377 21 3 ' ' 7 0.729 0.578 0.623 21 2 ' ' 8 0.525 0.721 0.994 73 6 ' ' 9 0.181 0.644 0.794 14 2 ' ' 10 0.525 0.779 0.494 73 6 ' ' 11 0.181 0.856 0.294 14 2 ' ' 12 0.729 0.922 0.123 21 2 ' ' _platon_squeeze_details ; Structure contains solvent accessible voids of 434.5 A3/per unit cell, i.e. some 4.4% of the total volume. Data were corrected for disordered electron density through use of the SQUEEZE procedure. Attempts to refine peaks of residual electron density as solvent water molecules were unsuccessful. Derived values (formula weight, density, absorption coefficient) do not contain the contribution of the disordered solvent molecule. ; _vrf_PLAT220_fwi-14 ; PROBLEM: PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: This large range may be attributed to the basic structural network which might best be described as systematic disorder for C atom. PROBLEM: PLAT220_ALERT_2_B Large Non-Solvent I Ueq(max)/Ueq(min) RESPONSE: This large range may be attributed to the basic structural network which might best be described as systematic disorder for I anions. ; _vrf_PLAT241_fwi-14 ; PROBLEM: Check High Ueq as Compared to Neighbors for N20 Check High Ueq as Compared to Neighbors for C79 Check High Ueq as Compared to Neighbors for N4 Check High Ueq as Compared to Neighbors for C14 Check High Ueq as Compared to Neighbors for C31 Check High Ueq as Compared to Neighbors for C47 Check High Ueq as Compared to Neighbors for C53 Check High Ueq as Compared to Neighbors for C86 RESPONSE: these atoms are disordered. ; _vrf_PLAT420_fwi-14 ; PROBLEM: D-H Without Acceptor N2 - H2 ... ? D-H Without Acceptor N8 - H8 ... ? D-H Without Acceptor N14 - H14 ... ? D-H Without Acceptor N18 - H18 ... ? D-H Without Acceptor N24 - H24 ... ? RESPONSE: The possible acceptors are solvent molecules (water). They are disordered without refinment. ; _vrf_PLAT234_fwi-14 ; PROBLEM: Large Hirshfeld Difference N4 -- C16 Large Hirshfeld Difference C13 -- C14 Large Hirshfeld Difference C29 -- C30 Large Hirshfeld Difference C45 -- C46 Large Hirshfeld Difference C46 -- C47 Large Hirshfeld Difference C51 -- C56 Large Hirshfeld Difference C70 -- C71 Large Hirshfeld Difference C85 -- C86 Large Hirshfeld Difference C86 -- C87 Large Hirshfeld Difference C93 -- C94 RESPONSE: these atoms are also disordered. ; # end Validation Reply Form