# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiao-Zeng Li' _publ_contact_author_email lixiaozeng321@tju.edu.cn loop_ _publ_author_name 'Xiao-Zeng Li' 'Peng-Peng Hao' 'Dan Wang' 'Wenqin Zhang' 'Li-Na Zhu' data_x _database_code_depnum_ccdc_archive 'CCDC 839539' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H120 N16 Na8 Ni4 O48' _chemical_formula_weight 2828.88 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' Na Na 0.0362 0.0249 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.433(12) _cell_length_b 12.141(3) _cell_length_c 30.332(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.958(7) _cell_angle_gamma 90.00 _cell_volume 12129(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5736 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8664 _exptl_absorpt_correction_T_max 0.8664 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41950 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10679 _reflns_number_gt 9273 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; The restraints (dfix, isorsimu) are applied to keep the bond geometries and dsps of ethanol and water molecules structurally reasonable. ISOR 0.008 O24 ISOR 0.01 O18 O24 simu 0.01 0.02 o21 > c54' dfix 1.55 0.01 c53 c54 c53' c54' dfix 1.40 0.01 o21 c53 o21' c53' Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+84.2653P] 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 10679 _refine_ls_number_parameters 896 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2068 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.000 _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 0.36970(2) 0.12034(5) 0.57204(2) 0.02337(19) Uani 1 1 d . . . Ni2 Ni 0.41252(2) -0.13002(5) 0.43147(2) 0.02215(18) Uani 1 1 d . . . O1 O 0.31431(12) 0.2206(3) 0.44933(12) 0.0315(9) Uani 1 1 d . C . O2 O 0.33627(12) 0.0058(3) 0.44765(12) 0.0300(8) Uani 1 1 d . C . O3 O 0.46769(12) -0.1835(3) 0.65323(13) 0.0336(9) Uani 1 1 d . . . O4 O 0.42261(12) -0.1466(3) 0.69143(12) 0.0317(9) Uani 1 1 d . . . O5 O 0.36911(15) 0.3602(4) 0.69602(14) 0.0429(11) Uani 1 1 d . . . O6 O 0.38965(13) 0.4922(3) 0.65550(14) 0.0371(10) Uani 1 1 d . . . O7 O 0.48664(11) -0.1184(3) 0.55550(12) 0.0280(8) Uani 1 1 d . . . O8 O 0.46095(13) -0.3253(3) 0.53464(13) 0.0352(9) Uani 1 1 d . . . O9 O 0.32570(14) -0.3847(3) 0.30608(14) 0.0411(10) Uani 1 1 d . . . O10 O 0.29489(13) -0.2324(4) 0.32049(14) 0.0397(10) Uani 1 1 d . . . O11 O 0.36274(12) 0.2100(3) 0.36170(13) 0.0299(8) Uani 1 1 d . C . O12 O 0.42750(11) 0.2494(3) 0.36565(12) 0.0283(8) Uani 1 1 d . . . N1 N 0.35447(13) 0.0096(3) 0.52847(14) 0.0231(9) Uani 1 1 d . . . N2 N 0.40812(14) 0.0318(3) 0.61398(15) 0.0255(9) Uani 1 1 d . . . N3 N 0.38548(14) 0.2339(4) 0.61530(15) 0.0271(10) Uani 1 1 d . . . N4 N 0.33383(13) 0.2098(3) 0.52939(15) 0.0251(9) Uani 1 1 d . . . N5 N 0.41584(14) -0.2594(3) 0.46643(14) 0.0243(9) Uani 1 1 d . . . N6 N 0.38302(14) -0.1981(3) 0.37660(14) 0.0254(9) Uani 1 1 d . . . N7 N 0.41101(14) -0.0040(4) 0.39493(15) 0.0252(9) Uani 1 1 d . . . N8 N 0.44121(13) -0.0597(3) 0.48609(14) 0.0219(9) Uani 1 1 d . . . C1 C 0.32842(16) 0.1734(4) 0.48602(18) 0.0263(11) Uani 1 1 d . . . C2 C 0.34114(15) 0.0503(4) 0.48545(18) 0.0237(11) Uani 1 1 d . . . C3 C 0.35698(16) -0.1048(4) 0.53783(18) 0.0241(11) Uani 1 1 d . . . C4 C 0.33271(17) -0.1800(4) 0.50612(19) 0.0285(12) Uani 1 1 d . . . H4 H 0.3168 -0.1545 0.4768 0.034 Uiso 1 1 calc R . . C5 C 0.33175(17) -0.2897(4) 0.51696(19) 0.0301(12) Uani 1 1 d . . . H5 H 0.3145 -0.3384 0.4954 0.036 Uiso 1 1 calc R . . C6 C 0.35565(18) -0.3304(4) 0.55898(19) 0.0308(12) Uani 1 1 d . . . H6 H 0.3549 -0.4063 0.5662 0.037 Uiso 1 1 calc R . . C7 C 0.38028(18) -0.2594(4) 0.58984(19) 0.0296(12) Uani 1 1 d . . . H7 H 0.3971 -0.2876 0.6182 0.036 Uiso 1 1 calc R . . C8 C 0.38148(17) -0.1449(4) 0.58074(18) 0.0260(11) Uani 1 1 d . . . C9 C 0.40853(16) -0.0769(4) 0.61616(17) 0.0257(11) Uani 1 1 d . . . C10 C 0.43600(17) -0.1414(4) 0.65754(17) 0.0258(11) Uani 1 1 d . . . C11 C 0.43724(17) 0.1004(4) 0.64462(18) 0.0278(12) Uani 1 1 d . . . C12 C 0.47743(19) 0.0715(5) 0.6682(2) 0.0400(14) Uani 1 1 d . . . H12 H 0.4865 -0.0020 0.6670 0.048 Uiso 1 1 calc R . . C13 C 0.5036(2) 0.1501(6) 0.6931(2) 0.0510(18) Uani 1 1 d . . . H13 H 0.5305 0.1295 0.7100 0.061 Uiso 1 1 calc R . . C14 C 0.4916(2) 0.2582(5) 0.6940(2) 0.0450(16) Uani 1 1 d . . . H14 H 0.5102 0.3111 0.7113 0.054 Uiso 1 1 calc R . . C15 C 0.45265(19) 0.2899(5) 0.6699(2) 0.0369(14) Uani 1 1 d . . . H15 H 0.4447 0.3649 0.6698 0.044 Uiso 1 1 calc R . . C16 C 0.42486(17) 0.2110(4) 0.64541(18) 0.0284(12) Uani 1 1 d . . . C17 C 0.36416(18) 0.3218(4) 0.61822(19) 0.0297(12) Uani 1 1 d . . . C18 C 0.37609(19) 0.3988(5) 0.6603(2) 0.0354(13) Uani 1 1 d . . . C19 C 0.32729(17) 0.3531(4) 0.5836(2) 0.0296(12) Uani 1 1 d . . . C20 C 0.30366(18) 0.4407(5) 0.5938(2) 0.0337(13) Uani 1 1 d . . . H20 H 0.3113 0.4715 0.6239 0.040 Uiso 1 1 calc R . . C21 C 0.27027(19) 0.4817(5) 0.5613(2) 0.0381(14) Uani 1 1 d . . . H21 H 0.2547 0.5390 0.5692 0.046 Uiso 1 1 calc R . . C22 C 0.25943(18) 0.4392(5) 0.5173(2) 0.0335(13) Uani 1 1 d . . . H22 H 0.2369 0.4693 0.4945 0.040 Uiso 1 1 calc R . . C23 C 0.28104(17) 0.3530(4) 0.50584(19) 0.0277(11) Uani 1 1 d . . . H23 H 0.2731 0.3252 0.4752 0.033 Uiso 1 1 calc R . . C24 C 0.31426(16) 0.3061(4) 0.53855(18) 0.0246(11) Uani 1 1 d . . . C25 C 0.46086(16) -0.1338(4) 0.51845(18) 0.0252(11) Uani 1 1 d . . . C26 C 0.44566(16) -0.2526(4) 0.50651(17) 0.0253(11) Uani 1 1 d . . . C27 C 0.39097(16) -0.3530(4) 0.45410(18) 0.0245(11) Uani 1 1 d . . . C28 C 0.39435(18) -0.4454(4) 0.48353(18) 0.0277(12) Uani 1 1 d . . . H28 H 0.4163 -0.4490 0.5111 0.033 Uiso 1 1 calc R . . C29 C 0.36629(18) -0.5306(4) 0.4729(2) 0.0324(13) Uani 1 1 d . . . H29 H 0.3693 -0.5912 0.4934 0.039 Uiso 1 1 calc R . . C30 C 0.33428(18) -0.5292(4) 0.4332(2) 0.0326(13) Uani 1 1 d . . . H30 H 0.3146 -0.5865 0.4271 0.039 Uiso 1 1 calc R . . C31 C 0.33104(18) -0.4438(4) 0.40274(19) 0.0312(12) Uani 1 1 d . . . H31 H 0.3091 -0.4434 0.3751 0.037 Uiso 1 1 calc R . . C32 C 0.35964(17) -0.3559(4) 0.41128(18) 0.0267(11) Uani 1 1 d . . . C33 C 0.35746(17) -0.2797(4) 0.37345(18) 0.0270(11) Uani 1 1 d . . . C34 C 0.32350(18) -0.3010(5) 0.32917(19) 0.0321(13) Uani 1 1 d . . . C35 C 0.38606(17) -0.1393(4) 0.33712(18) 0.0264(11) Uani 1 1 d . . . C36 C 0.37876(18) -0.1830(5) 0.29293(19) 0.0328(13) Uani 1 1 d . . . H36 H 0.3695 -0.2568 0.2868 0.039 Uiso 1 1 calc R . . C37 C 0.38507(19) -0.1187(5) 0.2581(2) 0.0364(14) Uani 1 1 d . . . H37 H 0.3789 -0.1470 0.2276 0.044 Uiso 1 1 calc R . . C38 C 0.4004(2) -0.0123(5) 0.2675(2) 0.0415(15) Uani 1 1 d . . . H38 H 0.4047 0.0318 0.2434 0.050 Uiso 1 1 calc R . . C39 C 0.4096(2) 0.0295(5) 0.3119(2) 0.0388(14) Uani 1 1 d . . . H39 H 0.4212 0.1008 0.3184 0.047 Uiso 1 1 calc R . . C40 C 0.40187(17) -0.0321(4) 0.34706(18) 0.0277(12) Uani 1 1 d . . . C41 C 0.41389(16) 0.0981(4) 0.40965(18) 0.0242(11) Uani 1 1 d . . . C42 C 0.40002(17) 0.1944(4) 0.37541(18) 0.0271(12) Uani 1 1 d . . . C43 C 0.42816(16) 0.1293(4) 0.45801(18) 0.0238(11) Uani 1 1 d . . . C44 C 0.42887(17) 0.2426(4) 0.46826(19) 0.0285(12) Uani 1 1 d . . . H44 H 0.4170 0.2929 0.4441 0.034 Uiso 1 1 calc R . . C45 C 0.44605(19) 0.2829(5) 0.5118(2) 0.0350(13) Uani 1 1 d . . . H45 H 0.4458 0.3597 0.5177 0.042 Uiso 1 1 calc R . . C46 C 0.46379(18) 0.2102(5) 0.5471(2) 0.0313(12) Uani 1 1 d . . . H46 H 0.4764 0.2374 0.5773 0.038 Uiso 1 1 calc R . . C47 C 0.46319(17) 0.0975(4) 0.53865(18) 0.0285(12) Uani 1 1 d . . . H47 H 0.4756 0.0488 0.5632 0.034 Uiso 1 1 calc R . . C48 C 0.44463(16) 0.0540(4) 0.49438(18) 0.0242(11) Uani 1 1 d . . . Na1 Na 0.49741(7) 0.26135(17) 0.39387(7) 0.0284(5) Uani 1 1 d . . . Na2 Na 0.42121(7) 0.37355(17) 0.30109(7) 0.0282(5) Uani 1 1 d . . . Na3 Na 0.31697(8) 0.3490(3) 0.23130(10) 0.0582(8) Uani 1 1 d . . . Na4 Na 0.31002(7) 0.1291(2) 0.38226(7) 0.0358(5) Uani 1 1 d . . . O14 O 0.46461(13) 0.2567(3) 0.27455(14) 0.0383(10) Uani 1 1 d . . . H14E H 0.4810 0.2240 0.2972 0.058 Uiso 1 1 d R . . H14D H 0.4569 0.2238 0.2487 0.058 Uiso 1 1 d R . . O15 O 0.35441(12) 0.3976(3) 0.30763(13) 0.0357(9) Uani 1 1 d . A . O16 O 0.37962(13) 0.3353(3) 0.21515(14) 0.0366(9) Uani 1 1 d . A . O13 O 0.48583(14) 0.4323(3) 0.35697(14) 0.0402(10) Uani 1 1 d . . . H13A H 0.5026 0.4402 0.3414 0.060 Uiso 1 1 d R . . C49 C 0.4905(2) 0.5287(6) 0.3836(3) 0.0534(18) Uani 1 1 d . . . H49A H 0.4818 0.5938 0.3634 0.064 Uiso 1 1 calc R . . H49B H 0.5193 0.5386 0.4016 0.064 Uiso 1 1 calc R . . C50 C 0.4653(2) 0.5161(6) 0.4142(3) 0.062(2) Uani 1 1 d . . . H50A H 0.4375 0.4976 0.3961 0.093 Uiso 1 1 calc R . . H50B H 0.4651 0.5851 0.4308 0.093 Uiso 1 1 calc R . . H50C H 0.4762 0.4569 0.4363 0.093 Uiso 1 1 calc R . . O19 O 0.27864(19) 0.3069(6) 0.1541(2) 0.0798(19) Uani 1 1 d . A . H19A H 0.2557 0.3495 0.1381 0.096 Uiso 1 1 calc R . . C51 C 0.2913(3) 0.2180(9) 0.1337(3) 0.079(3) Uani 1 1 d . . . H51A H 0.2929 0.1530 0.1539 0.094 Uiso 1 1 calc R A . H51B H 0.3191 0.2331 0.1321 0.094 Uiso 1 1 calc R . . C52 C 0.2662(3) 0.1896(8) 0.0878(3) 0.077(3) Uani 1 1 d . A . H52A H 0.2376 0.1875 0.0875 0.116 Uiso 1 1 calc R . . H52B H 0.2742 0.1171 0.0792 0.116 Uiso 1 1 calc R . . H52C H 0.2697 0.2449 0.0658 0.116 Uiso 1 1 calc R . . O22 O 0.30216(16) 0.5396(4) 0.21857(15) 0.0558(13) Uani 1 1 d . A . H22A H 0.3181 0.5888 0.2140 0.084 Uiso 1 1 d R . . H22B H 0.2770 0.5545 0.2098 0.084 Uiso 1 1 d R . . O23 O 0.42930(18) 0.5480(4) 0.26950(18) 0.0360(12) Uani 0.85 1 d P . . O23' O 0.4119(11) 0.561(2) 0.2843(11) 0.038(7) Uani 0.15 1 d P . . O24 O 0.5314(3) 0.4426(7) 0.2938(3) 0.112(3) Uani 1 1 d U . . O17 O 0.2764(3) 0.2280(9) 0.2497(3) 0.047(2) Uani 0.50 1 d P A 1 O18 O 0.2967(6) 0.0333(17) 0.2596(7) 0.134(6) Uani 0.50 1 d PU B 1 O20 O 0.2765(5) -0.0039(12) 0.3381(6) 0.082(4) Uani 0.50 1 d P C 1 O21 O 0.2679(3) 0.2804(9) 0.3413(4) 0.052(2) Uani 0.50 1 d PDU C 1 C53 C 0.2259(4) 0.3009(17) 0.3331(7) 0.076(3) Uani 0.50 1 d PDU C 1 H53A H 0.2118 0.2315 0.3360 0.091 Uiso 0.50 1 calc PR C 1 H53B H 0.2142 0.3293 0.3014 0.091 Uiso 0.50 1 calc PR C 1 C54 C 0.2198(5) 0.3859(16) 0.3682(6) 0.072(4) Uani 0.50 1 d PDU C 1 H54A H 0.1915 0.4113 0.3587 0.108 Uiso 0.50 1 calc PR C 1 H54B H 0.2379 0.4487 0.3694 0.108 Uiso 0.50 1 calc PR C 1 H54C H 0.2259 0.3517 0.3987 0.108 Uiso 0.50 1 calc PR C 1 O17' O 0.2544(3) 0.3371(10) 0.2599(4) 0.064(3) Uani 0.50 1 d P A 2 O18' O 0.3197(5) 0.1482(13) 0.2583(5) 0.101(5) Uani 0.50 1 d P A 2 O20' O 0.2893(4) 0.0106(10) 0.3160(4) 0.057(3) Uani 0.50 1 d P C 2 O21' O 0.2545(4) 0.2230(11) 0.3371(4) 0.069(3) Uani 0.50 1 d PDU C 2 C53' C 0.2337(5) 0.2952(13) 0.3598(6) 0.066(3) Uani 0.50 1 d PDU C 2 H53C H 0.2518 0.3194 0.3900 0.079 Uiso 0.50 1 calc PR C 2 H53D H 0.2095 0.2588 0.3645 0.079 Uiso 0.50 1 calc PR C 2 C54' C 0.2212(9) 0.394(2) 0.3260(9) 0.131(6) Uani 0.50 1 d PDU C 2 H54D H 0.2107 0.3669 0.2943 0.196 Uiso 0.50 1 calc PR C 2 H54E H 0.2449 0.4411 0.3284 0.196 Uiso 0.50 1 calc PR C 2 H54F H 0.2001 0.4374 0.3339 0.196 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0290(4) 0.0152(3) 0.0249(4) 0.0011(2) 0.0062(3) -0.0012(3) Ni2 0.0297(4) 0.0142(3) 0.0226(4) 0.0017(2) 0.0075(3) -0.0016(3) O1 0.041(2) 0.0236(19) 0.027(2) 0.0071(16) 0.0066(17) 0.0019(17) O2 0.037(2) 0.028(2) 0.026(2) -0.0004(16) 0.0095(16) 0.0021(17) O3 0.034(2) 0.033(2) 0.034(2) 0.0030(17) 0.0096(17) 0.0108(18) O4 0.047(2) 0.025(2) 0.025(2) 0.0018(15) 0.0123(17) 0.0042(18) O5 0.065(3) 0.034(2) 0.031(2) -0.0037(18) 0.016(2) -0.015(2) O6 0.049(3) 0.0187(19) 0.045(2) -0.0031(17) 0.016(2) -0.0073(18) O7 0.030(2) 0.0219(19) 0.028(2) 0.0016(15) 0.0032(17) -0.0019(16) O8 0.050(3) 0.0173(19) 0.032(2) 0.0064(16) 0.0013(18) 0.0015(18) O9 0.061(3) 0.026(2) 0.031(2) -0.0031(17) 0.004(2) -0.003(2) O10 0.037(2) 0.038(2) 0.040(2) 0.0041(19) 0.0056(19) -0.001(2) O11 0.031(2) 0.0240(19) 0.034(2) 0.0049(16) 0.0089(17) 0.0005(16) O12 0.031(2) 0.0189(18) 0.035(2) 0.0071(15) 0.0104(16) 0.0027(16) N1 0.024(2) 0.017(2) 0.027(2) 0.0018(17) 0.0073(18) 0.0006(17) N2 0.031(2) 0.016(2) 0.029(2) 0.0004(17) 0.0077(19) -0.0001(18) N3 0.033(2) 0.021(2) 0.026(2) 0.0021(18) 0.0057(19) -0.0034(19) N4 0.030(2) 0.016(2) 0.031(2) 0.0027(17) 0.0116(19) 0.0002(18) N5 0.035(2) 0.015(2) 0.023(2) -0.0001(16) 0.0076(19) -0.0032(18) N6 0.033(2) 0.015(2) 0.026(2) 0.0030(17) 0.0071(19) -0.0011(18) N7 0.031(2) 0.018(2) 0.027(2) 0.0028(17) 0.0098(19) 0.0012(18) N8 0.029(2) 0.013(2) 0.023(2) -0.0004(16) 0.0062(18) -0.0011(17) C1 0.024(3) 0.022(3) 0.032(3) 0.003(2) 0.007(2) -0.007(2) C2 0.019(2) 0.022(3) 0.031(3) 0.002(2) 0.009(2) -0.003(2) C3 0.027(3) 0.017(2) 0.032(3) 0.000(2) 0.014(2) -0.002(2) C4 0.034(3) 0.023(3) 0.029(3) -0.003(2) 0.010(2) -0.002(2) C5 0.033(3) 0.021(3) 0.038(3) -0.008(2) 0.012(2) -0.006(2) C6 0.041(3) 0.018(3) 0.039(3) -0.002(2) 0.020(3) 0.001(2) C7 0.045(3) 0.017(3) 0.028(3) 0.004(2) 0.013(2) 0.006(2) C8 0.035(3) 0.015(2) 0.030(3) 0.002(2) 0.014(2) -0.001(2) C9 0.028(3) 0.025(3) 0.027(3) 0.002(2) 0.011(2) 0.002(2) C10 0.035(3) 0.016(2) 0.024(3) 0.001(2) 0.005(2) 0.001(2) C11 0.032(3) 0.023(3) 0.025(3) 0.003(2) 0.003(2) -0.005(2) C12 0.039(3) 0.030(3) 0.045(4) 0.005(3) 0.002(3) -0.001(3) C13 0.037(4) 0.045(4) 0.055(4) 0.008(3) -0.011(3) -0.004(3) C14 0.043(4) 0.034(3) 0.051(4) -0.001(3) 0.002(3) -0.012(3) C15 0.043(3) 0.027(3) 0.036(3) 0.000(2) 0.003(3) -0.011(3) C16 0.037(3) 0.019(3) 0.027(3) 0.002(2) 0.005(2) -0.005(2) C17 0.038(3) 0.018(3) 0.037(3) 0.000(2) 0.018(3) -0.008(2) C18 0.045(4) 0.024(3) 0.038(3) -0.004(2) 0.014(3) 0.000(3) C19 0.035(3) 0.017(3) 0.040(3) 0.002(2) 0.016(3) 0.003(2) C20 0.038(3) 0.022(3) 0.045(3) -0.007(2) 0.019(3) -0.004(2) C21 0.039(3) 0.021(3) 0.058(4) 0.001(3) 0.020(3) 0.004(3) C22 0.030(3) 0.024(3) 0.048(3) 0.004(2) 0.013(3) -0.001(2) C23 0.032(3) 0.019(3) 0.031(3) 0.005(2) 0.008(2) -0.001(2) C24 0.027(3) 0.015(2) 0.035(3) 0.002(2) 0.014(2) -0.004(2) C25 0.031(3) 0.018(3) 0.028(3) 0.002(2) 0.010(2) 0.003(2) C26 0.030(3) 0.021(3) 0.027(3) -0.001(2) 0.011(2) 0.004(2) C27 0.032(3) 0.014(2) 0.029(3) 0.001(2) 0.013(2) -0.002(2) C28 0.040(3) 0.014(2) 0.031(3) 0.003(2) 0.013(2) 0.001(2) C29 0.042(3) 0.018(3) 0.043(3) 0.005(2) 0.022(3) 0.003(2) C30 0.040(3) 0.017(3) 0.047(3) -0.005(2) 0.022(3) -0.006(2) C31 0.037(3) 0.023(3) 0.033(3) -0.002(2) 0.011(2) -0.005(2) C32 0.035(3) 0.018(3) 0.028(3) 0.000(2) 0.011(2) 0.000(2) C33 0.034(3) 0.021(3) 0.027(3) 0.001(2) 0.010(2) 0.000(2) C34 0.040(3) 0.022(3) 0.032(3) 0.003(2) 0.007(3) -0.004(2) C35 0.032(3) 0.021(3) 0.025(3) 0.003(2) 0.007(2) 0.000(2) C36 0.037(3) 0.030(3) 0.031(3) -0.002(2) 0.010(2) 0.002(2) C37 0.048(4) 0.035(3) 0.027(3) 0.001(2) 0.013(3) 0.001(3) C38 0.063(4) 0.035(3) 0.032(3) 0.007(3) 0.021(3) 0.007(3) C39 0.062(4) 0.023(3) 0.037(3) 0.003(2) 0.022(3) 0.002(3) C40 0.035(3) 0.024(3) 0.026(3) 0.003(2) 0.011(2) 0.000(2) C41 0.026(3) 0.021(3) 0.029(3) 0.001(2) 0.013(2) 0.003(2) C42 0.037(3) 0.017(3) 0.028(3) -0.001(2) 0.012(2) -0.002(2) C43 0.031(3) 0.016(2) 0.026(3) 0.000(2) 0.011(2) -0.001(2) C44 0.038(3) 0.017(3) 0.033(3) 0.003(2) 0.014(2) 0.004(2) C45 0.045(3) 0.024(3) 0.039(3) 0.001(2) 0.016(3) 0.000(3) C46 0.038(3) 0.023(3) 0.033(3) -0.002(2) 0.011(2) -0.001(2) C47 0.037(3) 0.020(3) 0.027(3) -0.001(2) 0.007(2) 0.000(2) C48 0.026(3) 0.014(2) 0.035(3) 0.001(2) 0.012(2) -0.002(2) Na1 0.0352(12) 0.0194(10) 0.0288(11) 0.0032(8) 0.0066(9) 0.0029(9) Na2 0.0340(11) 0.0204(10) 0.0297(11) 0.0042(8) 0.0087(9) 0.0018(9) Na3 0.0409(15) 0.069(2) 0.0600(18) -0.0268(15) 0.0071(13) -0.0055(14) Na4 0.0364(12) 0.0417(14) 0.0282(12) 0.0063(9) 0.0076(10) -0.0068(10) O14 0.041(2) 0.036(2) 0.034(2) -0.0091(18) 0.0032(18) 0.0085(19) O15 0.039(2) 0.032(2) 0.036(2) 0.0049(17) 0.0100(18) 0.0072(18) O16 0.040(2) 0.027(2) 0.042(2) 0.0010(17) 0.0108(19) 0.0000(18) O13 0.053(3) 0.025(2) 0.037(2) 0.0045(17) 0.0036(19) -0.0101(19) C49 0.066(5) 0.038(4) 0.055(4) -0.008(3) 0.016(4) -0.004(3) C50 0.051(4) 0.037(4) 0.110(7) -0.009(4) 0.042(4) 0.004(3) O19 0.067(4) 0.102(5) 0.068(4) -0.033(4) 0.016(3) 0.004(4) C51 0.075(6) 0.093(7) 0.079(6) -0.031(5) 0.039(5) -0.010(5) C52 0.087(7) 0.088(7) 0.065(5) -0.023(5) 0.037(5) -0.038(6) O22 0.062(3) 0.065(3) 0.034(2) 0.002(2) 0.003(2) 0.004(3) O23 0.047(3) 0.024(3) 0.032(3) 0.002(2) 0.004(2) -0.005(2) O23' 0.07(2) 0.005(12) 0.046(19) -0.003(11) 0.025(16) 0.006(13) O24 0.126(5) 0.103(5) 0.131(5) -0.028(4) 0.074(4) -0.022(4) O17 0.033(5) 0.074(7) 0.031(5) -0.003(4) 0.004(4) -0.017(5) O18 0.136(10) 0.129(10) 0.149(10) -0.002(8) 0.058(8) -0.001(8) O20 0.075(10) 0.048(8) 0.100(12) -0.032(8) -0.010(8) -0.001(7) O21 0.036(5) 0.038(5) 0.076(5) 0.001(5) 0.010(4) 0.000(4) C53 0.059(6) 0.068(6) 0.090(6) 0.002(7) 0.004(6) 0.013(5) C54 0.052(8) 0.088(10) 0.083(9) -0.005(8) 0.030(7) 0.005(7) O17' 0.060(7) 0.075(8) 0.057(6) -0.004(6) 0.017(5) -0.014(6) O18' 0.121(13) 0.077(10) 0.117(12) 0.034(8) 0.055(10) 0.008(9) O20' 0.075(9) 0.043(6) 0.044(7) -0.001(5) 0.001(6) -0.022(6) O21' 0.048(5) 0.076(6) 0.078(5) 0.011(6) 0.009(5) 0.022(5) C53' 0.049(5) 0.061(6) 0.080(6) 0.005(6) 0.009(6) 0.010(5) C54' 0.105(11) 0.116(11) 0.136(11) -0.004(11) -0.019(11) 0.014(10) _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 1.850(4) . ? Ni1 N4 1.857(4) . ? Ni1 N3 1.872(4) . ? Ni1 N2 1.882(4) . ? Ni2 N8 1.870(4) . ? Ni2 N6 1.871(4) . ? Ni2 N5 1.880(4) . ? Ni2 N7 1.880(4) . ? O1 C1 1.220(6) . ? O1 Na4 2.284(4) . ? O2 C2 1.234(6) . ? O2 Na4 2.438(4) . ? O3 C10 1.246(7) . ? O3 Na1 2.319(4) 5_656 ? O4 C10 1.245(6) . ? O5 C18 1.265(7) . ? O6 C18 1.251(7) . ? O7 C25 1.227(6) . ? O7 Na1 2.276(4) 5_656 ? O8 C26 1.234(6) . ? O8 Na1 2.355(4) 5_656 ? O9 C34 1.249(7) . ? O10 C34 1.258(7) . ? O11 C42 1.243(7) . ? O11 Na4 2.304(4) . ? O12 C42 1.261(7) . ? O12 Na1 2.312(4) . ? O12 Na2 2.431(4) . ? N1 C2 1.345(7) . ? N1 C3 1.416(6) . ? N2 C9 1.321(7) . ? N2 C11 1.421(7) . ? N3 C17 1.313(7) . ? N3 C16 1.424(7) . ? N4 C1 1.348(7) . ? N4 C24 1.417(7) . ? N5 C26 1.346(7) . ? N5 C27 1.407(6) . ? N6 C33 1.310(7) . ? N6 C35 1.425(7) . ? N7 C41 1.312(7) . ? N7 C40 1.434(7) . ? N8 C25 1.358(7) . ? N8 C48 1.401(6) . ? C1 C2 1.558(7) . ? C3 C4 1.410(7) . ? C3 C8 1.415(8) . ? C4 C5 1.374(8) . ? C4 H4 0.9500 . ? C5 C6 1.390(8) . ? C5 H5 0.9500 . ? C6 C7 1.369(8) . ? C6 H6 0.9500 . ? C7 C8 1.420(7) . ? C7 H7 0.9500 . ? C8 C9 1.456(7) . ? C9 C10 1.546(7) . ? C11 C12 1.404(8) . ? C11 C16 1.411(8) . ? C12 C13 1.378(9) . ? C12 H12 0.9500 . ? C13 C14 1.378(10) . ? C13 H13 0.9500 . ? C14 C15 1.382(9) . ? C14 H14 0.9500 . ? C15 C16 1.403(8) . ? C15 H15 0.9500 . ? C17 C19 1.442(8) . ? C17 C18 1.538(8) . ? C19 C20 1.426(8) . ? C19 C24 1.427(8) . ? C20 C21 1.370(9) . ? C20 H20 0.9500 . ? C21 C22 1.379(9) . ? C21 H21 0.9500 . ? C22 C23 1.385(8) . ? C22 H22 0.9500 . ? C23 C24 1.398(7) . ? C23 H23 0.9500 . ? C25 C26 1.540(7) . ? C25 Na1 3.051(6) 5_656 ? C26 Na1 3.087(6) 5_656 ? C27 C28 1.417(7) . ? C27 C32 1.426(8) . ? C28 C29 1.388(8) . ? C28 H28 0.9500 . ? C29 C30 1.373(8) . ? C29 H29 0.9500 . ? C30 C31 1.372(8) . ? C30 H30 0.9500 . ? C31 C32 1.424(8) . ? C31 H31 0.9500 . ? C32 C33 1.458(7) . ? C33 C34 1.524(8) . ? C35 C36 1.395(8) . ? C35 C40 1.408(7) . ? C36 C37 1.382(8) . ? C36 H36 0.9500 . ? C37 C38 1.394(9) . ? C37 H37 0.9500 . ? C38 C39 1.387(8) . ? C38 H38 0.9500 . ? C39 C40 1.390(8) . ? C39 H39 0.9500 . ? C41 C43 1.455(7) . ? C41 C42 1.545(7) . ? C43 C44 1.409(7) . ? C43 C48 1.417(7) . ? C44 C45 1.371(8) . ? C44 H44 0.9500 . ? C45 C46 1.385(8) . ? C45 H45 0.9500 . ? C46 C47 1.391(7) . ? C46 H46 0.9500 . ? C47 C48 1.411(7) . ? C47 H47 0.9500 . ? Na1 O7 2.276(4) 5_656 ? Na1 O3 2.319(4) 5_656 ? Na1 O13 2.336(4) . ? Na1 O8 2.355(4) 5_656 ? Na1 C25 3.051(6) 5_656 ? Na1 C26 3.087(6) 5_656 ? Na2 O23' 2.33(3) . ? Na2 O14 2.366(4) . ? Na2 O23 2.374(5) . ? Na2 O15 2.384(5) . ? Na2 O13 2.476(5) . ? Na2 O16 2.624(5) . ? Na3 O17 2.209(10) . ? Na3 O16 2.353(5) . ? Na3 O15 2.373(5) . ? Na3 O22 2.377(6) . ? Na3 O19 2.385(6) . ? Na3 O17' 2.552(11) . ? Na3 O18' 2.564(15) . ? Na4 O20 2.198(13) . ? Na4 O21' 2.302(11) . ? Na4 O20' 2.404(13) . ? Na4 O21 2.444(11) . ? O14 H14E 0.8497 . ? O14 H14D 0.8506 . ? O13 C49 1.404(8) . ? O13 H13A 0.8502 . ? C49 C50 1.452(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O19 C51 1.377(10) . ? O19 H19A 0.9500 . ? C51 C52 1.450(12) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O22 H22A 0.8502 . ? O22 H22B 0.8499 . ? O21 C53 1.415(9) . ? C53 C54 1.541(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O21' C53' 1.430(10) . ? C53' C54' 1.558(10) . ? C53' H53C 0.9900 . ? C53' H53D 0.9900 . ? C54' H54D 0.9800 . ? C54' H54E 0.9800 . ? C54' H54F 0.9800 . ? 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 N4 86.28(19) . . ? N1 Ni1 N3 178.9(2) . . ? N4 Ni1 N3 93.18(19) . . ? N1 Ni1 N2 93.71(18) . . ? N4 Ni1 N2 177.1(2) . . ? N3 Ni1 N2 86.78(19) . . ? N8 Ni2 N6 178.8(2) . . ? N8 Ni2 N5 87.27(18) . . ? N6 Ni2 N5 93.46(18) . . ? N8 Ni2 N7 93.85(19) . . ? N6 Ni2 N7 85.46(18) . . ? N5 Ni2 N7 177.01(19) . . ? C1 O1 Na4 119.3(4) . . ? C2 O2 Na4 113.9(3) . . ? C10 O3 Na1 149.2(4) . 5_656 ? C25 O7 Na1 118.0(3) . 5_656 ? C26 O8 Na1 115.0(3) . 5_656 ? C42 O11 Na4 131.6(3) . . ? C42 O12 Na1 135.9(3) . . ? C42 O12 Na2 128.3(3) . . ? Na1 O12 Na2 95.61(15) . . ? C2 N1 C3 122.6(4) . . ? C2 N1 Ni1 111.8(3) . . ? C3 N1 Ni1 125.6(3) . . ? C9 N2 C11 123.9(5) . . ? C9 N2 Ni1 126.8(4) . . ? C11 N2 Ni1 109.3(3) . . ? C17 N3 C16 124.2(5) . . ? C17 N3 Ni1 126.3(4) . . ? C16 N3 Ni1 109.5(3) . . ? C1 N4 C24 121.6(4) . . ? C1 N4 Ni1 111.2(4) . . ? C24 N4 Ni1 127.2(4) . . ? C26 N5 C27 122.3(4) . . ? C26 N5 Ni2 111.3(3) . . ? C27 N5 Ni2 126.4(3) . . ? C33 N6 C35 122.0(5) . . ? C33 N6 Ni2 125.3(4) . . ? C35 N6 Ni2 111.8(3) . . ? C41 N7 C40 122.8(4) . . ? C41 N7 Ni2 125.6(4) . . ? C40 N7 Ni2 111.3(3) . . ? C25 N8 C48 121.7(4) . . ? C25 N8 Ni2 111.1(3) . . ? C48 N8 Ni2 127.1(3) . . ? O1 C1 N4 129.9(5) . . ? O1 C1 C2 118.6(5) . . ? N4 C1 C2 111.5(4) . . ? O2 C2 N1 131.0(5) . . ? O2 C2 C1 117.9(5) . . ? N1 C2 C1 111.0(4) . . ? C4 C3 C8 118.7(5) . . ? C4 C3 N1 120.6(5) . . ? C8 C3 N1 120.5(5) . . ? C5 C4 C3 121.0(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 119.1(5) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 122.0(5) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C3 C8 C7 118.2(5) . . ? C3 C8 C9 124.4(5) . . ? C7 C8 C9 117.4(5) . . ? N2 C9 C8 122.3(5) . . ? N2 C9 C10 122.8(5) . . ? C8 C9 C10 114.8(4) . . ? O4 C10 O3 127.8(5) . . ? O4 C10 C9 114.2(5) . . ? O3 C10 C9 118.0(5) . . ? C12 C11 C16 119.1(5) . . ? C12 C11 N2 126.1(5) . . ? C16 C11 N2 114.2(5) . . ? C13 C12 C11 119.8(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 121.2(6) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.8(6) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 119.7(5) . . ? C15 C16 N3 125.5(5) . . ? C11 C16 N3 114.2(5) . . ? N3 C17 C19 123.8(5) . . ? N3 C17 C18 122.0(5) . . ? C19 C17 C18 114.2(5) . . ? O6 C18 O5 127.3(5) . . ? O6 C18 C17 118.2(5) . . ? O5 C18 C17 114.5(5) . . ? C20 C19 C24 117.7(5) . . ? C20 C19 C17 118.4(5) . . ? C24 C19 C17 123.8(5) . . ? C21 C20 C19 121.9(6) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.6(6) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 120.8(6) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 121.2(5) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 N4 122.3(5) . . ? C23 C24 C19 118.7(5) . . ? N4 C24 C19 118.9(5) . . ? O7 C25 N8 129.5(5) . . ? O7 C25 C26 117.7(4) . . ? N8 C25 C26 112.8(4) . . ? O7 C25 Na1 41.2(2) . 5_656 ? N8 C25 Na1 167.2(4) . 5_656 ? C26 C25 Na1 76.8(3) . 5_656 ? O8 C26 N5 129.8(5) . . ? O8 C26 C25 117.4(5) . . ? N5 C26 C25 112.8(4) . . ? O8 C26 Na1 43.7(3) . 5_656 ? N5 C26 Na1 169.0(4) . 5_656 ? C25 C26 Na1 74.2(3) . 5_656 ? N5 C27 C28 122.7(5) . . ? N5 C27 C32 120.1(4) . . ? C28 C27 C32 117.1(5) . . ? C29 C28 C27 121.3(5) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C30 C29 C28 121.4(5) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 C29 119.1(5) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 121.9(5) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C32 C27 118.9(5) . . ? C31 C32 C33 117.3(5) . . ? C27 C32 C33 123.6(5) . . ? N6 C33 C32 122.9(5) . . ? N6 C33 C34 121.3(5) . . ? C32 C33 C34 115.9(5) . . ? O9 C34 O10 126.4(6) . . ? O9 C34 C33 118.4(5) . . ? O10 C34 C33 115.2(5) . . ? C36 C35 C40 120.5(5) . . ? C36 C35 N6 125.5(5) . . ? C40 C35 N6 113.7(5) . . ? C37 C36 C35 119.7(6) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.2(6) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 120.2(6) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.6(6) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 118.8(5) . . ? C39 C40 N7 127.9(5) . . ? C35 C40 N7 113.2(4) . . ? N7 C41 C43 124.0(5) . . ? N7 C41 C42 120.6(5) . . ? C43 C41 C42 115.3(4) . . ? O11 C42 O12 127.9(5) . . ? O11 C42 C41 115.2(5) . . ? O12 C42 C41 116.9(5) . . ? C44 C43 C48 118.7(5) . . ? C44 C43 C41 117.1(5) . . ? C48 C43 C41 123.9(5) . . ? C45 C44 C43 122.4(5) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? C44 C45 C46 119.1(5) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? C45 C46 C47 120.3(5) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 121.5(5) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? N8 C48 C47 122.1(5) . . ? N8 C48 C43 120.1(5) . . ? C47 C48 C43 117.8(5) . . ? O7 Na1 O12 102.82(15) 5_656 . ? O7 Na1 O3 92.19(15) 5_656 5_656 ? O12 Na1 O3 114.63(16) . 5_656 ? O7 Na1 O13 167.03(17) 5_656 . ? O12 Na1 O13 82.23(15) . . ? O3 Na1 O13 96.54(17) 5_656 . ? O7 Na1 O8 70.61(14) 5_656 5_656 ? O12 Na1 O8 130.54(17) . 5_656 ? O3 Na1 O8 114.58(17) 5_656 5_656 ? O13 Na1 O8 96.96(15) . 5_656 ? O7 Na1 C25 20.80(13) 5_656 5_656 ? O12 Na1 C25 117.74(15) . 5_656 ? O3 Na1 C25 97.65(15) 5_656 5_656 ? O13 Na1 C25 147.10(16) . 5_656 ? O8 Na1 C25 50.15(14) 5_656 5_656 ? O7 Na1 C26 49.75(14) 5_656 5_656 ? O12 Na1 C26 130.95(16) . 5_656 ? O3 Na1 C26 107.07(15) 5_656 5_656 ? O13 Na1 C26 118.07(16) . 5_656 ? O8 Na1 C26 21.25(13) 5_656 5_656 ? C25 Na1 C26 29.05(14) 5_656 5_656 ? O23' Na2 O14 124.8(9) . . ? O23' Na2 O23 21.1(8) . . ? O14 Na2 O23 103.7(2) . . ? O23' Na2 O15 79.8(9) . . ? O14 Na2 O15 145.35(17) . . ? O23 Na2 O15 98.9(2) . . ? O23' Na2 O12 139.0(8) . . ? O14 Na2 O12 89.16(15) . . ? O23 Na2 O12 152.27(18) . . ? O15 Na2 O12 82.56(14) . . ? O23' Na2 O13 84.7(9) . . ? O14 Na2 O13 82.82(16) . . ? O23 Na2 O13 80.30(17) . . ? O15 Na2 O13 127.15(17) . . ? O12 Na2 O13 77.06(14) . . ? O23' Na2 O16 87.4(8) . . ? O14 Na2 O16 76.80(15) . . ? O23 Na2 O16 81.45(16) . . ? O15 Na2 O16 81.03(15) . . ? O12 Na2 O16 125.82(15) . . ? O13 Na2 O16 148.44(16) . . ? O17 Na3 O16 133.8(3) . . ? O17 Na3 O15 97.0(3) . . ? O16 Na3 O15 87.16(17) . . ? O17 Na3 O22 124.5(3) . . ? O16 Na3 O22 101.6(2) . . ? O15 Na3 O22 86.90(17) . . ? O17 Na3 O19 84.1(3) . . ? O16 Na3 O19 93.4(2) . . ? O15 Na3 O19 177.9(3) . . ? O22 Na3 O19 91.0(2) . . ? O17 Na3 O17' 38.4(4) . . ? O16 Na3 O17' 169.5(3) . . ? O15 Na3 O17' 87.4(3) . . ? O22 Na3 O17' 87.0(3) . . ? O19 Na3 O17' 92.4(3) . . ? O17 Na3 O18' 41.7(4) . . ? O16 Na3 O18' 92.8(4) . . ? O15 Na3 O18' 88.0(4) . . ? O22 Na3 O18' 164.4(4) . . ? O19 Na3 O18' 93.9(4) . . ? O17' Na3 O18' 78.1(5) . . ? O20 Na4 O1 141.8(5) . . ? O20 Na4 O21' 78.7(5) . . ? O1 Na4 O21' 96.7(3) . . ? O20 Na4 O11 117.6(5) . . ? O1 Na4 O11 100.52(16) . . ? O21' Na4 O11 102.2(4) . . ? O20 Na4 O20' 22.5(5) . . ? O1 Na4 O20' 164.0(4) . . ? O21' Na4 O20' 78.8(5) . . ? O11 Na4 O20' 95.4(3) . . ? O20 Na4 O2 92.8(5) . . ? O1 Na4 O2 70.23(14) . . ? O21' Na4 O2 146.6(4) . . ? O11 Na4 O2 110.32(16) . . ? O20' Na4 O2 105.2(3) . . ? O20 Na4 O21 96.6(5) . . ? O1 Na4 O21 87.8(3) . . ? O21' Na4 O21 19.7(3) . . ? O11 Na4 O21 86.6(3) . . ? O20' Na4 O21 92.1(4) . . ? O2 Na4 O21 154.1(3) . . ? Na2 O14 H14E 110.1 . . ? Na2 O14 H14D 122.6 . . ? H14E O14 H14D 118.7 . . ? Na3 O15 Na2 98.69(17) . . ? Na3 O16 Na2 92.79(16) . . ? C49 O13 Na1 119.4(4) . . ? C49 O13 Na2 124.2(4) . . ? Na1 O13 Na2 93.77(15) . . ? C49 O13 H13A 104.0 . . ? Na1 O13 H13A 108.5 . . ? Na2 O13 H13A 105.8 . . ? O13 C49 C50 106.8(6) . . ? O13 C49 H49A 110.4 . . ? C50 C49 H49A 110.4 . . ? O13 C49 H49B 110.4 . . ? C50 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C51 O19 Na3 116.8(6) . . ? C51 O19 H19A 121.6 . . ? Na3 O19 H19A 121.6 . . ? O19 C51 C52 116.0(9) . . ? O19 C51 H51A 108.3 . . ? C52 C51 H51A 108.3 . . ? O19 C51 H51B 108.3 . . ? C52 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Na3 O22 H22A 126.4 . . ? Na3 O22 H22B 114.1 . . ? H22A O22 H22B 116.7 . . ? C53 O21 Na4 130.3(12) . . ? O21 C53 C54 109.6(13) . . ? O21 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? O21 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? C53' O21' Na4 117.6(10) . . ? O21' C53' C54' 103.8(17) . . ? O21' C53' H53C 111.0 . . ? C54' C53' H53C 111.0 . . ? O21' C53' H53D 111.0 . . ? C54' C53' H53D 111.0 . . ? H53C C53' H53D 109.0 . . ? C53' C54' H54D 109.5 . . ? C53' C54' H54E 109.5 . . ? H54D C54' H54E 109.5 . . ? C53' C54' H54F 109.5 . . ? H54D C54' H54F 109.5 . . ? H54E C54' H54F 109.5 . . ? 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 N4 Ni1 N1 C2 25.5(4) . . . . ? N3 Ni1 N1 C2 -35(11) . . . . ? N2 Ni1 N1 C2 -151.7(4) . . . . ? N4 Ni1 N1 C3 -155.9(4) . . . . ? N3 Ni1 N1 C3 143(11) . . . . ? N2 Ni1 N1 C3 26.9(4) . . . . ? N1 Ni1 N2 C9 -23.6(5) . . . . ? N4 Ni1 N2 C9 -113(4) . . . . ? N3 Ni1 N2 C9 157.4(5) . . . . ? N1 Ni1 N2 C11 157.5(4) . . . . ? N4 Ni1 N2 C11 68(4) . . . . ? N3 Ni1 N2 C11 -21.5(4) . . . . ? N1 Ni1 N3 C17 85(11) . . . . ? N4 Ni1 N3 C17 24.3(5) . . . . ? N2 Ni1 N3 C17 -158.5(5) . . . . ? N1 Ni1 N3 C16 -95(11) . . . . ? N4 Ni1 N3 C16 -155.7(4) . . . . ? N2 Ni1 N3 C16 21.4(4) . . . . ? N1 Ni1 N4 C1 -25.2(4) . . . . ? N3 Ni1 N4 C1 153.8(4) . . . . ? N2 Ni1 N4 C1 65(4) . . . . ? N1 Ni1 N4 C24 156.0(4) . . . . ? N3 Ni1 N4 C24 -25.0(4) . . . . ? N2 Ni1 N4 C24 -114(4) . . . . ? N8 Ni2 N5 C26 -19.3(4) . . . . ? N6 Ni2 N5 C26 161.6(4) . . . . ? N7 Ni2 N5 C26 93(4) . . . . ? N8 Ni2 N5 C27 160.2(4) . . . . ? N6 Ni2 N5 C27 -18.9(5) . . . . ? N7 Ni2 N5 C27 -88(4) . . . . ? N8 Ni2 N6 C33 -98(10) . . . . ? N5 Ni2 N6 C33 31.2(5) . . . . ? N7 Ni2 N6 C33 -151.6(5) . . . . ? N8 Ni2 N6 C35 72(10) . . . . ? N5 Ni2 N6 C35 -158.8(4) . . . . ? N7 Ni2 N6 C35 18.4(4) . . . . ? N8 Ni2 N7 C41 -24.1(5) . . . . ? N6 Ni2 N7 C41 154.9(5) . . . . ? N5 Ni2 N7 C41 -136(4) . . . . ? N8 Ni2 N7 C40 162.1(4) . . . . ? N6 Ni2 N7 C40 -18.8(4) . . . . ? N5 Ni2 N7 C40 50(4) . . . . ? N6 Ni2 N8 C25 148(10) . . . . ? N5 Ni2 N8 C25 19.2(4) . . . . ? N7 Ni2 N8 C25 -158.1(4) . . . . ? N6 Ni2 N8 C48 -34(10) . . . . ? N5 Ni2 N8 C48 -163.2(4) . . . . ? N7 Ni2 N8 C48 19.6(4) . . . . ? Na4 O1 C1 N4 -179.8(4) . . . . ? Na4 O1 C1 C2 -2.8(6) . . . . ? C24 N4 C1 O1 15.4(8) . . . . ? Ni1 N4 C1 O1 -163.4(5) . . . . ? C24 N4 C1 C2 -161.7(4) . . . . ? Ni1 N4 C1 C2 19.5(5) . . . . ? Na4 O2 C2 N1 179.4(4) . . . . ? Na4 O2 C2 C1 2.6(5) . . . . ? C3 N1 C2 O2 -15.3(8) . . . . ? Ni1 N1 C2 O2 163.4(5) . . . . ? C3 N1 C2 C1 161.6(4) . . . . ? Ni1 N1 C2 C1 -19.7(5) . . . . ? O1 C1 C2 O2 -0.1(7) . . . . ? N4 C1 C2 O2 177.4(5) . . . . ? O1 C1 C2 N1 -177.4(5) . . . . ? N4 C1 C2 N1 0.1(6) . . . . ? C2 N1 C3 C4 -23.5(7) . . . . ? Ni1 N1 C3 C4 158.1(4) . . . . ? C2 N1 C3 C8 161.6(5) . . . . ? Ni1 N1 C3 C8 -16.8(7) . . . . ? C8 C3 C4 C5 1.9(8) . . . . ? N1 C3 C4 C5 -173.1(5) . . . . ? C3 C4 C5 C6 -2.0(9) . . . . ? C4 C5 C6 C7 0.2(8) . . . . ? C5 C6 C7 C8 1.5(9) . . . . ? C4 C3 C8 C7 -0.2(8) . . . . ? N1 C3 C8 C7 174.8(5) . . . . ? C4 C3 C8 C9 178.7(5) . . . . ? N1 C3 C8 C9 -6.3(8) . . . . ? C6 C7 C8 C3 -1.5(8) . . . . ? C6 C7 C8 C9 179.5(5) . . . . ? C11 N2 C9 C8 -171.8(5) . . . . ? Ni1 N2 C9 C8 9.4(8) . . . . ? C11 N2 C9 C10 11.5(8) . . . . ? Ni1 N2 C9 C10 -167.3(4) . . . . ? C3 C8 C9 N2 10.2(8) . . . . ? C7 C8 C9 N2 -170.9(5) . . . . ? C3 C8 C9 C10 -172.9(5) . . . . ? C7 C8 C9 C10 6.0(7) . . . . ? Na1 O3 C10 O4 148.4(5) 5_656 . . . ? Na1 O3 C10 C9 -29.8(10) 5_656 . . . ? N2 C9 C10 O4 80.2(7) . . . . ? C8 C9 C10 O4 -96.7(6) . . . . ? N2 C9 C10 O3 -101.4(6) . . . . ? C8 C9 C10 O3 81.7(6) . . . . ? C9 N2 C11 C12 26.9(9) . . . . ? Ni1 N2 C11 C12 -154.2(5) . . . . ? C9 N2 C11 C16 -161.9(5) . . . . ? Ni1 N2 C11 C16 17.0(6) . . . . ? C16 C11 C12 C13 2.5(9) . . . . ? N2 C11 C12 C13 173.2(6) . . . . ? C11 C12 C13 C14 -2.4(11) . . . . ? C12 C13 C14 C15 0.2(12) . . . . ? C13 C14 C15 C16 1.9(10) . . . . ? C14 C15 C16 C11 -1.8(9) . . . . ? C14 C15 C16 N3 -172.9(6) . . . . ? C12 C11 C16 C15 -0.4(8) . . . . ? N2 C11 C16 C15 -172.2(5) . . . . ? C12 C11 C16 N3 171.7(5) . . . . ? N2 C11 C16 N3 -0.1(7) . . . . ? C17 N3 C16 C15 -25.4(9) . . . . ? Ni1 N3 C16 C15 154.7(5) . . . . ? C17 N3 C16 C11 163.1(5) . . . . ? Ni1 N3 C16 C11 -16.9(6) . . . . ? C16 N3 C17 C19 170.0(5) . . . . ? Ni1 N3 C17 C19 -10.0(8) . . . . ? C16 N3 C17 C18 -12.0(8) . . . . ? Ni1 N3 C17 C18 167.9(4) . . . . ? N3 C17 C18 O6 109.0(7) . . . . ? C19 C17 C18 O6 -72.8(7) . . . . ? N3 C17 C18 O5 -74.0(7) . . . . ? C19 C17 C18 O5 104.2(6) . . . . ? N3 C17 C19 C20 170.8(5) . . . . ? C18 C17 C19 C20 -7.4(7) . . . . ? N3 C17 C19 C24 -13.3(8) . . . . ? C18 C17 C19 C24 168.6(5) . . . . ? C24 C19 C20 C21 -2.1(8) . . . . ? C17 C19 C20 C21 174.1(5) . . . . ? C19 C20 C21 C22 -1.4(9) . . . . ? C20 C21 C22 C23 2.3(9) . . . . ? C21 C22 C23 C24 0.4(8) . . . . ? C22 C23 C24 N4 172.3(5) . . . . ? C22 C23 C24 C19 -3.8(8) . . . . ? C1 N4 C24 C23 16.5(7) . . . . ? Ni1 N4 C24 C23 -164.8(4) . . . . ? C1 N4 C24 C19 -167.4(5) . . . . ? Ni1 N4 C24 C19 11.3(7) . . . . ? C20 C19 C24 C23 4.6(7) . . . . ? C17 C19 C24 C23 -171.4(5) . . . . ? C20 C19 C24 N4 -171.7(5) . . . . ? C17 C19 C24 N4 12.4(8) . . . . ? Na1 O7 C25 N8 167.8(4) 5_656 . . . ? Na1 O7 C25 C26 -8.2(6) 5_656 . . . ? C48 N8 C25 O7 -8.8(9) . . . . ? Ni2 N8 C25 O7 169.0(5) . . . . ? C48 N8 C25 C26 167.3(4) . . . . ? Ni2 N8 C25 C26 -14.9(5) . . . . ? C48 N8 C25 Na1 30(2) . . . 5_656 ? Ni2 N8 C25 Na1 -151.9(15) . . . 5_656 ? Na1 O8 C26 N5 -167.8(5) 5_656 . . . ? Na1 O8 C26 C25 9.6(6) 5_656 . . . ? C27 N5 C26 O8 13.0(9) . . . . ? Ni2 N5 C26 O8 -167.5(5) . . . . ? C27 N5 C26 C25 -164.4(5) . . . . ? Ni2 N5 C26 C25 15.1(5) . . . . ? C27 N5 C26 Na1 -37(2) . . . 5_656 ? Ni2 N5 C26 Na1 142.6(17) . . . 5_656 ? O7 C25 C26 O8 -1.3(8) . . . . ? N8 C25 C26 O8 -177.9(5) . . . . ? Na1 C25 C26 O8 -6.9(4) 5_656 . . . ? O7 C25 C26 N5 176.4(5) . . . . ? N8 C25 C26 N5 -0.2(6) . . . . ? Na1 C25 C26 N5 170.9(4) 5_656 . . . ? O7 C25 C26 Na1 5.5(4) . . . 5_656 ? N8 C25 C26 Na1 -171.1(4) . . . 5_656 ? C26 N5 C27 C28 2.4(8) . . . . ? Ni2 N5 C27 C28 -177.0(4) . . . . ? C26 N5 C27 C32 179.7(5) . . . . ? Ni2 N5 C27 C32 0.2(7) . . . . ? N5 C27 C28 C29 172.1(5) . . . . ? C32 C27 C28 C29 -5.2(8) . . . . ? C27 C28 C29 C30 0.4(8) . . . . ? C28 C29 C30 C31 2.8(8) . . . . ? C29 C30 C31 C32 -0.9(8) . . . . ? C30 C31 C32 C27 -4.1(8) . . . . ? C30 C31 C32 C33 169.8(5) . . . . ? N5 C27 C32 C31 -170.5(5) . . . . ? C28 C27 C32 C31 6.9(7) . . . . ? N5 C27 C32 C33 16.0(8) . . . . ? C28 C27 C32 C33 -166.6(5) . . . . ? C35 N6 C33 C32 166.4(5) . . . . ? Ni2 N6 C33 C32 -24.6(7) . . . . ? C35 N6 C33 C34 -13.1(8) . . . . ? Ni2 N6 C33 C34 156.0(4) . . . . ? C31 C32 C33 N6 -177.4(5) . . . . ? C27 C32 C33 N6 -3.8(8) . . . . ? C31 C32 C33 C34 2.1(7) . . . . ? C27 C32 C33 C34 175.7(5) . . . . ? N6 C33 C34 O9 110.2(6) . . . . ? C32 C33 C34 O9 -69.3(7) . . . . ? N6 C33 C34 O10 -72.1(7) . . . . ? C32 C33 C34 O10 108.4(6) . . . . ? C33 N6 C35 C36 -30.5(8) . . . . ? Ni2 N6 C35 C36 159.1(5) . . . . ? C33 N6 C35 C40 156.2(5) . . . . ? Ni2 N6 C35 C40 -14.2(6) . . . . ? C40 C35 C36 C37 -3.4(9) . . . . ? N6 C35 C36 C37 -176.3(5) . . . . ? C35 C36 C37 C38 3.0(9) . . . . ? C36 C37 C38 C39 0.1(10) . . . . ? C37 C38 C39 C40 -2.8(10) . . . . ? C38 C39 C40 C35 2.3(9) . . . . ? C38 C39 C40 N7 176.9(6) . . . . ? C36 C35 C40 C39 0.8(9) . . . . ? N6 C35 C40 C39 174.4(5) . . . . ? C36 C35 C40 N7 -174.6(5) . . . . ? N6 C35 C40 N7 -0.9(7) . . . . ? C41 N7 C40 C39 26.7(9) . . . . ? Ni2 N7 C40 C39 -159.4(5) . . . . ? C41 N7 C40 C35 -158.5(5) . . . . ? Ni2 N7 C40 C35 15.5(6) . . . . ? C40 N7 C41 C43 -171.8(5) . . . . ? Ni2 N7 C41 C43 15.2(7) . . . . ? C40 N7 C41 C42 11.0(8) . . . . ? Ni2 N7 C41 C42 -162.1(4) . . . . ? Na4 O11 C42 O12 -172.6(4) . . . . ? Na4 O11 C42 C41 5.4(7) . . . . ? Na1 O12 C42 O11 167.1(4) . . . . ? Na2 O12 C42 O11 -19.2(8) . . . . ? Na1 O12 C42 C41 -10.8(7) . . . . ? Na2 O12 C42 C41 162.8(3) . . . . ? N7 C41 C42 O11 78.5(6) . . . . ? C43 C41 C42 O11 -99.0(6) . . . . ? N7 C41 C42 O12 -103.3(6) . . . . ? C43 C41 C42 O12 79.2(6) . . . . ? N7 C41 C43 C44 -179.0(5) . . . . ? C42 C41 C43 C44 -1.7(7) . . . . ? N7 C41 C43 C48 7.0(8) . . . . ? C42 C41 C43 C48 -175.6(5) . . . . ? C48 C43 C44 C45 2.1(8) . . . . ? C41 C43 C44 C45 -172.2(5) . . . . ? C43 C44 C45 C46 0.7(9) . . . . ? C44 C45 C46 C47 -1.7(9) . . . . ? C45 C46 C47 C48 -0.2(9) . . . . ? C25 N8 C48 C47 -10.1(8) . . . . ? Ni2 N8 C48 C47 172.4(4) . . . . ? C25 N8 C48 C43 171.7(5) . . . . ? Ni2 N8 C48 C43 -5.7(7) . . . . ? C46 C47 C48 N8 -175.3(5) . . . . ? C46 C47 C48 C43 2.9(8) . . . . ? C44 C43 C48 N8 174.4(5) . . . . ? C41 C43 C48 N8 -11.7(8) . . . . ? C44 C43 C48 C47 -3.8(8) . . . . ? C41 C43 C48 C47 170.1(5) . . . . ? C42 O12 Na1 O7 8.9(5) . . . 5_656 ? Na2 O12 Na1 O7 -166.17(15) . . . 5_656 ? C42 O12 Na1 O3 107.4(5) . . . 5_656 ? Na2 O12 Na1 O3 -67.69(19) . . . 5_656 ? C42 O12 Na1 O13 -159.0(5) . . . . ? Na2 O12 Na1 O13 25.98(15) . . . . ? C42 O12 Na1 O8 -66.5(5) . . . 5_656 ? Na2 O12 Na1 O8 118.51(19) . . . 5_656 ? C42 O12 Na1 C25 -6.6(5) . . . 5_656 ? Na2 O12 Na1 C25 178.32(15) . . . 5_656 ? C42 O12 Na1 C26 -38.3(6) . . . 5_656 ? Na2 O12 Na1 C26 146.67(17) . . . 5_656 ? C42 O12 Na2 O23' 93.7(15) . . . . ? Na1 O12 Na2 O23' -90.7(14) . . . . ? C42 O12 Na2 O14 -117.6(4) . . . . ? Na1 O12 Na2 O14 57.98(16) . . . . ? C42 O12 Na2 O23 123.5(5) . . . . ? Na1 O12 Na2 O23 -60.9(5) . . . . ? C42 O12 Na2 O15 28.6(4) . . . . ? Na1 O12 Na2 O15 -155.76(16) . . . . ? C42 O12 Na2 O13 159.6(4) . . . . ? Na1 O12 Na2 O13 -24.84(15) . . . . ? C42 O12 Na2 O16 -44.6(5) . . . . ? Na1 O12 Na2 O16 130.99(17) . . . . ? C1 O1 Na4 O20 71.1(8) . . . . ? C1 O1 Na4 O21' 151.3(5) . . . . ? C1 O1 Na4 O11 -105.0(4) . . . . ? C1 O1 Na4 O20' 78.8(14) . . . . ? C1 O1 Na4 O2 3.0(4) . . . . ? C1 O1 Na4 O21 168.9(5) . . . . ? C42 O11 Na4 O20 -98.0(6) . . . . ? C42 O11 Na4 O1 79.2(5) . . . . ? C42 O11 Na4 O21' 178.5(6) . . . . ? C42 O11 Na4 O20' -101.8(6) . . . . ? C42 O11 Na4 O2 6.6(5) . . . . ? C42 O11 Na4 O21 166.4(5) . . . . ? C2 O2 Na4 O20 -147.8(6) . . . . ? C2 O2 Na4 O1 -2.9(3) . . . . ? C2 O2 Na4 O21' -74.2(8) . . . . ? C2 O2 Na4 O11 91.4(4) . . . . ? C2 O2 Na4 O20' -166.8(5) . . . . ? C2 O2 Na4 O21 -36.6(8) . . . . ? O17 Na3 O15 Na2 129.1(3) . . . . ? O16 Na3 O15 Na2 -4.72(18) . . . . ? O22 Na3 O15 Na2 -106.51(19) . . . . ? O19 Na3 O15 Na2 -110(6) . . . . ? O17' Na3 O15 Na2 166.3(3) . . . . ? O18' Na3 O15 Na2 88.2(4) . . . . ? O23' Na2 O15 Na3 93.2(8) . . . . ? O14 Na2 O15 Na3 -46.3(3) . . . . ? O23 Na2 O15 Na3 84.1(2) . . . . ? O12 Na2 O15 Na3 -123.90(18) . . . . ? O13 Na2 O15 Na3 168.58(17) . . . . ? O16 Na2 O15 Na3 4.28(16) . . . . ? O17 Na3 O16 Na2 -92.8(4) . . . . ? O15 Na3 O16 Na2 4.24(16) . . . . ? O22 Na3 O16 Na2 90.49(17) . . . . ? O19 Na3 O16 Na2 -177.8(2) . . . . ? O17' Na3 O16 Na2 -54.6(16) . . . . ? O18' Na3 O16 Na2 -83.6(4) . . . . ? O23' Na2 O16 Na3 -84.4(9) . . . . ? O14 Na2 O16 Na3 148.90(19) . . . . ? O23 Na2 O16 Na3 -104.7(2) . . . . ? O15 Na2 O16 Na3 -4.27(16) . . . . ? O12 Na2 O16 Na3 69.7(2) . . . . ? O13 Na2 O16 Na3 -159.9(3) . . . . ? O7 Na1 O13 C49 -6.1(11) 5_656 . . . ? O12 Na1 O13 C49 107.8(5) . . . . ? O3 Na1 O13 C49 -138.1(5) 5_656 . . . ? O8 Na1 O13 C49 -22.3(5) 5_656 . . . ? C25 Na1 O13 C49 -23.1(7) 5_656 . . . ? C26 Na1 O13 C49 -24.8(5) 5_656 . . . ? O7 Na1 O13 Na2 -139.3(8) 5_656 . . . ? O12 Na1 O13 Na2 -25.39(15) . . . . ? O3 Na1 O13 Na2 88.68(18) 5_656 . . . ? O8 Na1 O13 Na2 -155.49(17) 5_656 . . . ? C25 Na1 O13 Na2 -156.2(3) 5_656 . . . ? C26 Na1 O13 Na2 -158.00(15) 5_656 . . . ? O23' Na2 O13 C49 37.8(10) . . . . ? O14 Na2 O13 C49 164.0(5) . . . . ? O23 Na2 O13 C49 58.6(5) . . . . ? O15 Na2 O13 C49 -35.2(5) . . . . ? O12 Na2 O13 C49 -105.2(5) . . . . ? O16 Na2 O13 C49 114.1(5) . . . . ? O23' Na2 O13 Na1 167.6(9) . . . . ? O14 Na2 O13 Na1 -66.29(17) . . . . ? O23 Na2 O13 Na1 -171.6(2) . . . . ? O15 Na2 O13 Na1 94.6(2) . . . . ? O12 Na2 O13 Na1 24.50(15) . . . . ? O16 Na2 O13 Na1 -116.1(3) . . . . ? Na1 O13 C49 C50 -53.9(8) . . . . ? Na2 O13 C49 C50 64.5(7) . . . . ? O17 Na3 O19 C51 -86.5(7) . . . . ? O16 Na3 O19 C51 47.2(7) . . . . ? O15 Na3 O19 C51 152(6) . . . . ? O22 Na3 O19 C51 148.9(7) . . . . ? O17' Na3 O19 C51 -124.1(7) . . . . ? O18' Na3 O19 C51 -45.9(7) . . . . ? Na3 O19 C51 C52 176.3(6) . . . . ? O20 Na4 O21 C53 59.9(14) . . . . ? O1 Na4 O21 C53 -82.0(13) . . . . ? O21' Na4 O21 C53 34.8(13) . . . . ? O11 Na4 O21 C53 177.3(13) . . . . ? O20' Na4 O21 C53 82.0(13) . . . . ? O2 Na4 O21 C53 -50.4(16) . . . . ? Na4 O21 C53 C54 99.4(17) . . . . ? O20 Na4 O21' C53' 132.4(14) . . . . ? O1 Na4 O21' C53' -9.2(13) . . . . ? O11 Na4 O21' C53' -111.5(12) . . . . ? O20' Na4 O21' C53' 155.3(13) . . . . ? O2 Na4 O21' C53' 54.6(16) . . . . ? O21 Na4 O21' C53' -73.1(17) . . . . ? Na4 O21' C53' C54' 142.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.665 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.113 # Attachment 'compound 2.cif' data_m091228f _database_code_depnum_ccdc_archive 'CCDC 839540' #TrackingRef 'compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Fe N4 Ni O11' _chemical_formula_weight 685.04 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.932(3) _cell_length_b 8.8699(19) _cell_length_c 19.240(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.679(4) _cell_angle_gamma 90.00 _cell_volume 2717.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9763 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7815 _exptl_absorpt_correction_T_max 0.8600 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19353 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4788 _reflns_number_gt 4364 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; The restraints (dfix,isor) are applied to keep the bond geometries and dsps of methanol and water molecules structurally reasonable. DFIX 1.43 0.01 O9 C25 DFIX 1.45 0.01 H8A H8B DFIX 0.85 0.01 O8 H8A O8 H8B ISOR 0.01 C25 C25' O9 C26 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+7.1133P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4788 _refine_ls_number_parameters 415 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.003 _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 0.80695(2) 0.44440(4) 0.111630(16) 0.01518(8) Uani 1 1 d . . . Fe1 Fe 1.04713(2) 0.51831(5) 0.29587(2) 0.02241(10) Uani 1 1 d . . . O1 O 0.97102(11) 0.3334(2) 0.25457(9) 0.0219(4) Uani 1 1 d . A . O2 O 1.01888(11) 0.5843(2) 0.18901(9) 0.0215(4) Uani 1 1 d . A . O3 O 0.71958(13) 0.8974(3) -0.03871(12) 0.0369(6) Uani 1 1 d . . . O4 O 0.70241(14) 0.6720(3) -0.09185(11) 0.0376(6) Uani 1 1 d . . . O5 O 0.58326(12) 0.0887(2) 0.06533(9) 0.0238(5) Uani 1 1 d . . . O6 O 0.57135(11) 0.1084(2) 0.18176(9) 0.0206(4) Uani 1 1 d . . . O7 O 1.10757(14) 0.7270(3) 0.30242(11) 0.0408(6) Uani 1 1 d . A . H7B H 1.1027 0.7886 0.2689 0.049 Uiso 1 1 d R . . H7C H 1.1369 0.7492 0.3385 0.049 Uiso 1 1 d R . . O8 O 1.07143(12) 0.4920(2) 0.40350(10) 0.0266(5) Uani 1 1 d D A . N1 N 0.90935(14) 0.5455(2) 0.10791(11) 0.0176(5) Uani 1 1 d . . . N2 N 0.75036(13) 0.5875(2) 0.05624(11) 0.0171(5) Uani 1 1 d . . . N3 N 0.70350(13) 0.3448(2) 0.11657(11) 0.0166(5) Uani 1 1 d . . . N4 N 0.86302(13) 0.3075(2) 0.17056(11) 0.0173(5) Uani 1 1 d . A . C1 C 0.92838(16) 0.3736(3) 0.20254(13) 0.0177(6) Uani 1 1 d . . . C2 C 0.95599(16) 0.5168(3) 0.16507(13) 0.0182(6) Uani 1 1 d . A . C3 C 0.93425(17) 0.6459(3) 0.05592(13) 0.0192(6) Uani 1 1 d . . . C4 C 1.01926(18) 0.6838(4) 0.04820(15) 0.0275(7) Uani 1 1 d . . . H4A H 1.0603 0.6473 0.0808 0.033 Uiso 1 1 calc R . . C5 C 1.04378(18) 0.7737(4) -0.00632(15) 0.0295(7) Uani 1 1 d . . . H5A H 1.1015 0.7972 -0.0108 0.035 Uiso 1 1 calc R . . C6 C 0.98605(18) 0.8297(4) -0.05418(15) 0.0280(7) Uani 1 1 d . . . H6A H 1.0035 0.8925 -0.0910 0.034 Uiso 1 1 calc R . . C7 C 0.90261(18) 0.7936(3) -0.04797(14) 0.0270(7) Uani 1 1 d . . . H7A H 0.8629 0.8314 -0.0813 0.032 Uiso 1 1 calc R . . C8 C 0.87419(17) 0.7012(3) 0.00698(13) 0.0203(6) Uani 1 1 d . . . C9 C 0.78392(17) 0.6770(3) 0.01098(13) 0.0212(6) Uani 1 1 d . . . C10 C 0.72952(18) 0.7573(4) -0.04507(15) 0.0295(7) Uani 1 1 d . . . C11 C 0.66163(16) 0.5784(3) 0.06527(13) 0.0174(6) Uani 1 1 d . . . C12 C 0.60396(17) 0.6926(3) 0.05106(14) 0.0218(6) Uani 1 1 d . . . H12A H 0.6223 0.7858 0.0325 0.026 Uiso 1 1 calc R . . C13 C 0.51963(17) 0.6706(3) 0.06389(14) 0.0238(7) Uani 1 1 d . . . H13A H 0.4798 0.7469 0.0523 0.029 Uiso 1 1 calc R . . C14 C 0.49392(18) 0.5379(3) 0.09337(15) 0.0233(7) Uani 1 1 d . . . H14A H 0.4360 0.5226 0.1013 0.028 Uiso 1 1 calc R . . C15 C 0.55107(17) 0.4262(3) 0.11178(14) 0.0216(6) Uani 1 1 d . . . H15A H 0.5327 0.3372 0.1342 0.026 Uiso 1 1 calc R . . C16 C 0.63553(17) 0.4448(3) 0.09731(13) 0.0180(6) Uani 1 1 d . . . C17 C 0.69292(16) 0.2034(3) 0.13210(13) 0.0177(6) Uani 1 1 d . . . C18 C 0.60718(16) 0.1268(3) 0.12440(14) 0.0193(6) Uani 1 1 d . . . C19 C 0.76010(17) 0.1047(3) 0.15864(13) 0.0191(6) Uani 1 1 d . A . C20 C 0.74160(18) -0.0503(3) 0.16483(14) 0.0223(6) Uani 1 1 d . . . H20A H 0.6879 -0.0858 0.1495 0.027 Uiso 1 1 calc R . . C21 C 0.79901(18) -0.1514(3) 0.19240(14) 0.0238(7) Uani 1 1 d . . . H21A H 0.7854 -0.2554 0.1955 0.029 Uiso 1 1 calc R . . C22 C 0.87738(18) -0.0990(3) 0.21564(14) 0.0234(7) Uani 1 1 d . . . H22A H 0.9176 -0.1679 0.2345 0.028 Uiso 1 1 calc R . . C23 C 0.89712(18) 0.0526(3) 0.21151(14) 0.0217(6) Uani 1 1 d . A . H23A H 0.9502 0.0867 0.2289 0.026 Uiso 1 1 calc R . . C24 C 0.84001(16) 0.1570(3) 0.18206(13) 0.0181(6) Uani 1 1 d . . . O9 O 1.1598(6) 0.4383(14) 0.2651(5) 0.059(3) Uani 0.25 1 d PDU A 1 C25 C 1.2047(11) 0.443(4) 0.2025(7) 0.117(6) Uani 0.25 1 d PDU A 1 O9' O 1.1519(2) 0.3771(4) 0.28173(16) 0.0395(9) Uani 0.75 1 d P A 2 C25' C 1.1639(5) 0.2729(10) 0.2281(4) 0.099(2) Uani 0.75 1 d PU A 2 O10 O 0.24065(18) 0.8475(3) 0.10827(15) 0.0578(8) Uani 1 1 d . . . H10 H 0.2280 0.9175 0.0805 0.087 Uiso 1 1 calc R . . C26 C 0.2657(3) 0.7154(6) 0.0694(3) 0.0820(16) Uani 1 1 d U . . H26A H 0.3269 0.7147 0.0655 0.123 Uiso 1 1 calc R . . H26B H 0.2393 0.7182 0.0228 0.123 Uiso 1 1 calc R . . H26C H 0.2480 0.6241 0.0936 0.123 Uiso 1 1 calc R . . O11 O 0.8976(3) 0.1003(5) 0.8140(2) 0.1122(16) Uani 1 1 d . . . H8B H 1.1211(4) 0.521(3) 0.4142(15) 0.135 Uiso 1 1 d D . . H8A H 1.0326(6) 0.524(3) 0.4292(10) 0.135 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01307(16) 0.01545(16) 0.01677(16) 0.00151(12) -0.00373(13) 0.00087(12) Fe1 0.01602(19) 0.0288(2) 0.02203(19) -0.00469(16) -0.00639(15) 0.00161(16) O1 0.0215(9) 0.0215(9) 0.0221(9) 0.0001(8) -0.0079(8) 0.0050(8) O2 0.0144(9) 0.0291(10) 0.0207(9) -0.0018(8) -0.0031(7) -0.0045(8) O3 0.0255(11) 0.0338(11) 0.0512(13) 0.0214(10) -0.0011(10) 0.0043(9) O4 0.0298(11) 0.0570(15) 0.0255(10) 0.0069(10) -0.0060(9) 0.0045(11) O5 0.0249(10) 0.0266(10) 0.0195(9) -0.0014(8) -0.0047(8) -0.0012(8) O6 0.0196(9) 0.0220(9) 0.0199(9) 0.0009(7) -0.0021(7) -0.0024(8) O7 0.0416(12) 0.0556(14) 0.0242(10) 0.0057(10) -0.0138(9) -0.0237(11) O8 0.0232(10) 0.0281(10) 0.0279(10) 0.0016(8) -0.0096(8) -0.0013(9) N1 0.0162(10) 0.0176(11) 0.0188(10) 0.0016(9) -0.0028(9) 0.0011(9) N2 0.0152(10) 0.0171(10) 0.0190(10) -0.0007(9) -0.0029(9) -0.0008(9) N3 0.0158(10) 0.0170(10) 0.0169(10) 0.0009(8) -0.0029(8) 0.0025(9) N4 0.0163(10) 0.0181(11) 0.0175(10) 0.0018(8) -0.0015(8) 0.0016(9) C1 0.0161(12) 0.0186(12) 0.0182(12) -0.0018(10) 0.0004(10) 0.0061(10) C2 0.0155(12) 0.0197(13) 0.0195(12) -0.0032(10) 0.0013(10) 0.0038(10) C3 0.0205(12) 0.0179(13) 0.0191(12) -0.0022(10) 0.0000(10) -0.0007(11) C4 0.0204(13) 0.0335(16) 0.0286(14) 0.0049(12) -0.0009(12) -0.0007(12) C5 0.0181(13) 0.0406(17) 0.0299(14) 0.0019(13) 0.0033(12) -0.0045(13) C6 0.0287(15) 0.0317(15) 0.0239(13) 0.0047(12) 0.0066(12) -0.0028(13) C7 0.0272(14) 0.0308(15) 0.0229(13) 0.0067(12) -0.0010(12) 0.0008(12) C8 0.0197(13) 0.0210(13) 0.0201(12) -0.0007(10) 0.0008(10) -0.0015(11) C9 0.0213(13) 0.0215(13) 0.0204(12) 0.0014(11) -0.0031(11) 0.0009(11) C10 0.0178(13) 0.0405(17) 0.0302(15) 0.0110(13) -0.0013(12) 0.0002(13) C11 0.0171(12) 0.0186(12) 0.0160(12) -0.0021(10) -0.0045(10) -0.0002(10) C12 0.0217(13) 0.0189(13) 0.0246(13) 0.0025(11) -0.0044(11) 0.0009(11) C13 0.0193(13) 0.0231(14) 0.0285(14) -0.0008(11) -0.0070(11) 0.0042(11) C14 0.0170(13) 0.0260(14) 0.0269(14) -0.0024(11) -0.0023(11) 0.0019(11) C15 0.0188(13) 0.0207(13) 0.0253(13) 0.0005(11) -0.0006(11) -0.0003(11) C16 0.0180(12) 0.0179(13) 0.0179(12) -0.0017(10) -0.0044(10) 0.0021(10) C17 0.0193(12) 0.0188(13) 0.0151(11) 0.0005(10) -0.0005(10) 0.0002(10) C18 0.0188(12) 0.0137(12) 0.0253(13) 0.0030(10) -0.0034(11) 0.0022(10) C19 0.0203(13) 0.0192(13) 0.0175(12) 0.0012(10) -0.0007(10) 0.0031(11) C20 0.0241(14) 0.0203(13) 0.0224(13) -0.0015(11) -0.0015(11) 0.0005(11) C21 0.0318(15) 0.0146(13) 0.0248(13) 0.0012(11) 0.0011(12) 0.0012(11) C22 0.0268(14) 0.0225(14) 0.0209(13) 0.0026(11) -0.0012(11) 0.0085(12) C23 0.0214(13) 0.0227(14) 0.0208(13) 0.0021(11) -0.0028(11) 0.0031(11) C24 0.0201(12) 0.0188(13) 0.0154(11) 0.0002(10) 0.0011(10) 0.0023(10) O9 0.046(5) 0.057(6) 0.073(6) -0.011(5) -0.019(5) 0.009(4) C25 0.107(9) 0.129(9) 0.113(9) -0.014(7) 0.000(7) 0.009(7) O9' 0.0273(15) 0.057(2) 0.0340(16) -0.0091(15) -0.0058(13) 0.0191(15) C25' 0.074(4) 0.141(5) 0.082(4) -0.051(4) -0.010(3) 0.041(4) O10 0.0535(16) 0.0586(17) 0.0614(16) 0.0067(14) 0.0000(14) -0.0032(14) C26 0.065(3) 0.076(3) 0.105(3) -0.039(3) -0.016(3) 0.021(2) O11 0.121(3) 0.107(3) 0.109(3) 0.044(3) 0.013(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.865(2) . ? Ni1 N4 1.871(2) . ? Ni1 N2 1.872(2) . ? Ni1 N3 1.875(2) . ? Fe1 O9 2.035(10) . ? Fe1 O7 2.089(2) . ? Fe1 O6 2.1060(19) 2_655 ? Fe1 O8 2.108(2) . ? Fe1 O9' 2.111(3) . ? Fe1 O2 2.1721(19) . ? Fe1 O1 2.1763(19) . ? O1 C1 1.245(3) . ? O2 C2 1.244(3) . ? O3 C10 1.260(4) . ? O4 C10 1.243(4) . ? O5 C18 1.235(3) . ? O6 C18 1.268(3) . ? O6 Fe1 2.1060(19) 2_645 ? O7 H7B 0.8471 . ? O7 H7C 0.8476 . ? O8 H8B 0.852(9) . ? O8 H8A 0.854(9) . ? N1 C2 1.333(3) . ? N1 C3 1.405(3) . ? N2 C9 1.304(3) . ? N2 C11 1.432(3) . ? N3 C17 1.301(3) . ? N3 C16 1.440(3) . ? N4 C1 1.330(3) . ? N4 C24 1.403(3) . ? C1 C2 1.531(4) . ? C3 C4 1.408(4) . ? C3 C8 1.411(4) . ? C4 C5 1.383(4) . ? C4 H4A 0.9500 . ? C5 C6 1.375(4) . ? C5 H5A 0.9500 . ? C6 C7 1.376(4) . ? C6 H6A 0.9500 . ? C7 C8 1.422(4) . ? C7 H7A 0.9500 . ? C8 C9 1.458(4) . ? C9 C10 1.538(4) . ? C11 C12 1.389(4) . ? C11 C16 1.404(4) . ? C12 C13 1.387(4) . ? C12 H12A 0.9500 . ? C13 C14 1.374(4) . ? C13 H13A 0.9500 . ? C14 C15 1.385(4) . ? C14 H14A 0.9500 . ? C15 C16 1.392(4) . ? C15 H15A 0.9500 . ? C17 C19 1.463(4) . ? C17 C18 1.529(4) . ? C19 C20 1.412(4) . ? C19 C24 1.416(4) . ? C20 C21 1.376(4) . ? C20 H20A 0.9500 . ? C21 C22 1.394(4) . ? C21 H21A 0.9500 . ? C22 C23 1.383(4) . ? C22 H22A 0.9500 . ? C23 C24 1.406(4) . ? C23 H23A 0.9500 . ? O9 C25 1.419(9) . ? O9' C25' 1.403(8) . ? O10 C26 1.453(6) . ? O10 H10 0.8400 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 N4 86.13(9) . . ? N1 Ni1 N2 93.41(9) . . ? N4 Ni1 N2 177.31(9) . . ? N1 Ni1 N3 179.07(10) . . ? N4 Ni1 N3 93.92(9) . . ? N2 Ni1 N3 86.49(9) . . ? O9 Fe1 O7 85.3(3) . . ? O9 Fe1 O6 174.7(3) . 2_655 ? O7 Fe1 O6 93.76(9) . 2_655 ? O9 Fe1 O8 96.3(3) . . ? O7 Fe1 O8 88.16(8) . . ? O6 Fe1 O8 88.93(7) 2_655 . ? O9 Fe1 O9' 17.8(3) . . ? O7 Fe1 O9' 99.70(12) . . ? O6 Fe1 O9' 165.60(12) 2_655 . ? O8 Fe1 O9' 86.43(10) . . ? O9 Fe1 O2 88.8(3) . . ? O7 Fe1 O2 84.31(8) . . ? O6 Fe1 O2 85.93(7) 2_655 . ? O8 Fe1 O2 170.58(8) . . ? O9' Fe1 O2 100.40(10) . . ? O9 Fe1 O1 96.8(3) . . ? O7 Fe1 O1 160.22(8) . . ? O6 Fe1 O1 82.39(7) 2_655 . ? O8 Fe1 O1 111.07(7) . . ? O9' Fe1 O1 86.57(11) . . ? O2 Fe1 O1 76.09(7) . . ? C1 O1 Fe1 111.24(17) . . ? C2 O2 Fe1 111.31(17) . . ? C18 O6 Fe1 130.98(17) . 2_645 ? Fe1 O7 H7B 119.6 . . ? Fe1 O7 H7C 119.8 . . ? H7B O7 H7C 120.6 . . ? Fe1 O8 H8B 110(2) . . ? Fe1 O8 H8A 114.6(15) . . ? H8B O8 H8A 116.3(17) . . ? C2 N1 C3 123.1(2) . . ? C2 N1 Ni1 110.12(18) . . ? C3 N1 Ni1 126.70(17) . . ? C9 N2 C11 122.7(2) . . ? C9 N2 Ni1 126.36(19) . . ? C11 N2 Ni1 110.71(16) . . ? C17 N3 C16 123.5(2) . . ? C17 N3 Ni1 125.84(18) . . ? C16 N3 Ni1 110.63(16) . . ? C1 N4 C24 123.4(2) . . ? C1 N4 Ni1 110.33(17) . . ? C24 N4 Ni1 126.21(17) . . ? O1 C1 N4 130.3(2) . . ? O1 C1 C2 117.3(2) . . ? N4 C1 C2 112.3(2) . . ? O2 C2 N1 129.6(3) . . ? O2 C2 C1 117.6(2) . . ? N1 C2 C1 112.7(2) . . ? N1 C3 C4 121.3(2) . . ? N1 C3 C8 119.7(2) . . ? C4 C3 C8 118.8(2) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 119.1(3) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C6 C7 C8 121.9(3) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C3 C8 C7 118.2(2) . . ? C3 C8 C9 124.4(2) . . ? C7 C8 C9 117.4(2) . . ? N2 C9 C8 123.3(2) . . ? N2 C9 C10 121.1(2) . . ? C8 C9 C10 115.5(2) . . ? O4 C10 O3 129.0(3) . . ? O4 C10 C9 113.7(3) . . ? O3 C10 C9 117.3(3) . . ? C12 C11 C16 119.9(2) . . ? C12 C11 N2 125.8(2) . . ? C16 C11 N2 114.0(2) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C11 119.2(2) . . ? C15 C16 N3 126.8(2) . . ? C11 C16 N3 113.7(2) . . ? N3 C17 C19 124.0(2) . . ? N3 C17 C18 121.8(2) . . ? C19 C17 C18 114.2(2) . . ? O5 C18 O6 129.1(2) . . ? O5 C18 C17 117.5(2) . . ? O6 C18 C17 113.4(2) . . ? C20 C19 C24 118.7(2) . . ? C20 C19 C17 117.4(2) . . ? C24 C19 C17 123.8(2) . . ? C21 C20 C19 122.0(3) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C20 C21 C22 119.0(3) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 121.2(3) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? N4 C24 C23 121.4(2) . . ? N4 C24 C19 119.9(2) . . ? C23 C24 C19 118.5(2) . . ? C25 O9 Fe1 135.0(12) . . ? C25' O9' Fe1 127.7(4) . . ? C26 O10 H10 109.5 . . ? O10 C26 H26A 109.5 . . ? O10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 O9 Fe1 O1 C1 -108.2(3) . . . . ? O7 Fe1 O1 C1 -13.3(3) . . . . ? O6 Fe1 O1 C1 66.55(17) 2_655 . . . ? O8 Fe1 O1 C1 152.44(16) . . . . ? O9' Fe1 O1 C1 -122.72(19) . . . . ? O2 Fe1 O1 C1 -21.12(16) . . . . ? O9 Fe1 O2 C2 118.2(4) . . . . ? O7 Fe1 O2 C2 -156.41(19) . . . . ? O6 Fe1 O2 C2 -62.21(18) 2_655 . . . ? O8 Fe1 O2 C2 -119.3(5) . . . . ? O9' Fe1 O2 C2 104.7(2) . . . . ? O1 Fe1 O2 C2 20.95(17) . . . . ? N4 Ni1 N1 C2 -25.60(18) . . . . ? N2 Ni1 N1 C2 151.75(18) . . . . ? N3 Ni1 N1 C2 68(6) . . . . ? N4 Ni1 N1 C3 158.3(2) . . . . ? N2 Ni1 N1 C3 -24.3(2) . . . . ? N3 Ni1 N1 C3 -109(6) . . . . ? N1 Ni1 N2 C9 24.8(2) . . . . ? N4 Ni1 N2 C9 105(2) . . . . ? N3 Ni1 N2 C9 -156.1(2) . . . . ? N1 Ni1 N2 C11 -160.25(17) . . . . ? N4 Ni1 N2 C11 -80(2) . . . . ? N3 Ni1 N2 C11 18.82(17) . . . . ? N1 Ni1 N3 C17 -116(6) . . . . ? N4 Ni1 N3 C17 -23.4(2) . . . . ? N2 Ni1 N3 C17 159.2(2) . . . . ? N1 Ni1 N3 C16 66(6) . . . . ? N4 Ni1 N3 C16 159.42(16) . . . . ? N2 Ni1 N3 C16 -17.92(16) . . . . ? N1 Ni1 N4 C1 25.46(18) . . . . ? N2 Ni1 N4 C1 -55(2) . . . . ? N3 Ni1 N4 C1 -153.60(18) . . . . ? N1 Ni1 N4 C24 -156.1(2) . . . . ? N2 Ni1 N4 C24 124(2) . . . . ? N3 Ni1 N4 C24 24.8(2) . . . . ? Fe1 O1 C1 N4 -165.1(2) . . . . ? Fe1 O1 C1 C2 18.8(3) . . . . ? C24 N4 C1 O1 -14.3(4) . . . . ? Ni1 N4 C1 O1 164.2(2) . . . . ? C24 N4 C1 C2 161.9(2) . . . . ? Ni1 N4 C1 C2 -19.6(3) . . . . ? Fe1 O2 C2 N1 165.6(2) . . . . ? Fe1 O2 C2 C1 -18.4(3) . . . . ? C3 N1 C2 O2 12.6(4) . . . . ? Ni1 N1 C2 O2 -163.6(2) . . . . ? C3 N1 C2 C1 -163.5(2) . . . . ? Ni1 N1 C2 C1 20.2(3) . . . . ? O1 C1 C2 O2 -0.3(4) . . . . ? N4 C1 C2 O2 -177.1(2) . . . . ? O1 C1 C2 N1 176.4(2) . . . . ? N4 C1 C2 N1 -0.4(3) . . . . ? C2 N1 C3 C4 21.7(4) . . . . ? Ni1 N1 C3 C4 -162.7(2) . . . . ? C2 N1 C3 C8 -163.2(2) . . . . ? Ni1 N1 C3 C8 12.3(4) . . . . ? N1 C3 C4 C5 175.1(3) . . . . ? C8 C3 C4 C5 0.0(4) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C4 C5 C6 C7 -0.9(5) . . . . ? C5 C6 C7 C8 0.7(5) . . . . ? N1 C3 C8 C7 -175.4(2) . . . . ? C4 C3 C8 C7 -0.2(4) . . . . ? N1 C3 C8 C9 8.2(4) . . . . ? C4 C3 C8 C9 -176.6(3) . . . . ? C6 C7 C8 C3 -0.1(4) . . . . ? C6 C7 C8 C9 176.6(3) . . . . ? C11 N2 C9 C8 172.2(2) . . . . ? Ni1 N2 C9 C8 -13.4(4) . . . . ? C11 N2 C9 C10 -11.5(4) . . . . ? Ni1 N2 C9 C10 162.9(2) . . . . ? C3 C8 C9 N2 -7.9(4) . . . . ? C7 C8 C9 N2 175.7(3) . . . . ? C3 C8 C9 C10 175.7(3) . . . . ? C7 C8 C9 C10 -0.7(4) . . . . ? N2 C9 C10 O4 -72.5(3) . . . . ? C8 C9 C10 O4 104.0(3) . . . . ? N2 C9 C10 O3 108.7(3) . . . . ? C8 C9 C10 O3 -74.8(3) . . . . ? C9 N2 C11 C12 -26.7(4) . . . . ? Ni1 N2 C11 C12 158.2(2) . . . . ? C9 N2 C11 C16 159.4(2) . . . . ? Ni1 N2 C11 C16 -15.8(3) . . . . ? C16 C11 C12 C13 -4.6(4) . . . . ? N2 C11 C12 C13 -178.3(2) . . . . ? C11 C12 C13 C14 2.7(4) . . . . ? C12 C13 C14 C15 1.2(4) . . . . ? C13 C14 C15 C16 -3.1(4) . . . . ? C14 C15 C16 C11 1.1(4) . . . . ? C14 C15 C16 N3 175.9(2) . . . . ? C12 C11 C16 C15 2.7(4) . . . . ? N2 C11 C16 C15 177.1(2) . . . . ? C12 C11 C16 N3 -172.7(2) . . . . ? N2 C11 C16 N3 1.6(3) . . . . ? C17 N3 C16 C15 21.0(4) . . . . ? Ni1 N3 C16 C15 -161.7(2) . . . . ? C17 N3 C16 C11 -164.0(2) . . . . ? Ni1 N3 C16 C11 13.3(3) . . . . ? C16 N3 C17 C19 -173.4(2) . . . . ? Ni1 N3 C17 C19 9.8(4) . . . . ? C16 N3 C17 C18 6.0(4) . . . . ? Ni1 N3 C17 C18 -170.82(18) . . . . ? Fe1 O6 C18 O5 -4.2(4) 2_645 . . . ? Fe1 O6 C18 C17 177.63(16) 2_645 . . . ? N3 C17 C18 O5 78.3(3) . . . . ? C19 C17 C18 O5 -102.2(3) . . . . ? N3 C17 C18 O6 -103.3(3) . . . . ? C19 C17 C18 O6 76.2(3) . . . . ? N3 C17 C19 C20 -172.2(2) . . . . ? C18 C17 C19 C20 8.3(3) . . . . ? N3 C17 C19 C24 11.7(4) . . . . ? C18 C17 C19 C24 -167.7(2) . . . . ? C24 C19 C20 C21 -0.5(4) . . . . ? C17 C19 C20 C21 -176.8(2) . . . . ? C19 C20 C21 C22 0.8(4) . . . . ? C20 C21 C22 C23 0.4(4) . . . . ? C21 C22 C23 C24 -1.9(4) . . . . ? C1 N4 C24 C23 -19.4(4) . . . . ? Ni1 N4 C24 C23 162.3(2) . . . . ? C1 N4 C24 C19 165.8(2) . . . . ? Ni1 N4 C24 C19 -12.5(3) . . . . ? C22 C23 C24 N4 -172.7(2) . . . . ? C22 C23 C24 C19 2.2(4) . . . . ? C20 C19 C24 N4 174.0(2) . . . . ? C17 C19 C24 N4 -10.0(4) . . . . ? C20 C19 C24 C23 -1.0(4) . . . . ? C17 C19 C24 C23 175.1(2) . . . . ? O7 Fe1 O9 C25 -77(2) . . . . ? O6 Fe1 O9 C25 3(5) 2_655 . . . ? O8 Fe1 O9 C25 -165(2) . . . . ? O9' Fe1 O9 C25 139(3) . . . . ? O2 Fe1 O9 C25 7(2) . . . . ? O1 Fe1 O9 C25 83(2) . . . . ? O9 Fe1 O9' C25' -89.4(11) . . . . ? O7 Fe1 O9' C25' -125.5(6) . . . . ? O6 Fe1 O9' C25' 75.6(7) 2_655 . . . ? O8 Fe1 O9' C25' 147.0(6) . . . . ? O2 Fe1 O9' C25' -39.5(6) . . . . ? O1 Fe1 O9' C25' 35.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.853 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.113 # Attachment 'compound 3.cif' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 839541' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 N4 Ni2 O12' _chemical_formula_weight 705.91 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3667(10) _cell_length_b 9.0896(6) _cell_length_c 24.9074(12) _cell_angle_alpha 90.00 _cell_angle_beta 126.332(3) _cell_angle_gamma 90.00 _cell_volume 2802.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9255 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.85 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7947 _exptl_absorpt_correction_T_max 0.8156 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13921 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4935 _reflns_number_gt 4282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.0951P] 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 4935 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.08465(2) 0.55365(3) 0.891858(14) 0.02509(9) Uani 1 1 d . . . Ni2 Ni -0.32533(2) 0.47250(3) 0.723514(14) 0.02618(9) Uani 1 1 d . . . N1 N -0.01609(15) 0.4482(2) 0.89546(9) 0.0275(4) Uani 1 1 d . . . N2 N -0.02926(14) 0.6761(2) 0.82985(9) 0.0264(4) Uani 1 1 d . . . N3 N 0.18548(14) 0.6531(2) 0.88555(9) 0.0275(4) Uani 1 1 d . . . N4 N 0.19890(15) 0.4311(2) 0.95293(9) 0.0287(4) Uani 1 1 d . . . O1 O -0.19972(12) 0.39744(18) 0.81641(8) 0.0303(4) Uani 1 1 d . . . O2 O -0.21490(12) 0.64192(18) 0.75208(8) 0.0316(4) Uani 1 1 d . . . O3 O 0.24774(12) 0.86991(18) 0.81030(8) 0.0317(4) Uani 1 1 d . . . O4 O 0.34395(14) 0.9191(2) 0.91976(9) 0.0445(5) Uani 1 1 d . . . O5 O 0.35787(17) 0.4341(2) 1.10557(10) 0.0572(6) Uani 1 1 d . . . O6 O 0.35726(14) 0.2006(2) 1.07847(9) 0.0492(5) Uani 1 1 d . . . O7 O -0.43642(14) 0.5630(2) 0.63324(9) 0.0463(5) Uani 1 1 d . . . H7A H -0.4223 0.5258 0.6079 0.069 Uiso 1 1 d R . . H7B H -0.4812 0.6339 0.6176 0.069 Uiso 1 1 d R . . O8 O -0.38780(15) 0.5684(2) 0.76828(10) 0.0478(5) Uani 1 1 d . . . H8A H -0.4532 0.5966 0.7428 0.072 Uiso 1 1 d R . . H8B H -0.3650 0.5377 0.8068 0.072 Uiso 1 1 d R . . O9 O -0.42280(13) 0.2933(2) 0.69560(9) 0.0409(4) Uani 1 1 d . . . H9A H -0.4118 0.2408 0.7273 0.061 Uiso 1 1 d R . . H9B H -0.4877 0.3013 0.6611 0.061 Uiso 1 1 d R . . C1 C -0.11497(17) 0.4689(2) 0.83936(11) 0.0257(5) Uani 1 1 d . . . C2 C -0.12372(17) 0.6065(2) 0.80142(11) 0.0255(5) Uani 1 1 d . . . C3 C -0.02050(18) 0.8229(3) 0.81603(11) 0.0281(5) Uani 1 1 d . . . C4 C 0.08188(18) 0.8796(3) 0.83938(12) 0.0289(5) Uani 1 1 d . . . C5 C 0.0917(2) 1.0321(3) 0.83316(14) 0.0387(6) Uani 1 1 d . . . H5 H 0.1588 1.0701 0.8482 0.046 Uiso 1 1 calc R . . C6 C 0.0057(2) 1.1253(3) 0.80580(14) 0.0419(6) Uani 1 1 d . . . H6 H 0.0149 1.2260 0.8042 0.050 Uiso 1 1 calc R . . C7 C -0.0953(2) 1.0680(3) 0.78038(14) 0.0413(6) Uani 1 1 d . . . H7 H -0.1547 1.1304 0.7605 0.050 Uiso 1 1 calc R . . C8 C -0.1087(2) 0.9193(3) 0.78425(13) 0.0379(6) Uani 1 1 d . . . H8 H -0.1776 0.8824 0.7654 0.045 Uiso 1 1 calc R . . C9 C 0.17752(18) 0.7882(3) 0.86610(11) 0.0284(5) Uani 1 1 d . . . C10 C 0.26674(18) 0.8650(3) 0.86649(12) 0.0308(5) Uani 1 1 d . . . C11 C 0.27573(18) 0.5588(3) 0.90688(11) 0.0300(5) Uani 1 1 d . . . C12 C 0.28391(18) 0.4394(3) 0.94535(11) 0.0294(5) Uani 1 1 d . . . C13 C 0.36213(19) 0.3328(3) 0.96557(13) 0.0375(6) Uani 1 1 d . . . H13 H 0.3671 0.2525 0.9904 0.045 Uiso 1 1 calc R . . C14 C 0.4323(2) 0.3464(3) 0.94871(13) 0.0406(6) Uani 1 1 d . . . H14 H 0.4861 0.2763 0.9633 0.049 Uiso 1 1 calc R . . C15 C 0.4238(2) 0.4623(3) 0.91055(13) 0.0399(6) Uani 1 1 d . . . H15 H 0.4713 0.4695 0.8991 0.048 Uiso 1 1 calc R . . C16 C 0.34539(19) 0.5684(3) 0.88896(13) 0.0359(6) Uani 1 1 d . . . H16 H 0.3393 0.6458 0.8625 0.043 Uiso 1 1 calc R . . C17 C 0.20737(18) 0.3606(3) 1.00149(11) 0.0304(5) Uani 1 1 d . . . C18 C 0.3190(2) 0.3264(3) 1.06714(13) 0.0386(6) Uani 1 1 d . . . C19 C 0.11439(19) 0.3213(3) 1.00002(12) 0.0314(5) Uani 1 1 d . . . C20 C 0.00570(19) 0.3531(3) 0.94662(11) 0.0294(5) Uani 1 1 d . . . C21 C -0.0764(2) 0.2973(3) 0.94921(13) 0.0414(6) Uani 1 1 d . . . H21 H -0.1479 0.3187 0.9148 0.050 Uiso 1 1 calc R . . C22 C -0.0537(2) 0.2109(3) 1.00178(14) 0.0464(7) Uani 1 1 d . . . H22 H -0.1099 0.1737 1.0020 0.056 Uiso 1 1 calc R . . C23 C 0.0515(2) 0.1797(3) 1.05378(14) 0.0458(7) Uani 1 1 d . . . H23 H 0.0667 0.1211 1.0890 0.055 Uiso 1 1 calc R . . C24 C 0.1332(2) 0.2353(3) 1.05322(13) 0.0425(6) Uani 1 1 d . . . H24 H 0.2042 0.2159 1.0892 0.051 Uiso 1 1 calc R . . C25 C 0.3268(3) 0.5408(4) 0.68186(18) 0.0703(10) Uani 1 1 d . . . H25A H 0.3111 0.4940 0.6420 0.084 Uiso 1 1 calc R . . H25B H 0.2603 0.5826 0.6713 0.084 Uiso 1 1 calc R . . C26 C 0.3683(3) 0.4314(4) 0.7349(2) 0.0845(13) Uani 1 1 d . . . H26A H 0.4376 0.3972 0.7481 0.127 Uiso 1 1 calc R . . H26B H 0.3191 0.3500 0.7188 0.127 Uiso 1 1 calc R . . H26C H 0.3756 0.4753 0.7724 0.127 Uiso 1 1 calc R . . O10 O 0.6109(3) 0.2677(4) 0.90009(18) 0.0613(8) Uani 0.636(4) 1 d P A 1 O10' O 0.6852(5) 0.2938(7) 0.9114(3) 0.0613(8) Uani 0.364(4) 1 d P A 2 O11 O 0.6944(3) 0.4373(3) 0.48515(16) 0.1242(14) Uani 1 1 d . . . H11A H 0.6498 0.4427 0.4947 0.186 Uiso 1 1 d R . . H11B H 0.7263 0.3555 0.4922 0.186 Uiso 1 1 d R . . O12 O 0.40426(15) 0.6540(2) 0.70256(9) 0.0458(5) Uani 1 1 d . . . H12 H 0.3888 0.7015 0.6700 0.069 Uiso 1 1 calc R . . 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 0.02137(15) 0.02590(16) 0.02689(16) 0.00457(12) 0.01369(13) 0.00126(11) Ni2 0.02105(15) 0.02956(17) 0.02821(16) 0.00181(12) 0.01475(13) 0.00182(12) N1 0.0251(10) 0.0278(10) 0.0276(10) 0.0044(8) 0.0146(8) -0.0005(8) N2 0.0234(9) 0.0257(10) 0.0303(10) 0.0043(8) 0.0161(8) 0.0005(8) N3 0.0240(9) 0.0306(11) 0.0288(10) 0.0014(8) 0.0161(8) 0.0012(8) N4 0.0253(10) 0.0294(10) 0.0291(10) 0.0023(8) 0.0149(9) 0.0015(8) O1 0.0248(8) 0.0335(9) 0.0293(8) 0.0033(7) 0.0143(7) -0.0034(7) O2 0.0232(8) 0.0309(9) 0.0343(9) 0.0070(7) 0.0135(7) 0.0028(7) O3 0.0312(8) 0.0353(9) 0.0335(9) -0.0019(7) 0.0218(8) -0.0064(7) O4 0.0382(10) 0.0585(12) 0.0358(10) -0.0113(9) 0.0214(9) -0.0180(9) O5 0.0559(13) 0.0590(13) 0.0346(11) -0.0058(10) 0.0147(10) -0.0071(11) O6 0.0407(10) 0.0515(12) 0.0431(11) 0.0133(9) 0.0181(9) 0.0149(9) O7 0.0390(10) 0.0543(12) 0.0395(10) 0.0156(9) 0.0199(9) 0.0208(9) O8 0.0418(10) 0.0648(13) 0.0445(11) 0.0026(9) 0.0299(9) 0.0122(9) O9 0.0312(9) 0.0471(11) 0.0359(10) 0.0016(8) 0.0152(8) -0.0099(8) C1 0.0260(11) 0.0257(12) 0.0286(12) 0.0007(9) 0.0181(10) 0.0010(9) C2 0.0256(11) 0.0267(12) 0.0274(12) 0.0014(9) 0.0174(10) 0.0023(9) C3 0.0325(12) 0.0265(12) 0.0304(12) 0.0034(9) 0.0214(11) 0.0018(10) C4 0.0320(12) 0.0286(12) 0.0321(12) 0.0017(10) 0.0223(11) -0.0001(10) C5 0.0426(14) 0.0301(13) 0.0519(16) -0.0009(12) 0.0328(13) -0.0055(11) C6 0.0554(16) 0.0244(13) 0.0567(17) 0.0059(12) 0.0390(15) 0.0004(12) C7 0.0449(15) 0.0320(14) 0.0502(16) 0.0112(12) 0.0300(14) 0.0112(12) C8 0.0334(13) 0.0327(14) 0.0475(15) 0.0106(11) 0.0240(12) 0.0048(11) C9 0.0287(12) 0.0317(13) 0.0268(12) -0.0025(10) 0.0176(10) -0.0043(10) C10 0.0302(12) 0.0295(13) 0.0363(14) -0.0001(10) 0.0217(11) -0.0015(10) C11 0.0242(11) 0.0337(13) 0.0292(12) -0.0019(10) 0.0141(10) 0.0010(10) C12 0.0244(11) 0.0330(13) 0.0256(12) -0.0022(10) 0.0120(10) 0.0010(10) C13 0.0344(13) 0.0360(14) 0.0378(14) 0.0033(11) 0.0191(12) 0.0063(11) C14 0.0321(13) 0.0431(15) 0.0422(15) -0.0048(12) 0.0196(12) 0.0079(11) C15 0.0313(13) 0.0520(17) 0.0410(15) -0.0040(12) 0.0240(12) 0.0031(12) C16 0.0316(13) 0.0405(14) 0.0390(14) 0.0004(11) 0.0227(12) 0.0002(11) C17 0.0310(12) 0.0272(12) 0.0279(12) 0.0019(10) 0.0146(10) 0.0033(10) C18 0.0344(13) 0.0453(16) 0.0311(14) 0.0065(12) 0.0166(12) 0.0019(12) C19 0.0338(12) 0.0306(13) 0.0282(12) 0.0036(10) 0.0175(11) 0.0025(10) C20 0.0332(12) 0.0277(12) 0.0275(12) 0.0014(10) 0.0181(10) -0.0009(10) C21 0.0349(14) 0.0479(16) 0.0390(15) 0.0092(12) 0.0206(12) -0.0022(12) C22 0.0498(16) 0.0515(17) 0.0460(16) 0.0112(13) 0.0329(14) -0.0031(14) C23 0.0567(17) 0.0489(17) 0.0403(15) 0.0172(13) 0.0334(15) 0.0088(14) C24 0.0420(15) 0.0509(17) 0.0324(14) 0.0138(12) 0.0209(12) 0.0112(13) C25 0.070(2) 0.070(2) 0.064(2) -0.0190(18) 0.0360(19) -0.0291(19) C26 0.073(2) 0.059(2) 0.131(4) 0.016(2) 0.066(3) -0.0034(19) O10 0.062(2) 0.0533(18) 0.0635(19) -0.0065(15) 0.035(2) -0.0074(17) O10' 0.062(2) 0.0533(18) 0.0635(19) -0.0065(15) 0.035(2) -0.0074(17) O11 0.261(4) 0.0655(17) 0.121(3) 0.0159(17) 0.154(3) 0.036(2) O12 0.0469(11) 0.0465(12) 0.0455(11) -0.0043(9) 0.0281(10) -0.0010(9) _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 N4 1.8632(19) . ? Ni1 N2 1.8667(18) . ? Ni1 N1 1.8675(19) . ? Ni1 N3 1.8791(19) . ? Ni2 O7 2.0243(17) . ? Ni2 O9 2.0362(17) . ? Ni2 O3 2.0469(16) 2_546 ? Ni2 O8 2.0475(18) . ? Ni2 O1 2.0622(15) . ? Ni2 O2 2.0801(16) . ? N1 C1 1.334(3) . ? N1 C20 1.406(3) . ? N2 C2 1.338(3) . ? N2 C3 1.404(3) . ? N3 C9 1.299(3) . ? N3 C11 1.438(3) . ? N4 C17 1.305(3) . ? N4 C12 1.428(3) . ? O1 C1 1.250(3) . ? O2 C2 1.240(3) . ? O3 C10 1.250(3) . ? O3 Ni2 2.0469(16) 2_556 ? O4 C10 1.243(3) . ? O5 C18 1.247(3) . ? O6 C18 1.240(3) . ? O7 H7A 0.8500 . ? O7 H7B 0.8505 . ? O8 H8A 0.8500 . ? O8 H8B 0.8501 . ? O9 H9A 0.8497 . ? O9 H9B 0.8502 . ? C1 C2 1.525(3) . ? C3 C8 1.400(3) . ? C3 C4 1.412(3) . ? C4 C5 1.413(3) . ? C4 C9 1.461(3) . ? C5 C6 1.363(4) . ? C5 H5 0.9300 . ? C6 C7 1.385(4) . ? C6 H6 0.9300 . ? C7 C8 1.379(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.533(3) . ? C11 C16 1.385(3) . ? C11 C12 1.403(3) . ? C12 C13 1.386(3) . ? C13 C14 1.375(4) . ? C13 H13 0.9300 . ? C14 C15 1.373(4) . ? C14 H14 0.9300 . ? C15 C16 1.379(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C19 1.452(3) . ? C17 C18 1.546(3) . ? C19 C24 1.413(3) . ? C19 C20 1.418(3) . ? C20 C21 1.395(3) . ? C21 C22 1.383(4) . ? C21 H21 0.9300 . ? C22 C23 1.375(4) . ? C22 H22 0.9300 . ? C23 C24 1.362(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O12 1.420(4) . ? C25 C26 1.463(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O11 H11A 0.8502 . ? O11 H11B 0.8500 . ? O12 H12 0.8200 . ? 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 N4 Ni1 N2 179.19(8) . . ? N4 Ni1 N1 93.49(8) . . ? N2 Ni1 N1 87.02(8) . . ? N4 Ni1 N3 86.05(8) . . ? N2 Ni1 N3 93.41(8) . . ? N1 Ni1 N3 177.36(9) . . ? O7 Ni2 O9 88.85(8) . . ? O7 Ni2 O3 92.38(7) . 2_546 ? O9 Ni2 O3 89.14(7) . 2_546 ? O7 Ni2 O8 94.19(8) . . ? O9 Ni2 O8 92.24(8) . . ? O3 Ni2 O8 173.31(7) 2_546 . ? O7 Ni2 O1 173.43(7) . . ? O9 Ni2 O1 97.39(7) . . ? O3 Ni2 O1 85.68(6) 2_546 . ? O8 Ni2 O1 87.65(7) . . ? O7 Ni2 O2 93.41(7) . . ? O9 Ni2 O2 174.29(7) . . ? O3 Ni2 O2 85.53(7) 2_546 . ? O8 Ni2 O2 92.83(8) . . ? O1 Ni2 O2 80.19(6) . . ? C1 N1 C20 123.19(19) . . ? C1 N1 Ni1 109.85(15) . . ? C20 N1 Ni1 126.86(15) . . ? C2 N2 C3 123.44(19) . . ? C2 N2 Ni1 110.33(14) . . ? C3 N2 Ni1 126.17(15) . . ? C9 N3 C11 124.0(2) . . ? C9 N3 Ni1 125.87(16) . . ? C11 N3 Ni1 110.16(15) . . ? C17 N4 C12 123.47(19) . . ? C17 N4 Ni1 125.33(16) . . ? C12 N4 Ni1 110.72(15) . . ? C1 O1 Ni2 111.73(14) . . ? C2 O2 Ni2 111.13(14) . . ? C10 O3 Ni2 132.10(15) . 2_556 ? Ni2 O7 H7A 104.2 . . ? Ni2 O7 H7B 137.5 . . ? H7A O7 H7B 117.1 . . ? Ni2 O8 H8A 116.8 . . ? Ni2 O8 H8B 117.6 . . ? H8A O8 H8B 117.1 . . ? Ni2 O9 H9A 115.6 . . ? Ni2 O9 H9B 117.5 . . ? H9A O9 H9B 117.1 . . ? O1 C1 N1 129.6(2) . . ? O1 C1 C2 117.21(19) . . ? N1 C1 C2 113.08(19) . . ? O2 C2 N2 129.5(2) . . ? O2 C2 C1 117.42(19) . . ? N2 C2 C1 112.97(18) . . ? C8 C3 N2 122.2(2) . . ? C8 C3 C4 118.2(2) . . ? N2 C3 C4 119.4(2) . . ? C3 C4 C5 118.5(2) . . ? C3 C4 C9 123.7(2) . . ? C5 C4 C9 117.7(2) . . ? C6 C5 C4 122.0(2) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 119.1(2) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 120.7(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 121.2(2) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? N3 C9 C4 123.7(2) . . ? N3 C9 C10 122.8(2) . . ? C4 C9 C10 113.5(2) . . ? O4 C10 O3 128.5(2) . . ? O4 C10 C9 118.1(2) . . ? O3 C10 C9 113.2(2) . . ? C16 C11 C12 119.7(2) . . ? C16 C11 N3 127.1(2) . . ? C12 C11 N3 113.0(2) . . ? C13 C12 C11 119.8(2) . . ? C13 C12 N4 125.4(2) . . ? C11 C12 N4 114.3(2) . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.6(2) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? N4 C17 C19 122.8(2) . . ? N4 C17 C18 121.2(2) . . ? C19 C17 C18 115.8(2) . . ? O6 C18 O5 127.1(2) . . ? O6 C18 C17 120.4(2) . . ? O5 C18 C17 112.4(2) . . ? C24 C19 C20 117.8(2) . . ? C24 C19 C17 117.4(2) . . ? C20 C19 C17 124.6(2) . . ? C21 C20 N1 121.9(2) . . ? C21 C20 C19 118.5(2) . . ? N1 C20 C19 119.4(2) . . ? C22 C21 C20 121.5(2) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 119.3(2) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 122.5(2) . . ? C23 C24 H24 118.7 . . ? C19 C24 H24 118.7 . . ? O12 C25 C26 110.0(3) . . ? O12 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? O12 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H11A O11 H11B 117.1 . . ? C25 O12 H12 109.5 . . ? 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 N4 Ni1 N1 C1 -155.72(16) . . . . ? N2 Ni1 N1 C1 23.65(16) . . . . ? N3 Ni1 N1 C1 -75.8(18) . . . . ? N4 Ni1 N1 C20 20.7(2) . . . . ? N2 Ni1 N1 C20 -159.9(2) . . . . ? N3 Ni1 N1 C20 100.6(18) . . . . ? N4 Ni1 N2 C2 107(6) . . . . ? N1 Ni1 N2 C2 -21.82(16) . . . . ? N3 Ni1 N2 C2 155.57(15) . . . . ? N4 Ni1 N2 C3 -76(6) . . . . ? N1 Ni1 N2 C3 155.35(19) . . . . ? N3 Ni1 N2 C3 -27.26(19) . . . . ? N4 Ni1 N3 C9 -157.1(2) . . . . ? N2 Ni1 N3 C9 23.5(2) . . . . ? N1 Ni1 N3 C9 122.7(17) . . . . ? N4 Ni1 N3 C11 21.68(15) . . . . ? N2 Ni1 N3 C11 -157.71(15) . . . . ? N1 Ni1 N3 C11 -58.4(18) . . . . ? N2 Ni1 N4 C17 -160(6) . . . . ? N1 Ni1 N4 C17 -30.6(2) . . . . ? N3 Ni1 N4 C17 152.1(2) . . . . ? N2 Ni1 N4 C12 28(6) . . . . ? N1 Ni1 N4 C12 157.24(16) . . . . ? N3 Ni1 N4 C12 -20.15(16) . . . . ? O7 Ni2 O1 C1 1.2(7) . . . . ? O9 Ni2 O1 C1 162.88(15) . . . . ? O3 Ni2 O1 C1 74.31(15) 2_546 . . . ? O8 Ni2 O1 C1 -105.17(16) . . . . ? O2 Ni2 O1 C1 -11.89(15) . . . . ? O7 Ni2 O2 C2 -164.99(16) . . . . ? O9 Ni2 O2 C2 -51.8(8) . . . . ? O3 Ni2 O2 C2 -72.86(15) 2_546 . . . ? O8 Ni2 O2 C2 100.64(16) . . . . ? O1 Ni2 O2 C2 13.52(15) . . . . ? Ni2 O1 C1 N1 -175.5(2) . . . . ? Ni2 O1 C1 C2 8.9(2) . . . . ? C20 N1 C1 O1 -12.5(4) . . . . ? Ni1 N1 C1 O1 164.1(2) . . . . ? C20 N1 C1 C2 163.3(2) . . . . ? Ni1 N1 C1 C2 -20.1(2) . . . . ? Ni2 O2 C2 N2 171.1(2) . . . . ? Ni2 O2 C2 C1 -13.0(2) . . . . ? C3 N2 C2 O2 14.2(4) . . . . ? Ni1 N2 C2 O2 -168.6(2) . . . . ? C3 N2 C2 C1 -161.9(2) . . . . ? Ni1 N2 C2 C1 15.4(2) . . . . ? O1 C1 C2 O2 3.0(3) . . . . ? N1 C1 C2 O2 -173.3(2) . . . . ? O1 C1 C2 N2 179.6(2) . . . . ? N1 C1 C2 N2 3.3(3) . . . . ? C2 N2 C3 C8 15.9(3) . . . . ? Ni1 N2 C3 C8 -160.95(19) . . . . ? C2 N2 C3 C4 -169.3(2) . . . . ? Ni1 N2 C3 C4 13.9(3) . . . . ? C8 C3 C4 C5 3.7(3) . . . . ? N2 C3 C4 C5 -171.3(2) . . . . ? C8 C3 C4 C9 -172.4(2) . . . . ? N2 C3 C4 C9 12.5(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C9 C4 C5 C6 176.8(2) . . . . ? C4 C5 C6 C7 -3.2(4) . . . . ? C5 C6 C7 C8 1.8(4) . . . . ? C6 C7 C8 C3 2.4(4) . . . . ? N2 C3 C8 C7 169.7(2) . . . . ? C4 C3 C8 C7 -5.2(4) . . . . ? C11 N3 C9 C4 174.8(2) . . . . ? Ni1 N3 C9 C4 -6.5(3) . . . . ? C11 N3 C9 C10 -2.6(3) . . . . ? Ni1 N3 C9 C10 176.00(16) . . . . ? C3 C4 C9 N3 -16.7(4) . . . . ? C5 C4 C9 N3 167.1(2) . . . . ? C3 C4 C9 C10 160.9(2) . . . . ? C5 C4 C9 C10 -15.3(3) . . . . ? Ni2 O3 C10 O4 -3.2(4) 2_556 . . . ? Ni2 O3 C10 C9 173.11(15) 2_556 . . . ? N3 C9 C10 O4 -82.4(3) . . . . ? C4 C9 C10 O4 99.9(3) . . . . ? N3 C9 C10 O3 100.9(3) . . . . ? C4 C9 C10 O3 -76.8(3) . . . . ? C9 N3 C11 C16 -25.5(4) . . . . ? Ni1 N3 C11 C16 155.7(2) . . . . ? C9 N3 C11 C12 160.2(2) . . . . ? Ni1 N3 C11 C12 -18.7(2) . . . . ? C16 C11 C12 C13 0.6(3) . . . . ? N3 C11 C12 C13 175.4(2) . . . . ? C16 C11 C12 N4 -171.9(2) . . . . ? N3 C11 C12 N4 2.9(3) . . . . ? C17 N4 C12 C13 30.1(4) . . . . ? Ni1 N4 C12 C13 -157.6(2) . . . . ? C17 N4 C12 C11 -158.0(2) . . . . ? Ni1 N4 C12 C11 14.4(2) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? N4 C12 C13 C14 172.7(2) . . . . ? C12 C13 C14 C15 -1.8(4) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C11 1.0(4) . . . . ? C12 C11 C16 C15 -1.6(4) . . . . ? N3 C11 C16 C15 -175.6(2) . . . . ? C12 N4 C17 C19 -164.0(2) . . . . ? Ni1 N4 C17 C19 24.7(3) . . . . ? C12 N4 C17 C18 21.5(3) . . . . ? Ni1 N4 C17 C18 -149.73(19) . . . . ? N4 C17 C18 O6 -103.8(3) . . . . ? C19 C17 C18 O6 81.4(3) . . . . ? N4 C17 C18 O5 80.4(3) . . . . ? C19 C17 C18 O5 -94.4(3) . . . . ? N4 C17 C19 C24 175.3(2) . . . . ? C18 C17 C19 C24 -10.0(3) . . . . ? N4 C17 C19 C20 0.5(4) . . . . ? C18 C17 C19 C20 175.2(2) . . . . ? C1 N1 C20 C21 -14.0(4) . . . . ? Ni1 N1 C20 C21 170.05(19) . . . . ? C1 N1 C20 C19 170.9(2) . . . . ? Ni1 N1 C20 C19 -5.0(3) . . . . ? C24 C19 C20 C21 -0.4(4) . . . . ? C17 C19 C20 C21 174.4(2) . . . . ? C24 C19 C20 N1 174.8(2) . . . . ? C17 C19 C20 N1 -10.4(4) . . . . ? N1 C20 C21 C22 -176.1(3) . . . . ? C19 C20 C21 C22 -1.0(4) . . . . ? C20 C21 C22 C23 1.1(5) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C19 -1.8(5) . . . . ? C20 C19 C24 C23 1.9(4) . . . . ? C17 C19 C24 C23 -173.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.052 # Attachment 'compound 4.cif' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 839542' #TrackingRef 'compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 N8 Ni2 O26 Zn2' _chemical_formula_weight 1405.14 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9653(18) _cell_length_b 15.482(3) _cell_length_c 19.932(4) _cell_angle_alpha 90.78(3) _cell_angle_beta 91.84(3) _cell_angle_gamma 91.97(3) _cell_volume 2763.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5535 _cell_measurement_theta_min 2.045 _cell_measurement_theta_max 27.831 _exptl_crystal_description prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.8289 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20607 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9723 _reflns_number_gt 6675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The restraints (dfix) are applied to keep the bond geometries and dsps of water molecules structurally reasonable such as: DFIX 0.85 0.01 O22 H22A O22 H22B O20 H20A O20 H20B DFIX 1.45 0.01 H20A H20B H22A H22B H23A H23B DFIX 0.85 0.01 O19 H19A O19 H19B O24 H24A O24 H24B DFIX 1.45 0.01 H19A H19B H24A H24B H25A H25B H26A H26B DFIX 0.85 0.01 O23 H23A O23 H23B O21 H21B DFIX 0.85 0.01 O26 H26A O25 H25A O26 H26B O25 H25B O21 H21A Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9723 _refine_ls_number_parameters 775 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.112 _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 Zn1 Zn 0.89740(8) 0.43782(5) 0.28176(4) 0.0180(2) Uani 1 1 d . . . Zn2 Zn 0.44194(8) 1.04247(5) 0.21283(4) 0.0178(2) Uani 1 1 d . . . Ni1 Ni 0.52921(9) 0.80419(5) 0.39014(4) 0.0150(2) Uani 1 1 d . . . Ni2 Ni 1.00674(9) 0.67110(5) 0.10444(4) 0.0161(2) Uani 1 1 d . . . O1 O 0.6103(5) 0.9590(3) 0.2447(2) 0.0188(10) Uani 1 1 d . . . O2 O 0.3691(5) 1.0083(3) 0.3115(2) 0.0171(10) Uani 1 1 d . . . O3 O 0.1388(5) 0.7216(3) 0.5631(2) 0.0223(11) Uani 1 1 d . . . O4 O 0.3791(5) 0.7173(3) 0.5983(2) 0.0258(11) Uani 1 1 d . . . O5 O 0.8866(5) 0.5760(3) 0.4209(2) 0.0217(10) Uani 1 1 d . . . O6 O 0.8299(5) 0.5612(3) 0.3100(2) 0.0187(10) Uani 1 1 d . . . O7 O 0.8376(5) 0.4678(3) 0.1843(2) 0.0207(10) Uani 1 1 d . . . O8 O 1.0954(5) 0.5145(3) 0.2509(2) 0.0196(10) Uani 1 1 d . . . O9 O 1.3712(5) 0.9053(3) 0.0717(2) 0.0216(11) Uani 1 1 d . . . O10 O 1.3286(5) 0.9242(3) 0.1821(2) 0.0202(10) Uani 1 1 d . . . O11 O 0.8004(5) 0.7544(3) -0.1064(2) 0.0273(11) Uani 1 1 d . . . O12 O 0.5756(5) 0.7268(3) -0.0637(2) 0.0244(11) Uani 1 1 d . . . O13 O 0.5696(5) 1.1444(3) 0.2500(2) 0.0297(12) Uani 1 1 d . . . H13A H 0.5731 1.1555 0.2919 0.036 Uiso 1 1 d R . . H13B H 0.6192 1.1760 0.2236 0.036 Uiso 1 1 d R . . O14 O 0.4967(6) 1.0577(3) 0.1153(2) 0.0308(13) Uani 1 1 d . . . H14A H 0.4713 1.0188 0.0862 0.037 Uiso 1 1 d R . . H14B H 0.5447 1.1031 0.1035 0.037 Uiso 1 1 d R . . O15 O 0.2524(5) 1.1126(3) 0.1978(2) 0.0279(11) Uani 1 1 d . . . H15A H 0.1886 1.1153 0.2283 0.033 Uiso 1 1 d R . . H15B H 0.2381 1.1387 0.1610 0.033 Uiso 1 1 d R . . O16 O 0.6871(5) 0.3848(3) 0.2958(2) 0.0239(11) Uani 1 1 d . . . H16A H 0.6120 0.4051 0.2752 0.029 Uiso 1 1 d R . . H16B H 0.6755 0.3426 0.3222 0.029 Uiso 1 1 d R . . O17 O 0.9825(5) 0.4185(3) 0.3760(2) 0.0217(11) Uani 1 1 d . . . H17A H 1.0683 0.4397 0.3877 0.026 Uiso 1 1 d R . . H17B H 0.9321 0.3893 0.4038 0.026 Uiso 1 1 d R . . O18 O 0.9773(5) 0.3209(3) 0.2503(2) 0.0273(11) Uani 1 1 d . . . H18A H 1.0621 0.3192 0.2326 0.033 Uiso 1 1 d R . . H18B H 0.9253 0.2746 0.2550 0.033 Uiso 1 1 d R . . N1 N 0.6502(6) 0.8572(3) 0.3281(2) 0.0152(11) Uani 1 1 d . . . N2 N 0.4320(6) 0.9082(3) 0.3938(2) 0.0156(11) Uani 1 1 d . . . N3 N 0.4016(5) 0.7503(3) 0.4501(2) 0.0142(11) Uani 1 1 d . . . N4 N 0.6236(6) 0.6985(3) 0.3839(2) 0.0149(11) Uani 1 1 d . . . N5 N 0.9045(6) 0.5651(4) 0.1010(2) 0.0193(12) Uani 1 1 d . . . N6 N 1.1287(6) 0.6239(3) 0.1710(2) 0.0164(12) Uani 1 1 d . . . N7 N 1.1045(6) 0.7802(3) 0.1102(2) 0.0163(12) Uani 1 1 d . . . N8 N 0.8765(6) 0.7197(3) 0.0413(2) 0.0178(12) Uani 1 1 d . . . C1 C 0.5799(7) 0.9199(4) 0.2968(3) 0.0176(14) Uani 1 1 d . . . C2 C 0.4443(7) 0.9493(4) 0.3355(3) 0.0168(14) Uani 1 1 d . . . C3 C 0.3456(7) 0.9383(4) 0.4470(3) 0.0160(14) Uani 1 1 d . . . C4 C 0.3123(7) 1.0255(4) 0.4530(3) 0.0192(14) Uani 1 1 d . . . H4 H 0.3446 1.0646 0.4197 0.023 Uiso 1 1 calc R . . C5 C 0.2336(8) 1.0566(5) 0.5063(3) 0.0257(16) Uani 1 1 d . . . H5 H 0.2099 1.1158 0.5088 0.031 Uiso 1 1 calc R . . C6 C 0.1892(8) 0.9996(5) 0.5564(4) 0.0288(17) Uani 1 1 d . . . H6 H 0.1344 1.0201 0.5930 0.035 Uiso 1 1 calc R . . C7 C 0.2248(8) 0.9149(5) 0.5525(3) 0.0253(16) Uani 1 1 d . . . H7 H 0.1953 0.8774 0.5874 0.030 Uiso 1 1 calc R . . C8 C 0.3048(7) 0.8802(4) 0.4981(3) 0.0198(15) Uani 1 1 d . . . C9 C 0.3289(7) 0.7886(4) 0.4972(3) 0.0172(14) Uani 1 1 d . . . C10 C 0.2753(8) 0.7360(4) 0.5583(3) 0.0209(15) Uani 1 1 d . . . C11 C 0.4051(7) 0.6586(4) 0.4420(3) 0.0189(14) Uani 1 1 d . . . C12 C 0.2902(7) 0.6009(4) 0.4601(3) 0.0212(15) Uani 1 1 d . . . H12 H 0.2042 0.6215 0.4810 0.025 Uiso 1 1 calc R . . C13 C 0.3037(7) 0.5127(4) 0.4471(3) 0.0226(16) Uani 1 1 d . . . H13 H 0.2283 0.4726 0.4606 0.027 Uiso 1 1 calc R . . C14 C 0.4261(7) 0.4840(4) 0.4148(3) 0.0206(15) Uani 1 1 d . . . H14 H 0.4356 0.4238 0.4072 0.025 Uiso 1 1 calc R . . C15 C 0.5355(7) 0.5410(4) 0.3932(3) 0.0193(14) Uani 1 1 d . . . H15 H 0.6170 0.5201 0.3692 0.023 Uiso 1 1 calc R . . C16 C 0.5261(7) 0.6292(4) 0.4066(3) 0.0175(14) Uani 1 1 d . . . C17 C 0.7576(7) 0.6872(4) 0.3636(3) 0.0162(14) Uani 1 1 d . . . C18 C 0.8309(7) 0.6005(4) 0.3659(3) 0.0169(14) Uani 1 1 d . . . C19 C 0.8519(7) 0.7565(4) 0.3360(3) 0.0171(14) Uani 1 1 d . . . C20 C 1.0047(7) 0.7396(4) 0.3283(3) 0.0218(15) Uani 1 1 d . . . H20 H 1.0416 0.6857 0.3423 0.026 Uiso 1 1 calc R . . C21 C 1.1016(7) 0.8002(5) 0.3006(3) 0.0254(16) Uani 1 1 d . . . H21 H 1.2048 0.7892 0.2976 0.031 Uiso 1 1 calc R . . C22 C 1.0458(7) 0.8772(5) 0.2775(3) 0.0237(16) Uani 1 1 d . . . H22 H 1.1112 0.9182 0.2574 0.028 Uiso 1 1 calc R . . C23 C 0.8978(7) 0.8952(4) 0.2829(3) 0.0222(15) Uani 1 1 d . . . H23 H 0.8619 0.9479 0.2661 0.027 Uiso 1 1 calc R . . C24 C 0.7977(7) 0.8356(4) 0.3136(3) 0.0163(14) Uani 1 1 d . . . C25 C 0.9189(7) 0.5260(4) 0.1605(3) 0.0171(14) Uani 1 1 d . . . C26 C 1.0592(7) 0.5569(4) 0.2001(3) 0.0160(14) Uani 1 1 d . . . C27 C 1.2781(7) 0.6500(4) 0.1869(3) 0.0184(14) Uani 1 1 d . . . C28 C 1.3758(8) 0.5971(5) 0.2217(3) 0.0246(16) Uani 1 1 d . . . H28 H 1.3374 0.5469 0.2431 0.030 Uiso 1 1 calc R . . C29 C 1.5290(8) 0.6166(5) 0.2257(3) 0.0267(16) Uani 1 1 d . . . H29 H 1.5945 0.5784 0.2477 0.032 Uiso 1 1 calc R . . C30 C 1.5858(8) 0.6919(5) 0.1976(3) 0.0244(16) Uani 1 1 d . . . H30 H 1.6903 0.7043 0.1991 0.029 Uiso 1 1 calc R . . C31 C 1.4908(7) 0.7482(5) 0.1677(3) 0.0221(15) Uani 1 1 d . . . H31 H 1.5300 0.8013 0.1512 0.027 Uiso 1 1 calc R . . C32 C 1.3353(7) 0.7291(4) 0.1609(3) 0.0156(14) Uani 1 1 d . . . C33 C 1.2418(7) 0.7948(4) 0.1308(3) 0.0190(15) Uani 1 1 d . . . C34 C 1.3209(7) 0.8839(4) 0.1280(3) 0.0211(15) Uani 1 1 d . . . C35 C 1.0085(7) 0.8449(4) 0.0863(3) 0.0172(14) Uani 1 1 d . . . C36 C 1.0190(7) 0.9336(4) 0.1017(3) 0.0222(15) Uani 1 1 d . . . H36 H 1.1000 0.9563 0.1292 0.027 Uiso 1 1 calc R . . C37 C 0.9125(8) 0.9878(4) 0.0772(3) 0.0249(16) Uani 1 1 d . . . H37 H 0.9231 1.0482 0.0861 0.030 Uiso 1 1 calc R . . C38 C 0.7896(8) 0.9551(4) 0.0398(3) 0.0254(16) Uani 1 1 d . . . H38 H 0.7166 0.9931 0.0232 0.030 Uiso 1 1 calc R . . C39 C 0.7730(8) 0.8676(4) 0.0265(3) 0.0251(16) Uani 1 1 d . . . H39 H 0.6863 0.8449 0.0029 0.030 Uiso 1 1 calc R . . C40 C 0.8837(7) 0.8129(4) 0.0479(3) 0.0186(14) Uani 1 1 d . . . C41 C 0.7895(7) 0.6790(4) -0.0041(3) 0.0181(14) Uani 1 1 d . . . C42 C 0.7149(8) 0.7258(4) -0.0627(3) 0.0224(16) Uani 1 1 d . . . C43 C 0.7633(7) 0.5851(4) -0.0040(3) 0.0164(14) Uani 1 1 d . . . C44 C 0.6743(8) 0.5463(5) -0.0570(3) 0.0237(16) Uani 1 1 d . . . H44 H 0.6439 0.5810 -0.0936 0.028 Uiso 1 1 calc R . . C45 C 0.6307(8) 0.4615(4) -0.0575(3) 0.0242(16) Uani 1 1 d . . . H45 H 0.5665 0.4384 -0.0926 0.029 Uiso 1 1 calc R . . C46 C 0.6814(8) 0.4081(5) -0.0057(3) 0.0258(17) Uani 1 1 d . . . H46 H 0.6540 0.3483 -0.0065 0.031 Uiso 1 1 calc R . . C47 C 0.7708(8) 0.4425(4) 0.0464(3) 0.0262(17) Uani 1 1 d . . . H47 H 0.8059 0.4060 0.0810 0.031 Uiso 1 1 calc R . . C48 C 0.8102(7) 0.5309(4) 0.0483(3) 0.0194(15) Uani 1 1 d . . . O19 O 0.3299(5) 0.8227(3) 0.9512(2) 0.0231(11) Uani 1 1 d D . . H19A H 0.3981 0.7865 0.9453 0.028 Uiso 1 1 d RD . . H19B H 0.3295 0.8463 0.9902 0.028 Uiso 1 1 d RD . . O20 O 0.5035(5) 0.3036(3) 0.2003(2) 0.0279(12) Uani 1 1 d D . . H20A H 0.5042 0.2992 0.1562 0.033 Uiso 1 1 d RD . . H20B H 0.4030 0.3136 0.2095 0.033 Uiso 1 1 d RD . . O21 O 0.6862(5) 0.7447(3) 0.6127(2) 0.0316(12) Uani 1 1 d D . . H21A H 0.5890 0.7420 0.6114 0.038 Uiso 1 1 d RD . . H21B H 0.7650 0.7463 0.5743 0.038 Uiso 1 1 d RD . . O22 O 0.1311(6) 0.1287(3) 0.3222(2) 0.0327(12) Uani 1 1 d D . . H22A H 0.1795 0.1719 0.3399 0.039 Uiso 1 1 d RD . . H22B H 0.1666 0.0789 0.3290 0.039 Uiso 1 1 d RD . . O23 O 0.8574(6) 0.7214(3) 0.5069(2) 0.0344(13) Uani 1 1 d D . . H23A H 0.8338 0.6747 0.5099 0.041 Uiso 1 1 d RD . . H23B H 0.9309 0.7463 0.5195 0.041 Uiso 1 1 d RD . . O24 O 0.2703(6) 0.3543(3) 0.2774(3) 0.0370(13) Uani 1 1 d D . . H24A H 0.2654 0.4058 0.2922 0.044 Uiso 1 1 d RD . . H24B H 0.2870 0.3154 0.3063 0.044 Uiso 1 1 d RD . . O25 O 0.0938(6) 0.7689(4) 0.8669(3) 0.0490(17) Uani 1 1 d D . . H25A H 0.0057 0.7625 0.8815 0.059 Uiso 1 1 d RD . . H25B H 0.1660 0.7793 0.8941 0.059 Uiso 1 1 d RD . . O26 O 0.8620(7) 0.1166(4) 0.2436(3) 0.0582(18) Uani 1 1 d D . . H26A H 0.8452 0.1568 0.2738 0.070 Uiso 1 1 d RD . . H26B H 0.9536 0.0990 0.2482 0.070 Uiso 1 1 d RD . . 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 Zn1 0.0215(4) 0.0165(4) 0.0162(4) 0.0030(3) 0.0007(3) 0.0010(3) Zn2 0.0208(4) 0.0162(4) 0.0164(4) 0.0034(3) -0.0008(3) -0.0006(3) Ni1 0.0159(4) 0.0138(4) 0.0156(4) 0.0034(3) 0.0018(3) 0.0010(3) Ni2 0.0176(5) 0.0145(4) 0.0158(4) 0.0032(3) -0.0037(3) -0.0009(3) O1 0.023(3) 0.019(3) 0.015(2) 0.0061(19) 0.0029(18) 0.001(2) O2 0.020(2) 0.019(2) 0.013(2) -0.0003(19) 0.0020(18) 0.002(2) O3 0.020(3) 0.025(3) 0.023(2) 0.005(2) 0.0072(19) 0.000(2) O4 0.025(3) 0.032(3) 0.021(2) 0.004(2) 0.001(2) 0.000(2) O5 0.026(3) 0.019(3) 0.020(2) 0.004(2) -0.008(2) 0.004(2) O6 0.020(2) 0.020(3) 0.016(2) -0.0006(19) -0.0004(18) 0.0014(19) O7 0.023(3) 0.020(3) 0.018(2) 0.004(2) -0.0020(19) -0.003(2) O8 0.022(3) 0.017(2) 0.020(2) 0.0038(19) -0.0026(19) 0.004(2) O9 0.027(3) 0.021(3) 0.016(2) 0.000(2) 0.0021(19) -0.006(2) O10 0.022(3) 0.025(3) 0.014(2) -0.003(2) 0.0007(18) -0.003(2) O11 0.025(3) 0.034(3) 0.024(3) 0.009(2) 0.001(2) 0.000(2) O12 0.018(3) 0.031(3) 0.024(3) -0.001(2) -0.002(2) 0.005(2) O13 0.033(3) 0.027(3) 0.028(3) 0.000(2) -0.003(2) -0.010(2) O14 0.051(3) 0.022(3) 0.020(3) -0.003(2) 0.010(2) -0.015(2) O15 0.026(3) 0.034(3) 0.025(3) 0.012(2) 0.002(2) 0.010(2) O16 0.027(3) 0.025(3) 0.019(2) 0.007(2) -0.003(2) -0.004(2) O17 0.019(2) 0.022(3) 0.024(2) 0.010(2) -0.0049(19) -0.006(2) O18 0.029(3) 0.018(3) 0.035(3) -0.001(2) 0.002(2) -0.001(2) N1 0.015(3) 0.012(3) 0.018(3) -0.003(2) -0.001(2) 0.000(2) N2 0.017(3) 0.014(3) 0.016(3) 0.005(2) 0.002(2) 0.000(2) N3 0.010(3) 0.015(3) 0.017(3) 0.003(2) 0.000(2) 0.003(2) N4 0.016(3) 0.014(3) 0.014(3) 0.000(2) 0.002(2) 0.001(2) N5 0.018(3) 0.024(3) 0.016(3) 0.002(2) -0.005(2) 0.000(2) N6 0.015(3) 0.016(3) 0.018(3) 0.003(2) 0.000(2) -0.002(2) N7 0.018(3) 0.014(3) 0.017(3) 0.003(2) -0.004(2) 0.002(2) N8 0.022(3) 0.016(3) 0.015(3) 0.002(2) 0.001(2) 0.000(2) C1 0.017(3) 0.016(4) 0.019(3) 0.000(3) -0.003(3) -0.004(3) C2 0.022(4) 0.011(3) 0.017(3) 0.002(3) -0.004(3) -0.004(3) C3 0.013(3) 0.022(4) 0.012(3) -0.004(3) -0.005(2) 0.000(3) C4 0.021(4) 0.017(4) 0.020(3) -0.003(3) 0.003(3) 0.005(3) C5 0.028(4) 0.027(4) 0.022(4) -0.001(3) 0.000(3) 0.002(3) C6 0.032(4) 0.029(4) 0.026(4) -0.009(3) 0.006(3) 0.004(3) C7 0.029(4) 0.028(4) 0.019(4) 0.007(3) 0.009(3) -0.003(3) C8 0.022(4) 0.018(4) 0.019(3) -0.006(3) 0.001(3) -0.001(3) C9 0.015(3) 0.019(4) 0.017(3) 0.000(3) -0.003(3) -0.005(3) C10 0.023(4) 0.017(4) 0.023(4) 0.004(3) 0.003(3) 0.007(3) C11 0.025(4) 0.017(4) 0.015(3) 0.003(3) -0.001(3) -0.001(3) C12 0.018(4) 0.019(4) 0.027(4) -0.002(3) 0.005(3) 0.000(3) C13 0.019(4) 0.025(4) 0.023(4) 0.000(3) -0.003(3) -0.003(3) C14 0.025(4) 0.012(3) 0.025(4) 0.004(3) -0.004(3) 0.000(3) C15 0.023(4) 0.015(3) 0.020(3) -0.002(3) 0.000(3) 0.001(3) C16 0.019(4) 0.017(4) 0.015(3) 0.008(3) -0.006(3) -0.009(3) C17 0.018(3) 0.015(3) 0.015(3) 0.001(3) -0.005(3) -0.001(3) C18 0.010(3) 0.017(3) 0.023(4) -0.002(3) -0.003(3) -0.005(3) C19 0.016(3) 0.025(4) 0.010(3) 0.003(3) -0.002(2) -0.001(3) C20 0.014(3) 0.019(4) 0.032(4) 0.002(3) 0.002(3) 0.002(3) C21 0.011(3) 0.034(4) 0.031(4) 0.000(3) 0.001(3) -0.001(3) C22 0.017(4) 0.030(4) 0.024(4) -0.002(3) 0.004(3) -0.001(3) C23 0.025(4) 0.021(4) 0.020(3) 0.001(3) -0.001(3) 0.002(3) C24 0.017(3) 0.018(4) 0.014(3) 0.000(3) 0.002(2) 0.002(3) C25 0.020(4) 0.014(3) 0.017(3) -0.002(3) -0.002(3) 0.004(3) C26 0.017(3) 0.019(4) 0.013(3) -0.002(3) 0.000(2) 0.007(3) C27 0.023(4) 0.021(4) 0.011(3) -0.004(3) 0.000(3) 0.002(3) C28 0.026(4) 0.025(4) 0.023(4) 0.008(3) -0.003(3) 0.000(3) C29 0.020(4) 0.036(4) 0.024(4) 0.001(3) -0.003(3) 0.010(3) C30 0.016(4) 0.033(4) 0.024(4) -0.004(3) 0.000(3) 0.002(3) C31 0.025(4) 0.023(4) 0.018(3) 0.002(3) -0.001(3) 0.000(3) C32 0.013(3) 0.014(3) 0.020(3) -0.003(3) -0.001(3) -0.002(3) C33 0.019(4) 0.027(4) 0.011(3) -0.001(3) 0.003(3) -0.001(3) C34 0.018(4) 0.019(4) 0.026(4) 0.002(3) -0.005(3) 0.001(3) C35 0.019(3) 0.019(4) 0.014(3) 0.003(3) 0.000(3) 0.002(3) C36 0.020(4) 0.020(4) 0.026(4) -0.004(3) -0.004(3) 0.001(3) C37 0.034(4) 0.011(3) 0.030(4) 0.003(3) -0.002(3) 0.009(3) C38 0.026(4) 0.020(4) 0.031(4) 0.003(3) -0.004(3) 0.010(3) C39 0.026(4) 0.019(4) 0.030(4) -0.001(3) -0.008(3) -0.001(3) C40 0.021(4) 0.016(4) 0.019(3) -0.001(3) 0.001(3) 0.000(3) C41 0.016(3) 0.022(4) 0.016(3) 0.001(3) 0.002(3) -0.002(3) C42 0.027(4) 0.017(4) 0.023(4) -0.002(3) -0.005(3) -0.002(3) C43 0.022(4) 0.012(3) 0.015(3) -0.001(3) 0.000(3) 0.000(3) C44 0.025(4) 0.030(4) 0.016(3) 0.000(3) 0.000(3) 0.001(3) C45 0.028(4) 0.020(4) 0.023(4) 0.000(3) -0.004(3) -0.005(3) C46 0.029(4) 0.029(4) 0.018(3) -0.003(3) 0.001(3) -0.013(3) C47 0.038(4) 0.021(4) 0.019(4) 0.012(3) -0.005(3) -0.004(3) C48 0.020(4) 0.021(4) 0.016(3) 0.002(3) -0.004(3) -0.004(3) O19 0.025(3) 0.021(3) 0.023(2) -0.006(2) 0.001(2) -0.004(2) O20 0.025(3) 0.033(3) 0.025(3) -0.001(2) -0.009(2) 0.002(2) O21 0.023(3) 0.039(3) 0.032(3) 0.001(2) 0.001(2) 0.001(2) O22 0.034(3) 0.033(3) 0.030(3) -0.002(2) -0.006(2) 0.006(2) O23 0.033(3) 0.037(3) 0.033(3) -0.004(2) -0.006(2) 0.001(2) O24 0.035(3) 0.033(3) 0.043(3) -0.005(3) -0.004(2) 0.006(2) O25 0.024(3) 0.085(5) 0.037(3) -0.023(3) -0.001(2) 0.002(3) O26 0.035(4) 0.051(4) 0.089(5) 0.005(4) -0.006(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O17 2.035(4) . ? Zn1 O16 2.059(4) . ? Zn1 O7 2.062(4) . ? Zn1 O18 2.066(5) . ? Zn1 O6 2.099(4) . ? Zn1 O8 2.210(4) . ? Zn2 O13 2.035(4) . ? Zn2 O14 2.036(5) . ? Zn2 O15 2.063(5) . ? Zn2 O1 2.108(5) . ? Zn2 O10 2.135(4) 1_455 ? Zn2 O2 2.159(4) . ? Ni1 N1 1.853(5) . ? Ni1 N2 1.859(5) . ? Ni1 N3 1.866(5) . ? Ni1 N4 1.873(5) . ? Ni2 N5 1.851(5) . ? Ni2 N6 1.865(5) . ? Ni2 N8 1.872(5) . ? Ni2 N7 1.876(5) . ? O1 C1 1.244(7) . ? O2 C2 1.246(8) . ? O3 C10 1.243(8) . ? O4 C10 1.251(8) . ? O5 C18 1.259(7) . ? O6 C18 1.261(7) . ? O7 C25 1.247(7) . ? O8 C26 1.254(7) . ? O9 C34 1.266(8) . ? O10 C34 1.237(7) . ? O10 Zn2 2.135(4) 1_655 ? O11 C42 1.253(8) . ? O12 C42 1.250(8) . ? O13 H13A 0.8501 . ? O13 H13B 0.8500 . ? O14 H14A 0.8499 . ? O14 H14B 0.8500 . ? O15 H15A 0.8500 . ? O15 H15B 0.8500 . ? O16 H16A 0.8499 . ? O16 H16B 0.8500 . ? O17 H17A 0.8500 . ? O17 H17B 0.8501 . ? O18 H18A 0.8500 . ? O18 H18B 0.8500 . ? N1 C1 1.327(8) . ? N1 C24 1.413(8) . ? N2 C2 1.337(8) . ? N2 C3 1.417(8) . ? N3 C9 1.308(8) . ? N3 C11 1.428(8) . ? N4 C17 1.296(8) . ? N4 C16 1.447(7) . ? N5 C25 1.345(8) . ? N5 C48 1.412(7) . ? N6 C26 1.340(8) . ? N6 C27 1.410(8) . ? N7 C33 1.296(8) . ? N7 C35 1.421(8) . ? N8 C41 1.315(7) . ? N8 C40 1.445(8) . ? C1 C2 1.538(9) . ? C3 C4 1.397(9) . ? C3 C8 1.417(9) . ? C4 C5 1.382(9) . ? C4 H4 0.9500 . ? C5 C6 1.399(10) . ? C5 H5 0.9500 . ? C6 C7 1.363(10) . ? C6 H6 0.9500 . ? C7 C8 1.428(9) . ? C7 H7 0.9500 . ? C8 C9 1.443(9) . ? C9 C10 1.553(9) . ? C11 C16 1.399(9) . ? C11 C12 1.400(9) . ? C12 C13 1.397(9) . ? C12 H12 0.9500 . ? C13 C14 1.374(9) . ? C13 H13 0.9500 . ? C14 C15 1.379(9) . ? C14 H14 0.9500 . ? C15 C16 1.394(9) . ? C15 H15 0.9500 . ? C17 C19 1.467(9) . ? C17 C18 1.516(9) . ? C19 C24 1.406(9) . ? C19 C20 1.416(9) . ? C20 C21 1.390(9) . ? C20 H20 0.9500 . ? C21 C22 1.387(10) . ? C21 H21 0.9500 . ? C22 C23 1.372(9) . ? C22 H22 0.9500 . ? C23 C24 1.422(9) . ? C23 H23 0.9500 . ? C25 C26 1.523(8) . ? C27 C28 1.394(9) . ? C27 C32 1.422(9) . ? C28 C29 1.396(9) . ? C28 H28 0.9500 . ? C29 C30 1.387(10) . ? C29 H29 0.9500 . ? C30 C31 1.368(10) . ? C30 H30 0.9500 . ? C31 C32 1.417(9) . ? C31 H31 0.9500 . ? C32 C33 1.463(9) . ? C33 C34 1.533(9) . ? C35 C36 1.402(9) . ? C35 C40 1.407(8) . ? C36 C37 1.375(9) . ? C36 H36 0.9500 . ? C37 C38 1.388(9) . ? C37 H37 0.9500 . ? C38 C39 1.379(9) . ? C38 H38 0.9500 . ? C39 C40 1.387(9) . ? C39 H39 0.9500 . ? C41 C43 1.464(9) . ? C41 C42 1.531(9) . ? C43 C48 1.410(9) . ? C43 C44 1.418(8) . ? C44 C45 1.355(9) . ? C44 H44 0.9500 . ? C45 C46 1.405(9) . ? C45 H45 0.9500 . ? C46 C47 1.380(9) . ? C46 H46 0.9500 . ? C47 C48 1.402(9) . ? C47 H47 0.9500 . ? O19 H19A 0.8538 . ? O19 H19B 0.8549 . ? O20 H20A 0.8815 . ? O20 H20B 0.9433 . ? O21 H21A 0.8713 . ? O21 H21B 1.0572 . ? O22 H22A 0.8510 . ? O22 H22B 0.8562 . ? O23 H23A 0.7503 . ? O23 H23B 0.7841 . ? O24 H24A 0.8493 . ? O24 H24B 0.8521 . ? O25 H25A 0.8527 . ? O25 H25B 0.8400 . ? O26 H26A 0.8790 . ? O26 H26B 0.8767 . ? 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 O17 Zn1 O16 97.31(18) . . ? O17 Zn1 O7 172.05(17) . . ? O16 Zn1 O7 90.50(17) . . ? O17 Zn1 O18 90.30(19) . . ? O16 Zn1 O18 92.45(19) . . ? O7 Zn1 O18 90.81(18) . . ? O17 Zn1 O6 90.71(17) . . ? O16 Zn1 O6 91.64(18) . . ? O7 Zn1 O6 87.61(17) . . ? O18 Zn1 O6 175.63(18) . . ? O17 Zn1 O8 93.77(16) . . ? O16 Zn1 O8 166.83(18) . . ? O7 Zn1 O8 78.29(16) . . ? O18 Zn1 O8 94.58(18) . . ? O6 Zn1 O8 81.11(17) . . ? O13 Zn2 O14 96.15(19) . . ? O13 Zn2 O15 94.9(2) . . ? O14 Zn2 O15 91.0(2) . . ? O13 Zn2 O1 89.09(18) . . ? O14 Zn2 O1 100.0(2) . . ? O15 Zn2 O1 167.92(18) . . ? O13 Zn2 O10 171.82(19) . 1_455 ? O14 Zn2 O10 87.37(17) . 1_455 ? O15 Zn2 O10 92.43(18) . 1_455 ? O1 Zn2 O10 83.03(17) . 1_455 ? O13 Zn2 O2 92.10(18) . . ? O14 Zn2 O2 171.61(16) . . ? O15 Zn2 O2 89.86(18) . . ? O1 Zn2 O2 78.57(17) . . ? O10 Zn2 O2 84.25(16) 1_455 . ? N1 Ni1 N2 86.0(2) . . ? N1 Ni1 N3 177.8(2) . . ? N2 Ni1 N3 93.5(2) . . ? N1 Ni1 N4 93.7(2) . . ? N2 Ni1 N4 178.1(2) . . ? N3 Ni1 N4 86.8(2) . . ? N5 Ni2 N6 86.4(2) . . ? N5 Ni2 N8 93.1(2) . . ? N6 Ni2 N8 176.8(2) . . ? N5 Ni2 N7 177.7(2) . . ? N6 Ni2 N7 93.9(2) . . ? N8 Ni2 N7 86.5(2) . . ? C1 O1 Zn2 113.1(4) . . ? C2 O2 Zn2 111.2(4) . . ? C18 O6 Zn1 132.3(4) . . ? C25 O7 Zn1 113.3(4) . . ? C26 O8 Zn1 108.4(4) . . ? C34 O10 Zn2 132.3(4) . 1_655 ? Zn2 O13 H13A 120.1 . . ? Zn2 O13 H13B 119.9 . . ? H13A O13 H13B 120.0 . . ? Zn2 O14 H14A 120.0 . . ? Zn2 O14 H14B 120.0 . . ? H14A O14 H14B 120.0 . . ? Zn2 O15 H15A 120.1 . . ? Zn2 O15 H15B 119.9 . . ? H15A O15 H15B 120.0 . . ? Zn1 O16 H16A 119.9 . . ? Zn1 O16 H16B 120.1 . . ? H16A O16 H16B 120.0 . . ? Zn1 O17 H17A 120.0 . . ? Zn1 O17 H17B 120.0 . . ? H17A O17 H17B 120.0 . . ? Zn1 O18 H18A 119.9 . . ? Zn1 O18 H18B 120.1 . . ? H18A O18 H18B 120.0 . . ? C1 N1 C24 122.5(6) . . ? C1 N1 Ni1 111.1(4) . . ? C24 N1 Ni1 126.4(4) . . ? C2 N2 C3 123.3(6) . . ? C2 N2 Ni1 110.0(4) . . ? C3 N2 Ni1 126.5(4) . . ? C9 N3 C11 123.5(6) . . ? C9 N3 Ni1 126.2(4) . . ? C11 N3 Ni1 110.1(4) . . ? C17 N4 C16 123.7(6) . . ? C17 N4 Ni1 126.1(4) . . ? C16 N4 Ni1 110.2(4) . . ? C25 N5 C48 122.2(5) . . ? C25 N5 Ni2 109.8(4) . . ? C48 N5 Ni2 127.6(4) . . ? C26 N6 C27 123.1(5) . . ? C26 N6 Ni2 111.1(4) . . ? C27 N6 Ni2 125.7(4) . . ? C33 N7 C35 124.3(6) . . ? C33 N7 Ni2 125.3(5) . . ? C35 N7 Ni2 110.4(4) . . ? C41 N8 C40 122.2(6) . . ? C41 N8 Ni2 127.6(5) . . ? C40 N8 Ni2 110.2(4) . . ? O1 C1 N1 130.5(6) . . ? O1 C1 C2 117.5(6) . . ? N1 C1 C2 112.0(5) . . ? O2 C2 N2 129.9(6) . . ? O2 C2 C1 118.2(6) . . ? N2 C2 C1 111.7(6) . . ? C4 C3 N2 121.1(6) . . ? C4 C3 C8 119.7(6) . . ? N2 C3 C8 118.9(6) . . ? C5 C4 C3 121.8(7) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 119.2(7) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 119.9(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 122.6(7) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C3 C8 C7 116.8(6) . . ? C3 C8 C9 125.3(6) . . ? C7 C8 C9 117.8(6) . . ? N3 C9 C8 122.8(6) . . ? N3 C9 C10 119.7(6) . . ? C8 C9 C10 117.3(6) . . ? O3 C10 O4 128.7(6) . . ? O3 C10 C9 117.8(6) . . ? O4 C10 C9 113.4(6) . . ? C16 C11 C12 120.4(6) . . ? C16 C11 N3 114.8(6) . . ? C12 C11 N3 124.4(6) . . ? C13 C12 C11 119.1(6) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 120.0(6) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 119.9(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 119.2(6) . . ? C15 C16 N4 127.5(6) . . ? C11 C16 N4 113.2(6) . . ? N4 C17 C19 123.5(6) . . ? N4 C17 C18 122.8(6) . . ? C19 C17 C18 113.7(6) . . ? O5 C18 O6 127.4(6) . . ? O5 C18 C17 118.6(5) . . ? O6 C18 C17 114.0(5) . . ? C24 C19 C20 118.8(6) . . ? C24 C19 C17 123.9(6) . . ? C20 C19 C17 117.1(6) . . ? C21 C20 C19 121.3(6) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 119.1(6) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C23 C22 C21 121.2(7) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 N1 119.1(6) . . ? C19 C24 C23 118.8(6) . . ? N1 C24 C23 121.8(6) . . ? O7 C25 N5 128.6(5) . . ? O7 C25 C26 118.9(5) . . ? N5 C25 C26 112.4(5) . . ? O8 C26 N6 130.8(6) . . ? O8 C26 C25 116.9(6) . . ? N6 C26 C25 112.1(5) . . ? C28 C27 N6 122.2(6) . . ? C28 C27 C32 118.6(6) . . ? N6 C27 C32 118.9(6) . . ? C27 C28 C29 121.1(7) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 120.1(7) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 121.4(6) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C27 118.6(6) . . ? C31 C32 C33 117.5(6) . . ? C27 C32 C33 123.8(6) . . ? N7 C33 C32 123.8(6) . . ? N7 C33 C34 123.1(6) . . ? C32 C33 C34 113.2(5) . . ? O10 C34 O9 129.2(6) . . ? O10 C34 C33 114.6(6) . . ? O9 C34 C33 116.2(5) . . ? C36 C35 C40 118.4(6) . . ? C36 C35 N7 127.0(6) . . ? C40 C35 N7 114.3(6) . . ? C37 C36 C35 120.3(6) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.6(6) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 120.3(7) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.6(6) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C35 120.8(6) . . ? C39 C40 N8 125.4(6) . . ? C35 C40 N8 113.4(6) . . ? N8 C41 C43 122.3(6) . . ? N8 C41 C42 122.3(6) . . ? C43 C41 C42 115.3(5) . . ? O12 C42 O11 127.3(6) . . ? O12 C42 C41 116.5(6) . . ? O11 C42 C41 116.1(6) . . ? C48 C43 C44 117.0(6) . . ? C48 C43 C41 124.4(5) . . ? C44 C43 C41 118.3(6) . . ? C45 C44 C43 122.6(6) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C44 C45 C46 119.5(6) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 120.1(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.3(6) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 120.4(5) . . ? C47 C48 N5 119.9(6) . . ? C43 C48 N5 119.6(6) . . ? H19A O19 H19B 115.6 . . ? H20A O20 H20B 104.1 . . ? H21A O21 H21B 132.0 . . ? H22A O22 H22B 116.8 . . ? H23A O23 H23B 130.5 . . ? H24A O24 H24B 116.8 . . ? H25A O25 H25B 119.8 . . ? H26A O26 H26B 110.7 . . ? 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 O13 Zn2 O1 C1 103.0(4) . . . . ? O14 Zn2 O1 C1 -160.9(4) . . . . ? O15 Zn2 O1 C1 -6.4(10) . . . . ? O10 Zn2 O1 C1 -74.8(4) 1_455 . . . ? O2 Zn2 O1 C1 10.7(4) . . . . ? O13 Zn2 O2 C2 -97.7(4) . . . . ? O14 Zn2 O2 C2 71.6(14) . . . . ? O15 Zn2 O2 C2 167.4(4) . . . . ? O1 Zn2 O2 C2 -9.1(4) . . . . ? O10 Zn2 O2 C2 75.0(4) 1_455 . . . ? O17 Zn1 O6 C18 -6.2(5) . . . . ? O16 Zn1 O6 C18 91.1(5) . . . . ? O7 Zn1 O6 C18 -178.5(5) . . . . ? O18 Zn1 O6 C18 -110(2) . . . . ? O8 Zn1 O6 C18 -100.0(5) . . . . ? O17 Zn1 O7 C25 -10.5(16) . . . . ? O16 Zn1 O7 C25 159.0(5) . . . . ? O18 Zn1 O7 C25 -108.5(5) . . . . ? O6 Zn1 O7 C25 67.4(5) . . . . ? O8 Zn1 O7 C25 -14.0(4) . . . . ? O17 Zn1 O8 C26 -161.3(4) . . . . ? O16 Zn1 O8 C26 -13.9(10) . . . . ? O7 Zn1 O8 C26 18.2(4) . . . . ? O18 Zn1 O8 C26 108.1(4) . . . . ? O6 Zn1 O8 C26 -71.2(4) . . . . ? N2 Ni1 N1 C1 -25.9(4) . . . . ? N3 Ni1 N1 C1 51(6) . . . . ? N4 Ni1 N1 C1 152.3(4) . . . . ? N2 Ni1 N1 C24 154.7(5) . . . . ? N3 Ni1 N1 C24 -128(6) . . . . ? N4 Ni1 N1 C24 -27.1(5) . . . . ? N1 Ni1 N2 C2 27.5(4) . . . . ? N3 Ni1 N2 C2 -150.3(4) . . . . ? N4 Ni1 N2 C2 -52(7) . . . . ? N1 Ni1 N2 C3 -157.7(5) . . . . ? N3 Ni1 N2 C3 24.5(5) . . . . ? N4 Ni1 N2 C3 123(7) . . . . ? N1 Ni1 N3 C9 -104(6) . . . . ? N2 Ni1 N3 C9 -27.5(5) . . . . ? N4 Ni1 N3 C9 154.4(5) . . . . ? N1 Ni1 N3 C11 82(6) . . . . ? N2 Ni1 N3 C11 158.4(4) . . . . ? N4 Ni1 N3 C11 -19.8(4) . . . . ? N1 Ni1 N4 C17 22.7(5) . . . . ? N2 Ni1 N4 C17 102(7) . . . . ? N3 Ni1 N4 C17 -159.5(5) . . . . ? N1 Ni1 N4 C16 -158.6(4) . . . . ? N2 Ni1 N4 C16 -79(7) . . . . ? N3 Ni1 N4 C16 19.2(4) . . . . ? N6 Ni2 N5 C25 26.5(5) . . . . ? N8 Ni2 N5 C25 -150.3(5) . . . . ? N7 Ni2 N5 C25 -71(6) . . . . ? N6 Ni2 N5 C48 -160.2(6) . . . . ? N8 Ni2 N5 C48 23.0(6) . . . . ? N7 Ni2 N5 C48 102(5) . . . . ? N5 Ni2 N6 C26 -22.3(4) . . . . ? N8 Ni2 N6 C26 59(4) . . . . ? N7 Ni2 N6 C26 155.4(4) . . . . ? N5 Ni2 N6 C27 153.9(5) . . . . ? N8 Ni2 N6 C27 -125(4) . . . . ? N7 Ni2 N6 C27 -28.4(5) . . . . ? N5 Ni2 N7 C33 123(5) . . . . ? N6 Ni2 N7 C33 25.8(5) . . . . ? N8 Ni2 N7 C33 -157.4(5) . . . . ? N5 Ni2 N7 C35 -59(6) . . . . ? N6 Ni2 N7 C35 -156.6(4) . . . . ? N8 Ni2 N7 C35 20.2(4) . . . . ? N5 Ni2 N8 C41 -22.6(6) . . . . ? N6 Ni2 N8 C41 -104(4) . . . . ? N7 Ni2 N8 C41 159.7(6) . . . . ? N5 Ni2 N8 C40 158.1(4) . . . . ? N6 Ni2 N8 C40 77(4) . . . . ? N7 Ni2 N8 C40 -19.6(4) . . . . ? Zn2 O1 C1 N1 173.0(5) . . . . ? Zn2 O1 C1 C2 -10.6(6) . . . . ? C24 N1 C1 O1 14.4(10) . . . . ? Ni1 N1 C1 O1 -165.0(5) . . . . ? C24 N1 C1 C2 -162.1(5) . . . . ? Ni1 N1 C1 C2 18.4(6) . . . . ? Zn2 O2 C2 N2 -177.6(5) . . . . ? Zn2 O2 C2 C1 6.6(6) . . . . ? C3 N2 C2 O2 -14.0(10) . . . . ? Ni1 N2 C2 O2 161.0(5) . . . . ? C3 N2 C2 C1 162.0(5) . . . . ? Ni1 N2 C2 C1 -23.0(6) . . . . ? O1 C1 C2 O2 2.6(8) . . . . ? N1 C1 C2 O2 179.7(5) . . . . ? O1 C1 C2 N2 -173.8(5) . . . . ? N1 C1 C2 N2 3.2(7) . . . . ? C2 N2 C3 C4 -23.6(8) . . . . ? Ni1 N2 C3 C4 162.2(4) . . . . ? C2 N2 C3 C8 162.4(6) . . . . ? Ni1 N2 C3 C8 -11.8(8) . . . . ? N2 C3 C4 C5 -177.2(5) . . . . ? C8 C3 C4 C5 -3.2(9) . . . . ? C3 C4 C5 C6 1.6(10) . . . . ? C4 C5 C6 C7 0.5(10) . . . . ? C5 C6 C7 C8 -1.1(11) . . . . ? C4 C3 C8 C7 2.5(9) . . . . ? N2 C3 C8 C7 176.6(5) . . . . ? C4 C3 C8 C9 178.3(6) . . . . ? N2 C3 C8 C9 -7.6(9) . . . . ? C6 C7 C8 C3 -0.4(10) . . . . ? C6 C7 C8 C9 -176.5(6) . . . . ? C11 N3 C9 C8 -169.0(5) . . . . ? Ni1 N3 C9 C8 17.6(9) . . . . ? C11 N3 C9 C10 15.7(9) . . . . ? Ni1 N3 C9 C10 -157.7(4) . . . . ? C3 C8 C9 N3 4.8(10) . . . . ? C7 C8 C9 N3 -179.5(6) . . . . ? C3 C8 C9 C10 -179.8(6) . . . . ? C7 C8 C9 C10 -4.1(9) . . . . ? N3 C9 C10 O3 -110.7(7) . . . . ? C8 C9 C10 O3 73.8(7) . . . . ? N3 C9 C10 O4 72.7(7) . . . . ? C8 C9 C10 O4 -102.8(7) . . . . ? C9 N3 C11 C16 -158.1(6) . . . . ? Ni1 N3 C11 C16 16.2(6) . . . . ? C9 N3 C11 C12 29.2(9) . . . . ? Ni1 N3 C11 C12 -156.5(5) . . . . ? C16 C11 C12 C13 5.0(9) . . . . ? N3 C11 C12 C13 177.3(6) . . . . ? C11 C12 C13 C14 -2.3(10) . . . . ? C12 C13 C14 C15 -1.6(10) . . . . ? C13 C14 C15 C16 2.8(9) . . . . ? C14 C15 C16 C11 0.0(9) . . . . ? C14 C15 C16 N4 -175.1(6) . . . . ? C12 C11 C16 C15 -3.9(9) . . . . ? N3 C11 C16 C15 -176.9(5) . . . . ? C12 C11 C16 N4 171.9(5) . . . . ? N3 C11 C16 N4 -1.0(7) . . . . ? C17 N4 C16 C15 -20.4(9) . . . . ? Ni1 N4 C16 C15 160.8(5) . . . . ? C17 N4 C16 C11 164.2(6) . . . . ? Ni1 N4 C16 C11 -14.6(6) . . . . ? C16 N4 C17 C19 175.4(5) . . . . ? Ni1 N4 C17 C19 -6.1(8) . . . . ? C16 N4 C17 C18 -4.2(9) . . . . ? Ni1 N4 C17 C18 174.4(4) . . . . ? Zn1 O6 C18 O5 6.2(10) . . . . ? Zn1 O6 C18 C17 -174.8(4) . . . . ? N4 C17 C18 O5 -79.6(7) . . . . ? C19 C17 C18 O5 100.8(7) . . . . ? N4 C17 C18 O6 101.3(7) . . . . ? C19 C17 C18 O6 -78.3(6) . . . . ? N4 C17 C19 C24 -15.9(9) . . . . ? C18 C17 C19 C24 163.7(5) . . . . ? N4 C17 C19 C20 167.9(6) . . . . ? C18 C17 C19 C20 -12.5(7) . . . . ? C24 C19 C20 C21 1.6(9) . . . . ? C17 C19 C20 C21 178.0(6) . . . . ? C19 C20 C21 C22 -2.9(10) . . . . ? C20 C21 C22 C23 1.6(10) . . . . ? C21 C22 C23 C24 1.0(9) . . . . ? C20 C19 C24 N1 -172.8(5) . . . . ? C17 C19 C24 N1 11.1(9) . . . . ? C20 C19 C24 C23 1.0(8) . . . . ? C17 C19 C24 C23 -175.1(5) . . . . ? C1 N1 C24 C19 -164.6(5) . . . . ? Ni1 N1 C24 C19 14.7(7) . . . . ? C1 N1 C24 C23 21.7(8) . . . . ? Ni1 N1 C24 C23 -158.9(4) . . . . ? C22 C23 C24 C19 -2.3(9) . . . . ? C22 C23 C24 N1 171.3(6) . . . . ? Zn1 O7 C25 N5 -174.6(6) . . . . ? Zn1 O7 C25 C26 8.7(7) . . . . ? C48 N5 C25 O7 -15.4(11) . . . . ? Ni2 N5 C25 O7 158.4(6) . . . . ? C48 N5 C25 C26 161.6(6) . . . . ? Ni2 N5 C25 C26 -24.7(7) . . . . ? Zn1 O8 C26 N6 165.4(6) . . . . ? Zn1 O8 C26 C25 -19.3(6) . . . . ? C27 N6 C26 O8 12.5(11) . . . . ? Ni2 N6 C26 O8 -171.2(6) . . . . ? C27 N6 C26 C25 -163.0(6) . . . . ? Ni2 N6 C26 C25 13.3(6) . . . . ? O7 C25 C26 O8 8.7(9) . . . . ? N5 C25 C26 O8 -168.6(6) . . . . ? O7 C25 C26 N6 -175.2(6) . . . . ? N5 C25 C26 N6 7.6(8) . . . . ? C26 N6 C27 C28 15.6(9) . . . . ? Ni2 N6 C27 C28 -160.1(5) . . . . ? C26 N6 C27 C32 -170.8(6) . . . . ? Ni2 N6 C27 C32 13.5(8) . . . . ? N6 C27 C28 C29 167.6(6) . . . . ? C32 C27 C28 C29 -6.1(10) . . . . ? C27 C28 C29 C30 3.2(10) . . . . ? C28 C29 C30 C31 2.0(10) . . . . ? C29 C30 C31 C32 -4.0(10) . . . . ? C30 C31 C32 C27 1.0(9) . . . . ? C30 C31 C32 C33 177.5(6) . . . . ? C28 C27 C32 C31 4.0(9) . . . . ? N6 C27 C32 C31 -169.9(6) . . . . ? C28 C27 C32 C33 -172.3(6) . . . . ? N6 C27 C32 C33 13.8(9) . . . . ? C35 N7 C33 C32 174.3(6) . . . . ? Ni2 N7 C33 C32 -8.3(9) . . . . ? C35 N7 C33 C34 -3.6(10) . . . . ? Ni2 N7 C33 C34 173.8(4) . . . . ? C31 C32 C33 N7 166.7(6) . . . . ? C27 C32 C33 N7 -17.0(10) . . . . ? C31 C32 C33 C34 -15.2(8) . . . . ? C27 C32 C33 C34 161.1(6) . . . . ? Zn2 O10 C34 O9 -6.0(11) 1_655 . . . ? Zn2 O10 C34 C33 172.5(4) 1_655 . . . ? N7 C33 C34 O10 100.7(7) . . . . ? C32 C33 C34 O10 -77.4(7) . . . . ? N7 C33 C34 O9 -80.6(8) . . . . ? C32 C33 C34 O9 101.3(7) . . . . ? C33 N7 C35 C36 -24.8(10) . . . . ? Ni2 N7 C35 C36 157.5(6) . . . . ? C33 N7 C35 C40 161.2(6) . . . . ? Ni2 N7 C35 C40 -16.5(7) . . . . ? C40 C35 C36 C37 -2.7(10) . . . . ? N7 C35 C36 C37 -176.5(6) . . . . ? C35 C36 C37 C38 3.2(11) . . . . ? C36 C37 C38 C39 -0.1(11) . . . . ? C37 C38 C39 C40 -3.3(11) . . . . ? C38 C39 C40 C35 3.7(10) . . . . ? C38 C39 C40 N8 175.7(6) . . . . ? C36 C35 C40 C39 -0.7(10) . . . . ? N7 C35 C40 C39 173.9(6) . . . . ? C36 C35 C40 N8 -173.6(6) . . . . ? N7 C35 C40 N8 1.0(8) . . . . ? C41 N8 C40 C39 23.2(10) . . . . ? Ni2 N8 C40 C39 -157.5(6) . . . . ? C41 N8 C40 C35 -164.3(6) . . . . ? Ni2 N8 C40 C35 15.0(7) . . . . ? C40 N8 C41 C43 -169.8(6) . . . . ? Ni2 N8 C41 C43 11.0(9) . . . . ? C40 N8 C41 C42 13.3(9) . . . . ? Ni2 N8 C41 C42 -165.9(5) . . . . ? N8 C41 C42 O12 -115.0(7) . . . . ? C43 C41 C42 O12 67.9(8) . . . . ? N8 C41 C42 O11 68.9(9) . . . . ? C43 C41 C42 O11 -108.1(7) . . . . ? N8 C41 C43 C48 8.9(10) . . . . ? C42 C41 C43 C48 -174.0(6) . . . . ? N8 C41 C43 C44 -176.7(6) . . . . ? C42 C41 C43 C44 0.4(9) . . . . ? C48 C43 C44 C45 2.0(10) . . . . ? C41 C43 C44 C45 -172.8(7) . . . . ? C43 C44 C45 C46 -3.5(11) . . . . ? C44 C45 C46 C47 2.1(11) . . . . ? C45 C46 C47 C48 0.8(11) . . . . ? C46 C47 C48 C43 -2.3(11) . . . . ? C46 C47 C48 N5 -178.6(6) . . . . ? C44 C43 C48 C47 0.9(10) . . . . ? C41 C43 C48 C47 175.4(7) . . . . ? C44 C43 C48 N5 177.2(6) . . . . ? C41 C43 C48 N5 -8.3(10) . . . . ? C25 N5 C48 C47 -23.0(10) . . . . ? Ni2 N5 C48 C47 164.4(5) . . . . ? C25 N5 C48 C43 160.6(6) . . . . ? Ni2 N5 C48 C43 -12.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.072 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.150 # Attachment 'compound 5.cif' data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 839543' #TrackingRef 'compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Cd N6 Ni O10' _chemical_formula_weight 805.71 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1075(17) _cell_length_b 14.004(2) _cell_length_c 19.542(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.756(3) _cell_angle_gamma 90.00 _cell_volume 3036.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10695 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 0.8509 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28616 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7248 _reflns_number_gt 6074 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; The following distance restraints were applied to the water molecules: DFIX 1.45 0.01 H7A H7B H8A H8B DFIX 0.85 0.01 O7 H7A O7 H7B O8 H8A O8 H8B Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7248 _refine_ls_number_parameters 453 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.005 _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 Cd1 Cd 0.667040(10) 0.213220(8) 0.019689(6) 0.01072(4) Uani 1 1 d . . . Ni1 Ni 0.648938(18) 0.286602(13) 0.294896(10) 0.00874(5) Uani 1 1 d . . . O1 O 0.54166(11) 0.22242(7) 0.11024(6) 0.0138(2) Uani 1 1 d . . . O2 O 0.77947(11) 0.27815(8) 0.11564(6) 0.0139(2) Uani 1 1 d . . . O3 O 0.31037(11) 0.12215(8) 0.41210(6) 0.0153(2) Uani 1 1 d . . . O4 O 0.33314(10) 0.27051(8) 0.45648(6) 0.0132(2) Uani 1 1 d . . . O5 O 0.91840(11) 0.40471(8) 0.47883(6) 0.0175(3) Uani 1 1 d . . . O6 O 1.04841(10) 0.31331(8) 0.42420(6) 0.0153(2) Uani 1 1 d . . . O7 O 0.71846(12) 0.06329(9) 0.04668(8) 0.0265(3) Uani 1 1 d D . . O8 O 0.61507(11) 0.36830(8) -0.00544(6) 0.0173(3) Uani 1 1 d D . . N1 N 0.53519(12) 0.27210(9) 0.22351(7) 0.0098(3) Uani 1 1 d . . . N2 N 0.54855(12) 0.23703(9) 0.36084(7) 0.0097(3) Uani 1 1 d . . . N3 N 0.76889(12) 0.29269(8) 0.36497(7) 0.0106(3) Uani 1 1 d . . . N4 N 0.75171(12) 0.32685(9) 0.22806(6) 0.0106(3) Uani 1 1 d . . . C1 C 0.58728(14) 0.25544(11) 0.16421(8) 0.0109(3) Uani 1 1 d . . . C2 C 0.71925(15) 0.28725(10) 0.16742(8) 0.0108(3) Uani 1 1 d . . . C3 C 0.41003(14) 0.27489(10) 0.22915(8) 0.0103(3) Uani 1 1 d . . . C4 C 0.33327(15) 0.29562(11) 0.17241(9) 0.0144(3) Uani 1 1 d . . . H4 H 0.3646 0.3003 0.1293 0.017 Uiso 1 1 calc R . . C5 C 0.21152(15) 0.30919(12) 0.17956(9) 0.0161(3) Uani 1 1 d . . . H5 H 0.1618 0.3248 0.1415 0.019 Uiso 1 1 calc R . . C6 C 0.16298(16) 0.29965(11) 0.24343(9) 0.0172(4) Uani 1 1 d . . . H6 H 0.0808 0.3087 0.2481 0.021 Uiso 1 1 calc R . . C7 C 0.23561(15) 0.27698(11) 0.29935(9) 0.0139(3) Uani 1 1 d . . . H7 H 0.2017 0.2698 0.3416 0.017 Uiso 1 1 calc R . . C8 C 0.36132(14) 0.26408(11) 0.29453(8) 0.0103(3) Uani 1 1 d . . . C9 C 0.43116(15) 0.23524(10) 0.35604(8) 0.0098(3) Uani 1 1 d . . . C10 C 0.35196(14) 0.20465(11) 0.41445(8) 0.0113(3) Uani 1 1 d . . . C11 C 0.62077(15) 0.19804(10) 0.41665(8) 0.0103(3) Uani 1 1 d . . . C12 C 0.58486(15) 0.12912(11) 0.46324(8) 0.0135(3) Uani 1 1 d . . . H12 H 0.5043 0.1112 0.4641 0.016 Uiso 1 1 calc R . . C13 C 0.66985(15) 0.08767(11) 0.50815(8) 0.0146(3) Uani 1 1 d . . . H13 H 0.6457 0.0422 0.5394 0.018 Uiso 1 1 calc R . . C14 C 0.78986(15) 0.11292(11) 0.50713(8) 0.0144(3) Uani 1 1 d . . . H14 H 0.8461 0.0834 0.5369 0.017 Uiso 1 1 calc R . . C15 C 0.82706(15) 0.18230(11) 0.46188(8) 0.0131(3) Uani 1 1 d . . . H15 H 0.9079 0.1993 0.4611 0.016 Uiso 1 1 calc R . . C16 C 0.74168(15) 0.22604(10) 0.41780(8) 0.0112(3) Uani 1 1 d . . . C17 C 0.86244(14) 0.34880(11) 0.36684(8) 0.0108(3) Uani 1 1 d . . . C18 C 0.94986(15) 0.35664(11) 0.42984(8) 0.0117(3) Uani 1 1 d . . . C19 C 0.89451(14) 0.40623(11) 0.30751(8) 0.0109(3) Uani 1 1 d . . . C20 C 0.98175(15) 0.47809(11) 0.31857(9) 0.0142(3) Uani 1 1 d . . . H20 H 1.0079 0.4933 0.3632 0.017 Uiso 1 1 calc R . . C21 C 1.02933(15) 0.52651(11) 0.26471(9) 0.0168(4) Uani 1 1 d . . . H21 H 1.0851 0.5752 0.2729 0.020 Uiso 1 1 calc R . . C22 C 0.99317(15) 0.50187(11) 0.19815(9) 0.0161(4) Uani 1 1 d . . . H22 H 1.0286 0.5318 0.1617 0.019 Uiso 1 1 calc R . . C23 C 0.90543(14) 0.43360(11) 0.18522(8) 0.0138(3) Uani 1 1 d . . . H23 H 0.8817 0.4185 0.1402 0.017 Uiso 1 1 calc R . . C24 C 0.85140(14) 0.38649(11) 0.23962(8) 0.0110(3) Uani 1 1 d . . . O9 O 0.95881(12) -0.03994(9) 0.39417(7) 0.0271(3) Uani 1 1 d . . . O10 O -0.07989(13) -0.03256(10) 0.08101(9) 0.0408(4) Uani 1 1 d . . . N5 N 0.94676(15) 0.04474(10) 0.29509(8) 0.0238(4) Uani 1 1 d . . . N6 N 0.09229(14) 0.05648(11) 0.08966(7) 0.0225(3) Uani 1 1 d . . . C25 C 0.90219(17) 0.00646(12) 0.35075(10) 0.0223(4) Uani 1 1 d . . . H25 H 0.8206 0.0159 0.3571 0.027 Uiso 1 1 calc R . . C26 C 1.07411(19) 0.03482(15) 0.28243(11) 0.0344(5) Uani 1 1 d . . . H26A H 1.1175 0.0170 0.3241 0.052 Uiso 1 1 calc R . . H26B H 1.1046 0.0945 0.2664 0.052 Uiso 1 1 calc R . . H26C H 1.0843 -0.0136 0.2484 0.052 Uiso 1 1 calc R . . C27 C 0.8702(2) 0.09066(17) 0.24312(12) 0.0438(6) Uani 1 1 d . . . H27A H 0.7896 0.0951 0.2586 0.066 Uiso 1 1 calc R . . H27B H 0.8696 0.0538 0.2017 0.066 Uiso 1 1 calc R . . H27C H 0.9003 0.1536 0.2345 0.066 Uiso 1 1 calc R . . C28 C 0.02977(19) -0.02401(14) 0.09076(10) 0.0286(4) Uani 1 1 d . . . H28 H 0.0732 -0.0797 0.0998 0.034 Uiso 1 1 calc R . . C29 C 0.22073(18) 0.05791(15) 0.10496(11) 0.0339(5) Uani 1 1 d . . . H29A H 0.2497 -0.0063 0.1107 0.051 Uiso 1 1 calc R . . H29B H 0.2376 0.0933 0.1464 0.051 Uiso 1 1 calc R . . H29C H 0.2603 0.0878 0.0679 0.051 Uiso 1 1 calc R . . C30 C 0.0334(2) 0.14642(14) 0.07207(12) 0.0372(5) Uani 1 1 d . . . H30A H -0.0383 0.1343 0.0440 0.056 Uiso 1 1 calc R . . H30B H 0.0872 0.1858 0.0474 0.056 Uiso 1 1 calc R . . H30C H 0.0124 0.1786 0.1132 0.056 Uiso 1 1 calc R . . H7A H 0.7888(10) 0.0409(15) 0.0580(12) 0.062(9) Uiso 1 1 d D . . H7B H 0.6657(14) 0.0198(12) 0.0384(11) 0.050(8) Uiso 1 1 d D . . H8A H 0.6718(14) 0.3882(12) -0.0297(8) 0.030(6) Uiso 1 1 d D . . H8B H 0.5967(18) 0.4041(13) 0.0271(8) 0.043(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.00985(7) 0.01436(7) 0.00809(7) -0.00036(4) 0.00180(5) -0.00009(4) Ni1 0.00701(10) 0.01277(10) 0.00646(11) 0.00100(7) 0.00061(8) -0.00070(7) O1 0.0114(6) 0.0212(6) 0.0091(6) -0.0032(4) 0.0020(5) -0.0020(5) O2 0.0113(6) 0.0224(6) 0.0084(6) -0.0022(4) 0.0033(5) -0.0014(5) O3 0.0142(6) 0.0138(6) 0.0183(6) 0.0004(5) 0.0039(5) -0.0014(5) O4 0.0116(6) 0.0174(6) 0.0108(6) -0.0021(4) 0.0026(5) -0.0008(4) O5 0.0201(7) 0.0189(6) 0.0134(6) -0.0031(5) -0.0008(5) 0.0020(5) O6 0.0101(6) 0.0212(6) 0.0146(6) 0.0028(5) -0.0004(5) 0.0017(5) O7 0.0164(7) 0.0170(6) 0.0453(9) 0.0065(6) -0.0062(6) -0.0027(5) O8 0.0172(7) 0.0170(6) 0.0182(7) -0.0007(5) 0.0061(5) 0.0008(5) N1 0.0071(6) 0.0149(7) 0.0076(7) 0.0010(5) 0.0016(5) 0.0005(5) N2 0.0104(7) 0.0102(6) 0.0085(7) 0.0001(5) 0.0002(5) 0.0008(5) N3 0.0110(7) 0.0122(6) 0.0088(7) 0.0009(5) 0.0015(5) 0.0009(5) N4 0.0090(7) 0.0143(6) 0.0086(7) 0.0012(5) 0.0009(5) -0.0007(5) C1 0.0099(8) 0.0121(7) 0.0106(8) 0.0017(6) 0.0019(6) 0.0003(6) C2 0.0089(8) 0.0124(7) 0.0111(8) 0.0023(6) 0.0003(6) 0.0015(6) C3 0.0081(8) 0.0112(7) 0.0118(8) -0.0008(6) 0.0009(6) 0.0003(6) C4 0.0124(8) 0.0204(8) 0.0105(8) 0.0020(6) 0.0011(6) 0.0006(6) C5 0.0114(8) 0.0222(8) 0.0145(9) 0.0025(7) -0.0027(7) 0.0035(7) C6 0.0093(8) 0.0227(9) 0.0198(9) -0.0001(7) 0.0024(7) 0.0037(6) C7 0.0107(8) 0.0188(8) 0.0125(8) 0.0000(6) 0.0035(7) 0.0012(6) C8 0.0093(8) 0.0107(7) 0.0109(8) 0.0006(6) 0.0008(6) 0.0007(6) C9 0.0116(8) 0.0075(7) 0.0105(8) -0.0028(6) 0.0028(6) 0.0003(6) C10 0.0078(8) 0.0162(8) 0.0098(8) 0.0025(6) 0.0006(6) 0.0018(6) C11 0.0125(8) 0.0121(7) 0.0061(8) -0.0007(6) 0.0001(6) 0.0026(6) C12 0.0124(8) 0.0151(8) 0.0131(8) -0.0007(6) 0.0014(6) -0.0024(6) C13 0.0197(9) 0.0133(8) 0.0110(8) 0.0027(6) 0.0013(7) -0.0019(6) C14 0.0180(9) 0.0139(8) 0.0109(8) 0.0015(6) -0.0044(7) 0.0020(6) C15 0.0116(8) 0.0149(7) 0.0126(8) -0.0005(6) -0.0011(6) -0.0007(6) C16 0.0133(8) 0.0117(7) 0.0086(8) -0.0004(6) 0.0020(6) 0.0001(6) C17 0.0101(8) 0.0117(7) 0.0104(8) -0.0016(6) 0.0008(6) 0.0018(6) C18 0.0128(8) 0.0118(7) 0.0107(8) 0.0032(6) 0.0013(6) -0.0030(6) C19 0.0098(8) 0.0111(7) 0.0120(8) 0.0015(6) 0.0018(6) 0.0009(6) C20 0.0147(8) 0.0129(8) 0.0148(9) -0.0008(6) -0.0020(7) -0.0003(6) C21 0.0147(9) 0.0139(8) 0.0216(9) 0.0029(7) -0.0011(7) -0.0042(6) C22 0.0144(9) 0.0169(8) 0.0170(9) 0.0069(7) 0.0012(7) -0.0010(7) C23 0.0111(8) 0.0169(8) 0.0133(8) 0.0021(6) 0.0006(6) 0.0004(6) C24 0.0090(8) 0.0109(7) 0.0130(8) 0.0005(6) 0.0001(6) 0.0012(6) O9 0.0304(8) 0.0281(7) 0.0229(7) 0.0052(6) 0.0034(6) 0.0003(6) O10 0.0229(8) 0.0268(8) 0.0714(12) 0.0038(7) -0.0107(8) 0.0012(6) N5 0.0294(9) 0.0193(8) 0.0228(9) 0.0053(6) 0.0019(7) 0.0014(7) N6 0.0244(9) 0.0211(8) 0.0215(8) 0.0036(6) -0.0037(7) 0.0026(6) C25 0.0235(10) 0.0168(8) 0.0268(11) -0.0050(8) 0.0020(8) -0.0022(7) C26 0.0358(13) 0.0310(11) 0.0373(13) 0.0119(9) 0.0128(10) 0.0022(9) C27 0.0485(15) 0.0441(13) 0.0387(14) 0.0144(11) 0.0011(11) 0.0165(11) C28 0.0297(12) 0.0218(9) 0.0339(12) 0.0024(8) -0.0044(9) 0.0056(8) C29 0.0222(11) 0.0386(12) 0.0411(13) -0.0036(10) 0.0029(9) 0.0010(9) C30 0.0380(13) 0.0229(10) 0.0487(14) 0.0095(9) -0.0173(11) -0.0007(9) _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 Cd1 O7 2.2325(13) . ? Cd1 O6 2.2626(12) 4_565 ? Cd1 O4 2.2805(11) 4_665 ? Cd1 O8 2.2943(12) . ? Cd1 O1 2.3075(11) . ? Cd1 O2 2.3826(12) . ? Ni1 N1 1.8478(14) . ? Ni1 N4 1.8628(12) . ? Ni1 N3 1.8661(14) . ? Ni1 N2 1.8773(13) . ? O1 C1 1.2376(19) . ? O2 C2 1.2462(19) . ? O3 C10 1.2443(18) . ? O4 C10 1.2591(19) . ? O4 Cd1 2.2806(11) 4_566 ? O5 C18 1.2344(19) . ? O6 C18 1.2611(19) . ? O6 Cd1 2.2628(12) 4_666 ? O7 H7A 0.861(9) . ? O7 H7B 0.854(9) . ? O8 H8A 0.853(9) . ? O8 H8B 0.843(9) . ? N1 C1 1.3403(19) . ? N1 C3 1.400(2) . ? N2 C9 1.303(2) . ? N2 C11 1.431(2) . ? N3 C17 1.302(2) . ? N3 C16 1.435(2) . ? N4 C2 1.342(2) . ? N4 C24 1.397(2) . ? C1 C2 1.530(2) . ? C3 C4 1.396(2) . ? C3 C8 1.419(2) . ? C4 C5 1.379(2) . ? C4 H4 0.9300 . ? C5 C6 1.390(2) . ? C5 H5 0.9300 . ? C6 C7 1.364(2) . ? C6 H6 0.9300 . ? C7 C8 1.416(2) . ? C7 H7 0.9300 . ? C8 C9 1.456(2) . ? C9 C10 1.535(2) . ? C11 C12 1.398(2) . ? C11 C16 1.398(2) . ? C12 C13 1.385(2) . ? C12 H12 0.9300 . ? C13 C14 1.380(2) . ? C13 H13 0.9300 . ? C14 C15 1.390(2) . ? C14 H14 0.9300 . ? C15 C16 1.392(2) . ? C15 H15 0.9300 . ? C17 C19 1.469(2) . ? C17 C18 1.535(2) . ? C19 C20 1.407(2) . ? C19 C24 1.416(2) . ? C20 C21 1.379(2) . ? C20 H20 0.9300 . ? C21 C22 1.386(2) . ? C21 H21 0.9300 . ? C22 C23 1.380(2) . ? C22 H22 0.9300 . ? C23 C24 1.409(2) . ? C23 H23 0.9300 . ? O9 C25 1.219(2) . ? O10 C28 1.230(2) . ? N5 C25 1.329(2) . ? N5 C27 1.444(3) . ? N5 C26 1.454(2) . ? N6 C28 1.325(2) . ? N6 C29 1.444(2) . ? N6 C30 1.453(2) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cd1 O6 99.94(5) . 4_565 ? O7 Cd1 O4 91.00(5) . 4_665 ? O6 Cd1 O4 91.37(4) 4_565 4_665 ? O7 Cd1 O8 178.67(5) . . ? O6 Cd1 O8 81.28(4) 4_565 . ? O4 Cd1 O8 89.50(4) 4_665 . ? O7 Cd1 O1 91.62(5) . . ? O6 Cd1 O1 107.01(4) 4_565 . ? O4 Cd1 O1 160.67(4) 4_665 . ? O8 Cd1 O1 87.50(4) . . ? O7 Cd1 O2 93.12(5) . . ? O6 Cd1 O2 166.92(4) 4_565 . ? O4 Cd1 O2 88.91(4) 4_665 . ? O8 Cd1 O2 85.65(4) . . ? O1 Cd1 O2 71.82(4) . . ? N1 Ni1 N4 85.63(6) . . ? N1 Ni1 N3 175.73(6) . . ? N4 Ni1 N3 93.48(6) . . ? N1 Ni1 N2 94.04(6) . . ? N4 Ni1 N2 175.90(6) . . ? N3 Ni1 N2 86.55(6) . . ? C1 O1 Cd1 115.91(10) . . ? C2 O2 Cd1 113.37(10) . . ? C10 O4 Cd1 126.19(10) . 4_566 ? C18 O6 Cd1 118.71(10) . 4_666 ? Cd1 O7 H7A 128.5(15) . . ? Cd1 O7 H7B 117.4(14) . . ? H7A O7 H7B 113.2(14) . . ? Cd1 O8 H8A 104.0(13) . . ? Cd1 O8 H8B 117.9(15) . . ? H8A O8 H8B 116.0(14) . . ? C1 N1 C3 122.98(14) . . ? C1 N1 Ni1 111.34(11) . . ? C3 N1 Ni1 125.65(10) . . ? C9 N2 C11 124.76(13) . . ? C9 N2 Ni1 125.66(11) . . ? C11 N2 Ni1 109.55(10) . . ? C17 N3 C16 124.61(14) . . ? C17 N3 Ni1 126.08(11) . . ? C16 N3 Ni1 109.31(10) . . ? C2 N4 C24 124.56(13) . . ? C2 N4 Ni1 110.27(10) . . ? C24 N4 Ni1 125.13(11) . . ? O1 C1 N1 128.74(15) . . ? O1 C1 C2 119.72(13) . . ? N1 C1 C2 111.49(14) . . ? O2 C2 N4 128.86(15) . . ? O2 C2 C1 119.17(14) . . ? N4 C2 C1 111.88(13) . . ? C4 C3 N1 120.92(14) . . ? C4 C3 C8 119.50(14) . . ? N1 C3 C8 119.39(14) . . ? C5 C4 C3 120.82(15) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.15(16) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.12(16) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 121.58(15) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C3 117.78(15) . . ? C7 C8 C9 117.95(14) . . ? C3 C8 C9 124.17(14) . . ? N2 C9 C8 123.08(14) . . ? N2 C9 C10 123.99(14) . . ? C8 C9 C10 112.92(14) . . ? O3 C10 O4 129.14(15) . . ? O3 C10 C9 117.17(13) . . ? O4 C10 C9 113.55(13) . . ? C12 C11 C16 119.15(15) . . ? C12 C11 N2 126.36(15) . . ? C16 C11 N2 114.09(13) . . ? C13 C12 C11 119.66(15) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.85(15) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.34(16) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.13(15) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C11 120.78(14) . . ? C15 C16 N3 124.80(15) . . ? C11 C16 N3 113.97(14) . . ? N3 C17 C19 122.14(15) . . ? N3 C17 C18 122.61(14) . . ? C19 C17 C18 115.20(13) . . ? O5 C18 O6 127.55(16) . . ? O5 C18 C17 117.99(14) . . ? O6 C18 C17 114.44(13) . . ? C20 C19 C24 118.90(14) . . ? C20 C19 C17 117.51(14) . . ? C24 C19 C17 123.28(14) . . ? C21 C20 C19 121.40(16) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.31(15) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.96(15) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.59(16) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? N4 C24 C23 121.40(15) . . ? N4 C24 C19 119.87(13) . . ? C23 C24 C19 118.56(15) . . ? C25 N5 C27 121.66(17) . . ? C25 N5 C26 120.28(16) . . ? C27 N5 C26 117.90(16) . . ? C28 N6 C29 121.48(16) . . ? C28 N6 C30 120.74(17) . . ? C29 N6 C30 117.78(16) . . ? O9 C25 N5 125.76(18) . . ? O9 C25 H25 117.1 . . ? N5 C25 H25 117.1 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 N6 126.62(18) . . ? O10 C28 H28 116.7 . . ? N6 C28 H28 116.7 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 O7 Cd1 O1 C1 93.06(11) . . . . ? O6 Cd1 O1 C1 -166.03(11) 4_565 . . . ? O4 Cd1 O1 C1 -4.62(19) 4_665 . . . ? O8 Cd1 O1 C1 -85.94(11) . . . . ? O2 Cd1 O1 C1 0.30(11) . . . . ? O7 Cd1 O2 C2 -91.50(10) . . . . ? O6 Cd1 O2 C2 86.2(2) 4_565 . . . ? O4 Cd1 O2 C2 177.56(10) 4_665 . . . ? O8 Cd1 O2 C2 87.98(10) . . . . ? O1 Cd1 O2 C2 -0.81(10) . . . . ? N4 Ni1 N1 C1 26.62(11) . . . . ? N3 Ni1 N1 C1 -51.5(8) . . . . ? N2 Ni1 N1 C1 -149.29(11) . . . . ? N4 Ni1 N1 C3 -155.17(12) . . . . ? N3 Ni1 N1 C3 126.8(7) . . . . ? N2 Ni1 N1 C3 28.92(12) . . . . ? N1 Ni1 N2 C9 -23.51(13) . . . . ? N4 Ni1 N2 C9 -108.7(8) . . . . ? N3 Ni1 N2 C9 160.72(13) . . . . ? N1 Ni1 N2 C11 154.43(10) . . . . ? N4 Ni1 N2 C11 69.2(9) . . . . ? N3 Ni1 N2 C11 -21.34(10) . . . . ? N1 Ni1 N3 C17 105.5(7) . . . . ? N4 Ni1 N3 C17 27.75(13) . . . . ? N2 Ni1 N3 C17 -156.36(13) . . . . ? N1 Ni1 N3 C16 -75.1(8) . . . . ? N4 Ni1 N3 C16 -152.91(10) . . . . ? N2 Ni1 N3 C16 22.98(10) . . . . ? N1 Ni1 N4 C2 -27.37(11) . . . . ? N3 Ni1 N4 C2 148.45(11) . . . . ? N2 Ni1 N4 C2 58.1(9) . . . . ? N1 Ni1 N4 C24 155.10(13) . . . . ? N3 Ni1 N4 C24 -29.08(13) . . . . ? N2 Ni1 N4 C24 -119.4(8) . . . . ? Cd1 O1 C1 N1 177.33(13) . . . . ? Cd1 O1 C1 C2 0.16(18) . . . . ? C3 N1 C1 O1 -15.5(3) . . . . ? Ni1 N1 C1 O1 162.75(14) . . . . ? C3 N1 C1 C2 161.86(13) . . . . ? Ni1 N1 C1 C2 -19.88(15) . . . . ? Cd1 O2 C2 N4 -175.14(13) . . . . ? Cd1 O2 C2 C1 1.18(17) . . . . ? C24 N4 C2 O2 16.2(3) . . . . ? Ni1 N4 C2 O2 -161.34(14) . . . . ? C24 N4 C2 C1 -160.34(14) . . . . ? Ni1 N4 C2 C1 22.11(15) . . . . ? O1 C1 C2 O2 -1.0(2) . . . . ? N1 C1 C2 O2 -178.61(13) . . . . ? O1 C1 C2 N4 175.94(14) . . . . ? N1 C1 C2 N4 -1.69(18) . . . . ? C1 N1 C3 C4 -24.0(2) . . . . ? Ni1 N1 C3 C4 158.02(12) . . . . ? C1 N1 C3 C8 161.13(14) . . . . ? Ni1 N1 C3 C8 -16.88(19) . . . . ? N1 C3 C4 C5 -172.47(14) . . . . ? C8 C3 C4 C5 2.4(2) . . . . ? C3 C4 C5 C6 -1.9(2) . . . . ? C4 C5 C6 C7 0.1(3) . . . . ? C5 C6 C7 C8 1.0(2) . . . . ? C6 C7 C8 C3 -0.4(2) . . . . ? C6 C7 C8 C9 -176.94(15) . . . . ? C4 C3 C8 C7 -1.3(2) . . . . ? N1 C3 C8 C7 173.69(13) . . . . ? C4 C3 C8 C9 175.01(14) . . . . ? N1 C3 C8 C9 -10.0(2) . . . . ? C11 N2 C9 C8 -171.54(14) . . . . ? Ni1 N2 C9 C8 6.1(2) . . . . ? C11 N2 C9 C10 9.7(2) . . . . ? Ni1 N2 C9 C10 -172.69(10) . . . . ? C7 C8 C9 N2 -167.92(14) . . . . ? C3 C8 C9 N2 15.8(2) . . . . ? C7 C8 C9 C10 10.98(19) . . . . ? C3 C8 C9 C10 -165.31(14) . . . . ? Cd1 O4 C10 O3 -24.7(3) 4_566 . . . ? Cd1 O4 C10 C9 150.89(10) 4_566 . . . ? N2 C9 C10 O3 -100.44(19) . . . . ? C8 C9 C10 O3 80.67(18) . . . . ? N2 C9 C10 O4 83.38(19) . . . . ? C8 C9 C10 O4 -95.51(17) . . . . ? C9 N2 C11 C12 20.4(2) . . . . ? Ni1 N2 C11 C12 -157.57(13) . . . . ? C9 N2 C11 C16 -167.04(14) . . . . ? Ni1 N2 C11 C16 15.00(16) . . . . ? C16 C11 C12 C13 -2.0(2) . . . . ? N2 C11 C12 C13 170.20(14) . . . . ? C11 C12 C13 C14 -0.5(2) . . . . ? C12 C13 C14 C15 1.5(2) . . . . ? C13 C14 C15 C16 0.2(2) . . . . ? C14 C15 C16 C11 -2.8(2) . . . . ? C14 C15 C16 N3 -174.63(14) . . . . ? C12 C11 C16 C15 3.7(2) . . . . ? N2 C11 C16 C15 -169.45(14) . . . . ? C12 C11 C16 N3 176.39(13) . . . . ? N2 C11 C16 N3 3.24(19) . . . . ? C17 N3 C16 C15 -28.3(2) . . . . ? Ni1 N3 C16 C15 152.33(13) . . . . ? C17 N3 C16 C11 159.34(14) . . . . ? Ni1 N3 C16 C11 -20.01(15) . . . . ? C16 N3 C17 C19 171.63(14) . . . . ? Ni1 N3 C17 C19 -9.1(2) . . . . ? C16 N3 C17 C18 -5.8(2) . . . . ? Ni1 N3 C17 C18 173.47(10) . . . . ? Cd1 O6 C18 O5 16.3(2) 4_666 . . . ? Cd1 O6 C18 C17 -165.17(9) 4_666 . . . ? N3 C17 C18 O5 -77.78(19) . . . . ? C19 C17 C18 O5 104.66(16) . . . . ? N3 C17 C18 O6 103.51(17) . . . . ? C19 C17 C18 O6 -74.06(17) . . . . ? N3 C17 C19 C20 167.60(15) . . . . ? C18 C17 C19 C20 -14.8(2) . . . . ? N3 C17 C19 C24 -19.0(2) . . . . ? C18 C17 C19 C24 158.61(14) . . . . ? C24 C19 C20 C21 -2.7(2) . . . . ? C17 C19 C20 C21 171.01(15) . . . . ? C19 C20 C21 C22 -2.0(2) . . . . ? C20 C21 C22 C23 3.8(2) . . . . ? C21 C22 C23 C24 -0.7(2) . . . . ? C2 N4 C24 C23 19.7(2) . . . . ? Ni1 N4 C24 C23 -163.14(11) . . . . ? C2 N4 C24 C19 -165.07(14) . . . . ? Ni1 N4 C24 C19 12.1(2) . . . . ? C22 C23 C24 N4 171.30(15) . . . . ? C22 C23 C24 C19 -4.0(2) . . . . ? C20 C19 C24 N4 -169.74(14) . . . . ? C17 C19 C24 N4 16.9(2) . . . . ? C20 C19 C24 C23 5.7(2) . . . . ? C17 C19 C24 C23 -167.70(14) . . . . ? C27 N5 C25 O9 173.86(19) . . . . ? C26 N5 C25 O9 -1.4(3) . . . . ? C29 N6 C28 O10 177.2(2) . . . . ? C30 N6 C28 O10 -3.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.443 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.074 # Attachment 'compound 6.cif' data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 839544' #TrackingRef 'compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H38 Cd2 N8 Ni2 O15' _chemical_formula_weight 1357.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.3958(17) _cell_length_b 18.9334(17) _cell_length_c 22.595(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.522(3) _cell_angle_gamma 90.00 _cell_volume 4843.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7563 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.77 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7592 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11760 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4269 _reflns_number_gt 3611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 1. 'Isor 0.01' commands were used to restraint the ADPs of C26 and O5: isor 0.01 C26 O5 2. The restraints (dfix) are applied to keep the bond geometries and dsps of ethanol molecule structurally reasonable The following distance restraints were applied to the ethanol molecule: dfix 1.45 0.01 O7 C25 dfix 1.53 0.01 C25 C26 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+52.5594P] 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 4269 _refine_ls_number_parameters 358 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.130 _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 Cd1 Cd 0.45143(4) 1.11268(2) 0.62137(3) 0.0640(2) Uani 1 1 d . . . Ni1 Ni 0.38763(6) 0.73906(3) 0.63730(3) 0.03294(17) Uani 1 1 d . . . O1 O 0.3894(3) 1.00331(18) 0.63119(19) 0.0451(10) Uani 1 1 d . . . O2 O 0.5133(3) 0.9702(2) 0.56683(19) 0.0466(10) Uani 1 1 d . . . O3 O 0.0478(3) 0.7174(2) 0.6164(2) 0.0558(12) Uani 1 1 d . . . O4 O 0.1497(4) 0.5929(2) 0.6484(2) 0.0513(11) Uani 1 1 d . . . O5 O 0.7796(6) 0.6268(3) 0.7155(3) 0.121(3) Uani 1 1 d U . . O6 O 0.7701(4) 0.6612(3) 0.6218(3) 0.087(2) Uani 1 1 d . . . O7 O 0.4262(5) 1.1178(3) 0.5202(3) 0.0930(19) Uani 1 1 d D . . H7' H 0.4460 1.0868 0.4961 0.140 Uiso 1 1 d R . . N1 N 0.4382(3) 0.8338(2) 0.63435(19) 0.0310(9) Uani 1 1 d . . . N2 N 0.2346(4) 0.7599(2) 0.6032(2) 0.0378(11) Uani 1 1 d . . . N3 N 0.3340(4) 0.6463(2) 0.6468(2) 0.0366(11) Uani 1 1 d . . . N4 N 0.5432(4) 0.7187(2) 0.6680(2) 0.0340(10) Uani 1 1 d . . . C1 C 0.3857(4) 0.8847(3) 0.6023(2) 0.0348(12) Uani 1 1 d . . . C2 C 0.2733(5) 0.8767(3) 0.5646(3) 0.0376(12) Uani 1 1 d . . . C3 C 0.1980(5) 0.8178(3) 0.5673(3) 0.0383(13) Uani 1 1 d . . . C4 C 0.0899(5) 0.8181(4) 0.5308(3) 0.0529(16) Uani 1 1 d . . . H4 H 0.0398 0.7794 0.5315 0.063 Uiso 1 1 calc R . . C5 C 0.0562(6) 0.8734(4) 0.4942(3) 0.0566(17) Uani 1 1 d . . . H5 H -0.0162 0.8719 0.4707 0.068 Uiso 1 1 calc R . . C6 C 0.1285(6) 0.9316(4) 0.4917(3) 0.0556(17) Uani 1 1 d . . . H6 H 0.1049 0.9697 0.4672 0.067 Uiso 1 1 calc R . . C7 C 0.2351(5) 0.9321(3) 0.5259(3) 0.0496(15) Uani 1 1 d . . . H7 H 0.2846 0.9708 0.5234 0.060 Uiso 1 1 calc R . . C8 C 0.1577(5) 0.7123(3) 0.6194(3) 0.0403(13) Uani 1 1 d . . . C9 C 0.2154(5) 0.6434(3) 0.6417(3) 0.0389(13) Uani 1 1 d . . . C10 C 0.4052(5) 0.5859(3) 0.6547(3) 0.0403(13) Uani 1 1 d . . . C11 C 0.5295(5) 0.5916(3) 0.6547(2) 0.0372(12) Uani 1 1 d . . . C12 C 0.5961(6) 0.5291(3) 0.6506(3) 0.0465(15) Uani 1 1 d . . . H12 H 0.6768 0.5325 0.6482 0.056 Uiso 1 1 calc R . . C13 C 0.5446(6) 0.4643(3) 0.6500(3) 0.0579(18) Uani 1 1 d . . . H13 H 0.5896 0.4241 0.6455 0.069 Uiso 1 1 calc R . . C14 C 0.4272(6) 0.4579(3) 0.6559(4) 0.066(2) Uani 1 1 d . . . H14 H 0.3937 0.4134 0.6585 0.079 Uiso 1 1 calc R . . C15 C 0.3581(6) 0.5177(3) 0.6582(4) 0.060(2) Uani 1 1 d . . . H15 H 0.2781 0.5126 0.6621 0.072 Uiso 1 1 calc R . . C16 C 0.7280(6) 0.6493(4) 0.6671(4) 0.065(2) Uani 1 1 d . . . C17 C 0.5940(5) 0.6575(3) 0.6637(2) 0.0361(12) Uani 1 1 d . . . C18 C 0.6040(4) 0.7807(3) 0.6899(2) 0.0353(12) Uani 1 1 d . . . C19 C 0.5447(4) 0.8441(3) 0.6739(2) 0.0348(12) Uani 1 1 d . . . C20 C 0.5882(5) 0.9069(3) 0.6987(3) 0.0430(14) Uani 1 1 d . . . H20 H 0.5484 0.9490 0.6889 0.052 Uiso 1 1 calc R . . C21 C 0.6899(5) 0.9078(3) 0.7381(3) 0.0496(15) Uani 1 1 d . . . H21 H 0.7183 0.9502 0.7549 0.060 Uiso 1 1 calc R . . C22 C 0.7495(6) 0.8457(4) 0.7524(3) 0.0558(17) Uani 1 1 d . . . H22 H 0.8198 0.8466 0.7777 0.067 Uiso 1 1 calc R . . C23 C 0.7059(5) 0.7821(3) 0.7296(3) 0.0494(15) Uani 1 1 d . . . H23 H 0.7450 0.7403 0.7408 0.059 Uiso 1 1 calc R . . C24 C 0.4368(5) 0.9592(3) 0.6002(3) 0.0391(13) Uani 1 1 d . . . C25 C 0.3620(7) 1.1723(4) 0.4853(4) 0.092(3) Uani 1 1 d D . . H25A H 0.4124 1.1926 0.4579 0.110 Uiso 1 1 calc R . . H25B H 0.3404 1.2095 0.5114 0.110 Uiso 1 1 calc R . . C26 C 0.2534(8) 1.1430(6) 0.4510(5) 0.127(4) Uani 1 1 d DU . . H26A H 0.2751 1.1086 0.4230 0.191 Uiso 1 1 calc R . . H26B H 0.2099 1.1805 0.4299 0.191 Uiso 1 1 calc R . . H26C H 0.2051 1.1211 0.4779 0.191 Uiso 1 1 calc R . . O8 O 0.0000 0.5932(7) 0.7500 0.159(5) Uani 1 2 d S . . 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 Cd1 0.0284(2) 0.0338(2) 0.1339(5) -0.0098(3) 0.0272(3) -0.00918(19) Ni1 0.0246(3) 0.0260(3) 0.0497(4) -0.0002(3) 0.0104(3) -0.0033(3) O1 0.044(2) 0.0220(18) 0.071(3) -0.0069(19) 0.015(2) 0.0015(17) O2 0.043(2) 0.035(2) 0.064(3) -0.0008(19) 0.019(2) -0.0078(18) O3 0.029(2) 0.039(2) 0.101(4) 0.002(2) 0.019(2) -0.0043(18) O4 0.043(2) 0.035(2) 0.076(3) 0.007(2) 0.006(2) -0.0161(19) O5 0.106(4) 0.090(4) 0.148(5) -0.025(4) -0.074(4) 0.043(4) O6 0.047(3) 0.044(3) 0.181(7) -0.013(3) 0.061(4) -0.003(2) O7 0.112(5) 0.070(4) 0.098(4) -0.021(3) 0.017(4) 0.038(3) N1 0.022(2) 0.031(2) 0.041(3) -0.0021(19) 0.0071(18) -0.0040(18) N2 0.026(2) 0.033(2) 0.056(3) 0.000(2) 0.011(2) -0.0067(19) N3 0.029(2) 0.025(2) 0.058(3) 0.000(2) 0.015(2) -0.0053(18) N4 0.030(2) 0.030(2) 0.043(3) 0.0017(19) 0.0081(19) -0.0017(19) C1 0.029(3) 0.027(3) 0.049(3) -0.002(2) 0.011(2) -0.004(2) C2 0.030(3) 0.033(3) 0.050(3) -0.002(2) 0.007(2) -0.001(2) C3 0.033(3) 0.033(3) 0.050(4) -0.006(2) 0.009(3) 0.001(2) C4 0.039(3) 0.055(4) 0.063(4) 0.002(3) -0.002(3) -0.015(3) C5 0.039(3) 0.068(5) 0.059(4) 0.006(4) -0.006(3) -0.004(3) C6 0.053(4) 0.054(4) 0.059(4) 0.012(3) -0.001(3) 0.003(3) C7 0.046(4) 0.036(3) 0.066(4) 0.004(3) 0.004(3) -0.006(3) C8 0.033(3) 0.033(3) 0.057(4) -0.006(3) 0.012(3) -0.005(2) C9 0.038(3) 0.030(3) 0.050(3) -0.005(2) 0.012(3) -0.008(2) C10 0.042(3) 0.030(3) 0.051(4) 0.005(2) 0.017(3) 0.002(2) C11 0.035(3) 0.034(3) 0.043(3) 0.007(2) 0.010(2) 0.003(2) C12 0.046(3) 0.037(3) 0.057(4) 0.007(3) 0.011(3) 0.006(3) C13 0.061(4) 0.043(4) 0.073(5) 0.006(3) 0.020(4) 0.015(3) C14 0.069(5) 0.027(3) 0.106(6) 0.013(3) 0.036(4) 0.006(3) C15 0.050(4) 0.027(3) 0.109(6) 0.006(3) 0.035(4) 0.000(3) C16 0.037(4) 0.039(4) 0.114(7) -0.021(4) -0.019(4) 0.006(3) C17 0.030(3) 0.039(3) 0.039(3) 0.002(2) 0.003(2) 0.001(2) C18 0.030(3) 0.035(3) 0.041(3) 0.000(2) 0.010(2) -0.005(2) C19 0.029(3) 0.038(3) 0.039(3) -0.001(2) 0.010(2) -0.008(2) C20 0.044(3) 0.035(3) 0.051(4) -0.002(3) 0.010(3) -0.008(3) C21 0.051(4) 0.048(4) 0.049(4) -0.006(3) 0.002(3) -0.016(3) C22 0.049(4) 0.062(4) 0.054(4) -0.001(3) -0.008(3) -0.011(3) C23 0.047(4) 0.047(4) 0.053(4) 0.000(3) -0.003(3) 0.000(3) C24 0.032(3) 0.030(3) 0.054(4) 0.003(3) 0.002(3) 0.002(2) C25 0.094(7) 0.067(6) 0.119(8) -0.025(5) 0.031(6) -0.008(5) C26 0.093(6) 0.132(7) 0.155(8) -0.037(7) 0.014(6) 0.009(6) O8 0.057(6) 0.211(13) 0.218(13) 0.000 0.060(7) 0.000 _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 Cd1 O1 2.208(4) . ? Cd1 O6 2.262(5) 3_455 ? Cd1 O7 2.273(6) . ? Cd1 O3 2.276(4) 3 ? Cd1 O4 2.303(4) 3 ? Ni1 N2 1.867(4) . ? Ni1 N4 1.868(4) . ? Ni1 N3 1.880(4) . ? Ni1 N1 1.888(4) . ? O1 C24 1.251(7) . ? O2 C24 1.233(7) . ? O3 C8 1.250(6) . ? O3 Cd1 2.276(4) 3_445 ? O4 C9 1.234(6) . ? O4 Cd1 2.303(4) 3_445 ? O5 C16 1.256(10) . ? O6 C16 1.201(10) . ? O6 Cd1 2.262(5) 3_545 ? O7 C25 1.446(7) . ? O7 H7' 0.8492 . ? N1 C1 1.309(7) . ? N1 C19 1.436(7) . ? N2 C8 1.337(7) . ? N2 C3 1.400(7) . ? N3 C9 1.344(7) . ? N3 C10 1.402(7) . ? N4 C17 1.305(7) . ? N4 C18 1.423(7) . ? C1 C2 1.463(8) . ? C1 C24 1.529(7) . ? C2 C7 1.403(8) . ? C2 C3 1.413(7) . ? C3 C4 1.403(8) . ? C4 C5 1.361(9) . ? C4 H4 0.9300 . ? C5 C6 1.382(9) . ? C5 H5 0.9300 . ? C6 C7 1.364(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.521(8) . ? C10 C15 1.405(8) . ? C10 C11 1.420(8) . ? C11 C12 1.414(8) . ? C11 C17 1.451(7) . ? C12 C13 1.359(9) . ? C12 H12 0.9300 . ? C13 C14 1.365(9) . ? C13 H13 0.9300 . ? C14 C15 1.383(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.528(8) . ? C18 C23 1.384(8) . ? C18 C19 1.406(7) . ? C19 C20 1.384(7) . ? C20 C21 1.379(8) . ? C20 H20 0.9300 . ? C21 C22 1.378(9) . ? C21 H21 0.9300 . ? C22 C23 1.380(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.491(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 O1 Cd1 O6 94.46(16) . 3_455 ? O1 Cd1 O7 97.79(19) . . ? O6 Cd1 O7 88.6(2) 3_455 . ? O1 Cd1 O3 169.80(15) . 3 ? O6 Cd1 O3 95.30(16) 3_455 3 ? O7 Cd1 O3 85.4(2) . 3 ? O1 Cd1 O4 97.85(14) . 3 ? O6 Cd1 O4 159.0(2) 3_455 3 ? O7 Cd1 O4 106.40(19) . 3 ? O3 Cd1 O4 71.95(14) 3 3 ? N2 Ni1 N4 177.3(2) . . ? N2 Ni1 N3 86.76(19) . . ? N4 Ni1 N3 94.16(19) . . ? N2 Ni1 N1 93.40(18) . . ? N4 Ni1 N1 85.90(18) . . ? N3 Ni1 N1 175.11(19) . . ? C24 O1 Cd1 114.0(4) . . ? C8 O3 Cd1 114.6(4) . 3_445 ? C9 O4 Cd1 115.6(4) . 3_445 ? C16 O6 Cd1 112.3(5) . 3_545 ? C25 O7 Cd1 125.3(5) . . ? C25 O7 H7' 107.3 . . ? Cd1 O7 H7' 127.2 . . ? C1 N1 C19 123.1(4) . . ? C1 N1 Ni1 126.7(4) . . ? C19 N1 Ni1 110.3(3) . . ? C8 N2 C3 121.7(5) . . ? C8 N2 Ni1 110.8(4) . . ? C3 N2 Ni1 127.4(3) . . ? C9 N3 C10 122.6(4) . . ? C9 N3 Ni1 111.5(4) . . ? C10 N3 Ni1 125.8(3) . . ? C17 N4 C18 123.7(4) . . ? C17 N4 Ni1 124.5(4) . . ? C18 N4 Ni1 111.4(3) . . ? N1 C1 C2 124.1(5) . . ? N1 C1 C24 123.0(5) . . ? C2 C1 C24 112.9(5) . . ? C7 C2 C3 118.1(5) . . ? C7 C2 C1 118.3(5) . . ? C3 C2 C1 123.5(5) . . ? N2 C3 C4 121.9(5) . . ? N2 C3 C2 120.1(5) . . ? C4 C3 C2 117.9(5) . . ? C5 C4 C3 121.9(6) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 120.7(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 118.6(6) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C2 122.8(6) . . ? C6 C7 H7 118.6 . . ? C2 C7 H7 118.6 . . ? O3 C8 N2 128.1(5) . . ? O3 C8 C9 118.5(5) . . ? N2 C8 C9 113.3(5) . . ? O4 C9 N3 129.8(5) . . ? O4 C9 C8 117.3(5) . . ? N3 C9 C8 112.7(4) . . ? N3 C10 C15 122.5(5) . . ? N3 C10 C11 120.1(5) . . ? C15 C10 C11 117.2(5) . . ? C12 C11 C10 118.6(5) . . ? C12 C11 C17 117.4(5) . . ? C10 C11 C17 123.7(5) . . ? C13 C12 C11 121.4(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 121.8(6) . . ? C14 C15 H15 119.1 . . ? C10 C15 H15 119.1 . . ? O6 C16 O5 127.9(8) . . ? O6 C16 C17 115.6(7) . . ? O5 C16 C17 116.3(9) . . ? N4 C17 C11 123.5(5) . . ? N4 C17 C16 122.4(5) . . ? C11 C17 C16 114.1(5) . . ? C23 C18 C19 119.6(5) . . ? C23 C18 N4 125.6(5) . . ? C19 C18 N4 114.4(5) . . ? C20 C19 C18 119.3(5) . . ? C20 C19 N1 127.4(5) . . ? C18 C19 N1 113.2(5) . . ? C21 C20 C19 120.6(6) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 119.8(6) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.6(6) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 120.0(6) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? O2 C24 O1 127.6(5) . . ? O2 C24 C1 118.2(5) . . ? O1 C24 C1 114.1(5) . . ? O7 C25 C26 111.0(8) . . ? O7 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? O7 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 O6 Cd1 O1 C24 139.6(4) 3_455 . . . ? O7 Cd1 O1 C24 50.5(4) . . . . ? O3 Cd1 O1 C24 -57.4(11) 3 . . . ? O4 Cd1 O1 C24 -57.4(4) 3 . . . ? O1 Cd1 O7 C25 128.0(6) . . . . ? O6 Cd1 O7 C25 33.7(6) 3_455 . . . ? O3 Cd1 O7 C25 -61.7(6) 3 . . . ? O4 Cd1 O7 C25 -131.4(6) 3 . . . ? N2 Ni1 N1 C1 -16.9(5) . . . . ? N4 Ni1 N1 C1 160.5(5) . . . . ? N3 Ni1 N1 C1 -109(2) . . . . ? N2 Ni1 N1 C19 162.2(3) . . . . ? N4 Ni1 N1 C19 -20.3(3) . . . . ? N3 Ni1 N1 C19 71(2) . . . . ? N4 Ni1 N2 C8 131(4) . . . . ? N3 Ni1 N2 C8 20.7(4) . . . . ? N1 Ni1 N2 C8 -154.4(4) . . . . ? N4 Ni1 N2 C3 -52(4) . . . . ? N3 Ni1 N2 C3 -161.8(5) . . . . ? N1 Ni1 N2 C3 23.1(5) . . . . ? N2 Ni1 N3 C9 -16.9(4) . . . . ? N4 Ni1 N3 C9 165.6(4) . . . . ? N1 Ni1 N3 C9 75(2) . . . . ? N2 Ni1 N3 C10 159.4(5) . . . . ? N4 Ni1 N3 C10 -18.1(5) . . . . ? N1 Ni1 N3 C10 -109(2) . . . . ? N2 Ni1 N4 C17 -80(4) . . . . ? N3 Ni1 N4 C17 30.3(5) . . . . ? N1 Ni1 N4 C17 -154.6(5) . . . . ? N2 Ni1 N4 C18 93(4) . . . . ? N3 Ni1 N4 C18 -157.1(4) . . . . ? N1 Ni1 N4 C18 18.0(4) . . . . ? C19 N1 C1 C2 -176.0(5) . . . . ? Ni1 N1 C1 C2 3.1(8) . . . . ? C19 N1 C1 C24 4.4(8) . . . . ? Ni1 N1 C1 C24 -176.6(4) . . . . ? N1 C1 C2 C7 -170.8(5) . . . . ? C24 C1 C2 C7 8.9(7) . . . . ? N1 C1 C2 C3 12.6(9) . . . . ? C24 C1 C2 C3 -167.7(5) . . . . ? C8 N2 C3 C4 -21.3(8) . . . . ? Ni1 N2 C3 C4 161.5(5) . . . . ? C8 N2 C3 C2 162.1(5) . . . . ? Ni1 N2 C3 C2 -15.0(8) . . . . ? C7 C2 C3 N2 177.0(5) . . . . ? C1 C2 C3 N2 -6.3(8) . . . . ? C7 C2 C3 C4 0.3(8) . . . . ? C1 C2 C3 C4 177.0(5) . . . . ? N2 C3 C4 C5 -177.6(6) . . . . ? C2 C3 C4 C5 -0.9(10) . . . . ? C3 C4 C5 C6 0.2(11) . . . . ? C4 C5 C6 C7 1.0(11) . . . . ? C5 C6 C7 C2 -1.6(11) . . . . ? C3 C2 C7 C6 0.9(9) . . . . ? C1 C2 C7 C6 -175.9(6) . . . . ? Cd1 O3 C8 N2 161.6(5) 3_445 . . . ? Cd1 O3 C8 C9 -15.8(7) 3_445 . . . ? C3 N2 C8 O3 -15.0(10) . . . . ? Ni1 N2 C8 O3 162.6(5) . . . . ? C3 N2 C8 C9 162.6(5) . . . . ? Ni1 N2 C8 C9 -19.8(6) . . . . ? Cd1 O4 C9 N3 -171.7(5) 3_445 . . . ? Cd1 O4 C9 C8 2.7(7) 3_445 . . . ? C10 N3 C9 O4 7.9(10) . . . . ? Ni1 N3 C9 O4 -175.6(5) . . . . ? C10 N3 C9 C8 -166.7(5) . . . . ? Ni1 N3 C9 C8 9.8(6) . . . . ? O3 C8 C9 O4 9.1(8) . . . . ? N2 C8 C9 O4 -168.7(5) . . . . ? O3 C8 C9 N3 -175.5(5) . . . . ? N2 C8 C9 N3 6.7(7) . . . . ? C9 N3 C10 C15 -0.4(9) . . . . ? Ni1 N3 C10 C15 -176.3(5) . . . . ? C9 N3 C10 C11 174.6(5) . . . . ? Ni1 N3 C10 C11 -1.4(8) . . . . ? N3 C10 C11 C12 -167.3(5) . . . . ? C15 C10 C11 C12 7.9(9) . . . . ? N3 C10 C11 C17 18.0(9) . . . . ? C15 C10 C11 C17 -166.8(6) . . . . ? C10 C11 C12 C13 -3.8(9) . . . . ? C17 C11 C12 C13 171.3(6) . . . . ? C11 C12 C13 C14 -2.7(11) . . . . ? C12 C13 C14 C15 4.8(12) . . . . ? C13 C14 C15 C10 -0.2(12) . . . . ? N3 C10 C15 C14 169.0(7) . . . . ? C11 C10 C15 C14 -6.1(11) . . . . ? Cd1 O6 C16 O5 15.0(10) 3_545 . . . ? Cd1 O6 C16 C17 -160.2(4) 3_545 . . . ? C18 N4 C17 C11 165.2(5) . . . . ? Ni1 N4 C17 C11 -23.1(8) . . . . ? C18 N4 C17 C16 -15.6(9) . . . . ? Ni1 N4 C17 C16 156.2(5) . . . . ? C12 C11 C17 N4 179.6(5) . . . . ? C10 C11 C17 N4 -5.6(9) . . . . ? C12 C11 C17 C16 0.3(8) . . . . ? C10 C11 C17 C16 175.1(6) . . . . ? O6 C16 C17 N4 -81.5(8) . . . . ? O5 C16 C17 N4 102.7(7) . . . . ? O6 C16 C17 C11 97.8(7) . . . . ? O5 C16 C17 C11 -77.9(7) . . . . ? C17 N4 C18 C23 -26.6(8) . . . . ? Ni1 N4 C18 C23 160.7(5) . . . . ? C17 N4 C18 C19 160.9(5) . . . . ? Ni1 N4 C18 C19 -11.8(6) . . . . ? C23 C18 C19 C20 -1.0(8) . . . . ? N4 C18 C19 C20 172.0(5) . . . . ? C23 C18 C19 N1 -177.6(5) . . . . ? N4 C18 C19 N1 -4.6(6) . . . . ? C1 N1 C19 C20 21.5(8) . . . . ? Ni1 N1 C19 C20 -157.7(5) . . . . ? C1 N1 C19 C18 -162.2(5) . . . . ? Ni1 N1 C19 C18 18.6(5) . . . . ? C18 C19 C20 C21 1.2(8) . . . . ? N1 C19 C20 C21 177.3(5) . . . . ? C19 C20 C21 C22 0.6(9) . . . . ? C20 C21 C22 C23 -2.6(10) . . . . ? C21 C22 C23 C18 2.7(10) . . . . ? C19 C18 C23 C22 -0.9(9) . . . . ? N4 C18 C23 C22 -173.1(6) . . . . ? Cd1 O1 C24 O2 1.5(8) . . . . ? Cd1 O1 C24 C1 -174.5(3) . . . . ? N1 C1 C24 O2 81.8(7) . . . . ? C2 C1 C24 O2 -97.9(6) . . . . ? N1 C1 C24 O1 -101.9(6) . . . . ? C2 C1 C24 O1 78.4(6) . . . . ? Cd1 O7 C25 C26 -113.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.851 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.089