# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jan Reedijk' _publ_contact_author_email REEDIJK@CHEM.LEIDENUNIV.NL _publ_section_title ; Hydrogen-bond assisted co-crystallization of a bimetallic MnIII2NiII2 cluster and a NiII2 cluster unit: Synthesis, structure, spectroscopy and magnetism ; loop_ _publ_author_name 'Jan Reedijk' 'Guillem Aromi' 'Patrick Gamez' 'Sanjit Nayak' 'Jordi Ribas-Arino' 'Simon J. Teat' # Attachment 'nayak_Compound_1.CIF' data_ns168 _database_code_depnum_ccdc_archive 'CCDC 747743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H124 Cl6 Mn4 N10 Ni6 O34' _chemical_formula_weight 2818.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cl Cl 0.1408 0.1896 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Mn Mn 0.2237 0.8587 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Ni Ni 0.1906 1.3024 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _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 12.0420(13) _cell_length_b 16.2062(18) _cell_length_c 16.7613(18) _cell_angle_alpha 87.338(2) _cell_angle_beta 69.454(2) _cell_angle_gamma 71.207(2) _cell_volume 2891.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8899 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 31.09 _exptl_crystal_description lath _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 2.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'SADABS-2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 40431 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 30.65 _reflns_number_total 13690 _reflns_number_gt 9921 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.56a' _computing_data_reduction 'Bruker SAINT v7.56a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogens atoms were refined anisotrpically except the 20% occupied Chloride ion. Hydrogen atoms were place geometrically on the carbon atoms, with the exception of the methanol were the atoms were found in the difference map and constrain. All these hydrogens were refined using a riding model. The hydroxyl and water hydrogens were found in the difference map, their distance to their oxygens were restrained and their displacement parameter were set to ride on those of their oxygens. ; _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^)+(0.0489P)^2^+3.1538P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13690 _refine_ls_number_parameters 760 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.61748(4) 0.46213(3) 0.02711(2) 0.02007(10) Uani 1 1 d . . . Mn1 Mn 0.35992(5) 0.44622(3) 0.13589(3) 0.01981(11) Uani 1 1 d . . . O1 O 0.5020(2) 0.49797(16) 0.14648(14) 0.0235(5) Uani 1 1 d . . . C1 C 0.5196(3) 0.5438(2) 0.20191(19) 0.0208(7) Uani 1 1 d . . . C2 C 0.4192(3) 0.5842(2) 0.2771(2) 0.0246(7) Uani 1 1 d . . . H2A H 0.3391 0.5793 0.2866 0.030 Uiso 1 1 calc R . . C3 C 0.4335(3) 0.6307(2) 0.3377(2) 0.0271(8) Uani 1 1 d . . . H3A H 0.3632 0.6582 0.3872 0.033 Uiso 1 1 calc R . . C4 C 0.5504(4) 0.6378(2) 0.3269(2) 0.0282(8) Uani 1 1 d . . . H4A H 0.5609 0.6684 0.3691 0.034 Uiso 1 1 calc R . . C5 C 0.6502(3) 0.5991(2) 0.2533(2) 0.0263(7) Uani 1 1 d . . . H5A H 0.7301 0.6034 0.2457 0.032 Uiso 1 1 calc R . . C6 C 0.6380(3) 0.5536(2) 0.1890(2) 0.0224(7) Uani 1 1 d . . . C7 C 0.7482(3) 0.5267(2) 0.1101(2) 0.0233(7) Uani 1 1 d . . . H7A H 0.8241 0.5313 0.1116 0.028 Uiso 1 1 calc R . . N1 N 0.7513(3) 0.49770(18) 0.03985(17) 0.0218(6) Uani 1 1 d . . . C8 C 0.8638(3) 0.4829(2) -0.0387(2) 0.0231(7) Uani 1 1 d . . . H8A H 0.9398 0.4506 -0.0246 0.028 Uiso 1 1 calc R . . C9 C 0.8529(3) 0.4253(2) -0.1047(2) 0.0230(7) Uani 1 1 d . . . H9A H 0.9056 0.4337 -0.1628 0.028 Uiso 1 1 calc R . . H9B H 0.8852 0.3631 -0.0940 0.028 Uiso 1 1 calc R . . O2 O 0.7269(2) 0.44566(15) -0.10067(13) 0.0204(5) Uani 1 1 d . . . C10 C 0.8764(3) 0.5694(2) -0.0728(2) 0.0229(7) Uani 1 1 d . . . H10A H 0.8790 0.6056 -0.0280 0.027 Uiso 1 1 calc R . . H10B H 0.9556 0.5585 -0.1224 0.027 Uiso 1 1 calc R . . O3 O 0.7719(2) 0.61512(16) -0.09831(16) 0.0253(5) Uani 1 1 d D . . O4 O 0.2567(2) 0.45890(15) 0.24998(14) 0.0236(5) Uani 1 1 d . . . C11 C 0.2575(3) 0.3996(2) 0.3082(2) 0.0240(7) Uani 1 1 d . . . C12 C 0.1706(4) 0.4264(3) 0.3917(2) 0.0297(8) Uani 1 1 d . . . H12A H 0.1162 0.4852 0.4052 0.036 Uiso 1 1 calc R . . C13 C 0.1641(4) 0.3679(3) 0.4540(2) 0.0390(10) Uani 1 1 d . . . H13A H 0.1048 0.3870 0.5101 0.047 Uiso 1 1 calc R . . C14 C 0.2429(4) 0.2815(3) 0.4365(2) 0.0416(10) Uani 1 1 d . . . H14A H 0.2367 0.2420 0.4802 0.050 Uiso 1 1 calc R . . C15 C 0.3300(4) 0.2533(3) 0.3557(2) 0.0338(9) Uani 1 1 d . . . H15A H 0.3847 0.1945 0.3441 0.041 Uiso 1 1 calc R . . C16 C 0.3383(3) 0.3113(2) 0.2900(2) 0.0247(7) Uani 1 1 d . . . C17 C 0.4285(3) 0.2768(2) 0.2072(2) 0.0257(7) Uani 1 1 d . . . H17A H 0.4762 0.2164 0.2006 0.031 Uiso 1 1 calc R . . N2 N 0.4505(3) 0.32120(18) 0.14021(17) 0.0219(6) Uani 1 1 d . . . C18 C 0.5462(3) 0.2749(2) 0.0569(2) 0.0249(7) Uani 1 1 d . . . H18A H 0.5342 0.2178 0.0496 0.030 Uiso 1 1 calc R . . C19 C 0.6779(3) 0.2569(2) 0.0548(2) 0.0274(8) Uani 1 1 d . . . H19A H 0.6891 0.2231 0.1037 0.033 Uiso 1 1 calc R . . H19B H 0.7383 0.2214 0.0015 0.033 Uiso 1 1 calc R . . O5 O 0.4771(2) 0.42277(15) 0.01847(13) 0.0210(5) Uani 1 1 d . . . C20 C 0.5163(3) 0.3326(2) -0.0130(2) 0.0235(7) Uani 1 1 d . . . H20A H 0.5917 0.3197 -0.0657 0.028 Uiso 1 1 calc R . . H20B H 0.4486 0.3212 -0.0264 0.028 Uiso 1 1 calc R . . O6 O 0.7028(2) 0.33732(17) 0.05887(16) 0.0275(5) Uani 1 1 d D . . Ni2 Ni 0.87091(4) -0.01424(3) 0.52059(2) 0.01726(9) Uani 1 1 d . . . Mn2 Mn 0.89977(5) 0.15774(3) 0.45479(3) 0.01727(11) Uani 1 1 d . . . O7 O 0.9698(2) -0.13746(14) 0.47488(14) 0.0192(5) Uani 1 1 d . . . C21 C 0.9518(3) -0.1798(2) 0.41782(19) 0.0193(6) Uani 1 1 d . . . C22 C 1.0367(3) -0.2645(2) 0.38362(19) 0.0206(7) Uani 1 1 d . . . H22A H 1.1065 -0.2887 0.4015 0.025 Uiso 1 1 calc R . . C23 C 1.0208(3) -0.3126(2) 0.3252(2) 0.0233(7) Uani 1 1 d . . . H23A H 1.0792 -0.3693 0.3039 0.028 Uiso 1 1 calc R . . C24 C 0.9192(3) -0.2789(2) 0.2969(2) 0.0249(7) Uani 1 1 d . . . H24A H 0.9082 -0.3119 0.2566 0.030 Uiso 1 1 calc R . . C25 C 0.8364(3) -0.1969(2) 0.3290(2) 0.0237(7) Uani 1 1 d . . . H25A H 0.7674 -0.1739 0.3101 0.028 Uiso 1 1 calc R . . C26 C 0.8486(3) -0.1453(2) 0.3885(2) 0.0204(7) Uani 1 1 d . . . C27 C 0.7526(3) -0.0600(2) 0.4145(2) 0.0220(7) Uani 1 1 d . . . H27A H 0.6868 -0.0470 0.3923 0.026 Uiso 1 1 calc R . . N3 N 0.7482(3) -0.00033(17) 0.46496(17) 0.0191(5) Uani 1 1 d . . . C28 C 0.6495(3) 0.0863(2) 0.4810(2) 0.0237(7) Uani 1 1 d . . . H28A H 0.5656 0.0778 0.5009 0.028 Uiso 1 1 calc R . . C29 C 0.6576(3) 0.1376(2) 0.5527(2) 0.0233(7) Uani 1 1 d . . . H29A H 0.6193 0.2009 0.5489 0.028 Uiso 1 1 calc R . . H29B H 0.6087 0.1218 0.6087 0.028 Uiso 1 1 calc R . . O8 O 0.7842(2) 0.12034(14) 0.54817(14) 0.0196(5) Uani 1 1 d . . . C30 C 0.6647(3) 0.1351(2) 0.4002(2) 0.0258(7) Uani 1 1 d . . . H30A H 0.6637 0.0995 0.3542 0.031 Uiso 1 1 calc R . . H30B H 0.5943 0.1909 0.4112 0.031 Uiso 1 1 calc R . . O9 O 0.7814(2) 0.15230(16) 0.37433(15) 0.0248(5) Uani 1 1 d D . . O10 O 0.8218(2) 0.27929(14) 0.47476(14) 0.0219(5) Uani 1 1 d . . . C31 C 0.8509(3) 0.3424(2) 0.4264(2) 0.0207(7) Uani 1 1 d . . . C32 C 0.7774(4) 0.4295(2) 0.4556(2) 0.0284(8) Uani 1 1 d . . . H32A H 0.7088 0.4417 0.5084 0.034 Uiso 1 1 calc R . . C33 C 0.8038(4) 0.4977(2) 0.4085(2) 0.0309(8) Uani 1 1 d . . . H33A H 0.7528 0.5561 0.4296 0.037 Uiso 1 1 calc R . . C34 C 0.9031(4) 0.4825(2) 0.3310(2) 0.0321(8) Uani 1 1 d . . . H34A H 0.9207 0.5299 0.2994 0.038 Uiso 1 1 calc R . . C35 C 0.9758(3) 0.3974(2) 0.3007(2) 0.0294(8) Uani 1 1 d . . . H35A H 1.0439 0.3866 0.2477 0.035 Uiso 1 1 calc R . . C36 C 0.9514(3) 0.3262(2) 0.3464(2) 0.0223(7) Uani 1 1 d . . . C37 C 1.0282(3) 0.2399(2) 0.3072(2) 0.0224(7) Uani 1 1 d . . . H37A H 1.0901 0.2355 0.2521 0.027 Uiso 1 1 calc R . . N4 N 1.0197(3) 0.16852(18) 0.34082(16) 0.0201(6) Uani 1 1 d . . . C38 C 1.1039(3) 0.0837(2) 0.2912(2) 0.0210(7) Uani 1 1 d . . . H38A H 1.1034 0.0874 0.2316 0.025 Uiso 1 1 calc R . . C39 C 1.0460(3) 0.0137(2) 0.33333(19) 0.0211(7) Uani 1 1 d . . . H39A H 0.9781 0.0138 0.3130 0.025 Uiso 1 1 calc R . . H39B H 1.1107 -0.0449 0.3187 0.025 Uiso 1 1 calc R . . O11 O 0.9966(2) 0.03436(14) 0.42417(13) 0.0181(4) Uani 1 1 d . . . C40 C 1.2372(3) 0.0648(2) 0.2871(2) 0.0226(7) Uani 1 1 d . . . H40A H 1.2926 0.0117 0.2487 0.027 Uiso 1 1 calc R . . H40B H 1.2666 0.1143 0.2633 0.027 Uiso 1 1 calc R . . O12 O 1.2446(2) 0.05206(16) 0.37047(14) 0.0232(5) Uani 1 1 d D . . Ni3 Ni 0.59961(4) 0.93990(3) 0.03549(3) 0.02040(10) Uani 1 1 d . . . Cl1 Cl 0.68729(8) 0.82637(5) -0.08586(5) 0.02465(17) Uani 1 1 d . . . O1W O 0.5472(2) 1.04594(16) 0.12438(15) 0.0240(5) Uani 1 1 d D . . H1WA H 0.525(4) 1.029(3) 0.1740(12) 0.036 Uiso 1 1 d D . . H1WB H 0.478(2) 1.082(2) 0.127(3) 0.036 Uiso 1 1 d D . . O13 O 0.4178(2) 0.96504(15) 0.04849(14) 0.0215(5) Uani 1 1 d . . . C41 C 0.3397(3) 0.9235(2) 0.09261(19) 0.0219(7) Uani 1 1 d . . . C42 C 0.2224(3) 0.9420(3) 0.0842(2) 0.0285(8) Uani 1 1 d . . . H42A H 0.2005 0.9844 0.0465 0.034 Uiso 1 1 calc R . . C43 C 0.1373(4) 0.9005(3) 0.1290(2) 0.0348(9) Uani 1 1 d . . . H43A H 0.0589 0.9148 0.1213 0.042 Uiso 1 1 calc R . . C44 C 0.1651(4) 0.8384(3) 0.1847(2) 0.0346(9) Uani 1 1 d . . . H44A H 0.1069 0.8099 0.2153 0.042 Uiso 1 1 calc R . . C45 C 0.2791(4) 0.8190(2) 0.1950(2) 0.0308(8) Uani 1 1 d . . . H45A H 0.2983 0.7767 0.2335 0.037 Uiso 1 1 calc R . . C46 C 0.3695(3) 0.8597(2) 0.1503(2) 0.0240(7) Uani 1 1 d . . . C47 C 0.4844(3) 0.8333(2) 0.1667(2) 0.0260(7) Uani 1 1 d . . . H47A H 0.4902 0.7937 0.2098 0.031 Uiso 1 1 calc R . . N5 N 0.5808(3) 0.85767(18) 0.12902(17) 0.0241(6) Uani 1 1 d . . . C48 C 0.6943(4) 0.8169(2) 0.1497(2) 0.0301(8) Uani 1 1 d . . . H48A H 0.6710 0.8075 0.2120 0.036 Uiso 1 1 calc R . . C49 C 0.7735(4) 0.8769(3) 0.1262(2) 0.0311(8) Uani 1 1 d . . . H49A H 0.7344 0.9282 0.1683 0.037 Uiso 1 1 calc R . . H49B H 0.8583 0.8454 0.1273 0.037 Uiso 1 1 calc R . . O14 O 0.7830(2) 0.9054(2) 0.04217(16) 0.0344(6) Uani 1 1 d D . . C50 C 0.7595(4) 0.7287(3) 0.0968(3) 0.0357(9) Uani 1 1 d . . . H50A H 0.7028 0.6932 0.1134 0.043 Uiso 1 1 calc R . . H50B H 0.7771 0.7387 0.0355 0.043 Uiso 1 1 calc R . . O15 O 0.8736(3) 0.68210(19) 0.10910(19) 0.0410(7) Uani 1 1 d D . . Cl2 Cl 1.52146(8) 0.00704(6) 0.31266(5) 0.02775(18) Uani 1 1 d . . . Cl3 Cl 1.02724(11) 0.73799(8) -0.05918(8) 0.0353(3) Uani 0.80 1 d P A 1 Cl3' Cl 1.0804(5) 0.6895(3) -0.1056(3) 0.0348(10) Uiso 0.20 1 d P B 2 O1S O 0.7723(4) 0.2552(2) 0.2478(2) 0.0692(11) Uani 1 1 d . . . H1S H 0.8313 0.2561 0.2026 0.104 Uiso 1 1 calc R . . C1S C 0.6854(8) 0.3429(4) 0.2750(5) 0.091(2) Uani 1 1 d . . . H1S1 H 0.6331 0.3454 0.3353 0.136 Uiso 1 1 calc R . . H1S2 H 0.6319 0.3589 0.2404 0.136 Uiso 1 1 calc R . . H1S3 H 0.7324 0.3838 0.2678 0.136 Uiso 1 1 calc R . . H3O H 0.768(7) 0.6677(16) -0.103(5) 0.136 Uiso 1 1 d D . . H6O H 0.775(3) 0.331(5) 0.059(5) 0.136 Uiso 1 1 d D . . H9O H 0.779(8) 0.189(4) 0.337(4) 0.136 Uiso 1 1 d D . . H12O H 1.321(2) 0.041(5) 0.364(5) 0.136 Uiso 1 1 d D . . H14O H 0.839(5) 0.870(4) 0.002(3) 0.136 Uiso 1 1 d D . . H15O H 0.920(6) 0.705(5) 0.072(4) 0.136 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 0.0212(2) 0.0218(2) 0.01541(19) 0.00109(16) -0.00352(16) -0.00806(17) Mn1 0.0211(3) 0.0194(3) 0.0158(2) 0.00164(18) -0.00289(19) -0.0065(2) O1 0.0252(12) 0.0289(13) 0.0168(10) 0.0021(9) -0.0053(9) -0.0119(10) C1 0.0256(17) 0.0193(16) 0.0165(14) 0.0041(12) -0.0078(13) -0.0062(13) C2 0.0256(18) 0.0235(18) 0.0198(15) 0.0022(13) -0.0023(13) -0.0080(14) C3 0.0310(19) 0.0275(19) 0.0170(15) 0.0010(13) -0.0036(14) -0.0074(15) C4 0.037(2) 0.0293(19) 0.0185(15) -0.0017(14) -0.0107(15) -0.0093(16) C5 0.0232(18) 0.0313(19) 0.0230(16) 0.0020(14) -0.0090(14) -0.0061(15) C6 0.0236(17) 0.0222(17) 0.0194(15) 0.0033(13) -0.0072(13) -0.0054(14) C7 0.0196(16) 0.0237(17) 0.0242(16) 0.0017(13) -0.0071(13) -0.0049(14) N1 0.0224(14) 0.0201(14) 0.0201(13) 0.0003(11) -0.0050(11) -0.0059(12) C8 0.0227(17) 0.0242(18) 0.0203(15) 0.0012(13) -0.0040(13) -0.0088(14) C9 0.0204(17) 0.0233(17) 0.0212(15) -0.0016(13) -0.0038(13) -0.0053(14) O2 0.0219(12) 0.0197(12) 0.0183(10) 0.0004(9) -0.0041(9) -0.0084(9) C10 0.0215(17) 0.0223(17) 0.0220(15) 0.0010(13) -0.0050(13) -0.0063(14) O3 0.0238(12) 0.0218(13) 0.0290(12) 0.0028(10) -0.0097(10) -0.0054(10) O4 0.0248(12) 0.0231(12) 0.0190(11) 0.0038(9) -0.0027(9) -0.0089(10) C11 0.0265(18) 0.0264(18) 0.0226(16) 0.0026(13) -0.0074(14) -0.0147(15) C12 0.032(2) 0.034(2) 0.0208(16) 0.0023(15) -0.0029(15) -0.0146(17) C13 0.046(2) 0.045(3) 0.0238(18) 0.0036(17) -0.0028(17) -0.024(2) C14 0.055(3) 0.047(3) 0.0275(19) 0.0159(18) -0.0111(19) -0.028(2) C15 0.043(2) 0.029(2) 0.034(2) 0.0125(16) -0.0149(17) -0.0191(18) C16 0.0309(19) 0.0262(18) 0.0219(16) 0.0067(14) -0.0097(14) -0.0161(15) C17 0.0286(19) 0.0206(17) 0.0309(18) 0.0034(14) -0.0138(15) -0.0087(14) N2 0.0216(14) 0.0228(15) 0.0207(13) 0.0013(11) -0.0058(11) -0.0085(12) C18 0.0255(18) 0.0220(17) 0.0234(16) -0.0034(13) -0.0047(14) -0.0064(14) C19 0.0259(18) 0.0223(18) 0.0293(18) 0.0013(14) -0.0051(14) -0.0070(15) O5 0.0231(12) 0.0189(12) 0.0179(11) -0.0013(9) -0.0032(9) -0.0071(9) C20 0.0249(17) 0.0210(17) 0.0210(15) -0.0035(13) -0.0031(13) -0.0075(14) O6 0.0302(14) 0.0251(13) 0.0301(13) 0.0061(10) -0.0114(11) -0.0127(11) Ni2 0.0192(2) 0.0147(2) 0.01826(19) 0.00297(15) -0.00812(16) -0.00470(16) Mn2 0.0194(2) 0.0140(2) 0.0171(2) 0.00317(18) -0.00616(19) -0.00451(19) O7 0.0227(12) 0.0151(11) 0.0207(11) 0.0011(9) -0.0101(9) -0.0045(9) C21 0.0258(17) 0.0176(16) 0.0161(14) 0.0058(12) -0.0064(13) -0.0108(13) C22 0.0237(17) 0.0203(16) 0.0179(14) 0.0049(12) -0.0080(13) -0.0073(13) C23 0.0291(18) 0.0175(16) 0.0198(15) 0.0011(12) -0.0048(13) -0.0071(14) C24 0.034(2) 0.0235(18) 0.0215(16) 0.0020(13) -0.0119(14) -0.0138(15) C25 0.0270(18) 0.0248(18) 0.0239(16) 0.0065(13) -0.0134(14) -0.0104(15) C26 0.0227(17) 0.0205(16) 0.0199(15) 0.0069(12) -0.0080(13) -0.0096(13) C27 0.0264(18) 0.0227(17) 0.0214(15) 0.0071(13) -0.0112(13) -0.0113(14) N3 0.0202(14) 0.0160(13) 0.0220(13) 0.0036(10) -0.0094(11) -0.0050(11) C28 0.0211(17) 0.0189(17) 0.0306(17) 0.0049(14) -0.0111(14) -0.0040(13) C29 0.0199(16) 0.0200(17) 0.0260(16) 0.0003(13) -0.0069(13) -0.0026(13) O8 0.0196(11) 0.0183(11) 0.0205(11) 0.0032(9) -0.0068(9) -0.0063(9) C30 0.0256(18) 0.0218(17) 0.0342(18) 0.0091(14) -0.0163(15) -0.0078(14) O9 0.0278(13) 0.0253(13) 0.0268(12) 0.0087(10) -0.0143(10) -0.0118(11) O10 0.0247(12) 0.0164(11) 0.0206(11) 0.0048(9) -0.0052(9) -0.0053(9) C31 0.0243(17) 0.0188(16) 0.0227(15) 0.0053(13) -0.0125(13) -0.0078(13) C32 0.033(2) 0.0205(18) 0.0267(17) 0.0012(14) -0.0103(15) -0.0031(15) C33 0.038(2) 0.0185(18) 0.037(2) 0.0039(15) -0.0178(17) -0.0066(16) C34 0.036(2) 0.0230(19) 0.039(2) 0.0149(16) -0.0156(17) -0.0111(16) C35 0.0282(19) 0.0263(19) 0.0314(18) 0.0111(15) -0.0082(15) -0.0097(15) C36 0.0212(17) 0.0223(17) 0.0232(16) 0.0062(13) -0.0087(13) -0.0064(14) C37 0.0225(17) 0.0236(17) 0.0201(15) 0.0054(13) -0.0070(13) -0.0074(14) N4 0.0220(14) 0.0191(14) 0.0183(12) 0.0017(10) -0.0081(11) -0.0045(11) C38 0.0248(17) 0.0203(16) 0.0163(14) -0.0010(12) -0.0065(13) -0.0058(14) C39 0.0246(17) 0.0181(16) 0.0185(15) -0.0009(12) -0.0083(13) -0.0031(13) O11 0.0216(11) 0.0148(11) 0.0170(10) 0.0012(8) -0.0067(9) -0.0050(9) C40 0.0227(17) 0.0229(17) 0.0195(15) 0.0021(13) -0.0065(13) -0.0049(14) O12 0.0234(12) 0.0260(13) 0.0212(11) 0.0065(9) -0.0091(10) -0.0087(10) Ni3 0.0213(2) 0.0205(2) 0.0196(2) 0.00452(16) -0.00801(17) -0.00665(17) Cl1 0.0283(4) 0.0220(4) 0.0221(4) 0.0033(3) -0.0099(3) -0.0054(3) O1W 0.0273(13) 0.0227(13) 0.0229(11) 0.0057(10) -0.0107(10) -0.0080(10) O13 0.0219(12) 0.0210(12) 0.0230(11) 0.0069(9) -0.0076(9) -0.0101(10) C41 0.0270(18) 0.0210(17) 0.0166(14) -0.0001(12) -0.0038(13) -0.0104(14) C42 0.0280(19) 0.035(2) 0.0254(17) 0.0037(15) -0.0066(15) -0.0172(16) C43 0.033(2) 0.043(2) 0.0296(19) -0.0033(17) -0.0039(16) -0.0203(18) C44 0.039(2) 0.035(2) 0.0269(18) -0.0046(16) 0.0037(16) -0.0238(18) C45 0.043(2) 0.0195(18) 0.0209(16) 0.0013(13) 0.0014(15) -0.0120(16) C46 0.0304(18) 0.0183(16) 0.0196(15) -0.0003(13) -0.0032(13) -0.0092(14) C47 0.036(2) 0.0162(16) 0.0208(16) 0.0046(13) -0.0063(14) -0.0077(15) N5 0.0292(16) 0.0192(14) 0.0212(13) 0.0006(11) -0.0115(12) -0.0018(12) C48 0.037(2) 0.0231(18) 0.0277(18) 0.0021(14) -0.0173(16) 0.0001(16) C49 0.032(2) 0.034(2) 0.0245(17) 0.0023(15) -0.0129(15) -0.0031(16) O14 0.0267(14) 0.0477(18) 0.0300(14) 0.0107(12) -0.0124(11) -0.0123(13) C50 0.039(2) 0.028(2) 0.040(2) -0.0009(16) -0.0254(18) 0.0027(17) O15 0.0422(17) 0.0324(16) 0.0447(17) -0.0053(13) -0.0286(14) 0.0080(13) Cl2 0.0230(4) 0.0362(5) 0.0251(4) 0.0050(3) -0.0111(3) -0.0086(4) Cl3 0.0239(6) 0.0345(6) 0.0424(6) 0.0126(5) -0.0101(5) -0.0059(5) O1S 0.106(3) 0.067(3) 0.071(2) 0.048(2) -0.058(2) -0.050(2) C1S 0.166(7) 0.042(3) 0.107(5) 0.031(3) -0.100(5) -0.037(4) _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 Mn1 3.0843(7) . ? Ni1 Mn1 3.0177(7) 2_665 ? Ni1 O1 1.977(2) . ? Ni1 N1 1.956(3) . ? Ni1 O2 2.059(2) . ? Ni1 O5 2.040(2) . ? Ni1 O5 2.114(2) 2_665 ? Ni1 O6 2.092(3) . ? Mn1 Ni1 3.0176(7) 2_665 ? Mn1 O1 2.194(2) . ? Mn1 O2 1.916(2) 2_665 ? Mn1 O3 2.383(3) 2_665 ? Mn1 O4 1.857(2) . ? Mn1 N2 1.979(3) . ? Mn1 O5 1.945(2) . ? O1 C1 1.328(4) . ? C1 C2 1.406(4) . ? C1 C6 1.425(5) . ? C2 H2A 0.9500 . ? C2 C3 1.381(5) . ? C3 H3A 0.9500 . ? C3 C4 1.396(5) . ? C4 H4A 0.9500 . ? C4 C5 1.380(5) . ? C5 H5A 0.9500 . ? C5 C6 1.407(5) . ? C6 C7 1.466(4) . ? C7 H7A 0.9500 . ? C7 N1 1.272(4) . ? N1 C8 1.482(4) . ? C8 H8A 1.0000 . ? C8 C9 1.545(5) . ? C8 C10 1.521(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 O2 1.422(4) . ? O2 Mn1 1.915(2) 2_665 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 O3 1.436(4) . ? O3 Mn1 2.383(3) 2_665 ? O3 H3O 0.839(10) . ? O4 C11 1.338(4) . ? C11 C12 1.407(5) . ? C11 C16 1.422(5) . ? C12 H12A 0.9500 . ? C12 C13 1.376(5) . ? C13 H13A 0.9500 . ? C13 C14 1.391(6) . ? C14 H14A 0.9500 . ? C14 C15 1.375(6) . ? C15 H15A 0.9500 . ? C15 C16 1.413(5) . ? C16 C17 1.428(5) . ? C17 H17A 0.9500 . ? C17 N2 1.300(4) . ? N2 C18 1.501(4) . ? C18 H18A 1.0000 . ? C18 C19 1.505(5) . ? C18 C20 1.533(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 O6 1.438(4) . ? O5 Ni1 2.114(2) 2_665 ? O5 C20 1.445(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O6 H6O 0.839(10) . ? Ni2 Mn2 3.0289(7) . ? Ni2 O7 1.991(2) . ? Ni2 N3 1.959(3) . ? Ni2 O8 2.085(2) . ? Ni2 O11 2.111(2) . ? Ni2 O11 2.046(2) 2_756 ? Ni2 O12 2.075(2) 2_756 ? Mn2 O7 2.212(2) 2_756 ? Mn2 O8 1.918(2) . ? Mn2 O9 2.302(2) . ? Mn2 O10 1.877(2) . ? Mn2 N4 1.990(3) . ? Mn2 O11 1.948(2) . ? O7 Mn2 2.212(2) 2_756 ? O7 C21 1.318(4) . ? C21 C22 1.420(4) . ? C21 C26 1.432(5) . ? C22 H22A 0.9500 . ? C22 C23 1.380(5) . ? C23 H23A 0.9500 . ? C23 C24 1.405(5) . ? C24 H24A 0.9500 . ? C24 C25 1.373(5) . ? C25 H25A 0.9500 . ? C25 C26 1.406(5) . ? C26 C27 1.453(5) . ? C27 H27A 0.9500 . ? C27 N3 1.290(4) . ? N3 C28 1.481(4) . ? C28 H28A 1.0000 . ? C28 C29 1.541(5) . ? C28 C30 1.520(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 O8 1.433(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C30 O9 1.432(4) . ? O9 H9O 0.835(10) . ? O10 C31 1.335(4) . ? C31 C32 1.403(5) . ? C31 C36 1.422(5) . ? C32 H32A 0.9500 . ? C32 C33 1.385(5) . ? C33 H33A 0.9500 . ? C33 C34 1.388(5) . ? C34 H34A 0.9500 . ? C34 C35 1.379(5) . ? C35 H35A 0.9500 . ? C35 C36 1.409(5) . ? C36 C37 1.438(5) . ? C37 H37A 0.9500 . ? C37 N4 1.282(4) . ? N4 C38 1.492(4) . ? C38 H38A 1.0000 . ? C38 C39 1.536(5) . ? C38 C40 1.511(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 O11 1.438(4) . ? O11 Ni2 2.046(2) 2_756 ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 O12 1.433(4) . ? O12 Ni2 2.075(2) 2_756 ? O12 H12O 0.841(10) . ? Ni3 Cl1 2.4951(9) . ? Ni3 O1W 2.110(3) . ? Ni3 O13 2.026(2) . ? Ni3 O13 2.049(2) 2_675 ? Ni3 N5 2.009(3) . ? Ni3 O14 2.139(3) . ? O1W H1WA 0.840(10) . ? O1W H1WB 0.843(10) . ? O13 Ni3 2.048(2) 2_675 ? O13 C41 1.326(4) . ? C41 C42 1.403(5) . ? C41 C46 1.430(5) . ? C42 H42A 0.9500 . ? C42 C43 1.387(5) . ? C43 H43A 0.9500 . ? C43 C44 1.382(6) . ? C44 H44A 0.9500 . ? C44 C45 1.377(6) . ? C45 H45A 0.9500 . ? C45 C46 1.422(5) . ? C46 C47 1.431(5) . ? C47 H47A 0.9500 . ? C47 N5 1.289(5) . ? N5 C48 1.467(4) . ? C48 H48A 1.0000 . ? C48 C49 1.520(6) . ? C48 C50 1.533(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 O14 1.439(4) . ? O14 H14O 0.843(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 O15 1.421(5) . ? O15 H15O 0.841(10) . ? O1S H1S 0.8400 . ? O1S C1S 1.446(7) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 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 Mn1 Ni1 Mn1 118.271(17) . 2_665 ? Mn1 Ni1 O1 45.12(7) . . ? Mn1 Ni1 O1 132.21(7) 2_665 . ? Mn1 Ni1 N1 140.01(8) . . ? Mn1 Ni1 N1 90.49(8) 2_665 . ? Mn1 Ni1 O2 136.26(7) . . ? Mn1 Ni1 O2 38.86(6) 2_665 . ? Mn1 Ni1 O5 38.19(6) . . ? Mn1 Ni1 O5 91.85(6) 2_665 . ? Mn1 Ni1 O5 39.87(6) 2_665 2_665 ? Mn1 Ni1 O5 88.61(6) . 2_665 ? Mn1 Ni1 O6 88.74(7) . . ? Mn1 Ni1 O6 135.55(7) 2_665 . ? O1 Ni1 N1 95.16(10) . . ? O1 Ni1 O2 170.77(10) . . ? O1 Ni1 O5 83.17(9) . . ? O1 Ni1 O5 92.53(9) . 2_665 ? O1 Ni1 O6 92.10(10) . . ? N1 Ni1 O2 83.64(10) . . ? N1 Ni1 O5 177.66(10) . . ? N1 Ni1 O5 99.53(10) . 2_665 ? N1 Ni1 O6 88.38(11) . . ? O2 Ni1 O5 98.27(9) . . ? O2 Ni1 O5 78.69(9) . 2_665 ? O2 Ni1 O6 97.00(9) . . ? O5 Ni1 O5 82.20(9) . 2_665 ? O5 Ni1 O6 90.05(9) . . ? O5 Ni1 O6 170.43(10) 2_665 . ? Ni1 Mn1 Ni1 61.728(17) . 2_665 ? Ni1 Mn1 O1 39.67(6) . . ? Ni1 Mn1 O1 86.53(6) 2_665 . ? Ni1 Mn1 O2 42.42(6) 2_665 2_665 ? Ni1 Mn1 O2 91.75(7) . 2_665 ? Ni1 Mn1 O3 85.93(6) 2_665 2_665 ? Ni1 Mn1 O3 130.24(6) . 2_665 ? Ni1 Mn1 O4 138.72(8) . . ? Ni1 Mn1 O4 141.00(8) 2_665 . ? Ni1 Mn1 N2 86.73(8) . . ? Ni1 Mn1 N2 124.03(8) 2_665 . ? Ni1 Mn1 O5 40.42(7) . . ? Ni1 Mn1 O5 44.17(7) 2_665 . ? O1 Mn1 O2 92.31(9) . 2_665 ? O1 Mn1 O3 169.87(8) . 2_665 ? O1 Mn1 O4 99.75(10) . . ? O1 Mn1 N2 97.20(11) . . ? O1 Mn1 O5 79.96(9) . . ? O2 Mn1 O3 86.68(9) 2_665 2_665 ? O2 Mn1 O4 98.64(10) 2_665 . ? O2 Mn1 N2 163.03(11) 2_665 . ? O2 Mn1 O5 86.53(9) 2_665 . ? O3 Mn1 O4 90.37(10) 2_665 . ? O3 Mn1 N2 81.49(10) 2_665 . ? O3 Mn1 O5 89.91(9) 2_665 . ? O4 Mn1 N2 93.57(11) . . ? O4 Mn1 O5 174.83(10) . . ? N2 Mn1 O5 81.36(10) . . ? Ni1 O1 Mn1 95.21(9) . . ? Ni1 O1 C1 124.6(2) . . ? Mn1 O1 C1 140.0(2) . . ? O1 C1 C2 119.8(3) . . ? O1 C1 C6 122.6(3) . . ? C2 C1 C6 117.6(3) . . ? C1 C2 H2A 119.0 . . ? C1 C2 C3 121.9(3) . . ? H2A C2 C3 119.0 . . ? C2 C3 H3A 119.7 . . ? C2 C3 C4 120.6(3) . . ? H3A C3 C4 119.7 . . ? C3 C4 H4A 120.8 . . ? C3 C4 C5 118.4(3) . . ? H4A C4 C5 120.8 . . ? C4 C5 H5A 118.8 . . ? C4 C5 C6 122.4(3) . . ? H5A C5 C6 118.8 . . ? C1 C6 C5 118.9(3) . . ? C1 C6 C7 125.3(3) . . ? C5 C6 C7 115.6(3) . . ? C6 C7 H7A 117.0 . . ? C6 C7 N1 125.9(3) . . ? H7A C7 N1 117.0 . . ? Ni1 N1 C7 124.2(2) . . ? Ni1 N1 C8 114.7(2) . . ? C7 N1 C8 121.0(3) . . ? N1 C8 H8A 108.6 . . ? N1 C8 C9 108.0(3) . . ? N1 C8 C10 110.8(3) . . ? H8A C8 C9 108.6 . . ? H8A C8 C10 108.6 . . ? C9 C8 C10 112.0(3) . . ? C8 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C8 C9 O2 112.0(3) . . ? H9A C9 H9B 107.9 . . ? H9A C9 O2 109.2 . . ? H9B C9 O2 109.2 . . ? Ni1 O2 Mn1 98.73(10) . 2_665 ? Ni1 O2 C9 106.33(18) . . ? Mn1 O2 C9 122.0(2) 2_665 . ? C8 C10 H10A 109.7 . . ? C8 C10 H10B 109.7 . . ? C8 C10 O3 109.8(3) . . ? H10A C10 H10B 108.2 . . ? H10A C10 O3 109.7 . . ? H10B C10 O3 109.7 . . ? Mn1 O3 C10 127.2(2) 2_665 . ? Mn1 O3 H3O 124(6) 2_665 . ? C10 O3 H3O 109(6) . . ? Mn1 O4 C11 128.5(2) . . ? O4 C11 C12 117.5(3) . . ? O4 C11 C16 123.9(3) . . ? C12 C11 C16 118.6(3) . . ? C11 C12 H12A 119.8 . . ? C11 C12 C13 120.4(4) . . ? H12A C12 C13 119.8 . . ? C12 C13 H13A 119.4 . . ? C12 C13 C14 121.2(4) . . ? H13A C13 C14 119.4 . . ? C13 C14 H14A 120.0 . . ? C13 C14 C15 120.0(4) . . ? H14A C14 C15 120.0 . . ? C14 C15 H15A 119.8 . . ? C14 C15 C16 120.3(4) . . ? H15A C15 C16 119.8 . . ? C11 C16 C15 119.5(3) . . ? C11 C16 C17 123.3(3) . . ? C15 C16 C17 117.2(3) . . ? C16 C17 H17A 117.3 . . ? C16 C17 N2 125.3(3) . . ? H17A C17 N2 117.3 . . ? Mn1 N2 C17 125.3(2) . . ? Mn1 N2 C18 115.6(2) . . ? C17 N2 C18 119.0(3) . . ? N2 C18 H18A 108.5 . . ? N2 C18 C19 111.6(3) . . ? N2 C18 C20 106.1(3) . . ? H18A C18 C19 108.5 . . ? H18A C18 C20 108.5 . . ? C19 C18 C20 113.5(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 O6 110.7(3) . . ? H19A C19 H19B 108.1 . . ? H19A C19 O6 109.5 . . ? H19B C19 O6 109.5 . . ? Ni1 O5 Ni1 97.80(9) . 2_665 ? Ni1 O5 Mn1 101.39(10) . . ? Ni1 O5 Mn1 95.96(10) 2_665 . ? Ni1 O5 C20 114.48(19) . . ? Ni1 O5 C20 129.71(19) 2_665 . ? Mn1 O5 C20 112.87(18) . . ? C18 C20 O5 107.9(3) . . ? C18 C20 H20A 110.1 . . ? C18 C20 H20B 110.1 . . ? O5 C20 H20A 110.1 . . ? O5 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? Ni1 O6 C19 130.4(2) . . ? Ni1 O6 H6O 112(6) . . ? C19 O6 H6O 115(6) . . ? Mn2 Ni2 O7 131.71(7) . . ? Mn2 Ni2 N3 88.38(8) . . ? Mn2 Ni2 O8 38.81(6) . . ? Mn2 Ni2 O11 39.72(6) . . ? Mn2 Ni2 O11 93.22(6) . 2_756 ? Mn2 Ni2 O12 135.64(7) . 2_756 ? O7 Ni2 N3 95.49(10) . . ? O7 Ni2 O8 170.26(9) . . ? O7 Ni2 O11 92.24(9) . . ? O7 Ni2 O11 81.89(9) . 2_756 ? O7 Ni2 O12 92.53(9) . 2_756 ? N3 Ni2 O8 82.95(10) . . ? N3 Ni2 O11 97.29(10) . . ? N3 Ni2 O11 177.37(10) . 2_756 ? N3 Ni2 O12 90.58(10) . 2_756 ? O8 Ni2 O11 78.47(8) . . ? O8 Ni2 O11 99.60(9) . 2_756 ? O8 Ni2 O12 97.10(9) . 2_756 ? O11 Ni2 O11 82.65(9) . 2_756 ? O11 Ni2 O12 89.74(9) 2_756 2_756 ? O11 Ni2 O12 170.37(9) . 2_756 ? Ni2 Mn2 O7 84.93(6) . 2_756 ? Ni2 Mn2 O8 42.95(7) . . ? Ni2 Mn2 O9 87.32(6) . . ? Ni2 Mn2 O10 142.63(7) . . ? Ni2 Mn2 N4 123.92(8) . . ? Ni2 Mn2 O11 43.82(6) . . ? O7 Mn2 O8 90.94(9) 2_756 . ? O7 Mn2 O9 169.65(9) 2_756 . ? O7 Mn2 O10 100.17(9) 2_756 . ? O7 Mn2 N4 96.82(10) 2_756 . ? O7 Mn2 O11 78.68(9) 2_756 . ? O8 Mn2 O9 88.04(9) . . ? O8 Mn2 O10 99.72(10) . . ? O8 Mn2 N4 164.19(11) . . ? O8 Mn2 O11 86.70(9) . . ? O9 Mn2 O10 90.15(10) . . ? O9 Mn2 N4 81.85(10) . . ? O9 Mn2 O11 90.97(9) . . ? O10 Mn2 N4 92.47(10) . . ? O10 Mn2 O11 173.51(10) . . ? N4 Mn2 O11 81.37(10) . . ? Ni2 O7 Mn2 96.00(9) . 2_756 ? Ni2 O7 C21 124.7(2) . . ? Mn2 O7 C21 139.2(2) 2_756 . ? O7 C21 C22 119.4(3) . . ? O7 C21 C26 123.3(3) . . ? C22 C21 C26 117.3(3) . . ? C21 C22 H22A 119.1 . . ? C21 C22 C23 121.9(3) . . ? H22A C22 C23 119.1 . . ? C22 C23 H23A 119.6 . . ? C22 C23 C24 120.7(3) . . ? H23A C23 C24 119.6 . . ? C23 C24 H24A 120.9 . . ? C23 C24 C25 118.2(3) . . ? H24A C24 C25 120.9 . . ? C24 C25 H25A 118.4 . . ? C24 C25 C26 123.1(3) . . ? H25A C25 C26 118.4 . . ? C21 C26 C25 118.7(3) . . ? C21 C26 C27 126.0(3) . . ? C25 C26 C27 115.3(3) . . ? C26 C27 H27A 116.9 . . ? C26 C27 N3 126.2(3) . . ? H27A C27 N3 116.9 . . ? Ni2 N3 C27 123.9(2) . . ? Ni2 N3 C28 115.8(2) . . ? C27 N3 C28 120.3(3) . . ? N3 C28 H28A 108.8 . . ? N3 C28 C29 107.7(3) . . ? N3 C28 C30 111.2(3) . . ? H28A C28 C29 108.8 . . ? H28A C28 C30 108.8 . . ? C29 C28 C30 111.4(3) . . ? C28 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? C28 C29 O8 112.6(3) . . ? H29A C29 H29B 107.8 . . ? H29A C29 O8 109.1 . . ? H29B C29 O8 109.1 . . ? Ni2 O8 Mn2 98.24(10) . . ? Ni2 O8 C29 105.72(18) . . ? Mn2 O8 C29 120.29(19) . . ? C28 C30 H30A 109.9 . . ? C28 C30 H30B 109.9 . . ? C28 C30 O9 109.0(3) . . ? H30A C30 H30B 108.3 . . ? H30A C30 O9 109.9 . . ? H30B C30 O9 109.9 . . ? Mn2 O9 C30 129.0(2) . . ? Mn2 O9 H9O 116(6) . . ? C30 O9 H9O 106(6) . . ? Mn2 O10 C31 129.1(2) . . ? O10 C31 C32 118.3(3) . . ? O10 C31 C36 123.5(3) . . ? C32 C31 C36 118.2(3) . . ? C31 C32 H32A 119.6 . . ? C31 C32 C33 120.8(3) . . ? H32A C32 C33 119.6 . . ? C32 C33 H33A 119.3 . . ? C32 C33 C34 121.4(3) . . ? H33A C33 C34 119.3 . . ? C33 C34 H34A 120.6 . . ? C33 C34 C35 118.8(3) . . ? H34A C34 C35 120.6 . . ? C34 C35 H35A 119.2 . . ? C34 C35 C36 121.6(3) . . ? H35A C35 C36 119.2 . . ? C31 C36 C35 119.3(3) . . ? C31 C36 C37 123.4(3) . . ? C35 C36 C37 117.3(3) . . ? C36 C37 H37A 117.5 . . ? C36 C37 N4 125.1(3) . . ? H37A C37 N4 117.5 . . ? Mn2 N4 C37 126.3(2) . . ? Mn2 N4 C38 114.8(2) . . ? C37 N4 C38 118.9(3) . . ? N4 C38 H38A 108.4 . . ? N4 C38 C39 106.6(2) . . ? N4 C38 C40 111.3(3) . . ? H38A C38 C39 108.4 . . ? H38A C38 C40 108.4 . . ? C39 C38 C40 113.7(3) . . ? C38 C39 H39A 110.2 . . ? C38 C39 H39B 110.2 . . ? C38 C39 O11 107.5(2) . . ? H39A C39 H39B 108.5 . . ? H39A C39 O11 110.2 . . ? H39B C39 O11 110.2 . . ? Ni2 O11 Ni2 97.35(9) . 2_756 ? Ni2 O11 Mn2 96.46(9) . . ? Ni2 O11 Mn2 103.05(10) 2_756 . ? Ni2 O11 C39 128.99(19) . . ? Ni2 O11 C39 114.84(19) 2_756 . ? Mn2 O11 C39 112.12(18) . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 O12 110.5(3) . . ? H40A C40 H40B 108.1 . . ? H40A C40 O12 109.5 . . ? H40B C40 O12 109.5 . . ? Ni2 O12 C40 130.9(2) 2_756 . ? Ni2 O12 H12O 118(5) 2_756 . ? C40 O12 H12O 106(5) . . ? Cl1 Ni3 O1W 170.20(7) . . ? Cl1 Ni3 O13 95.47(7) . . ? Cl1 Ni3 O13 89.35(7) . 2_675 ? Cl1 Ni3 N5 96.42(8) . . ? Cl1 Ni3 O14 88.49(8) . . ? O1W Ni3 O13 90.49(10) . . ? O1W Ni3 O13 84.03(9) . 2_675 ? O1W Ni3 N5 91.33(10) . . ? O1W Ni3 O14 86.81(11) . . ? O13 Ni3 O13 80.00(9) . 2_675 ? O13 Ni3 N5 90.02(11) . . ? O13 Ni3 N5 168.93(11) 2_675 . ? O13 Ni3 O14 170.56(9) . . ? O13 Ni3 O14 108.66(10) 2_675 . ? N5 Ni3 O14 81.01(11) . . ? Ni3 O1W H1WA 109(3) . . ? Ni3 O1W H1WB 110(3) . . ? H1WA O1W H1WB 99(4) . . ? Ni3 O13 Ni3 100.00(9) . 2_675 ? Ni3 O13 C41 128.3(2) . . ? Ni3 O13 C41 131.4(2) 2_675 . ? O13 C41 C42 120.1(3) . . ? O13 C41 C46 122.5(3) . . ? C42 C41 C46 117.4(3) . . ? C41 C42 H42A 118.8 . . ? C41 C42 C43 122.3(4) . . ? H42A C42 C43 118.8 . . ? C42 C43 H43A 119.6 . . ? C42 C43 C44 120.8(4) . . ? H43A C43 C44 119.6 . . ? C43 C44 H44A 120.8 . . ? C43 C44 C45 118.4(3) . . ? H44A C44 C45 120.8 . . ? C44 C45 H45A 118.6 . . ? C44 C45 C46 122.8(3) . . ? H45A C45 C46 118.6 . . ? C41 C46 C45 118.2(3) . . ? C41 C46 C47 124.7(3) . . ? C45 C46 C47 117.1(3) . . ? C46 C47 H47A 116.6 . . ? C46 C47 N5 126.7(3) . . ? H47A C47 N5 116.6 . . ? Ni3 N5 C47 126.8(2) . . ? Ni3 N5 C48 114.7(2) . . ? C47 N5 C48 118.3(3) . . ? N5 C48 H48A 110.1 . . ? N5 C48 C49 108.4(3) . . ? N5 C48 C50 105.2(3) . . ? H48A C48 C49 110.1 . . ? H48A C48 C50 110.1 . . ? C49 C48 C50 112.8(3) . . ? C48 C49 H49A 109.8 . . ? C48 C49 H49B 109.8 . . ? C48 C49 O14 109.5(3) . . ? H49A C49 H49B 108.2 . . ? H49A C49 O14 109.8 . . ? H49B C49 O14 109.8 . . ? Ni3 O14 C49 107.0(2) . . ? Ni3 O14 H14O 114(6) . . ? C49 O14 H14O 115(6) . . ? C48 C50 H50A 109.3 . . ? C48 C50 H50B 109.3 . . ? C48 C50 O15 111.5(3) . . ? H50A C50 H50B 108.0 . . ? H50A C50 O15 109.3 . . ? H50B C50 O15 109.3 . . ? C50 O15 H15O 98(6) . . ? H1S O1S C1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA Cl2 0.840(10) 2.322(19) 3.116(2) 158(4) 1_465 O1W H1WB Cl1 0.843(10) 2.361(16) 3.173(3) 162(4) 2_675 O1S H1S Cl3' 0.84 1.95 2.737(6) 155.0 2_765 O1S H1S Cl3 0.84 2.43 3.258(4) 169.1 2_765 O3 H3O Cl1 0.839(10) 2.43(3) 3.236(3) 162(7) . O6 H6O Cl3' 0.839(10) 2.08(3) 2.879(6) 159(7) 2_765 O6 H6O Cl3 0.839(10) 2.29(3) 3.084(3) 159(8) 2_765 O9 H9O O1S 0.835(10) 1.818(16) 2.647(4) 172(8) . O12 H12O Cl2 0.841(10) 2.15(2) 2.970(3) 165(7) . O14 H14O Cl3 0.843(10) 2.49(4) 3.268(3) 153(7) . O15 H15O Cl3 0.841(10) 2.26(3) 3.062(3) 159(8) . O15 H15O Cl3' 0.841(10) 2.89(5) 3.609(6) 145(7) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.65 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.171 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.090