# 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 _publ_contact_author_name 'Kou, Hui-Zhong' _publ_contact_author_email kouhz@mail.tsinghua.edu.cn _publ_section_title ; Ferromagnetic coupling in oximato-bridged multi-decker NiII clusters ; loop_ _publ_author_name 'Hui-Zhong Kou' 'Bingwu Wang' 'Ai-Li Cui' # Attachment '- dalton-sub.cif' #=================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 770171' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 Cl2 N16 Ni4 O12' _chemical_formula_weight 1292.68 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.586(2) _cell_length_b 10.925(2) _cell_length_c 11.471(2) _cell_angle_alpha 90.07(3) _cell_angle_beta 99.39(3) _cell_angle_gamma 103.55(3) _cell_volume 1271.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4461 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.47 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12573 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5769 _reflns_number_gt 4461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0518P)^2^+0.3856P] 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 5769 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.45461(3) 0.99927(3) 0.16503(3) 0.03413(11) Uani 1 1 d . . . Ni2 Ni 0.39021(3) 1.26960(3) 0.07340(3) 0.03484(11) Uani 1 1 d . . . Cl1 Cl 0.81851(8) 0.60333(7) 0.35080(7) 0.05133(19) Uani 1 1 d . . . O1 O 0.40981(19) 1.11964(19) 0.27785(16) 0.0422(4) Uani 1 1 d . . . O2 O 0.46256(18) 1.13828(18) 0.04605(16) 0.0381(4) Uani 1 1 d . . . N1 N 0.2962(2) 1.3887(2) 0.1077(2) 0.0406(5) Uani 1 1 d . . . N2 N 0.3623(2) 1.2124(2) 0.2220(2) 0.0387(5) Uani 1 1 d . . . N3 N 0.2628(3) 1.2346(3) 0.3857(2) 0.0562(7) Uani 1 1 d . . . H3B H 0.2900 1.1732 0.4197 0.067 Uiso 1 1 calc R . . H3C H 0.2166 1.2741 0.4198 0.067 Uiso 1 1 calc R . . N6 N 0.4298(2) 1.3197(2) -0.0720(2) 0.0423(5) Uani 1 1 d . . . H6 H 0.4158 1.3875 -0.1041 0.051 Uiso 1 1 calc R . . N8 N 0.6605(2) 1.0741(2) 0.2493(2) 0.0402(5) Uani 1 1 d . . . C1 C 0.2628(3) 1.4795(3) 0.0387(3) 0.0504(7) Uani 1 1 d . . . H1 H 0.2958 1.4942 -0.0316 0.061 Uiso 1 1 calc R . . C2 C 0.1811(3) 1.5517(3) 0.0690(3) 0.0605(9) Uani 1 1 d . . . H2 H 0.1598 1.6138 0.0195 0.073 Uiso 1 1 calc R . . C3 C 0.1318(3) 1.5313(3) 0.1719(3) 0.0621(9) Uani 1 1 d . . . H3A H 0.0760 1.5790 0.1925 0.074 Uiso 1 1 calc R . . C4 C 0.1653(3) 1.4395(3) 0.2455(3) 0.0533(8) Uani 1 1 d . . . H4 H 0.1330 1.4250 0.3162 0.064 Uiso 1 1 calc R . . C5 C 0.2484(3) 1.3692(3) 0.2117(3) 0.0415(6) Uani 1 1 d . . . C6 C 0.2928(3) 1.2692(3) 0.2774(3) 0.0412(6) Uani 1 1 d . . . O3 O 0.8073(3) 0.7312(2) 0.3449(3) 0.0871(9) Uani 1 1 d . . . C18 C 0.7380(3) 1.0013(3) 0.2993(3) 0.0550(8) Uani 1 1 d . . . H18 H 0.7096 0.9147 0.2841 0.066 Uiso 1 1 calc R . . O6 O 0.7791(4) 0.5557(3) 0.4556(3) 0.1010(11) Uani 1 1 d . . . C19 C 0.8568(3) 1.0463(4) 0.3715(4) 0.0724(11) Uani 1 1 d . . . H19 H 0.9059 0.9913 0.4054 0.087 Uiso 1 1 calc R . . C22 C 0.7081(3) 1.1979(3) 0.2680(3) 0.0492(7) Uani 1 1 d . . . H22 H 0.6583 1.2512 0.2313 0.059 Uiso 1 1 calc R . . C21 C 0.8273(3) 1.2520(3) 0.3386(4) 0.0674(10) Uani 1 1 d . . . H21 H 0.8562 1.3391 0.3492 0.081 Uiso 1 1 calc R . . C20 C 0.9021(4) 1.1742(4) 0.3930(4) 0.0753(12) Uani 1 1 d . . . H20 H 0.9814 1.2073 0.4430 0.090 Uiso 1 1 calc R . . O5 O 0.7372(4) 0.5304(3) 0.2545(3) 0.1301(16) Uani 1 1 d . . . C17 C 0.1975(3) 0.8995(3) -0.0049(3) 0.0537(8) Uani 1 1 d . . . H17 H 0.2552 0.9092 -0.0590 0.064 Uiso 1 1 calc R . . C13 C 0.1606(3) 0.9159(3) 0.1832(3) 0.0573(8) Uani 1 1 d . . . H13 H 0.1925 0.9390 0.2625 0.069 Uiso 1 1 calc R . . C14 C 0.0285(3) 0.8667(4) 0.1500(4) 0.0723(11) Uani 1 1 d . . . H14 H -0.0274 0.8553 0.2059 0.087 Uiso 1 1 calc R . . O4 O 0.9500(3) 0.5956(4) 0.3545(4) 0.1276(14) Uani 1 1 d . . . C16 C 0.0661(4) 0.8519(4) -0.0446(4) 0.0775(12) Uani 1 1 d . . . H16 H 0.0357 0.8315 -0.1246 0.093 Uiso 1 1 calc R . . C15 C -0.0204(4) 0.8343(4) 0.0336(5) 0.0787(13) Uani 1 1 d . . . H15 H -0.1100 0.8012 0.0083 0.094 Uiso 1 1 calc R . . N7 N 0.2462(2) 0.9326(2) 0.1080(2) 0.0414(5) Uani 1 1 d . . . C11 C 0.5218(2) 1.2500(2) -0.2399(2) 0.0369(6) Uani 1 1 d . . . C12 C 0.4830(2) 1.2377(2) -0.1215(2) 0.0349(5) Uani 1 1 d . . . C10 C 0.5254(3) 1.3562(3) -0.3043(3) 0.0464(7) Uani 1 1 d . . . H10 H 0.5037 1.4261 -0.2740 0.056 Uiso 1 1 calc R . . C8 C 0.5923(3) 1.2524(4) -0.4575(3) 0.0613(9) Uani 1 1 d . . . H8 H 0.6167 1.2512 -0.5317 0.074 Uiso 1 1 calc R . . C7 C 0.5861(3) 1.1489(3) -0.3890(3) 0.0525(8) Uani 1 1 d . . . H7 H 0.6054 1.0775 -0.4190 0.063 Uiso 1 1 calc R . . C9 C 0.5619(3) 1.3579(3) -0.4150(3) 0.0578(8) Uani 1 1 d . . . H9 H 0.5657 1.4291 -0.4599 0.069 Uiso 1 1 calc R . . N5 N 0.5040(2) 1.1384(2) -0.06469(19) 0.0341(5) Uani 1 1 d . . . N4 N 0.5535(2) 1.1461(2) -0.2810(2) 0.0397(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03616(19) 0.03548(19) 0.03451(19) -0.00050(14) 0.00903(14) 0.01383(14) Ni2 0.03507(19) 0.03348(19) 0.0393(2) -0.00310(14) 0.00774(14) 0.01369(14) Cl1 0.0671(5) 0.0500(4) 0.0478(4) 0.0068(3) 0.0198(3) 0.0286(4) O1 0.0503(11) 0.0490(11) 0.0353(10) 0.0010(8) 0.0100(8) 0.0256(9) O2 0.0489(10) 0.0415(10) 0.0329(9) 0.0030(8) 0.0160(8) 0.0224(8) N1 0.0392(12) 0.0368(12) 0.0471(13) -0.0043(10) 0.0047(10) 0.0137(10) N2 0.0374(12) 0.0404(12) 0.0406(12) -0.0071(10) 0.0072(10) 0.0137(10) N3 0.0675(17) 0.0693(18) 0.0456(14) 0.0012(13) 0.0236(13) 0.0341(14) N6 0.0505(13) 0.0343(12) 0.0475(14) 0.0027(10) 0.0123(11) 0.0179(10) N8 0.0422(12) 0.0381(12) 0.0415(12) -0.0057(10) 0.0062(10) 0.0121(10) C1 0.0527(17) 0.0440(16) 0.0583(19) -0.0045(14) 0.0081(14) 0.0197(14) C2 0.064(2) 0.0505(19) 0.074(2) -0.0012(17) 0.0046(18) 0.0312(16) C3 0.0547(19) 0.062(2) 0.080(2) -0.0071(19) 0.0129(17) 0.0339(16) C4 0.0467(17) 0.0547(19) 0.064(2) -0.0105(16) 0.0156(15) 0.0194(14) C5 0.0330(13) 0.0411(15) 0.0503(16) -0.0099(13) 0.0039(12) 0.0107(11) C6 0.0345(13) 0.0444(15) 0.0461(16) -0.0110(13) 0.0085(12) 0.0108(11) O3 0.105(2) 0.0461(14) 0.122(3) 0.0174(15) 0.0312(19) 0.0321(14) C18 0.0465(17) 0.0420(16) 0.073(2) 0.0011(15) -0.0036(15) 0.0131(13) O6 0.171(3) 0.080(2) 0.0739(19) 0.0228(16) 0.067(2) 0.042(2) C19 0.0479(19) 0.062(2) 0.098(3) 0.004(2) -0.0172(19) 0.0150(17) C22 0.0446(16) 0.0401(15) 0.066(2) -0.0029(14) 0.0137(14) 0.0129(13) C21 0.0534(19) 0.0394(17) 0.107(3) -0.0190(19) 0.015(2) 0.0043(15) C20 0.0464(19) 0.070(2) 0.096(3) -0.023(2) -0.0153(19) 0.0054(18) O5 0.207(4) 0.100(2) 0.082(2) -0.0362(19) -0.054(2) 0.088(3) C17 0.0503(18) 0.062(2) 0.0488(18) -0.0071(15) 0.0043(14) 0.0160(15) C13 0.0448(17) 0.071(2) 0.060(2) 0.0058(17) 0.0203(15) 0.0133(15) C14 0.0470(19) 0.068(2) 0.106(3) 0.007(2) 0.029(2) 0.0106(17) O4 0.087(2) 0.124(3) 0.198(4) 0.008(3) 0.064(3) 0.050(2) C16 0.060(2) 0.083(3) 0.081(3) -0.029(2) -0.015(2) 0.018(2) C15 0.0416(19) 0.059(2) 0.125(4) -0.025(2) 0.000(2) 0.0008(16) N7 0.0395(12) 0.0430(13) 0.0441(13) 0.0009(10) 0.0103(10) 0.0124(10) C11 0.0337(13) 0.0361(13) 0.0374(14) 0.0008(11) 0.0041(11) 0.0028(11) C12 0.0336(13) 0.0294(12) 0.0407(14) -0.0036(11) 0.0052(11) 0.0063(10) C10 0.0479(16) 0.0412(15) 0.0471(16) 0.0074(13) 0.0061(13) 0.0060(13) C8 0.063(2) 0.084(3) 0.0406(17) 0.0189(17) 0.0194(15) 0.0183(18) C7 0.0570(18) 0.064(2) 0.0416(16) 0.0019(15) 0.0151(14) 0.0203(15) C9 0.063(2) 0.058(2) 0.0532(19) 0.0194(16) 0.0132(16) 0.0125(16) N5 0.0376(11) 0.0343(11) 0.0332(11) 0.0004(9) 0.0092(9) 0.0117(9) N4 0.0389(12) 0.0442(13) 0.0383(12) 0.0010(10) 0.0090(9) 0.0126(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 O1 2.029(2) . ? Ni1 O2 2.0393(19) . ? Ni1 N5 2.061(2) 2_675 ? Ni1 N4 2.068(2) 2_675 ? Ni1 N7 2.145(2) . ? Ni1 N8 2.197(2) . ? Ni2 O2 1.8264(19) . ? Ni2 N6 1.839(2) . ? Ni2 N2 1.862(2) . ? Ni2 N1 1.889(2) . ? Cl1 O6 1.398(3) . ? Cl1 O5 1.401(3) . ? Cl1 O4 1.408(3) . ? Cl1 O3 1.430(3) . ? O1 N2 1.351(3) . ? O2 N5 1.410(3) . ? N1 C1 1.346(4) . ? N1 C5 1.368(4) . ? N2 C6 1.302(3) . ? N3 C6 1.364(4) . ? N3 H3B 0.8600 . ? N3 H3C 0.8600 . ? N6 C12 1.335(3) . ? N6 H6 0.8600 . ? N8 C22 1.333(4) . ? N8 C18 1.337(4) . ? C1 C2 1.381(4) . ? C1 H1 0.9300 . ? C2 C3 1.365(5) . ? C2 H2 0.9300 . ? C3 C4 1.384(5) . ? C3 H3A 0.9300 . ? C4 C5 1.393(4) . ? C4 H4 0.9300 . ? C5 C6 1.453(4) . ? C18 C19 1.370(4) . ? C18 H18 0.9300 . ? C19 C20 1.374(5) . ? C19 H19 0.9300 . ? C22 C21 1.383(5) . ? C22 H22 0.9300 . ? C21 C20 1.377(5) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? C17 N7 1.329(4) . ? C17 C16 1.366(5) . ? C17 H17 0.9300 . ? C13 N7 1.334(4) . ? C13 C14 1.364(5) . ? C13 H13 0.9300 . ? C14 C15 1.365(6) . ? C14 H14 0.9300 . ? C16 C15 1.366(6) . ? C16 H16 0.9300 . ? C15 H15 0.9300 . ? C11 N4 1.361(4) . ? C11 C10 1.373(4) . ? C11 C12 1.479(4) . ? C12 N5 1.311(3) . ? C10 C9 1.385(4) . ? C10 H10 0.9300 . ? C8 C7 1.373(5) . ? C8 C9 1.376(5) . ? C8 H8 0.9300 . ? C7 N4 1.338(4) . ? C7 H7 0.9300 . ? C9 H9 0.9300 . ? N5 Ni1 2.061(2) 2_675 ? N4 Ni1 2.068(2) 2_675 ? 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 Ni1 O2 87.09(8) . . ? O1 Ni1 N5 173.43(8) . 2_675 ? O2 Ni1 N5 99.44(8) . 2_675 ? O1 Ni1 N4 94.85(9) . 2_675 ? O2 Ni1 N4 178.01(8) . 2_675 ? N5 Ni1 N4 78.62(9) 2_675 2_675 ? O1 Ni1 N7 86.62(9) . . ? O2 Ni1 N7 91.08(9) . . ? N5 Ni1 N7 92.46(9) 2_675 . ? N4 Ni1 N7 88.59(9) 2_675 . ? O1 Ni1 N8 85.85(9) . . ? O2 Ni1 N8 92.74(9) . . ? N5 Ni1 N8 94.54(9) 2_675 . ? N4 Ni1 N8 87.86(9) 2_675 . ? N7 Ni1 N8 171.37(9) . . ? O2 Ni2 N6 84.39(9) . . ? O2 Ni2 N2 91.30(9) . . ? N6 Ni2 N2 175.09(10) . . ? O2 Ni2 N1 172.16(9) . . ? N6 Ni2 N1 100.89(11) . . ? N2 Ni2 N1 83.65(10) . . ? O6 Cl1 O5 109.2(3) . . ? O6 Cl1 O4 107.6(2) . . ? O5 Cl1 O4 110.1(3) . . ? O6 Cl1 O3 108.07(19) . . ? O5 Cl1 O3 110.7(2) . . ? O4 Cl1 O3 111.2(2) . . ? N2 O1 Ni1 112.89(15) . . ? N5 O2 Ni2 114.28(15) . . ? N5 O2 Ni1 127.09(15) . . ? Ni2 O2 Ni1 118.15(9) . . ? C1 N1 C5 118.3(2) . . ? C1 N1 Ni2 128.0(2) . . ? C5 N1 Ni2 113.39(18) . . ? C6 N2 O1 117.6(2) . . ? C6 N2 Ni2 116.5(2) . . ? O1 N2 Ni2 125.87(17) . . ? C6 N3 H3B 120.0 . . ? C6 N3 H3C 120.0 . . ? H3B N3 H3C 120.0 . . ? C12 N6 Ni2 111.45(19) . . ? C12 N6 H6 124.3 . . ? Ni2 N6 H6 124.3 . . ? C22 N8 C18 116.0(3) . . ? C22 N8 Ni1 120.1(2) . . ? C18 N8 Ni1 123.2(2) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 112.5(2) . . ? C4 C5 C6 126.0(3) . . ? N2 C6 N3 122.4(3) . . ? N2 C6 C5 113.7(3) . . ? N3 C6 C5 123.9(3) . . ? N8 C18 C19 124.1(3) . . ? N8 C18 H18 118.0 . . ? C19 C18 H18 118.0 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N8 C22 C21 123.9(3) . . ? N8 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? C20 C21 C22 118.6(3) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C19 C20 C21 118.4(3) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? N7 C17 C16 122.7(3) . . ? N7 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? N7 C13 C14 123.5(3) . . ? N7 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C14 C15 C16 118.1(3) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C17 N7 C13 116.9(3) . . ? C17 N7 Ni1 120.6(2) . . ? C13 N7 Ni1 122.4(2) . . ? N4 C11 C10 122.1(3) . . ? N4 C11 C12 114.3(2) . . ? C10 C11 C12 123.6(3) . . ? N5 C12 N6 120.1(2) . . ? N5 C12 C11 115.6(2) . . ? N6 C12 C11 124.2(2) . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C7 C8 C9 119.2(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? N4 C7 C8 122.9(3) . . ? N4 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C12 N5 O2 109.7(2) . . ? C12 N5 Ni1 115.49(18) . 2_675 ? O2 N5 Ni1 132.90(16) . 2_675 ? C7 N4 C11 117.8(3) . . ? C7 N4 Ni1 127.7(2) . 2_675 ? C11 N4 Ni1 114.56(18) . 2_675 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.414 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.076 #===End data_2 _database_code_depnum_ccdc_archive 'CCDC 770172' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Cl2 N16 Ni4 O12' _chemical_formula_weight 1348.78 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' Cl Cl 0.1484 0.1585 '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 11.010(2) _cell_length_b 11.330(2) _cell_length_c 12.912(3) _cell_angle_alpha 90.01(3) _cell_angle_beta 101.31(3) _cell_angle_gamma 107.17(3) _cell_volume 1506.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3066 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 25.00 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11914 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5288 _reflns_number_gt 3066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1458P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.019(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5288 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2779 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 0.95220(10) 0.82520(9) 0.03269(7) 0.0457(4) Uani 1 1 d . . . Ni2 Ni 0.90918(10) 0.94992(9) 0.25300(7) 0.0465(4) Uani 1 1 d . . . Cl1 Cl 0.7881(3) 0.3070(3) 0.48104(19) 0.0827(9) Uani 1 1 d . . . O1 O 0.9168(6) 0.7236(5) 0.1574(4) 0.0525(14) Uani 1 1 d . . . O2 O 1.0419(6) 1.0269(5) -0.1266(4) 0.0517(14) Uani 1 1 d . . . O3 O 0.8029(14) 0.4318(8) 0.5084(7) 0.154(5) Uani 1 1 d . . . O4 O 0.8218(11) 0.2464(7) 0.5717(5) 0.121(3) Uani 1 1 d . . . O5 O 0.8654(13) 0.3011(9) 0.4078(7) 0.147(5) Uani 1 1 d . . . O6 O 0.6630(13) 0.2390(15) 0.4336(10) 0.205(7) Uani 1 1 d . . . N1 N 0.8565(7) 0.9078(6) 0.3819(5) 0.0490(17) Uani 1 1 d . . . N2 N 0.8919(6) 0.7828(6) 0.2393(4) 0.0458(16) Uani 1 1 d . . . N3 N 0.8561(8) 0.5970(6) 0.3218(5) 0.067(2) Uani 1 1 d . . . H3A H 0.8694 0.5600 0.2689 0.080 Uiso 1 1 calc R . . H3B H 0.8376 0.5569 0.3760 0.080 Uiso 1 1 calc R . . N4 N 0.9308(7) 0.6706(6) -0.0650(4) 0.0485(17) Uani 1 1 d . . . N5 N 0.9943(7) 0.9016(6) -0.1029(5) 0.0482(16) Uani 1 1 d . . . N6 N 1.0593(7) 0.8802(6) -0.2593(5) 0.0536(18) Uani 1 1 d . . . H6A H 1.0758 0.8394 -0.3082 0.064 Uiso 1 1 calc R . . N7 N 0.7427(7) 0.7848(6) -0.0261(5) 0.0561(18) Uani 1 1 d . . . N8 N 1.1586(7) 0.8602(6) 0.0948(5) 0.0512(17) Uani 1 1 d . . . C1 C 0.8751(9) 0.5544(7) -0.0469(6) 0.056(2) Uani 1 1 d . . . H1A H 0.8546 0.5372 0.0191 0.068 Uiso 1 1 calc R . . C2 C 0.8459(10) 0.4569(8) -0.1213(7) 0.064(3) Uani 1 1 d . . . H2A H 0.8069 0.3763 -0.1053 0.077 Uiso 1 1 calc R . . C3 C 0.8753(10) 0.4812(8) -0.2188(7) 0.069(3) Uani 1 1 d . . . H3C H 0.8560 0.4178 -0.2707 0.083 Uiso 1 1 calc R . . C4 C 0.9356(10) 0.6050(8) -0.2384(6) 0.059(2) Uani 1 1 d . . . H4A H 0.9584 0.6240 -0.3034 0.071 Uiso 1 1 calc R . . C5 C 0.9604(8) 0.6964(7) -0.1621(6) 0.051(2) Uani 1 1 d . . . C6 C 1.0076(8) 0.8283(7) -0.1779(5) 0.0449(18) Uani 1 1 d . . . C8 C 0.8350(9) 0.9817(8) 0.4529(6) 0.058(2) Uani 1 1 d . . . H8A H 0.8499 1.0652 0.4407 0.069 Uiso 1 1 calc R . . C9 C 0.7917(11) 0.9392(9) 0.5436(6) 0.069(3) Uani 1 1 d . . . H9A H 0.7743 0.9919 0.5900 0.083 Uiso 1 1 calc R . . C10 C 0.7750(11) 0.8150(10) 0.5633(7) 0.073(3) Uani 1 1 d . . . H10A H 0.7475 0.7839 0.6242 0.088 Uiso 1 1 calc R . . C11 C 0.7989(11) 0.7403(9) 0.4937(7) 0.068(3) Uani 1 1 d . . . H11A H 0.7881 0.6573 0.5062 0.081 Uiso 1 1 calc R . . C12 C 0.8394(8) 0.7880(8) 0.4038(6) 0.051(2) Uani 1 1 d . . . C13 C 0.8640(9) 0.7159(7) 0.3197(6) 0.054(2) Uani 1 1 d . . . C14 C 1.2039(9) 0.8587(8) 0.2001(6) 0.056(2) Uani 1 1 d . . . H14A H 1.1441 0.8433 0.2440 0.067 Uiso 1 1 calc R . . C15 C 1.3282(9) 0.8777(9) 0.2448(7) 0.066(3) Uani 1 1 d . . . H15A H 1.3529 0.8792 0.3181 0.079 Uiso 1 1 calc R . . C16 C 1.4217(10) 0.8953(10) 0.1828(8) 0.074(3) Uani 1 1 d . . . C17 C 1.3782(10) 0.8961(10) 0.0741(8) 0.074(3) Uani 1 1 d . . . H17A H 1.4359 0.9075 0.0285 0.089 Uiso 1 1 calc R . . C18 C 1.2502(9) 0.8798(8) 0.0359(7) 0.061(2) Uani 1 1 d . . . H18A H 1.2235 0.8823 -0.0368 0.073 Uiso 1 1 calc R . . C19 C 1.5639(12) 0.9198(15) 0.2310(10) 0.121(5) Uani 1 1 d . . . H19A H 1.5754 0.9187 0.3066 0.181 Uiso 1 1 calc R . . H19B H 1.6123 0.9993 0.2123 0.181 Uiso 1 1 calc R . . H19C H 1.5944 0.8568 0.2048 0.181 Uiso 1 1 calc R . . C20 C 0.6924(10) 0.8149(9) -0.1220(7) 0.067(3) Uani 1 1 d . . . H20A H 0.7497 0.8623 -0.1610 0.080 Uiso 1 1 calc R . . C21 C 0.5630(10) 0.7809(9) -0.1663(7) 0.070(3) Uani 1 1 d . . . H21A H 0.5347 0.8050 -0.2333 0.084 Uiso 1 1 calc R . . C22 C 0.4751(11) 0.7112(10) -0.1121(7) 0.075(3) Uani 1 1 d . . . C23 C 0.5253(11) 0.6797(11) -0.0153(8) 0.086(3) Uani 1 1 d . . . H23A H 0.4693 0.6325 0.0248 0.103 Uiso 1 1 calc R . . C24 C 0.6565(9) 0.7156(9) 0.0248(7) 0.065(3) Uani 1 1 d . . . H24A H 0.6863 0.6902 0.0909 0.078 Uiso 1 1 calc R . . C25 C 0.3313(11) 0.6723(14) -0.1567(9) 0.110(5) Uani 1 1 d . . . H25A H 0.3150 0.7061 -0.2243 0.165 Uiso 1 1 calc R . . H25B H 0.2883 0.7023 -0.1093 0.165 Uiso 1 1 calc R . . H25C H 0.2988 0.5836 -0.1648 0.165 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 0.0546(8) 0.0426(6) 0.0417(6) 0.0026(4) 0.0159(5) 0.0132(5) Ni2 0.0556(8) 0.0452(7) 0.0413(6) 0.0040(4) 0.0166(5) 0.0147(5) Cl1 0.122(3) 0.0722(17) 0.0599(14) 0.0095(12) 0.0317(15) 0.0297(17) O1 0.063(4) 0.051(3) 0.047(3) 0.001(2) 0.018(3) 0.020(3) O2 0.073(4) 0.043(3) 0.041(3) 0.011(2) 0.023(3) 0.014(3) O3 0.315(16) 0.074(6) 0.120(7) 0.025(5) 0.102(9) 0.094(8) O4 0.213(11) 0.091(6) 0.063(4) 0.032(4) 0.034(5) 0.048(6) O5 0.250(14) 0.131(8) 0.126(7) 0.040(6) 0.130(8) 0.099(9) O6 0.120(11) 0.269(18) 0.171(11) 0.002(11) -0.023(9) 0.009(11) N1 0.060(5) 0.043(4) 0.042(3) 0.008(3) 0.014(3) 0.011(3) N2 0.047(4) 0.052(4) 0.040(3) 0.005(3) 0.014(3) 0.013(3) N3 0.103(7) 0.051(4) 0.053(4) 0.009(3) 0.030(4) 0.023(4) N4 0.065(5) 0.045(4) 0.040(3) 0.004(3) 0.016(3) 0.020(3) N5 0.057(4) 0.043(4) 0.046(3) 0.004(3) 0.014(3) 0.015(3) N6 0.062(5) 0.057(4) 0.044(3) 0.003(3) 0.024(3) 0.012(4) N7 0.063(5) 0.054(4) 0.054(4) 0.007(3) 0.010(3) 0.023(4) N8 0.061(5) 0.050(4) 0.048(4) 0.010(3) 0.020(3) 0.018(3) C1 0.081(7) 0.043(5) 0.051(4) 0.013(4) 0.024(4) 0.021(4) C2 0.082(7) 0.041(5) 0.063(5) -0.003(4) 0.018(5) 0.008(5) C3 0.092(8) 0.048(5) 0.068(6) -0.008(4) 0.024(5) 0.018(5) C4 0.082(7) 0.055(5) 0.049(4) 0.005(4) 0.023(4) 0.026(5) C5 0.057(6) 0.041(4) 0.050(4) 0.002(3) 0.009(4) 0.010(4) C6 0.047(5) 0.048(4) 0.040(4) 0.000(3) 0.010(3) 0.013(4) C8 0.070(6) 0.056(5) 0.051(4) 0.003(4) 0.023(4) 0.019(5) C9 0.099(8) 0.075(7) 0.046(5) 0.001(4) 0.027(5) 0.035(6) C10 0.096(8) 0.075(7) 0.052(5) 0.004(5) 0.030(5) 0.023(6) C11 0.093(8) 0.057(6) 0.057(5) 0.008(4) 0.027(5) 0.021(5) C12 0.053(5) 0.058(5) 0.039(4) -0.002(4) 0.009(3) 0.012(4) C13 0.064(6) 0.045(5) 0.053(5) 0.008(4) 0.018(4) 0.011(4) C14 0.052(6) 0.061(5) 0.055(5) 0.003(4) 0.016(4) 0.015(4) C15 0.047(6) 0.084(7) 0.061(5) -0.004(5) 0.001(4) 0.018(5) C16 0.050(6) 0.082(7) 0.084(7) -0.006(5) 0.003(5) 0.015(5) C17 0.058(7) 0.088(8) 0.071(6) 0.001(5) 0.018(5) 0.012(6) C18 0.054(6) 0.067(6) 0.063(5) 0.008(4) 0.023(4) 0.013(5) C19 0.060(8) 0.169(15) 0.117(10) 0.010(9) 0.003(7) 0.020(9) C20 0.060(6) 0.067(6) 0.069(6) 0.010(5) 0.012(5) 0.013(5) C21 0.072(7) 0.079(7) 0.053(5) 0.002(5) 0.002(5) 0.019(6) C22 0.076(8) 0.081(7) 0.060(6) -0.009(5) 0.003(5) 0.018(6) C23 0.061(7) 0.114(9) 0.070(6) 0.011(6) 0.017(5) 0.006(6) C24 0.048(6) 0.082(7) 0.061(5) 0.017(5) 0.015(4) 0.009(5) C25 0.055(8) 0.151(13) 0.095(8) -0.011(8) -0.008(6) 0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.013(5) . ? Ni1 N5 2.027(6) . ? Ni1 O2 2.046(5) 2_775 ? Ni1 N4 2.087(6) . ? Ni1 N8 2.172(7) . ? Ni1 N7 2.190(8) . ? Ni2 O2 1.812(5) 2_775 ? Ni2 N2 1.852(7) . ? Ni2 N6 1.851(7) 2_775 ? Ni2 N1 1.884(6) . ? Cl1 O6 1.382(12) . ? Cl1 O4 1.400(7) . ? Cl1 O5 1.404(8) . ? Cl1 O3 1.412(8) . ? O1 N2 1.366(8) . ? O2 N5 1.418(8) . ? O2 Ni2 1.812(5) 2_775 ? O2 Ni1 2.046(5) 2_775 ? N1 C8 1.342(10) . ? N1 C12 1.351(10) . ? N2 C13 1.318(9) . ? N3 C13 1.324(10) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C1 1.321(10) . ? N4 C5 1.365(9) . ? N5 C6 1.333(9) . ? N6 C6 1.346(9) . ? N6 Ni2 1.851(7) 2_775 ? N6 H6A 0.8600 . ? N7 C24 1.324(10) . ? N7 C20 1.342(10) . ? N8 C18 1.346(10) . ? N8 C14 1.355(10) . ? C1 C2 1.383(12) . ? C1 H1A 0.9300 . ? C2 C3 1.369(11) . ? C2 H2A 0.9300 . ? C3 C4 1.410(12) . ? C3 H3C 0.9300 . ? C4 C5 1.359(11) . ? C4 H4A 0.9300 . ? C5 C6 1.459(11) . ? C8 C9 1.383(11) . ? C8 H8A 0.9300 . ? C9 C10 1.395(13) . ? C9 H9A 0.9300 . ? C10 C11 1.348(13) . ? C10 H10A 0.9300 . ? C11 C12 1.378(11) . ? C11 H11A 0.9300 . ? C12 C13 1.472(11) . ? C14 C15 1.329(12) . ? C14 H14A 0.9300 . ? C15 C16 1.395(13) . ? C15 H15A 0.9300 . ? C16 C17 1.392(13) . ? C16 C19 1.509(15) . ? C17 C18 1.355(13) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.364(13) . ? C20 H20A 0.9300 . ? C21 C22 1.365(13) . ? C21 H21A 0.9300 . ? C22 C23 1.357(13) . ? C22 C25 1.504(15) . ? C23 C24 1.371(13) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 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 Ni1 N5 170.0(2) . . ? O1 Ni1 O2 86.0(2) . 2_775 ? N5 Ni1 O2 103.6(2) . 2_775 ? O1 Ni1 N4 93.1(2) . . ? N5 Ni1 N4 77.5(2) . . ? O2 Ni1 N4 175.7(3) 2_775 . ? O1 Ni1 N8 88.6(2) . . ? N5 Ni1 N8 89.1(3) . . ? O2 Ni1 N8 88.7(3) 2_775 . ? N4 Ni1 N8 95.5(3) . . ? O1 Ni1 N7 89.5(2) . . ? N5 Ni1 N7 92.7(3) . . ? O2 Ni1 N7 91.6(3) 2_775 . ? N4 Ni1 N7 84.1(3) . . ? N8 Ni1 N7 178.0(2) . . ? O2 Ni2 N2 90.6(2) 2_775 . ? O2 Ni2 N6 84.4(2) 2_775 2_775 ? N2 Ni2 N6 174.0(3) . 2_775 ? O2 Ni2 N1 173.9(3) 2_775 . ? N2 Ni2 N1 83.2(3) . . ? N6 Ni2 N1 101.8(3) 2_775 . ? O6 Cl1 O4 106.0(8) . . ? O6 Cl1 O5 105.8(8) . . ? O4 Cl1 O5 110.7(7) . . ? O6 Cl1 O3 114.3(10) . . ? O4 Cl1 O3 110.2(5) . . ? O5 Cl1 O3 109.8(6) . . ? N2 O1 Ni1 115.6(4) . . ? N5 O2 Ni2 115.1(4) . 2_775 ? N5 O2 Ni1 124.3(4) . 2_775 ? Ni2 O2 Ni1 120.5(3) 2_775 2_775 ? C8 N1 C12 117.4(6) . . ? C8 N1 Ni2 128.0(5) . . ? C12 N1 Ni2 114.7(5) . . ? C13 N2 O1 116.2(7) . . ? C13 N2 Ni2 117.5(5) . . ? O1 N2 Ni2 126.1(4) . . ? C13 N3 H3A 120.0 . . ? C13 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C1 N4 C5 118.7(7) . . ? C1 N4 Ni1 125.6(5) . . ? C5 N4 Ni1 115.0(5) . . ? C6 N5 O2 109.5(6) . . ? C6 N5 Ni1 117.8(5) . . ? O2 N5 Ni1 131.1(5) . . ? C6 N6 Ni2 111.7(5) . 2_775 ? C6 N6 H6A 124.1 . . ? Ni2 N6 H6A 124.1 2_775 . ? C24 N7 C20 114.9(8) . . ? C24 N7 Ni1 122.2(6) . . ? C20 N7 Ni1 122.5(6) . . ? C18 N8 C14 114.5(8) . . ? C18 N8 Ni1 125.1(6) . . ? C14 N8 Ni1 120.3(5) . . ? N4 C1 C2 123.2(7) . . ? N4 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 118.9(8) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 118.2(8) . . ? C2 C3 H3C 120.9 . . ? C4 C3 H3C 120.9 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 N4 121.2(7) . . ? C4 C5 C6 124.3(7) . . ? N4 C5 C6 114.2(7) . . ? N5 C6 N6 118.8(7) . . ? N5 C6 C5 114.2(6) . . ? N6 C6 C5 126.9(7) . . ? N1 C8 C9 122.9(8) . . ? N1 C8 H8A 118.6 . . ? C9 C8 H8A 118.6 . . ? C8 C9 C10 118.0(8) . . ? C8 C9 H9A 121.0 . . ? C10 C9 H9A 121.0 . . ? C11 C10 C9 119.7(8) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 119.3(9) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? N1 C12 C11 122.7(8) . . ? N1 C12 C13 112.4(6) . . ? C11 C12 C13 124.8(8) . . ? N2 C13 N3 123.1(8) . . ? N2 C13 C12 111.9(7) . . ? N3 C13 C12 124.9(7) . . ? C15 C14 N8 124.4(8) . . ? C15 C14 H14A 117.8 . . ? N8 C14 H14A 117.8 . . ? C14 C15 C16 120.5(9) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C17 C16 C15 116.5(9) . . ? C17 C16 C19 121.5(10) . . ? C15 C16 C19 121.9(10) . . ? C18 C17 C16 118.9(9) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.6 . . ? N8 C18 C17 125.2(9) . . ? N8 C18 H18A 117.4 . . ? C17 C18 H18A 117.4 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N7 C20 C21 124.6(9) . . ? N7 C20 H20A 117.7 . . ? C21 C20 H20A 117.7 . . ? C20 C21 C22 119.9(9) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C23 C22 C21 116.0(10) . . ? C23 C22 C25 121.9(10) . . ? C21 C22 C25 122.1(9) . . ? C22 C23 C24 121.6(10) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? N7 C24 C23 123.1(8) . . ? N7 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.376 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.162 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 770173' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Cl2 N16 Ni4 O12' _chemical_formula_weight 1348.78 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' Cl Cl 0.1484 0.1585 '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 28.626(6) _cell_length_b 20.554(4) _cell_length_c 23.646(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.86(3) _cell_angle_gamma 90.00 _cell_volume 12066(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5386 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 55834 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.1130 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13666 _reflns_number_gt 5386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0984P)^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 13666 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1968 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2147 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 0.13319(3) 0.31176(4) 0.16260(4) 0.0622(2) Uani 1 1 d . . . Ni2 Ni 0.20828(3) 0.43081(4) 0.09852(4) 0.0616(2) Uani 1 1 d . . . Ni3 Ni 0.28447(3) 0.45182(4) 0.25896(4) 0.0638(3) Uani 1 1 d . . . Ni4 Ni 0.05422(3) 0.29495(4) 0.00166(4) 0.0709(3) Uani 1 1 d . . . Cl1 Cl 0.0000 0.33077(13) -0.2500 0.0892(8) Uani 1 2 d S . . Cl2 Cl 0.5000 0.67142(16) 0.2500 0.0918(8) Uani 1 2 d S . . Cl3 Cl 0.15689(11) 0.90785(16) 0.97939(11) 0.1284(10) Uani 1 1 d . . . N2 N 0.1984(2) 0.3700(2) 0.2117(2) 0.0672(14) Uani 1 1 d . . . N1 N 0.1551(2) 0.2913(2) 0.2585(2) 0.0681(14) Uani 1 1 d . . . N6 N -0.0230(2) 0.1872(3) 0.0706(3) 0.0896(18) Uani 1 1 d . . . H6A H -0.0037 0.1878 0.1124 0.108 Uiso 1 1 calc R . . H6B H -0.0530 0.1664 0.0520 0.108 Uiso 1 1 calc R . . N12 N 0.3552(3) 0.5675(4) 0.1896(3) 0.144(3) Uani 1 1 d . . . H12A H 0.3349 0.5679 0.1479 0.172 Uiso 1 1 calc R . . H12B H 0.3842 0.5904 0.2076 0.172 Uiso 1 1 calc R . . N10 N 0.3481(2) 0.4909(3) 0.3221(3) 0.0808(16) Uani 1 1 d . . . N3 N 0.26677(19) 0.4045(2) 0.3114(2) 0.0661(13) Uani 1 1 d . . . H3A H 0.2844 0.4054 0.3533 0.079 Uiso 1 1 calc R . . N4 N -0.0085(3) 0.2528(3) -0.0608(3) 0.100(2) Uani 1 1 d . . . N7 N 0.1896(2) 0.4452(2) 0.0022(2) 0.0635(13) Uani 1 1 d . . . N8 N 0.14347(19) 0.3717(2) 0.0486(2) 0.0594(12) Uani 1 1 d . . . N9 N 0.0745(2) 0.3388(3) -0.0497(2) 0.0757(15) Uani 1 1 d . . . H9A H 0.0566 0.3380 -0.0916 0.091 Uiso 1 1 calc R . . N13 N 0.0809(2) 0.3868(3) 0.1651(2) 0.0666(13) Uani 1 1 d . . . N11 N 0.2982(2) 0.4963(2) 0.2012(3) 0.0709(14) Uani 1 1 d . . . N14 N 0.1810(2) 0.2275(3) 0.1631(3) 0.0757(15) Uani 1 1 d . . . N15 N 0.2659(2) 0.3580(3) 0.1073(3) 0.0887(17) Uani 1 1 d . . . N16 N 0.1519(2) 0.5138(3) 0.0766(3) 0.0755(15) Uani 1 1 d . . . N5 N 0.0391(2) 0.2513(2) 0.0594(3) 0.0669(13) Uani 1 1 d . . . O1 O 0.22418(16) 0.4161(2) 0.19229(19) 0.0700(12) Uani 1 1 d . . . O2 O 0.07001(17) 0.2517(2) 0.1254(2) 0.0689(11) Uani 1 1 d . . . O3 O 0.11291(15) 0.33317(19) 0.06826(18) 0.0648(11) Uani 1 1 d . . . O4 O 0.26819(17) 0.4951(2) 0.1355(2) 0.0766(12) Uani 1 1 d . . . O7 O 0.4585(3) 0.6420(3) 0.2462(5) 0.218(5) Uani 1 1 d . . . O6 O -0.0133(4) 0.3697(4) -0.2135(4) 0.217(4) Uani 1 1 d . . . O5 O 0.0405(3) 0.2928(4) -0.2065(4) 0.178(3) Uani 1 1 d . . . O8 O 0.4844(4) 0.7192(5) 0.1999(5) 0.236(5) Uani 1 1 d . . . C5 C 0.1981(2) 0.3235(3) 0.3029(3) 0.0603(15) Uani 1 1 d . . . C17 C 0.1459(2) 0.4141(3) -0.0421(3) 0.0594(15) Uani 1 1 d . . . C6 C 0.2228(3) 0.3685(3) 0.2757(3) 0.0625(16) Uani 1 1 d . . . C18 C 0.1199(2) 0.3723(3) -0.0152(3) 0.0606(15) Uani 1 1 d . . . C13 C 0.2155(3) 0.4856(3) -0.0185(3) 0.0758(18) Uani 1 1 d . . . H13A H 0.2459 0.5079 0.0122 0.091 Uiso 1 1 calc R . . C1 C 0.1301(3) 0.2502(3) 0.2776(4) 0.086(2) Uani 1 1 d . . . H1A H 0.1003 0.2276 0.2463 0.104 Uiso 1 1 calc R . . C12 C -0.0061(3) 0.2188(3) 0.0342(4) 0.0705(18) Uani 1 1 d . . . C4 C 0.2181(3) 0.3158(3) 0.3689(3) 0.0762(19) Uani 1 1 d . . . H4A H 0.2482 0.3384 0.3997 0.091 Uiso 1 1 calc R . . C24 C 0.3416(3) 0.5313(4) 0.2266(4) 0.089(2) Uani 1 1 d . . . C14 C 0.1981(3) 0.4944(3) -0.0834(3) 0.081(2) Uani 1 1 d . . . H14A H 0.2166 0.5221 -0.0966 0.097 Uiso 1 1 calc R . . C21 C 0.4435(5) 0.5534(6) 0.4039(5) 0.200(7) Uani 1 1 d . . . H21A H 0.4760 0.5741 0.4310 0.240 Uiso 1 1 calc R . . C25 C 0.0340(3) 0.3711(3) 0.1595(3) 0.0776(19) Uani 1 1 d . . . H25A H 0.0242 0.3274 0.1530 0.093 Uiso 1 1 calc R . . C3 C 0.1903(3) 0.2716(4) 0.3869(4) 0.093(2) Uani 1 1 d . . . H3B H 0.2025 0.2644 0.4309 0.111 Uiso 1 1 calc R . . C15 C 0.1536(3) 0.4621(4) -0.1283(3) 0.086(2) Uani 1 1 d . . . H15A H 0.1413 0.4679 -0.1726 0.103 Uiso 1 1 calc R . . C2 C 0.1470(3) 0.2399(4) 0.3426(4) 0.090(2) Uani 1 1 d . . . H2A H 0.1285 0.2114 0.3551 0.108 Uiso 1 1 calc R . . C38 C 0.0639(4) 0.5592(5) 0.0236(5) 0.125(3) Uani 1 1 d . . . H38A H 0.0270 0.5534 0.0062 0.150 Uiso 1 1 calc R . . C16 C 0.1268(3) 0.4211(3) -0.1084(3) 0.0765(19) Uani 1 1 d . . . H16A H 0.0964 0.3984 -0.1387 0.092 Uiso 1 1 calc R . . C11 C -0.0342(3) 0.2180(3) -0.0361(4) 0.080(2) Uani 1 1 d . . . C29 C 0.0943(3) 0.4492(4) 0.1752(3) 0.083(2) Uani 1 1 d . . . H29A H 0.1270 0.4618 0.1791 0.100 Uiso 1 1 calc R . . C26 C -0.0017(3) 0.4141(4) 0.1625(4) 0.097(2) Uani 1 1 d . . . C40 C 0.1379(5) 0.6270(4) 0.0472(6) 0.129(3) Uani 1 1 d . . . C22 C 0.4180(4) 0.5628(6) 0.3368(5) 0.189(6) Uani 1 1 d . . . H22A H 0.4322 0.5917 0.3190 0.226 Uiso 1 1 calc R . . C41 C 0.1705(4) 0.5730(4) 0.0747(5) 0.105(3) Uani 1 1 d . . . H41A H 0.2075 0.5782 0.0930 0.126 Uiso 1 1 calc R . . C43 C 0.3108(4) 0.3744(5) 0.1086(6) 0.148(4) Uani 1 1 d . . . H43A H 0.3185 0.4184 0.1090 0.178 Uiso 1 1 calc R . . C20 C 0.4214(4) 0.5147(5) 0.4292(4) 0.149(4) Uani 1 1 d . . . H20A H 0.4380 0.5084 0.4740 0.178 Uiso 1 1 calc R . . C31 C 0.2245(4) 0.2068(5) 0.2124(5) 0.143(4) Uani 1 1 d . . . H31A H 0.2395 0.2318 0.2501 0.171 Uiso 1 1 calc R . . C27 C 0.0139(4) 0.4786(4) 0.1735(5) 0.115(3) Uani 1 1 d . . . H27A H -0.0085 0.5097 0.1763 0.138 Uiso 1 1 calc R . . C37 C 0.0982(3) 0.5088(4) 0.0495(4) 0.089(2) Uani 1 1 d . . . H37A H 0.0838 0.4680 0.0487 0.106 Uiso 1 1 calc R . . C23 C 0.3717(3) 0.5290(4) 0.2972(4) 0.102(3) Uani 1 1 d . . . C44 C 0.3484(4) 0.3284(8) 0.1094(7) 0.173(5) Uani 1 1 d . . . C28 C 0.0627(4) 0.4963(4) 0.1803(4) 0.108(3) Uani 1 1 d . . . H28A H 0.0741 0.5394 0.1882 0.130 Uiso 1 1 calc R . . C19 C 0.3729(3) 0.4838(4) 0.3874(4) 0.105(3) Uani 1 1 d . . . H19A H 0.3572 0.4573 0.4052 0.125 Uiso 1 1 calc R . . C46 C 0.2906(6) 0.2506(7) 0.1011(11) 0.330(14) Uani 1 1 d . . . H46A H 0.2810 0.2069 0.0976 0.396 Uiso 1 1 calc R . . C47 C 0.2559(5) 0.2977(6) 0.1008(8) 0.208(8) Uani 1 1 d . . . H47A H 0.2229 0.2841 0.0955 0.250 Uiso 1 1 calc R . . C39 C 0.0849(5) 0.6197(5) 0.0236(6) 0.152(4) Uani 1 1 d . . . H39A H 0.0621 0.6555 0.0071 0.182 Uiso 1 1 calc R . . C48 C 0.3954(7) 0.3578(8) 0.0999(12) 0.379(16) Uani 1 1 d . . . H48A H 0.4183 0.3233 0.1008 0.569 Uiso 1 1 calc R . . H48B H 0.4161 0.3880 0.1345 0.569 Uiso 1 1 calc R . . H48C H 0.3801 0.3799 0.0587 0.569 Uiso 1 1 calc R . . C42 C 0.1623(6) 0.6915(5) 0.0442(8) 0.237(8) Uani 1 1 d . . . H42A H 0.1343 0.7235 0.0236 0.355 Uiso 1 1 calc R . . H42B H 0.1804 0.6864 0.0194 0.355 Uiso 1 1 calc R . . H42C H 0.1878 0.7055 0.0876 0.355 Uiso 1 1 calc R . . C45 C 0.3352(6) 0.2660(6) 0.1060(8) 0.208(7) Uani 1 1 d . . . H45A H 0.3586 0.2339 0.1073 0.250 Uiso 1 1 calc R . . C10 C -0.0816(4) 0.1847(5) -0.0751(5) 0.124(3) Uani 1 1 d . . . H10A H -0.0981 0.1611 -0.0563 0.149 Uiso 1 1 calc R . . C30 C -0.0558(4) 0.3894(5) 0.1546(5) 0.145(4) Uani 1 1 d . . . H30A H -0.0758 0.4256 0.1574 0.218 Uiso 1 1 calc R . . H30B H -0.0487 0.3588 0.1885 0.218 Uiso 1 1 calc R . . H30C H -0.0763 0.3687 0.1129 0.218 Uiso 1 1 calc R . . C35 C 0.1630(4) 0.1898(5) 0.1120(5) 0.124(3) Uani 1 1 d . . . H35A H 0.1304 0.2017 0.0760 0.149 Uiso 1 1 calc R . . C33 C 0.2317(5) 0.1141(5) 0.1596(7) 0.131(3) Uani 1 1 d . . . H33A H 0.2491 0.0759 0.1595 0.157 Uiso 1 1 calc R . . C34 C 0.1877(5) 0.1330(5) 0.1053(6) 0.147(4) Uani 1 1 d . . . H34A H 0.1742 0.1105 0.0661 0.176 Uiso 1 1 calc R . . C9 C -0.1035(4) 0.1868(6) -0.1401(6) 0.177(5) Uani 1 1 d . . . H9B H -0.1354 0.1647 -0.1669 0.212 Uiso 1 1 calc R . . C32 C 0.2510(6) 0.1491(6) 0.2136(7) 0.171(5) Uani 1 1 d . . . C36 C 0.3062(9) 0.1297(11) 0.2749(9) 0.420(18) Uani 1 1 d . . . H36A H 0.3182 0.0889 0.2668 0.630 Uiso 1 1 calc R . . H36B H 0.3015 0.1256 0.3122 0.630 Uiso 1 1 calc R . . H36C H 0.3325 0.1627 0.2830 0.630 Uiso 1 1 calc R . . C8 C -0.0776(5) 0.2231(7) -0.1670(5) 0.223(8) Uani 1 1 d . . . H8B H -0.0928 0.2261 -0.2120 0.267 Uiso 1 1 calc R . . C7 C -0.0294(4) 0.2544(6) -0.1261(5) 0.162(5) Uani 1 1 d . . . H7A H -0.0113 0.2766 -0.1437 0.195 Uiso 1 1 calc R . . O9 O 0.2066(10) 0.8834(12) 0.9686(15) 0.132(10) Uani 0.40 1 d P . . O10 O 0.1172(12) 0.903(3) 0.9252(12) 0.39(4) Uani 0.40 1 d P . . O11 O 0.1589(9) 0.8783(11) 1.0322(8) 0.116(6) Uani 0.40 1 d P . . O12 O 0.1622(9) 0.9771(9) 0.982(2) 0.207(13) Uani 0.40 1 d P . . O12' O 0.1899(4) 0.9323(8) 1.0416(5) 0.119(4) Uani 0.60 1 d P . . O10' O 0.1458(7) 0.8397(8) 0.9830(13) 0.223(8) Uani 0.60 1 d P . . O9' O 0.0998(6) 0.9283(8) 0.9586(11) 0.226(8) Uani 0.60 1 d P . . O11' O 0.1753(11) 0.9092(16) 0.9437(11) 0.253(18) Uani 0.60 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0554(5) 0.0702(5) 0.0599(5) 0.0037(4) 0.0278(4) -0.0129(4) Ni2 0.0525(5) 0.0729(5) 0.0554(5) 0.0019(4) 0.0238(4) -0.0145(4) Ni3 0.0582(5) 0.0686(5) 0.0554(5) 0.0024(4) 0.0214(4) -0.0155(4) Ni4 0.0595(6) 0.0869(6) 0.0621(5) -0.0051(4) 0.0271(5) -0.0263(4) Cl1 0.108(2) 0.0768(16) 0.0584(15) 0.000 0.0228(17) 0.000 Cl2 0.0599(17) 0.138(2) 0.094(2) 0.000 0.0509(16) 0.000 Cl3 0.101(2) 0.207(3) 0.0599(15) 0.0078(16) 0.0264(15) -0.0748(19) N2 0.063(3) 0.079(3) 0.061(3) 0.011(3) 0.032(3) -0.017(3) N1 0.062(4) 0.082(4) 0.064(3) 0.013(3) 0.034(3) -0.012(3) N6 0.084(4) 0.092(4) 0.103(5) 0.006(3) 0.054(4) -0.026(3) N12 0.125(6) 0.197(8) 0.081(5) 0.019(5) 0.030(5) -0.103(6) N10 0.081(4) 0.082(4) 0.066(4) 0.007(3) 0.027(3) -0.026(3) N3 0.055(3) 0.074(3) 0.052(3) 0.003(3) 0.014(3) -0.019(3) N4 0.097(5) 0.129(5) 0.071(4) -0.008(4) 0.040(4) -0.050(4) N7 0.057(3) 0.073(3) 0.064(3) 0.008(3) 0.033(3) -0.008(3) N8 0.056(3) 0.064(3) 0.064(3) 0.008(2) 0.035(3) -0.009(2) N9 0.061(4) 0.097(4) 0.057(3) -0.005(3) 0.020(3) -0.034(3) N13 0.058(4) 0.077(4) 0.058(3) 0.000(3) 0.024(3) -0.008(3) N11 0.060(3) 0.076(3) 0.066(4) 0.007(3) 0.024(3) -0.024(3) N14 0.066(4) 0.085(4) 0.077(4) 0.005(3) 0.035(4) -0.004(3) N15 0.061(4) 0.101(5) 0.098(5) 0.025(4) 0.036(4) 0.001(3) N16 0.081(4) 0.075(4) 0.072(4) 0.006(3) 0.039(3) -0.006(3) N5 0.062(4) 0.067(3) 0.073(4) -0.003(3) 0.034(3) -0.018(3) O1 0.065(3) 0.082(3) 0.056(3) 0.007(2) 0.025(2) -0.025(2) O2 0.066(3) 0.078(3) 0.068(3) 0.000(2) 0.037(3) -0.015(2) O3 0.059(3) 0.074(3) 0.061(3) 0.002(2) 0.029(2) -0.017(2) O4 0.069(3) 0.095(3) 0.056(3) 0.004(2) 0.025(3) -0.029(2) O7 0.095(5) 0.130(5) 0.435(15) 0.089(7) 0.137(8) 0.004(4) O6 0.375(13) 0.143(6) 0.216(9) -0.038(6) 0.211(10) 0.029(7) O5 0.140(6) 0.169(6) 0.146(6) 0.056(5) 0.011(5) 0.058(5) O8 0.268(11) 0.259(10) 0.234(10) 0.117(8) 0.165(10) 0.033(9) C5 0.054(4) 0.072(4) 0.055(4) 0.008(3) 0.027(3) -0.006(3) C17 0.048(4) 0.069(4) 0.056(4) 0.001(3) 0.022(3) -0.015(3) C6 0.066(4) 0.063(4) 0.066(4) 0.005(3) 0.038(4) -0.002(3) C18 0.058(4) 0.070(4) 0.057(4) 0.001(3) 0.030(4) -0.006(3) C13 0.067(5) 0.089(5) 0.070(5) 0.001(4) 0.032(4) -0.019(4) C1 0.079(5) 0.100(5) 0.084(5) 0.009(4) 0.043(5) -0.023(4) C12 0.061(4) 0.070(4) 0.085(5) -0.007(4) 0.041(4) -0.012(3) C4 0.070(5) 0.091(5) 0.054(4) 0.003(3) 0.021(4) -0.007(4) C24 0.078(5) 0.101(5) 0.070(5) 0.015(4) 0.024(4) -0.037(4) C14 0.079(5) 0.105(5) 0.065(5) 0.012(4) 0.039(4) -0.020(4) C21 0.166(11) 0.255(13) 0.078(7) 0.021(8) -0.014(7) -0.148(10) C25 0.072(5) 0.078(4) 0.087(5) -0.003(4) 0.043(4) 0.002(4) C3 0.097(6) 0.120(6) 0.075(5) 0.016(5) 0.053(5) -0.017(5) C15 0.081(5) 0.116(6) 0.061(5) 0.007(4) 0.035(4) -0.021(5) C2 0.087(6) 0.107(6) 0.083(6) 0.004(5) 0.048(5) -0.033(5) C38 0.105(8) 0.100(7) 0.170(10) 0.020(7) 0.069(7) 0.017(6) C16 0.066(5) 0.096(5) 0.056(4) 0.005(4) 0.022(4) -0.017(4) C11 0.061(5) 0.098(5) 0.076(5) -0.012(4) 0.030(4) -0.033(4) C29 0.087(6) 0.075(5) 0.084(5) 0.000(4) 0.039(5) -0.004(4) C26 0.080(6) 0.105(6) 0.099(6) -0.005(5) 0.039(5) 0.002(5) C40 0.139(9) 0.069(6) 0.184(11) 0.018(6) 0.083(9) -0.001(6) C22 0.159(10) 0.245(12) 0.080(7) 0.023(7) -0.003(7) -0.150(10) C41 0.106(7) 0.070(5) 0.153(8) 0.006(5) 0.074(6) -0.001(5) C43 0.078(6) 0.134(8) 0.248(14) -0.008(8) 0.091(8) -0.006(6) C20 0.143(9) 0.179(9) 0.060(5) 0.010(6) 0.003(6) -0.102(8) C31 0.130(9) 0.153(9) 0.100(8) -0.005(6) 0.023(7) 0.058(8) C27 0.119(8) 0.093(7) 0.135(8) 0.000(6) 0.065(7) 0.023(6) C37 0.070(5) 0.092(5) 0.105(6) 0.007(5) 0.044(5) 0.006(4) C23 0.095(6) 0.117(6) 0.062(5) 0.005(4) 0.015(4) -0.059(5) C44 0.086(8) 0.209(13) 0.251(15) 0.003(12) 0.104(9) 0.010(9) C28 0.130(8) 0.072(5) 0.125(7) -0.003(5) 0.066(7) 0.003(5) C19 0.104(7) 0.113(6) 0.071(5) 0.009(5) 0.024(5) -0.035(5) C46 0.188(15) 0.147(11) 0.76(4) 0.149(18) 0.32(2) 0.072(11) C47 0.141(10) 0.126(9) 0.43(2) 0.115(12) 0.194(14) 0.049(8) C39 0.130(10) 0.111(8) 0.220(13) 0.040(8) 0.090(10) 0.038(7) C48 0.249(19) 0.258(19) 0.80(5) 0.00(2) 0.39(3) -0.005(15) C42 0.226(16) 0.103(8) 0.42(3) 0.043(11) 0.193(18) 0.003(9) C45 0.150(12) 0.108(9) 0.39(2) 0.059(12) 0.154(15) 0.036(9) C10 0.100(7) 0.170(9) 0.085(7) -0.020(6) 0.032(6) -0.073(6) C30 0.105(7) 0.164(9) 0.196(11) -0.032(8) 0.097(8) 0.005(7) C35 0.087(7) 0.133(8) 0.139(9) -0.021(7) 0.045(7) 0.028(6) C33 0.151(11) 0.104(7) 0.148(10) -0.001(7) 0.082(9) 0.019(7) C34 0.131(10) 0.147(10) 0.155(11) -0.006(8) 0.066(9) 0.035(8) C9 0.126(10) 0.250(14) 0.132(10) -0.031(9) 0.048(8) -0.114(9) C32 0.176(12) 0.169(11) 0.123(10) 0.022(8) 0.041(9) 0.101(10) C36 0.42(3) 0.51(4) 0.191(18) -0.02(2) 0.042(19) 0.33(3) C8 0.169(11) 0.365(19) 0.082(7) -0.035(9) 0.023(8) -0.186(13) C7 0.131(9) 0.264(13) 0.082(7) -0.022(7) 0.046(7) -0.122(9) O9 0.116(17) 0.141(14) 0.17(2) -0.067(14) 0.093(17) -0.061(12) O10 0.15(2) 0.95(11) 0.081(17) 0.14(3) 0.066(18) 0.26(5) O11 0.152(17) 0.133(15) 0.092(11) 0.021(10) 0.083(13) 0.031(13) O12 0.126(19) 0.116(15) 0.40(4) 0.06(2) 0.15(3) -0.011(12) O12' 0.081(7) 0.197(13) 0.070(7) -0.025(7) 0.031(6) -0.018(8) O10' 0.156(14) 0.184(16) 0.33(3) 0.002(17) 0.123(18) -0.051(12) O9' 0.085(11) 0.212(15) 0.28(2) 0.010(14) 0.018(12) -0.012(10) O11' 0.25(3) 0.45(4) 0.131(17) -0.10(2) 0.15(2) -0.17(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 O2 1.996(4) . ? Ni1 N2 2.027(5) . ? Ni1 O3 2.054(4) . ? Ni1 N1 2.073(5) . ? Ni1 N13 2.169(5) . ? Ni1 N14 2.203(6) . ? Ni2 O4 1.989(4) . ? Ni2 N8 2.032(5) . ? Ni2 O1 2.052(4) . ? Ni2 N7 2.084(5) . ? Ni2 N15 2.159(6) . ? Ni2 N16 2.225(6) . ? Ni3 O1 1.815(4) . ? Ni3 N3 1.834(5) . ? Ni3 N11 1.841(5) . ? Ni3 N10 1.866(6) . ? Ni4 O3 1.812(4) . ? Ni4 N9 1.823(5) . ? Ni4 N5 1.856(5) . ? Ni4 N4 1.875(6) . ? Cl1 O5 1.351(6) 2_554 ? Cl1 O5 1.351(6) . ? Cl1 O6 1.363(6) . ? Cl1 O6 1.363(6) 2_554 ? Cl2 O7 1.296(6) . ? Cl2 O7 1.296(6) 2_655 ? Cl2 O8 1.428(8) 2_655 ? Cl2 O8 1.428(8) . ? Cl3 O11' 1.198(18) . ? Cl3 O10 1.22(3) . ? Cl3 O11 1.364(15) . ? Cl3 O12' 1.388(10) . ? Cl3 O12 1.429(19) . ? Cl3 O10' 1.447(16) . ? Cl3 O9' 1.514(16) . ? Cl3 O9 1.64(2) . ? N2 C6 1.314(7) . ? N2 O1 1.411(5) . ? N1 C1 1.323(7) . ? N1 C5 1.331(7) . ? N6 C12 1.345(8) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N12 C24 1.346(8) . ? N12 H12A 0.8600 . ? N12 H12B 0.8600 . ? N10 C23 1.346(8) . ? N10 C19 1.348(8) . ? N3 C6 1.337(7) . ? N3 H3A 0.8600 . ? N4 C11 1.349(8) . ? N4 C7 1.351(10) . ? N7 C17 1.329(7) . ? N7 C13 1.357(7) . ? N8 C18 1.310(7) . ? N8 O3 1.419(5) . ? N9 C18 1.331(7) . ? N9 H9A 0.8600 . ? N13 C25 1.322(7) . ? N13 C29 1.327(8) . ? N11 C24 1.295(7) . ? N11 O4 1.351(6) . ? N14 C31 1.283(10) . ? N14 C35 1.307(10) . ? N15 C47 1.264(12) . ? N15 C43 1.315(9) . ? N16 C41 1.336(8) . ? N16 C37 1.344(8) . ? N5 C12 1.306(7) . ? N5 O2 1.358(6) . ? C5 C4 1.377(8) . ? C5 C6 1.491(8) . ? C17 C16 1.387(8) . ? C17 C18 1.474(7) . ? C13 C14 1.370(9) . ? C13 H13A 0.9300 . ? C1 C2 1.378(9) . ? C1 H1A 0.9300 . ? C12 C11 1.443(9) . ? C4 C3 1.407(9) . ? C4 H4A 0.9300 . ? C24 C23 1.450(9) . ? C14 C15 1.358(9) . ? C14 H14A 0.9300 . ? C21 C20 1.329(12) . ? C21 C22 1.390(12) . ? C21 H21A 0.9300 . ? C25 C26 1.378(9) . ? C25 H25A 0.9300 . ? C3 C2 1.329(9) . ? C3 H3B 0.9300 . ? C15 C16 1.372(8) . ? C15 H15A 0.9300 . ? C2 H2A 0.9300 . ? C38 C37 1.347(10) . ? C38 C39 1.381(12) . ? C38 H38A 0.9300 . ? C16 H16A 0.9300 . ? C11 C10 1.383(9) . ? C29 C28 1.369(10) . ? C29 H29A 0.9300 . ? C26 C27 1.381(11) . ? C26 C30 1.550(11) . ? C40 C39 1.339(12) . ? C40 C41 1.386(11) . ? C40 C42 1.518(12) . ? C22 C23 1.371(10) . ? C22 H22A 0.9300 . ? C41 H41A 0.9300 . ? C43 C44 1.426(13) . ? C43 H43A 0.9300 . ? C20 C19 1.393(10) . ? C20 H20A 0.9300 . ? C31 C32 1.400(13) . ? C31 H31A 0.9300 . ? C27 C28 1.374(11) . ? C27 H27A 0.9300 . ? C37 H37A 0.9300 . ? C44 C45 1.328(15) . ? C44 C48 1.589(15) . ? C28 H28A 0.9300 . ? C19 H19A 0.9300 . ? C46 C45 1.263(13) . ? C46 C47 1.387(14) . ? C46 H46A 0.9300 . ? C47 H47A 0.9300 . ? C39 H39A 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C45 H45A 0.9300 . ? C10 C9 1.341(12) . ? C10 H10A 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C35 C34 1.413(12) . ? C35 H35A 0.9300 . ? C33 C32 1.323(14) . ? C33 C34 1.333(13) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C9 C8 1.407(13) . ? C9 H9B 0.9300 . ? C32 C36 1.573(18) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C8 C7 1.388(11) . ? C8 H8B 0.9300 . ? C7 H7A 0.9300 . ? O9 O11' 0.95(4) . ? O10 O9' 1.24(3) . ? O10 O11' 1.50(4) . ? O10 O10' 1.76(4) . ? O11 O10' 1.30(2) . ? O11 O12' 1.37(2) . ? O12 O12' 1.53(3) . ? 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 O2 Ni1 N2 172.66(18) . . ? O2 Ni1 O3 87.09(16) . . ? N2 Ni1 O3 100.22(17) . . ? O2 Ni1 N1 94.08(19) . . ? N2 Ni1 N1 78.6(2) . . ? O3 Ni1 N1 178.82(18) . . ? O2 Ni1 N13 88.07(19) . . ? N2 Ni1 N13 90.9(2) . . ? O3 Ni1 N13 92.98(17) . . ? N1 Ni1 N13 87.19(19) . . ? O2 Ni1 N14 86.59(19) . . ? N2 Ni1 N14 93.9(2) . . ? O3 Ni1 N14 90.8(2) . . ? N1 Ni1 N14 89.2(2) . . ? N13 Ni1 N14 173.32(19) . . ? O4 Ni2 N8 171.91(19) . . ? O4 Ni2 O1 86.81(16) . . ? N8 Ni2 O1 100.77(17) . . ? O4 Ni2 N7 94.69(18) . . ? N8 Ni2 N7 77.68(19) . . ? O1 Ni2 N7 178.20(17) . . ? O4 Ni2 N15 88.2(2) . . ? N8 Ni2 N15 94.2(2) . . ? O1 Ni2 N15 92.7(2) . . ? N7 Ni2 N15 88.4(2) . . ? O4 Ni2 N16 87.7(2) . . ? N8 Ni2 N16 88.7(2) . . ? O1 Ni2 N16 96.29(18) . . ? N7 Ni2 N16 82.79(19) . . ? N15 Ni2 N16 169.9(2) . . ? O1 Ni3 N3 84.81(19) . . ? O1 Ni3 N11 91.1(2) . . ? N3 Ni3 N11 175.8(2) . . ? O1 Ni3 N10 175.0(2) . . ? N3 Ni3 N10 100.1(2) . . ? N11 Ni3 N10 84.0(2) . . ? O3 Ni4 N9 84.24(19) . . ? O3 Ni4 N5 91.5(2) . . ? N9 Ni4 N5 175.5(2) . . ? O3 Ni4 N4 174.0(2) . . ? N9 Ni4 N4 101.6(2) . . ? N5 Ni4 N4 82.7(2) . . ? O5 Cl1 O5 109.3(7) 2_554 . ? O5 Cl1 O6 114.7(6) 2_554 . ? O5 Cl1 O6 105.2(6) . . ? O5 Cl1 O6 105.2(6) 2_554 2_554 ? O5 Cl1 O6 114.7(6) . 2_554 ? O6 Cl1 O6 108.1(7) . 2_554 ? O7 Cl2 O7 124.4(7) . 2_655 ? O7 Cl2 O8 105.9(6) . 2_655 ? O7 Cl2 O8 111.5(6) 2_655 2_655 ? O7 Cl2 O8 111.5(6) . . ? O7 Cl2 O8 105.9(6) 2_655 . ? O8 Cl2 O8 93.1(10) 2_655 . ? O11' Cl3 O10 76.6(15) . . ? O11' Cl3 O11 145.5(19) . . ? O10 Cl3 O11 121(2) . . ? O11' Cl3 O12' 115.7(12) . . ? O10 Cl3 O12' 158(2) . . ? O11 Cl3 O12' 59.6(9) . . ? O11' Cl3 O12 86.4(17) . . ? O10 Cl3 O12 99(3) . . ? O11 Cl3 O12 116.3(17) . . ? O12' Cl3 O12 65.6(14) . . ? O11' Cl3 O10' 104.5(19) . . ? O10 Cl3 O10' 82(3) . . ? O11 Cl3 O10' 55.0(9) . . ? O12' Cl3 O10' 110.0(11) . . ? O12 Cl3 O10' 168.9(14) . . ? O11' Cl3 O9' 123.2(17) . . ? O10 Cl3 O9' 52.7(13) . . ? O11 Cl3 O9' 88.0(12) . . ? O12' Cl3 O9' 107.3(10) . . ? O12 Cl3 O9' 79.1(11) . . ? O10' Cl3 O9' 93.2(9) . . ? O11' Cl3 O9 35(2) . . ? O10 Cl3 O9 103.6(15) . . ? O11 Cl3 O9 111.2(13) . . ? O12' Cl3 O9 95.2(10) . . ? O12 Cl3 O9 103.4(12) . . ? O10' Cl3 O9 86.9(12) . . ? O9' Cl3 O9 155.9(14) . . ? C6 N2 O1 109.1(5) . . ? C6 N2 Ni1 117.1(4) . . ? O1 N2 Ni1 133.8(4) . . ? C1 N1 C5 119.5(5) . . ? C1 N1 Ni1 125.6(5) . . ? C5 N1 Ni1 114.8(4) . . ? C12 N6 H6A 120.0 . . ? C12 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C24 N12 H12A 120.0 . . ? C24 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C23 N10 C19 118.0(6) . . ? C23 N10 Ni3 113.8(5) . . ? C19 N10 Ni3 128.2(5) . . ? C6 N3 Ni3 111.0(4) . . ? C6 N3 H3A 124.5 . . ? Ni3 N3 H3A 124.5 . . ? C11 N4 C7 118.8(6) . . ? C11 N4 Ni4 114.8(5) . . ? C7 N4 Ni4 126.4(5) . . ? C17 N7 C13 118.6(5) . . ? C17 N7 Ni2 115.0(4) . . ? C13 N7 Ni2 126.3(4) . . ? C18 N8 O3 109.5(5) . . ? C18 N8 Ni2 117.5(4) . . ? O3 N8 Ni2 132.6(3) . . ? C18 N9 Ni4 112.7(4) . . ? C18 N9 H9A 123.7 . . ? Ni4 N9 H9A 123.7 . . ? C25 N13 C29 116.2(6) . . ? C25 N13 Ni1 120.3(5) . . ? C29 N13 Ni1 123.5(5) . . ? C24 N11 O4 117.2(5) . . ? C24 N11 Ni3 116.2(5) . . ? O4 N11 Ni3 126.6(4) . . ? C31 N14 C35 113.6(8) . . ? C31 N14 Ni1 125.9(6) . . ? C35 N14 Ni1 120.2(6) . . ? C47 N15 C43 114.5(8) . . ? C47 N15 Ni2 123.4(6) . . ? C43 N15 Ni2 121.0(6) . . ? C41 N16 C37 115.7(7) . . ? C41 N16 Ni2 116.9(5) . . ? C37 N16 Ni2 125.3(5) . . ? C12 N5 O2 117.3(5) . . ? C12 N5 Ni4 117.0(5) . . ? O2 N5 Ni4 125.7(4) . . ? N2 O1 Ni3 114.5(3) . . ? N2 O1 Ni2 125.4(3) . . ? Ni3 O1 Ni2 118.85(18) . . ? N5 O2 Ni1 116.1(3) . . ? N8 O3 Ni4 114.4(3) . . ? N8 O3 Ni1 126.1(3) . . ? Ni4 O3 Ni1 119.30(18) . . ? N11 O4 Ni2 115.7(3) . . ? N1 C5 C4 122.4(5) . . ? N1 C5 C6 114.8(5) . . ? C4 C5 C6 122.8(6) . . ? N7 C17 C16 122.0(5) . . ? N7 C17 C18 114.8(5) . . ? C16 C17 C18 123.3(6) . . ? N2 C6 N3 120.4(5) . . ? N2 C6 C5 114.7(6) . . ? N3 C6 C5 124.8(6) . . ? N8 C18 N9 119.1(5) . . ? N8 C18 C17 114.9(5) . . ? N9 C18 C17 125.9(6) . . ? N7 C13 C14 121.8(6) . . ? N7 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? N1 C1 C2 122.0(7) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? N5 C12 N6 123.0(7) . . ? N5 C12 C11 112.8(6) . . ? N6 C12 C11 124.1(6) . . ? C5 C4 C3 116.1(6) . . ? C5 C4 H4A 122.0 . . ? C3 C4 H4A 122.0 . . ? N11 C24 N12 121.8(7) . . ? N11 C24 C23 113.5(6) . . ? N12 C24 C23 124.7(6) . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C20 C21 C22 120.0(8) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? N13 C25 C26 125.4(7) . . ? N13 C25 H25A 117.3 . . ? C26 C25 H25A 117.3 . . ? C2 C3 C4 121.6(7) . . ? C2 C3 H3B 119.2 . . ? C4 C3 H3B 119.2 . . ? C14 C15 C16 120.0(6) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C3 C2 C1 118.4(6) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C37 C38 C39 118.3(9) . . ? C37 C38 H38A 120.9 . . ? C39 C38 H38A 120.8 . . ? C15 C16 C17 118.5(6) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? N4 C11 C10 122.7(7) . . ? N4 C11 C12 112.4(6) . . ? C10 C11 C12 124.9(7) . . ? N13 C29 C28 123.8(7) . . ? N13 C29 H29A 118.1 . . ? C28 C29 H29A 118.1 . . ? C25 C26 C27 116.6(8) . . ? C25 C26 C30 120.3(8) . . ? C27 C26 C30 123.0(8) . . ? C39 C40 C41 117.7(9) . . ? C39 C40 C42 122.1(11) . . ? C41 C40 C42 120.3(10) . . ? C23 C22 C21 119.2(8) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? N16 C41 C40 124.0(8) . . ? N16 C41 H41A 118.0 . . ? C40 C41 H41A 118.0 . . ? N15 C43 C44 123.5(10) . . ? N15 C43 H43A 118.2 . . ? C44 C43 H43A 118.2 . . ? C21 C20 C19 118.8(8) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? N14 C31 C32 124.8(10) . . ? N14 C31 H31A 117.6 . . ? C32 C31 H31A 117.6 . . ? C28 C27 C26 119.3(8) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? N16 C37 C38 124.0(8) . . ? N16 C37 H37A 118.0 . . ? C38 C37 H37A 118.0 . . ? N10 C23 C22 121.5(7) . . ? N10 C23 C24 112.5(6) . . ? C22 C23 C24 126.0(7) . . ? C45 C44 C43 116.7(10) . . ? C45 C44 C48 126.5(13) . . ? C43 C44 C48 115.5(12) . . ? C29 C28 C27 118.7(8) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? N10 C19 C20 122.3(7) . . ? N10 C19 H19A 118.8 . . ? C20 C19 H19A 118.8 . . ? C45 C46 C47 120.9(13) . . ? C45 C46 H46A 119.5 . . ? C47 C46 H46A 119.5 . . ? N15 C47 C46 124.4(10) . . ? N15 C47 H47A 117.8 . . ? C46 C47 H47A 117.8 . . ? C40 C39 C38 120.2(10) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C46 C45 C44 119.6(13) . . ? C46 C45 H45A 120.2 . . ? C44 C45 H45A 120.2 . . ? C9 C10 C11 119.5(8) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N14 C35 C34 127.2(10) . . ? N14 C35 H35A 116.4 . . ? C34 C35 H35A 116.4 . . ? C32 C33 C34 120.7(11) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C33 C34 C35 114.8(11) . . ? C33 C34 H34A 122.6 . . ? C35 C34 H34A 122.6 . . ? C10 C9 C8 118.9(9) . . ? C10 C9 H9B 120.5 . . ? C8 C9 H9B 120.5 . . ? C33 C32 C31 118.6(11) . . ? C33 C32 C36 119.8(12) . . ? C31 C32 C36 121.3(13) . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C7 C8 C9 119.8(10) . . ? C7 C8 H8B 120.1 . . ? C9 C8 H8B 120.1 . . ? N4 C7 C8 120.3(8) . . ? N4 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? O11' O9 Cl3 46.0(19) . . ? Cl3 O10 O9' 76(2) . . ? Cl3 O10 O11' 51.0(14) . . ? O9' O10 O11' 121(4) . . ? Cl3 O10 O10' 54.5(14) . . ? O9' O10 O10' 90(2) . . ? O11' O10 O10' 79.6(19) . . ? O10' O11 Cl3 65.7(11) . . ? O10' O11 O12' 120.9(16) . . ? Cl3 O11 O12' 61.0(9) . . ? Cl3 O12 O12' 55.9(9) . . ? O11 O12' Cl3 59.3(8) . . ? O11 O12' O12 109.9(14) . . ? Cl3 O12' O12 58.5(11) . . ? O11 O10' Cl3 59.3(10) . . ? O11 O10' O10 94(2) . . ? Cl3 O10' O10 43.4(18) . . ? O10 O9' Cl3 51.5(14) . . ? O9 O11' Cl3 99(3) . . ? O9 O11' O10 134(4) . . ? Cl3 O11' O10 52.5(12) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.626 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.083 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 770174' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52 Cl2 N22 Ni4 O12' _chemical_formula_weight 1386.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.306(2) _cell_length_b 11.476(2) _cell_length_c 12.802(3) _cell_angle_alpha 90.84(3) _cell_angle_beta 103.82(3) _cell_angle_gamma 105.62(3) _cell_volume 1410.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3672 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 25.00 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.488 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6619 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4388 _reflns_number_gt 3672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0759P)^2^+0.5024P] 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 4388 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.94705(4) 0.32815(3) 0.02658(3) 0.02925(15) Uani 1 1 d . . . Ni2 Ni 0.88618(4) 0.44748(4) 0.24545(3) 0.03232(15) Uani 1 1 d . . . Cl1 Cl 0.76378(13) 0.81534(10) 0.47347(8) 0.0609(3) Uani 1 1 d . . . N6 N 0.8290(3) 0.0981(3) 0.3070(2) 0.0447(7) Uani 1 1 d . . . H6A H 0.8384 0.0602 0.2521 0.054 Uiso 1 1 calc R . . H6B H 0.8117 0.0595 0.3614 0.054 Uiso 1 1 calc R . . O2 O 0.8886(3) 0.2236(2) 0.14406(18) 0.0387(5) Uani 1 1 d . . . N1 N 0.9371(3) 0.1788(2) -0.0730(2) 0.0329(6) Uani 1 1 d . . . C1 C 0.9775(3) 0.2051(3) -0.1645(3) 0.0331(7) Uani 1 1 d . . . N2 N 1.0101(3) 0.4068(2) -0.1018(2) 0.0325(6) Uani 1 1 d . . . N5 N 0.8676(3) 0.2824(2) 0.2275(2) 0.0338(6) Uani 1 1 d . . . N9 N 1.1576(3) 0.3511(3) 0.1074(2) 0.0407(7) Uani 1 1 d . . . N7 N 0.7352(3) 0.3009(3) -0.0535(2) 0.0396(7) Uani 1 1 d . . . N4 N 0.8325(3) 0.4069(3) 0.3746(2) 0.0388(7) Uani 1 1 d . . . C6 C 1.0290(3) 0.3372(3) -0.1759(3) 0.0330(7) Uani 1 1 d . . . C12 C 0.8414(3) 0.2190(3) 0.3079(3) 0.0359(7) Uani 1 1 d . . . C7 C 0.8177(4) 0.2887(3) 0.3934(3) 0.0387(8) Uani 1 1 d . . . C5 C 0.8802(4) 0.0634(3) -0.0586(3) 0.0379(8) Uani 1 1 d . . . H5A H 0.8517 0.0453 0.0044 0.045 Uiso 1 1 calc R . . C11 C 0.8103(5) 0.4802(4) 0.4472(3) 0.0526(10) Uani 1 1 d . . . H11A H 0.8200 0.5614 0.4348 0.063 Uiso 1 1 calc R . . C2 C 0.9639(4) 0.1149(3) -0.2436(3) 0.0420(8) Uani 1 1 d . . . H2A H 0.9934 0.1345 -0.3060 0.050 Uiso 1 1 calc R . . C18 C 1.3476(5) 0.3647(4) 0.2386(4) 0.0637(12) Uani 1 1 d . . . H18A H 1.4061 0.3631 0.3059 0.076 Uiso 1 1 calc R . . C13 C 0.6287(4) 0.2315(4) -0.0260(3) 0.0495(9) Uani 1 1 d . . . H13A H 0.6340 0.1946 0.0385 0.059 Uiso 1 1 calc R . . N8 N 0.5103(3) 0.2198(3) -0.1019(3) 0.0596(10) Uani 1 1 d . . . C19 C 1.2061(4) 0.3408(4) 0.2144(3) 0.0538(10) Uani 1 1 d . . . H19A H 1.1515 0.3207 0.2633 0.065 Uiso 1 1 calc R . . C4 C 0.8621(4) -0.0307(3) -0.1345(3) 0.0439(8) Uani 1 1 d . . . H4A H 0.8211 -0.1106 -0.1231 0.053 Uiso 1 1 calc R . . C3 C 0.9057(4) -0.0043(3) -0.2270(3) 0.0462(9) Uani 1 1 d . . . H3B H 0.8960 -0.0664 -0.2782 0.055 Uiso 1 1 calc R . . C14 C 0.6817(4) 0.3360(4) -0.1535(3) 0.0549(10) Uani 1 1 d . . . H14A H 0.7337 0.3869 -0.1937 0.066 Uiso 1 1 calc R . . C17 C 1.2682(4) 0.3816(4) 0.0693(4) 0.0617(12) Uani 1 1 d . . . H17A H 1.2676 0.3954 -0.0022 0.074 Uiso 1 1 calc R . . C15 C 0.5449(5) 0.2861(5) -0.1840(4) 0.0674(13) Uani 1 1 d . . . H15A H 0.4846 0.2947 -0.2484 0.081 Uiso 1 1 calc R . . C10 C 0.7734(6) 0.4384(4) 0.5394(4) 0.0680(14) Uani 1 1 d . . . H10A H 0.7588 0.4910 0.5886 0.082 Uiso 1 1 calc R . . C9 C 0.7584(6) 0.3190(4) 0.5581(4) 0.0685(13) Uani 1 1 d . . . H9A H 0.7323 0.2896 0.6196 0.082 Uiso 1 1 calc R . . N10 N 1.3844(4) 0.3900(4) 0.1503(5) 0.0810(13) Uani 1 1 d . . . C16 C 0.3709(5) 0.1447(6) -0.0982(5) 0.093(2) Uani 1 1 d . . . H16A H 0.3772 0.1071 -0.0314 0.140 Uiso 1 1 calc R . . H16B H 0.3356 0.0830 -0.1574 0.140 Uiso 1 1 calc R . . H16C H 0.3091 0.1950 -0.1033 0.140 Uiso 1 1 calc R . . O6 O 0.7755(5) 0.7894(5) 0.3699(3) 0.1050(15) Uani 1 1 d . . . O5 O 0.8361(6) 0.7616(4) 0.5541(3) 0.1179(17) Uani 1 1 d . . . C22 C 0.5241(6) -0.0642(6) -0.2517(6) 0.0838(16) Uani 1 1 d . . . O4 O 0.7867(9) 0.9374(5) 0.4996(4) 0.167(3) Uani 1 1 d . . . C8 C 0.7822(5) 0.2427(4) 0.4855(3) 0.0567(11) Uani 1 1 d . . . H8A H 0.7746 0.1618 0.4980 0.068 Uiso 1 1 calc R . . C20 C 1.5267(6) 0.4253(9) 0.1432(7) 0.133(3) Uani 1 1 d . . . H20A H 1.5872 0.4249 0.2129 0.200 Uiso 1 1 calc R . . H20B H 1.5486 0.5054 0.1190 0.200 Uiso 1 1 calc R . . H20C H 1.5392 0.3690 0.0928 0.200 Uiso 1 1 calc R . . O3 O 0.6208(7) 0.7633(9) 0.4697(6) 0.210(4) Uani 1 1 d . . . C21 C 0.5509(7) 0.0073(7) -0.3418(6) 0.108(2) Uani 1 1 d . . . N11 N 0.5056(6) -0.1184(8) -0.1822(6) 0.137(3) Uani 1 1 d . . . N3 N 1.0851(3) 0.3862(3) -0.2544(2) 0.0408(7) Uani 1 1 d . . . H3A H 1.1052 0.3460 -0.3026 0.049 Uiso 1 1 calc R . . O1 O 1.0567(2) 0.52821(19) -0.12158(18) 0.0364(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0371(2) 0.0239(2) 0.0269(2) 0.00051(16) 0.00953(18) 0.00760(17) Ni2 0.0424(3) 0.0272(2) 0.0289(2) 0.00151(17) 0.01360(19) 0.00845(18) Cl1 0.0925(8) 0.0613(6) 0.0391(5) 0.0105(5) 0.0181(5) 0.0366(6) N6 0.067(2) 0.0339(16) 0.0367(16) 0.0105(13) 0.0183(15) 0.0153(14) O2 0.0589(14) 0.0287(12) 0.0307(12) 0.0012(9) 0.0165(11) 0.0115(11) N1 0.0385(14) 0.0266(13) 0.0320(14) -0.0005(11) 0.0069(12) 0.0083(11) C1 0.0371(17) 0.0291(16) 0.0325(17) -0.0025(13) 0.0068(14) 0.0103(13) N2 0.0460(15) 0.0219(12) 0.0301(14) 0.0009(11) 0.0113(12) 0.0087(11) N5 0.0415(15) 0.0321(14) 0.0292(14) 0.0016(11) 0.0110(12) 0.0109(12) N9 0.0388(15) 0.0324(15) 0.0468(17) -0.0001(13) 0.0050(14) 0.0083(12) N7 0.0415(16) 0.0379(16) 0.0375(16) -0.0027(13) 0.0056(13) 0.0121(13) N4 0.0487(16) 0.0356(15) 0.0322(15) 0.0017(12) 0.0151(13) 0.0079(13) C6 0.0372(17) 0.0302(16) 0.0320(17) -0.0005(13) 0.0107(14) 0.0086(13) C12 0.0396(17) 0.0330(17) 0.0333(17) 0.0031(14) 0.0088(15) 0.0076(14) C7 0.0453(19) 0.0399(19) 0.0283(17) 0.0036(14) 0.0098(15) 0.0071(15) C5 0.0428(18) 0.0300(17) 0.0396(18) 0.0034(14) 0.0107(15) 0.0079(14) C11 0.074(3) 0.044(2) 0.047(2) 0.0029(17) 0.029(2) 0.016(2) C2 0.054(2) 0.0350(18) 0.0411(19) -0.0024(15) 0.0187(17) 0.0131(16) C18 0.057(3) 0.056(3) 0.065(3) 0.000(2) -0.016(2) 0.021(2) C13 0.041(2) 0.055(2) 0.051(2) 0.0026(19) 0.0141(18) 0.0088(18) N8 0.0396(17) 0.063(2) 0.066(2) -0.0138(19) 0.0039(17) 0.0072(16) C19 0.059(2) 0.043(2) 0.053(2) -0.0073(18) -0.004(2) 0.0203(18) C4 0.052(2) 0.0260(17) 0.049(2) -0.0012(15) 0.0096(17) 0.0074(15) C3 0.056(2) 0.0318(18) 0.048(2) -0.0096(16) 0.0053(18) 0.0156(16) C14 0.059(2) 0.053(2) 0.045(2) 0.0045(19) 0.0010(19) 0.0132(19) C17 0.051(2) 0.053(3) 0.076(3) 0.009(2) 0.008(2) 0.0132(19) C15 0.056(3) 0.074(3) 0.060(3) -0.002(2) -0.008(2) 0.017(2) C10 0.108(4) 0.057(3) 0.052(3) -0.003(2) 0.045(3) 0.023(3) C9 0.106(4) 0.064(3) 0.046(2) 0.011(2) 0.043(3) 0.019(3) N10 0.0399(19) 0.073(3) 0.116(4) 0.002(3) -0.009(2) 0.0178(18) C16 0.040(2) 0.111(5) 0.108(4) -0.013(4) 0.009(3) -0.003(3) O6 0.123(3) 0.150(4) 0.057(2) -0.008(2) 0.035(2) 0.052(3) O5 0.175(4) 0.090(3) 0.078(3) 0.008(2) -0.024(3) 0.068(3) C22 0.056(3) 0.103(4) 0.097(4) 0.022(4) 0.021(3) 0.027(3) O4 0.359(10) 0.090(3) 0.082(3) 0.022(3) 0.061(4) 0.109(5) C8 0.087(3) 0.048(2) 0.038(2) 0.0094(18) 0.027(2) 0.015(2) C20 0.072(4) 0.174(8) 0.159(7) 0.027(7) 0.039(5) 0.035(5) O3 0.114(4) 0.346(12) 0.171(6) 0.055(7) 0.076(5) 0.029(6) C21 0.101(5) 0.127(6) 0.117(5) 0.053(5) 0.045(4) 0.049(4) N11 0.081(4) 0.199(7) 0.144(6) 0.084(6) 0.045(4) 0.042(4) N3 0.0564(17) 0.0317(15) 0.0407(16) -0.0002(12) 0.0241(14) 0.0128(13) O1 0.0557(14) 0.0215(11) 0.0345(12) 0.0020(9) 0.0201(11) 0.0072(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 O2 2.040(2) . ? Ni1 N2 2.044(3) . ? Ni1 O1 2.048(2) 2_765 ? Ni1 N1 2.086(3) . ? Ni1 N9 2.112(3) . ? Ni1 N7 2.114(3) . ? Ni2 O1 1.819(2) 2_765 ? Ni2 N3 1.848(3) 2_765 ? Ni2 N5 1.857(3) . ? Ni2 N4 1.891(3) . ? Cl1 O4 1.379(5) . ? Cl1 O5 1.379(4) . ? Cl1 O6 1.395(3) . ? Cl1 O3 1.422(6) . ? N6 C12 1.358(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O2 N5 1.346(3) . ? N1 C5 1.331(4) . ? N1 C1 1.347(4) . ? C1 C2 1.393(4) . ? C1 C6 1.487(5) . ? N2 C6 1.313(4) . ? N2 O1 1.395(3) . ? N5 C12 1.307(4) . ? N9 C17 1.310(5) . ? N9 C19 1.359(5) . ? N7 C13 1.298(5) . ? N7 C14 1.379(5) . ? N4 C11 1.344(5) . ? N4 C7 1.355(5) . ? C6 N3 1.335(4) . ? C12 C7 1.451(5) . ? C7 C8 1.388(5) . ? C5 C4 1.385(5) . ? C5 H5A 0.9300 . ? C11 C10 1.380(6) . ? C11 H11A 0.9300 . ? C2 C3 1.380(5) . ? C2 H2A 0.9300 . ? C18 N10 1.289(7) . ? C18 C19 1.365(6) . ? C18 H18A 0.9300 . ? C13 N8 1.339(5) . ? C13 H13A 0.9300 . ? N8 C15 1.366(6) . ? N8 C16 1.476(6) . ? C19 H19A 0.9300 . ? C4 C3 1.374(5) . ? C4 H4A 0.9300 . ? C3 H3B 0.9300 . ? C14 C15 1.328(6) . ? C14 H14A 0.9300 . ? C17 N10 1.364(6) . ? C17 H17A 0.9300 . ? C15 H15A 0.9300 . ? C10 C9 1.368(7) . ? C10 H10A 0.9300 . ? C9 C8 1.375(6) . ? C9 H9A 0.9300 . ? N10 C20 1.438(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C22 N11 1.117(8) . ? C22 C21 1.463(9) . ? C8 H8A 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N3 Ni2 1.848(3) 2_765 ? N3 H3A 0.8600 . ? O1 Ni2 1.819(2) 2_765 ? O1 Ni1 2.048(2) 2_765 ? 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 O2 Ni1 N2 170.28(10) . . ? O2 Ni1 O1 85.83(9) . 2_765 ? N2 Ni1 O1 103.76(10) . 2_765 ? O2 Ni1 N1 93.24(10) . . ? N2 Ni1 N1 77.27(10) . . ? O1 Ni1 N1 176.36(10) 2_765 . ? O2 Ni1 N9 89.22(11) . . ? N2 Ni1 N9 89.24(12) . . ? O1 Ni1 N9 90.05(11) 2_765 . ? N1 Ni1 N9 93.45(11) . . ? O2 Ni1 N7 89.76(12) . . ? N2 Ni1 N7 91.62(12) . . ? O1 Ni1 N7 90.74(11) 2_765 . ? N1 Ni1 N7 85.73(11) . . ? N9 Ni1 N7 178.66(11) . . ? O1 Ni2 N3 84.20(11) 2_765 2_765 ? O1 Ni2 N5 90.79(11) 2_765 . ? N3 Ni2 N5 174.73(11) 2_765 . ? O1 Ni2 N4 173.96(12) 2_765 . ? N3 Ni2 N4 101.35(12) 2_765 . ? N5 Ni2 N4 83.59(12) . . ? O4 Cl1 O5 112.3(3) . . ? O4 Cl1 O6 113.4(3) . . ? O5 Cl1 O6 115.1(3) . . ? O4 Cl1 O3 104.2(5) . . ? O5 Cl1 O3 105.5(4) . . ? O6 Cl1 O3 105.0(4) . . ? C12 N6 H6A 120.0 . . ? C12 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N5 O2 Ni1 115.99(18) . . ? C5 N1 C1 119.0(3) . . ? C5 N1 Ni1 125.1(2) . . ? C1 N1 Ni1 115.4(2) . . ? N1 C1 C2 121.9(3) . . ? N1 C1 C6 114.4(3) . . ? C2 C1 C6 123.6(3) . . ? C6 N2 O1 109.5(3) . . ? C6 N2 Ni1 118.3(2) . . ? O1 N2 Ni1 131.54(19) . . ? C12 N5 O2 116.9(3) . . ? C12 N5 Ni2 116.3(2) . . ? O2 N5 Ni2 126.5(2) . . ? C17 N9 C19 105.4(4) . . ? C17 N9 Ni1 129.1(3) . . ? C19 N9 Ni1 125.5(3) . . ? C13 N7 C14 105.3(3) . . ? C13 N7 Ni1 126.4(3) . . ? C14 N7 Ni1 127.6(3) . . ? C11 N4 C7 118.5(3) . . ? C11 N4 Ni2 128.1(3) . . ? C7 N4 Ni2 113.4(2) . . ? N2 C6 N3 120.4(3) . . ? N2 C6 C1 113.8(3) . . ? N3 C6 C1 125.8(3) . . ? N5 C12 N6 122.7(3) . . ? N5 C12 C7 113.3(3) . . ? N6 C12 C7 123.9(3) . . ? N4 C7 C8 121.8(3) . . ? N4 C7 C12 113.0(3) . . ? C8 C7 C12 125.2(3) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? N4 C11 C10 121.9(4) . . ? N4 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? N10 C18 C19 106.8(4) . . ? N10 C18 H18A 126.6 . . ? C19 C18 H18A 126.6 . . ? N7 C13 N8 111.6(4) . . ? N7 C13 H13A 124.2 . . ? N8 C13 H13A 124.2 . . ? C13 N8 C15 107.0(3) . . ? C13 N8 C16 125.8(4) . . ? C15 N8 C16 127.2(4) . . ? N9 C19 C18 109.3(4) . . ? N9 C19 H19A 125.4 . . ? C18 C19 H19A 125.4 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3B 120.1 . . ? C2 C3 H3B 120.1 . . ? C15 C14 N7 109.9(4) . . ? C15 C14 H14A 125.0 . . ? N7 C14 H14A 125.0 . . ? N9 C17 N10 109.7(5) . . ? N9 C17 H17A 125.1 . . ? N10 C17 H17A 125.1 . . ? C14 C15 N8 106.2(4) . . ? C14 C15 H15A 126.9 . . ? N8 C15 H15A 126.9 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C18 N10 C17 108.8(4) . . ? C18 N10 C20 123.9(5) . . ? C17 N10 C20 127.3(6) . . ? N8 C16 H16A 109.5 . . ? N8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N11 C22 C21 179.1(7) . . ? C9 C8 C7 118.7(4) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 N3 Ni2 110.6(2) . 2_765 ? C6 N3 H3A 124.7 . . ? Ni2 N3 H3A 124.7 2_765 . ? N2 O1 Ni2 114.87(17) . 2_765 ? N2 O1 Ni1 124.35(18) . 2_765 ? Ni2 O1 Ni1 120.69(11) 2_765 2_765 ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 1.050 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.072 #===End data_5 _database_code_depnum_ccdc_archive 'CCDC 770175' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H80 Br4 N24 Ni8 O26' _chemical_formula_weight 2198.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.313(3) _cell_length_b 12.909(3) _cell_length_c 13.706(3) _cell_angle_alpha 100.29(3) _cell_angle_beta 111.88(3) _cell_angle_gamma 97.79(3) _cell_volume 1939.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2511 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 26.00 _exptl_crystal_description platelet _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 4.046 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6152 _exptl_absorpt_correction_T_max 0.6878 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16096 _diffrn_reflns_av_R_equivalents 0.1561 _diffrn_reflns_av_sigmaI/netI 0.2283 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7412 _reflns_number_gt 2511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1200P)^2^+1.9000P] 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 7412 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2844 _refine_ls_R_factor_gt 0.1136 _refine_ls_wR_factor_ref 0.3025 _refine_ls_wR_factor_gt 0.2375 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.81098(17) 0.45616(16) 0.39438(17) 0.0529(6) Uani 1 1 d . . . Ni2 Ni 0.59770(16) 0.31162(15) 0.44151(16) 0.0493(6) Uani 1 1 d . . . Ni3 Ni 0.44777(17) 0.45003(15) 0.69376(16) 0.0512(6) Uani 1 1 d . . . Ni4 Ni 0.63995(16) 0.59703(15) 0.63129(16) 0.0496(6) Uani 1 1 d . . . Br1 Br 0.4681(3) 1.1291(2) 0.8537(2) 0.1413(12) Uani 1 1 d . . . Br2 Br 0.8984(3) 1.2122(2) 0.8598(2) 0.1356(11) Uani 1 1 d . . . O1 O 0.6811(8) 0.2399(8) 0.3561(8) 0.055(3) Uani 1 1 d . . . O2 O 0.5149(7) 0.4600(7) 0.5972(8) 0.045(2) Uani 1 1 d . . . O3 O 0.5403(8) 0.6668(7) 0.7023(8) 0.049(3) Uani 1 1 d . . . O4 O 0.7158(7) 0.4509(7) 0.4689(9) 0.050(3) Uani 1 1 d . . . O1W O 0.7278(10) 0.3026(11) 0.5945(10) 0.096(4) Uani 1 1 d . . . O2W O 0.7413(8) 0.5541(9) 0.7745(8) 0.065(3) Uani 1 1 d . . . O3W O 0.6905(11) 1.3327(10) 0.8128(9) 0.091(4) Uani 1 1 d . . . O4W O 0.7392(13) 1.0629(14) 0.9606(11) 0.128(6) Uani 1 1 d . . . O5W O 1.1615(13) 1.2763(12) 1.0413(12) 0.123(5) Uani 1 1 d . . . O6W O 0.7689(17) 0.9058(16) 1.0452(18) 0.200(9) Uani 1 1 d . . . O7W O 0.2150(15) 1.0857(11) 0.6697(16) 0.148(7) Uani 1 1 d . . . O8W O 0.8402(12) 1.1282(13) 0.4678(11) 0.110(5) Uani 1 1 d . . . O9W O 1.0227(12) 1.1902(11) 0.6699(12) 0.123(6) Uani 1 1 d . . . N1 N 0.8843(10) 0.4483(12) 0.2935(12) 0.062(4) Uani 1 1 d . . . N2 N 0.7488(12) 0.3103(11) 0.3289(11) 0.063(4) Uani 1 1 d . . . N3 N 0.7458(13) 0.1626(12) 0.1955(13) 0.084(5) Uani 1 1 d . . . H3A H 0.6973 0.1185 0.2087 0.101 Uiso 1 1 calc R . . H3B H 0.7709 0.1401 0.1465 0.101 Uiso 1 1 calc R . . N4 N 0.4879(10) 0.1697(10) 0.4187(10) 0.048(3) Uani 1 1 d . . . N5 N 0.4875(10) 0.3619(9) 0.5180(10) 0.046(3) Uani 1 1 d . . . N6 N 0.4084(11) 0.3054(10) 0.6310(11) 0.062(4) Uani 1 1 d . . . H6 H 0.3749 0.2572 0.6530 0.074 Uiso 1 1 calc R . . N7 N 0.3884(10) 0.4522(10) 0.8007(10) 0.050(3) Uani 1 1 d . . . N8 N 0.4949(10) 0.5979(9) 0.7490(10) 0.042(3) Uani 1 1 d . . . N9 N 0.5109(10) 0.7420(11) 0.8874(10) 0.064(4) Uani 1 1 d . . . H9A H 0.5455 0.7893 0.8651 0.077 Uiso 1 1 calc R . . H9B H 0.4968 0.7616 0.9440 0.077 Uiso 1 1 calc R . . N10 N 0.7751(10) 0.7339(9) 0.6750(10) 0.046(3) Uani 1 1 d . . . N11 N 0.7358(10) 0.5459(10) 0.5490(10) 0.050(3) Uani 1 1 d . . . N12 N 0.8695(10) 0.5964(9) 0.4737(10) 0.056(3) Uani 1 1 d . . . H12 H 0.9218 0.6421 0.4663 0.067 Uiso 1 1 calc R . . C1 C 0.9469(14) 0.5301(16) 0.2799(15) 0.074(5) Uani 1 1 d . . . H1 H 0.9656 0.5978 0.3270 0.088 Uiso 1 1 calc R . . C2 C 0.9863(16) 0.5184(15) 0.1963(14) 0.074(5) Uani 1 1 d . . . H2 H 1.0288 0.5785 0.1872 0.088 Uiso 1 1 calc R . . C3 C 0.9641(15) 0.4225(14) 0.1296(15) 0.070(5) Uani 1 1 d . . . H3 H 0.9918 0.4156 0.0748 0.084 Uiso 1 1 calc R . . C4 C 0.8994(14) 0.3322(16) 0.1419(14) 0.070(5) Uani 1 1 d . . . H4 H 0.8811 0.2638 0.0962 0.084 Uiso 1 1 calc R . . C5 C 0.8639(15) 0.3519(14) 0.2279(15) 0.066(5) Uani 1 1 d . . . C6 C 0.7835(16) 0.2703(16) 0.2531(15) 0.071(5) Uani 1 1 d . . . C7 C 0.4729(12) 0.0742(13) 0.3539(12) 0.051(4) Uani 1 1 d . . . H7 H 0.5169 0.0709 0.3115 0.061 Uiso 1 1 calc R . . C8 C 0.3984(14) -0.0199(12) 0.3440(14) 0.060(5) Uani 1 1 d . . . H8 H 0.3942 -0.0856 0.3004 0.072 Uiso 1 1 calc R . . C9 C 0.3304(15) -0.0093(13) 0.4037(14) 0.069(5) Uani 1 1 d . . . H9 H 0.2753 -0.0703 0.3959 0.083 Uiso 1 1 calc R . . C10 C 0.3376(13) 0.0841(12) 0.4738(13) 0.056(4) Uani 1 1 d . . . H10 H 0.2919 0.0887 0.5146 0.068 Uiso 1 1 calc R . . C11 C 0.4225(13) 0.1735(12) 0.4778(13) 0.051(4) Uani 1 1 d . . . C12 C 0.4383(12) 0.2839(12) 0.5464(13) 0.050(4) Uani 1 1 d . . . C13 C 0.3268(14) 0.3724(15) 0.8205(13) 0.063(5) Uani 1 1 d . . . H13 H 0.3066 0.3033 0.7758 0.076 Uiso 1 1 calc R . . C14 C 0.2923(15) 0.3889(17) 0.9043(16) 0.078(6) Uani 1 1 d . . . H14 H 0.2513 0.3305 0.9171 0.093 Uiso 1 1 calc R . . C15 C 0.3168(14) 0.4898(15) 0.9703(14) 0.064(5) Uani 1 1 d . . . H15 H 0.2903 0.4998 1.0259 0.077 Uiso 1 1 calc R . . C16 C 0.3808(13) 0.5768(13) 0.9543(13) 0.059(4) Uani 1 1 d . . . H16 H 0.3989 0.6462 0.9980 0.070 Uiso 1 1 calc R . . C17 C 0.4166(14) 0.5554(14) 0.8701(13) 0.059(4) Uani 1 1 d . . . C18 C 0.4794(13) 0.6385(14) 0.8342(14) 0.058(4) Uani 1 1 d . . . C19 C 0.7990(13) 0.8250(12) 0.7529(14) 0.060(5) Uani 1 1 d . . . H19 H 0.7488 0.8301 0.7894 0.072 Uiso 1 1 calc R . . C20 C 0.8920(16) 0.9088(14) 0.7802(14) 0.068(5) Uani 1 1 d . . . H20 H 0.9074 0.9693 0.8357 0.082 Uiso 1 1 calc R . . C21 C 0.9617(15) 0.9017(14) 0.7247(15) 0.077(6) Uani 1 1 d . . . H21 H 1.0243 0.9599 0.7407 0.092 Uiso 1 1 calc R . . C22 C 0.9435(13) 0.8107(13) 0.6441(15) 0.069(5) Uani 1 1 d . . . H22 H 0.9917 0.8061 0.6056 0.083 Uiso 1 1 calc R . . C23 C 0.8487(12) 0.7271(13) 0.6251(13) 0.053(4) Uani 1 1 d . . . C24 C 0.8192(15) 0.6191(12) 0.5463(12) 0.052(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0583(13) 0.0491(13) 0.0546(15) 0.0110(10) 0.0275(10) 0.0115(9) Ni2 0.0614(13) 0.0399(12) 0.0501(14) 0.0098(10) 0.0277(10) 0.0102(9) Ni3 0.0663(13) 0.0414(13) 0.0508(14) 0.0106(10) 0.0303(11) 0.0096(9) Ni4 0.0578(12) 0.0417(12) 0.0492(14) 0.0064(10) 0.0249(10) 0.0083(9) Br1 0.158(2) 0.147(3) 0.112(2) -0.0082(18) 0.0617(19) 0.0496(19) Br2 0.158(2) 0.105(2) 0.138(3) 0.0211(18) 0.059(2) 0.0256(17) O1 0.060(6) 0.042(6) 0.064(8) 0.012(5) 0.030(6) 0.002(5) O2 0.059(6) 0.035(6) 0.051(7) -0.005(5) 0.042(5) 0.001(4) O3 0.069(6) 0.031(6) 0.047(7) 0.007(5) 0.028(5) 0.001(4) O4 0.034(5) 0.039(6) 0.085(8) 0.008(6) 0.035(5) 0.009(4) O1W 0.086(9) 0.109(11) 0.083(10) 0.016(8) 0.029(7) 0.019(7) O2W 0.060(7) 0.091(9) 0.048(7) 0.014(6) 0.026(6) 0.024(6) O3W 0.118(10) 0.101(10) 0.054(8) 0.001(7) 0.055(7) -0.009(7) O4W 0.143(13) 0.182(17) 0.056(10) 0.016(10) 0.050(9) 0.022(11) O5W 0.156(14) 0.137(14) 0.097(12) 0.022(10) 0.080(11) 0.026(10) O6W 0.187(18) 0.157(19) 0.21(2) -0.031(16) 0.076(16) -0.008(14) O7W 0.189(15) 0.074(11) 0.27(2) 0.026(12) 0.188(16) 0.041(10) O8W 0.121(11) 0.148(14) 0.093(11) 0.046(10) 0.060(9) 0.066(10) O9W 0.118(11) 0.095(11) 0.118(13) -0.008(9) 0.022(10) 0.019(8) N1 0.048(8) 0.059(10) 0.092(12) 0.017(9) 0.043(8) 0.010(6) N2 0.085(10) 0.059(10) 0.046(9) -0.002(7) 0.036(8) 0.013(7) N3 0.101(12) 0.078(12) 0.101(13) 0.026(10) 0.065(10) 0.031(9) N4 0.063(8) 0.044(8) 0.038(8) 0.009(6) 0.025(6) 0.008(6) N5 0.062(8) 0.028(7) 0.067(9) 0.021(6) 0.040(7) 0.016(5) N6 0.099(10) 0.039(8) 0.070(10) 0.023(7) 0.057(9) 0.010(7) N7 0.069(8) 0.043(8) 0.055(9) 0.015(7) 0.041(7) 0.019(6) N8 0.058(8) 0.032(7) 0.044(8) 0.001(6) 0.030(6) 0.018(5) N9 0.073(9) 0.068(10) 0.048(9) -0.002(8) 0.029(7) 0.011(7) N10 0.056(8) 0.033(7) 0.053(9) 0.010(6) 0.025(7) 0.010(5) N11 0.041(7) 0.041(8) 0.070(10) 0.013(7) 0.024(7) 0.014(6) N12 0.066(8) 0.033(7) 0.060(10) 0.001(6) 0.026(7) -0.002(6) C1 0.061(12) 0.085(15) 0.062(13) -0.005(11) 0.027(10) 0.001(9) C2 0.102(14) 0.061(13) 0.058(13) 0.009(10) 0.041(11) 0.003(10) C3 0.102(14) 0.053(12) 0.075(14) 0.020(10) 0.058(11) 0.012(10) C4 0.073(12) 0.092(15) 0.053(12) 0.001(10) 0.037(10) 0.032(10) C5 0.084(13) 0.047(11) 0.069(14) 0.022(10) 0.027(10) 0.026(9) C6 0.087(13) 0.063(13) 0.057(13) 0.020(10) 0.015(10) 0.028(10) C7 0.051(9) 0.064(12) 0.044(10) 0.007(9) 0.027(8) 0.020(8) C8 0.082(12) 0.034(10) 0.077(13) 0.003(8) 0.049(10) 0.020(8) C9 0.080(12) 0.048(11) 0.058(13) -0.004(9) 0.020(10) -0.002(9) C10 0.081(11) 0.047(10) 0.057(12) 0.012(9) 0.044(9) 0.018(8) C11 0.076(11) 0.038(9) 0.049(11) 0.023(8) 0.032(9) 0.008(7) C12 0.049(9) 0.044(10) 0.063(12) 0.018(9) 0.024(8) 0.016(7) C13 0.072(11) 0.080(13) 0.046(11) 0.026(9) 0.032(9) 0.007(9) C14 0.076(13) 0.090(16) 0.067(14) 0.028(12) 0.027(11) 0.014(10) C15 0.081(12) 0.071(13) 0.059(13) 0.030(10) 0.039(10) 0.029(10) C16 0.075(11) 0.056(11) 0.050(11) 0.008(9) 0.033(9) 0.017(9) C17 0.083(12) 0.062(12) 0.055(12) 0.021(9) 0.042(10) 0.042(9) C18 0.056(10) 0.062(12) 0.053(12) 0.006(10) 0.020(8) 0.026(8) C19 0.062(11) 0.042(10) 0.079(13) 0.008(9) 0.034(9) 0.015(8) C20 0.097(14) 0.056(12) 0.063(13) 0.010(9) 0.054(11) -0.003(9) C21 0.075(13) 0.053(12) 0.070(14) -0.002(10) 0.012(10) -0.017(9) C22 0.043(10) 0.059(12) 0.089(15) 0.009(10) 0.021(9) -0.013(8) C23 0.032(9) 0.069(12) 0.050(11) 0.010(9) 0.009(7) 0.021(7) C24 0.083(12) 0.045(10) 0.026(9) -0.002(7) 0.023(8) 0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 1.821(9) . ? Ni1 N12 1.827(12) . ? Ni1 N2 1.852(14) . ? Ni1 N1 1.909(14) . ? Ni2 O1 2.011(10) . ? Ni2 N4 2.023(12) . ? Ni2 O4 2.033(9) . ? Ni2 N5 2.101(11) . ? Ni2 O1W 2.147(12) . ? Ni2 O3 2.163(10) 2_666 ? Ni3 O2 1.816(9) . ? Ni3 N6 1.825(13) . ? Ni3 N8 1.847(11) . ? Ni3 N7 1.864(12) . ? Ni4 N11 2.009(12) . ? Ni4 O3 2.036(10) . ? Ni4 O2 2.037(8) . ? Ni4 N10 2.081(11) . ? Ni4 O2W 2.114(10) . ? Ni4 N5 2.269(12) 2_666 ? O1 N2 1.345(16) . ? O2 N5 1.420(13) . ? O3 N8 1.359(14) . ? O3 Ni2 2.163(10) 2_666 ? O4 N11 1.415(15) . ? N1 C1 1.30(2) . ? N1 C5 1.33(2) . ? N2 C6 1.31(2) . ? N3 C6 1.39(2) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C7 1.330(17) . ? N4 C11 1.338(18) . ? N5 C12 1.297(17) . ? N5 Ni4 2.269(12) 2_666 ? N6 C12 1.337(19) . ? N6 H6 0.8600 . ? N7 C13 1.322(18) . ? N7 C17 1.406(19) . ? N8 C18 1.284(19) . ? N9 C18 1.329(19) . ? N9 H9A 0.8600 . ? N9 H9B 0.8600 . ? N10 C23 1.327(18) . ? N10 C19 1.354(18) . ? N11 C24 1.314(18) . ? N12 C24 1.365(18) . ? N12 H12 0.8600 . ? C1 C2 1.39(2) . ? C1 H1 0.9300 . ? C2 C3 1.33(2) . ? C2 H2 0.9300 . ? C3 C4 1.39(2) . ? C3 H3 0.9300 . ? C4 C5 1.40(2) . ? C4 H4 0.9300 . ? C5 C6 1.52(2) . ? C7 C8 1.37(2) . ? C7 H7 0.9300 . ? C8 C9 1.37(2) . ? C8 H8 0.9300 . ? C9 C10 1.37(2) . ? C9 H9 0.9300 . ? C10 C11 1.426(19) . ? C10 H10 0.9300 . ? C11 C12 1.50(2) . ? C13 C14 1.36(2) . ? C13 H13 0.9300 . ? C14 C15 1.37(2) . ? C14 H14 0.9300 . ? C15 C16 1.38(2) . ? C15 H15 0.9300 . ? C16 C17 1.38(2) . ? C16 H16 0.9300 . ? C17 C18 1.50(2) . ? C19 C20 1.35(2) . ? C19 H19 0.9300 . ? C20 C21 1.34(2) . ? C20 H20 0.9300 . ? C21 C22 1.39(2) . ? C21 H21 0.9300 . ? C22 C23 1.39(2) . ? C22 H22 0.9300 . ? C23 C24 1.51(2) . ? 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 O4 Ni1 N12 84.4(5) . . ? O4 Ni1 N2 89.4(5) . . ? N12 Ni1 N2 172.8(6) . . ? O4 Ni1 N1 169.5(5) . . ? N12 Ni1 N1 102.9(6) . . ? N2 Ni1 N1 83.7(6) . . ? O1 Ni2 N4 92.1(5) . . ? O1 Ni2 O4 86.5(4) . . ? N4 Ni2 O4 176.9(4) . . ? O1 Ni2 N5 170.1(4) . . ? N4 Ni2 N5 78.5(5) . . ? O4 Ni2 N5 103.1(4) . . ? O1 Ni2 O1W 93.5(5) . . ? N4 Ni2 O1W 94.1(5) . . ? O4 Ni2 O1W 83.3(5) . . ? N5 Ni2 O1W 90.0(5) . . ? O1 Ni2 O3 92.6(4) . 2_666 ? N4 Ni2 O3 87.2(4) . 2_666 ? O4 Ni2 O3 95.6(4) . 2_666 ? N5 Ni2 O3 84.2(4) . 2_666 ? O1W Ni2 O3 173.6(4) . 2_666 ? O2 Ni3 N6 84.4(5) . . ? O2 Ni3 N8 90.2(5) . . ? N6 Ni3 N8 174.7(6) . . ? O2 Ni3 N7 174.7(5) . . ? N6 Ni3 N7 100.5(6) . . ? N8 Ni3 N7 84.8(5) . . ? N11 Ni4 O3 171.3(4) . . ? N11 Ni4 O2 101.7(4) . . ? O3 Ni4 O2 83.6(4) . . ? N11 Ni4 N10 78.3(5) . . ? O3 Ni4 N10 96.9(4) . . ? O2 Ni4 N10 176.2(4) . . ? N11 Ni4 O2W 95.3(4) . . ? O3 Ni4 O2W 91.8(4) . . ? O2 Ni4 O2W 86.7(4) . . ? N10 Ni4 O2W 89.4(4) . . ? N11 Ni4 N5 90.2(4) . 2_666 ? O3 Ni4 N5 83.0(4) . 2_666 ? O2 Ni4 N5 88.5(4) . 2_666 ? N10 Ni4 N5 95.3(4) . 2_666 ? O2W Ni4 N5 173.4(4) . 2_666 ? N2 O1 Ni2 113.2(9) . . ? N5 O2 Ni3 113.7(7) . . ? N5 O2 Ni4 128.2(7) . . ? Ni3 O2 Ni4 117.0(4) . . ? N8 O3 Ni4 110.6(7) . . ? N8 O3 Ni2 111.9(7) . 2_666 ? Ni4 O3 Ni2 98.5(4) . 2_666 ? N11 O4 Ni1 115.8(7) . . ? N11 O4 Ni2 124.0(8) . . ? Ni1 O4 Ni2 120.1(5) . . ? C1 N1 C5 117.7(16) . . ? C1 N1 Ni1 125.4(13) . . ? C5 N1 Ni1 116.7(12) . . ? C6 N2 O1 116.8(14) . . ? C6 N2 Ni1 115.5(13) . . ? O1 N2 Ni1 127.5(10) . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C7 N4 C11 116.4(13) . . ? C7 N4 Ni2 128.8(11) . . ? C11 N4 Ni2 114.8(10) . . ? C12 N5 O2 109.1(12) . . ? C12 N5 Ni2 112.1(10) . . ? O2 N5 Ni2 126.1(7) . . ? C12 N5 Ni4 113.8(9) . 2_666 ? O2 N5 Ni4 100.4(7) . 2_666 ? Ni2 N5 Ni4 93.4(5) . 2_666 ? C12 N6 Ni3 111.4(10) . . ? C12 N6 H6 124.3 . . ? Ni3 N6 H6 124.3 . . ? C13 N7 C17 117.2(14) . . ? C13 N7 Ni3 129.9(12) . . ? C17 N7 Ni3 113.0(10) . . ? C18 N8 O3 118.0(13) . . ? C18 N8 Ni3 118.0(12) . . ? O3 N8 Ni3 124.0(9) . . ? C18 N9 H9A 120.0 . . ? C18 N9 H9B 120.0 . . ? H9A N9 H9B 120.0 . . ? C23 N10 C19 117.6(13) . . ? C23 N10 Ni4 115.6(10) . . ? C19 N10 Ni4 126.6(11) . . ? C24 N11 O4 108.0(12) . . ? C24 N11 Ni4 117.1(10) . . ? O4 N11 Ni4 132.8(8) . . ? C24 N12 Ni1 111.0(10) . . ? C24 N12 H12 124.5 . . ? Ni1 N12 H12 124.5 . . ? N1 C1 C2 121.4(17) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 120.9(18) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.9(18) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 115.0(17) . . ? C3 C4 H4 122.5 . . ? C5 C4 H4 122.5 . . ? N1 C5 C4 125.0(18) . . ? N1 C5 C6 108.9(17) . . ? C4 C5 C6 125.8(17) . . ? N2 C6 N3 123.4(18) . . ? N2 C6 C5 115.1(17) . . ? N3 C6 C5 121.5(18) . . ? N4 C7 C8 125.9(14) . . ? N4 C7 H7 117.1 . . ? C8 C7 H7 117.1 . . ? C7 C8 C9 114.7(15) . . ? C7 C8 H8 122.7 . . ? C9 C8 H8 122.7 . . ? C10 C9 C8 125.1(16) . . ? C10 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? C9 C10 C11 113.1(15) . . ? C9 C10 H10 123.5 . . ? C11 C10 H10 123.5 . . ? N4 C11 C10 124.7(15) . . ? N4 C11 C12 114.6(13) . . ? C10 C11 C12 120.6(14) . . ? N5 C12 N6 120.2(14) . . ? N5 C12 C11 113.8(15) . . ? N6 C12 C11 125.9(14) . . ? N7 C13 C14 121.7(18) . . ? N7 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 121.3(19) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 120.0(18) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 116.4(16) . . ? C17 C16 H16 121.8 . . ? C15 C16 H16 121.8 . . ? C16 C17 N7 123.3(16) . . ? C16 C17 C18 125.1(15) . . ? N7 C17 C18 111.3(14) . . ? N8 C18 N9 126.7(17) . . ? N8 C18 C17 112.5(15) . . ? N9 C18 C17 120.8(16) . . ? N10 C19 C20 123.3(16) . . ? N10 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 117.8(17) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C20 C21 C22 122.4(16) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 115.5(17) . . ? C21 C22 H22 122.3 . . ? C23 C22 H22 122.3 . . ? N10 C23 C22 123.3(15) . . ? N10 C23 C24 113.1(14) . . ? C22 C23 C24 123.6(16) . . ? N11 C24 N12 120.6(13) . . ? N11 C24 C23 114.7(15) . . ? N12 C24 C23 124.6(15) . . ? 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 Ni2 O1 N2 166.1(9) . . . . ? O4 Ni2 O1 N2 -16.7(9) . . . . ? N5 Ni2 O1 N2 150(2) . . . . ? O1W Ni2 O1 N2 -99.7(9) . . . . ? O3 Ni2 O1 N2 78.8(9) 2_666 . . . ? N6 Ni3 O2 N5 9.1(8) . . . . ? N8 Ni3 O2 N5 -171.1(8) . . . . ? N7 Ni3 O2 N5 166(5) . . . . ? N6 Ni3 O2 Ni4 -160.3(6) . . . . ? N8 Ni3 O2 Ni4 19.4(6) . . . . ? N7 Ni3 O2 Ni4 -3(5) . . . . ? N11 Ni4 O2 N5 -12.0(10) . . . . ? O3 Ni4 O2 N5 161.0(10) . . . . ? N10 Ni4 O2 N5 -101(7) . . . . ? O2W Ni4 O2 N5 -106.8(9) . . . . ? N5 Ni4 O2 N5 77.9(10) 2_666 . . . ? N11 Ni4 O2 Ni3 155.6(5) . . . . ? O3 Ni4 O2 Ni3 -31.4(5) . . . . ? N10 Ni4 O2 Ni3 67(7) . . . . ? O2W Ni4 O2 Ni3 60.9(5) . . . . ? N5 Ni4 O2 Ni3 -114.5(6) 2_666 . . . ? N11 Ni4 O3 N8 163(3) . . . . ? O2 Ni4 O3 N8 35.2(8) . . . . ? N10 Ni4 O3 N8 -141.0(8) . . . . ? O2W Ni4 O3 N8 -51.3(8) . . . . ? N5 Ni4 O3 N8 124.5(8) 2_666 . . . ? N11 Ni4 O3 Ni2 46(3) . . . 2_666 ? O2 Ni4 O3 Ni2 -82.1(4) . . . 2_666 ? N10 Ni4 O3 Ni2 101.7(4) . . . 2_666 ? O2W Ni4 O3 Ni2 -168.6(4) . . . 2_666 ? N5 Ni4 O3 Ni2 7.2(4) 2_666 . . 2_666 ? N12 Ni1 O4 N11 -3.4(9) . . . . ? N2 Ni1 O4 N11 172.8(9) . . . . ? N1 Ni1 O4 N11 -138(3) . . . . ? N12 Ni1 O4 Ni2 -179.7(6) . . . . ? N2 Ni1 O4 Ni2 -3.4(7) . . . . ? N1 Ni1 O4 Ni2 46(3) . . . . ? O1 Ni2 O4 N11 -165.2(9) . . . . ? N4 Ni2 O4 N11 -102(9) . . . . ? N5 Ni2 O4 N11 17.2(10) . . . . ? O1W Ni2 O4 N11 -71.2(9) . . . . ? O3 Ni2 O4 N11 102.5(9) 2_666 . . . ? O1 Ni2 O4 Ni1 10.7(6) . . . . ? N4 Ni2 O4 Ni1 74(9) . . . . ? N5 Ni2 O4 Ni1 -166.9(5) . . . . ? O1W Ni2 O4 Ni1 104.7(6) . . . . ? O3 Ni2 O4 Ni1 -81.6(6) 2_666 . . . ? O4 Ni1 N1 C1 125(3) . . . . ? N12 Ni1 N1 C1 -8.0(15) . . . . ? N2 Ni1 N1 C1 175.0(15) . . . . ? O4 Ni1 N1 C5 -51(3) . . . . ? N12 Ni1 N1 C5 175.9(11) . . . . ? N2 Ni1 N1 C5 -1.2(12) . . . . ? Ni2 O1 N2 C6 -164.7(12) . . . . ? Ni2 O1 N2 Ni1 21.3(15) . . . . ? O4 Ni1 N2 C6 174.3(13) . . . . ? N12 Ni1 N2 C6 -154(4) . . . . ? N1 Ni1 N2 C6 2.4(13) . . . . ? O4 Ni1 N2 O1 -11.6(13) . . . . ? N12 Ni1 N2 O1 20(5) . . . . ? N1 Ni1 N2 O1 176.4(13) . . . . ? O1 Ni2 N4 C7 -9.4(12) . . . . ? O4 Ni2 N4 C7 -72(9) . . . . ? N5 Ni2 N4 C7 167.7(13) . . . . ? O1W Ni2 N4 C7 -103.1(12) . . . . ? O3 Ni2 N4 C7 83.1(12) 2_666 . . . ? O1 Ni2 N4 C11 170.1(10) . . . . ? O4 Ni2 N4 C11 107(9) . . . . ? N5 Ni2 N4 C11 -12.7(10) . . . . ? O1W Ni2 N4 C11 76.4(11) . . . . ? O3 Ni2 N4 C11 -97.3(10) 2_666 . . . ? Ni3 O2 N5 C12 -11.4(12) . . . . ? Ni4 O2 N5 C12 156.6(9) . . . . ? Ni3 O2 N5 Ni2 -149.5(6) . . . . ? Ni4 O2 N5 Ni2 18.5(14) . . . . ? Ni3 O2 N5 Ni4 108.4(6) . . . 2_666 ? Ni4 O2 N5 Ni4 -83.6(8) . . . 2_666 ? O1 Ni2 N5 C12 39(3) . . . . ? N4 Ni2 N5 C12 22.2(10) . . . . ? O4 Ni2 N5 C12 -155.0(10) . . . . ? O1W Ni2 N5 C12 -72.0(11) . . . . ? O3 Ni2 N5 C12 110.5(11) 2_666 . . . ? O1 Ni2 N5 O2 176(2) . . . . ? N4 Ni2 N5 O2 159.3(10) . . . . ? O4 Ni2 N5 O2 -18.0(10) . . . . ? O1W Ni2 N5 O2 65.1(10) . . . . ? O3 Ni2 N5 O2 -112.4(10) 2_666 . . . ? O1 Ni2 N5 Ni4 -78(3) . . . 2_666 ? N4 Ni2 N5 Ni4 -95.3(5) . . . 2_666 ? O4 Ni2 N5 Ni4 87.5(4) . . . 2_666 ? O1W Ni2 N5 Ni4 170.6(5) . . . 2_666 ? O3 Ni2 N5 Ni4 -6.9(4) 2_666 . . 2_666 ? O2 Ni3 N6 C12 -4.9(11) . . . . ? N8 Ni3 N6 C12 -8(7) . . . . ? N7 Ni3 N6 C12 177.2(10) . . . . ? O2 Ni3 N7 C13 -162(5) . . . . ? N6 Ni3 N7 C13 -4.6(15) . . . . ? N8 Ni3 N7 C13 175.9(14) . . . . ? O2 Ni3 N7 C17 18(6) . . . . ? N6 Ni3 N7 C17 174.5(10) . . . . ? N8 Ni3 N7 C17 -5.0(10) . . . . ? Ni4 O3 N8 C18 148.7(10) . . . . ? Ni2 O3 N8 C18 -102.6(12) 2_666 . . . ? Ni4 O3 N8 Ni3 -34.2(11) . . . . ? Ni2 O3 N8 Ni3 74.6(10) 2_666 . . . ? O2 Ni3 N8 C18 -172.9(11) . . . . ? N6 Ni3 N8 C18 -170(6) . . . . ? N7 Ni3 N8 C18 5.1(11) . . . . ? O2 Ni3 N8 O3 10.0(10) . . . . ? N6 Ni3 N8 O3 13(6) . . . . ? N7 Ni3 N8 O3 -172.1(10) . . . . ? N11 Ni4 N10 C23 5.3(10) . . . . ? O3 Ni4 N10 C23 -167.4(10) . . . . ? O2 Ni4 N10 C23 95(7) . . . . ? O2W Ni4 N10 C23 100.8(10) . . . . ? N5 Ni4 N10 C23 -83.8(10) 2_666 . . . ? N11 Ni4 N10 C19 -170.4(13) . . . . ? O3 Ni4 N10 C19 16.9(12) . . . . ? O2 Ni4 N10 C19 -81(7) . . . . ? O2W Ni4 N10 C19 -74.9(12) . . . . ? N5 Ni4 N10 C19 100.5(12) 2_666 . . . ? Ni1 O4 N11 C24 2.5(14) . . . . ? Ni2 O4 N11 C24 178.6(9) . . . . ? Ni1 O4 N11 Ni4 165.2(7) . . . . ? Ni2 O4 N11 Ni4 -18.7(16) . . . . ? O3 Ni4 N11 C24 47(3) . . . . ? O2 Ni4 N11 C24 174.1(11) . . . . ? N10 Ni4 N11 C24 -9.9(11) . . . . ? O2W Ni4 N11 C24 -98.2(11) . . . . ? N5 Ni4 N11 C24 85.5(11) 2_666 . . . ? O3 Ni4 N11 O4 -114(3) . . . . ? O2 Ni4 N11 O4 12.6(12) . . . . ? N10 Ni4 N11 O4 -171.4(13) . . . . ? O2W Ni4 N11 O4 100.3(12) . . . . ? N5 Ni4 N11 O4 -76.0(12) 2_666 . . . ? O4 Ni1 N12 C24 3.4(10) . . . . ? N2 Ni1 N12 C24 -28(5) . . . . ? N1 Ni1 N12 C24 175.7(10) . . . . ? C5 N1 C1 C2 3(3) . . . . ? Ni1 N1 C1 C2 -173.1(13) . . . . ? N1 C1 C2 C3 -2(3) . . . . ? C1 C2 C3 C4 1(3) . . . . ? C2 C3 C4 C5 -1(3) . . . . ? C1 N1 C5 C4 -3(3) . . . . ? Ni1 N1 C5 C4 173.1(13) . . . . ? C1 N1 C5 C6 -176.5(15) . . . . ? Ni1 N1 C5 C6 0.0(17) . . . . ? C3 C4 C5 N1 2(3) . . . . ? C3 C4 C5 C6 174.2(15) . . . . ? O1 N2 C6 N3 5(2) . . . . ? Ni1 N2 C6 N3 -180.0(12) . . . . ? O1 N2 C6 C5 -177.7(12) . . . . ? Ni1 N2 C6 C5 -3.0(19) . . . . ? N1 C5 C6 N2 2(2) . . . . ? C4 C5 C6 N2 -171.2(16) . . . . ? N1 C5 C6 N3 179.0(14) . . . . ? C4 C5 C6 N3 6(3) . . . . ? C11 N4 C7 C8 -1(2) . . . . ? Ni2 N4 C7 C8 178.5(12) . . . . ? N4 C7 C8 C9 4(2) . . . . ? C7 C8 C9 C10 -4(3) . . . . ? C8 C9 C10 C11 2(2) . . . . ? C7 N4 C11 C10 -2(2) . . . . ? Ni2 N4 C11 C10 178.9(11) . . . . ? C7 N4 C11 C12 -177.5(12) . . . . ? Ni2 N4 C11 C12 2.8(16) . . . . ? C9 C10 C11 N4 1(2) . . . . ? C9 C10 C11 C12 177.1(14) . . . . ? O2 N5 C12 N6 7.8(18) . . . . ? Ni2 N5 C12 N6 152.2(11) . . . . ? Ni4 N5 C12 N6 -103.4(14) 2_666 . . . ? O2 N5 C12 C11 -171.1(10) . . . . ? Ni2 N5 C12 C11 -26.7(15) . . . . ? Ni4 N5 C12 C11 77.7(13) 2_666 . . . ? Ni3 N6 C12 N5 -0.7(18) . . . . ? Ni3 N6 C12 C11 178.0(11) . . . . ? N4 C11 C12 N5 16.6(18) . . . . ? C10 C11 C12 N5 -159.6(14) . . . . ? N4 C11 C12 N6 -162.2(14) . . . . ? C10 C11 C12 N6 22(2) . . . . ? C17 N7 C13 C14 0(2) . . . . ? Ni3 N7 C13 C14 178.8(12) . . . . ? N7 C13 C14 C15 2(3) . . . . ? C13 C14 C15 C16 -2(3) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C15 C16 C17 N7 2(2) . . . . ? C15 C16 C17 C18 175.8(15) . . . . ? C13 N7 C17 C16 -2(2) . . . . ? Ni3 N7 C17 C16 179.2(12) . . . . ? C13 N7 C17 C18 -176.5(13) . . . . ? Ni3 N7 C17 C18 4.3(15) . . . . ? O3 N8 C18 N9 -5(2) . . . . ? Ni3 N8 C18 N9 177.7(11) . . . . ? O3 N8 C18 C17 173.6(11) . . . . ? Ni3 N8 C18 C17 -3.7(17) . . . . ? C16 C17 C18 N8 -175.3(15) . . . . ? N7 C17 C18 N8 -0.5(18) . . . . ? C16 C17 C18 N9 3(2) . . . . ? N7 C17 C18 N9 178.2(12) . . . . ? C23 N10 C19 C20 1(2) . . . . ? Ni4 N10 C19 C20 176.8(13) . . . . ? N10 C19 C20 C21 2(3) . . . . ? C19 C20 C21 C22 -2(3) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C19 N10 C23 C22 -4(2) . . . . ? Ni4 N10 C23 C22 179.9(12) . . . . ? C19 N10 C23 C24 175.5(12) . . . . ? Ni4 N10 C23 C24 -0.6(16) . . . . ? C21 C22 C23 N10 4(2) . . . . ? C21 C22 C23 C24 -176.0(15) . . . . ? O4 N11 C24 N12 0.5(19) . . . . ? Ni4 N11 C24 N12 -165.4(11) . . . . ? O4 N11 C24 C23 178.3(11) . . . . ? Ni4 N11 C24 C23 12.4(17) . . . . ? Ni1 N12 C24 N11 -3.1(18) . . . . ? Ni1 N12 C24 C23 179.3(11) . . . . ? N10 C23 C24 N11 -7.6(19) . . . . ? C22 C23 C24 N11 172.0(15) . . . . ? N10 C23 C24 N12 170.2(14) . . . . ? C22 C23 C24 N12 -10(2) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.113 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.171 #===End data_6 _database_code_depnum_ccdc_archive 'CCDC 770176' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H76 N34 Ni8 O20' _chemical_formula_weight 2087.25 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 P2(1)/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 12.939(1) _cell_length_b 18.097(2) _cell_length_c 20.456(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.94(1) _cell_angle_gamma 90.00 _cell_volume 4411.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2573 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 25.00 _exptl_crystal_description platelet _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2140 _exptl_absorpt_coefficient_mu 1.752 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7252 _exptl_absorpt_correction_T_max 0.8278 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33670 _diffrn_reflns_av_R_equivalents 0.2327 _diffrn_reflns_av_sigmaI/netI 0.1968 _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 -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7737 _reflns_number_gt 2570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0916P)^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 7737 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2540 _refine_ls_R_factor_gt 0.0972 _refine_ls_wR_factor_ref 0.2455 _refine_ls_wR_factor_gt 0.1996 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.54000(12) 0.42610(9) 0.43566(9) 0.0650(5) Uani 1 1 d . . . Ni2 Ni 0.39897(12) 0.35833(8) 0.52919(9) 0.0632(5) Uani 1 1 d . . . Ni3 Ni 0.13692(12) 0.42436(10) 0.45590(9) 0.0689(5) Uani 1 1 d . . . Ni4 Ni 0.28436(12) 0.48905(9) 0.35997(9) 0.0661(5) Uani 1 1 d . . . N1 N 0.5138(8) 0.2734(5) 0.5570(5) 0.067(3) Uani 1 1 d . . . N2 N 0.5475(7) 0.4137(5) 0.5615(5) 0.061(3) Uani 1 1 d . . . N3 N 0.7309(8) 0.4091(5) 0.6457(5) 0.067(3) Uani 1 1 d . . . H3A H 0.7900 0.3858 0.6729 0.080 Uiso 1 1 calc R . . N4 N 0.6555(9) 0.3420(6) 0.4562(6) 0.072(3) Uani 1 1 d . . . N5 N 0.6871(7) 0.4820(5) 0.4743(5) 0.059(3) Uani 1 1 d . . . N6 N 0.8803(8) 0.4744(5) 0.5363(5) 0.071(3) Uani 1 1 d . . . H6A H 0.9437 0.4517 0.5535 0.085 Uiso 1 1 calc R . . N7 N -0.0135(9) 0.3967(8) 0.3974(6) 0.090(4) Uani 1 1 d . . . N8 N 0.1652(9) 0.3246(6) 0.4563(6) 0.069(3) Uani 1 1 d . . . N9 N 0.0869(9) 0.2061(8) 0.4109(7) 0.115(5) Uani 1 1 d . . . H9A H 0.1512 0.1854 0.4322 0.138 Uiso 1 1 calc R . . H9B H 0.0297 0.1799 0.3858 0.138 Uiso 1 1 calc R . . N10 N 0.1490(8) 0.4553(7) 0.2912(6) 0.078(3) Uani 1 1 d . . . N11 N 0.3107(8) 0.3875(5) 0.3716(5) 0.056(2) Uani 1 1 d . . . N12 N 0.2537(9) 0.2696(6) 0.3312(5) 0.088(4) Uani 1 1 d . . . H12A H 0.3156 0.2520 0.3615 0.106 Uiso 1 1 calc R . . H12B H 0.2040 0.2404 0.3028 0.106 Uiso 1 1 calc R . . N13 N 0.3960(10) 0.3503(6) 0.6296(6) 0.076(3) Uani 1 1 d . . . N14 N 0.3323(13) 0.3621(8) 0.7131(9) 0.113(4) Uani 1 1 d . . . H14 H 0.2874 0.3717 0.7338 0.136 Uiso 1 1 calc R . . N15 N 0.5065(8) 0.4229(7) 0.3295(6) 0.072(3) Uani 1 1 d . . . N16 N 0.4639(13) 0.4549(11) 0.2179(9) 0.126(5) Uani 1 1 d . . . H16 H 0.4562 0.4815 0.1815 0.152 Uiso 1 1 calc R . . N17 N 0.0421(18) 0.3507(10) 0.6905(11) 0.133(6) Uani 1 1 d . . . O1 O 0.5724(5) 0.4914(4) 0.5770(4) 0.063(2) Uani 1 1 d . . . O2 O 0.7138(6) 0.5576(4) 0.4933(4) 0.066(2) Uani 1 1 d . . . O3 O 0.2659(7) 0.2902(4) 0.4897(5) 0.074(2) Uani 1 1 d . . . O4 O 0.4076(6) 0.3592(4) 0.4243(4) 0.065(2) Uani 1 1 d . . . O5 O 0.1245(11) 0.3627(8) 0.7484(8) 0.151(5) Uani 1 1 d . . . O6 O -0.0434(11) 0.3249(8) 0.6884(11) 0.214(10) Uani 1 1 d . . . O7 O 0.0637(10) 0.3774(9) 0.6404(9) 0.178(6) Uani 1 1 d . . . O8 O 0.3749(18) 0.1040(18) 0.3947(8) 0.38(2) Uani 1 1 d . . . O9 O 0.2418(19) 0.1871(11) 0.5878(10) 0.324(12) Uani 1 1 d . . . O10 O 0.5895(17) 0.0466(12) 0.4037(11) 0.293(10) Uani 1 1 d . . . C1 C 0.4919(11) 0.2007(8) 0.5476(7) 0.080(4) Uani 1 1 d . . . H1A H 0.4187 0.1851 0.5216 0.096 Uiso 1 1 calc R . . C2 C 0.5751(15) 0.1490(8) 0.5755(9) 0.102(5) Uani 1 1 d . . . H2A H 0.5581 0.0990 0.5675 0.123 Uiso 1 1 calc R . . C3 C 0.6829(12) 0.1702(8) 0.6149(8) 0.084(4) Uani 1 1 d . . . H3B H 0.7385 0.1352 0.6363 0.101 Uiso 1 1 calc R . . C4 C 0.7073(11) 0.2441(9) 0.6223(7) 0.086(4) Uani 1 1 d . . . H4A H 0.7815 0.2590 0.6454 0.103 Uiso 1 1 calc R . . C5 C 0.6223(10) 0.2984(8) 0.5956(7) 0.070(4) Uani 1 1 d . . . C6 C 0.6375(11) 0.3775(7) 0.6018(7) 0.063(3) Uani 1 1 d . . . C7 C 0.6351(12) 0.2698(8) 0.4425(7) 0.085(4) Uani 1 1 d . . . H7A H 0.5609 0.2538 0.4236 0.101 Uiso 1 1 calc R . . C8 C 0.7206(13) 0.2172(8) 0.4553(8) 0.095(5) Uani 1 1 d . . . H8A H 0.7025 0.1685 0.4411 0.114 Uiso 1 1 calc R . . C9 C 0.8269(13) 0.2371(8) 0.4877(8) 0.087(5) Uani 1 1 d . . . H9C H 0.8837 0.2019 0.4995 0.105 Uiso 1 1 calc R . . C10 C 0.8525(11) 0.3113(8) 0.5039(8) 0.085(4) Uani 1 1 d . . . H10A H 0.9265 0.3269 0.5263 0.103 Uiso 1 1 calc R . . C11 C 0.7641(11) 0.3615(7) 0.4855(7) 0.067(4) Uani 1 1 d . . . C12 C 0.7784(11) 0.4398(8) 0.4994(7) 0.070(4) Uani 1 1 d . . . C13 C -0.1027(11) 0.4450(10) 0.3696(8) 0.101(5) Uani 1 1 d . . . H13 H -0.0971 0.4955 0.3790 0.121 Uiso 1 1 calc R . . C14 C -0.2058(12) 0.4092(15) 0.3242(10) 0.140(8) Uani 1 1 d . . . H14B H -0.2688 0.4391 0.3041 0.169 Uiso 1 1 calc R . . C15 C -0.2191(14) 0.3365(12) 0.3084(9) 0.101(6) Uani 1 1 d . . . H15A H -0.2876 0.3173 0.2778 0.121 Uiso 1 1 calc R . . C16 C -0.1312(13) 0.2945(10) 0.3381(8) 0.105(6) Uani 1 1 d . . . H16B H -0.1375 0.2438 0.3299 0.126 Uiso 1 1 calc R . . C17 C -0.0303(13) 0.3237(9) 0.3810(8) 0.078(4) Uani 1 1 d . . . C18 C 0.0752(14) 0.2843(10) 0.4170(8) 0.093(5) Uani 1 1 d . . . C19 C 0.0586(12) 0.4955(9) 0.2509(9) 0.105(5) Uani 1 1 d . . . H19 H 0.0590 0.5465 0.2566 0.126 Uiso 1 1 calc R . . C20 C -0.0379(13) 0.4600(16) 0.1995(10) 0.162(10) Uani 1 1 d . . . H20A H -0.0986 0.4884 0.1710 0.194 Uiso 1 1 calc R . . C21 C -0.0417(18) 0.3852(12) 0.1919(11) 0.152(9) Uani 1 1 d . . . H21A H -0.1035 0.3617 0.1583 0.183 Uiso 1 1 calc R . . C22 C 0.0462(12) 0.3476(10) 0.2342(9) 0.113(6) Uani 1 1 d . . . H22A H 0.0436 0.2963 0.2315 0.135 Uiso 1 1 calc R . . C23 C 0.1373(11) 0.3789(8) 0.2801(8) 0.082(4) Uani 1 1 d . . . C24 C 0.2342(12) 0.3451(9) 0.3281(7) 0.077(4) Uani 1 1 d . . . C25 C 0.4697(15) 0.3659(10) 0.2817(11) 0.107(5) Uani 1 1 d . . . H25A H 0.4667 0.3177 0.2967 0.129 Uiso 1 1 calc R . . C26 C 0.5023(13) 0.4798(10) 0.2866(11) 0.106(5) Uani 1 1 d . . . H26A H 0.5221 0.5283 0.3011 0.128 Uiso 1 1 calc R . . C27 C 0.4399(15) 0.3812(12) 0.2164(11) 0.110(6) Uani 1 1 d . . . H27 H 0.4094 0.3501 0.1773 0.132 Uiso 1 1 calc R . . C28 C 0.4753(13) 0.3308(9) 0.6942(10) 0.101(6) Uani 1 1 d . . . H28A H 0.5469 0.3150 0.7006 0.121 Uiso 1 1 calc R . . C29 C 0.3077(13) 0.3695(9) 0.6425(9) 0.100(5) Uani 1 1 d . . . H29A H 0.2395 0.3856 0.6088 0.120 Uiso 1 1 calc R . . C30 C 0.4410(15) 0.3366(9) 0.7461(11) 0.112(6) Uani 1 1 d . . . H30 H 0.4803 0.3261 0.7940 0.134 Uiso 1 1 calc R . . C31 C 0.279(2) 0.0978(11) 0.4232(13) 0.204(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0569(9) 0.0479(10) 0.0854(13) -0.0069(9) 0.0225(9) -0.0010(8) Ni2 0.0547(9) 0.0482(10) 0.0808(12) 0.0018(9) 0.0198(9) 0.0002(8) Ni3 0.0497(9) 0.0671(12) 0.0848(13) -0.0005(10) 0.0206(9) -0.0045(9) Ni4 0.0519(9) 0.0587(12) 0.0785(12) -0.0024(9) 0.0155(9) -0.0052(8) N1 0.067(7) 0.033(6) 0.097(8) 0.007(6) 0.028(6) 0.003(5) N2 0.054(6) 0.040(7) 0.082(7) -0.011(6) 0.020(6) -0.007(5) N3 0.059(6) 0.036(6) 0.094(8) 0.011(6) 0.017(6) 0.007(5) N4 0.080(8) 0.033(7) 0.111(9) 0.010(6) 0.045(7) 0.021(6) N5 0.048(6) 0.050(7) 0.077(7) 0.011(6) 0.020(5) 0.003(5) N6 0.057(6) 0.052(7) 0.102(8) 0.006(6) 0.029(6) 0.012(5) N7 0.057(7) 0.103(11) 0.103(10) -0.005(8) 0.024(7) -0.011(8) N8 0.066(7) 0.055(7) 0.086(8) -0.015(6) 0.030(6) -0.007(6) N9 0.079(8) 0.111(12) 0.154(12) -0.044(10) 0.044(8) -0.045(8) N10 0.048(6) 0.086(9) 0.079(8) 0.016(7) 0.002(6) -0.001(6) N11 0.053(6) 0.047(6) 0.055(7) 0.011(5) 0.007(5) 0.004(5) N12 0.091(8) 0.074(9) 0.088(9) -0.032(7) 0.022(7) -0.036(7) N13 0.061(7) 0.065(8) 0.092(9) 0.016(7) 0.019(7) 0.005(6) N14 0.140(13) 0.107(12) 0.118(12) 0.008(10) 0.078(11) -0.011(10) N15 0.064(6) 0.071(8) 0.093(9) -0.010(8) 0.042(6) 0.007(6) N16 0.128(12) 0.162(18) 0.080(12) 0.019(11) 0.031(9) 0.027(12) N17 0.130(17) 0.113(14) 0.146(19) 0.056(13) 0.045(15) 0.022(13) O1 0.043(4) 0.052(6) 0.084(6) -0.008(5) 0.014(4) 0.000(4) O2 0.046(4) 0.054(6) 0.092(6) -0.010(5) 0.018(4) -0.003(4) O3 0.062(5) 0.045(5) 0.109(7) 0.000(5) 0.028(5) -0.002(4) O4 0.063(5) 0.044(5) 0.078(6) -0.011(4) 0.018(5) -0.008(4) O5 0.110(10) 0.197(15) 0.132(11) 0.042(11) 0.030(9) 0.021(10) O6 0.104(10) 0.131(13) 0.43(3) 0.076(14) 0.132(15) 0.020(9) O7 0.088(9) 0.198(17) 0.196(16) 0.056(13) -0.004(10) 0.006(9) O8 0.27(2) 0.76(5) 0.074(10) -0.063(18) 0.027(12) 0.25(3) O9 0.37(3) 0.22(2) 0.220(18) 0.104(16) -0.057(18) -0.064(19) O10 0.32(2) 0.30(2) 0.28(2) -0.100(19) 0.14(2) -0.13(2) C1 0.071(9) 0.058(10) 0.096(11) 0.015(8) 0.016(8) -0.005(8) C2 0.112(13) 0.053(10) 0.144(15) 0.012(10) 0.054(12) 0.000(10) C3 0.074(10) 0.049(10) 0.124(13) 0.027(9) 0.032(10) 0.023(8) C4 0.072(9) 0.094(13) 0.076(10) 0.013(9) 0.012(8) -0.003(10) C5 0.055(8) 0.072(11) 0.080(10) 0.017(8) 0.023(8) 0.014(8) C6 0.056(8) 0.053(10) 0.072(10) 0.017(7) 0.017(7) 0.011(7) C7 0.097(10) 0.060(10) 0.101(11) 0.013(9) 0.043(9) 0.029(9) C8 0.100(12) 0.059(11) 0.136(14) 0.027(10) 0.058(12) 0.027(10) C9 0.094(11) 0.043(10) 0.129(13) 0.031(9) 0.048(11) 0.049(9) C10 0.079(9) 0.065(11) 0.116(12) 0.026(9) 0.042(9) 0.016(8) C11 0.067(9) 0.051(9) 0.094(11) 0.010(8) 0.042(8) 0.016(8) C12 0.056(8) 0.071(11) 0.082(10) 0.019(8) 0.027(8) 0.014(8) C13 0.049(8) 0.136(15) 0.112(12) 0.030(11) 0.024(8) -0.001(10) C14 0.033(8) 0.24(3) 0.128(16) -0.005(18) 0.011(9) -0.019(14) C15 0.047(9) 0.145(18) 0.096(13) -0.024(13) 0.011(9) -0.034(12) C16 0.057(9) 0.124(15) 0.117(13) -0.037(11) 0.016(9) -0.056(11) C17 0.084(11) 0.071(11) 0.095(11) 0.000(9) 0.050(10) 0.001(10) C18 0.094(12) 0.076(12) 0.106(13) -0.023(10) 0.036(10) -0.010(11) C19 0.082(11) 0.092(12) 0.137(15) -0.006(11) 0.039(11) -0.004(10) C20 0.050(10) 0.27(3) 0.113(15) -0.036(19) -0.023(9) -0.036(16) C21 0.117(17) 0.118(18) 0.148(19) -0.023(15) -0.029(14) -0.069(15) C22 0.053(9) 0.109(14) 0.129(14) -0.011(12) -0.016(9) -0.007(10) C23 0.055(9) 0.061(11) 0.103(12) -0.001(9) 0.001(8) -0.012(8) C24 0.081(10) 0.061(11) 0.081(11) -0.037(9) 0.023(9) -0.025(9) C25 0.149(15) 0.086(14) 0.094(14) -0.026(13) 0.056(13) -0.002(12) C26 0.132(14) 0.093(14) 0.098(15) 0.022(13) 0.049(12) 0.003(11) C27 0.133(15) 0.107(17) 0.082(15) -0.021(13) 0.032(12) -0.031(13) C28 0.090(12) 0.125(15) 0.102(14) 0.019(12) 0.055(12) 0.029(10) C29 0.092(11) 0.119(15) 0.099(14) 0.037(11) 0.046(11) -0.008(10) C30 0.096(13) 0.084(13) 0.137(18) 0.031(12) 0.024(13) 0.015(10) C31 0.22(2) 0.089(15) 0.19(2) -0.063(15) -0.051(19) 0.008(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.024(9) . ? Ni1 O1 2.028(7) 3_666 ? Ni1 O4 2.036(7) . ? Ni1 N15 2.043(11) . ? Ni1 N4 2.059(9) . ? Ni1 N2 2.548(10) . ? Ni2 O3 2.014(8) . ? Ni2 O2 2.032(7) 3_666 ? Ni2 N2 2.036(9) . ? Ni2 N1 2.058(9) . ? Ni2 N13 2.074(12) . ? Ni2 O4 2.192(8) . ? Ni3 O2 1.832(7) 3_666 ? Ni3 N8 1.841(10) . ? Ni3 N6 1.861(9) 3_666 ? Ni3 N7 1.912(11) . ? Ni4 O1 1.834(7) 3_666 ? Ni4 N3 1.853(9) 3_666 ? Ni4 N11 1.868(9) . ? Ni4 N10 1.871(10) . ? N1 C1 1.345(15) . ? N1 C5 1.392(14) . ? N2 C6 1.310(13) . ? N2 O1 1.451(11) . ? N3 C6 1.322(14) . ? N3 Ni4 1.853(9) 3_666 ? N4 C7 1.341(15) . ? N4 C11 1.342(15) . ? N5 C12 1.330(13) . ? N5 O2 1.428(11) . ? N6 C12 1.386(14) . ? N6 Ni3 1.861(9) 3_666 ? N7 C17 1.359(16) . ? N7 C13 1.382(16) . ? N8 C18 1.344(16) . ? N8 O3 1.363(11) . ? N9 C18 1.433(17) . ? N10 C19 1.351(16) . ? N10 C23 1.400(16) . ? N11 C24 1.293(14) . ? N11 O4 1.393(10) . ? N12 C24 1.387(15) . ? N13 C29 1.316(16) . ? N13 C28 1.365(17) . ? N14 C29 1.359(16) . ? N14 C30 1.380(17) . ? N15 C26 1.340(16) . ? N15 C25 1.372(17) . ? N16 C27 1.367(19) . ? N16 C26 1.371(18) . ? N17 O6 1.186(19) . ? N17 O7 1.258(18) . ? N17 O5 1.27(2) . ? O1 Ni4 1.834(7) 3_666 ? O1 Ni1 2.028(7) 3_666 ? O2 Ni3 1.832(7) 3_666 ? O2 Ni2 2.032(7) 3_666 ? O8 C31 1.56(3) . ? C1 C2 1.372(17) . ? C2 C3 1.366(18) . ? C3 C4 1.369(17) . ? C4 C5 1.417(17) . ? C5 C6 1.443(17) . ? C7 C8 1.404(16) . ? C8 C9 1.323(17) . ? C9 C10 1.391(18) . ? C10 C11 1.393(16) . ? C11 C12 1.444(17) . ? C13 C14 1.45(2) . ? C14 C15 1.35(2) . ? C15 C16 1.31(2) . ? C16 C17 1.365(18) . ? C17 C18 1.459(19) . ? C19 C20 1.43(2) . ? C20 C21 1.36(3) . ? C21 C22 1.32(2) . ? C22 C23 1.314(18) . ? C23 C24 1.397(18) . ? C25 C27 1.269(19) . ? C28 C30 1.306(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ni1 O1 101.5(4) . 3_666 ? N5 Ni1 O4 164.4(3) . . ? O1 Ni1 O4 83.9(3) 3_666 . ? N5 Ni1 N15 102.0(4) . . ? O1 Ni1 N15 92.3(4) 3_666 . ? O4 Ni1 N15 92.3(4) . . ? N5 Ni1 N4 78.0(4) . . ? O1 Ni1 N4 175.8(4) 3_666 . ? O4 Ni1 N4 95.5(4) . . ? N15 Ni1 N4 91.9(4) . . ? O3 Ni2 O2 86.6(3) . 3_666 ? O3 Ni2 N2 169.5(4) . . ? O2 Ni2 N2 102.1(4) 3_666 . ? O3 Ni2 N1 93.8(4) . . ? O2 Ni2 N1 177.2(4) 3_666 . ? N2 Ni2 N1 77.8(4) . . ? O3 Ni2 N13 90.7(4) . . ? O2 Ni2 N13 89.3(4) 3_666 . ? N2 Ni2 N13 95.3(4) . . ? N1 Ni2 N13 87.9(4) . . ? O3 Ni2 O4 88.5(3) . . ? O2 Ni2 O4 94.5(3) 3_666 . ? N2 Ni2 O4 85.0(3) . . ? N1 Ni2 O4 88.2(3) . . ? N13 Ni2 O4 176.0(4) . . ? O2 Ni3 N8 90.5(4) 3_666 . ? O2 Ni3 N6 84.9(4) 3_666 3_666 ? N8 Ni3 N6 174.6(5) . 3_666 ? O2 Ni3 N7 173.4(5) 3_666 . ? N8 Ni3 N7 84.2(6) . . ? N6 Ni3 N7 100.7(5) 3_666 . ? O1 Ni4 N3 84.6(4) 3_666 3_666 ? O1 Ni4 N11 90.9(4) 3_666 . ? N3 Ni4 N11 175.5(5) 3_666 . ? O1 Ni4 N10 170.3(5) 3_666 . ? N3 Ni4 N10 103.4(5) 3_666 . ? N11 Ni4 N10 81.1(5) . . ? C1 N1 C5 120.7(11) . . ? C1 N1 Ni2 127.0(9) . . ? C5 N1 Ni2 111.9(8) . . ? C6 N2 O1 106.3(9) . . ? C6 N2 Ni2 117.0(8) . . ? O1 N2 Ni2 130.5(6) . . ? Ni1 N2 Ni2 93.2(4) . . ? C6 N3 Ni4 109.9(8) . 3_666 ? C7 N4 C11 115.9(11) . . ? C7 N4 Ni1 127.6(10) . . ? C11 N4 Ni1 116.6(9) . . ? C12 N5 O2 111.1(10) . . ? C12 N5 Ni1 115.0(9) . . ? O2 N5 Ni1 132.5(6) . . ? C12 N6 Ni3 111.7(8) . 3_666 ? C17 N7 C13 119.1(13) . . ? C17 N7 Ni3 115.7(11) . . ? C13 N7 Ni3 125.1(11) . . ? C18 N8 O3 119.2(11) . . ? C18 N8 Ni3 113.9(10) . . ? O3 N8 Ni3 126.9(8) . . ? C19 N10 C23 114.8(12) . . ? C19 N10 Ni4 128.1(11) . . ? C23 N10 Ni4 117.1(9) . . ? C24 N11 O4 122.1(11) . . ? C24 N11 Ni4 116.3(10) . . ? O4 N11 Ni4 121.6(7) . . ? C29 N13 C28 104.9(13) . . ? C29 N13 Ni2 122.2(11) . . ? C28 N13 Ni2 132.8(11) . . ? C29 N14 C30 109.0(14) . . ? C26 N15 C25 101.4(14) . . ? C26 N15 Ni1 127.7(13) . . ? C25 N15 Ni1 130.5(13) . . ? C27 N16 C26 109.4(16) . . ? O6 N17 O7 128(2) . . ? O6 N17 O5 122(2) . . ? O7 N17 O5 109(2) . . ? N2 O1 Ni4 114.7(6) . 3_666 ? N2 O1 Ni1 126.8(6) . 3_666 ? Ni4 O1 Ni1 115.2(4) 3_666 3_666 ? N5 O2 Ni3 114.5(6) . 3_666 ? N5 O2 Ni2 125.4(6) . 3_666 ? Ni3 O2 Ni2 120.0(4) 3_666 3_666 ? N8 O3 Ni2 114.9(7) . . ? N11 O4 Ni1 109.5(6) . . ? N11 O4 Ni2 112.7(5) . . ? Ni1 O4 Ni2 104.7(3) . . ? N1 C1 C2 121.3(13) . . ? C3 C2 C1 120.6(14) . . ? C2 C3 C4 118.6(13) . . ? C3 C4 C5 121.7(13) . . ? N1 C5 C4 116.9(13) . . ? N1 C5 C6 116.5(11) . . ? C4 C5 C6 126.6(13) . . ? N2 C6 N3 124.4(12) . . ? N2 C6 C5 112.5(12) . . ? N3 C6 C5 123.0(11) . . ? N4 C7 C8 123.0(14) . . ? C9 C8 C7 120.0(15) . . ? C8 C9 C10 119.1(13) . . ? C9 C10 C11 118.1(13) . . ? N4 C11 C10 123.8(13) . . ? N4 C11 C12 112.2(11) . . ? C10 C11 C12 124.0(13) . . ? N5 C12 N6 117.7(12) . . ? N5 C12 C11 117.4(12) . . ? N6 C12 C11 124.9(11) . . ? N7 C13 C14 113.1(16) . . ? C15 C14 C13 126.1(19) . . ? C16 C15 C14 116.8(17) . . ? C15 C16 C17 121.0(17) . . ? N7 C17 C16 123.8(15) . . ? N7 C17 C18 108.8(14) . . ? C16 C17 C18 127.4(16) . . ? N8 C18 N9 119.4(14) . . ? N8 C18 C17 117.3(15) . . ? N9 C18 C17 123.3(15) . . ? N10 C19 C20 120.4(17) . . ? C21 C20 C19 121(2) . . ? C22 C21 C20 117.0(19) . . ? C23 C22 C21 123.4(18) . . ? C22 C23 C24 128.5(15) . . ? C22 C23 N10 123.5(15) . . ? C24 C23 N10 107.9(12) . . ? N11 C24 N12 118.4(14) . . ? N11 C24 C23 117.4(14) . . ? N12 C24 C23 124.1(12) . . ? C27 C25 N15 117.6(18) . . ? N15 C26 N16 108.9(16) . . ? C25 C27 N16 102.5(17) . . ? C30 C28 N13 113.7(14) . . ? N13 C29 N14 109.0(15) . . ? C28 C30 N14 103.4(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.013 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.118 #===End data_7 _database_code_depnum_ccdc_archive 'CCDC 770177' #TrackingRef '- dalton-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H114 Cl6 N36 Ni12 O36' _chemical_formula_weight 2977.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.743(3) _cell_length_b 14.563(3) _cell_length_c 14.993(3) _cell_angle_alpha 75.69(3) _cell_angle_beta 72.86(3) _cell_angle_gamma 85.06(3) _cell_volume 2778.1(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9364 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.49 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 2.220 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22611 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12165 _reflns_number_gt 9364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1031P)^2^+12.4400P] 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 12165 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2295 _refine_ls_wR_factor_gt 0.2120 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.004 _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 0.19290(5) -0.17671(5) -0.02650(5) 0.01873(19) Uani 1 1 d . . . Ni2 Ni 0.09741(6) 0.02310(5) -0.13068(5) 0.01894(19) Uani 1 1 d . . . Ni3 Ni 0.21718(6) -0.01361(6) 0.08564(5) 0.02060(19) Uani 1 1 d . . . Ni4 Ni 0.08126(6) -0.13491(6) -0.23785(5) 0.0214(2) Uani 1 1 d . . . Ni5 Ni 0.11221(6) 0.17669(6) -0.01877(5) 0.0203(2) Uani 1 1 d . . . Ni6 Ni 0.16434(6) -0.34723(6) -0.13799(5) 0.0208(2) Uani 1 1 d . . . Cl1 Cl 0.14986(17) 0.39236(13) 0.13937(14) 0.0455(5) Uani 1 1 d . . . Cl2A Cl 0.5974(8) -0.1571(10) -0.3942(8) 0.064(3) Uani 0.20 1 d P . . Cl2B Cl 0.6027(4) -0.0520(6) -0.4801(4) 0.090(2) Uani 0.50 1 d P . . Cl2C Cl 0.5746(10) -0.0974(12) -0.5759(9) 0.135(6) Uani 0.30 1 d P . . Cl3 Cl 0.2837(3) -0.2013(4) 0.3849(2) 0.154(2) Uani 1 1 d . . . N1 N 0.3133(4) -0.2521(4) -0.0461(4) 0.0214(10) Uani 1 1 d . . . N2 N 0.2446(4) -0.1255(3) -0.1562(4) 0.0201(10) Uani 1 1 d . . . N3 N 0.3824(4) -0.1212(4) -0.2947(4) 0.0280(12) Uani 1 1 d . . . H3B H 0.3540 -0.0788 -0.3306 0.034 Uiso 1 1 calc R . . H3C H 0.4418 -0.1433 -0.3188 0.034 Uiso 1 1 calc R . . N4 N -0.1083(4) -0.1392(3) 0.2435(3) 0.0194(10) Uani 1 1 d . . . N6 N 0.1289(4) -0.2233(4) 0.1028(3) 0.0208(10) Uani 1 1 d . . . H6A H 0.1542 -0.2667 0.1404 0.025 Uiso 1 1 calc R . . N5 N 0.0054(4) -0.1153(4) 0.0657(3) 0.0225(11) Uani 1 1 d . . . N7 N 0.3440(4) -0.0787(4) 0.0684(4) 0.0238(11) Uani 1 1 d . . . N8 N 0.2661(4) 0.0346(4) -0.0448(3) 0.0210(10) Uani 1 1 d . . . N9 N 0.4034(4) 0.0432(4) -0.1828(4) 0.0252(11) Uani 1 1 d . . . H9B H 0.3721 0.0825 -0.2184 0.030 Uiso 1 1 calc R . . H9C H 0.4643 0.0244 -0.2073 0.030 Uiso 1 1 calc R . . N10 N -0.0812(4) 0.0284(4) 0.3563(3) 0.0225(11) Uani 1 1 d . . . C21 C -0.0545(5) -0.1145(5) 0.5069(5) 0.0302(15) Uani 1 1 d . . . H21A H -0.0452 -0.1623 0.5580 0.036 Uiso 1 1 calc R . . N11 N 0.0250(4) 0.0396(3) 0.1767(3) 0.0197(10) Uani 1 1 d . . . N12 N 0.1566(4) -0.0535(4) 0.2170(4) 0.0223(11) Uani 1 1 d . . . H12A H 0.1852 -0.0911 0.2563 0.027 Uiso 1 1 calc R . . N13 N 0.2743(4) -0.4345(4) -0.1584(4) 0.0248(11) Uani 1 1 d . . . N14 N 0.2256(4) -0.2886(4) -0.2652(4) 0.0234(11) Uani 1 1 d . . . N15 N 0.3615(5) -0.2934(4) -0.4032(4) 0.0375(15) Uani 1 1 d . . . H15B H 0.3408 -0.2429 -0.4368 0.045 Uiso 1 1 calc R . . H15C H 0.4159 -0.3224 -0.4287 0.045 Uiso 1 1 calc R . . N16 N -0.1392(4) -0.3004(4) 0.1262(3) 0.0213(10) Uani 1 1 d . . . N17 N -0.0048(4) -0.2651(4) -0.0401(3) 0.0210(10) Uani 1 1 d . . . N18 N 0.0886(4) -0.4021(4) -0.0139(4) 0.0247(11) Uani 1 1 d . . . H18A H 0.1026 -0.4559 0.0197 0.030 Uiso 1 1 calc R . . C1 C 0.3394(5) -0.3246(5) 0.0179(5) 0.0276(14) Uani 1 1 d . . . H1A H 0.2957 -0.3411 0.0798 0.033 Uiso 1 1 calc R . . C2 C 0.4292(5) -0.3757(5) -0.0051(5) 0.0331(16) Uani 1 1 d . . . H2A H 0.4459 -0.4254 0.0406 0.040 Uiso 1 1 calc R . . C3 C 0.4945(5) -0.3513(5) -0.0984(5) 0.0326(15) Uani 1 1 d . . . H3A H 0.5556 -0.3843 -0.1154 0.039 Uiso 1 1 calc R . . C4 C 0.4675(5) -0.2774(5) -0.1654(5) 0.0288(14) Uani 1 1 d . . . H4A H 0.5098 -0.2603 -0.2278 0.035 Uiso 1 1 calc R . . C5 C 0.3761(5) -0.2295(4) -0.1375(4) 0.0214(12) Uani 1 1 d . . . C6 C 0.3343(4) -0.1525(4) -0.2020(4) 0.0210(12) Uani 1 1 d . . . C7 C -0.1808(5) -0.1534(5) 0.3277(4) 0.0238(13) Uani 1 1 d . . . H7A H -0.2337 -0.1093 0.3374 0.029 Uiso 1 1 calc R . . C8 C -0.1782(5) -0.2331(4) 0.4008(4) 0.0259(13) Uani 1 1 d . . . H8A H -0.2292 -0.2427 0.4588 0.031 Uiso 1 1 calc R . . C9 C -0.0988(5) -0.2977(5) 0.3862(5) 0.0313(15) Uani 1 1 d . . . H9A H -0.0947 -0.3506 0.4347 0.038 Uiso 1 1 calc R . . C10 C -0.0256(5) -0.2825(4) 0.2985(4) 0.0234(13) Uani 1 1 d . . . H10A H 0.0278 -0.3258 0.2872 0.028 Uiso 1 1 calc R . . C11 C -0.0318(4) -0.2032(4) 0.2280(4) 0.0194(12) Uani 1 1 d . . . C12 C 0.0401(4) -0.1816(4) 0.1296(4) 0.0192(12) Uani 1 1 d . . . C13 C 0.3777(5) -0.1422(5) 0.1342(5) 0.0273(14) Uani 1 1 d . . . H13A H 0.3360 -0.1577 0.1970 0.033 Uiso 1 1 calc R . . C14 C 0.4723(5) -0.1858(5) 0.1120(5) 0.0296(14) Uani 1 1 d . . . H14A H 0.4941 -0.2287 0.1597 0.036 Uiso 1 1 calc R . . C15 C 0.5339(5) -0.1653(5) 0.0193(5) 0.0313(15) Uani 1 1 d . . . H15A H 0.5972 -0.1951 0.0033 0.038 Uiso 1 1 calc R . . C16 C 0.5004(5) -0.0990(5) -0.0509(5) 0.0273(14) Uani 1 1 d . . . H16A H 0.5414 -0.0834 -0.1140 0.033 Uiso 1 1 calc R . . C17 C 0.4052(5) -0.0573(4) -0.0247(4) 0.0245(13) Uani 1 1 d . . . C18 C 0.3577(4) 0.0115(4) -0.0901(4) 0.0219(12) Uani 1 1 d . . . C19 C -0.1461(5) 0.0187(5) 0.4438(4) 0.0264(14) Uani 1 1 d . . . H19A H -0.2006 0.0611 0.4533 0.032 Uiso 1 1 calc R . . C20 C -0.1353(5) -0.0524(5) 0.5211(4) 0.0293(15) Uani 1 1 d . . . H20A H -0.1820 -0.0578 0.5814 0.035 Uiso 1 1 calc R . . C22 C 0.0131(5) -0.1057(5) 0.4167(4) 0.0285(14) Uani 1 1 d . . . H22A H 0.0678 -0.1478 0.4060 0.034 Uiso 1 1 calc R . . C23 C -0.0019(5) -0.0340(5) 0.3433(4) 0.0246(13) Uani 1 1 d . . . C24 C 0.0647(5) -0.0171(4) 0.2422(4) 0.0223(12) Uani 1 1 d . . . C25 C 0.2930(5) -0.5129(5) -0.0958(5) 0.0274(14) Uani 1 1 d . . . H25A H 0.2478 -0.5290 -0.0347 0.033 Uiso 1 1 calc R . . C26 C 0.3766(6) -0.5694(5) -0.1198(6) 0.0365(17) Uani 1 1 d . . . H26A H 0.3868 -0.6238 -0.0755 0.044 Uiso 1 1 calc R . . C27 C 0.4463(6) -0.5457(5) -0.2100(6) 0.0359(16) Uani 1 1 d . . . H27A H 0.5042 -0.5830 -0.2265 0.043 Uiso 1 1 calc R . . C28 C 0.4278(5) -0.4657(5) -0.2744(5) 0.0350(16) Uani 1 1 d . . . H28A H 0.4736 -0.4479 -0.3351 0.042 Uiso 1 1 calc R . . C29 C 0.3400(5) -0.4114(4) -0.2482(5) 0.0245(13) Uani 1 1 d . . . C30 C 0.3085(5) -0.3272(5) -0.3102(5) 0.0272(14) Uani 1 1 d . . . C31 C -0.2160(5) -0.3152(5) 0.2067(4) 0.0245(13) Uani 1 1 d . . . H31A H -0.2659 -0.2684 0.2160 0.029 Uiso 1 1 calc R . . C32 C -0.2234(5) -0.3997(5) 0.2776(4) 0.0293(14) Uani 1 1 d . . . H32A H -0.2770 -0.4090 0.3337 0.035 Uiso 1 1 calc R . . C33 C -0.1493(5) -0.4689(4) 0.2623(4) 0.0252(13) Uani 1 1 d . . . H33A H -0.1522 -0.5252 0.3087 0.030 Uiso 1 1 calc R . . C36 C 0.0095(4) -0.3465(4) 0.0157(4) 0.0206(12) Uani 1 1 d . . . C35 C -0.0679(5) -0.3694(4) 0.1108(4) 0.0234(13) Uani 1 1 d . . . C34 C -0.0708(5) -0.4547(5) 0.1778(4) 0.0246(13) Uani 1 1 d . . . H34A H -0.0211 -0.5013 0.1662 0.030 Uiso 1 1 calc R . . O1 O 0.1937(3) -0.0599(3) -0.2106(3) 0.0227(9) Uani 1 1 d . . . O2 O 0.0851(3) -0.0939(3) -0.0222(3) 0.0206(9) Uani 1 1 d . . . O3 O 0.2105(3) 0.0936(3) -0.0991(3) 0.0212(9) Uani 1 1 d . . . O4 O 0.1009(3) 0.0566(3) 0.0872(3) 0.0219(9) Uani 1 1 d . . . O5 O 0.1884(3) -0.2107(3) -0.3166(3) 0.0276(10) Uani 1 1 d . . . O6 O 0.0715(3) -0.2501(3) -0.1277(3) 0.0236(9) Uani 1 1 d . . . O1W O -0.0374(3) -0.2007(3) -0.2640(3) 0.0284(10) Uani 1 1 d . . . O2W O 0.2213(3) 0.2248(3) 0.0350(3) 0.0271(10) Uani 1 1 d . . . O3W O 0.1138(5) -0.2955(5) -0.4282(4) 0.0561(16) Uani 1 1 d . . . O4W O 0.5388(10) -0.2268(13) -0.6485(8) 0.225(9) Uani 1 1 d . . . O5W O 0.2281(6) -0.3508(5) 0.2605(5) 0.072(2) Uani 1 1 d . . . O6W O 0.3090(6) 0.4803(6) 0.2059(6) 0.081(2) Uani 1 1 d . . . O7W O 0.2456(4) 0.1505(4) 0.2169(4) 0.0399(12) Uani 1 1 d . . . O8W O -0.0761(7) -0.3662(6) -0.3632(6) 0.088(3) Uani 1 1 d . . . O9W O 0.5641(7) -0.4042(6) -0.5132(5) 0.109(3) Uani 1 1 d . . . O10W O 0.2852(9) 0.2754(11) 0.3245(7) 0.169(6) Uani 1 1 d . . . O11W O 0.0911(10) -0.4843(7) 0.4360(8) 0.135(4) Uani 1 1 d . . . O12W O 0.6294(4) 0.0059(5) -0.3001(4) 0.0497(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0143(4) 0.0226(4) 0.0155(4) -0.0037(3) -0.0003(3) 0.0040(3) Ni2 0.0159(4) 0.0223(4) 0.0130(4) -0.0019(3) 0.0014(3) 0.0040(3) Ni3 0.0168(4) 0.0248(4) 0.0157(4) -0.0027(3) -0.0007(3) 0.0041(3) Ni4 0.0200(4) 0.0250(4) 0.0141(4) -0.0031(3) 0.0007(3) 0.0032(3) Ni5 0.0164(4) 0.0248(4) 0.0148(4) -0.0028(3) 0.0006(3) 0.0029(3) Ni6 0.0183(4) 0.0228(4) 0.0172(4) -0.0051(3) 0.0004(3) 0.0031(3) Cl1 0.0580(12) 0.0316(9) 0.0351(10) -0.0030(7) -0.0007(9) 0.0037(9) Cl2A 0.039(6) 0.082(9) 0.047(6) 0.004(6) 0.005(5) 0.005(6) Cl2B 0.030(2) 0.178(7) 0.075(4) -0.072(4) 0.000(2) 0.004(3) Cl2C 0.087(8) 0.168(14) 0.083(8) 0.045(9) 0.005(6) 0.031(9) Cl3 0.099(3) 0.256(6) 0.0477(18) 0.033(3) 0.0044(18) 0.022(3) N1 0.018(2) 0.023(3) 0.023(3) -0.008(2) -0.005(2) 0.002(2) N2 0.015(2) 0.021(2) 0.020(2) -0.0025(19) -0.003(2) 0.0049(19) N3 0.020(3) 0.037(3) 0.019(3) -0.004(2) 0.005(2) 0.002(2) N4 0.020(2) 0.020(2) 0.015(2) -0.0027(19) -0.0012(19) 0.004(2) N6 0.018(2) 0.025(3) 0.017(2) -0.003(2) -0.005(2) 0.006(2) N5 0.022(3) 0.027(3) 0.012(2) -0.0023(19) 0.0028(19) 0.003(2) N7 0.021(3) 0.028(3) 0.021(3) -0.005(2) -0.006(2) 0.002(2) N8 0.015(2) 0.028(3) 0.017(2) -0.006(2) -0.0022(19) 0.004(2) N9 0.016(2) 0.036(3) 0.019(2) -0.004(2) 0.000(2) 0.001(2) N10 0.019(2) 0.028(3) 0.015(2) -0.002(2) -0.001(2) -0.001(2) C21 0.032(4) 0.036(4) 0.018(3) 0.002(3) -0.004(3) -0.004(3) N11 0.017(2) 0.023(2) 0.011(2) -0.0009(18) 0.0052(18) 0.000(2) N12 0.019(2) 0.025(3) 0.019(2) -0.001(2) -0.005(2) 0.004(2) N13 0.022(3) 0.024(3) 0.026(3) -0.010(2) 0.000(2) 0.000(2) N14 0.021(3) 0.023(3) 0.023(3) -0.007(2) -0.002(2) 0.005(2) N15 0.034(3) 0.038(3) 0.027(3) -0.010(3) 0.009(3) 0.010(3) N16 0.021(2) 0.024(3) 0.014(2) -0.0006(19) 0.0005(19) -0.004(2) N17 0.018(2) 0.027(3) 0.013(2) -0.0031(19) 0.0028(19) -0.001(2) N18 0.024(3) 0.024(3) 0.023(3) -0.004(2) -0.004(2) 0.006(2) C1 0.024(3) 0.030(3) 0.028(3) -0.006(3) -0.008(3) 0.004(3) C2 0.031(4) 0.038(4) 0.034(4) -0.014(3) -0.012(3) 0.011(3) C3 0.022(3) 0.034(4) 0.042(4) -0.019(3) -0.005(3) 0.010(3) C4 0.023(3) 0.035(4) 0.028(3) -0.012(3) -0.003(3) 0.005(3) C5 0.020(3) 0.020(3) 0.022(3) -0.004(2) -0.004(2) 0.002(2) C6 0.019(3) 0.024(3) 0.019(3) -0.008(2) -0.002(2) 0.001(2) C7 0.021(3) 0.029(3) 0.019(3) -0.009(2) 0.001(2) 0.000(2) C8 0.030(3) 0.027(3) 0.013(3) 0.002(2) 0.001(2) -0.004(3) C9 0.034(4) 0.033(4) 0.021(3) 0.000(3) -0.004(3) -0.003(3) C10 0.026(3) 0.019(3) 0.020(3) 0.000(2) -0.004(2) 0.002(2) C11 0.022(3) 0.024(3) 0.009(2) -0.003(2) -0.001(2) -0.003(2) C12 0.020(3) 0.018(3) 0.018(3) -0.005(2) -0.003(2) 0.004(2) C13 0.031(3) 0.028(3) 0.022(3) -0.007(3) -0.008(3) 0.004(3) C14 0.025(3) 0.028(3) 0.037(4) -0.007(3) -0.013(3) 0.005(3) C15 0.018(3) 0.031(4) 0.049(4) -0.017(3) -0.010(3) 0.004(3) C16 0.021(3) 0.035(4) 0.026(3) -0.010(3) -0.006(3) 0.003(3) C17 0.022(3) 0.029(3) 0.020(3) -0.008(2) 0.000(2) 0.000(3) C18 0.017(3) 0.023(3) 0.022(3) -0.007(2) 0.001(2) -0.001(2) C19 0.026(3) 0.034(3) 0.016(3) -0.009(2) 0.002(2) -0.001(3) C20 0.027(3) 0.042(4) 0.014(3) -0.007(3) 0.003(2) -0.001(3) C22 0.032(3) 0.028(3) 0.020(3) 0.000(3) -0.002(3) -0.004(3) C23 0.029(3) 0.028(3) 0.015(3) -0.003(2) -0.003(2) -0.005(3) C24 0.023(3) 0.023(3) 0.021(3) -0.007(2) -0.005(2) 0.000(2) C25 0.024(3) 0.028(3) 0.027(3) -0.005(3) -0.006(3) 0.003(3) C26 0.033(4) 0.028(4) 0.045(4) -0.005(3) -0.012(3) 0.010(3) C27 0.032(4) 0.026(3) 0.048(4) -0.013(3) -0.008(3) 0.009(3) C28 0.029(4) 0.036(4) 0.037(4) -0.014(3) 0.000(3) -0.001(3) C29 0.020(3) 0.025(3) 0.028(3) -0.014(3) 0.001(2) 0.001(2) C30 0.025(3) 0.033(3) 0.024(3) -0.011(3) -0.003(3) -0.002(3) C31 0.024(3) 0.028(3) 0.017(3) -0.005(2) 0.001(2) -0.004(3) C32 0.031(3) 0.034(4) 0.016(3) 0.000(3) 0.001(3) -0.008(3) C33 0.030(3) 0.025(3) 0.019(3) 0.000(2) -0.008(3) -0.005(3) C36 0.019(3) 0.022(3) 0.020(3) -0.003(2) -0.006(2) 0.000(2) C35 0.024(3) 0.020(3) 0.020(3) -0.004(2) 0.001(2) 0.000(2) C34 0.028(3) 0.027(3) 0.018(3) -0.003(2) -0.007(2) -0.001(3) O1 0.020(2) 0.025(2) 0.018(2) -0.0035(17) -0.0011(17) 0.0061(17) O2 0.0166(19) 0.023(2) 0.0142(19) -0.0002(16) 0.0037(16) 0.0025(16) O3 0.020(2) 0.024(2) 0.0132(19) -0.0006(16) 0.0002(16) 0.0055(17) O4 0.0159(19) 0.031(2) 0.0123(19) -0.0013(16) 0.0027(16) 0.0031(17) O5 0.027(2) 0.030(2) 0.018(2) -0.0016(18) 0.0006(18) 0.0073(19) O6 0.025(2) 0.026(2) 0.0112(19) -0.0018(16) 0.0040(16) 0.0037(18) O1W 0.029(2) 0.030(2) 0.024(2) -0.0030(18) -0.0055(19) -0.0033(19) O2W 0.021(2) 0.032(2) 0.023(2) -0.0035(18) -0.0018(18) 0.0025(19) O3W 0.063(4) 0.064(4) 0.052(4) -0.025(3) -0.026(3) 0.013(3) O4W 0.146(11) 0.31(2) 0.085(8) 0.085(10) 0.028(7) 0.088(12) O5W 0.070(5) 0.075(5) 0.060(4) -0.014(4) -0.005(4) 0.011(4) O6W 0.059(4) 0.090(6) 0.079(5) -0.007(4) -0.006(4) 0.002(4) O7W 0.032(3) 0.055(3) 0.028(3) -0.009(2) -0.002(2) 0.000(2) O8W 0.097(6) 0.099(6) 0.066(5) -0.002(4) -0.023(5) -0.032(5) O9W 0.122(7) 0.101(6) 0.044(4) -0.018(4) 0.062(4) 0.014(5) O10W 0.138(9) 0.294(16) 0.069(6) -0.048(8) 0.026(6) -0.151(10) O11W 0.195(12) 0.085(7) 0.128(9) 0.001(6) -0.073(9) 0.004(7) O12W 0.021(2) 0.108(5) 0.037(3) -0.048(3) -0.019(2) 0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.824(4) . ? Ni1 N2 1.845(5) . ? Ni1 N6 1.855(5) . ? Ni1 N1 1.895(5) . ? Ni2 O2 2.024(4) . ? Ni2 O1 2.038(4) . ? Ni2 N4 2.056(5) 2 ? Ni2 N5 2.063(5) 2 ? Ni2 O3 2.154(4) . ? Ni2 N11 2.324(5) 2 ? Ni3 O4 1.818(4) . ? Ni3 N8 1.843(5) . ? Ni3 N12 1.861(5) . ? Ni3 N7 1.890(5) . ? Ni4 O6 2.024(4) . ? Ni4 O5 2.030(4) . ? Ni4 N10 2.049(5) 2 ? Ni4 N11 2.095(5) 2 ? Ni4 O1W 2.136(5) . ? Ni4 O1 2.151(5) . ? Ni5 N17 2.020(5) 2 ? Ni5 O4 2.034(4) . ? Ni5 O3 2.054(4) . ? Ni5 N16 2.075(5) 2 ? Ni5 O2W 2.136(5) . ? Ni5 N5 2.267(6) 2 ? Ni6 O6 1.825(4) . ? Ni6 N18 1.857(5) . ? Ni6 N14 1.857(5) . ? Ni6 N13 1.893(5) . ? N1 C1 1.343(8) . ? N1 C5 1.363(8) . ? N2 C6 1.303(7) . ? N2 O1 1.380(6) . ? N3 C6 1.332(8) . ? N3 H3B 0.8600 . ? N3 H3C 0.8600 . ? N4 C7 1.339(7) . ? N4 C11 1.349(8) . ? N4 Ni2 2.056(5) 2 ? N6 C12 1.313(7) . ? N6 H6A 0.8600 . ? N5 C12 1.345(8) . ? N5 O2 1.427(6) . ? N5 Ni2 2.063(5) 2 ? N5 Ni5 2.267(6) 2 ? N7 C13 1.337(8) . ? N7 C17 1.375(7) . ? N8 C18 1.302(7) . ? N8 O3 1.377(6) . ? N9 C18 1.325(7) . ? N9 H9B 0.8600 . ? N9 H9C 0.8600 . ? N10 C19 1.333(7) . ? N10 C23 1.357(8) . ? N10 Ni4 2.049(5) 2 ? C21 C20 1.372(10) . ? C21 C22 1.379(9) . ? C21 H21A 0.9300 . ? N11 C24 1.335(8) . ? N11 O4 1.417(6) . ? N11 Ni4 2.095(5) 2 ? N11 Ni2 2.324(5) 2 ? N12 C24 1.311(8) . ? N12 H12A 0.8600 . ? N13 C25 1.346(8) . ? N13 C29 1.361(8) . ? N14 C30 1.302(8) . ? N14 O5 1.357(6) . ? N15 C30 1.357(8) . ? N15 H15B 0.8600 . ? N15 H15C 0.8600 . ? N16 C31 1.333(7) . ? N16 C35 1.355(8) . ? N16 Ni5 2.075(5) 2 ? N17 C36 1.308(8) . ? N17 O6 1.400(6) . ? N17 Ni5 2.020(5) 2 ? N18 C36 1.333(8) . ? N18 H18A 0.8600 . ? C1 C2 1.383(9) . ? C1 H1A 0.9300 . ? C2 C3 1.400(10) . ? C2 H2A 0.9300 . ? C3 C4 1.386(10) . ? C3 H3A 0.9300 . ? C4 C5 1.387(8) . ? C4 H4A 0.9300 . ? C5 C6 1.484(8) . ? C7 C8 1.391(8) . ? C7 H7A 0.9300 . ? C8 C9 1.382(10) . ? C8 H8A 0.9300 . ? C9 C10 1.379(8) . ? C9 H9A 0.9300 . ? C10 C11 1.376(8) . ? C10 H10A 0.9300 . ? C11 C12 1.489(7) . ? C13 C14 1.383(9) . ? C13 H13A 0.9300 . ? C14 C15 1.372(10) . ? C14 H14A 0.9300 . ? C15 C16 1.399(10) . ? C15 H15A 0.9300 . ? C16 C17 1.384(8) . ? C16 H16A 0.9300 . ? C17 C18 1.473(9) . ? C19 C20 1.384(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C22 C23 1.370(9) . ? C22 H22A 0.9300 . ? C23 C24 1.493(8) . ? C25 C26 1.366(9) . ? C25 H25A 0.9300 . ? C26 C27 1.390(10) . ? C26 H26A 0.9300 . ? C27 C28 1.375(10) . ? C27 H27A 0.9300 . ? C28 C29 1.395(9) . ? C28 H28A 0.9300 . ? C29 C30 1.462(9) . ? C31 C32 1.403(9) . ? C31 H31A 0.9300 . ? C32 C33 1.380(9) . ? C32 H32A 0.9300 . ? C33 C34 1.384(8) . ? C33 H33A 0.9300 . ? C36 C35 1.485(8) . ? C35 C34 1.386(8) . ? C34 H34A 0.9300 . ? Cl2A Cl2B 1.730(14) . ? Cl2B Cl2C 1.87(2) . ? 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 O2 Ni1 N2 90.11(19) . . ? O2 Ni1 N6 84.7(2) . . ? N2 Ni1 N6 174.5(2) . . ? O2 Ni1 N1 172.7(2) . . ? N2 Ni1 N1 82.9(2) . . ? N6 Ni1 N1 102.3(2) . . ? O2 Ni2 O1 84.12(16) . . ? O2 Ni2 N4 178.02(19) . 2 ? O1 Ni2 N4 94.79(18) . 2 ? O2 Ni2 N5 102.07(17) . 2 ? O1 Ni2 N5 172.55(18) . 2 ? N4 Ni2 N5 78.90(19) 2 2 ? O2 Ni2 O3 97.27(17) . . ? O1 Ni2 O3 97.96(17) . . ? N4 Ni2 O3 84.50(18) 2 . ? N5 Ni2 O3 85.47(19) 2 . ? O2 Ni2 N11 88.42(17) . 2 ? O1 Ni2 N11 82.97(17) . 2 ? N4 Ni2 N11 89.81(19) 2 2 ? N5 Ni2 N11 92.97(19) 2 2 ? O3 Ni2 N11 174.29(16) . 2 ? O4 Ni3 N8 90.1(2) . . ? O4 Ni3 N12 84.1(2) . . ? N8 Ni3 N12 174.1(2) . . ? O4 Ni3 N7 173.1(2) . . ? N8 Ni3 N7 83.1(2) . . ? N12 Ni3 N7 102.8(2) . . ? O6 Ni4 O5 85.70(17) . . ? O6 Ni4 N10 172.5(2) . 2 ? O5 Ni4 N10 92.17(19) . 2 ? O6 Ni4 N11 103.45(17) . 2 ? O5 Ni4 N11 170.85(18) . 2 ? N10 Ni4 N11 78.75(19) 2 2 ? O6 Ni4 O1W 84.44(18) . . ? O5 Ni4 O1W 90.85(19) . . ? N10 Ni4 O1W 88.43(19) 2 . ? N11 Ni4 O1W 90.08(19) 2 . ? O6 Ni4 O1 97.77(17) . . ? O5 Ni4 O1 92.76(18) . . ? N10 Ni4 O1 89.48(19) 2 . ? N11 Ni4 O1 86.05(18) 2 . ? O1W Ni4 O1 175.90(17) . . ? N17 Ni5 O4 104.42(18) 2 . ? N17 Ni5 O3 169.67(19) 2 . ? O4 Ni5 O3 82.59(16) . . ? N17 Ni5 N16 78.4(2) 2 2 ? O4 Ni5 N16 173.94(19) . 2 ? O3 Ni5 N16 95.32(18) . 2 ? N17 Ni5 O2W 90.98(19) 2 . ? O4 Ni5 O2W 87.61(17) . . ? O3 Ni5 O2W 96.95(17) . . ? N16 Ni5 O2W 87.00(19) 2 . ? N17 Ni5 N5 89.8(2) 2 2 ? O4 Ni5 N5 87.77(18) . 2 ? O3 Ni5 N5 82.81(18) . 2 ? N16 Ni5 N5 97.63(19) 2 2 ? O2W Ni5 N5 175.37(18) . 2 ? O6 Ni6 N18 84.6(2) . . ? O6 Ni6 N14 90.5(2) . . ? N18 Ni6 N14 173.3(2) . . ? O6 Ni6 N13 171.9(2) . . ? N18 Ni6 N13 101.8(2) . . ? N14 Ni6 N13 83.5(2) . . ? C1 N1 C5 119.0(5) . . ? C1 N1 Ni1 127.2(4) . . ? C5 N1 Ni1 113.7(4) . . ? C6 N2 O1 116.1(5) . . ? C6 N2 Ni1 119.5(4) . . ? O1 N2 Ni1 124.3(3) . . ? C6 N3 H3B 120.0 . . ? C6 N3 H3C 120.0 . . ? H3B N3 H3C 120.0 . . ? C7 N4 C11 120.1(5) . . ? C7 N4 Ni2 125.9(4) . 2 ? C11 N4 Ni2 113.9(4) . 2 ? C12 N6 Ni1 111.4(4) . . ? C12 N6 H6A 124.3 . . ? Ni1 N6 H6A 124.3 . . ? C12 N5 O2 108.4(4) . . ? C12 N5 Ni2 112.0(4) . 2 ? O2 N5 Ni2 128.3(4) . 2 ? C12 N5 Ni5 110.8(4) . 2 ? O2 N5 Ni5 100.9(3) . 2 ? Ni2 N5 Ni5 93.7(2) 2 2 ? C13 N7 C17 118.6(5) . . ? C13 N7 Ni3 127.9(4) . . ? C17 N7 Ni3 113.5(4) . . ? C18 N8 O3 116.8(5) . . ? C18 N8 Ni3 119.5(4) . . ? O3 N8 Ni3 123.7(3) . . ? C18 N9 H9B 120.0 . . ? C18 N9 H9C 120.0 . . ? H9B N9 H9C 120.0 . . ? C19 N10 C23 118.3(5) . . ? C19 N10 Ni4 126.8(4) . 2 ? C23 N10 Ni4 114.7(4) . 2 ? C20 C21 C22 119.7(6) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C24 N11 O4 108.3(4) . . ? C24 N11 Ni4 110.9(4) . 2 ? O4 N11 Ni4 128.9(3) . 2 ? C24 N11 Ni2 117.8(4) . 2 ? O4 N11 Ni2 98.0(3) . 2 ? Ni4 N11 Ni2 91.55(19) 2 2 ? C24 N12 Ni3 111.4(4) . . ? C24 N12 H12A 124.3 . . ? Ni3 N12 H12A 124.3 . . ? C25 N13 C29 119.1(5) . . ? C25 N13 Ni6 127.8(4) . . ? C29 N13 Ni6 113.1(4) . . ? C30 N14 O5 117.1(5) . . ? C30 N14 Ni6 117.7(4) . . ? O5 N14 Ni6 125.2(4) . . ? C30 N15 H15B 120.0 . . ? C30 N15 H15C 120.0 . . ? H15B N15 H15C 120.0 . . ? C31 N16 C35 119.5(5) . . ? C31 N16 Ni5 126.3(4) . 2 ? C35 N16 Ni5 114.1(4) . 2 ? C36 N17 O6 110.5(5) . . ? C36 N17 Ni5 117.3(4) . 2 ? O6 N17 Ni5 131.3(4) . 2 ? C36 N18 Ni6 110.5(4) . . ? C36 N18 H18A 124.8 . . ? Ni6 N18 H18A 124.8 . . ? N1 C1 C2 122.1(6) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 118.8(7) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C5 C4 C3 118.7(6) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 121.9(6) . . ? N1 C5 C6 113.1(5) . . ? C4 C5 C6 125.0(6) . . ? N2 C6 N3 126.6(6) . . ? N2 C6 C5 110.5(5) . . ? N3 C6 C5 122.8(5) . . ? N4 C7 C8 121.0(6) . . ? N4 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C9 C8 C7 119.2(6) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C10 C9 C8 118.9(6) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C11 C10 C9 119.9(6) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? N4 C11 C10 120.9(5) . . ? N4 C11 C12 114.6(5) . . ? C10 C11 C12 124.5(5) . . ? N6 C12 N5 120.5(5) . . ? N6 C12 C11 125.4(5) . . ? N5 C12 C11 114.0(5) . . ? N7 C13 C14 122.3(6) . . ? N7 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C15 C14 C13 119.7(6) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 119.2(6) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 118.8(6) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? N7 C17 C16 121.5(6) . . ? N7 C17 C18 113.0(5) . . ? C16 C17 C18 125.5(6) . . ? N8 C18 N9 125.7(6) . . ? N8 C18 C17 110.9(5) . . ? N9 C18 C17 123.4(5) . . ? N10 C19 C20 122.4(6) . . ? N10 C19 H19A 118.8 . . ? C20 C19 H19A 118.8 . . ? C21 C20 C19 118.6(6) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C23 C22 C21 118.8(6) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? N10 C23 C22 122.1(6) . . ? N10 C23 C24 113.6(5) . . ? C22 C23 C24 124.2(6) . . ? N12 C24 N11 120.7(5) . . ? N12 C24 C23 123.9(6) . . ? N11 C24 C23 115.3(5) . . ? N13 C25 C26 121.7(6) . . ? N13 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C25 C26 C27 120.2(7) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 118.4(6) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.8 . . ? C27 C28 C29 119.7(7) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? N13 C29 C28 120.8(6) . . ? N13 C29 C30 113.6(5) . . ? C28 C29 C30 125.6(6) . . ? N14 C30 N15 124.7(6) . . ? N14 C30 C29 112.1(6) . . ? N15 C30 C29 123.2(6) . . ? N16 C31 C32 121.6(6) . . ? N16 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C33 C32 C31 118.5(6) . . ? C33 C32 H32A 120.7 . . ? C31 C32 H32A 120.7 . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? N17 C36 N18 120.4(5) . . ? N17 C36 C35 114.8(5) . . ? N18 C36 C35 124.8(5) . . ? N16 C35 C34 121.8(5) . . ? N16 C35 C36 114.1(5) . . ? C34 C35 C36 124.0(6) . . ? C33 C34 C35 118.4(6) . . ? C33 C34 H34A 120.8 . . ? C35 C34 H34A 120.8 . . ? N2 O1 Ni2 111.5(3) . . ? N2 O1 Ni4 107.5(3) . . ? Ni2 O1 Ni4 98.33(17) . . ? N5 O2 Ni1 113.8(3) . . ? N5 O2 Ni2 127.4(3) . . ? Ni1 O2 Ni2 118.4(2) . . ? N8 O3 Ni5 110.2(3) . . ? N8 O3 Ni2 114.5(3) . . ? Ni5 O3 Ni2 97.37(17) . . ? N11 O4 Ni3 115.0(3) . . ? N11 O4 Ni5 125.2(3) . . ? Ni3 O4 Ni5 116.2(2) . . ? N14 O5 Ni4 115.4(3) . . ? N17 O6 Ni6 114.0(3) . . ? N17 O6 Ni4 125.2(3) . . ? Ni6 O6 Ni4 120.8(2) . . ? Cl2A Cl2B Cl2C 99.6(8) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.460 _refine_diff_density_min -1.917 _refine_diff_density_rms 0.164 #===End