# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; An One-Dimensional Metal-azido Complex Constructed by Double EO Azido Bridged Trinuclear Nickel(?) Unit: Design, Structure and Magnetic Properties ; loop_ _publ_author_name 'Xian-He Bu.' 'Bo-Wen Hu.' 'Fu-Chen Liu.' 'J. Ribas' 'Yong-Fei Zeng.' ; Jiong-Peng Zhao ; # Attachment '1.cif.cif' data_060117c _database_code_depnum_ccdc_archive 'CCDC 730934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 N18 Ni3 O4' _chemical_formula_weight 948.86 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8807(17) _cell_length_b 9.9140(14) _cell_length_c 17.161(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.588(2) _cell_angle_gamma 90.00 _cell_volume 1915.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3975 _cell_measurement_theta_min 2.5043 _cell_measurement_theta_max 26.2228 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.351 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.201 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10943 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.48 _reflns_number_total 3960 _reflns_number_gt 3182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.5442P] 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 3960 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.68532(3) 0.27652(3) 1.02370(2) 0.02272(10) Uani 1 1 d . . . Ni2 Ni 0.5000 0.5000 1.0000 0.02164(12) Uani 1 2 d S . . N1 N 0.7865(2) 0.1945(3) 0.95725(16) 0.0346(6) Uani 1 1 d . . . N2 N 0.8470(2) 0.3659(2) 1.08396(16) 0.0308(6) Uani 1 1 d . . . N3 N 0.27566(19) -0.1017(2) 0.90007(15) 0.0262(5) Uani 1 1 d . . . N4 N 0.5844(2) 0.3593(2) 1.09162(14) 0.0247(5) Uani 1 1 d . . . N5 N 0.5242(2) 0.2829(3) 1.11643(16) 0.0339(6) Uani 1 1 d . . . N6 N 0.4675(3) 0.2123(3) 1.1411(2) 0.0704(11) Uani 1 1 d . . . N7 N 0.3641(2) 0.5473(2) 1.04962(16) 0.0271(5) Uani 1 1 d . . . N8 N 0.3803(2) 0.5629(3) 1.12146(18) 0.0318(6) Uani 1 1 d . . . N9 N 0.3925(3) 0.5774(4) 1.1902(2) 0.0618(9) Uani 1 1 d . . . O1 O 0.53302(16) 0.18836(19) 0.94838(12) 0.0274(5) Uani 1 1 d . . . O2 O 0.39285(16) 0.35079(18) 0.92642(12) 0.0288(5) Uani 1 1 d . . . C1 C 0.7539(4) 0.1078(4) 0.8957(2) 0.0545(10) Uani 1 1 d . . . H1 H 0.6747 0.0815 0.8758 0.065 Uiso 1 1 calc R . . C2 C 0.8332(5) 0.0544(5) 0.8595(3) 0.0798(15) Uani 1 1 d . . . H2 H 0.8078 -0.0080 0.8170 0.096 Uiso 1 1 calc R . . C3 C 0.9482(4) 0.0945(5) 0.8869(3) 0.0797(15) Uani 1 1 d . . . H3 H 1.0015 0.0611 0.8621 0.096 Uiso 1 1 calc R . . C11 C 0.9880(3) 0.1861(4) 0.9525(3) 0.0581(11) Uani 1 1 d . . . C4 C 1.1066(4) 0.2350(5) 0.9862(4) 0.0843(16) Uani 1 1 d . . . H5 H 1.1648 0.2035 0.9652 0.101 Uiso 1 1 calc R . . C5 C 1.1357(3) 0.3239(5) 1.0467(4) 0.0771(15) Uani 1 1 d . . . H6 H 1.2135 0.3553 1.0660 0.093 Uiso 1 1 calc R . . C12 C 1.0513(3) 0.3734(4) 1.0836(3) 0.0551(11) Uani 1 1 d . . . C6 C 1.0757(4) 0.4682(5) 1.1470(3) 0.0711(13) Uani 1 1 d . . . H8 H 1.1521 0.5029 1.1688 0.085 Uiso 1 1 calc R . . C7 C 0.9887(4) 0.5103(4) 1.1771(3) 0.0630(11) Uani 1 1 d . . . H9 H 1.0053 0.5736 1.2193 0.076 Uiso 1 1 calc R . . C8 C 0.8729(3) 0.4572(3) 1.1439(2) 0.0433(9) Uani 1 1 d . . . H10 H 0.8134 0.4867 1.1644 0.052 Uiso 1 1 calc R . . C10 C 0.9343(3) 0.3262(3) 1.0531(2) 0.0366(8) Uani 1 1 d . . . C9 C 0.9017(3) 0.2326(3) 0.9861(2) 0.0376(8) Uani 1 1 d . . . C13 C 0.4285(2) 0.2324(3) 0.92224(16) 0.0241(6) Uani 1 1 d . . . C14 C 0.3464(2) 0.0049(3) 0.92633(18) 0.0294(7) Uani 1 1 d . . . H14 H 0.4063 -0.0023 0.9767 0.035 Uiso 1 1 calc R . . C15 C 0.3368(2) 0.1254(3) 0.88365(17) 0.0225(6) Uani 1 1 d . . . C16 C 0.2468(3) 0.1371(3) 0.81060(18) 0.0333(7) Uani 1 1 d . . . H16 H 0.2352 0.2172 0.7809 0.040 Uiso 1 1 calc R . . C17 C 0.1733(3) 0.0270(3) 0.78167(19) 0.0403(8) Uani 1 1 d . . . H17 H 0.1127 0.0317 0.7316 0.048 Uiso 1 1 calc R . . C18 C 0.1908(2) -0.0890(3) 0.82769(17) 0.0293(7) Uani 1 1 d . . . H18 H 0.1411 -0.1621 0.8074 0.035 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 0.01825(18) 0.01814(18) 0.0291(2) -0.00072(15) 0.00378(13) -0.00114(15) Ni2 0.0222(3) 0.0149(2) 0.0265(3) 0.0006(2) 0.0058(2) -0.0003(2) N1 0.0328(14) 0.0369(15) 0.0341(16) 0.0002(12) 0.0110(12) 0.0060(11) N2 0.0261(13) 0.0285(14) 0.0337(15) 0.0018(11) 0.0038(11) -0.0066(11) N3 0.0215(12) 0.0215(12) 0.0321(14) -0.0008(10) 0.0037(10) -0.0012(10) N4 0.0298(13) 0.0177(11) 0.0269(13) 0.0008(10) 0.0094(10) -0.0004(10) N5 0.0390(15) 0.0299(14) 0.0355(16) 0.0061(12) 0.0157(13) 0.0041(12) N6 0.077(2) 0.060(2) 0.091(3) 0.022(2) 0.052(2) -0.0064(18) N7 0.0260(13) 0.0227(11) 0.0326(14) 0.0024(12) 0.0091(11) -0.0011(10) N8 0.0258(14) 0.0354(15) 0.0350(16) 0.0058(13) 0.0108(12) 0.0034(11) N9 0.060(2) 0.091(3) 0.0344(18) 0.0097(18) 0.0151(16) 0.0160(19) O1 0.0223(10) 0.0207(10) 0.0336(12) -0.0004(8) 0.0012(9) -0.0014(8) O2 0.0258(10) 0.0159(10) 0.0390(12) -0.0013(8) 0.0022(9) -0.0010(8) C1 0.055(2) 0.062(3) 0.045(2) -0.0171(19) 0.0129(19) 0.0109(19) C2 0.085(4) 0.099(4) 0.059(3) -0.030(3) 0.028(3) 0.019(3) C3 0.081(3) 0.098(4) 0.077(3) -0.013(3) 0.050(3) 0.023(3) C11 0.044(2) 0.073(3) 0.069(3) 0.011(2) 0.034(2) 0.013(2) C4 0.049(3) 0.104(4) 0.119(5) 0.013(4) 0.053(3) 0.013(3) C5 0.025(2) 0.093(4) 0.116(5) 0.009(3) 0.026(2) -0.006(2) C12 0.0302(19) 0.058(3) 0.072(3) 0.012(2) 0.0098(19) -0.0085(17) C6 0.036(2) 0.078(3) 0.083(3) 0.003(3) -0.004(2) -0.026(2) C7 0.056(3) 0.056(2) 0.061(3) -0.014(2) -0.003(2) -0.023(2) C8 0.0417(19) 0.039(2) 0.043(2) -0.0030(16) 0.0048(17) -0.0080(16) C10 0.0245(16) 0.0370(18) 0.049(2) 0.0130(16) 0.0121(15) 0.0002(14) C9 0.0316(16) 0.0413(19) 0.043(2) 0.0114(16) 0.0161(15) 0.0072(15) C13 0.0249(14) 0.0230(14) 0.0215(15) 0.0037(11) 0.0034(11) -0.0018(12) C14 0.0236(14) 0.0208(15) 0.0337(17) 0.0018(13) -0.0050(12) -0.0020(12) C15 0.0219(14) 0.0179(14) 0.0271(15) -0.0015(12) 0.0071(12) 0.0010(11) C16 0.0339(16) 0.0279(17) 0.0324(18) 0.0075(13) 0.0025(14) -0.0099(13) C17 0.0376(18) 0.046(2) 0.0252(16) 0.0078(15) -0.0069(14) -0.0129(15) C18 0.0283(15) 0.0276(16) 0.0294(16) -0.0043(13) 0.0059(13) -0.0106(12) _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 2.0536(19) . ? Ni1 N2 2.069(2) . ? Ni1 N1 2.069(3) . ? Ni1 N4 2.088(2) . ? Ni1 N7 2.123(2) 3_667 ? Ni1 N3 2.132(2) 3_657 ? Ni2 O2 2.0925(18) . ? Ni2 O2 2.0925(18) 3_667 ? Ni2 N4 2.102(2) 3_667 ? Ni2 N4 2.102(2) . ? Ni2 N7 2.104(2) 3_667 ? Ni2 N7 2.104(2) . ? N1 C1 1.321(4) . ? N1 C9 1.352(4) . ? N2 C8 1.331(4) . ? N2 C10 1.364(4) . ? N3 C18 1.333(3) . ? N3 C14 1.336(3) . ? N3 Ni1 2.132(2) 3_657 ? N4 N5 1.209(3) . ? N5 N6 1.143(4) . ? N7 N8 1.196(3) . ? N7 Ni1 2.123(2) 3_667 ? N8 N9 1.151(4) . ? O1 C13 1.256(3) . ? O2 C13 1.257(3) . ? C1 C2 1.388(5) . ? C1 H1 0.9300 . ? C2 C3 1.356(6) . ? C2 H2 0.9300 . ? C3 C11 1.405(6) . ? C3 H3 0.9300 . ? C11 C9 1.405(5) . ? C11 C4 1.427(6) . ? C4 C5 1.321(7) . ? C4 H5 0.9300 . ? C5 C12 1.432(6) . ? C5 H6 0.9300 . ? C12 C6 1.396(6) . ? C12 C10 1.401(4) . ? C6 C7 1.361(6) . ? C6 H8 0.9300 . ? C7 C8 1.412(5) . ? C7 H9 0.9300 . ? C8 H10 0.9300 . ? C10 C9 1.431(5) . ? C13 C15 1.514(4) . ? C14 C15 1.387(4) . ? C14 H14 0.9300 . ? C15 C16 1.369(4) . ? C16 C17 1.387(4) . ? C16 H16 0.9300 . ? C17 C18 1.372(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 N2 171.31(10) . . ? O1 Ni1 N1 92.07(9) . . ? N2 Ni1 N1 80.43(10) . . ? O1 Ni1 N4 88.35(8) . . ? N2 Ni1 N4 99.18(10) . . ? N1 Ni1 N4 179.53(10) . . ? O1 Ni1 N7 87.43(8) . 3_667 ? N2 Ni1 N7 88.92(9) . 3_667 ? N1 Ni1 N7 95.53(10) . 3_667 ? N4 Ni1 N7 84.72(9) . 3_667 ? O1 Ni1 N3 90.90(8) . 3_657 ? N2 Ni1 N3 93.22(9) . 3_657 ? N1 Ni1 N3 88.14(10) . 3_657 ? N4 Ni1 N3 91.61(9) . 3_657 ? N7 Ni1 N3 176.02(9) 3_667 3_657 ? O2 Ni2 O2 180.0 . 3_667 ? O2 Ni2 N4 87.96(8) . 3_667 ? O2 Ni2 N4 92.04(8) 3_667 3_667 ? O2 Ni2 N4 92.04(8) . . ? O2 Ni2 N4 87.96(8) 3_667 . ? N4 Ni2 N4 180.00(10) 3_667 . ? O2 Ni2 N7 89.76(8) . 3_667 ? O2 Ni2 N7 90.24(8) 3_667 3_667 ? N4 Ni2 N7 95.16(9) 3_667 3_667 ? N4 Ni2 N7 84.84(9) . 3_667 ? O2 Ni2 N7 90.24(8) . . ? O2 Ni2 N7 89.76(8) 3_667 . ? N4 Ni2 N7 84.84(9) 3_667 . ? N4 Ni2 N7 95.16(9) . . ? N7 Ni2 N7 180.000(1) 3_667 . ? C1 N1 C9 118.7(3) . . ? C1 N1 Ni1 128.5(2) . . ? C9 N1 Ni1 112.7(2) . . ? C8 N2 C10 118.7(3) . . ? C8 N2 Ni1 128.8(2) . . ? C10 N2 Ni1 112.4(2) . . ? C18 N3 C14 116.6(2) . . ? C18 N3 Ni1 126.90(19) . 3_657 ? C14 N3 Ni1 116.45(18) . 3_657 ? N5 N4 Ni1 117.42(18) . . ? N5 N4 Ni2 118.95(19) . . ? Ni1 N4 Ni2 93.74(9) . . ? N6 N5 N4 178.7(4) . . ? N8 N7 Ni2 123.66(19) . . ? N8 N7 Ni1 115.35(19) . 3_667 ? Ni2 N7 Ni1 92.67(9) . 3_667 ? N9 N8 N7 178.1(3) . . ? C13 O1 Ni1 130.46(18) . . ? C13 O2 Ni2 122.87(16) . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C11 120.8(4) . . ? C2 C3 H3 119.6 . . ? C11 C3 H3 119.6 . . ? C9 C11 C3 115.9(4) . . ? C9 C11 C4 118.6(4) . . ? C3 C11 C4 125.5(4) . . ? C5 C4 C11 121.5(4) . . ? C5 C4 H5 119.2 . . ? C11 C4 H5 119.2 . . ? C4 C5 C12 122.0(4) . . ? C4 C5 H6 119.0 . . ? C12 C5 H6 119.0 . . ? C6 C12 C10 116.8(4) . . ? C6 C12 C5 125.0(4) . . ? C10 C12 C5 118.2(4) . . ? C7 C6 C12 120.6(3) . . ? C7 C6 H8 119.7 . . ? C12 C6 H8 119.7 . . ? C6 C7 C8 119.5(4) . . ? C6 C7 H9 120.3 . . ? C8 C7 H9 120.3 . . ? N2 C8 C7 121.4(4) . . ? N2 C8 H10 119.3 . . ? C7 C8 H10 119.3 . . ? N2 C10 C12 123.0(3) . . ? N2 C10 C9 117.1(3) . . ? C12 C10 C9 119.9(3) . . ? N1 C9 C11 123.0(4) . . ? N1 C9 C10 117.3(3) . . ? C11 C9 C10 119.7(3) . . ? O1 C13 O2 128.1(2) . . ? O1 C13 C15 113.8(2) . . ? O2 C13 C15 118.0(2) . . ? N3 C14 C15 124.5(3) . . ? N3 C14 H14 117.8 . . ? C15 C14 H14 117.8 . . ? C16 C15 C14 117.7(3) . . ? C16 C15 C13 125.8(2) . . ? C14 C15 C13 116.5(2) . . ? C15 C16 C17 118.7(3) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 119.4(3) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? N3 C18 C17 123.1(3) . . ? N3 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 N1 C1 -5.7(3) . . . . ? N2 Ni1 N1 C1 178.7(3) . . . . ? N4 Ni1 N1 C1 144(12) . . . . ? N7 Ni1 N1 C1 -93.4(3) 3_667 . . . ? N3 Ni1 N1 C1 85.1(3) 3_657 . . . ? O1 Ni1 N1 C9 178.0(2) . . . . ? N2 Ni1 N1 C9 2.4(2) . . . . ? N4 Ni1 N1 C9 -32(12) . . . . ? N7 Ni1 N1 C9 90.4(2) 3_667 . . . ? N3 Ni1 N1 C9 -91.2(2) 3_657 . . . ? O1 Ni1 N2 C8 145.0(5) . . . . ? N1 Ni1 N2 C8 175.7(3) . . . . ? N4 Ni1 N2 C8 -4.6(3) . . . . ? N7 Ni1 N2 C8 79.9(3) 3_667 . . . ? N3 Ni1 N2 C8 -96.8(3) 3_657 . . . ? O1 Ni1 N2 C10 -32.0(7) . . . . ? N1 Ni1 N2 C10 -1.4(2) . . . . ? N4 Ni1 N2 C10 178.3(2) . . . . ? N7 Ni1 N2 C10 -97.2(2) 3_667 . . . ? N3 Ni1 N2 C10 86.2(2) 3_657 . . . ? O1 Ni1 N4 N5 53.0(2) . . . . ? N2 Ni1 N4 N5 -131.3(2) . . . . ? N1 Ni1 N4 N5 -97(12) . . . . ? N7 Ni1 N4 N5 140.6(2) 3_667 . . . ? N3 Ni1 N4 N5 -37.8(2) 3_657 . . . ? O1 Ni1 N4 Ni2 -72.43(8) . . . . ? N2 Ni1 N4 Ni2 103.18(9) . . . . ? N1 Ni1 N4 Ni2 137(12) . . . . ? N7 Ni1 N4 Ni2 15.14(9) 3_667 . . . ? N3 Ni1 N4 Ni2 -163.29(8) 3_657 . . . ? O2 Ni2 N4 N5 -50.0(2) . . . . ? O2 Ni2 N4 N5 130.0(2) 3_667 . . . ? N4 Ni2 N4 N5 118(100) 3_667 . . . ? N7 Ni2 N4 N5 -139.6(2) 3_667 . . . ? N7 Ni2 N4 N5 40.4(2) . . . . ? O2 Ni2 N4 Ni1 74.30(9) . . . . ? O2 Ni2 N4 Ni1 -105.70(9) 3_667 . . . ? N4 Ni2 N4 Ni1 -118(100) 3_667 . . . ? N7 Ni2 N4 Ni1 -15.27(9) 3_667 . . . ? N7 Ni2 N4 Ni1 164.73(9) . . . . ? Ni1 N4 N5 N6 149(16) . . . . ? Ni2 N4 N5 N6 -99(16) . . . . ? O2 Ni2 N7 N8 134.0(2) . . . . ? O2 Ni2 N7 N8 -46.0(2) 3_667 . . . ? N4 Ni2 N7 N8 -138.1(2) 3_667 . . . ? N4 Ni2 N7 N8 41.9(2) . . . . ? N7 Ni2 N7 N8 -174(100) 3_667 . . . ? O2 Ni2 N7 Ni1 -102.93(9) . . . 3_667 ? O2 Ni2 N7 Ni1 77.07(9) 3_667 . . 3_667 ? N4 Ni2 N7 Ni1 -15.00(9) 3_667 . . 3_667 ? N4 Ni2 N7 Ni1 165.00(9) . . . 3_667 ? N7 Ni2 N7 Ni1 -51(100) 3_667 . . 3_667 ? Ni2 N7 N8 N9 -162(10) . . . . ? Ni1 N7 N8 N9 86(10) 3_667 . . . ? N2 Ni1 O1 C13 -111.7(6) . . . . ? N1 Ni1 O1 C13 -141.9(3) . . . . ? N4 Ni1 O1 C13 38.4(2) . . . . ? N7 Ni1 O1 C13 -46.4(2) 3_667 . . . ? N3 Ni1 O1 C13 130.0(2) 3_657 . . . ? O2 Ni2 O2 C13 93(100) 3_667 . . . ? N4 Ni2 O2 C13 144.7(2) 3_667 . . . ? N4 Ni2 O2 C13 -35.3(2) . . . . ? N7 Ni2 O2 C13 49.5(2) 3_667 . . . ? N7 Ni2 O2 C13 -130.5(2) . . . . ? C9 N1 C1 C2 0.0(6) . . . . ? Ni1 N1 C1 C2 -176.1(3) . . . . ? N1 C1 C2 C3 -1.4(7) . . . . ? C1 C2 C3 C11 1.7(8) . . . . ? C2 C3 C11 C9 -0.5(7) . . . . ? C2 C3 C11 C4 -180.0(5) . . . . ? C9 C11 C4 C5 -1.2(8) . . . . ? C3 C11 C4 C5 178.2(5) . . . . ? C11 C4 C5 C12 1.9(9) . . . . ? C4 C5 C12 C6 -179.3(5) . . . . ? C4 C5 C12 C10 -0.8(7) . . . . ? C10 C12 C6 C7 0.6(6) . . . . ? C5 C12 C6 C7 179.1(4) . . . . ? C12 C6 C7 C8 0.1(7) . . . . ? C10 N2 C8 C7 -1.7(5) . . . . ? Ni1 N2 C8 C7 -178.5(3) . . . . ? C6 C7 C8 N2 0.5(6) . . . . ? C8 N2 C10 C12 2.4(5) . . . . ? Ni1 N2 C10 C12 179.8(3) . . . . ? C8 N2 C10 C9 -177.2(3) . . . . ? Ni1 N2 C10 C9 0.2(3) . . . . ? C6 C12 C10 N2 -1.8(5) . . . . ? C5 C12 C10 N2 179.6(4) . . . . ? C6 C12 C10 C9 177.7(3) . . . . ? C5 C12 C10 C9 -0.9(5) . . . . ? C1 N1 C9 C11 1.2(5) . . . . ? Ni1 N1 C9 C11 177.9(3) . . . . ? C1 N1 C9 C10 -179.7(3) . . . . ? Ni1 N1 C9 C10 -3.1(4) . . . . ? C3 C11 C9 N1 -0.9(6) . . . . ? C4 C11 C9 N1 178.6(4) . . . . ? C3 C11 C9 C10 -180.0(4) . . . . ? C4 C11 C9 C10 -0.5(6) . . . . ? N2 C10 C9 N1 2.0(4) . . . . ? C12 C10 C9 N1 -177.6(3) . . . . ? N2 C10 C9 C11 -178.9(3) . . . . ? C12 C10 C9 C11 1.5(5) . . . . ? Ni1 O1 C13 O2 11.0(5) . . . . ? Ni1 O1 C13 C15 -167.07(18) . . . . ? Ni2 O2 C13 O1 -12.1(4) . . . . ? Ni2 O2 C13 C15 165.89(18) . . . . ? C18 N3 C14 C15 0.1(4) . . . . ? Ni1 N3 C14 C15 177.9(2) 3_657 . . . ? N3 C14 C15 C16 1.6(5) . . . . ? N3 C14 C15 C13 -177.7(3) . . . . ? O1 C13 C15 C16 -133.9(3) . . . . ? O2 C13 C15 C16 47.9(4) . . . . ? O1 C13 C15 C14 45.4(4) . . . . ? O2 C13 C15 C14 -132.8(3) . . . . ? C14 C15 C16 C17 -2.4(4) . . . . ? C13 C15 C16 C17 176.9(3) . . . . ? C15 C16 C17 C18 1.5(5) . . . . ? C14 N3 C18 C17 -1.1(4) . . . . ? Ni1 N3 C18 C17 -178.6(2) 3_657 . . . ? C16 C17 C18 N3 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.458 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.078