Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_cj105 _database_code_CSD 152732 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Amoroso, A. J.' 'Burrows, M. W.' 'Dickinson, A. A.' 'Jones, C.' 'Willock, D. J.' 'Wong, Wing-tak' _publ_contact_author_name 'Dr A J Amoroso' _publ_contact_author_address ; Dr A J Amoroso Department of Chemistry Cardiff University PO Box 912 Cardiff CF10 3TB UNITED KINGDOM ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H26 Cl2 N6 Ni O11' _chemical_formula_weight 788.19 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' _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 7.074(2) _cell_length_b 12.042(3) _cell_length_c 38.653(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.62(2) _cell_angle_gamma 90.00 _cell_volume 3292.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6005 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2049 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.29 _reflns_number_total 6005 _reflns_number_gt 2573 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0915P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6005 _refine_ls_number_parameters 462 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2144 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.029 _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 0.49024(13) 0.28092(7) 0.12151(2) 0.0328(3) Uani 1 1 d . . . Cl1 Cl 0.8382(4) 0.74800(17) 0.23892(6) 0.0637(7) Uani 1 1 d . . . Cl2 Cl 0.8706(3) 0.20379(19) -0.07510(5) 0.0596(6) Uani 1 1 d . . . N1 N 0.7024(8) 0.3920(4) 0.13348(14) 0.0358(14) Uani 1 1 d . . . N2 N 0.3816(8) 0.3532(4) 0.16420(13) 0.0329(14) Uani 1 1 d . . . N3 N 0.1571(8) 0.1602(5) 0.14220(15) 0.0382(15) Uani 1 1 d . . . N4 N 0.5743(8) 0.1293(5) 0.14061(15) 0.0408(15) Uani 1 1 d . . . N5 N 0.5919(7) 0.2084(5) 0.07768(14) 0.0334(13) Uani 1 1 d . . . N6 N 0.5044(9) 0.4442(5) 0.06664(15) 0.0410(15) Uani 1 1 d . . . O1 O 0.2215(6) 0.2162(4) 0.11490(11) 0.0395(11) Uani 1 1 d . . . O2 O 0.3799(7) 0.3970(4) 0.08768(12) 0.0410(12) Uani 1 1 d . . . O3 O 0.9210(13) 0.7762(6) 0.20823(19) 0.118(3) Uani 1 1 d . . . O4 O 0.8354(13) 0.8215(7) 0.2657(2) 0.134(3) Uani 1 1 d . . . O5 O 0.8377(11) 0.6353(6) 0.24636(18) 0.100(2) Uani 1 1 d U . . O6 O 0.6338(15) 0.7545(9) 0.2271(2) 0.157(4) Uani 1 1 d . . . O7 O 0.8838(10) 0.2929(6) -0.05217(17) 0.093(2) Uani 1 1 d . . . O8 O 1.0457(14) 0.1709(8) -0.0864(3) 0.180(5) Uani 1 1 d . . . O9 O 0.7755(14) 0.2431(7) -0.1059(2) 0.130(3) Uani 1 1 d . . . O10 O 0.7673(12) 0.1161(7) -0.0617(2) 0.117(3) Uani 1 1 d U . . O11 O 0.1017(11) 0.2780(6) 0.04137(17) 0.091(2) Uani 1 1 d . . . H11 H 0.1583 0.2893 0.0596 0.136 Uiso 1 1 calc R . . C1 C 0.8676(10) 0.4040(7) 0.11700(18) 0.0442(19) Uani 1 1 d . . . H1 H 0.9101 0.3473 0.1027 0.053 Uiso 1 1 calc R . . C2 C 0.9762(11) 0.4998(7) 0.1209(2) 0.050(2) Uani 1 1 d . . . H2 H 1.0898 0.5070 0.1092 0.060 Uiso 1 1 calc R . . C3 C 0.9156(12) 0.5823(6) 0.1418(2) 0.051(2) Uani 1 1 d . . . H3 H 0.9860 0.6471 0.1442 0.061 Uiso 1 1 calc R . . C4 C 0.7474(11) 0.5698(6) 0.15968(18) 0.045(2) Uani 1 1 d . . . H4 H 0.7054 0.6252 0.1745 0.055 Uiso 1 1 calc R . . C5 C 0.6444(10) 0.4741(6) 0.15512(18) 0.0380(18) Uani 1 1 d . . . C6 C 0.4629(10) 0.4506(6) 0.17232(17) 0.0340(17) Uani 1 1 d . . . C7 C 0.3830(11) 0.5232(6) 0.19589(19) 0.050(2) Uani 1 1 d . . . H7 H 0.4411 0.5905 0.2011 0.060 Uiso 1 1 calc R . . C8 C 0.2169(11) 0.4938(7) 0.21128(19) 0.052(2) Uani 1 1 d . . . H8 H 0.1602 0.5418 0.2269 0.062 Uiso 1 1 calc R . . C9 C 0.1337(11) 0.3934(7) 0.20372(18) 0.047(2) Uani 1 1 d . . . H9 H 0.0218 0.3723 0.2143 0.056 Uiso 1 1 calc R . . C10 C 0.2205(11) 0.3243(6) 0.17994(18) 0.0398(18) Uani 1 1 d . . . C11 C 0.1481(10) 0.2097(6) 0.17404(18) 0.0386(17) Uani 1 1 d . . . C12 C 0.0805(11) 0.1476(6) 0.2015(2) 0.052(2) Uani 1 1 d . . . H12 H 0.0720 0.1801 0.2232 0.062 Uiso 1 1 calc R . . C13 C 0.0248(12) 0.0373(7) 0.1970(2) 0.059(2) Uani 1 1 d . . . H13 H -0.0218 -0.0042 0.2153 0.071 Uiso 1 1 calc R . . C14 C 0.0416(11) -0.0082(7) 0.1643(2) 0.058(2) Uani 1 1 d . . . H14 H 0.0077 -0.0819 0.1605 0.070 Uiso 1 1 calc R . . C15 C 0.1079(10) 0.0546(6) 0.1373(2) 0.0449(19) Uani 1 1 d . . . H15 H 0.1184 0.0230 0.1155 0.054 Uiso 1 1 calc R . . C16 C 0.5619(10) 0.0946(6) 0.17367(19) 0.0442(19) Uani 1 1 d . . . H16 H 0.5552 0.1473 0.1912 0.053 Uiso 1 1 calc R . . C17 C 0.5590(11) -0.0156(7) 0.1823(2) 0.053(2) Uani 1 1 d . . . H17 H 0.5512 -0.0370 0.2053 0.063 Uiso 1 1 calc R . . C18 C 0.5677(12) -0.0948(7) 0.1565(2) 0.058(2) Uani 1 1 d . . . H18 H 0.5597 -0.1699 0.1618 0.070 Uiso 1 1 calc R . . C19 C 0.5885(11) -0.0602(6) 0.1229(2) 0.047(2) Uani 1 1 d . . . H19 H 0.6014 -0.1122 0.1053 0.056 Uiso 1 1 calc R . . C20 C 0.5904(10) 0.0513(6) 0.11524(17) 0.0357(17) Uani 1 1 d . . . C21 C 0.6099(9) 0.0981(5) 0.08020(17) 0.0314(16) Uani 1 1 d . . . C22 C 0.6499(10) 0.0334(6) 0.05103(19) 0.0429(19) Uani 1 1 d . . . H22 H 0.6631 -0.0432 0.0529 0.052 Uiso 1 1 calc R . . C23 C 0.6689(11) 0.0849(7) 0.0199(2) 0.052(2) Uani 1 1 d . . . H23 H 0.6943 0.0432 0.0002 0.062 Uiso 1 1 calc R . . C24 C 0.6507(10) 0.1981(6) 0.01731(18) 0.0435(19) Uani 1 1 d . . . H24 H 0.6636 0.2331 -0.0040 0.052 Uiso 1 1 calc R . . C25 C 0.6134(9) 0.2588(5) 0.04625(18) 0.0332(16) Uani 1 1 d . . . C26 C 0.6142(10) 0.3825(6) 0.04527(17) 0.0365(17) Uani 1 1 d . . . C27 C 0.7340(11) 0.4367(7) 0.02303(19) 0.046(2) Uani 1 1 d . . . H27 H 0.8095 0.3960 0.0081 0.055 Uiso 1 1 calc R . . C28 C 0.7422(12) 0.5519(8) 0.0229(2) 0.058(2) Uani 1 1 d . . . H28 H 0.8207 0.5885 0.0075 0.070 Uiso 1 1 calc R . . C29 C 0.6345(12) 0.6112(7) 0.0454(2) 0.058(2) Uani 1 1 d . . . H29 H 0.6436 0.6882 0.0463 0.070 Uiso 1 1 calc R . . C30 C 0.5131(10) 0.5559(6) 0.06663(18) 0.0420(19) Uani 1 1 d . . . H30 H 0.4353 0.5960 0.0813 0.050 Uiso 1 1 calc R . . C31 C 0.1328(14) 0.1708(8) 0.0308(3) 0.086(3) Uani 1 1 d . . . H31A H 0.2629 0.1623 0.0245 0.129 Uiso 1 1 calc R . . H31B H 0.0531 0.1543 0.0112 0.129 Uiso 1 1 calc R . . H31C H 0.1042 0.1207 0.0494 0.129 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 0.0338(5) 0.0324(5) 0.0324(5) -0.0026(4) 0.0052(4) 0.0027(5) Cl1 0.101(2) 0.0437(13) 0.0467(12) -0.0005(10) 0.0085(13) 0.0059(12) Cl2 0.0720(15) 0.0555(14) 0.0516(13) -0.0089(11) 0.0155(11) -0.0076(13) N1 0.038(4) 0.029(3) 0.040(3) -0.002(3) 0.002(3) 0.002(3) N2 0.036(3) 0.033(3) 0.029(3) -0.003(3) 0.001(3) -0.003(3) N3 0.034(4) 0.032(3) 0.049(4) 0.008(3) 0.009(3) -0.010(3) N4 0.042(4) 0.037(3) 0.043(4) -0.002(3) 0.003(3) -0.004(3) N5 0.030(3) 0.032(3) 0.038(3) -0.003(3) 0.000(3) 0.002(3) N6 0.044(4) 0.036(4) 0.042(4) 0.008(3) 0.002(3) -0.002(3) O1 0.041(3) 0.040(3) 0.038(3) 0.003(2) 0.004(2) -0.006(3) O2 0.040(3) 0.037(3) 0.046(3) 0.009(2) 0.013(2) 0.005(2) O3 0.160(8) 0.096(6) 0.100(6) 0.005(5) 0.057(5) -0.044(6) O4 0.144(8) 0.125(7) 0.134(7) -0.085(6) 0.022(6) -0.027(6) O5 0.120(4) 0.088(4) 0.091(3) 0.011(3) 0.013(3) 0.004(3) O6 0.150(9) 0.182(10) 0.138(8) -0.022(7) -0.043(7) 0.026(7) O7 0.113(6) 0.080(5) 0.085(5) -0.026(4) 0.027(4) -0.026(4) O8 0.122(8) 0.154(9) 0.265(13) -0.044(8) 0.064(8) 0.062(7) O9 0.162(8) 0.145(8) 0.084(5) 0.026(5) -0.017(5) -0.055(6) O10 0.134(4) 0.112(4) 0.105(4) 0.008(3) 0.013(3) -0.031(3) O11 0.098(6) 0.105(6) 0.069(5) -0.006(4) -0.027(4) 0.017(5) C1 0.036(5) 0.053(5) 0.044(4) 0.000(4) 0.009(4) 0.003(4) C2 0.031(4) 0.063(5) 0.055(5) 0.007(5) 0.012(4) -0.008(5) C3 0.057(6) 0.036(5) 0.060(5) -0.003(4) -0.001(5) -0.009(4) C4 0.050(5) 0.041(5) 0.046(5) -0.007(4) 0.008(4) -0.013(4) C5 0.042(5) 0.033(4) 0.039(4) 0.003(3) 0.004(4) 0.001(4) C6 0.032(4) 0.033(4) 0.037(4) -0.002(3) 0.009(3) 0.007(3) C7 0.057(5) 0.041(5) 0.052(5) -0.006(4) 0.011(4) -0.007(4) C8 0.056(5) 0.051(5) 0.048(5) -0.018(4) 0.016(4) 0.009(5) C9 0.049(5) 0.057(5) 0.034(4) -0.006(4) 0.016(4) 0.006(4) C10 0.041(5) 0.040(4) 0.039(4) -0.001(4) 0.004(4) 0.005(4) C11 0.035(4) 0.041(4) 0.040(4) -0.006(4) 0.009(3) -0.003(4) C12 0.055(5) 0.051(5) 0.050(5) 0.000(4) 0.022(4) -0.007(4) C13 0.063(6) 0.058(6) 0.058(6) 0.005(5) 0.026(5) -0.014(5) C14 0.048(5) 0.044(5) 0.083(7) 0.012(5) 0.013(5) -0.009(4) C15 0.040(5) 0.047(5) 0.048(5) 0.004(4) 0.004(4) 0.000(4) C16 0.044(5) 0.051(5) 0.037(4) 0.002(4) 0.000(4) 0.009(4) C17 0.067(6) 0.047(5) 0.044(5) 0.015(4) 0.001(4) 0.002(5) C18 0.066(6) 0.035(5) 0.073(6) 0.009(5) -0.004(5) -0.005(4) C19 0.058(5) 0.035(4) 0.048(5) -0.004(4) 0.001(4) 0.000(4) C20 0.038(4) 0.031(4) 0.037(4) -0.001(3) -0.011(3) -0.003(3) C21 0.028(4) 0.031(4) 0.035(4) -0.002(3) -0.006(3) 0.005(3) C22 0.040(5) 0.038(4) 0.051(5) -0.014(4) 0.004(4) 0.000(4) C23 0.056(6) 0.049(5) 0.051(5) -0.020(4) 0.011(4) -0.005(4) C24 0.039(5) 0.058(5) 0.033(4) -0.002(4) 0.009(3) -0.007(4) C25 0.022(4) 0.037(4) 0.040(4) -0.004(3) 0.003(3) 0.002(3) C26 0.036(4) 0.042(4) 0.032(4) 0.000(3) -0.002(3) 0.001(4) C27 0.046(5) 0.049(5) 0.043(5) 0.009(4) 0.008(4) -0.004(4) C28 0.049(5) 0.069(6) 0.058(6) 0.009(5) 0.010(4) -0.014(5) C29 0.061(6) 0.049(5) 0.064(6) 0.015(5) 0.002(5) -0.003(5) C30 0.041(5) 0.035(4) 0.050(5) 0.011(4) -0.002(4) 0.008(4) C31 0.068(7) 0.084(7) 0.106(8) -0.001(7) -0.031(6) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.025(5) . ? Ni1 N5 2.044(5) . ? Ni1 N4 2.055(6) . ? Ni1 N1 2.059(6) . ? Ni1 O2 2.062(5) . ? Ni1 O1 2.067(5) . ? Cl1 O4 1.363(7) . ? Cl1 O3 1.371(7) . ? Cl1 O5 1.387(7) . ? Cl1 O6 1.514(10) . ? Cl2 O8 1.375(9) . ? Cl2 O10 1.388(8) . ? Cl2 O7 1.395(6) . ? Cl2 O9 1.442(8) . ? N1 C1 1.345(9) . ? N1 C5 1.361(8) . ? N2 C6 1.342(8) . ? N2 C10 1.344(9) . ? N3 C15 1.333(9) . ? N3 O1 1.337(6) . ? N3 C11 1.369(8) . ? N4 C16 1.348(8) . ? N4 C20 1.364(8) . ? N5 C21 1.337(8) . ? N5 C25 1.368(8) . ? N6 O2 1.332(7) . ? N6 C30 1.346(9) . ? N6 C26 1.360(8) . ? O11 C31 1.372(10) . ? C1 C2 1.393(10) . ? C2 C3 1.353(10) . ? C3 C4 1.390(10) . ? C4 C5 1.374(9) . ? C5 C6 1.480(9) . ? C6 C7 1.387(9) . ? C7 C8 1.370(10) . ? C8 C9 1.374(10) . ? C9 C10 1.388(9) . ? C10 C11 1.488(10) . ? C11 C12 1.387(10) . ? C12 C13 1.396(10) . ? C13 C14 1.386(11) . ? C14 C15 1.373(10) . ? C16 C17 1.368(10) . ? C17 C18 1.380(10) . ? C18 C19 1.374(10) . ? C19 C20 1.374(9) . ? C20 C21 1.475(9) . ? C21 C22 1.401(9) . ? C22 C23 1.363(10) . ? C23 C24 1.372(10) . ? C24 C25 1.364(9) . ? C25 C26 1.490(9) . ? C26 C27 1.378(10) . ? C27 C28 1.388(11) . ? C28 C29 1.365(11) . ? C29 C30 1.366(10) . ? 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 N2 Ni1 N5 178.2(2) . . ? N2 Ni1 N4 101.6(2) . . ? N5 Ni1 N4 79.3(2) . . ? N2 Ni1 N1 79.6(2) . . ? N5 Ni1 N1 101.6(2) . . ? N4 Ni1 N1 106.8(2) . . ? N2 Ni1 O2 94.6(2) . . ? N5 Ni1 O2 84.2(2) . . ? N4 Ni1 O2 159.4(2) . . ? N1 Ni1 O2 88.4(2) . . ? N2 Ni1 O1 84.6(2) . . ? N5 Ni1 O1 93.9(2) . . ? N4 Ni1 O1 88.4(2) . . ? N1 Ni1 O1 159.9(2) . . ? O2 Ni1 O1 80.55(19) . . ? O4 Cl1 O3 120.4(5) . . ? O4 Cl1 O5 118.5(5) . . ? O3 Cl1 O5 115.1(5) . . ? O4 Cl1 O6 100.0(6) . . ? O3 Cl1 O6 98.1(6) . . ? O5 Cl1 O6 96.3(5) . . ? O8 Cl2 O10 112.3(6) . . ? O8 Cl2 O7 111.6(6) . . ? O10 Cl2 O7 112.3(4) . . ? O8 Cl2 O9 104.3(7) . . ? O10 Cl2 O9 108.4(5) . . ? O7 Cl2 O9 107.4(5) . . ? C1 N1 C5 118.8(6) . . ? C1 N1 Ni1 126.8(5) . . ? C5 N1 Ni1 112.7(5) . . ? C6 N2 C10 119.0(6) . . ? C6 N2 Ni1 113.6(4) . . ? C10 N2 Ni1 126.1(5) . . ? C15 N3 O1 117.4(6) . . ? C15 N3 C11 121.9(6) . . ? O1 N3 C11 120.6(6) . . ? C16 N4 C20 118.4(6) . . ? C16 N4 Ni1 126.4(5) . . ? C20 N4 Ni1 112.3(4) . . ? C21 N5 C25 119.6(6) . . ? C21 N5 Ni1 113.5(4) . . ? C25 N5 Ni1 126.2(4) . . ? O2 N6 C30 117.1(6) . . ? O2 N6 C26 121.6(6) . . ? C30 N6 C26 121.2(7) . . ? N3 O1 Ni1 114.4(4) . . ? N6 O2 Ni1 115.3(4) . . ? N1 C1 C2 121.2(7) . . ? C3 C2 C1 119.7(7) . . ? C2 C3 C4 119.7(7) . . ? C5 C4 C3 118.9(7) . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 114.0(6) . . ? C4 C5 C6 124.3(7) . . ? N2 C6 C7 121.9(7) . . ? N2 C6 C5 115.7(6) . . ? C7 C6 C5 122.4(7) . . ? C8 C7 C6 118.7(7) . . ? C7 C8 C9 120.2(7) . . ? C8 C9 C10 118.5(7) . . ? N2 C10 C9 121.8(7) . . ? N2 C10 C11 117.6(6) . . ? C9 C10 C11 120.3(7) . . ? N3 C11 C12 118.2(7) . . ? N3 C11 C10 121.5(6) . . ? C12 C11 C10 120.2(7) . . ? C11 C12 C13 121.2(7) . . ? C14 C13 C12 117.5(8) . . ? C15 C14 C13 120.5(8) . . ? N3 C15 C14 120.6(8) . . ? N4 C16 C17 122.1(7) . . ? C16 C17 C18 119.6(7) . . ? C19 C18 C17 118.6(7) . . ? C20 C19 C18 120.1(7) . . ? N4 C20 C19 121.1(7) . . ? N4 C20 C21 114.0(6) . . ? C19 C20 C21 124.9(6) . . ? N5 C21 C22 120.9(6) . . ? N5 C21 C20 115.9(6) . . ? C22 C21 C20 123.2(6) . . ? C23 C22 C21 118.7(7) . . ? C22 C23 C24 120.3(7) . . ? C25 C24 C23 119.5(7) . . ? C24 C25 N5 121.0(6) . . ? C24 C25 C26 120.9(7) . . ? N5 C25 C26 117.8(6) . . ? N6 C26 C27 118.7(7) . . ? N6 C26 C25 121.8(6) . . ? C27 C26 C25 119.5(7) . . ? C26 C27 C28 120.1(8) . . ? C29 C28 C27 119.7(8) . . ? C30 C29 C28 119.1(8) . . ? N6 C30 C29 121.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 177.3(6) . . . . ? N5 Ni1 N1 C1 -4.0(6) . . . . ? N4 Ni1 N1 C1 78.2(6) . . . . ? O2 Ni1 N1 C1 -87.7(6) . . . . ? O1 Ni1 N1 C1 -144.0(6) . . . . ? N2 Ni1 N1 C5 -17.9(4) . . . . ? N5 Ni1 N1 C5 160.8(4) . . . . ? N4 Ni1 N1 C5 -117.0(5) . . . . ? O2 Ni1 N1 C5 77.1(5) . . . . ? O1 Ni1 N1 C5 20.8(9) . . . . ? N5 Ni1 N2 C6 -117(7) . . . . ? N4 Ni1 N2 C6 123.1(5) . . . . ? N1 Ni1 N2 C6 17.9(5) . . . . ? O2 Ni1 N2 C6 -69.6(5) . . . . ? O1 Ni1 N2 C6 -149.6(5) . . . . ? N5 Ni1 N2 C10 50(8) . . . . ? N4 Ni1 N2 C10 -70.3(6) . . . . ? N1 Ni1 N2 C10 -175.5(6) . . . . ? O2 Ni1 N2 C10 97.0(6) . . . . ? O1 Ni1 N2 C10 17.0(6) . . . . ? N2 Ni1 N4 C16 -2.1(6) . . . . ? N5 Ni1 N4 C16 179.4(6) . . . . ? N1 Ni1 N4 C16 80.4(6) . . . . ? O2 Ni1 N4 C16 -143.4(6) . . . . ? O1 Ni1 N4 C16 -86.3(6) . . . . ? N2 Ni1 N4 C20 158.2(5) . . . . ? N5 Ni1 N4 C20 -20.2(5) . . . . ? N1 Ni1 N4 C20 -119.3(5) . . . . ? O2 Ni1 N4 C20 17.0(9) . . . . ? O1 Ni1 N4 C20 74.1(5) . . . . ? N2 Ni1 N5 C21 -103(7) . . . . ? N4 Ni1 N5 C21 17.1(5) . . . . ? N1 Ni1 N5 C21 122.3(5) . . . . ? O2 Ni1 N5 C21 -150.6(5) . . . . ? O1 Ni1 N5 C21 -70.5(5) . . . . ? N2 Ni1 N5 C25 67(8) . . . . ? N4 Ni1 N5 C25 -173.2(6) . . . . ? N1 Ni1 N5 C25 -68.0(5) . . . . ? O2 Ni1 N5 C25 19.1(5) . . . . ? O1 Ni1 N5 C25 99.2(5) . . . . ? C15 N3 O1 Ni1 -121.8(5) . . . . ? C11 N3 O1 Ni1 56.4(7) . . . . ? N2 Ni1 O1 N3 -54.7(4) . . . . ? N5 Ni1 O1 N3 126.2(4) . . . . ? N4 Ni1 O1 N3 47.0(4) . . . . ? N1 Ni1 O1 N3 -92.9(7) . . . . ? O2 Ni1 O1 N3 -150.4(4) . . . . ? C30 N6 O2 Ni1 -125.4(5) . . . . ? C26 N6 O2 Ni1 56.6(7) . . . . ? N2 Ni1 O2 N6 126.8(4) . . . . ? N5 Ni1 O2 N6 -54.6(4) . . . . ? N4 Ni1 O2 N6 -91.2(7) . . . . ? N1 Ni1 O2 N6 47.3(4) . . . . ? O1 Ni1 O2 N6 -149.5(4) . . . . ? C5 N1 C1 C2 -2.0(10) . . . . ? Ni1 N1 C1 C2 162.0(5) . . . . ? N1 C1 C2 C3 0.4(12) . . . . ? C1 C2 C3 C4 1.3(12) . . . . ? C2 C3 C4 C5 -1.3(12) . . . . ? C1 N1 C5 C4 2.0(10) . . . . ? Ni1 N1 C5 C4 -164.1(5) . . . . ? C1 N1 C5 C6 -178.8(6) . . . . ? Ni1 N1 C5 C6 15.1(7) . . . . ? C3 C4 C5 N1 -0.4(11) . . . . ? C3 C4 C5 C6 -179.5(7) . . . . ? C10 N2 C6 C7 -1.5(10) . . . . ? Ni1 N2 C6 C7 166.2(6) . . . . ? C10 N2 C6 C5 177.2(6) . . . . ? Ni1 N2 C6 C5 -15.1(7) . . . . ? N1 C5 C6 N2 -0.2(9) . . . . ? C4 C5 C6 N2 179.0(7) . . . . ? N1 C5 C6 C7 178.5(7) . . . . ? C4 C5 C6 C7 -2.3(11) . . . . ? N2 C6 C7 C8 0.3(11) . . . . ? C5 C6 C7 C8 -178.4(7) . . . . ? C6 C7 C8 C9 1.0(12) . . . . ? C7 C8 C9 C10 -0.9(12) . . . . ? C6 N2 C10 C9 1.5(10) . . . . ? Ni1 N2 C10 C9 -164.4(5) . . . . ? C6 N2 C10 C11 -171.8(6) . . . . ? Ni1 N2 C10 C11 22.2(9) . . . . ? C8 C9 C10 N2 -0.3(11) . . . . ? C8 C9 C10 C11 172.8(7) . . . . ? C15 N3 C11 C12 -1.8(10) . . . . ? O1 N3 C11 C12 -179.9(6) . . . . ? C15 N3 C11 C10 174.1(6) . . . . ? O1 N3 C11 C10 -3.9(10) . . . . ? N2 C10 C11 N3 -39.5(9) . . . . ? C9 C10 C11 N3 147.0(7) . . . . ? N2 C10 C11 C12 136.4(7) . . . . ? C9 C10 C11 C12 -37.1(10) . . . . ? N3 C11 C12 C13 0.7(11) . . . . ? C10 C11 C12 C13 -175.3(7) . . . . ? C11 C12 C13 C14 0.7(12) . . . . ? C12 C13 C14 C15 -1.0(12) . . . . ? O1 N3 C15 C14 179.6(6) . . . . ? C11 N3 C15 C14 1.5(11) . . . . ? C13 C14 C15 N3 0.0(12) . . . . ? C20 N4 C16 C17 -2.1(11) . . . . ? Ni1 N4 C16 C17 157.2(6) . . . . ? N4 C16 C17 C18 -0.4(12) . . . . ? C16 C17 C18 C19 3.2(12) . . . . ? C17 C18 C19 C20 -3.4(12) . . . . ? C16 N4 C20 C19 1.9(10) . . . . ? Ni1 N4 C20 C19 -160.2(6) . . . . ? C16 N4 C20 C21 -177.9(6) . . . . ? Ni1 N4 C20 C21 20.0(7) . . . . ? C18 C19 C20 N4 0.8(12) . . . . ? C18 C19 C20 C21 -179.4(7) . . . . ? C25 N5 C21 C22 -0.3(10) . . . . ? Ni1 N5 C21 C22 170.2(5) . . . . ? C25 N5 C21 C20 178.1(6) . . . . ? Ni1 N5 C21 C20 -11.4(7) . . . . ? N4 C20 C21 N5 -5.9(9) . . . . ? C19 C20 C21 N5 174.3(7) . . . . ? N4 C20 C21 C22 172.5(6) . . . . ? C19 C20 C21 C22 -7.3(11) . . . . ? N5 C21 C22 C23 -0.4(10) . . . . ? C20 C21 C22 C23 -178.7(7) . . . . ? C21 C22 C23 C24 0.5(11) . . . . ? C22 C23 C24 C25 0.0(12) . . . . ? C23 C24 C25 N5 -0.7(11) . . . . ? C23 C24 C25 C26 173.0(7) . . . . ? C21 N5 C25 C24 0.9(10) . . . . ? Ni1 N5 C25 C24 -168.3(5) . . . . ? C21 N5 C25 C26 -173.1(6) . . . . ? Ni1 N5 C25 C26 17.8(8) . . . . ? O2 N6 C26 C27 177.1(6) . . . . ? C30 N6 C26 C27 -0.9(10) . . . . ? O2 N6 C26 C25 -5.2(10) . . . . ? C30 N6 C26 C25 176.8(6) . . . . ? C24 C25 C26 N6 150.7(7) . . . . ? N5 C25 C26 N6 -35.3(9) . . . . ? C24 C25 C26 C27 -31.6(10) . . . . ? N5 C25 C26 C27 142.4(7) . . . . ? N6 C26 C27 C28 0.5(11) . . . . ? C25 C26 C27 C28 -177.3(7) . . . . ? C26 C27 C28 C29 1.6(12) . . . . ? C27 C28 C29 C30 -3.2(12) . . . . ? O2 N6 C30 C29 -178.9(6) . . . . ? C26 N6 C30 C29 -0.8(11) . . . . ? C28 C29 C30 N6 2.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.303 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.102