# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full ? _journal_coden_cambridge 222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Jones, M. B.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'Hardcastle, K. I.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; _publ_contact_author_address ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; _publ_contact_author_email cmacbet@emory.edu _publ_contact_author_phone 404-727-7033 _publ_contact_author_name 'C. E. MacBeth' _publ_requested_journal da _publ_requested_category SC _publ_section_title ; Chelating tris(amidate) ligands: versatile scaffolds for nickel(II) ; data_mbj_6_219s _database_code_depnum_ccdc_archive 'CCDC 738758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H126 Co N12 Ni O6' _chemical_formula_weight 1529.62 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' Co Co 0.3494 0.9721 '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 Rhombohedral _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 19.0019(17) _cell_length_b 19.0019(17) _cell_length_c 21.787(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6812.7(15) _cell_formula_units_Z 3 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used 3402 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 17.83 _exptl_crystal_description prism _exptl_crystal_colour pink-purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2469 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9446 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41833 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.1243 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 30.43 _reflns_number_total 8677 _reflns_number_gt 4281 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.618 304.6 60.3 2 0.333 0.667 0.284 303.5 60.4 3 0.667 0.333 -0.049 305.2 60.2 _platon_squeeze_details ; ; _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^)+(0.0700P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 8677 _refine_ls_number_parameters 317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1447 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.2913(3) 0.7108(3) 1.0266(3) 0.0444(15) Uani 1 1 d . . . C2 C 0.2450(3) 0.7009(3) 1.0768(3) 0.0646(14) Uani 1 1 d . . . H2A H 0.2400 0.6638 1.1080 0.078 Uiso 1 1 calc R . . C3 C 0.2047(4) 0.7450(4) 1.0828(3) 0.0831(19) Uani 1 1 d . . . H3A H 0.1742 0.7390 1.1190 0.100 Uiso 1 1 calc R . . C4 C 0.2079(5) 0.7939(4) 1.0400(4) 0.087(3) Uani 1 1 d . . . H4A H 0.1732 0.8164 1.0420 0.105 Uiso 1 1 calc R . . C5 C 0.2629(4) 0.8142(3) 0.9899(3) 0.0758(15) Uani 1 1 d . . . H5A H 0.2715 0.8563 0.9621 0.091 Uiso 1 1 calc R . . C6 C 0.3042(3) 0.7707(3) 0.9825(2) 0.0514(11) Uani 1 1 d . . . C7 C 0.4108(4) 0.8537(3) 0.9118(3) 0.077(2) Uani 1 1 d . . . C8 C 0.4678(5) 0.8616(3) 0.8631(3) 0.095(2) Uani 1 1 d . . . H8A H 0.4554 0.8060 0.8505 0.114 Uiso 1 1 calc R . . C9 C 0.5535(5) 0.9066(5) 0.8905(5) 0.172(5) Uani 1 1 d . . . H9A H 0.5574 0.8745 0.9241 0.258 Uiso 1 1 calc R . . H9B H 0.5647 0.9596 0.9061 0.258 Uiso 1 1 calc R . . H9C H 0.5932 0.9146 0.8587 0.258 Uiso 1 1 calc R . . C10 C 0.4424(8) 0.9014(7) 0.8074(5) 0.167(5) Uani 1 1 d . . . H10A H 0.3858 0.8643 0.7957 0.250 Uiso 1 1 calc R . . H10B H 0.4779 0.9107 0.7721 0.250 Uiso 1 1 calc R . . H10C H 0.4483 0.9533 0.8209 0.250 Uiso 1 1 calc R . . C11 C 0.3333 0.6667 0.8126(6) 0.038(2) Uani 1 3 d S . . C12 C 0.3754(3) 0.7527(3) 0.5433(3) 0.0448(15) Uani 1 1 d . . . C13 C 0.3625(3) 0.8006(3) 0.5874(2) 0.0543(12) Uani 1 1 d . . . C14 C 0.4042(3) 0.8848(3) 0.5801(3) 0.0728(15) Uani 1 1 d . . . H14A H 0.3958 0.9182 0.6081 0.087 Uiso 1 1 calc R . . C15 C 0.4582(5) 0.9193(4) 0.5314(4) 0.088(3) Uani 1 1 d . . . H15A H 0.4929 0.9766 0.5300 0.106 Uiso 1 1 calc R . . C16 C 0.4619(4) 0.8739(4) 0.4873(3) 0.0793(18) Uani 1 1 d . . . H16A H 0.4924 0.8989 0.4513 0.095 Uiso 1 1 calc R . . C17 C 0.4213(3) 0.7894(3) 0.4929(2) 0.0656(14) Uani 1 1 d . . . H17A H 0.4258 0.7574 0.4613 0.079 Uiso 1 1 calc R . . C18 C 0.2555(4) 0.7753(4) 0.6570(3) 0.0753(19) Uani 1 1 d . . . C19 C 0.2002(5) 0.7282(5) 0.7073(3) 0.102(3) Uani 1 1 d . . . H19A H 0.2130 0.6850 0.7194 0.122 Uiso 1 1 calc R . . C20 C 0.1123(5) 0.6845(7) 0.6775(5) 0.166(5) Uani 1 1 d . . . H20A H 0.1103 0.6490 0.6440 0.249 Uiso 1 1 calc R . . H20B H 0.1004 0.7255 0.6612 0.249 Uiso 1 1 calc R . . H20C H 0.0719 0.6520 0.7087 0.249 Uiso 1 1 calc R . . C21 C 0.2270(8) 0.7915(6) 0.7625(5) 0.166(5) Uani 1 1 d . . . H21A H 0.2841 0.8109 0.7728 0.249 Uiso 1 1 calc R . . H21B H 0.1929 0.7648 0.7984 0.249 Uiso 1 1 calc R . . H21C H 0.2206 0.8376 0.7502 0.249 Uiso 1 1 calc R . . C1S C 0.3852(7) 0.9312(6) 0.1413(7) 0.226(8) Uani 1 1 d . . . H1SA H 0.3945 0.8887 0.1593 0.271 Uiso 1 1 calc R . . H1SB H 0.3460 0.9070 0.1071 0.271 Uiso 1 1 calc R . . C2S C 0.3489(7) 0.9679(8) 0.1944(6) 0.192(5) Uani 1 1 d . . . H2SA H 0.2973 0.9238 0.2102 0.288 Uiso 1 1 calc R . . H2SB H 0.3401 1.0099 0.1761 0.288 Uiso 1 1 calc R . . H2SC H 0.3881 0.9914 0.2282 0.288 Uiso 1 1 calc R . . C3S C 0.4553(9) 1.0693(6) 0.0953(8) 0.239(9) Uani 1 1 d . . . H3SA H 0.5073 1.1106 0.0768 0.287 Uiso 1 1 calc R . . H3SB H 0.4415 1.0949 0.1292 0.287 Uiso 1 1 calc R . . C4S C 0.3803(10) 1.0322(8) 0.0415(6) 0.207(6) Uani 1 1 d . . . H4SA H 0.3740 1.0767 0.0250 0.311 Uiso 1 1 calc R . . H4SB H 0.3291 0.9915 0.0603 0.311 Uiso 1 1 calc R . . H4SC H 0.3946 1.0070 0.0081 0.311 Uiso 1 1 calc R . . C5S C 0.4893(9) 0.9606(8) 0.0715(7) 0.205(8) Uani 1 1 d . . . H5SA H 0.4903 0.9140 0.0910 0.246 Uiso 1 1 calc R . . H5SB H 0.4478 0.9385 0.0386 0.246 Uiso 1 1 calc R . . C6S C 0.5655(8) 1.0106(10) 0.0442(8) 0.303(13) Uani 1 1 d . . . H6SA H 0.5713 0.9834 0.0079 0.454 Uiso 1 1 calc R . . H6SB H 0.6086 1.0212 0.0737 0.454 Uiso 1 1 calc R . . H6SC H 0.5696 1.0622 0.0319 0.454 Uiso 1 1 calc R . . C7S C 0.5284(7) 1.0407(7) 0.1633(7) 0.191(7) Uani 1 1 d . . . H7SA H 0.5107 1.0650 0.1957 0.229 Uiso 1 1 calc R . . H7SB H 0.5759 1.0856 0.1424 0.229 Uiso 1 1 calc R . . C8S C 0.5541(9) 0.9879(10) 0.1925(8) 0.300(12) Uani 1 1 d . . . H8SA H 0.6005 1.0204 0.2196 0.449 Uiso 1 1 calc R . . H8SB H 0.5700 0.9619 0.1609 0.449 Uiso 1 1 calc R . . H8SC H 0.5091 0.9462 0.2167 0.449 Uiso 1 1 calc R . . Co1 Co 0.3333 0.6667 0.90574(4) 0.0347(3) Uani 1 3 d S . . N1 N 0.3333 0.6667 1.0138(4) 0.045(2) Uani 1 3 d S . . N2 N 0.3333 0.6667 0.7590(6) 0.055(3) Uani 1 3 d S . . N3 N 0.3539(3) 0.7785(2) 0.93084(17) 0.0568(10) Uani 1 1 d . . . N4 N 0.3333 0.6667 0.5547(4) 0.042(2) Uani 1 3 d S . . N5 N 0.3130(3) 0.7578(2) 0.63891(18) 0.0571(10) Uani 1 1 d . . . N1S N 0.4628(4) 1.0001(4) 0.1189(4) 0.136(3) Uani 1 1 d . . . Ni1 Ni 0.3333 0.6667 0.66436(4) 0.0394(3) Uani 1 3 d S . . O1 O 0.4166(3) 0.9181(2) 0.9360(2) 0.1089(16) Uani 1 1 d . . . O2 O 0.2495(3) 0.8343(3) 0.6338(2) 0.1114(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 C1 0.052(3) 0.034(3) 0.055(5) -0.016(3) -0.009(3) 0.028(3) C2 0.064(3) 0.066(3) 0.069(4) 0.010(3) 0.020(3) 0.037(3) C3 0.075(4) 0.082(4) 0.102(5) -0.004(4) 0.040(4) 0.047(4) C4 0.116(6) 0.089(5) 0.096(7) 0.011(5) 0.035(5) 0.080(5) C5 0.090(4) 0.065(3) 0.083(4) -0.008(3) 0.004(3) 0.047(3) C6 0.052(3) 0.041(2) 0.066(3) -0.007(2) 0.006(2) 0.027(2) C7 0.099(5) 0.037(3) 0.084(5) 0.006(3) 0.034(4) 0.026(3) C8 0.133(6) 0.043(3) 0.092(5) 0.011(3) 0.048(4) 0.030(4) C9 0.109(7) 0.117(7) 0.214(10) -0.071(7) 0.069(7) 0.000(5) C10 0.287(14) 0.133(9) 0.118(9) 0.086(7) 0.069(9) 0.132(10) C11 0.037(4) 0.037(4) 0.040(8) 0.000 0.000 0.019(2) C12 0.051(3) 0.043(3) 0.050(4) 0.005(3) -0.007(3) 0.030(3) C13 0.053(3) 0.041(2) 0.069(3) 0.014(2) 0.010(2) 0.023(2) C14 0.077(4) 0.049(3) 0.088(4) 0.012(3) 0.012(3) 0.028(3) C15 0.103(6) 0.048(4) 0.109(7) 0.027(5) 0.030(5) 0.035(4) C16 0.070(4) 0.063(4) 0.089(5) 0.042(4) 0.029(3) 0.021(3) C17 0.066(3) 0.064(3) 0.064(3) 0.008(3) 0.015(3) 0.031(3) C18 0.103(5) 0.088(4) 0.075(4) 0.024(4) 0.028(4) 0.077(4) C19 0.167(7) 0.117(5) 0.084(4) 0.045(4) 0.060(5) 0.118(6) C20 0.094(6) 0.238(11) 0.192(9) 0.122(9) 0.049(6) 0.102(7) C21 0.288(14) 0.162(9) 0.109(9) -0.006(6) 0.055(9) 0.158(10) C1S 0.160(11) 0.080(6) 0.36(2) -0.033(9) -0.151(14) 0.000(7) C2S 0.137(9) 0.155(11) 0.221(14) 0.009(9) -0.060(9) 0.025(8) C3S 0.238(15) 0.076(6) 0.40(2) -0.049(10) 0.123(16) 0.075(8) C4S 0.283(17) 0.154(11) 0.228(15) 0.002(9) 0.077(13) 0.142(12) C5S 0.183(12) 0.183(12) 0.284(19) -0.176(14) -0.081(13) 0.117(11) C6S 0.147(11) 0.39(3) 0.33(2) -0.23(2) 0.026(12) 0.099(13) C7S 0.119(8) 0.158(11) 0.281(18) -0.138(13) -0.076(9) 0.058(8) C8S 0.34(2) 0.40(3) 0.32(2) -0.22(2) -0.247(18) 0.30(2) Co1 0.0317(4) 0.0317(4) 0.0406(8) 0.000 0.000 0.01586(18) N1 0.036(3) 0.036(3) 0.064(7) 0.000 0.000 0.0179(15) N2 0.048(4) 0.048(4) 0.068(9) 0.000 0.000 0.0242(19) N3 0.079(3) 0.046(2) 0.057(2) 0.0130(18) 0.018(2) 0.040(2) N4 0.040(3) 0.040(3) 0.046(6) 0.000 0.000 0.0201(15) N5 0.075(3) 0.050(2) 0.058(2) 0.0078(19) 0.017(2) 0.040(2) N1S 0.095(4) 0.081(4) 0.224(7) -0.082(4) -0.040(5) 0.038(4) Ni1 0.0363(4) 0.0363(4) 0.0457(8) 0.000 0.000 0.01815(19) O1 0.162(4) 0.041(2) 0.115(3) 0.004(2) 0.047(3) 0.045(3) O2 0.163(4) 0.119(4) 0.117(4) 0.044(3) 0.055(3) 0.120(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.357(8) . ? C1 C6 1.413(7) . ? C1 N1 1.446(5) . ? C2 C3 1.395(8) . ? C2 H2A 0.9500 . ? C3 C4 1.297(9) . ? C3 H3A 0.9500 . ? C4 C5 1.424(9) . ? C4 H4A 0.9500 . ? C5 C6 1.405(7) . ? C5 H5A 0.9500 . ? C6 N3 1.429(6) . ? C7 O1 1.285(6) . ? C7 N3 1.356(7) . ? C7 C8 1.470(9) . ? C8 C9 1.532(12) . ? C8 C10 1.626(11) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N2 1.167(7) . ? C11 Co1 2.029(13) . ? C12 C17 1.358(8) . ? C12 C13 1.426(7) . ? C12 N4 1.438(6) . ? C13 C14 1.394(7) . ? C13 N5 1.428(6) . ? C14 C15 1.391(9) . ? C14 H14A 0.9500 . ? C15 C16 1.316(9) . ? C15 H15A 0.9500 . ? C16 C17 1.397(8) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 O2 1.285(6) . ? C18 N5 1.352(7) . ? C18 C19 1.471(8) . ? C19 C20 1.586(13) . ? C19 C21 1.594(12) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C1S N1S 1.482(14) . ? C1S C2S 1.667(18) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S N1S 1.484(14) . ? C3S C4S 1.702(19) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5S C6S 1.406(18) . ? C5S N1S 1.503(13) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? C7S N1S 1.459(12) . ? C7S C8S 1.462(18) . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C8S H8SA 0.9800 . ? C8S H8SB 0.9800 . ? C8S H8SC 0.9800 . ? Co1 N3 2.035(4) 2_665 ? Co1 N3 2.035(4) . ? Co1 N3 2.035(4) 3_565 ? Co1 N1 2.354(9) . ? N1 C1 1.446(5) 3_565 ? N1 C1 1.446(5) 2_665 ? N2 Ni1 2.063(12) . ? N4 C12 1.438(6) 2_665 ? N4 C12 1.438(6) 3_565 ? N4 Ni1 2.390(9) . ? N5 Ni1 2.030(4) . ? Ni1 N5 2.030(4) 2_665 ? Ni1 N5 2.030(4) 3_565 ? 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 C2 C1 C6 120.0(5) . . ? C2 C1 N1 125.6(6) . . ? C6 C1 N1 114.4(6) . . ? C1 C2 C3 120.3(5) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 121.2(6) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 120.8(6) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 118.5(6) . . ? C6 C5 H5A 120.7 . . ? C4 C5 H5A 120.7 . . ? C5 C6 C1 118.2(5) . . ? C5 C6 N3 124.3(4) . . ? C1 C6 N3 117.3(4) . . ? O1 C7 N3 121.5(5) . . ? O1 C7 C8 119.3(5) . . ? N3 C7 C8 119.1(5) . . ? C7 C8 C9 107.4(7) . . ? C7 C8 C10 102.2(7) . . ? C9 C8 C10 120.7(8) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C10 C8 H8A 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 Co1 180.000(4) . . ? C17 C12 C13 119.2(5) . . ? C17 C12 N4 124.9(6) . . ? C13 C12 N4 115.7(6) . . ? C14 C13 C12 118.3(5) . . ? C14 C13 N5 125.3(4) . . ? C12 C13 N5 116.1(4) . . ? C15 C14 C13 119.4(6) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C12 C17 C16 120.3(5) . . ? C12 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? O2 C18 N5 122.3(5) . . ? O2 C18 C19 118.5(5) . . ? N5 C18 C19 119.1(5) . . ? C18 C19 C20 104.9(7) . . ? C18 C19 C21 103.9(7) . . ? C20 C19 C21 124.0(8) . . ? C18 C19 H19A 107.6 . . ? C20 C19 H19A 107.6 . . ? C21 C19 H19A 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1S C1S C2S 107.3(8) . . ? N1S C1S H1SA 110.3 . . ? C2S C1S H1SA 110.3 . . ? N1S C1S H1SB 110.3 . . ? C2S C1S H1SB 110.3 . . ? H1SA C1S H1SB 108.5 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N1S C3S C4S 107.6(8) . . ? N1S C3S H3SA 110.2 . . ? C4S C3S H3SA 110.2 . . ? N1S C3S H3SB 110.2 . . ? C4S C3S H3SB 110.2 . . ? H3SA C3S H3SB 108.5 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? C6S C5S N1S 116.2(10) . . ? C6S C5S H5SA 108.2 . . ? N1S C5S H5SA 108.2 . . ? C6S C5S H5SB 108.2 . . ? N1S C5S H5SB 108.2 . . ? H5SA C5S H5SB 107.4 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? N1S C7S C8S 114.7(9) . . ? N1S C7S H7SA 108.6 . . ? C8S C7S H7SA 108.6 . . ? N1S C7S H7SB 108.6 . . ? C8S C7S H7SB 108.6 . . ? H7SA C7S H7SB 107.6 . . ? C7S C8S H8SA 109.5 . . ? C7S C8S H8SB 109.5 . . ? H8SA C8S H8SB 109.5 . . ? C7S C8S H8SC 109.5 . . ? H8SA C8S H8SC 109.5 . . ? H8SB C8S H8SC 109.5 . . ? C11 Co1 N3 105.59(11) . 2_665 ? C11 Co1 N3 105.59(11) . . ? N3 Co1 N3 113.06(9) 2_665 . ? C11 Co1 N3 105.59(11) . 3_565 ? N3 Co1 N3 113.05(9) 2_665 3_565 ? N3 Co1 N3 113.06(9) . 3_565 ? C11 Co1 N1 180.000(5) . . ? N3 Co1 N1 74.41(11) 2_665 . ? N3 Co1 N1 74.41(11) . . ? N3 Co1 N1 74.41(11) 3_565 . ? C1 N1 C1 116.4(3) 3_565 2_665 ? C1 N1 C1 116.4(3) 3_565 . ? C1 N1 C1 116.4(3) 2_665 . ? C1 N1 Co1 101.1(5) 3_565 . ? C1 N1 Co1 101.1(5) 2_665 . ? C1 N1 Co1 101.1(5) . . ? C11 N2 Ni1 180.000(5) . . ? C7 N3 C6 119.2(4) . . ? C7 N3 Co1 130.9(3) . . ? C6 N3 Co1 109.4(3) . . ? C12 N4 C12 117.1(3) 2_665 . ? C12 N4 C12 117.1(3) 2_665 3_565 ? C12 N4 C12 117.1(3) . 3_565 ? C12 N4 Ni1 99.9(4) 2_665 . ? C12 N4 Ni1 99.9(4) . . ? C12 N4 Ni1 99.9(4) 3_565 . ? C18 N5 C13 118.1(4) . . ? C18 N5 Ni1 130.8(4) . . ? C13 N5 Ni1 110.4(3) . . ? C7S N1S C1S 117.3(11) . . ? C7S N1S C3S 101.3(8) . . ? C1S N1S C3S 113.7(8) . . ? C7S N1S C5S 108.0(7) . . ? C1S N1S C5S 102.7(8) . . ? C3S N1S C5S 114.2(11) . . ? N5 Ni1 N5 112.83(9) . 2_665 ? N5 Ni1 N5 112.83(9) . 3_565 ? N5 Ni1 N5 112.83(9) 2_665 3_565 ? N5 Ni1 N2 105.86(11) . . ? N5 Ni1 N2 105.86(11) 2_665 . ? N5 Ni1 N2 105.86(11) 3_565 . ? N5 Ni1 N4 74.14(11) . . ? N5 Ni1 N4 74.14(11) 2_665 . ? N5 Ni1 N4 74.14(11) 3_565 . ? N2 Ni1 N4 180.000(4) . . ? 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 C6 C1 C2 C3 5.1(9) . . . . ? N1 C1 C2 C3 -177.4(5) . . . . ? C1 C2 C3 C4 2.5(11) . . . . ? C2 C3 C4 C5 -10.1(12) . . . . ? C3 C4 C5 C6 9.9(11) . . . . ? C4 C5 C6 C1 -2.3(8) . . . . ? C4 C5 C6 N3 172.8(6) . . . . ? C2 C1 C6 C5 -5.0(7) . . . . ? N1 C1 C6 C5 177.3(5) . . . . ? C2 C1 C6 N3 179.7(5) . . . . ? N1 C1 C6 N3 1.9(6) . . . . ? O1 C7 C8 C9 61.3(10) . . . . ? N3 C7 C8 C9 -117.8(8) . . . . ? O1 C7 C8 C10 -66.7(10) . . . . ? N3 C7 C8 C10 114.2(8) . . . . ? C17 C12 C13 C14 -6.2(7) . . . . ? N4 C12 C13 C14 177.6(5) . . . . ? C17 C12 C13 N5 179.4(5) . . . . ? N4 C12 C13 N5 3.2(6) . . . . ? C12 C13 C14 C15 -1.7(8) . . . . ? N5 C13 C14 C15 172.1(6) . . . . ? C13 C14 C15 C16 10.0(11) . . . . ? C14 C15 C16 C17 -10.2(12) . . . . ? C13 C12 C17 C16 6.3(8) . . . . ? N4 C12 C17 C16 -177.9(5) . . . . ? C15 C16 C17 C12 1.9(10) . . . . ? O2 C18 C19 C20 65.2(9) . . . . ? N5 C18 C19 C20 -118.0(8) . . . . ? O2 C18 C19 C21 -66.4(10) . . . . ? N5 C18 C19 C21 110.4(8) . . . . ? N2 C11 Co1 N3 167(100) . . . 2_665 ? N2 C11 Co1 N3 47(100) . . . . ? N2 C11 Co1 N3 -73(100) . . . 3_565 ? N2 C11 Co1 N1 0(70) . . . . ? C2 C1 N1 C1 -101.0(7) . . . 3_565 ? C6 C1 N1 C1 76.6(10) . . . 3_565 ? C2 C1 N1 C1 42.1(11) . . . 2_665 ? C6 C1 N1 C1 -140.4(7) . . . 2_665 ? C2 C1 N1 Co1 150.5(5) . . . . ? C6 C1 N1 Co1 -31.9(4) . . . . ? C11 Co1 N1 C1 146(100) . . . 3_565 ? N3 Co1 N1 C1 159.1(2) 2_665 . . 3_565 ? N3 Co1 N1 C1 -80.9(2) . . . 3_565 ? N3 Co1 N1 C1 39.1(2) 3_565 . . 3_565 ? C11 Co1 N1 C1 26(100) . . . 2_665 ? N3 Co1 N1 C1 39.1(2) 2_665 . . 2_665 ? N3 Co1 N1 C1 159.1(2) . . . 2_665 ? N3 Co1 N1 C1 -80.9(2) 3_565 . . 2_665 ? C11 Co1 N1 C1 -94(100) . . . . ? N3 Co1 N1 C1 -80.9(2) 2_665 . . . ? N3 Co1 N1 C1 39.1(2) . . . . ? N3 Co1 N1 C1 159.1(2) 3_565 . . . ? Co1 C11 N2 Ni1 0(100) . . . . ? O1 C7 N3 C6 -5.8(10) . . . . ? C8 C7 N3 C6 173.3(7) . . . . ? O1 C7 N3 Co1 -176.1(5) . . . . ? C8 C7 N3 Co1 3.0(11) . . . . ? C5 C6 N3 C7 48.9(8) . . . . ? C1 C6 N3 C7 -136.0(6) . . . . ? C5 C6 N3 Co1 -138.8(4) . . . . ? C1 C6 N3 Co1 36.2(5) . . . . ? C11 Co1 N3 C7 -48.6(6) . . . . ? N3 Co1 N3 C7 -163.6(5) 2_665 . . . ? N3 Co1 N3 C7 66.3(7) 3_565 . . . ? N1 Co1 N3 C7 131.4(6) . . . . ? C11 Co1 N3 C6 140.3(3) . . . . ? N3 Co1 N3 C6 25.3(4) 2_665 . . . ? N3 Co1 N3 C6 -104.7(2) 3_565 . . . ? N1 Co1 N3 C6 -39.7(3) . . . . ? C17 C12 N4 C12 -101.8(7) . . . 2_665 ? C13 C12 N4 C12 74.1(10) . . . 2_665 ? C17 C12 N4 C12 44.9(10) . . . 3_565 ? C13 C12 N4 C12 -139.1(6) . . . 3_565 ? C17 C12 N4 Ni1 151.5(5) . . . . ? C13 C12 N4 Ni1 -32.5(4) . . . . ? O2 C18 N5 C13 -7.3(10) . . . . ? C19 C18 N5 C13 176.0(7) . . . . ? O2 C18 N5 Ni1 -176.9(5) . . . . ? C19 C18 N5 Ni1 6.4(11) . . . . ? C14 C13 N5 C18 50.6(8) . . . . ? C12 C13 N5 C18 -135.5(5) . . . . ? C14 C13 N5 Ni1 -137.8(4) . . . . ? C12 C13 N5 Ni1 36.1(5) . . . . ? C8S C7S N1S C1S 59.2(16) . . . . ? C8S C7S N1S C3S -176.4(13) . . . . ? C8S C7S N1S C5S -56.1(19) . . . . ? C2S C1S N1S C7S 62.2(12) . . . . ? C2S C1S N1S C3S -55.7(14) . . . . ? C2S C1S N1S C5S -179.6(10) . . . . ? C4S C3S N1S C7S 179.6(10) . . . . ? C4S C3S N1S C1S -53.6(14) . . . . ? C4S C3S N1S C5S 63.8(12) . . . . ? C6S C5S N1S C7S -51(2) . . . . ? C6S C5S N1S C1S -176.0(15) . . . . ? C6S C5S N1S C3S 60.4(17) . . . . ? C18 N5 Ni1 N5 65.5(7) . . . 2_665 ? C13 N5 Ni1 N5 -104.7(3) . . . 2_665 ? C18 N5 Ni1 N5 -165.2(5) . . . 3_565 ? C13 N5 Ni1 N5 24.6(4) . . . 3_565 ? C18 N5 Ni1 N2 -49.8(6) . . . . ? C13 N5 Ni1 N2 140.0(3) . . . . ? C18 N5 Ni1 N4 130.2(6) . . . . ? C13 N5 Ni1 N4 -40.0(3) . . . . ? C11 N2 Ni1 N5 114(62) . . . . ? C11 N2 Ni1 N5 -6(46) . . . 2_665 ? C11 N2 Ni1 N5 -126(43) . . . 3_565 ? C11 N2 Ni1 N4 0(100) . . . . ? C12 N4 Ni1 N5 -80.9(2) 2_665 . . . ? C12 N4 Ni1 N5 39.1(2) . . . . ? C12 N4 Ni1 N5 159.1(2) 3_565 . . . ? C12 N4 Ni1 N5 39.1(2) 2_665 . . 2_665 ? C12 N4 Ni1 N5 159.1(2) . . . 2_665 ? C12 N4 Ni1 N5 -80.9(2) 3_565 . . 2_665 ? C12 N4 Ni1 N5 159.1(2) 2_665 . . 3_565 ? C12 N4 Ni1 N5 -80.9(2) . . . 3_565 ? C12 N4 Ni1 N5 39.1(2) 3_565 . . 3_565 ? C12 N4 Ni1 N2 -147(41) 2_665 . . . ? C12 N4 Ni1 N2 -27(41) . . . . ? C12 N4 Ni1 N2 93(44) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 30.43 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.542 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.069 # Attachment 'laa_02_077Ntosub.cif' data_laa_02_077N _database_code_depnum_ccdc_archive 'CCDC 738759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62.40 H72 N5 Ni O4.60 P' _chemical_formula_sum 'C62.40 H72 N5 Ni O4.60 P' _chemical_formula_weight 1055.33 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' P P 0.1023 0.0942 '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 14.4575(8) _cell_length_b 15.1016(8) _cell_length_c 15.4786(8) _cell_angle_alpha 64.786(3) _cell_angle_beta 72.689(3) _cell_angle_gamma 77.867(3) _cell_volume 2905.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8142 _exptl_absorpt_correction_T_max 0.9295 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42454 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11735 _reflns_number_gt 8875 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0800P)^2^+2.5000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11735 _refine_ls_number_parameters 683 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1633 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.58625(18) 0.9634(2) 0.8018(2) 0.0266(6) Uani 1 1 d . . . C2 C 0.51854(19) 0.9670(2) 0.8858(2) 0.0319(6) Uani 1 1 d . . . H2 H 0.5182 0.9135 0.9474 0.038 Uiso 1 1 calc R . . C3 C 0.45132(19) 1.0488(2) 0.8796(2) 0.0347(7) Uani 1 1 d . . . H3 H 0.4051 1.0522 0.9367 0.042 Uiso 1 1 calc R . . C4 C 0.45267(19) 1.1250(2) 0.7894(2) 0.0352(7) Uani 1 1 d . . . H4 H 0.4070 1.1812 0.7849 0.042 Uiso 1 1 calc R . . C5 C 0.5190(2) 1.1214(2) 0.7052(2) 0.0336(6) Uani 1 1 d . . . H5 H 0.5182 1.1751 0.6440 0.040 Uiso 1 1 calc R . . C6 C 0.58786(18) 1.0393(2) 0.7089(2) 0.0282(6) Uani 1 1 d . . . C7 C 0.6500(2) 1.0772(2) 0.5360(2) 0.0391(7) Uani 1 1 d . . . C8 C 0.7039(2) 1.0330(2) 0.4586(2) 0.0373(7) Uani 1 1 d . . . C9 C 0.6252(3) 1.0254(3) 0.4143(3) 0.0611(11) Uani 1 1 d . . . H9A H 0.6561 1.0033 0.3604 0.092 Uiso 1 1 d R . . H9B H 0.5892 1.0901 0.3892 0.092 Uiso 1 1 d R . . H9C H 0.5803 0.9782 0.4650 0.092 Uiso 1 1 d R . . C10 C 0.7763(3) 1.1039(3) 0.3784(3) 0.0625(11) Uani 1 1 d . . . H10A H 0.8295 1.1044 0.4054 0.094 Uiso 1 1 d R . . H10B H 0.7428 1.1703 0.3551 0.094 Uiso 1 1 d R . . H10C H 0.8028 1.0825 0.3236 0.094 Uiso 1 1 d R . . C11 C 0.7571(2) 0.9316(2) 0.4981(2) 0.0399(7) Uani 1 1 d . . . H11A H 0.7819 0.9064 0.4459 0.060 Uiso 1 1 d R . . H11B H 0.7122 0.8871 0.5528 0.060 Uiso 1 1 d R . . H11C H 0.8117 0.9356 0.5212 0.060 Uiso 1 1 d R . . C12 C 0.70580(18) 0.8559(2) 0.88830(19) 0.0265(6) Uani 1 1 d . . . C13 C 0.67860(19) 0.7811(2) 0.9789(2) 0.0295(6) Uani 1 1 d . . . H13 H 0.6310 0.7404 0.9896 0.035 Uiso 1 1 calc R . . C14 C 0.7209(2) 0.7656(2) 1.0543(2) 0.0322(6) Uani 1 1 d . . . H14 H 0.7043 0.7131 1.1163 0.039 Uiso 1 1 calc R . . C15 C 0.7876(2) 0.8280(2) 1.0373(2) 0.0337(6) Uani 1 1 d . . . H15 H 0.8158 0.8186 1.0891 0.040 Uiso 1 1 calc R . . C16 C 0.81448(19) 0.9036(2) 0.9472(2) 0.0316(6) Uani 1 1 d . . . H16 H 0.8594 0.9461 0.9384 0.038 Uiso 1 1 calc R . . C17 C 0.77583(18) 0.9183(2) 0.86791(19) 0.0263(6) Uani 1 1 d . . . C18 C 0.85485(18) 1.0593(2) 0.7449(2) 0.0281(6) Uani 1 1 d . . . C19 C 0.89473(19) 1.1189(2) 0.6346(2) 0.0316(6) Uani 1 1 d . . . C20 C 0.8183(3) 1.2037(3) 0.6002(3) 0.0630(11) Uani 1 1 d . . . H20A H 0.8062 1.2445 0.6383 0.095 Uiso 1 1 d R . . H20B H 0.7578 1.1775 0.6100 0.095 Uiso 1 1 d R . . H20C H 0.8418 1.2437 0.5304 0.095 Uiso 1 1 d R . . C21 C 0.9184(3) 1.0594(2) 0.5724(2) 0.0471(8) Uani 1 1 d . . . H21A H 0.9570 1.0965 0.5070 0.071 Uiso 1 1 d R . . H21B H 0.8580 1.0456 0.5662 0.071 Uiso 1 1 d R . . H21C H 0.9559 0.9973 0.6033 0.071 Uiso 1 1 d R . . C22 C 0.9883(3) 1.1589(4) 0.6223(3) 0.0727(13) Uani 1 1 d . . . H22A H 1.0378 1.1041 0.6427 0.109 Uiso 1 1 d R . . H22B H 0.9756 1.1973 0.6628 0.109 Uiso 1 1 d R . . H22C H 1.0117 1.2011 0.5531 0.109 Uiso 1 1 d R . . C23 C 0.63121(19) 0.7962(2) 0.79891(19) 0.0281(6) Uani 1 1 d . . . C24 C 0.5412(2) 0.8054(2) 0.7790(2) 0.0376(7) Uani 1 1 d . . . H24 H 0.4975 0.8624 0.7773 0.045 Uiso 1 1 calc R . . C25 C 0.5142(2) 0.7328(3) 0.7617(3) 0.0468(8) Uani 1 1 d . . . H25 H 0.4530 0.7407 0.7470 0.056 Uiso 1 1 calc R . . C26 C 0.5763(3) 0.6494(3) 0.7660(3) 0.0473(8) Uani 1 1 d . . . H26 H 0.5578 0.5987 0.7554 0.057 Uiso 1 1 calc R . . C27 C 0.6660(2) 0.6398(2) 0.7857(2) 0.0394(7) Uani 1 1 d . . . H27 H 0.7079 0.5814 0.7893 0.047 Uiso 1 1 calc R . . C28 C 0.69740(19) 0.7127(2) 0.80036(19) 0.0294(6) Uani 1 1 d . . . C29 C 0.86093(19) 0.7426(2) 0.76645(19) 0.0284(6) Uani 1 1 d . . . C30 C 0.96205(19) 0.7058(2) 0.7883(2) 0.0325(6) Uani 1 1 d . . . C31 C 1.0032(2) 0.7889(3) 0.7930(3) 0.0539(9) Uani 1 1 d . . . H31A H 0.9620 0.8056 0.8480 0.081 Uiso 1 1 d R . . H31B H 1.0042 0.8468 0.7315 0.081 Uiso 1 1 d R . . H31C H 1.0695 0.7673 0.8026 0.081 Uiso 1 1 d R . . C32 C 0.9594(2) 0.6178(3) 0.8850(2) 0.0459(8) Uani 1 1 d . . . H32A H 0.9176 0.6360 0.9388 0.069 Uiso 1 1 d R . . H32B H 1.0254 0.5966 0.8956 0.069 Uiso 1 1 d R . . H32C H 0.9335 0.5638 0.8831 0.069 Uiso 1 1 d R . . C33 C 1.0276(3) 0.6782(3) 0.7040(3) 0.0579(10) Uani 1 1 d . . . H33A H 1.0937 0.6572 0.7145 0.087 Uiso 1 1 d R . . H33B H 1.0292 0.7353 0.6417 0.087 Uiso 1 1 d R . . H33C H 1.0020 0.6242 0.7017 0.087 Uiso 1 1 d R . . C34 C 0.76759(18) 0.3509(2) 1.0442(2) 0.0285(6) Uani 1 1 d . . . C35 C 0.7440(2) 0.3092(2) 1.1464(2) 0.0332(6) Uani 1 1 d . . . H35 H 0.7454 0.2399 1.1803 0.040 Uiso 1 1 calc R . . C36 C 0.7183(2) 0.3696(2) 1.1986(2) 0.0398(7) Uani 1 1 d . . . H36 H 0.7020 0.3413 1.2684 0.048 Uiso 1 1 calc R . . C37 C 0.7163(2) 0.4705(2) 1.1497(2) 0.0406(7) Uani 1 1 d . . . H37 H 0.6986 0.5114 1.1859 0.049 Uiso 1 1 calc R . . C38 C 0.7400(2) 0.5120(2) 1.0478(2) 0.0374(7) Uani 1 1 d . . . H38 H 0.7383 0.5815 1.0143 0.045 Uiso 1 1 calc R . . C39 C 0.7661(2) 0.4531(2) 0.9954(2) 0.0344(6) Uani 1 1 d . . . H39 H 0.7833 0.4819 0.9256 0.041 Uiso 1 1 calc R . . C40 C 0.91210(19) 0.3126(2) 0.8854(2) 0.0317(6) Uani 1 1 d . . . C41 C 0.9756(2) 0.3546(2) 0.9057(2) 0.0368(7) Uani 1 1 d . . . H41 H 0.9582 0.3657 0.9647 0.044 Uiso 1 1 calc R . . C42 C 1.0640(2) 0.3804(2) 0.8402(3) 0.0442(8) Uani 1 1 d . . . H42 H 1.1067 0.4098 0.8542 0.053 Uiso 1 1 calc R . . C43 C 1.0900(2) 0.3638(3) 0.7557(3) 0.0508(9) Uani 1 1 d . . . H43 H 1.1501 0.3829 0.7103 0.061 Uiso 1 1 calc R . . C44 C 1.0292(3) 0.3194(3) 0.7365(3) 0.0626(11) Uani 1 1 d . . . H44 H 1.0484 0.3063 0.6785 0.075 Uiso 1 1 calc R . . C45 C 0.9394(3) 0.2935(3) 0.8014(3) 0.0520(9) Uani 1 1 d . . . H45 H 0.8975 0.2629 0.7877 0.062 Uiso 1 1 calc R . . C46 C 0.81839(19) 0.1488(2) 1.0528(2) 0.0296(6) Uani 1 1 d . . . C47 C 0.9115(2) 0.1062(2) 1.0644(2) 0.0391(7) Uani 1 1 d . . . H47 H 0.9658 0.1435 1.0288 0.047 Uiso 1 1 calc R . . C48 C 0.9246(2) 0.0091(2) 1.1282(3) 0.0467(8) Uani 1 1 d . . . H48 H 0.9880 -0.0204 1.1360 0.056 Uiso 1 1 calc R . . C49 C 0.8454(2) -0.0447(2) 1.1802(2) 0.0438(8) Uani 1 1 d . . . H49 H 0.8546 -0.1111 1.2242 0.053 Uiso 1 1 calc R . . C50 C 0.7534(2) -0.0029(2) 1.1689(2) 0.0405(7) Uani 1 1 d . . . H50 H 0.6994 -0.0405 1.2051 0.049 Uiso 1 1 calc R . . C51 C 0.7390(2) 0.0936(2) 1.1052(2) 0.0354(7) Uani 1 1 d . . . H51 H 0.6754 0.1221 1.0972 0.042 Uiso 1 1 calc R . . C52 C 0.70167(19) 0.2886(2) 0.9189(2) 0.0326(6) Uani 1 1 d . . . C53 C 0.7023(2) 0.2210(3) 0.8787(2) 0.0416(7) Uani 1 1 d . . . H53 H 0.7535 0.1696 0.8809 0.050 Uiso 1 1 calc R . . C54 C 0.6276(2) 0.2299(3) 0.8357(3) 0.0492(8) Uani 1 1 d . . . H54 H 0.6278 0.1848 0.8077 0.059 Uiso 1 1 calc R . . C55 C 0.5532(2) 0.3037(3) 0.8334(3) 0.0504(9) Uani 1 1 d . . . H55 H 0.5025 0.3096 0.8034 0.061 Uiso 1 1 calc R . . C56 C 0.5515(2) 0.3692(3) 0.8743(3) 0.0504(9) Uani 1 1 d . . . H56 H 0.4993 0.4195 0.8732 0.060 Uiso 1 1 calc R . . C57 C 0.6261(2) 0.3620(2) 0.9172(3) 0.0421(7) Uani 1 1 d . . . H57 H 0.6251 0.4074 0.9453 0.050 Uiso 1 1 calc R . . C1S C 0.6449(3) 0.5256(3) 0.3813(3) 0.0519(9) Uani 1 1 d . . . H1S H 0.6912 0.5342 0.4090 0.062 Uiso 1 1 calc R . . C2S C 0.5263(3) 0.4244(3) 0.3971(3) 0.0672(11) Uani 1 1 d . . . H2S1 H 0.4620 0.4304 0.4398 0.101 Uiso 1 1 d R . . H2S2 H 0.5410 0.3575 0.3985 0.101 Uiso 1 1 d R . . H2S3 H 0.5267 0.4715 0.3297 0.101 Uiso 1 1 d R . . C3S C 0.6144(3) 0.3744(3) 0.5272(4) 0.0767(13) Uani 1 1 d . . . H3S1 H 0.6644 0.3951 0.5437 0.115 Uiso 1 1 d R . . H3S2 H 0.6356 0.3092 0.5249 0.115 Uiso 1 1 d R . . H3S3 H 0.5534 0.3714 0.5774 0.115 Uiso 1 1 d R . . C4S C 0.6829(4) 0.7486(3) 0.4160(4) 0.0450(14) Uani 0.60 1 d P B . H4S1 H 0.7321 0.7799 0.3565 0.067 Uiso 0.60 1 calc PR . . H4S2 H 0.6365 0.7993 0.4334 0.067 Uiso 0.60 1 calc PR . . H4S3 H 0.6482 0.7071 0.4042 0.067 Uiso 0.60 1 calc PR . . C5S C 0.7304(4) 0.6879(4) 0.4968(5) 0.0493(15) Uani 0.60 1 d PD . . H5S1 H 0.7840 0.7224 0.4920 0.059 Uiso 0.60 1 calc PR A 1 H5S2 H 0.6826 0.6806 0.5598 0.059 Uiso 0.60 1 calc PR A 1 O2SA O 0.7649(5) 0.6022(5) 0.4978(5) 0.0271(10) Uiso 0.30 1 d PD B 1 C6SA C 0.8414(10) 0.5530(11) 0.5493(11) 0.060(3) Uiso 0.30 1 d PD B 1 H6S1 H 0.9019 0.5390 0.5043 0.072 Uiso 0.30 1 calc PR B 1 H6S2 H 0.8552 0.5935 0.5794 0.072 Uiso 0.30 1 calc PR B 1 C7SA C 0.805(2) 0.4677(17) 0.6199(18) 0.141(6) Uiso 0.30 1 d PD B 1 H7S1 H 0.7356 0.4812 0.6472 0.211 Uiso 0.30 1 calc PR B 1 H7S2 H 0.8400 0.4413 0.6724 0.211 Uiso 0.30 1 calc PR B 1 H7S3 H 0.8131 0.4196 0.5906 0.211 Uiso 0.30 1 calc PR B 1 O2SB O 0.7928(5) 0.6075(5) 0.4773(5) 0.0271(10) Uiso 0.30 1 d PD B 2 C6SB C 0.8126(11) 0.5426(11) 0.5743(10) 0.060(3) Uiso 0.30 1 d PD B 2 H6S3 H 0.7523 0.5237 0.6263 0.072 Uiso 0.30 1 calc PR B 2 H6S4 H 0.8541 0.5712 0.5946 0.072 Uiso 0.30 1 calc PR B 2 C7SB C 0.8654(19) 0.4606(17) 0.545(2) 0.141(6) Uiso 0.30 1 d PD B 2 H7S4 H 0.8183 0.4212 0.5470 0.211 Uiso 0.30 1 calc PR B 2 H7S5 H 0.9065 0.4191 0.5908 0.211 Uiso 0.30 1 calc PR B 2 H7S6 H 0.9062 0.4872 0.4784 0.211 Uiso 0.30 1 calc PR B 2 N1 N 0.65978(15) 0.87849(16) 0.80823(16) 0.0251(5) Uani 1 1 d . . . N2 N 0.65673(16) 1.02320(17) 0.63027(16) 0.0291(5) Uani 1 1 d . . . N3 N 0.80515(15) 0.98286(17) 0.76914(16) 0.0272(5) Uani 1 1 d . . . N4 N 0.78977(16) 0.69005(17) 0.82215(17) 0.0297(5) Uani 1 1 d . . . N1S N 0.5987(2) 0.4450(2) 0.4318(2) 0.0496(7) Uani 1 1 d . . . Ni1 Ni 0.76573(2) 0.93475(3) 0.68382(2) 0.02630(12) Uani 1 1 d . . . O1 O 0.6019(2) 1.15730(19) 0.50719(18) 0.0697(9) Uani 1 1 d . . . O2 O 0.86940(14) 1.08784(15) 0.80440(15) 0.0369(5) Uani 1 1 d . . . O3 O 0.85899(13) 0.82296(14) 0.68813(14) 0.0330(4) Uani 1 1 d . . . O1S O 0.6339(2) 0.5896(2) 0.30299(19) 0.0665(8) Uani 1 1 d . . . P1 P 0.79965(5) 0.27534(5) 0.97449(5) 0.02762(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 C1 0.0209(12) 0.0291(14) 0.0334(14) -0.0146(12) -0.0088(10) -0.0010(10) C2 0.0251(13) 0.0404(17) 0.0321(15) -0.0148(13) -0.0086(11) -0.0027(12) C3 0.0222(13) 0.0474(18) 0.0412(16) -0.0256(15) -0.0079(12) 0.0017(12) C4 0.0241(13) 0.0375(17) 0.0511(18) -0.0240(15) -0.0135(12) 0.0042(12) C5 0.0305(14) 0.0309(15) 0.0399(16) -0.0123(13) -0.0142(12) 0.0011(12) C6 0.0239(12) 0.0315(15) 0.0335(14) -0.0150(12) -0.0102(11) -0.0011(11) C7 0.0455(17) 0.0336(17) 0.0351(16) -0.0117(14) -0.0137(13) 0.0047(13) C8 0.0434(16) 0.0358(17) 0.0286(15) -0.0099(13) -0.0105(13) 0.0017(13) C9 0.057(2) 0.081(3) 0.063(2) -0.044(2) -0.0314(19) 0.019(2) C10 0.088(3) 0.051(2) 0.0351(19) -0.0074(17) -0.0011(18) -0.017(2) C11 0.0458(17) 0.0389(18) 0.0343(16) -0.0173(14) -0.0095(13) 0.0044(14) C12 0.0240(12) 0.0303(15) 0.0255(13) -0.0124(11) -0.0074(10) 0.0025(11) C13 0.0285(13) 0.0276(14) 0.0309(14) -0.0118(12) -0.0057(11) -0.0009(11) C14 0.0361(14) 0.0286(15) 0.0276(14) -0.0100(12) -0.0086(11) 0.0049(12) C15 0.0340(14) 0.0379(17) 0.0329(15) -0.0176(13) -0.0160(12) 0.0090(12) C16 0.0256(13) 0.0350(16) 0.0379(16) -0.0165(13) -0.0119(11) 0.0011(11) C17 0.0211(12) 0.0263(14) 0.0302(14) -0.0115(11) -0.0078(10) 0.0036(10) C18 0.0212(12) 0.0266(14) 0.0386(15) -0.0152(12) -0.0098(11) 0.0032(10) C19 0.0271(13) 0.0278(15) 0.0375(15) -0.0120(12) -0.0033(11) -0.0054(11) C20 0.065(2) 0.041(2) 0.048(2) -0.0022(17) -0.0008(18) 0.0147(18) C21 0.063(2) 0.0385(19) 0.0357(17) -0.0142(15) 0.0011(15) -0.0143(16) C22 0.057(2) 0.115(4) 0.058(2) -0.043(3) 0.0121(19) -0.051(3) C23 0.0274(13) 0.0310(15) 0.0250(13) -0.0086(11) -0.0036(10) -0.0096(11) C24 0.0282(14) 0.0394(17) 0.0457(18) -0.0148(14) -0.0109(13) -0.0050(12) C25 0.0390(17) 0.047(2) 0.064(2) -0.0196(17) -0.0243(16) -0.0102(15) C26 0.054(2) 0.0399(19) 0.060(2) -0.0190(17) -0.0254(17) -0.0126(16) C27 0.0467(17) 0.0305(16) 0.0454(18) -0.0128(14) -0.0191(14) -0.0050(13) C28 0.0319(14) 0.0290(15) 0.0267(14) -0.0085(12) -0.0079(11) -0.0056(11) C29 0.0300(13) 0.0254(14) 0.0282(14) -0.0101(12) -0.0080(11) 0.0010(11) C30 0.0263(13) 0.0306(15) 0.0383(16) -0.0126(13) -0.0072(11) -0.0002(11) C31 0.0316(16) 0.0411(19) 0.092(3) -0.0238(19) -0.0234(17) -0.0007(14) C32 0.0365(16) 0.046(2) 0.0486(19) -0.0058(16) -0.0212(14) -0.0034(14) C33 0.0447(19) 0.071(3) 0.052(2) -0.030(2) -0.0139(16) 0.0242(18) C34 0.0235(12) 0.0292(15) 0.0338(15) -0.0127(12) -0.0085(11) -0.0007(11) C35 0.0345(14) 0.0301(15) 0.0345(15) -0.0111(13) -0.0098(12) -0.0025(12) C36 0.0430(17) 0.0434(19) 0.0336(16) -0.0163(14) -0.0091(13) -0.0022(14) C37 0.0369(16) 0.0403(18) 0.0514(19) -0.0268(16) -0.0091(14) 0.0004(13) C38 0.0359(15) 0.0309(16) 0.0463(18) -0.0158(14) -0.0105(13) -0.0022(12) C39 0.0316(14) 0.0345(16) 0.0346(15) -0.0103(13) -0.0097(12) -0.0026(12) C40 0.0270(13) 0.0279(15) 0.0365(15) -0.0094(12) -0.0067(11) -0.0032(11) C41 0.0287(14) 0.0391(17) 0.0446(17) -0.0170(14) -0.0111(12) -0.0021(12) C42 0.0314(15) 0.0407(18) 0.061(2) -0.0181(16) -0.0111(14) -0.0067(13) C43 0.0395(17) 0.047(2) 0.058(2) -0.0208(18) 0.0062(15) -0.0136(15) C44 0.057(2) 0.082(3) 0.054(2) -0.039(2) 0.0127(18) -0.028(2) C45 0.0510(19) 0.066(2) 0.049(2) -0.0317(19) 0.0039(16) -0.0260(18) C46 0.0281(13) 0.0308(15) 0.0339(15) -0.0145(12) -0.0097(11) -0.0031(11) C47 0.0292(14) 0.0354(17) 0.0502(18) -0.0107(14) -0.0133(13) -0.0051(12) C48 0.0364(16) 0.0370(18) 0.061(2) -0.0096(16) -0.0215(15) 0.0010(14) C49 0.0534(19) 0.0304(17) 0.0493(19) -0.0078(15) -0.0246(16) -0.0062(14) C50 0.0434(17) 0.0383(18) 0.0417(17) -0.0094(14) -0.0131(14) -0.0170(14) C51 0.0297(14) 0.0382(17) 0.0395(16) -0.0132(14) -0.0110(12) -0.0056(12) C52 0.0260(13) 0.0376(16) 0.0347(15) -0.0120(13) -0.0101(11) -0.0046(12) C53 0.0318(15) 0.055(2) 0.0464(18) -0.0284(16) -0.0088(13) -0.0027(14) C54 0.0423(18) 0.070(2) 0.0460(19) -0.0286(18) -0.0095(15) -0.0153(17) C55 0.0374(17) 0.062(2) 0.052(2) -0.0096(18) -0.0221(15) -0.0152(16) C56 0.0345(16) 0.0419(19) 0.073(2) -0.0137(18) -0.0251(16) -0.0008(14) C57 0.0334(15) 0.0381(18) 0.059(2) -0.0191(16) -0.0186(14) -0.0013(13) C1S 0.054(2) 0.051(2) 0.055(2) -0.0261(19) -0.0071(17) -0.0089(17) C2S 0.056(2) 0.076(3) 0.082(3) -0.045(2) -0.004(2) -0.018(2) C3S 0.079(3) 0.045(2) 0.086(3) -0.004(2) -0.029(3) 0.002(2) C4S 0.050(3) 0.015(2) 0.074(4) -0.009(2) -0.033(3) -0.003(2) C5S 0.048(3) 0.061(4) 0.065(4) -0.045(3) -0.032(3) 0.015(3) N1 0.0222(10) 0.0265(12) 0.0266(11) -0.0094(9) -0.0075(9) -0.0016(9) N2 0.0285(11) 0.0289(12) 0.0279(12) -0.0102(10) -0.0071(9) -0.0001(9) N3 0.0222(10) 0.0287(12) 0.0298(12) -0.0107(10) -0.0068(9) -0.0013(9) N4 0.0293(11) 0.0276(12) 0.0333(12) -0.0116(10) -0.0108(10) -0.0006(9) N1S 0.0500(16) 0.0407(16) 0.0581(18) -0.0182(14) -0.0126(14) -0.0065(13) Ni1 0.02402(18) 0.0269(2) 0.02627(19) -0.00923(15) -0.00583(13) -0.00150(13) O1 0.108(2) 0.0474(15) 0.0400(14) -0.0151(12) -0.0309(14) 0.0365(15) O2 0.0398(11) 0.0346(11) 0.0428(12) -0.0184(10) -0.0138(9) -0.0038(9) O3 0.0301(10) 0.0299(11) 0.0307(10) -0.0077(9) -0.0046(8) 0.0015(8) O1S 0.095(2) 0.0579(17) 0.0428(15) -0.0152(13) -0.0086(14) -0.0202(15) P1 0.0229(3) 0.0290(4) 0.0320(4) -0.0120(3) -0.0083(3) -0.0017(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 C1 C2 1.390(4) . ? C1 C6 1.404(4) . ? C1 N1 1.472(3) . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.409(4) . ? C5 H5 0.9500 . ? C6 N2 1.400(3) . ? C7 O1 1.232(4) . ? C7 N2 1.357(4) . ? C7 C8 1.548(4) . ? C8 C11 1.516(4) . ? C8 C10 1.533(5) . ? C8 C9 1.536(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.381(4) . ? C12 C17 1.404(4) . ? C12 N1 1.460(3) . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C17 1.410(4) . ? C16 H16 0.9500 . ? C17 N3 1.409(3) . ? C18 O2 1.252(3) . ? C18 N3 1.346(3) . ? C18 C19 1.543(4) . ? C19 C21 1.505(4) . ? C19 C20 1.522(4) . ? C19 C22 1.524(4) . ? C20 H20A 0.9799 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9799 . ? C22 H22B 0.9801 . ? C22 H22C 0.9800 . ? C23 C24 1.391(4) . ? C23 C28 1.410(4) . ? C23 N1 1.463(3) . ? C24 C25 1.384(4) . ? C24 H24 0.9500 . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C26 C27 1.384(4) . ? C26 H26 0.9500 . ? C27 C28 1.399(4) . ? C27 H27 0.9500 . ? C28 N4 1.411(3) . ? C29 N4 1.290(4) . ? C29 O3 1.302(3) . ? C29 C30 1.534(4) . ? C30 C32 1.517(4) . ? C30 C33 1.529(4) . ? C30 C31 1.533(4) . ? C31 H31A 0.9801 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9801 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.391(4) . ? C34 C39 1.399(4) . ? C34 P1 1.792(3) . ? C35 C36 1.389(4) . ? C35 H35 0.9500 . ? C36 C37 1.381(5) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 H37 0.9500 . ? C38 C39 1.373(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.378(4) . ? C40 C41 1.388(4) . ? C40 P1 1.803(3) . ? C41 C42 1.383(4) . ? C41 H41 0.9500 . ? C42 C43 1.365(5) . ? C42 H42 0.9500 . ? C43 C44 1.372(5) . ? C43 H43 0.9500 . ? C44 C45 1.396(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.392(4) . ? C46 C51 1.393(4) . ? C46 P1 1.789(3) . ? C47 C48 1.386(4) . ? C47 H47 0.9500 . ? C48 C49 1.379(5) . ? C48 H48 0.9500 . ? C49 C50 1.375(4) . ? C49 H49 0.9500 . ? C50 C51 1.381(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.381(4) . ? C52 C53 1.401(4) . ? C52 P1 1.802(3) . ? C53 C54 1.385(4) . ? C53 H53 0.9500 . ? C54 C55 1.373(5) . ? C54 H54 0.9500 . ? C55 C56 1.376(5) . ? C55 H55 0.9500 . ? C56 C57 1.389(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C1S O1S 1.216(4) . ? C1S N1S 1.327(5) . ? C1S H1S 0.9500 . ? C2S N1S 1.447(5) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S N1S 1.458(5) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S C5S 1.464(7) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C5S O2SA 1.280(8) . ? C5S O2SB 1.438(8) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? O2SA C6SA 1.443(13) . ? C6SA C7SA 1.369(17) . ? C6SA H6S1 0.9900 . ? C6SA H6S2 0.9900 . ? C7SA H7S1 0.9800 . ? C7SA H7S2 0.9800 . ? C7SA H7S3 0.9800 . ? O2SB C6SB 1.477(13) . ? C6SB C7SB 1.481(17) . ? C6SB H6S3 0.9900 . ? C6SB H6S4 0.9900 . ? C7SB H7S4 0.9800 . ? C7SB H7S5 0.9800 . ? C7SB H7S6 0.9800 . ? N1 Ni1 2.043(2) . ? N2 Ni1 1.976(2) . ? N3 Ni1 2.009(2) . ? Ni1 O3 1.9167(19) . ? 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 C2 C1 C6 122.1(2) . . ? C2 C1 N1 120.2(2) . . ? C6 C1 N1 117.6(2) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 119.0(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 121.0(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N2 C6 C1 115.8(2) . . ? N2 C6 C5 127.7(3) . . ? C1 C6 C5 116.5(2) . . ? O1 C7 N2 125.4(3) . . ? O1 C7 C8 117.0(3) . . ? N2 C7 C8 117.5(2) . . ? C11 C8 C10 109.2(3) . . ? C11 C8 C9 108.0(3) . . ? C10 C8 C9 109.6(3) . . ? C11 C8 C7 115.4(2) . . ? C10 C8 C7 108.6(3) . . ? C9 C8 C7 105.9(3) . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.7 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.6 . . ? C8 C10 H10B 109.4 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.4 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.4 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 122.8(2) . . ? C13 C12 N1 121.9(2) . . ? C17 C12 N1 115.3(2) . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 121.8(3) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 N3 116.3(2) . . ? C12 C17 C16 116.1(2) . . ? N3 C17 C16 127.4(2) . . ? O2 C18 N3 125.4(3) . . ? O2 C18 C19 117.1(2) . . ? N3 C18 C19 117.4(2) . . ? C21 C19 C20 109.8(3) . . ? C21 C19 C22 107.5(3) . . ? C20 C19 C22 109.8(3) . . ? C21 C19 C18 113.8(2) . . ? C20 C19 C18 107.4(2) . . ? C22 C19 C18 108.5(3) . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.6 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.4 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.6 . . ? C19 C22 H22B 109.6 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.2 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 120.1(3) . . ? C24 C23 N1 119.0(3) . . ? C28 C23 N1 120.6(2) . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 119.4(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 122.6(3) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 116.9(3) . . ? C27 C28 N4 115.3(3) . . ? C23 C28 N4 127.6(2) . . ? N4 C29 O3 127.3(2) . . ? N4 C29 C30 118.4(2) . . ? O3 C29 C30 114.1(2) . . ? C32 C30 C33 109.8(3) . . ? C32 C30 C31 108.4(3) . . ? C33 C30 C31 109.4(3) . . ? C32 C30 C29 112.4(2) . . ? C33 C30 C29 107.7(2) . . ? C31 C30 C29 109.1(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.4 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.4 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 119.5(3) . . ? C35 C34 P1 120.8(2) . . ? C39 C34 P1 119.6(2) . . ? C36 C35 C34 119.6(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C37 C36 C35 120.4(3) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C34 120.3(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C45 C40 C41 119.4(3) . . ? C45 C40 P1 121.2(2) . . ? C41 C40 P1 119.2(2) . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.3(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C45 120.6(3) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C40 C45 C44 119.4(3) . . ? C40 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C51 119.8(3) . . ? C47 C46 P1 120.3(2) . . ? C51 C46 P1 119.8(2) . . ? C48 C47 C46 119.7(3) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C49 C48 C47 120.0(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 120.4(3) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 120.4(3) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C46 119.6(3) . . ? C50 C51 H51 120.2 . . ? C46 C51 H51 120.2 . . ? C57 C52 C53 120.1(3) . . ? C57 C52 P1 121.4(2) . . ? C53 C52 P1 118.5(2) . . ? C54 C53 C52 119.3(3) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 120.2(3) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C55 C56 C57 120.2(3) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C52 C57 C56 119.6(3) . . ? C52 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? O1S C1S N1S 126.4(4) . . ? O1S C1S H1S 116.8 . . ? N1S C1S H1S 116.8 . . ? N1S C2S H2S1 109.2 . . ? N1S C2S H2S2 109.6 . . ? H2S1 C2S H2S2 109.5 . . ? N1S C2S H2S3 109.7 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1S C3S H3S1 109.4 . . ? N1S C3S H3S2 109.6 . . ? H3S1 C3S H3S2 109.5 . . ? N1S C3S H3S3 109.4 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C5S C4S H4S1 109.5 . . ? C5S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C5S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O2SA C5S O2SB 17.0(4) . . ? O2SA C5S C4S 113.9(5) . . ? O2SB C5S C4S 110.9(5) . . ? O2SA C5S H5S1 108.8 . . ? O2SB C5S H5S1 95.2 . . ? C4S C5S H5S1 108.8 . . ? O2SA C5S H5S2 108.8 . . ? O2SB C5S H5S2 123.9 . . ? C4S C5S H5S2 108.8 . . ? H5S1 C5S H5S2 107.7 . . ? C5S O2SA C6SA 116.5(8) . . ? C7SA C6SA O2SA 104.0(15) . . ? C7SA C6SA H6S1 110.9 . . ? O2SA C6SA H6S1 110.9 . . ? C7SA C6SA H6S2 110.9 . . ? O2SA C6SA H6S2 110.9 . . ? H6S1 C6SA H6S2 109.0 . . ? C5S O2SB C6SB 102.6(7) . . ? O2SB C6SB C7SB 95.8(14) . . ? O2SB C6SB H6S3 112.6 . . ? C7SB C6SB H6S3 112.6 . . ? O2SB C6SB H6S4 112.6 . . ? C7SB C6SB H6S4 112.6 . . ? H6S3 C6SB H6S4 110.1 . . ? C6SB C7SB H7S4 109.5 . . ? C6SB C7SB H7S5 109.5 . . ? H7S4 C7SB H7S5 109.5 . . ? C6SB C7SB H7S6 109.5 . . ? H7S4 C7SB H7S6 109.5 . . ? H7S5 C7SB H7S6 109.5 . . ? C12 N1 C23 117.6(2) . . ? C12 N1 C1 109.9(2) . . ? C23 N1 C1 116.0(2) . . ? C12 N1 Ni1 104.30(15) . . ? C23 N1 Ni1 104.46(15) . . ? C1 N1 Ni1 102.45(15) . . ? C7 N2 C6 121.3(2) . . ? C7 N2 Ni1 130.58(19) . . ? C6 N2 Ni1 106.96(16) . . ? C18 N3 C17 120.8(2) . . ? C18 N3 Ni1 130.46(19) . . ? C17 N3 Ni1 108.65(17) . . ? C29 N4 C28 121.8(2) . . ? C1S N1S C2S 121.6(3) . . ? C1S N1S C3S 122.2(3) . . ? C2S N1S C3S 116.1(3) . . ? O3 Ni1 N2 148.45(9) . . ? O3 Ni1 N3 101.30(9) . . ? N2 Ni1 N3 110.16(9) . . ? O3 Ni1 N1 102.78(8) . . ? N2 Ni1 N1 84.25(9) . . ? N3 Ni1 N1 82.16(9) . . ? C29 O3 Ni1 123.96(17) . . ? C46 P1 C34 110.37(13) . . ? C46 P1 C52 108.20(13) . . ? C34 P1 C52 109.27(13) . . ? C46 P1 C40 108.81(13) . . ? C34 P1 C40 107.33(13) . . ? C52 P1 C40 112.87(13) . . ? 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 C6 C1 C2 C3 -1.8(4) . . . . ? N1 C1 C2 C3 178.0(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C2 C1 C6 N2 -176.6(2) . . . . ? N1 C1 C6 N2 3.6(3) . . . . ? C2 C1 C6 C5 2.0(4) . . . . ? N1 C1 C6 C5 -177.8(2) . . . . ? C4 C5 C6 N2 177.4(3) . . . . ? C4 C5 C6 C1 -1.1(4) . . . . ? O1 C7 C8 C11 -176.4(3) . . . . ? N2 C7 C8 C11 1.2(4) . . . . ? O1 C7 C8 C10 60.7(4) . . . . ? N2 C7 C8 C10 -121.7(3) . . . . ? O1 C7 C8 C9 -57.0(4) . . . . ? N2 C7 C8 C9 120.6(3) . . . . ? C17 C12 C13 C14 0.2(4) . . . . ? N1 C12 C13 C14 -176.7(2) . . . . ? C12 C13 C14 C15 2.0(4) . . . . ? C13 C14 C15 C16 -1.3(4) . . . . ? C14 C15 C16 C17 -1.5(4) . . . . ? C13 C12 C17 N3 172.1(2) . . . . ? N1 C12 C17 N3 -10.8(3) . . . . ? C13 C12 C17 C16 -2.9(4) . . . . ? N1 C12 C17 C16 174.2(2) . . . . ? C15 C16 C17 C12 3.5(4) . . . . ? C15 C16 C17 N3 -170.9(3) . . . . ? O2 C18 C19 C21 152.3(3) . . . . ? N3 C18 C19 C21 -29.4(3) . . . . ? O2 C18 C19 C20 -85.9(3) . . . . ? N3 C18 C19 C20 92.4(3) . . . . ? O2 C18 C19 C22 32.8(4) . . . . ? N3 C18 C19 C22 -149.0(3) . . . . ? C28 C23 C24 C25 0.9(4) . . . . ? N1 C23 C24 C25 174.8(3) . . . . ? C23 C24 C25 C26 1.2(5) . . . . ? C24 C25 C26 C27 -1.2(5) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C23 2.9(5) . . . . ? C26 C27 C28 N4 178.5(3) . . . . ? C24 C23 C28 C27 -2.9(4) . . . . ? N1 C23 C28 C27 -176.6(2) . . . . ? C24 C23 C28 N4 -177.8(3) . . . . ? N1 C23 C28 N4 8.5(4) . . . . ? N4 C29 C30 C32 -9.0(4) . . . . ? O3 C29 C30 C32 174.6(3) . . . . ? N4 C29 C30 C33 112.0(3) . . . . ? O3 C29 C30 C33 -64.3(3) . . . . ? N4 C29 C30 C31 -129.3(3) . . . . ? O3 C29 C30 C31 54.4(3) . . . . ? C39 C34 C35 C36 0.7(4) . . . . ? P1 C34 C35 C36 -179.3(2) . . . . ? C34 C35 C36 C37 -0.1(4) . . . . ? C35 C36 C37 C38 0.0(5) . . . . ? C36 C37 C38 C39 -0.4(4) . . . . ? C37 C38 C39 C34 0.9(4) . . . . ? C35 C34 C39 C38 -1.1(4) . . . . ? P1 C34 C39 C38 178.8(2) . . . . ? C45 C40 C41 C42 2.4(5) . . . . ? P1 C40 C41 C42 177.5(2) . . . . ? C40 C41 C42 C43 -0.7(5) . . . . ? C41 C42 C43 C44 -1.4(6) . . . . ? C42 C43 C44 C45 1.8(6) . . . . ? C41 C40 C45 C44 -2.0(5) . . . . ? P1 C40 C45 C44 -177.0(3) . . . . ? C43 C44 C45 C40 -0.1(6) . . . . ? C51 C46 C47 C48 -0.1(5) . . . . ? P1 C46 C47 C48 177.6(3) . . . . ? C46 C47 C48 C49 -0.4(5) . . . . ? C47 C48 C49 C50 0.4(5) . . . . ? C48 C49 C50 C51 0.0(5) . . . . ? C49 C50 C51 C46 -0.5(5) . . . . ? C47 C46 C51 C50 0.6(4) . . . . ? P1 C46 C51 C50 -177.2(2) . . . . ? C57 C52 C53 C54 1.3(5) . . . . ? P1 C52 C53 C54 180.0(3) . . . . ? C52 C53 C54 C55 -0.6(5) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? C54 C55 C56 C57 0.9(5) . . . . ? C53 C52 C57 C56 -0.9(5) . . . . ? P1 C52 C57 C56 -179.5(3) . . . . ? C55 C56 C57 C52 -0.2(5) . . . . ? O2SB C5S O2SA C6SA 74.4(18) . . . . ? C4S C5S O2SA C6SA 157.8(8) . . . . ? C5S O2SA C6SA C7SA 121.2(16) . . . . ? O2SA C5S O2SB C6SB -62.4(18) . . . . ? C4S C5S O2SB C6SB -165.9(8) . . . . ? C5S O2SB C6SB C7SB 173.4(13) . . . . ? C13 C12 N1 C23 -35.9(3) . . . . ? C17 C12 N1 C23 147.0(2) . . . . ? C13 C12 N1 C1 99.8(3) . . . . ? C17 C12 N1 C1 -77.4(3) . . . . ? C13 C12 N1 Ni1 -151.0(2) . . . . ? C17 C12 N1 Ni1 31.8(2) . . . . ? C24 C23 N1 C12 136.9(3) . . . . ? C28 C23 N1 C12 -49.3(3) . . . . ? C24 C23 N1 C1 3.9(3) . . . . ? C28 C23 N1 C1 177.7(2) . . . . ? C24 C23 N1 Ni1 -108.1(2) . . . . ? C28 C23 N1 Ni1 65.7(3) . . . . ? C2 C1 N1 C12 -48.0(3) . . . . ? C6 C1 N1 C12 131.8(2) . . . . ? C2 C1 N1 C23 88.5(3) . . . . ? C6 C1 N1 C23 -91.7(3) . . . . ? C2 C1 N1 Ni1 -158.4(2) . . . . ? C6 C1 N1 Ni1 21.4(3) . . . . ? O1 C7 N2 C6 18.8(5) . . . . ? C8 C7 N2 C6 -158.6(3) . . . . ? O1 C7 N2 Ni1 -147.4(3) . . . . ? C8 C7 N2 Ni1 35.3(4) . . . . ? C1 C6 N2 C7 163.0(3) . . . . ? C5 C6 N2 C7 -15.5(4) . . . . ? C1 C6 N2 Ni1 -28.0(3) . . . . ? C5 C6 N2 Ni1 153.6(2) . . . . ? O2 C18 N3 C17 -9.1(4) . . . . ? C19 C18 N3 C17 172.9(2) . . . . ? O2 C18 N3 Ni1 174.17(19) . . . . ? C19 C18 N3 Ni1 -3.9(3) . . . . ? C12 C17 N3 C18 165.4(2) . . . . ? C16 C17 N3 C18 -20.2(4) . . . . ? C12 C17 N3 Ni1 -17.1(3) . . . . ? C16 C17 N3 Ni1 157.2(2) . . . . ? O3 C29 N4 C28 3.2(4) . . . . ? C30 C29 N4 C28 -172.5(2) . . . . ? C27 C28 N4 C29 119.3(3) . . . . ? C23 C28 N4 C29 -65.7(4) . . . . ? O1S C1S N1S C2S -0.4(6) . . . . ? O1S C1S N1S C3S -177.5(4) . . . . ? C7 N2 Ni1 O3 -55.3(3) . . . . ? C6 N2 Ni1 O3 137.04(18) . . . . ? C7 N2 Ni1 N3 120.1(3) . . . . ? C6 N2 Ni1 N3 -47.55(19) . . . . ? C7 N2 Ni1 N1 -160.5(3) . . . . ? C6 N2 Ni1 N1 31.90(18) . . . . ? C18 N3 Ni1 O3 103.2(2) . . . . ? C17 N3 Ni1 O3 -73.87(16) . . . . ? C18 N3 Ni1 N2 -74.4(2) . . . . ? C17 N3 Ni1 N2 108.57(16) . . . . ? C18 N3 Ni1 N1 -155.2(2) . . . . ? C17 N3 Ni1 N1 27.68(16) . . . . ? C12 N1 Ni1 O3 68.13(17) . . . . ? C23 N1 Ni1 O3 -55.93(16) . . . . ? C1 N1 Ni1 O3 -177.28(14) . . . . ? C12 N1 Ni1 N2 -143.06(17) . . . . ? C23 N1 Ni1 N2 92.88(16) . . . . ? C1 N1 Ni1 N2 -28.47(15) . . . . ? C12 N1 Ni1 N3 -31.75(16) . . . . ? C23 N1 Ni1 N3 -155.81(16) . . . . ? C1 N1 Ni1 N3 82.84(15) . . . . ? N4 C29 O3 Ni1 52.0(4) . . . . ? C30 C29 O3 Ni1 -132.0(2) . . . . ? N2 Ni1 O3 C29 -116.2(2) . . . . ? N3 Ni1 O3 C29 68.2(2) . . . . ? N1 Ni1 O3 C29 -16.2(2) . . . . ? C47 C46 P1 C34 -94.0(3) . . . . ? C51 C46 P1 C34 83.7(2) . . . . ? C47 C46 P1 C52 146.5(2) . . . . ? C51 C46 P1 C52 -35.8(3) . . . . ? C47 C46 P1 C40 23.5(3) . . . . ? C51 C46 P1 C40 -158.8(2) . . . . ? C35 C34 P1 C46 -11.1(3) . . . . ? C39 C34 P1 C46 169.0(2) . . . . ? C35 C34 P1 C52 107.8(2) . . . . ? C39 C34 P1 C52 -72.1(2) . . . . ? C35 C34 P1 C40 -129.5(2) . . . . ? C39 C34 P1 C40 50.6(2) . . . . ? C57 C52 P1 C46 132.2(3) . . . . ? C53 C52 P1 C46 -46.4(3) . . . . ? C57 C52 P1 C34 12.0(3) . . . . ? C53 C52 P1 C34 -166.7(2) . . . . ? C57 C52 P1 C40 -107.4(3) . . . . ? C53 C52 P1 C40 74.0(3) . . . . ? C45 C40 P1 C46 82.3(3) . . . . ? C41 C40 P1 C46 -92.7(3) . . . . ? C45 C40 P1 C34 -158.2(3) . . . . ? C41 C40 P1 C34 26.7(3) . . . . ? C45 C40 P1 C52 -37.8(3) . . . . ? C41 C40 P1 C52 147.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.144 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.075 # Attachment 'laa_02_077Ntosub.cif' # Attachment 'mbj3028tosub.cif' data_mbj3028s _database_code_depnum_ccdc_archive 'CCDC 738760' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H67 N6 Ni O5 P' _chemical_formula_weight 1041.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 11.38710(10) _cell_length_b 16.0284(2) _cell_length_c 16.8718(2) _cell_angle_alpha 115.3630(10) _cell_angle_beta 102.2640(10) _cell_angle_gamma 91.6840(10) _cell_volume 2693.69(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9929 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.8781 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39239 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10982 _reflns_number_gt 9357 _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^)+(0.0655P)^2^+1.1251P] 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 10982 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.95736(16) 0.67975(12) 0.16416(12) 0.0274(4) Uani 1 1 d . . . C2 C 1.00898(18) 0.59824(13) 0.13212(14) 0.0340(4) Uani 1 1 d . . . H2 H 1.0766 0.5957 0.1068 0.041 Uiso 1 1 calc R . . C3 C 0.9615(2) 0.52015(14) 0.13712(15) 0.0399(5) Uani 1 1 d . . . H3 H 0.9963 0.4639 0.1155 0.048 Uiso 1 1 calc R . . C4 C 0.8632(2) 0.52563(14) 0.17397(16) 0.0417(5) Uani 1 1 d . . . H4 H 0.8322 0.4731 0.1793 0.050 Uiso 1 1 calc R . . C5 C 0.8086(2) 0.60600(14) 0.20346(15) 0.0377(5) Uani 1 1 d . . . H5 H 0.7399 0.6073 0.2273 0.045 Uiso 1 1 calc R . . C6 C 0.85420(17) 0.68570(13) 0.19838(13) 0.0290(4) Uani 1 1 d . . . C7 C 0.72323(17) 0.79273(13) 0.27311(13) 0.0305(4) Uani 1 1 d . . . C8 C 0.67750(19) 0.88609(15) 0.28934(14) 0.0355(4) Uani 1 1 d . . . H8 H 0.6721 0.8954 0.2338 0.043 Uiso 1 1 calc R . . C9 C 0.5523(2) 0.88731(19) 0.30760(19) 0.0531(6) Uani 1 1 d . . . H9A H 0.4951 0.8376 0.2553 0.080 Uiso 1 1 calc R . . H9B H 0.5252 0.9477 0.3178 0.080 Uiso 1 1 calc R . . H9C H 0.5560 0.8774 0.3614 0.080 Uiso 1 1 calc R . . C10 C 0.7670(2) 0.96554(16) 0.36898(17) 0.0481(6) Uani 1 1 d . . . H10A H 0.7738 0.9569 0.4238 0.072 Uiso 1 1 calc R . . H10B H 0.7379 1.0252 0.3784 0.072 Uiso 1 1 calc R . . H10C H 0.8467 0.9654 0.3557 0.072 Uiso 1 1 calc R . . C11 C 1.03612(17) 0.75089(12) 0.07809(13) 0.0281(4) Uani 1 1 d . . . C12 C 1.14885(18) 0.73267(13) 0.06175(14) 0.0334(4) Uani 1 1 d . . . H12 H 1.2115 0.7288 0.1068 0.040 Uiso 1 1 calc R . . C13 C 1.17056(19) 0.72001(14) -0.02015(15) 0.0381(5) Uani 1 1 d . . . H13 H 1.2481 0.7081 -0.0313 0.046 Uiso 1 1 calc R . . C14 C 1.0785(2) 0.72488(14) -0.08528(15) 0.0387(5) Uani 1 1 d . . . H14 H 1.0929 0.7151 -0.1419 0.046 Uiso 1 1 calc R . . C15 C 0.9650(2) 0.74383(14) -0.06956(14) 0.0362(5) Uani 1 1 d . . . H15 H 0.9027 0.7467 -0.1154 0.043 Uiso 1 1 calc R . . C16 C 0.94177(18) 0.75875(12) 0.01342(13) 0.0301(4) Uani 1 1 d . . . C17 C 0.72955(19) 0.77891(14) -0.01677(14) 0.0337(4) Uani 1 1 d . . . C18 C 0.62876(19) 0.82094(15) 0.02868(15) 0.0374(5) Uani 1 1 d . . . H18 H 0.6671 0.8674 0.0926 0.045 Uiso 1 1 calc R . . C19 C 0.5493(2) 0.74448(19) 0.03066(18) 0.0509(6) Uani 1 1 d . . . H19A H 0.5073 0.7001 -0.0314 0.076 Uiso 1 1 calc R . . H19B H 0.4894 0.7720 0.0649 0.076 Uiso 1 1 calc R . . H19C H 0.5998 0.7120 0.0598 0.076 Uiso 1 1 calc R . . C20 C 0.5550(2) 0.8711(2) -0.01948(18) 0.0546(6) Uani 1 1 d . . . H20A H 0.6078 0.9226 -0.0159 0.082 Uiso 1 1 calc R . . H20B H 0.4895 0.8957 0.0097 0.082 Uiso 1 1 calc R . . H20C H 0.5202 0.8273 -0.0831 0.082 Uiso 1 1 calc R . . C21 C 1.10712(16) 0.82237(13) 0.24507(13) 0.0289(4) Uani 1 1 d . . . C22 C 1.19494(18) 0.78381(15) 0.28339(15) 0.0376(5) Uani 1 1 d . . . H22 H 1.1932 0.7181 0.2578 0.045 Uiso 1 1 calc R . . C23 C 1.28614(19) 0.84130(17) 0.35959(15) 0.0437(5) Uani 1 1 d . . . H23 H 1.3467 0.8153 0.3866 0.052 Uiso 1 1 calc R . . C24 C 1.28709(19) 0.93664(17) 0.39523(15) 0.0451(6) Uani 1 1 d . . . H24 H 1.3499 0.9762 0.4464 0.054 Uiso 1 1 calc R . . C25 C 1.1986(2) 0.97563(15) 0.35797(15) 0.0420(5) Uani 1 1 d . . . H25 H 1.2012 1.0415 0.3842 0.050 Uiso 1 1 calc R . . C26 C 1.10473(17) 0.91947(13) 0.28197(13) 0.0318(4) Uani 1 1 d . . . C27 C 1.0011(2) 1.03902(14) 0.25588(16) 0.0430(5) Uani 1 1 d . . . C28 C 0.8849(2) 1.05326(15) 0.2020(2) 0.0564(7) Uani 1 1 d . . . H28 H 0.8193 1.0037 0.1906 0.068 Uiso 1 1 calc R . . C29 C 0.9024(4) 1.0405(3) 0.1100(3) 0.0918(12) Uani 1 1 d . . . H29A H 0.9657 1.0889 0.1194 0.138 Uiso 1 1 calc R . . H29B H 0.8261 1.0456 0.0735 0.138 Uiso 1 1 calc R . . H29C H 0.9265 0.9790 0.0785 0.138 Uiso 1 1 calc R . . C30 C 0.8452(3) 1.1473(2) 0.2531(3) 0.0987(14) Uani 1 1 d . . . H30A H 0.8360 1.1535 0.3118 0.148 Uiso 1 1 calc R . . H30B H 0.7675 1.1518 0.2177 0.148 Uiso 1 1 calc R . . H30C H 0.9066 1.1971 0.2628 0.148 Uiso 1 1 calc R . . C1A C 0.29468(18) 0.46398(14) 0.33362(13) 0.0325(4) Uani 1 1 d . . . C2A C 0.3122(2) 0.38398(15) 0.34528(15) 0.0411(5) Uani 1 1 d . . . H2A H 0.3894 0.3628 0.3481 0.049 Uiso 1 1 calc R . . C3A C 0.2147(3) 0.33549(17) 0.35272(17) 0.0530(6) Uani 1 1 d . . . H3A H 0.2250 0.2804 0.3601 0.064 Uiso 1 1 calc R . . C4A C 0.1033(2) 0.3672(2) 0.34944(18) 0.0574(7) Uani 1 1 d . . . H4A H 0.0380 0.3346 0.3561 0.069 Uiso 1 1 calc R . . C5A C 0.0858(2) 0.4455(2) 0.33665(18) 0.0540(6) Uani 1 1 d . . . H5A H 0.0085 0.4663 0.3338 0.065 Uiso 1 1 calc R . . C6A C 0.18114(19) 0.49404(17) 0.32786(16) 0.0428(5) Uani 1 1 d . . . H6A H 0.1690 0.5475 0.3180 0.051 Uiso 1 1 calc R . . C7A C 0.37509(17) 0.53898(13) 0.22126(13) 0.0308(4) Uani 1 1 d . . . C8A C 0.2902(2) 0.47071(15) 0.14873(15) 0.0400(5) Uani 1 1 d . . . H8A H 0.2477 0.4240 0.1565 0.048 Uiso 1 1 calc R . . C9A C 0.2676(2) 0.47080(17) 0.06489(16) 0.0491(6) Uani 1 1 d . . . H9A1 H 0.2096 0.4238 0.0151 0.059 Uiso 1 1 calc R . . C10A C 0.3275(3) 0.53749(19) 0.05308(17) 0.0544(6) Uani 1 1 d . . . H10D H 0.3138 0.5356 -0.0052 0.065 Uiso 1 1 calc R . . C11A C 0.4080(3) 0.6078(2) 0.1258(2) 0.0666(8) Uani 1 1 d . . . H11A H 0.4471 0.6558 0.1178 0.080 Uiso 1 1 calc R . . C12A C 0.4325(2) 0.60925(19) 0.21018(17) 0.0525(6) Uani 1 1 d . . . H12A H 0.4883 0.6580 0.2601 0.063 Uiso 1 1 calc R . . C13A C 0.45529(16) 0.64305(12) 0.42267(13) 0.0275(4) Uani 1 1 d . . . C14A C 0.55430(18) 0.70333(14) 0.43205(14) 0.0335(4) Uani 1 1 d . . . H14A H 0.6008 0.6845 0.3882 0.040 Uiso 1 1 calc R . . C15A C 0.58404(19) 0.79044(14) 0.50545(15) 0.0394(5) Uani 1 1 d . . . H15A H 0.6501 0.8320 0.5113 0.047 Uiso 1 1 calc R . . C16A C 0.5184(2) 0.81740(15) 0.57021(15) 0.0436(5) Uani 1 1 d . . . H16A H 0.5395 0.8773 0.6206 0.052 Uiso 1 1 calc R . . C17A C 0.4219(2) 0.75727(16) 0.56186(15) 0.0437(5) Uani 1 1 d . . . H17A H 0.3773 0.7759 0.6068 0.052 Uiso 1 1 calc R . . C18A C 0.38991(18) 0.66989(15) 0.48813(14) 0.0352(4) Uani 1 1 d . . . H18A H 0.3236 0.6287 0.4826 0.042 Uiso 1 1 calc R . . C19A C 0.54931(17) 0.47133(13) 0.32551(13) 0.0307(4) Uani 1 1 d . . . C20A C 0.5531(2) 0.39209(16) 0.24737(16) 0.0484(6) Uani 1 1 d . . . H20D H 0.4882 0.3711 0.1945 0.058 Uiso 1 1 calc R . . C21A C 0.6521(2) 0.34450(18) 0.24777(19) 0.0576(7) Uani 1 1 d . . . H21A H 0.6554 0.2907 0.1947 0.069 Uiso 1 1 calc R . . C22A C 0.7460(2) 0.37411(17) 0.32407(19) 0.0498(6) Uani 1 1 d . . . H22A H 0.8137 0.3407 0.3233 0.060 Uiso 1 1 calc R . . C23A C 0.7425(2) 0.45190(16) 0.40163(17) 0.0451(5) Uani 1 1 d . . . H23A H 0.8074 0.4719 0.4544 0.054 Uiso 1 1 calc R . . C24A C 0.64442(19) 0.50076(15) 0.40254(15) 0.0371(5) Uani 1 1 d . . . H24A H 0.6420 0.5546 0.4559 0.044 Uiso 1 1 calc R . . C1S C 1.1031(2) 0.7291(2) 0.4879(2) 0.0581(7) Uani 1 1 d . . . H1S H 1.1746 0.7582 0.4845 0.070 Uiso 1 1 calc R . . C2S C 0.8892(2) 0.7235(2) 0.4766(2) 0.0591(7) Uani 1 1 d . . . H2S1 H 0.8959 0.6601 0.4699 0.089 Uiso 1 1 calc R . . H2S2 H 0.8229 0.7216 0.4279 0.089 Uiso 1 1 calc R . . H2S3 H 0.8727 0.7621 0.5353 0.089 Uiso 1 1 calc R . . C3S C 0.9989(2) 0.84419(18) 0.45456(18) 0.0520(6) Uani 1 1 d . . . H3S1 H 1.0806 0.8652 0.4545 0.078 Uiso 1 1 calc R . . H3S2 H 0.9709 0.8942 0.5021 0.078 Uiso 1 1 calc R . . H3S3 H 0.9434 0.8282 0.3956 0.078 Uiso 1 1 calc R . . C4S C 0.5177(4) 0.9267(3) 0.7992(2) 0.0764(9) Uani 1 1 d . . . H4S H 0.4927 0.8634 0.7836 0.092 Uiso 1 1 calc R . . C5S C 0.6887(3) 1.0473(2) 0.8538(2) 0.0788(10) Uani 1 1 d . . . H5S1 H 0.6224 1.0848 0.8534 0.118 Uiso 1 1 calc R . . H5S2 H 0.7371 1.0507 0.8134 0.118 Uiso 1 1 calc R . . H5S3 H 0.7403 1.0713 0.9155 0.118 Uiso 1 1 calc R . . C6S C 0.7213(5) 0.8872(3) 0.8199(4) 0.1189(18) Uani 1 1 d . . . H6S1 H 0.7739 0.9059 0.8805 0.178 Uiso 1 1 calc R . . H6S2 H 0.7711 0.8843 0.7782 0.178 Uiso 1 1 calc R . . H6S3 H 0.6752 0.8257 0.7984 0.178 Uiso 1 1 calc R . . N1 N 1.00921(13) 0.76497(10) 0.16405(10) 0.0260(3) Uani 1 1 d . . . N2 N 0.80141(14) 0.76869(11) 0.21970(11) 0.0288(3) Uani 1 1 d . . . N3 N 0.83623(14) 0.78851(11) 0.04165(11) 0.0308(3) Uani 1 1 d . . . N4 N 1.00526(15) 0.94936(11) 0.24183(12) 0.0339(4) Uani 1 1 d . . . N1S N 1.00154(16) 0.76285(13) 0.47160(13) 0.0411(4) Uani 1 1 d . . . N2S N 0.6399(2) 0.95328(14) 0.82352(14) 0.0503(5) Uani 1 1 d . . . Ni1 Ni 0.87460(2) 0.845313(15) 0.174056(16) 0.02728(9) Uani 1 1 d . . . O1 O 0.69098(13) 0.74875(11) 0.31163(10) 0.0406(3) Uani 1 1 d . . . O2 O 0.70643(14) 0.73765(11) -0.10041(10) 0.0425(4) Uani 1 1 d . . . O3 O 1.08225(16) 1.10523(11) 0.30409(13) 0.0580(5) Uani 1 1 d . . . O1S O 1.11362(19) 0.66372(17) 0.50684(18) 0.0783(6) Uani 1 1 d . . . O2S O 0.4414(3) 0.9704(3) 0.7952(2) 0.1289(13) Uani 1 1 d . . . P1A P 0.41797(4) 0.53018(3) 0.32602(3) 0.02646(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 C1 0.0293(9) 0.0222(8) 0.0265(9) 0.0097(7) 0.0015(7) 0.0013(7) C2 0.0336(10) 0.0277(10) 0.0379(11) 0.0127(8) 0.0073(8) 0.0052(8) C3 0.0467(12) 0.0233(9) 0.0460(13) 0.0138(9) 0.0076(10) 0.0077(9) C4 0.0532(13) 0.0249(10) 0.0471(13) 0.0181(9) 0.0089(10) -0.0008(9) C5 0.0452(12) 0.0301(10) 0.0387(12) 0.0151(9) 0.0134(9) 0.0002(9) C6 0.0342(10) 0.0238(9) 0.0261(9) 0.0099(7) 0.0044(8) 0.0026(7) C7 0.0285(9) 0.0329(10) 0.0280(10) 0.0131(8) 0.0042(8) 0.0015(8) C8 0.0382(11) 0.0393(11) 0.0340(11) 0.0177(9) 0.0151(9) 0.0116(9) C9 0.0434(13) 0.0613(16) 0.0663(17) 0.0331(14) 0.0250(12) 0.0212(11) C10 0.0572(14) 0.0354(11) 0.0465(14) 0.0095(10) 0.0207(11) 0.0110(10) C11 0.0341(10) 0.0177(8) 0.0298(10) 0.0071(7) 0.0106(8) 0.0017(7) C12 0.0344(10) 0.0245(9) 0.0350(11) 0.0074(8) 0.0090(8) 0.0033(8) C13 0.0383(11) 0.0287(10) 0.0426(12) 0.0073(9) 0.0195(9) 0.0042(8) C14 0.0511(13) 0.0303(10) 0.0367(11) 0.0122(9) 0.0213(10) 0.0046(9) C15 0.0442(11) 0.0318(10) 0.0360(11) 0.0166(9) 0.0136(9) 0.0058(9) C16 0.0368(10) 0.0219(9) 0.0335(10) 0.0125(8) 0.0121(8) 0.0034(7) C17 0.0393(11) 0.0310(10) 0.0349(11) 0.0183(9) 0.0093(9) 0.0071(8) C18 0.0363(11) 0.0433(12) 0.0336(11) 0.0183(9) 0.0076(9) 0.0105(9) C19 0.0421(13) 0.0597(15) 0.0561(15) 0.0287(13) 0.0163(11) 0.0057(11) C20 0.0578(15) 0.0676(17) 0.0532(15) 0.0362(14) 0.0203(12) 0.0315(13) C21 0.0255(9) 0.0295(9) 0.0280(10) 0.0089(8) 0.0079(7) -0.0010(7) C22 0.0316(10) 0.0379(11) 0.0402(12) 0.0152(9) 0.0077(9) 0.0032(8) C23 0.0291(10) 0.0577(14) 0.0405(12) 0.0208(11) 0.0041(9) 0.0011(10) C24 0.0309(11) 0.0555(14) 0.0304(11) 0.0042(10) 0.0051(9) -0.0056(10) C25 0.0393(11) 0.0332(11) 0.0378(12) 0.0009(9) 0.0121(9) -0.0040(9) C26 0.0312(10) 0.0300(10) 0.0295(10) 0.0074(8) 0.0119(8) -0.0011(8) C27 0.0514(13) 0.0244(10) 0.0501(13) 0.0108(9) 0.0200(11) 0.0006(9) C28 0.0586(15) 0.0239(10) 0.0788(19) 0.0200(12) 0.0080(13) 0.0046(10) C29 0.112(3) 0.081(2) 0.093(3) 0.060(2) 0.002(2) 0.009(2) C30 0.074(2) 0.0326(14) 0.150(4) 0.0134(18) 0.006(2) 0.0167(14) C1A 0.0333(10) 0.0306(10) 0.0290(10) 0.0111(8) 0.0044(8) -0.0057(8) C2A 0.0490(13) 0.0347(11) 0.0371(12) 0.0158(9) 0.0074(10) -0.0014(9) C3A 0.0701(17) 0.0419(13) 0.0458(14) 0.0229(11) 0.0075(12) -0.0139(12) C4A 0.0479(14) 0.0672(17) 0.0509(15) 0.0287(13) -0.0006(11) -0.0270(13) C5A 0.0339(12) 0.0705(17) 0.0548(15) 0.0298(13) 0.0036(10) -0.0105(11) C6A 0.0327(11) 0.0471(12) 0.0468(13) 0.0230(11) 0.0035(9) -0.0044(9) C7A 0.0321(10) 0.0309(10) 0.0290(10) 0.0134(8) 0.0065(8) 0.0073(8) C8A 0.0445(12) 0.0327(10) 0.0358(11) 0.0131(9) 0.0009(9) 0.0022(9) C9A 0.0555(14) 0.0448(13) 0.0327(12) 0.0099(10) -0.0024(10) 0.0095(11) C10A 0.0682(16) 0.0645(16) 0.0334(13) 0.0264(12) 0.0078(11) 0.0149(13) C11A 0.0723(18) 0.081(2) 0.0555(17) 0.0443(16) 0.0058(14) -0.0124(15) C12A 0.0542(14) 0.0591(15) 0.0431(13) 0.0286(12) -0.0003(11) -0.0121(12) C13A 0.0281(9) 0.0243(9) 0.0264(9) 0.0089(7) 0.0047(7) 0.0028(7) C14A 0.0347(10) 0.0297(10) 0.0337(11) 0.0108(8) 0.0112(8) 0.0008(8) C15A 0.0388(11) 0.0312(10) 0.0396(12) 0.0105(9) 0.0051(9) -0.0033(9) C16A 0.0476(12) 0.0319(11) 0.0363(12) 0.0042(9) 0.0044(10) 0.0061(9) C17A 0.0409(12) 0.0492(13) 0.0322(11) 0.0076(10) 0.0138(9) 0.0100(10) C18A 0.0310(10) 0.0392(11) 0.0328(11) 0.0130(9) 0.0096(8) 0.0021(8) C19A 0.0312(10) 0.0275(9) 0.0324(10) 0.0132(8) 0.0064(8) 0.0045(7) C20A 0.0420(12) 0.0435(13) 0.0401(13) 0.0037(10) 0.0023(10) 0.0145(10) C21A 0.0522(14) 0.0454(14) 0.0543(16) 0.0037(12) 0.0095(12) 0.0219(11) C22A 0.0387(12) 0.0413(12) 0.0673(17) 0.0227(12) 0.0105(11) 0.0157(10) C23A 0.0398(12) 0.0438(12) 0.0481(13) 0.0231(11) -0.0021(10) 0.0080(10) C24A 0.0401(11) 0.0323(10) 0.0340(11) 0.0127(9) 0.0038(9) 0.0078(9) C1S 0.0400(13) 0.0763(19) 0.0749(19) 0.0455(16) 0.0209(12) 0.0189(12) C2S 0.0381(13) 0.084(2) 0.0739(19) 0.0524(17) 0.0135(12) 0.0077(12) C3S 0.0481(13) 0.0545(14) 0.0558(15) 0.0306(13) 0.0045(11) 0.0067(11) C4S 0.102(3) 0.093(2) 0.0456(17) 0.0392(17) 0.0230(17) 0.003(2) C5S 0.106(3) 0.0529(17) 0.077(2) 0.0213(16) 0.041(2) -0.0061(17) C6S 0.172(4) 0.103(3) 0.167(4) 0.094(3) 0.128(4) 0.084(3) N1 0.0270(8) 0.0210(7) 0.0265(8) 0.0080(6) 0.0052(6) 0.0020(6) N2 0.0309(8) 0.0256(8) 0.0311(9) 0.0123(7) 0.0106(7) 0.0042(6) N3 0.0330(8) 0.0319(8) 0.0298(9) 0.0152(7) 0.0095(7) 0.0062(7) N4 0.0351(9) 0.0213(8) 0.0392(10) 0.0076(7) 0.0102(7) 0.0010(6) N1S 0.0334(9) 0.0496(11) 0.0443(11) 0.0243(9) 0.0095(8) 0.0085(8) N2S 0.0696(14) 0.0416(11) 0.0454(12) 0.0195(9) 0.0256(10) 0.0059(10) Ni1 0.02991(14) 0.02063(13) 0.03000(15) 0.00958(10) 0.00845(10) 0.00424(9) O1 0.0420(8) 0.0447(8) 0.0462(9) 0.0262(7) 0.0201(7) 0.0080(7) O2 0.0460(9) 0.0470(9) 0.0302(8) 0.0144(7) 0.0066(6) 0.0086(7) O3 0.0619(11) 0.0268(8) 0.0715(12) 0.0128(8) 0.0107(9) -0.0091(7) O1S 0.0647(13) 0.0911(16) 0.1151(19) 0.0736(15) 0.0305(12) 0.0364(12) O2S 0.085(2) 0.207(4) 0.138(3) 0.124(3) 0.0137(19) 0.017(2) P1A 0.0266(2) 0.0238(2) 0.0269(3) 0.01007(19) 0.00550(19) 0.00146(18) _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 C1 C2 1.386(3) . ? C1 C6 1.404(3) . ? C1 N1 1.473(2) . ? C2 C3 1.391(3) . ? C3 C4 1.379(3) . ? C4 C5 1.387(3) . ? C5 C6 1.408(3) . ? C6 N2 1.410(2) . ? C7 O1 1.238(2) . ? C7 N2 1.348(3) . ? C7 C8 1.530(3) . ? C8 C9 1.520(3) . ? C8 C10 1.531(3) . ? C11 C12 1.383(3) . ? C11 C16 1.410(3) . ? C11 N1 1.470(2) . ? C12 C13 1.386(3) . ? C13 C14 1.379(3) . ? C14 C15 1.390(3) . ? C15 C16 1.400(3) . ? C16 N3 1.407(3) . ? C17 O2 1.237(2) . ? C17 N3 1.350(3) . ? C17 C18 1.528(3) . ? C18 C19 1.518(3) . ? C18 C20 1.524(3) . ? C21 C22 1.380(3) . ? C21 C26 1.411(3) . ? C21 N1 1.474(2) . ? C22 C23 1.394(3) . ? C23 C24 1.381(3) . ? C24 C25 1.381(3) . ? C25 C26 1.403(3) . ? C26 N4 1.398(3) . ? C27 O3 1.235(3) . ? C27 N4 1.357(3) . ? C27 C28 1.521(4) . ? C28 C30 1.520(4) . ? C28 C29 1.533(5) . ? C1A C6A 1.392(3) . ? C1A C2A 1.392(3) . ? C1A P1A 1.7941(19) . ? C2A C3A 1.395(3) . ? C3A C4A 1.379(4) . ? C4A C5A 1.375(4) . ? C5A C6A 1.387(3) . ? C7A C8A 1.385(3) . ? C7A C12A 1.386(3) . ? C7A P1A 1.798(2) . ? C8A C9A 1.384(3) . ? C9A C10A 1.358(4) . ? C10A C11A 1.375(4) . ? C11A C12A 1.382(4) . ? C13A C18A 1.386(3) . ? C13A C14A 1.400(3) . ? C13A P1A 1.8016(19) . ? C14A C15A 1.382(3) . ? C15A C16A 1.379(3) . ? C16A C17A 1.382(3) . ? C17A C18A 1.388(3) . ? C19A C24A 1.390(3) . ? C19A C20A 1.395(3) . ? C19A P1A 1.791(2) . ? C20A C21A 1.381(3) . ? C21A C22A 1.374(4) . ? C22A C23A 1.377(4) . ? C23A C24A 1.382(3) . ? C1S O1S 1.222(3) . ? C1S N1S 1.317(3) . ? C2S N1S 1.443(3) . ? C3S N1S 1.450(3) . ? C4S O2S 1.141(5) . ? C4S N2S 1.364(4) . ? C5S N2S 1.418(3) . ? C6S N2S 1.418(4) . ? N1 Ni1 2.0189(15) . ? N2 Ni1 1.9542(15) . ? N3 Ni1 1.9570(16) . ? N4 Ni1 1.9493(16) . ? 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 C2 C1 C6 122.18(17) . . ? C2 C1 N1 121.10(17) . . ? C6 C1 N1 116.71(16) . . ? C1 C2 C3 119.8(2) . . ? C4 C3 C2 119.0(2) . . ? C3 C4 C5 121.56(19) . . ? C4 C5 C6 120.6(2) . . ? C1 C6 C5 116.83(18) . . ? C1 C6 N2 117.31(16) . . ? C5 C6 N2 125.75(18) . . ? O1 C7 N2 126.16(19) . . ? O1 C7 C8 119.09(18) . . ? N2 C7 C8 114.68(16) . . ? C9 C8 C7 111.08(18) . . ? C9 C8 C10 110.14(19) . . ? C7 C8 C10 109.87(18) . . ? C12 C11 C16 121.40(18) . . ? C12 C11 N1 121.95(18) . . ? C16 C11 N1 116.64(16) . . ? C11 C12 C13 120.1(2) . . ? C14 C13 C12 119.4(2) . . ? C13 C14 C15 121.1(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 N3 126.06(18) . . ? C15 C16 C11 117.46(18) . . ? N3 C16 C11 116.27(17) . . ? O2 C17 N3 126.63(19) . . ? O2 C17 C18 119.09(18) . . ? N3 C17 C18 114.22(18) . . ? C19 C18 C20 111.6(2) . . ? C19 C18 C17 109.22(18) . . ? C20 C18 C17 111.02(18) . . ? C22 C21 C26 121.86(18) . . ? C22 C21 N1 122.31(17) . . ? C26 C21 N1 115.83(17) . . ? C21 C22 C23 120.0(2) . . ? C24 C23 C22 118.9(2) . . ? C23 C24 C25 121.4(2) . . ? C24 C25 C26 121.0(2) . . ? N4 C26 C25 126.69(19) . . ? N4 C26 C21 116.39(17) . . ? C25 C26 C21 116.82(19) . . ? O3 C27 N4 126.2(2) . . ? O3 C27 C28 120.2(2) . . ? N4 C27 C28 113.59(18) . . ? C30 C28 C27 112.3(2) . . ? C30 C28 C29 111.5(3) . . ? C27 C28 C29 109.2(3) . . ? C6A C1A C2A 120.49(19) . . ? C6A C1A P1A 118.90(16) . . ? C2A C1A P1A 120.61(17) . . ? C1A C2A C3A 118.9(2) . . ? C4A C3A C2A 120.3(2) . . ? C5A C4A C3A 120.7(2) . . ? C4A C5A C6A 120.0(2) . . ? C5A C6A C1A 119.7(2) . . ? C8A C7A C12A 119.6(2) . . ? C8A C7A P1A 119.46(16) . . ? C12A C7A P1A 120.74(16) . . ? C9A C8A C7A 119.7(2) . . ? C10A C9A C8A 120.6(2) . . ? C9A C10A C11A 119.8(2) . . ? C10A C11A C12A 120.7(2) . . ? C11A C12A C7A 119.3(2) . . ? C18A C13A C14A 119.93(18) . . ? C18A C13A P1A 121.35(14) . . ? C14A C13A P1A 118.70(15) . . ? C15A C14A C13A 119.61(19) . . ? C16A C15A C14A 120.42(19) . . ? C15A C16A C17A 120.0(2) . . ? C16A C17A C18A 120.4(2) . . ? C13A C18A C17A 119.61(19) . . ? C24A C19A C20A 119.7(2) . . ? C24A C19A P1A 121.18(16) . . ? C20A C19A P1A 119.01(16) . . ? C21A C20A C19A 119.2(2) . . ? C22A C21A C20A 120.8(2) . . ? C21A C22A C23A 120.4(2) . . ? C22A C23A C24A 119.8(2) . . ? C23A C24A C19A 120.1(2) . . ? O1S C1S N1S 125.8(3) . . ? O2S C4S N2S 128.6(4) . . ? C11 N1 C1 114.49(14) . . ? C11 N1 C21 114.29(14) . . ? C1 N1 C21 113.95(14) . . ? C11 N1 Ni1 103.52(11) . . ? C1 N1 Ni1 105.07(11) . . ? C21 N1 Ni1 103.80(11) . . ? C7 N2 C6 122.59(16) . . ? C7 N2 Ni1 127.19(13) . . ? C6 N2 Ni1 109.77(12) . . ? C17 N3 C16 122.93(17) . . ? C17 N3 Ni1 128.36(14) . . ? C16 N3 Ni1 108.70(12) . . ? C27 N4 C26 123.57(17) . . ? C27 N4 Ni1 127.21(15) . . ? C26 N4 Ni1 109.01(12) . . ? C1S N1S C2S 120.6(2) . . ? C1S N1S C3S 122.0(2) . . ? C2S N1S C3S 117.3(2) . . ? C4S N2S C5S 121.1(3) . . ? C4S N2S C6S 120.4(3) . . ? C5S N2S C6S 118.5(3) . . ? N4 Ni1 N2 127.19(7) . . ? N4 Ni1 N3 118.29(7) . . ? N2 Ni1 N3 112.68(7) . . ? N4 Ni1 N1 84.85(7) . . ? N2 Ni1 N1 86.32(6) . . ? N3 Ni1 N1 85.39(7) . . ? C19A P1A C1A 109.78(9) . . ? C19A P1A C7A 108.48(9) . . ? C1A P1A C7A 108.53(9) . . ? C19A P1A C13A 108.14(9) . . ? C1A P1A C13A 109.95(9) . . ? C7A P1A C13A 111.94(9) . . ? 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 C6 C1 C2 C3 -2.9(3) . . . . ? N1 C1 C2 C3 176.90(18) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 2.0(3) . . . . ? C3 C4 C5 C6 -1.4(3) . . . . ? C2 C1 C6 C5 3.4(3) . . . . ? N1 C1 C6 C5 -176.42(17) . . . . ? C2 C1 C6 N2 -173.08(18) . . . . ? N1 C1 C6 N2 7.1(2) . . . . ? C4 C5 C6 C1 -1.2(3) . . . . ? C4 C5 C6 N2 174.91(19) . . . . ? O1 C7 C8 C9 -30.8(3) . . . . ? N2 C7 C8 C9 152.16(19) . . . . ? O1 C7 C8 C10 91.3(2) . . . . ? N2 C7 C8 C10 -85.7(2) . . . . ? C16 C11 C12 C13 -1.2(3) . . . . ? N1 C11 C12 C13 -179.87(17) . . . . ? C11 C12 C13 C14 -0.6(3) . . . . ? C12 C13 C14 C15 1.1(3) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C14 C15 C16 N3 172.47(18) . . . . ? C14 C15 C16 C11 -1.9(3) . . . . ? C12 C11 C16 C15 2.4(3) . . . . ? N1 C11 C16 C15 -178.82(16) . . . . ? C12 C11 C16 N3 -172.53(16) . . . . ? N1 C11 C16 N3 6.2(2) . . . . ? O2 C17 C18 C19 79.8(2) . . . . ? N3 C17 C18 C19 -97.6(2) . . . . ? O2 C17 C18 C20 -43.6(3) . . . . ? N3 C17 C18 C20 138.9(2) . . . . ? C26 C21 C22 C23 -1.4(3) . . . . ? N1 C21 C22 C23 179.48(18) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C22 C23 C24 C25 1.2(3) . . . . ? C23 C24 C25 C26 -0.4(3) . . . . ? C24 C25 C26 N4 175.0(2) . . . . ? C24 C25 C26 C21 -1.2(3) . . . . ? C22 C21 C26 N4 -174.51(18) . . . . ? N1 C21 C26 N4 4.7(2) . . . . ? C22 C21 C26 C25 2.1(3) . . . . ? N1 C21 C26 C25 -178.67(17) . . . . ? O3 C27 C28 C30 -36.6(4) . . . . ? N4 C27 C28 C30 145.8(3) . . . . ? O3 C27 C28 C29 87.6(3) . . . . ? N4 C27 C28 C29 -89.9(3) . . . . ? C6A C1A C2A C3A -1.1(3) . . . . ? P1A C1A C2A C3A 178.72(17) . . . . ? C1A C2A C3A C4A -0.7(4) . . . . ? C2A C3A C4A C5A 1.6(4) . . . . ? C3A C4A C5A C6A -0.7(4) . . . . ? C4A C5A C6A C1A -1.1(4) . . . . ? C2A C1A C6A C5A 2.0(3) . . . . ? P1A C1A C6A C5A -177.84(19) . . . . ? C12A C7A C8A C9A 3.0(3) . . . . ? P1A C7A C8A C9A -172.20(18) . . . . ? C7A C8A C9A C10A -0.3(4) . . . . ? C8A C9A C10A C11A -2.5(4) . . . . ? C9A C10A C11A C12A 2.7(5) . . . . ? C10A C11A C12A C7A 0.0(5) . . . . ? C8A C7A C12A C11A -2.8(4) . . . . ? P1A C7A C12A C11A 172.3(2) . . . . ? C18A C13A C14A C15A -1.8(3) . . . . ? P1A C13A C14A C15A 179.65(16) . . . . ? C13A C14A C15A C16A 1.3(3) . . . . ? C14A C15A C16A C17A -0.2(4) . . . . ? C15A C16A C17A C18A -0.5(4) . . . . ? C14A C13A C18A C17A 1.2(3) . . . . ? P1A C13A C18A C17A 179.65(17) . . . . ? C16A C17A C18A C13A 0.0(3) . . . . ? C24A C19A C20A C21A -0.5(4) . . . . ? P1A C19A C20A C21A -177.6(2) . . . . ? C19A C20A C21A C22A 0.3(4) . . . . ? C20A C21A C22A C23A 0.1(4) . . . . ? C21A C22A C23A C24A -0.4(4) . . . . ? C22A C23A C24A C19A 0.2(3) . . . . ? C20A C19A C24A C23A 0.2(3) . . . . ? P1A C19A C24A C23A 177.28(17) . . . . ? C12 C11 N1 C1 -92.3(2) . . . . ? C16 C11 N1 C1 88.98(19) . . . . ? C12 C11 N1 C21 41.7(2) . . . . ? C16 C11 N1 C21 -137.00(16) . . . . ? C12 C11 N1 Ni1 153.93(14) . . . . ? C16 C11 N1 Ni1 -24.81(17) . . . . ? C2 C1 N1 C11 47.9(2) . . . . ? C6 C1 N1 C11 -132.24(17) . . . . ? C2 C1 N1 C21 -86.2(2) . . . . ? C6 C1 N1 C21 93.58(19) . . . . ? C2 C1 N1 Ni1 160.82(15) . . . . ? C6 C1 N1 Ni1 -19.37(18) . . . . ? C22 C21 N1 C11 -93.3(2) . . . . ? C26 C21 N1 C11 87.54(19) . . . . ? C22 C21 N1 C1 41.0(2) . . . . ? C26 C21 N1 C1 -138.19(17) . . . . ? C22 C21 N1 Ni1 154.71(16) . . . . ? C26 C21 N1 Ni1 -24.48(18) . . . . ? O1 C7 N2 C6 2.3(3) . . . . ? C8 C7 N2 C6 179.09(17) . . . . ? O1 C7 N2 Ni1 -169.18(15) . . . . ? C8 C7 N2 Ni1 7.6(2) . . . . ? C1 C6 N2 C7 -162.83(17) . . . . ? C5 C6 N2 C7 21.1(3) . . . . ? C1 C6 N2 Ni1 10.0(2) . . . . ? C5 C6 N2 Ni1 -166.15(17) . . . . ? O2 C17 N3 C16 6.1(3) . . . . ? C18 C17 N3 C16 -176.70(16) . . . . ? O2 C17 N3 Ni1 -175.37(15) . . . . ? C18 C17 N3 Ni1 1.8(2) . . . . ? C15 C16 N3 C17 21.4(3) . . . . ? C11 C16 N3 C17 -164.14(17) . . . . ? C15 C16 N3 Ni1 -157.39(16) . . . . ? C11 C16 N3 Ni1 17.07(18) . . . . ? O3 C27 N4 C26 0.6(4) . . . . ? C28 C27 N4 C26 177.9(2) . . . . ? O3 C27 N4 Ni1 174.79(18) . . . . ? C28 C27 N4 Ni1 -7.9(3) . . . . ? C25 C26 N4 C27 17.9(3) . . . . ? C21 C26 N4 C27 -165.79(19) . . . . ? C25 C26 N4 Ni1 -157.19(18) . . . . ? C21 C26 N4 Ni1 19.1(2) . . . . ? O1S C1S N1S C2S 0.9(5) . . . . ? O1S C1S N1S C3S 176.4(3) . . . . ? O2S C4S N2S C5S 4.0(5) . . . . ? O2S C4S N2S C6S -176.6(4) . . . . ? C27 N4 Ni1 N2 -119.94(18) . . . . ? C26 N4 Ni1 N2 54.96(16) . . . . ? C27 N4 Ni1 N3 76.7(2) . . . . ? C26 N4 Ni1 N3 -108.39(14) . . . . ? C27 N4 Ni1 N1 158.64(19) . . . . ? C26 N4 Ni1 N1 -26.46(13) . . . . ? C7 N2 Ni1 N4 74.90(18) . . . . ? C6 N2 Ni1 N4 -97.48(13) . . . . ? C7 N2 Ni1 N3 -120.97(16) . . . . ? C6 N2 Ni1 N3 66.66(14) . . . . ? C7 N2 Ni1 N1 155.59(16) . . . . ? C6 N2 Ni1 N1 -16.78(12) . . . . ? C17 N3 Ni1 N4 -122.09(16) . . . . ? C16 N3 Ni1 N4 56.61(14) . . . . ? C17 N3 Ni1 N2 72.23(17) . . . . ? C16 N3 Ni1 N2 -109.07(12) . . . . ? C17 N3 Ni1 N1 156.29(17) . . . . ? C16 N3 Ni1 N1 -25.00(12) . . . . ? C11 N1 Ni1 N4 -92.35(11) . . . . ? C1 N1 Ni1 N4 147.23(12) . . . . ? C21 N1 Ni1 N4 27.30(11) . . . . ? C11 N1 Ni1 N2 139.77(11) . . . . ? C1 N1 Ni1 N2 19.36(11) . . . . ? C21 N1 Ni1 N2 -100.58(11) . . . . ? C11 N1 Ni1 N3 26.64(10) . . . . ? C1 N1 Ni1 N3 -93.78(11) . . . . ? C21 N1 Ni1 N3 146.29(11) . . . . ? C24A C19A P1A C1A -102.71(18) . . . . ? C20A C19A P1A C1A 74.4(2) . . . . ? C24A C19A P1A C7A 138.85(17) . . . . ? C20A C19A P1A C7A -44.1(2) . . . . ? C24A C19A P1A C13A 17.25(19) . . . . ? C20A C19A P1A C13A -165.66(18) . . . . ? C6A C1A P1A C19A -175.04(17) . . . . ? C2A C1A P1A C19A 5.1(2) . . . . ? C6A C1A P1A C7A -56.63(19) . . . . ? C2A C1A P1A C7A 123.52(17) . . . . ? C6A C1A P1A C13A 66.11(19) . . . . ? C2A C1A P1A C13A -113.74(18) . . . . ? C8A C7A P1A C19A 92.99(18) . . . . ? C12A C7A P1A C19A -82.1(2) . . . . ? C8A C7A P1A C1A -26.2(2) . . . . ? C12A C7A P1A C1A 158.7(2) . . . . ? C8A C7A P1A C13A -147.77(17) . . . . ? C12A C7A P1A C13A 37.1(2) . . . . ? C18A C13A P1A C19A -122.11(17) . . . . ? C14A C13A P1A C19A 56.40(18) . . . . ? C18A C13A P1A C1A -2.3(2) . . . . ? C14A C13A P1A C1A 176.26(16) . . . . ? C18A C13A P1A C7A 118.45(17) . . . . ? C14A C13A P1A C7A -63.04(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.054 # Attachment 'laa_02_077Ntosub.cif' # Attachment 'mbj3_005_0tosub.cif' data_mbj3_005_0m _database_code_depnum_ccdc_archive 'CCDC 738761' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H73 N7 Ni O3' _chemical_formula_sum 'C47 H73 N7 Ni O3' _chemical_formula_weight 842.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 11.412(6) _cell_length_b 18.653(10) _cell_length_c 43.91(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.676(14) _cell_angle_gamma 90.00 _cell_volume 9285(8) _cell_formula_units_Z 8 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used 9369 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.41 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details 'SADABS V2.10, Sheldrick 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 159728 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 22.17 _reflns_number_total 11486 _reflns_number_gt 9748 _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^)+(0.0653P)^2^+52.5000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11486 _refine_ls_number_parameters 603 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1873 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 C1 C 0.3666(5) 0.6084(3) 0.08843(13) 0.0268(13) Uiso 1 1 d . . . C2 C 0.4132(6) 0.5393(3) 0.09553(14) 0.0374(15) Uiso 1 1 d . . . H2 H 0.4894 0.5275 0.0903 0.045 Uiso 1 1 calc R . . C3 C 0.3514(6) 0.4894(4) 0.10968(15) 0.0427(17) Uiso 1 1 d . . . H3 H 0.3850 0.4434 0.1138 0.051 Uiso 1 1 calc R . . C4 C 0.2420(6) 0.5040(4) 0.11812(15) 0.0436(17) Uiso 1 1 d . . . H4 H 0.2003 0.4690 0.1283 0.052 Uiso 1 1 calc R . . C5 C 0.1940(5) 0.5709(3) 0.11144(13) 0.0339(15) Uiso 1 1 d . . . H5 H 0.1180 0.5820 0.1170 0.041 Uiso 1 1 calc R . . C6 C 0.2554(5) 0.6218(3) 0.09676(13) 0.0269(13) Uiso 1 1 d . . . C7 C 0.2381(5) 0.7718(3) 0.13413(13) 0.0279(14) Uiso 1 1 d . . . C8 C 0.1932(5) 0.8050(3) 0.15893(14) 0.0355(15) Uiso 1 1 d . . . H8 H 0.2442 0.8332 0.1728 0.043 Uiso 1 1 calc R . . C9 C 0.0766(6) 0.7973(3) 0.16362(15) 0.0388(16) Uiso 1 1 d . . . H9 H 0.0477 0.8212 0.1803 0.047 Uiso 1 1 calc R . . C10 C 0.0027(6) 0.7562(4) 0.14464(15) 0.0435(17) Uiso 1 1 d . . . H10 H -0.0776 0.7514 0.1480 0.052 Uiso 1 1 calc R . . C11 C 0.0445(5) 0.7213(3) 0.12030(13) 0.0325(14) Uiso 1 1 d . . . H11 H -0.0072 0.6923 0.1070 0.039 Uiso 1 1 calc R . . C12 C 0.1601(5) 0.7284(3) 0.11536(13) 0.0270(13) Uiso 1 1 d . . . C13 C 0.1262(5) 0.6963(3) 0.06132(13) 0.0283(14) Uiso 1 1 d . . . C14 C 0.0628(5) 0.6395(3) 0.04861(14) 0.0375(15) Uiso 1 1 d . . . H14 H 0.0714 0.5935 0.0579 0.045 Uiso 1 1 calc R . . C15 C -0.0137(6) 0.6491(4) 0.02220(15) 0.0450(17) Uiso 1 1 d . . . H15 H -0.0596 0.6101 0.0136 0.054 Uiso 1 1 calc R . . C16 C -0.0235(6) 0.7147(4) 0.00847(15) 0.0426(17) Uiso 1 1 d . . . H16 H -0.0754 0.7209 -0.0099 0.051 Uiso 1 1 calc R . . C17 C 0.0410(5) 0.7719(3) 0.02090(14) 0.0376(16) Uiso 1 1 d . . . H17 H 0.0330 0.8171 0.0109 0.045 Uiso 1 1 calc R . . C18 C 0.1176(5) 0.7656(3) 0.04778(13) 0.0319(14) Uiso 1 1 d . . . C19 C 0.5156(5) 0.6454(3) 0.05941(14) 0.0322(15) Uiso 1 1 d . . . C20 C 0.6165(5) 0.6974(3) 0.05923(14) 0.0352(15) Uiso 1 1 d . . . H20 H 0.5923 0.7452 0.0667 0.042 Uiso 1 1 calc R . . C21 C 0.7173(7) 0.6680(4) 0.08117(18) 0.060(2) Uiso 1 1 d . . . H21A H 0.6957 0.6693 0.1021 0.091 Uiso 1 1 calc R . . H21B H 0.7880 0.6972 0.0800 0.091 Uiso 1 1 calc R . . H21C H 0.7333 0.6183 0.0756 0.091 Uiso 1 1 calc R . . C22 C 0.6523(7) 0.7055(4) 0.02700(17) 0.061(2) Uiso 1 1 d . . . H22A H 0.6528 0.6583 0.0172 0.091 Uiso 1 1 calc R . . H22B H 0.7313 0.7266 0.0282 0.091 Uiso 1 1 calc R . . H22C H 0.5958 0.7368 0.0149 0.091 Uiso 1 1 calc R . . C23 C 0.4397(5) 0.8035(3) 0.14494(14) 0.0323(15) Uiso 1 1 d . . . C24 C 0.5499(5) 0.8261(3) 0.13173(15) 0.0382(16) Uiso 1 1 d . . . H24 H 0.5540 0.8009 0.1118 0.046 Uiso 1 1 calc R . . C25 C 0.5463(6) 0.9073(4) 0.12627(16) 0.0503(18) Uiso 1 1 d . . . H25A H 0.4850 0.9185 0.1094 0.075 Uiso 1 1 calc R . . H25B H 0.6231 0.9235 0.1210 0.075 Uiso 1 1 calc R . . H25C H 0.5285 0.9317 0.1449 0.075 Uiso 1 1 calc R . . C26 C 0.6584(6) 0.8081(4) 0.15355(16) 0.0525(19) Uiso 1 1 d . . . H26A H 0.6511 0.8290 0.1737 0.079 Uiso 1 1 calc R . . H26B H 0.7285 0.8276 0.1456 0.079 Uiso 1 1 calc R . . H26C H 0.6660 0.7559 0.1555 0.079 Uiso 1 1 calc R . . C27 C 0.1663(5) 0.8865(3) 0.06051(14) 0.0322(15) Uiso 1 1 d . . . C28 C 0.2350(6) 0.9342(3) 0.08436(14) 0.0383(16) Uiso 1 1 d . . . H28 H 0.3001 0.9052 0.0955 0.046 Uiso 1 1 calc R . . C29 C 0.1525(6) 0.9580(4) 0.10736(15) 0.0471(18) Uiso 1 1 d . . . H29A H 0.0893 0.9878 0.0969 0.071 Uiso 1 1 calc R . . H29B H 0.1970 0.9858 0.1237 0.071 Uiso 1 1 calc R . . H29C H 0.1181 0.9157 0.1162 0.071 Uiso 1 1 calc R . . C30 C 0.2890(6) 0.9986(4) 0.07039(16) 0.0475(18) Uiso 1 1 d . . . H30A H 0.3424 0.9824 0.0559 0.071 Uiso 1 1 calc R . . H30B H 0.3332 1.0270 0.0866 0.071 Uiso 1 1 calc R . . H30C H 0.2263 1.0281 0.0596 0.071 Uiso 1 1 calc R . . C31 C 0.4344(5) 0.8289(3) 0.05483(14) 0.0271(13) Uiso 1 1 d . . . C32 C 0.8041(5) 0.2354(3) 0.21250(13) 0.0284(14) Uiso 1 1 d . . . C33 C 0.7711(5) 0.2226(3) 0.24140(13) 0.0311(14) Uiso 1 1 d . . . H33 H 0.7872 0.1772 0.2508 0.037 Uiso 1 1 calc R . . C34 C 0.7149(5) 0.2752(3) 0.25697(15) 0.0378(16) Uiso 1 1 d . . . H34 H 0.6925 0.2654 0.2767 0.045 Uiso 1 1 calc R . . C35 C 0.6917(5) 0.3418(3) 0.24364(14) 0.0373(15) Uiso 1 1 d . . . H35 H 0.6543 0.3781 0.2542 0.045 Uiso 1 1 calc R . . C36 C 0.7233(5) 0.3547(3) 0.21500(13) 0.0328(14) Uiso 1 1 d . . . H36 H 0.7069 0.4000 0.2056 0.039 Uiso 1 1 calc R . . C37 C 0.7785(5) 0.3027(3) 0.19980(12) 0.0245(13) Uiso 1 1 d . . . C38 C 0.9554(5) 0.4083(3) 0.16577(12) 0.0261(13) Uiso 1 1 d . . . C39 C 0.9787(5) 0.4774(3) 0.15657(13) 0.0334(15) Uiso 1 1 d . . . H39 H 1.0570 0.4952 0.1604 0.040 Uiso 1 1 calc R . . C40 C 0.8918(6) 0.5214(4) 0.14206(14) 0.0394(16) Uiso 1 1 d . . . H40 H 0.9114 0.5684 0.1359 0.047 Uiso 1 1 calc R . . C41 C 0.7787(6) 0.4979(3) 0.13656(14) 0.0375(15) Uiso 1 1 d . . . H41 H 0.7188 0.5282 0.1268 0.045 Uiso 1 1 calc R . . C42 C 0.7521(5) 0.4294(3) 0.14540(13) 0.0318(14) Uiso 1 1 d . . . H42 H 0.6735 0.4123 0.1413 0.038 Uiso 1 1 calc R . . C43 C 0.8385(5) 0.3852(3) 0.16017(13) 0.0267(13) Uiso 1 1 d . . . C44 C 0.7917(5) 0.2431(3) 0.12240(13) 0.0292(14) Uiso 1 1 d . . . C45 C 0.7208(5) 0.2073(3) 0.09921(14) 0.0373(15) Uiso 1 1 d . . . H45 H 0.7556 0.1852 0.0830 0.045 Uiso 1 1 calc R . . C46 C 0.6012(6) 0.2038(4) 0.09982(16) 0.0464(17) Uiso 1 1 d . . . H46 H 0.5539 0.1791 0.0839 0.056 Uiso 1 1 calc R . . C47 C 0.5478(6) 0.2356(4) 0.12312(15) 0.0452(17) Uiso 1 1 d . . . H47 H 0.4647 0.2329 0.1232 0.054 Uiso 1 1 calc R . . C48 C 0.6171(5) 0.2711(3) 0.14626(14) 0.0328(14) Uiso 1 1 d . . . H48 H 0.5822 0.2927 0.1626 0.039 Uiso 1 1 calc R . . C49 C 0.7357(5) 0.2750(3) 0.14537(12) 0.0254(13) Uiso 1 1 d . . . C50 C 0.8592(5) 0.1168(3) 0.19782(13) 0.0296(14) Uiso 1 1 d . . . C51 C 0.8977(5) 0.0726(3) 0.17206(14) 0.0361(15) Uiso 1 1 d . . . H51 H 0.9443 0.1038 0.1594 0.043 Uiso 1 1 calc R . . C52 C 0.7876(7) 0.0477(4) 0.15240(18) 0.061(2) Uiso 1 1 d . . . H52A H 0.7421 0.0161 0.1645 0.092 Uiso 1 1 calc R . . H52B H 0.8098 0.0214 0.1346 0.092 Uiso 1 1 calc R . . H52C H 0.7395 0.0893 0.1454 0.092 Uiso 1 1 calc R . . C53 C 0.9731(7) 0.0107(4) 0.18392(18) 0.060(2) Uiso 1 1 d . . . H53A H 1.0412 0.0285 0.1975 0.090 Uiso 1 1 calc R . . H53B H 1.0007 -0.0151 0.1667 0.090 Uiso 1 1 calc R . . H53C H 0.9269 -0.0218 0.1954 0.090 Uiso 1 1 calc R . . C54 C 1.1380(5) 0.3839(3) 0.19502(13) 0.0292(14) Uiso 1 1 d . . . C55 C 1.2370(5) 0.3322(3) 0.20295(14) 0.0363(15) Uiso 1 1 d . . . H55 H 1.2036 0.2826 0.2032 0.044 Uiso 1 1 calc R . . C56 C 1.3187(6) 0.3364(4) 0.17804(16) 0.0487(18) Uiso 1 1 d . . . H56A H 1.2747 0.3242 0.1582 0.073 Uiso 1 1 calc R . . H56B H 1.3840 0.3025 0.1827 0.073 Uiso 1 1 calc R . . H56C H 1.3502 0.3851 0.1772 0.073 Uiso 1 1 calc R . . C57 C 1.3032(6) 0.3483(4) 0.23463(15) 0.0483(18) Uiso 1 1 d . . . H57A H 1.3351 0.3971 0.2348 0.072 Uiso 1 1 calc R . . H57B H 1.3681 0.3140 0.2391 0.072 Uiso 1 1 calc R . . H57C H 1.2489 0.3440 0.2502 0.072 Uiso 1 1 calc R . . C58 C 0.9724(5) 0.2471(3) 0.10088(14) 0.0313(14) Uiso 1 1 d . . . C59 C 1.1051(5) 0.2488(3) 0.10696(15) 0.0379(15) Uiso 1 1 d . . . H59 H 1.1270 0.2566 0.1294 0.045 Uiso 1 1 calc R . . C60 C 1.1552(8) 0.3095(5) 0.0902(2) 0.080(3) Uiso 1 1 d . . . H60A H 1.1339 0.3034 0.0681 0.121 Uiso 1 1 calc R . . H60B H 1.2413 0.3098 0.0948 0.121 Uiso 1 1 calc R . . H60C H 1.1232 0.3550 0.0968 0.121 Uiso 1 1 calc R . . C61 C 1.1556(8) 0.1779(5) 0.0987(2) 0.082(3) Uiso 1 1 d . . . H61A H 1.1198 0.1394 0.1097 0.123 Uiso 1 1 calc R . . H61B H 1.2411 0.1780 0.1045 0.123 Uiso 1 1 calc R . . H61C H 1.1386 0.1700 0.0766 0.123 Uiso 1 1 calc R . . C62 C 1.1112(5) 0.1860(3) 0.17893(13) 0.0289(14) Uiso 1 1 d . . . C1S C 0.6622(6) 1.0125(4) 0.02150(17) 0.0544(19) Uiso 1 1 d . . . H1S1 H 0.6833 1.0437 0.0047 0.065 Uiso 1 1 calc R . . H1S2 H 0.6071 0.9755 0.0122 0.065 Uiso 1 1 calc R . . C2S C 0.5981(8) 1.0574(5) 0.0428(2) 0.072(2) Uiso 1 1 d . . . H2S1 H 0.5741 1.0271 0.0592 0.109 Uiso 1 1 calc R . . H2S2 H 0.5280 1.0789 0.0313 0.109 Uiso 1 1 calc R . . H2S3 H 0.6505 1.0955 0.0517 0.109 Uiso 1 1 calc R . . C3S C 0.7393(7) 0.9212(4) 0.05880(17) 0.057(2) Uiso 1 1 d . . . H3S1 H 0.7038 0.9472 0.0751 0.068 Uiso 1 1 calc R . . H3S2 H 0.6777 0.8894 0.0484 0.068 Uiso 1 1 calc R . . C4S C 0.8358(7) 0.8759(4) 0.07348(19) 0.066(2) Uiso 1 1 d . . . H4S1 H 0.8696 0.8478 0.0578 0.099 Uiso 1 1 calc R . . H4S2 H 0.8047 0.8434 0.0881 0.099 Uiso 1 1 calc R . . H4S3 H 0.8970 0.9064 0.0843 0.099 Uiso 1 1 calc R . . C5S C 0.8310(6) 0.9405(3) 0.01053(15) 0.0403(16) Uiso 1 1 d . . . H5S1 H 0.8453 0.9778 -0.0047 0.048 Uiso 1 1 calc R . . H5S2 H 0.9089 0.9221 0.0194 0.048 Uiso 1 1 calc R . . C6S C 0.7644(7) 0.8804(4) -0.00602(17) 0.0546(19) Uiso 1 1 d . . . H6S1 H 0.7551 0.8412 0.0084 0.082 Uiso 1 1 calc R . . H6S2 H 0.8080 0.8631 -0.0225 0.082 Uiso 1 1 calc R . . H6S3 H 0.6864 0.8975 -0.0148 0.082 Uiso 1 1 calc R . . C7S C 0.8577(6) 1.0276(4) 0.05229(15) 0.0449(17) Uiso 1 1 d . . . H7S1 H 0.9311 1.0015 0.0597 0.054 Uiso 1 1 calc R . . H7S2 H 0.8232 1.0455 0.0705 0.054 Uiso 1 1 calc R . . C8S C 0.8896(7) 1.0908(4) 0.03382(17) 0.057(2) Uiso 1 1 d . . . H8S1 H 0.9343 1.0744 0.0174 0.085 Uiso 1 1 calc R . . H8S2 H 0.9379 1.1243 0.0471 0.085 Uiso 1 1 calc R . . H8S3 H 0.8175 1.1150 0.0249 0.085 Uiso 1 1 calc R . . C9S C 0.5551(6) -0.0415(3) 0.22198(15) 0.0424(16) Uiso 1 1 d . . . H9S1 H 0.5449 -0.0535 0.1999 0.051 Uiso 1 1 calc R . . H9S2 H 0.6403 -0.0335 0.2281 0.051 Uiso 1 1 calc R . . C10S C 0.5172(6) -0.1041(4) 0.23926(15) 0.0450(17) Uiso 1 1 d . . . H10A H 0.5228 -0.0922 0.2611 0.068 Uiso 1 1 calc R . . H10B H 0.5684 -0.1451 0.2363 0.068 Uiso 1 1 calc R . . H10C H 0.4354 -0.1163 0.2317 0.068 Uiso 1 1 calc R . . C11S C 0.3605(5) 0.0180(4) 0.21846(14) 0.0387(16) Uiso 1 1 d . . . H11A H 0.3209 0.0643 0.2213 0.046 Uiso 1 1 calc R . . H11B H 0.3319 -0.0168 0.2329 0.046 Uiso 1 1 calc R . . C12S C 0.3255(7) -0.0080(4) 0.18626(17) 0.057(2) Uiso 1 1 d . . . H12A H 0.3549 0.0256 0.1717 0.085 Uiso 1 1 calc R . . H12B H 0.2393 -0.0109 0.1824 0.085 Uiso 1 1 calc R . . H12C H 0.3596 -0.0555 0.1837 0.085 Uiso 1 1 calc R . . C13S C 0.5090(5) 0.0504(4) 0.25964(14) 0.0389(16) Uiso 1 1 d . . . H13A H 0.4723 0.0981 0.2614 0.047 Uiso 1 1 calc R . . H13B H 0.4668 0.0163 0.2717 0.047 Uiso 1 1 calc R . . C14S C 0.6343(6) 0.0546(4) 0.27359(17) 0.0542(19) Uiso 1 1 d . . . H14A H 0.6671 0.0061 0.2761 0.081 Uiso 1 1 calc R . . H14B H 0.6382 0.0780 0.2937 0.081 Uiso 1 1 calc R . . H14C H 0.6801 0.0824 0.2602 0.081 Uiso 1 1 calc R . . C15S C 0.5398(6) 0.0835(4) 0.20611(16) 0.0456(17) Uiso 1 1 d . . . H15A H 0.6257 0.0876 0.2123 0.055 Uiso 1 1 calc R . . H15B H 0.5287 0.0660 0.1847 0.055 Uiso 1 1 calc R . . C16S C 0.4874(7) 0.1563(4) 0.20674(19) 0.064(2) Uiso 1 1 d . . . H16A H 0.4021 0.1534 0.2007 0.096 Uiso 1 1 calc R . . H16B H 0.5231 0.1876 0.1924 0.096 Uiso 1 1 calc R . . H16C H 0.5023 0.1760 0.2275 0.096 Uiso 1 1 calc R . . C17S C 0.4165(6) 0.6366(4) 0.23724(16) 0.0475(18) Uiso 1 1 d . . . H17A H 0.3480 0.6136 0.2452 0.057 Uiso 1 1 calc R . . H17B H 0.4887 0.6194 0.2498 0.057 Uiso 1 1 calc R . . C18S C 0.4075(6) 0.7165(4) 0.24105(17) 0.0514(19) Uiso 1 1 d . . . H18A H 0.4777 0.7396 0.2346 0.077 Uiso 1 1 calc R . . H18B H 0.4018 0.7278 0.2626 0.077 Uiso 1 1 calc R . . H18C H 0.3370 0.7342 0.2284 0.077 Uiso 1 1 calc R . . C19S C 0.3212(5) 0.6434(4) 0.18313(15) 0.0405(16) Uiso 1 1 d . . . H19A H 0.3246 0.6236 0.1623 0.049 Uiso 1 1 calc R . . H19B H 0.3319 0.6960 0.1820 0.049 Uiso 1 1 calc R . . C20S C 0.2019(6) 0.6282(4) 0.19274(17) 0.0531(19) Uiso 1 1 d . . . H20A H 0.1920 0.5763 0.1949 0.080 Uiso 1 1 calc R . . H20B H 0.1408 0.6466 0.1772 0.080 Uiso 1 1 calc R . . H20C H 0.1949 0.6516 0.2124 0.080 Uiso 1 1 calc R . . C21S C 0.4157(6) 0.5323(4) 0.20293(16) 0.0454(17) Uiso 1 1 d . . . H21D H 0.3453 0.5161 0.2122 0.054 Uiso 1 1 calc R . . H21E H 0.4052 0.5175 0.1811 0.054 Uiso 1 1 calc R . . C22S C 0.5212(7) 0.4949(4) 0.21861(18) 0.061(2) Uiso 1 1 d . . . H22D H 0.5910 0.5082 0.2089 0.091 Uiso 1 1 calc R . . H22E H 0.5093 0.4429 0.2170 0.091 Uiso 1 1 calc R . . H22F H 0.5326 0.5088 0.2403 0.091 Uiso 1 1 calc R . . C23S C 0.5339(6) 0.6408(4) 0.19414(15) 0.0411(16) Uiso 1 1 d . . . H23A H 0.6007 0.6241 0.2088 0.049 Uiso 1 1 calc R . . H23B H 0.5327 0.6938 0.1951 0.049 Uiso 1 1 calc R . . C24S C 0.5561(8) 0.6183(5) 0.16189(19) 0.071(2) Uiso 1 1 d . . . H24A H 0.5437 0.5665 0.1595 0.106 Uiso 1 1 calc R . . H24B H 0.6374 0.6301 0.1587 0.106 Uiso 1 1 calc R . . H24C H 0.5013 0.6437 0.1468 0.106 Uiso 1 1 calc R . . C25S C 0.6927(8) 0.3417(4) 0.00654(19) 0.067(2) Uiso 1 1 d . . . H25D H 0.6121 0.3501 -0.0039 0.080 Uiso 1 1 calc R . . H25E H 0.7481 0.3474 -0.0090 0.080 Uiso 1 1 calc R . . C26S C 0.6995(8) 0.2666(4) 0.0174(2) 0.069(2) Uiso 1 1 d . . . H26D H 0.7750 0.2588 0.0301 0.104 Uiso 1 1 calc R . . H26E H 0.6935 0.2342 -0.0003 0.104 Uiso 1 1 calc R . . H26F H 0.6346 0.2571 0.0296 0.104 Uiso 1 1 calc R . . C27S C 0.6636(9) 0.3865(6) 0.0591(2) 0.090(3) Uiso 1 1 d . . . H27A H 0.6863 0.4257 0.0738 0.108 Uiso 1 1 calc R . . H27B H 0.6958 0.3413 0.0684 0.108 Uiso 1 1 calc R . . C28S C 0.5295(9) 0.3812(6) 0.0544(2) 0.092(3) Uiso 1 1 d . . . H28A H 0.4969 0.4220 0.0422 0.139 Uiso 1 1 calc R . . H28B H 0.4992 0.3817 0.0744 0.139 Uiso 1 1 calc R . . H28C H 0.5061 0.3364 0.0437 0.139 Uiso 1 1 calc R . . C29S C 0.6842(9) 0.4699(5) 0.0162(2) 0.089(3) Uiso 1 1 d . . . H29D H 0.5983 0.4679 0.0097 0.107 Uiso 1 1 calc R . . H29E H 0.6970 0.5072 0.0323 0.107 Uiso 1 1 calc R . . C30S C 0.7411(8) 0.4944(5) -0.0099(2) 0.083(3) Uiso 1 1 d . . . H30D H 0.8265 0.4972 -0.0041 0.125 Uiso 1 1 calc R . . H30E H 0.7107 0.5418 -0.0163 0.125 Uiso 1 1 calc R . . H30F H 0.7242 0.4605 -0.0269 0.125 Uiso 1 1 calc R . . C31S C 0.8523(7) 0.3973(5) 0.0393(2) 0.068(2) Uiso 1 1 d . . . H31A H 0.8732 0.3497 0.0483 0.082 Uiso 1 1 calc R . . H31B H 0.8909 0.4016 0.0203 0.082 Uiso 1 1 calc R . . C32S C 0.9017(8) 0.4531(5) 0.0611(2) 0.081(3) Uiso 1 1 d . . . H32A H 0.8769 0.5005 0.0533 0.121 Uiso 1 1 calc R . . H32B H 0.9880 0.4502 0.0636 0.121 Uiso 1 1 calc R . . H32C H 0.8728 0.4454 0.0811 0.121 Uiso 1 1 calc R . . N1 N 0.4295(4) 0.6639(3) 0.07670(11) 0.0282(11) Uani 1 1 d . . . N2 N 0.3488(4) 0.7820(2) 0.12480(10) 0.0238(11) Uani 1 1 d . . . N3 N 0.1886(4) 0.8172(2) 0.06338(10) 0.0264(11) Uani 1 1 d . . . N4 N 0.2055(4) 0.6920(2) 0.08945(10) 0.0263(11) Uani 1 1 d . . . N5 N 0.4667(5) 0.8649(3) 0.03778(13) 0.0469(15) Uani 1 1 d . . . N6 N 0.8619(4) 0.1888(2) 0.19380(10) 0.0263(11) Uani 1 1 d . . . N7 N 1.0389(4) 0.3582(2) 0.17821(10) 0.0249(11) Uani 1 1 d . . . N8 N 0.9147(4) 0.2457(2) 0.12584(10) 0.0264(11) Uani 1 1 d . . . N9 N 0.8119(4) 0.3131(2) 0.16900(10) 0.0243(11) Uani 1 1 d . . . N10 N 1.1803(5) 0.1481(3) 0.18537(15) 0.0549(16) Uani 1 1 d . . . N1S N 0.7729(4) 0.9755(3) 0.03573(11) 0.0349(12) Uani 1 1 d . . . N2S N 0.4909(4) 0.0275(3) 0.22632(11) 0.0318(12) Uani 1 1 d . . . N3S N 0.4206(4) 0.6126(3) 0.20431(11) 0.0311(12) Uani 1 1 d . . . N4S N 0.7198(5) 0.3999(3) 0.03068(12) 0.0445(14) Uani 1 1 d . . . Ni1 Ni 0.34236(6) 0.76199(4) 0.079274(16) 0.0260(2) Uani 1 1 d . . . Ni2 Ni 0.97295(6) 0.25362(4) 0.171010(16) 0.0242(2) Uani 1 1 d . . . O1 O 0.5211(4) 0.5880(2) 0.04532(10) 0.0417(11) Uani 1 1 d . . . O2 O 0.4380(4) 0.8085(2) 0.17333(9) 0.0438(11) Uani 1 1 d . . . O3 O 0.0906(4) 0.9157(2) 0.04211(10) 0.0452(12) Uani 1 1 d . . . O4 O 0.8228(4) 0.0858(2) 0.21983(10) 0.0389(11) Uani 1 1 d . . . O5 O 1.1533(3) 0.4467(2) 0.20356(10) 0.0376(10) Uani 1 1 d . . . O6 O 0.9267(4) 0.2478(3) 0.07399(9) 0.0478(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 N1 0.016(2) 0.035(3) 0.034(3) 0.000(2) 0.006(2) 0.001(2) N2 0.023(3) 0.022(3) 0.026(3) -0.003(2) 0.006(2) -0.002(2) N3 0.021(3) 0.026(3) 0.031(3) 0.002(2) -0.004(2) 0.002(2) N4 0.021(3) 0.026(3) 0.031(3) 0.001(2) 0.001(2) 0.000(2) N5 0.035(3) 0.055(4) 0.049(4) -0.003(3) -0.002(3) 0.003(3) N6 0.023(3) 0.024(3) 0.032(3) -0.003(2) 0.004(2) -0.002(2) N7 0.019(3) 0.026(3) 0.030(3) -0.003(2) 0.006(2) 0.000(2) N8 0.022(3) 0.026(3) 0.031(3) -0.005(2) 0.003(2) 0.000(2) N9 0.019(2) 0.030(3) 0.024(3) -0.002(2) -0.001(2) 0.001(2) N10 0.044(4) 0.034(3) 0.085(5) -0.008(3) 0.001(3) -0.001(3) N1S 0.026(3) 0.043(3) 0.036(3) 0.001(2) 0.003(2) 0.002(2) N2S 0.027(3) 0.040(3) 0.030(3) 0.002(2) 0.006(2) 0.002(2) N3S 0.030(3) 0.029(3) 0.034(3) 0.000(2) 0.002(2) 0.001(2) N4S 0.057(4) 0.042(3) 0.034(3) -0.008(3) 0.005(3) 0.009(3) Ni1 0.0278(4) 0.0235(4) 0.0270(4) 0.0001(3) 0.0043(3) -0.0020(3) Ni2 0.0200(4) 0.0235(4) 0.0291(4) -0.0019(3) 0.0025(3) 0.0018(3) O1 0.039(3) 0.036(3) 0.053(3) -0.014(2) 0.017(2) -0.001(2) O2 0.043(3) 0.055(3) 0.032(3) -0.006(2) 0.000(2) -0.009(2) O3 0.043(3) 0.041(3) 0.046(3) 0.003(2) -0.017(2) 0.007(2) O4 0.036(2) 0.031(2) 0.051(3) 0.005(2) 0.008(2) -0.002(2) O5 0.031(2) 0.027(2) 0.054(3) -0.007(2) 0.003(2) -0.0032(19) O6 0.044(3) 0.073(3) 0.027(2) -0.003(2) 0.003(2) -0.002(2) _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 C1 C6 1.384(8) . ? C1 N1 1.393(7) . ? C1 C2 1.414(8) . ? C2 C3 1.361(9) . ? C2 H2 0.9500 . ? C3 C4 1.370(9) . ? C3 H3 0.9500 . ? C4 C5 1.380(9) . ? C4 H4 0.9500 . ? C5 C6 1.383(8) . ? C5 H5 0.9500 . ? C6 N4 1.450(7) . ? C7 N2 1.385(7) . ? C7 C12 1.399(8) . ? C7 C8 1.400(8) . ? C8 C9 1.378(9) . ? C8 H8 0.9500 . ? C9 C10 1.353(9) . ? C9 H9 0.9500 . ? C10 C11 1.383(9) . ? C10 H10 0.9500 . ? C11 C12 1.368(8) . ? C11 H11 0.9500 . ? C12 N4 1.470(7) . ? C13 C14 1.366(8) . ? C13 C18 1.421(8) . ? C13 N4 1.446(7) . ? C14 C15 1.380(9) . ? C14 H14 0.9500 . ? C15 C16 1.363(9) . ? C15 H15 0.9500 . ? C16 C17 1.372(9) . ? C16 H16 0.9500 . ? C17 C18 1.390(9) . ? C17 H17 0.9500 . ? C18 N3 1.387(7) . ? C19 O1 1.241(7) . ? C19 N1 1.355(7) . ? C19 C20 1.507(9) . ? C20 C21 1.516(10) . ? C20 C22 1.526(9) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O2 1.253(7) . ? C23 N2 1.344(7) . ? C23 C24 1.505(9) . ? C24 C26 1.513(9) . ? C24 C25 1.532(9) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O3 1.238(7) . ? C27 N3 1.322(8) . ? C27 C28 1.521(9) . ? C28 C30 1.512(9) . ? C28 C29 1.524(9) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N5 1.102(7) . ? C31 Ni1 2.018(6) . ? C32 C33 1.385(8) . ? C32 C37 1.391(8) . ? C32 N6 1.410(7) . ? C33 C34 1.395(8) . ? C33 H33 0.9500 . ? C34 C35 1.386(9) . ? C34 H34 0.9500 . ? C35 C36 1.370(8) . ? C35 H35 0.9500 . ? C36 C37 1.371(8) . ? C36 H36 0.9500 . ? C37 N9 1.461(7) . ? C38 C39 1.386(8) . ? C38 C43 1.396(8) . ? C38 N7 1.400(7) . ? C39 C40 1.384(9) . ? C39 H39 0.9500 . ? C40 C41 1.358(9) . ? C40 H40 0.9500 . ? C41 C42 1.380(9) . ? C41 H41 0.9500 . ? C42 C43 1.387(8) . ? C42 H42 0.9500 . ? C43 N9 1.443(7) . ? C44 C49 1.389(8) . ? C44 C45 1.395(8) . ? C44 N8 1.396(7) . ? C45 C46 1.370(9) . ? C45 H45 0.9500 . ? C46 C47 1.384(9) . ? C46 H46 0.9500 . ? C47 C48 1.382(9) . ? C47 H47 0.9500 . ? C48 C49 1.361(8) . ? C48 H48 0.9500 . ? C49 N9 1.459(7) . ? C50 O4 1.239(7) . ? C50 N6 1.356(7) . ? C50 C51 1.506(8) . ? C51 C53 1.497(10) . ? C51 C52 1.513(10) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 O5 1.237(7) . ? C54 N7 1.364(7) . ? C54 C55 1.495(8) . ? C55 C56 1.520(9) . ? C55 C57 1.534(9) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 O6 1.234(7) . ? C58 N8 1.343(7) . ? C58 C59 1.507(9) . ? C59 C60 1.499(11) . ? C59 C61 1.503(11) . ? C59 H59 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 N10 1.072(7) . ? C62 Ni2 2.019(7) . ? C1S C2S 1.507(11) . ? C1S N1S 1.510(9) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S C4S 1.475(10) . ? C3S N1S 1.514(9) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C5S C6S 1.495(9) . ? C5S N1S 1.503(8) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? C7S N1S 1.498(8) . ? C7S C8S 1.500(10) . ? C7S H7S1 0.9900 . ? C7S H7S2 0.9900 . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? C9S C10S 1.485(9) . ? C9S N2S 1.503(8) . ? C9S H9S1 0.9900 . ? C9S H9S2 0.9900 . ? C10S H10A 0.9800 . ? C10S H10B 0.9800 . ? C10S H10C 0.9800 . ? C11S N2S 1.499(8) . ? C11S C12S 1.504(9) . ? C11S H11A 0.9900 . ? C11S H11B 0.9900 . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? C13S C14S 1.491(9) . ? C13S N2S 1.515(8) . ? C13S H13A 0.9900 . ? C13S H13B 0.9900 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? C15S C16S 1.485(10) . ? C15S N2S 1.519(8) . ? C15S H15A 0.9900 . ? C15S H15B 0.9900 . ? C16S H16A 0.9800 . ? C16S H16B 0.9800 . ? C16S H16C 0.9800 . ? C17S C18S 1.506(10) . ? C17S N3S 1.520(8) . ? C17S H17A 0.9900 . ? C17S H17B 0.9900 . ? C18S H18A 0.9800 . ? C18S H18B 0.9800 . ? C18S H18C 0.9800 . ? C19S N3S 1.495(8) . ? C19S C20S 1.499(9) . ? C19S H19A 0.9900 . ? C19S H19B 0.9900 . ? C20S H20A 0.9800 . ? C20S H20B 0.9800 . ? C20S H20C 0.9800 . ? C21S C22S 1.489(10) . ? C21S N3S 1.500(8) . ? C21S H21D 0.9900 . ? C21S H21E 0.9900 . ? C22S H22D 0.9800 . ? C22S H22E 0.9800 . ? C22S H22F 0.9800 . ? C23S N3S 1.511(8) . ? C23S C24S 1.527(10) . ? C23S H23A 0.9900 . ? C23S H23B 0.9900 . ? C24S H24A 0.9800 . ? C24S H24B 0.9800 . ? C24S H24C 0.9800 . ? C25S C26S 1.479(11) . ? C25S N4S 1.524(10) . ? C25S H25D 0.9900 . ? C25S H25E 0.9900 . ? C26S H26D 0.9800 . ? C26S H26E 0.9800 . ? C26S H26F 0.9800 . ? C27S N4S 1.487(11) . ? C27S C28S 1.524(13) . ? C27S H27A 0.9900 . ? C27S H27B 0.9900 . ? C28S H28A 0.9800 . ? C28S H28B 0.9800 . ? C28S H28C 0.9800 . ? C29S C30S 1.456(12) . ? C29S N4S 1.487(11) . ? C29S H29D 0.9900 . ? C29S H29E 0.9900 . ? C30S H30D 0.9800 . ? C30S H30E 0.9800 . ? C30S H30F 0.9800 . ? C31S C32S 1.482(12) . ? C31S N4S 1.517(10) . ? C31S H31A 0.9900 . ? C31S H31B 0.9900 . ? C32S H32A 0.9800 . ? C32S H32B 0.9800 . ? C32S H32C 0.9800 . ? N1 Ni1 2.091(5) . ? N2 Ni1 2.027(4) . ? N3 Ni1 2.083(4) . ? N4 Ni1 2.122(5) . ? N6 Ni2 2.089(5) . ? N7 Ni2 2.101(5) . ? N8 Ni2 2.023(5) . ? N9 Ni2 2.139(4) . ? 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 C6 C1 N1 119.4(5) . . ? C6 C1 C2 116.1(5) . . ? N1 C1 C2 124.2(5) . . ? C3 C2 C1 121.4(6) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 121.6(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 118.3(6) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 120.6(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 121.9(5) . . ? C5 C6 N4 121.1(5) . . ? C1 C6 N4 117.0(5) . . ? N2 C7 C12 116.4(5) . . ? N2 C7 C8 126.7(5) . . ? C12 C7 C8 116.7(5) . . ? C9 C8 C7 121.2(6) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.8(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 121.4(5) . . ? C11 C12 N4 120.8(5) . . ? C7 C12 N4 117.8(5) . . ? C14 C13 C18 121.8(5) . . ? C14 C13 N4 123.7(5) . . ? C18 C13 N4 114.5(5) . . ? C13 C14 C15 119.7(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.0(7) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.6(6) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 121.8(6) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? N3 C18 C17 129.4(6) . . ? N3 C18 C13 114.6(5) . . ? C17 C18 C13 116.0(5) . . ? O1 C19 N1 125.6(5) . . ? O1 C19 C20 118.1(5) . . ? N1 C19 C20 116.2(5) . . ? C19 C20 C21 106.6(5) . . ? C19 C20 C22 110.8(5) . . ? C21 C20 C22 111.1(6) . . ? C19 C20 H20 109.4 . . ? C21 C20 H20 109.4 . . ? C22 C20 H20 109.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 N2 125.3(5) . . ? O2 C23 C24 118.2(5) . . ? N2 C23 C24 116.5(5) . . ? C23 C24 C26 110.7(5) . . ? C23 C24 C25 109.2(5) . . ? C26 C24 C25 108.9(6) . . ? C23 C24 H24 109.4 . . ? C26 C24 H24 109.4 . . ? C25 C24 H24 109.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 N3 127.2(6) . . ? O3 C27 C28 117.2(5) . . ? N3 C27 C28 115.4(5) . . ? C30 C28 C27 112.8(5) . . ? C30 C28 C29 110.5(6) . . ? C27 C28 C29 108.6(5) . . ? C30 C28 H28 108.3 . . ? C27 C28 H28 108.3 . . ? C29 C28 H28 108.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 Ni1 167.2(5) . . ? C33 C32 C37 117.1(5) . . ? C33 C32 N6 128.5(5) . . ? C37 C32 N6 114.4(5) . . ? C32 C33 C34 121.1(6) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120.0(6) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 119.2(6) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.5(6) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 122.0(5) . . ? C36 C37 N9 122.8(5) . . ? C32 C37 N9 115.2(5) . . ? C39 C38 C43 116.5(5) . . ? C39 C38 N7 126.1(5) . . ? C43 C38 N7 117.2(5) . . ? C40 C39 C38 122.3(6) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C41 C40 C39 120.3(6) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 119.0(6) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C41 C42 C43 121.0(6) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C38 120.8(5) . . ? C42 C43 N9 121.3(5) . . ? C38 C43 N9 117.8(5) . . ? C49 C44 C45 117.3(5) . . ? C49 C44 N8 116.6(5) . . ? C45 C44 N8 125.9(5) . . ? C46 C45 C44 120.2(6) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 121.3(7) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 119.1(6) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C49 C48 C47 119.4(6) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C44 122.7(5) . . ? C48 C49 N9 121.2(5) . . ? C44 C49 N9 116.0(5) . . ? O4 C50 N6 125.4(5) . . ? O4 C50 C51 118.9(5) . . ? N6 C50 C51 115.6(5) . . ? C53 C51 C50 111.5(5) . . ? C53 C51 C52 111.5(6) . . ? C50 C51 C52 107.6(5) . . ? C53 C51 H51 108.7 . . ? C50 C51 H51 108.7 . . ? C52 C51 H51 108.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O5 C54 N7 125.1(5) . . ? O5 C54 C55 117.7(5) . . ? N7 C54 C55 117.1(5) . . ? C54 C55 C56 108.0(5) . . ? C54 C55 C57 111.4(5) . . ? C56 C55 C57 111.3(5) . . ? C54 C55 H55 108.7 . . ? C56 C55 H55 108.7 . . ? C57 C55 H55 108.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O6 C58 N8 126.0(5) . . ? O6 C58 C59 118.3(5) . . ? N8 C58 C59 115.7(5) . . ? C60 C59 C61 111.6(7) . . ? C60 C59 C58 111.2(6) . . ? C61 C59 C58 110.1(6) . . ? C60 C59 H59 107.9 . . ? C61 C59 H59 107.9 . . ? C58 C59 H59 107.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N10 C62 Ni2 173.6(6) . . ? C2S C1S N1S 116.1(6) . . ? C2S C1S H1S1 108.3 . . ? N1S C1S H1S1 108.3 . . ? C2S C1S H1S2 108.3 . . ? N1S C1S H1S2 108.3 . . ? H1S1 C1S H1S2 107.4 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C4S C3S N1S 116.2(6) . . ? C4S C3S H3S1 108.2 . . ? N1S C3S H3S1 108.2 . . ? C4S C3S H3S2 108.2 . . ? N1S C3S H3S2 108.2 . . ? H3S1 C3S H3S2 107.4 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C6S C5S N1S 116.2(5) . . ? C6S C5S H5S1 108.2 . . ? N1S C5S H5S1 108.2 . . ? C6S C5S H5S2 108.2 . . ? N1S C5S H5S2 108.2 . . ? H5S1 C5S H5S2 107.4 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N1S C7S C8S 115.5(6) . . ? N1S C7S H7S1 108.4 . . ? C8S C7S H7S1 108.4 . . ? N1S C7S H7S2 108.4 . . ? C8S C7S H7S2 108.4 . . ? H7S1 C7S H7S2 107.5 . . ? C7S C8S H8S1 109.5 . . ? C7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? C10S C9S N2S 115.7(5) . . ? C10S C9S H9S1 108.4 . . ? N2S C9S H9S1 108.4 . . ? C10S C9S H9S2 108.4 . . ? N2S C9S H9S2 108.4 . . ? H9S1 C9S H9S2 107.4 . . ? C9S C10S H10A 109.5 . . ? C9S C10S H10B 109.5 . . ? H10A C10S H10B 109.5 . . ? C9S C10S H10C 109.5 . . ? H10A C10S H10C 109.5 . . ? H10B C10S H10C 109.5 . . ? N2S C11S C12S 113.7(5) . . ? N2S C11S H11A 108.8 . . ? C12S C11S H11A 108.8 . . ? N2S C11S H11B 108.8 . . ? C12S C11S H11B 108.8 . . ? H11A C11S H11B 107.7 . . ? C11S C12S H12A 109.5 . . ? C11S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? C11S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? C14S C13S N2S 115.3(5) . . ? C14S C13S H13A 108.4 . . ? N2S C13S H13A 108.4 . . ? C14S C13S H13B 108.4 . . ? N2S C13S H13B 108.4 . . ? H13A C13S H13B 107.5 . . ? C13S C14S H14A 109.5 . . ? C13S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? C13S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? C16S C15S N2S 116.3(6) . . ? C16S C15S H15A 108.2 . . ? N2S C15S H15A 108.2 . . ? C16S C15S H15B 108.2 . . ? N2S C15S H15B 108.2 . . ? H15A C15S H15B 107.4 . . ? C15S C16S H16A 109.5 . . ? C15S C16S H16B 109.5 . . ? H16A C16S H16B 109.5 . . ? C15S C16S H16C 109.5 . . ? H16A C16S H16C 109.5 . . ? H16B C16S H16C 109.5 . . ? C18S C17S N3S 114.0(6) . . ? C18S C17S H17A 108.7 . . ? N3S C17S H17A 108.7 . . ? C18S C17S H17B 108.7 . . ? N3S C17S H17B 108.7 . . ? H17A C17S H17B 107.6 . . ? C17S C18S H18A 109.5 . . ? C17S C18S H18B 109.5 . . ? H18A C18S H18B 109.5 . . ? C17S C18S H18C 109.5 . . ? H18A C18S H18C 109.5 . . ? H18B C18S H18C 109.5 . . ? N3S C19S C20S 113.6(5) . . ? N3S C19S H19A 108.8 . . ? C20S C19S H19A 108.8 . . ? N3S C19S H19B 108.8 . . ? C20S C19S H19B 108.8 . . ? H19A C19S H19B 107.7 . . ? C19S C20S H20A 109.5 . . ? C19S C20S H20B 109.5 . . ? H20A C20S H20B 109.5 . . ? C19S C20S H20C 109.5 . . ? H20A C20S H20C 109.5 . . ? H20B C20S H20C 109.5 . . ? C22S C21S N3S 115.2(6) . . ? C22S C21S H21D 108.5 . . ? N3S C21S H21D 108.5 . . ? C22S C21S H21E 108.5 . . ? N3S C21S H21E 108.5 . . ? H21D C21S H21E 107.5 . . ? C21S C22S H22D 109.5 . . ? C21S C22S H22E 109.5 . . ? H22D C22S H22E 109.5 . . ? C21S C22S H22F 109.5 . . ? H22D C22S H22F 109.5 . . ? H22E C22S H22F 109.5 . . ? N3S C23S C24S 114.7(6) . . ? N3S C23S H23A 108.6 . . ? C24S C23S H23A 108.6 . . ? N3S C23S H23B 108.6 . . ? C24S C23S H23B 108.6 . . ? H23A C23S H23B 107.6 . . ? C23S C24S H24A 109.5 . . ? C23S C24S H24B 109.5 . . ? H24A C24S H24B 109.5 . . ? C23S C24S H24C 109.5 . . ? H24A C24S H24C 109.5 . . ? H24B C24S H24C 109.5 . . ? C26S C25S N4S 116.9(7) . . ? C26S C25S H25D 108.1 . . ? N4S C25S H25D 108.1 . . ? C26S C25S H25E 108.1 . . ? N4S C25S H25E 108.1 . . ? H25D C25S H25E 107.3 . . ? C25S C26S H26D 109.5 . . ? C25S C26S H26E 109.5 . . ? H26D C26S H26E 109.5 . . ? C25S C26S H26F 109.5 . . ? H26D C26S H26F 109.5 . . ? H26E C26S H26F 109.5 . . ? N4S C27S C28S 115.0(8) . . ? N4S C27S H27A 108.5 . . ? C28S C27S H27A 108.5 . . ? N4S C27S H27B 108.5 . . ? C28S C27S H27B 108.5 . . ? H27A C27S H27B 107.5 . . ? C27S C28S H28A 109.5 . . ? C27S C28S H28B 109.5 . . ? H28A C28S H28B 109.5 . . ? C27S C28S H28C 109.5 . . ? H28A C28S H28C 109.5 . . ? H28B C28S H28C 109.5 . . ? C30S C29S N4S 119.2(8) . . ? C30S C29S H29D 107.5 . . ? N4S C29S H29D 107.5 . . ? C30S C29S H29E 107.5 . . ? N4S C29S H29E 107.5 . . ? H29D C29S H29E 107.0 . . ? C29S C30S H30D 109.5 . . ? C29S C30S H30E 109.5 . . ? H30D C30S H30E 109.5 . . ? C29S C30S H30F 109.5 . . ? H30D C30S H30F 109.5 . . ? H30E C30S H30F 109.5 . . ? C32S C31S N4S 115.6(7) . . ? C32S C31S H31A 108.4 . . ? N4S C31S H31A 108.4 . . ? C32S C31S H31B 108.4 . . ? N4S C31S H31B 108.4 . . ? H31A C31S H31B 107.5 . . ? C31S C32S H32A 109.5 . . ? C31S C32S H32B 109.5 . . ? H32A C32S H32B 109.5 . . ? C31S C32S H32C 109.5 . . ? H32A C32S H32C 109.5 . . ? H32B C32S H32C 109.5 . . ? C19 N1 C1 117.1(5) . . ? C19 N1 Ni1 129.4(4) . . ? C1 N1 Ni1 111.2(3) . . ? C23 N2 C7 120.5(5) . . ? C23 N2 Ni1 129.8(4) . . ? C7 N2 Ni1 109.7(3) . . ? C27 N3 C18 122.4(5) . . ? C27 N3 Ni1 131.4(4) . . ? C18 N3 Ni1 104.1(4) . . ? C13 N4 C6 115.5(4) . . ? C13 N4 C12 113.2(4) . . ? C6 N4 C12 114.2(4) . . ? C13 N4 Ni1 100.9(3) . . ? C6 N4 Ni1 108.8(3) . . ? C12 N4 Ni1 102.3(3) . . ? C50 N6 C32 121.0(5) . . ? C50 N6 Ni2 131.3(4) . . ? C32 N6 Ni2 105.9(3) . . ? C54 N7 C38 117.4(5) . . ? C54 N7 Ni2 131.9(4) . . ? C38 N7 Ni2 110.2(3) . . ? C58 N8 C44 119.7(5) . . ? C58 N8 Ni2 131.5(4) . . ? C44 N8 Ni2 108.7(3) . . ? C43 N9 C49 113.0(4) . . ? C43 N9 C37 117.3(4) . . ? C49 N9 C37 113.3(4) . . ? C43 N9 Ni2 106.8(3) . . ? C49 N9 Ni2 102.4(3) . . ? C37 N9 Ni2 102.1(3) . . ? C7S N1S C5S 108.9(5) . . ? C7S N1S C1S 111.5(5) . . ? C5S N1S C1S 108.2(5) . . ? C7S N1S C3S 108.0(5) . . ? C5S N1S C3S 111.7(5) . . ? C1S N1S C3S 108.6(5) . . ? C11S N2S C9S 110.8(5) . . ? C11S N2S C13S 106.0(4) . . ? C9S N2S C13S 110.5(5) . . ? C11S N2S C15S 111.6(5) . . ? C9S N2S C15S 107.3(5) . . ? C13S N2S C15S 110.6(5) . . ? C19S N3S C21S 109.7(5) . . ? C19S N3S C23S 107.2(5) . . ? C21S N3S C23S 111.4(5) . . ? C19S N3S C17S 112.0(5) . . ? C21S N3S C17S 109.1(5) . . ? C23S N3S C17S 107.5(5) . . ? C29S N4S C27S 112.5(7) . . ? C29S N4S C31S 110.4(6) . . ? C27S N4S C31S 107.4(6) . . ? C29S N4S C25S 107.8(6) . . ? C27S N4S C25S 113.0(6) . . ? C31S N4S C25S 105.4(6) . . ? C31 Ni1 N2 116.7(2) . . ? C31 Ni1 N3 89.2(2) . . ? N2 Ni1 N3 99.91(18) . . ? C31 Ni1 N1 103.4(2) . . ? N2 Ni1 N1 104.56(18) . . ? N3 Ni1 N1 143.25(18) . . ? C31 Ni1 N4 158.9(2) . . ? N2 Ni1 N4 81.29(18) . . ? N3 Ni1 N4 76.29(18) . . ? N1 Ni1 N4 80.77(18) . . ? C62 Ni2 N8 106.5(2) . . ? C62 Ni2 N6 93.5(2) . . ? N8 Ni2 N6 106.21(18) . . ? C62 Ni2 N7 107.2(2) . . ? N8 Ni2 N7 106.65(18) . . ? N6 Ni2 N7 133.76(17) . . ? C62 Ni2 N9 169.0(2) . . ? N8 Ni2 N9 79.34(17) . . ? N6 Ni2 N9 75.74(18) . . ? N7 Ni2 N9 79.40(17) . . ? 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 C6 C1 C2 C3 0.1(9) . . . . ? N1 C1 C2 C3 173.5(6) . . . . ? C1 C2 C3 C4 -1.0(10) . . . . ? C2 C3 C4 C5 1.1(10) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? C4 C5 C6 C1 -0.5(9) . . . . ? C4 C5 C6 N4 179.6(5) . . . . ? N1 C1 C6 C5 -173.2(5) . . . . ? C2 C1 C6 C5 0.6(8) . . . . ? N1 C1 C6 N4 6.7(8) . . . . ? C2 C1 C6 N4 -179.5(5) . . . . ? N2 C7 C8 C9 171.7(6) . . . . ? C12 C7 C8 C9 -2.8(9) . . . . ? C7 C8 C9 C10 1.4(10) . . . . ? C8 C9 C10 C11 0.2(10) . . . . ? C9 C10 C11 C12 -0.2(9) . . . . ? C10 C11 C12 C7 -1.4(9) . . . . ? C10 C11 C12 N4 -179.5(5) . . . . ? N2 C7 C12 C11 -172.3(5) . . . . ? C8 C7 C12 C11 2.8(8) . . . . ? N2 C7 C12 N4 5.9(8) . . . . ? C8 C7 C12 N4 -179.0(5) . . . . ? C18 C13 C14 C15 -1.3(9) . . . . ? N4 C13 C14 C15 177.9(6) . . . . ? C13 C14 C15 C16 1.8(10) . . . . ? C14 C15 C16 C17 -1.0(10) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? C16 C17 C18 N3 -180.0(6) . . . . ? C16 C17 C18 C13 0.8(9) . . . . ? C14 C13 C18 N3 -179.3(5) . . . . ? N4 C13 C18 N3 1.4(7) . . . . ? C14 C13 C18 C17 0.0(9) . . . . ? N4 C13 C18 C17 -179.2(5) . . . . ? O1 C19 C20 C21 -75.7(7) . . . . ? N1 C19 C20 C21 100.5(6) . . . . ? O1 C19 C20 C22 45.4(8) . . . . ? N1 C19 C20 C22 -138.5(6) . . . . ? O2 C23 C24 C26 35.1(8) . . . . ? N2 C23 C24 C26 -147.4(6) . . . . ? O2 C23 C24 C25 -84.8(7) . . . . ? N2 C23 C24 C25 92.7(7) . . . . ? O3 C27 C28 C30 -52.1(8) . . . . ? N3 C27 C28 C30 132.9(6) . . . . ? O3 C27 C28 C29 70.7(7) . . . . ? N3 C27 C28 C29 -104.4(6) . . . . ? C37 C32 C33 C34 -0.1(8) . . . . ? N6 C32 C33 C34 179.5(6) . . . . ? C32 C33 C34 C35 -0.4(9) . . . . ? C33 C34 C35 C36 0.8(9) . . . . ? C34 C35 C36 C37 -0.7(9) . . . . ? C35 C36 C37 C32 0.2(9) . . . . ? C35 C36 C37 N9 178.7(5) . . . . ? C33 C32 C37 C36 0.2(8) . . . . ? N6 C32 C37 C36 -179.5(5) . . . . ? C33 C32 C37 N9 -178.4(5) . . . . ? N6 C32 C37 N9 1.9(7) . . . . ? C43 C38 C39 C40 -1.1(9) . . . . ? N7 C38 C39 C40 174.3(6) . . . . ? C38 C39 C40 C41 0.6(10) . . . . ? C39 C40 C41 C42 -0.6(9) . . . . ? C40 C41 C42 C43 1.1(9) . . . . ? C41 C42 C43 C38 -1.7(9) . . . . ? C41 C42 C43 N9 -178.9(5) . . . . ? C39 C38 C43 C42 1.6(8) . . . . ? N7 C38 C43 C42 -174.3(5) . . . . ? C39 C38 C43 N9 178.9(5) . . . . ? N7 C38 C43 N9 3.0(7) . . . . ? C49 C44 C45 C46 -0.7(9) . . . . ? N8 C44 C45 C46 174.6(6) . . . . ? C44 C45 C46 C47 0.2(10) . . . . ? C45 C46 C47 C48 -0.3(10) . . . . ? C46 C47 C48 C49 0.9(9) . . . . ? C47 C48 C49 C44 -1.5(9) . . . . ? C47 C48 C49 N9 178.9(5) . . . . ? C45 C44 C49 C48 1.4(9) . . . . ? N8 C44 C49 C48 -174.3(5) . . . . ? C45 C44 C49 N9 -179.0(5) . . . . ? N8 C44 C49 N9 5.3(7) . . . . ? O4 C50 C51 C53 -44.8(8) . . . . ? N6 C50 C51 C53 138.7(6) . . . . ? O4 C50 C51 C52 77.8(7) . . . . ? N6 C50 C51 C52 -98.7(6) . . . . ? O5 C54 C55 C56 -86.5(7) . . . . ? N7 C54 C55 C56 91.8(6) . . . . ? O5 C54 C55 C57 36.0(8) . . . . ? N7 C54 C55 C57 -145.6(5) . . . . ? O6 C58 C59 C60 52.0(8) . . . . ? N8 C58 C59 C60 -127.4(6) . . . . ? O6 C58 C59 C61 -72.2(8) . . . . ? N8 C58 C59 C61 108.4(7) . . . . ? O1 C19 N1 C1 23.5(9) . . . . ? C20 C19 N1 C1 -152.3(5) . . . . ? O1 C19 N1 Ni1 -137.5(5) . . . . ? C20 C19 N1 Ni1 46.7(7) . . . . ? C6 C1 N1 C19 -157.8(5) . . . . ? C2 C1 N1 C19 29.0(8) . . . . ? C6 C1 N1 Ni1 6.6(6) . . . . ? C2 C1 N1 Ni1 -166.6(5) . . . . ? O2 C23 N2 C7 8.3(9) . . . . ? C24 C23 N2 C7 -169.1(5) . . . . ? O2 C23 N2 Ni1 -173.3(4) . . . . ? C24 C23 N2 Ni1 9.4(8) . . . . ? C12 C7 N2 C23 -159.8(5) . . . . ? C8 C7 N2 C23 25.6(9) . . . . ? C12 C7 N2 Ni1 21.5(6) . . . . ? C8 C7 N2 Ni1 -153.1(5) . . . . ? O3 C27 N3 C18 -8.0(10) . . . . ? C28 C27 N3 C18 166.4(5) . . . . ? O3 C27 N3 Ni1 153.0(5) . . . . ? C28 C27 N3 Ni1 -32.5(8) . . . . ? C17 C18 N3 C27 23.1(10) . . . . ? C13 C18 N3 C27 -157.7(5) . . . . ? C17 C18 N3 Ni1 -142.4(6) . . . . ? C13 C18 N3 Ni1 36.9(6) . . . . ? C14 C13 N4 C6 26.1(8) . . . . ? C18 C13 N4 C6 -154.7(5) . . . . ? C14 C13 N4 C12 -108.2(6) . . . . ? C18 C13 N4 C12 71.0(6) . . . . ? C14 C13 N4 Ni1 143.2(5) . . . . ? C18 C13 N4 Ni1 -37.5(5) . . . . ? C5 C6 N4 C13 -83.6(7) . . . . ? C1 C6 N4 C13 96.5(6) . . . . ? C5 C6 N4 C12 50.3(7) . . . . ? C1 C6 N4 C12 -129.7(5) . . . . ? C5 C6 N4 Ni1 163.9(4) . . . . ? C1 C6 N4 Ni1 -16.0(6) . . . . ? C11 C12 N4 C13 42.8(7) . . . . ? C7 C12 N4 C13 -135.4(5) . . . . ? C11 C12 N4 C6 -92.1(6) . . . . ? C7 C12 N4 C6 89.7(6) . . . . ? C11 C12 N4 Ni1 150.5(5) . . . . ? C7 C12 N4 Ni1 -27.7(6) . . . . ? O4 C50 N6 C32 -10.6(9) . . . . ? C51 C50 N6 C32 165.6(5) . . . . ? O4 C50 N6 Ni2 151.7(5) . . . . ? C51 C50 N6 Ni2 -32.1(7) . . . . ? C33 C32 N6 C50 21.8(9) . . . . ? C37 C32 N6 C50 -158.6(5) . . . . ? C33 C32 N6 Ni2 -144.4(5) . . . . ? C37 C32 N6 Ni2 35.1(5) . . . . ? O5 C54 N7 C38 10.1(8) . . . . ? C55 C54 N7 C38 -168.2(5) . . . . ? O5 C54 N7 Ni2 -161.2(4) . . . . ? C55 C54 N7 Ni2 20.6(8) . . . . ? C39 C38 N7 C54 30.7(8) . . . . ? C43 C38 N7 C54 -153.8(5) . . . . ? C39 C38 N7 Ni2 -156.2(5) . . . . ? C43 C38 N7 Ni2 19.2(6) . . . . ? O6 C58 N8 C44 1.6(9) . . . . ? C59 C58 N8 C44 -179.1(5) . . . . ? O6 C58 N8 Ni2 -173.4(5) . . . . ? C59 C58 N8 Ni2 5.9(8) . . . . ? C49 C44 N8 C58 -150.0(5) . . . . ? C45 C44 N8 C58 34.7(8) . . . . ? C49 C44 N8 Ni2 26.1(6) . . . . ? C45 C44 N8 Ni2 -149.3(5) . . . . ? C42 C43 N9 C49 42.7(7) . . . . ? C38 C43 N9 C49 -134.6(5) . . . . ? C42 C43 N9 C37 -91.9(6) . . . . ? C38 C43 N9 C37 90.8(6) . . . . ? C42 C43 N9 Ni2 154.5(5) . . . . ? C38 C43 N9 Ni2 -22.8(6) . . . . ? C48 C49 N9 C43 -97.0(6) . . . . ? C44 C49 N9 C43 83.4(6) . . . . ? C48 C49 N9 C37 39.4(7) . . . . ? C44 C49 N9 C37 -140.2(5) . . . . ? C48 C49 N9 Ni2 148.5(5) . . . . ? C44 C49 N9 Ni2 -31.1(5) . . . . ? C36 C37 N9 C43 28.8(7) . . . . ? C32 C37 N9 C43 -152.6(5) . . . . ? C36 C37 N9 C49 -105.6(6) . . . . ? C32 C37 N9 C49 73.0(6) . . . . ? C36 C37 N9 Ni2 145.1(5) . . . . ? C32 C37 N9 Ni2 -36.3(5) . . . . ? C8S C7S N1S C5S 65.7(7) . . . . ? C8S C7S N1S C1S -53.7(8) . . . . ? C8S C7S N1S C3S -172.9(6) . . . . ? C6S C5S N1S C7S 172.8(6) . . . . ? C6S C5S N1S C1S -65.8(7) . . . . ? C6S C5S N1S C3S 53.7(7) . . . . ? C2S C1S N1S C7S -54.1(8) . . . . ? C2S C1S N1S C5S -173.8(6) . . . . ? C2S C1S N1S C3S 64.7(8) . . . . ? C4S C3S N1S C7S -63.3(8) . . . . ? C4S C3S N1S C5S 56.5(8) . . . . ? C4S C3S N1S C1S 175.7(6) . . . . ? C12S C11S N2S C9S -57.7(7) . . . . ? C12S C11S N2S C13S -177.6(5) . . . . ? C12S C11S N2S C15S 61.8(7) . . . . ? C10S C9S N2S C11S -56.1(7) . . . . ? C10S C9S N2S C13S 61.1(7) . . . . ? C10S C9S N2S C15S -178.2(6) . . . . ? C14S C13S N2S C11S 172.9(6) . . . . ? C14S C13S N2S C9S 52.8(7) . . . . ? C14S C13S N2S C15S -65.9(7) . . . . ? C16S C15S N2S C11S 58.0(8) . . . . ? C16S C15S N2S C9S 179.6(6) . . . . ? C16S C15S N2S C13S -59.8(7) . . . . ? C20S C19S N3S C21S 66.6(7) . . . . ? C20S C19S N3S C23S -172.4(5) . . . . ? C20S C19S N3S C17S -54.7(7) . . . . ? C22S C21S N3S C19S 169.6(6) . . . . ? C22S C21S N3S C23S 51.1(7) . . . . ? C22S C21S N3S C17S -67.4(7) . . . . ? C24S C23S N3S C19S -62.6(7) . . . . ? C24S C23S N3S C21S 57.4(7) . . . . ? C24S C23S N3S C17S 176.8(6) . . . . ? C18S C17S N3S C19S -52.0(7) . . . . ? C18S C17S N3S C21S -173.6(6) . . . . ? C18S C17S N3S C23S 65.4(7) . . . . ? C30S C29S N4S C27S 173.6(8) . . . . ? C30S C29S N4S C31S 53.6(11) . . . . ? C30S C29S N4S C25S -61.1(10) . . . . ? C28S C27S N4S C29S 62.9(10) . . . . ? C28S C27S N4S C31S -175.3(8) . . . . ? C28S C27S N4S C25S -59.5(10) . . . . ? C32S C31S N4S C29S 59.7(9) . . . . ? C32S C31S N4S C27S -63.4(9) . . . . ? C32S C31S N4S C25S 175.8(7) . . . . ? C26S C25S N4S C29S -168.6(8) . . . . ? C26S C25S N4S C27S -43.6(10) . . . . ? C26S C25S N4S C31S 73.4(9) . . . . ? N5 C31 Ni1 N2 -136(2) . . . . ? N5 C31 Ni1 N3 -36(3) . . . . ? N5 C31 Ni1 N1 110(3) . . . . ? N5 C31 Ni1 N4 10(3) . . . . ? C23 N2 Ni1 C31 -39.1(6) . . . . ? C7 N2 Ni1 C31 139.4(4) . . . . ? C23 N2 Ni1 N3 -133.3(5) . . . . ? C7 N2 Ni1 N3 45.3(4) . . . . ? C23 N2 Ni1 N1 74.4(5) . . . . ? C7 N2 Ni1 N1 -107.1(4) . . . . ? C23 N2 Ni1 N4 152.4(5) . . . . ? C7 N2 Ni1 N4 -29.0(4) . . . . ? C27 N3 Ni1 C31 -44.0(5) . . . . ? C18 N3 Ni1 C31 119.7(4) . . . . ? C27 N3 Ni1 N2 73.1(5) . . . . ? C18 N3 Ni1 N2 -123.3(4) . . . . ? C27 N3 Ni1 N1 -155.6(5) . . . . ? C18 N3 Ni1 N1 8.0(5) . . . . ? C27 N3 Ni1 N4 151.5(6) . . . . ? C18 N3 Ni1 N4 -44.9(4) . . . . ? C19 N1 Ni1 C31 -8.8(5) . . . . ? C1 N1 Ni1 C31 -170.7(4) . . . . ? C19 N1 Ni1 N2 -131.4(5) . . . . ? C1 N1 Ni1 N2 66.6(4) . . . . ? C19 N1 Ni1 N3 98.4(5) . . . . ? C1 N1 Ni1 N3 -63.5(5) . . . . ? C19 N1 Ni1 N4 150.1(5) . . . . ? C1 N1 Ni1 N4 -11.8(4) . . . . ? C13 N4 Ni1 C31 -3.9(7) . . . . ? C6 N4 Ni1 C31 118.0(6) . . . . ? C12 N4 Ni1 C31 -120.7(6) . . . . ? C13 N4 Ni1 N2 146.3(3) . . . . ? C6 N4 Ni1 N2 -91.8(4) . . . . ? C12 N4 Ni1 N2 29.5(3) . . . . ? C13 N4 Ni1 N3 43.8(3) . . . . ? C6 N4 Ni1 N3 165.7(4) . . . . ? C12 N4 Ni1 N3 -73.0(3) . . . . ? C13 N4 Ni1 N1 -107.2(3) . . . . ? C6 N4 Ni1 N1 14.7(3) . . . . ? C12 N4 Ni1 N1 135.9(3) . . . . ? N10 C62 Ni2 N8 -134(5) . . . . ? N10 C62 Ni2 N6 -26(5) . . . . ? N10 C62 Ni2 N7 112(5) . . . . ? N10 C62 Ni2 N9 -14(6) . . . . ? C58 N8 Ni2 C62 -47.8(5) . . . . ? C44 N8 Ni2 C62 136.8(4) . . . . ? C58 N8 Ni2 N6 -146.6(5) . . . . ? C44 N8 Ni2 N6 38.0(4) . . . . ? C58 N8 Ni2 N7 66.4(5) . . . . ? C44 N8 Ni2 N7 -109.0(4) . . . . ? C58 N8 Ni2 N9 141.8(5) . . . . ? C44 N8 Ni2 N9 -33.6(4) . . . . ? C50 N6 Ni2 C62 -29.4(5) . . . . ? C32 N6 Ni2 C62 134.8(4) . . . . ? C50 N6 Ni2 N8 78.9(5) . . . . ? C32 N6 Ni2 N8 -116.8(3) . . . . ? C50 N6 Ni2 N7 -147.3(5) . . . . ? C32 N6 Ni2 N7 16.9(5) . . . . ? C50 N6 Ni2 N9 153.1(5) . . . . ? C32 N6 Ni2 N9 -42.7(3) . . . . ? C54 N7 Ni2 C62 -23.4(5) . . . . ? C38 N7 Ni2 C62 164.9(4) . . . . ? C54 N7 Ni2 N8 -137.1(5) . . . . ? C38 N7 Ni2 N8 51.2(4) . . . . ? C54 N7 Ni2 N6 89.3(5) . . . . ? C38 N7 Ni2 N6 -82.4(4) . . . . ? C54 N7 Ni2 N9 147.5(5) . . . . ? C38 N7 Ni2 N9 -24.2(3) . . . . ? C43 N9 Ni2 C62 152.2(10) . . . . ? C49 N9 Ni2 C62 -88.9(11) . . . . ? C37 N9 Ni2 C62 28.5(12) . . . . ? C43 N9 Ni2 N8 -84.7(3) . . . . ? C49 N9 Ni2 N8 34.2(3) . . . . ? C37 N9 Ni2 N8 151.6(3) . . . . ? C43 N9 Ni2 N6 165.3(4) . . . . ? C49 N9 Ni2 N6 -75.8(3) . . . . ? C37 N9 Ni2 N6 41.7(3) . . . . ? C43 N9 Ni2 N7 24.7(3) . . . . ? C49 N9 Ni2 N7 143.6(3) . . . . ? C37 N9 Ni2 N7 -99.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.17 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.777 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.078 # Attachment 'laa_02_077Ntosub.cif' # Attachment 'mbj_3_255tosub.cif' data_mbj_3_255s _database_code_depnum_ccdc_archive 'CCDC 738762' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H56 N7 Ni O3 P' _chemical_formula_sum 'C69 H56 N7 Ni O3 P' _chemical_formula_weight 1120.89 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' P P 0.1023 0.0942 '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 10.9218(3) _cell_length_b 25.9666(9) _cell_length_c 20.1405(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.153(17) _cell_angle_gamma 90.00 _cell_volume 5711.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.13 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8730 _exptl_absorpt_correction_T_max 0.9201 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60804 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.52 _reflns_number_total 10176 _reflns_number_gt 6377 _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^)+(0.1022P)^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 10176 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.3548(3) 0.92971(14) 0.87134(18) 0.0290(8) Uani 1 1 d . . . C2 C 0.3523(4) 0.88811(15) 0.9138(2) 0.0363(9) Uani 1 1 d . . . H2 H 0.2849 0.8836 0.9429 0.044 Uiso 1 1 calc R . . C3 C 0.4463(4) 0.85328(16) 0.9143(2) 0.0444(11) Uani 1 1 d . . . H3 H 0.4443 0.8247 0.9437 0.053 Uiso 1 1 calc R . . C4 C 0.5433(4) 0.85967(17) 0.8723(2) 0.0461(11) Uani 1 1 d . . . H4 H 0.6076 0.8350 0.8721 0.055 Uiso 1 1 calc R . . C5 C 0.5488(4) 0.90196(18) 0.8296(2) 0.0412(10) Uani 1 1 d . . . H5 H 0.6177 0.9062 0.8015 0.049 Uiso 1 1 calc R . . C6 C 0.4550(3) 0.93771(15) 0.82792(18) 0.0332(9) Uani 1 1 d . . . C7 C 0.5370(4) 0.99746(19) 0.7477(2) 0.0443(11) Uani 1 1 d . . . C8 C 0.5252(4) 1.04995(19) 0.7186(2) 0.0446(11) Uani 1 1 d . . . C9 C 0.6011(6) 1.0630(2) 0.6657(3) 0.0723(16) Uani 1 1 d . . . H9 H 0.6601 1.0393 0.6493 0.087 Uiso 1 1 calc R . . C10 C 0.5880(8) 1.1125(3) 0.6369(3) 0.106(3) Uani 1 1 d . . . H10 H 0.6360 1.1210 0.5992 0.127 Uiso 1 1 calc R . . C11 C 0.5092(7) 1.1481(3) 0.6614(3) 0.090(2) Uani 1 1 d . . . H11 H 0.5055 1.1816 0.6425 0.109 Uiso 1 1 calc R . . C12 C 0.4343(5) 1.1353(2) 0.7142(3) 0.0615(14) Uani 1 1 d . . . H12 H 0.3762 1.1592 0.7308 0.074 Uiso 1 1 calc R . . C13 C 0.4460(4) 1.08661(19) 0.7425(2) 0.0481(11) Uani 1 1 d . . . H13 H 0.3971 1.0784 0.7800 0.058 Uiso 1 1 calc R . . C14 C 0.2766(3) 1.01537(13) 0.89985(17) 0.0259(8) Uani 1 1 d . . . C15 C 0.3395(3) 1.01884(14) 0.95843(18) 0.0297(8) Uani 1 1 d . . . H15 H 0.3703 0.9884 0.9787 0.036 Uiso 1 1 calc R . . C16 C 0.3590(3) 1.06612(15) 0.98859(19) 0.0334(9) Uani 1 1 d . . . H16 H 0.4034 1.0685 1.0291 0.040 Uiso 1 1 calc R . . C17 C 0.3129(4) 1.10917(15) 0.9587(2) 0.0367(9) Uani 1 1 d . . . H17 H 0.3248 1.1417 0.9793 0.044 Uiso 1 1 calc R . . C18 C 0.2488(4) 1.10670(14) 0.89879(19) 0.0331(9) Uani 1 1 d . . . H18 H 0.2175 1.1374 0.8796 0.040 Uiso 1 1 calc R . . C19 C 0.2302(3) 1.05984(14) 0.86678(18) 0.0282(8) Uani 1 1 d . . . C20 C 0.1229(3) 1.08850(15) 0.76877(19) 0.0336(9) Uani 1 1 d . . . C21 C 0.0649(4) 1.07225(16) 0.7049(2) 0.0389(10) Uani 1 1 d . . . C22 C 0.0797(4) 1.10300(18) 0.6487(2) 0.0488(11) Uani 1 1 d . . . H22 H 0.1240 1.1344 0.6520 0.059 Uiso 1 1 calc R . . C23 C 0.0310(5) 1.0883(2) 0.5887(2) 0.0644(15) Uani 1 1 d . . . H23 H 0.0430 1.1093 0.5507 0.077 Uiso 1 1 calc R . . C24 C -0.0348(5) 1.0435(2) 0.5832(3) 0.0670(15) Uani 1 1 d . . . H24 H -0.0646 1.0327 0.5411 0.080 Uiso 1 1 calc R . . C25 C -0.0577(5) 1.0142(2) 0.6391(3) 0.0626(14) Uani 1 1 d . . . H25 H -0.1083 0.9845 0.6362 0.075 Uiso 1 1 calc R . . C26 C -0.0065(4) 1.02830(18) 0.6995(2) 0.0435(10) Uani 1 1 d . . . H26 H -0.0205 1.0076 0.7376 0.052 Uiso 1 1 calc R . . C27 C 0.1334(3) 0.94488(13) 0.87878(18) 0.0257(7) Uani 1 1 d . . . C28 C 0.0793(3) 0.94763(14) 0.94084(18) 0.0293(8) Uani 1 1 d . . . H28 H 0.1208 0.9642 0.9764 0.035 Uiso 1 1 calc R . . C29 C -0.0351(4) 0.92624(14) 0.9508(2) 0.0337(9) Uani 1 1 d . . . H29 H -0.0737 0.9282 0.9930 0.040 Uiso 1 1 calc R . . C30 C -0.0921(4) 0.90186(15) 0.8979(2) 0.0360(9) Uani 1 1 d . . . H30 H -0.1697 0.8862 0.9047 0.043 Uiso 1 1 calc R . . C31 C -0.0400(4) 0.89953(15) 0.8360(2) 0.0347(9) Uani 1 1 d . . . H31 H -0.0824 0.8830 0.8007 0.042 Uiso 1 1 calc R . . C32 C 0.0759(3) 0.92146(13) 0.82467(19) 0.0289(8) Uani 1 1 d . . . C33 C 0.1143(4) 0.89254(15) 0.7133(2) 0.0348(9) Uani 1 1 d . . . C34 C 0.2048(4) 0.89208(14) 0.6577(2) 0.0354(9) Uani 1 1 d . . . C35 C 0.3305(4) 0.88830(17) 0.6710(2) 0.0426(10) Uani 1 1 d . . . H35 H 0.3588 0.8865 0.7156 0.051 Uiso 1 1 calc R . . C36 C 0.4133(5) 0.8871(2) 0.6193(3) 0.0588(13) Uani 1 1 d . . . H36 H 0.4985 0.8850 0.6286 0.071 Uiso 1 1 calc R . . C37 C 0.3730(5) 0.8891(2) 0.5543(3) 0.0636(14) Uani 1 1 d . . . H37 H 0.4302 0.8882 0.5189 0.076 Uiso 1 1 calc R . . C38 C 0.2506(5) 0.8923(2) 0.5412(2) 0.0567(13) Uani 1 1 d . . . H38 H 0.2230 0.8941 0.4965 0.068 Uiso 1 1 calc R . . C39 C 0.1659(4) 0.89316(18) 0.5928(2) 0.0486(11) Uani 1 1 d . . . H39 H 0.0809 0.8945 0.5830 0.058 Uiso 1 1 calc R . . C40 C 0.3005(4) 1.01568(18) 0.6178(2) 0.0460(11) Uani 1 1 d . . . C41 C 0.3346(7) 1.0310(3) 0.5499(3) 0.087(2) Uani 1 1 d . . . H41A H 0.2934 1.0085 0.5178 0.130 Uiso 1 1 calc R . . H41B H 0.4235 1.0280 0.5446 0.130 Uiso 1 1 calc R . . H41C H 0.3097 1.0668 0.5421 0.130 Uiso 1 1 calc R . . C42 C 0.8860(4) 0.21833(15) 0.9138(2) 0.0363(9) Uani 1 1 d . . . C43 C 0.9422(4) 0.26547(17) 0.8974(2) 0.0496(11) Uani 1 1 d . . . H43 H 0.9175 0.2834 0.8585 0.060 Uiso 1 1 calc R . . C44 C 1.0308(5) 0.2854(2) 0.9366(3) 0.0594(13) Uani 1 1 d . . . H44 H 1.0687 0.3169 0.9245 0.071 Uiso 1 1 calc R . . C45 C 1.0675(4) 0.26053(19) 0.9943(3) 0.0552(12) Uani 1 1 d . . . H45 H 1.1285 0.2753 1.0221 0.066 Uiso 1 1 calc R . . C46 C 1.0145(5) 0.21422(18) 1.0110(2) 0.0541(12) Uani 1 1 d . . . H46 H 1.0404 0.1965 1.0499 0.065 Uiso 1 1 calc R . . C47 C 0.9244(4) 0.19364(16) 0.9716(2) 0.0454(11) Uani 1 1 d . . . H47 H 0.8874 0.1620 0.9840 0.054 Uiso 1 1 calc R . . C48 C 0.7542(4) 0.12652(15) 0.8738(2) 0.0342(9) Uani 1 1 d . . . C49 C 0.8625(4) 0.09838(16) 0.8658(2) 0.0381(9) Uani 1 1 d . . . H49 H 0.9377 0.1159 0.8583 0.046 Uiso 1 1 calc R . . C50 C 0.8602(4) 0.04575(16) 0.8686(2) 0.0416(10) Uani 1 1 d . . . H50 H 0.9339 0.0266 0.8641 0.050 Uiso 1 1 calc R . . C51 C 0.7496(4) 0.02041(16) 0.8781(2) 0.0382(9) Uani 1 1 d . . . H51 H 0.7469 -0.0162 0.8785 0.046 Uiso 1 1 calc R . . C52 C 0.6443(4) 0.04841(16) 0.8869(2) 0.0408(10) Uani 1 1 d . . . H52 H 0.5694 0.0308 0.8948 0.049 Uiso 1 1 calc R . . C53 C 0.6447(4) 0.10060(16) 0.8845(2) 0.0368(9) Uani 1 1 d . . . H53 H 0.5708 0.1193 0.8902 0.044 Uiso 1 1 calc R . . C54 C 0.7728(4) 0.21456(17) 0.7812(2) 0.0432(10) Uani 1 1 d . . . C55 C 0.7367(5) 0.2633(2) 0.7638(2) 0.0568(13) Uani 1 1 d . . . H55 H 0.7028 0.2855 0.7965 0.068 Uiso 1 1 calc R . . C56 C 0.7490(6) 0.2806(2) 0.6990(3) 0.0791(18) Uani 1 1 d . . . H56 H 0.7238 0.3145 0.6872 0.095 Uiso 1 1 calc R . . C57 C 0.7984(6) 0.2481(3) 0.6516(3) 0.089(2) Uani 1 1 d . . . H57 H 0.8060 0.2595 0.6069 0.107 Uiso 1 1 calc R . . C58 C 0.8368(7) 0.1990(3) 0.6691(3) 0.086(2) Uani 1 1 d . . . H58 H 0.8735 0.1774 0.6366 0.103 Uiso 1 1 calc R . . C59 C 0.8222(5) 0.1808(2) 0.7333(3) 0.0642(15) Uani 1 1 d . . . H59 H 0.8449 0.1467 0.7448 0.077 Uiso 1 1 calc R . . C60 C 0.6207(4) 0.22281(16) 0.8986(3) 0.0489(12) Uani 1 1 d . . . C61 C 0.6208(5) 0.2487(2) 0.9579(3) 0.0664(15) Uani 1 1 d . . . H61 H 0.6953 0.2541 0.9813 0.080 Uiso 1 1 calc R . . C62 C 0.5119(8) 0.2670(2) 0.9832(4) 0.100(3) Uani 1 1 d . . . H62 H 0.5105 0.2834 1.0254 0.119 Uiso 1 1 calc R . . C63 C 0.4081(8) 0.2617(3) 0.9482(6) 0.115(4) Uani 1 1 d . . . H63 H 0.3341 0.2758 0.9650 0.138 Uiso 1 1 calc R . . C64 C 0.4071(6) 0.2371(3) 0.8906(6) 0.106(3) Uani 1 1 d . . . H64 H 0.3317 0.2331 0.8676 0.127 Uiso 1 1 calc R . . C65 C 0.5131(5) 0.2171(2) 0.8627(4) 0.0794(19) Uani 1 1 d . . . H65 H 0.5119 0.2002 0.8209 0.095 Uiso 1 1 calc R . . C1S C 0.1161(7) 0.2544(3) 0.7426(3) 0.0862(19) Uiso 1 1 d . . . H1S1 H 0.0361 0.2695 0.7323 0.129 Uiso 1 1 calc R . . H1S2 H 0.1579 0.2756 0.7759 0.129 Uiso 1 1 calc R . . H1S3 H 0.1049 0.2194 0.7599 0.129 Uiso 1 1 calc R . . C2S C 0.1889(6) 0.2524(2) 0.6832(3) 0.0709(15) Uiso 1 1 d . . . C3S C 0.2538(6) 0.3747(2) 0.8261(3) 0.0771(17) Uiso 1 1 d . . . H3S1 H 0.3008 0.3440 0.8135 0.116 Uiso 1 1 calc R . . H3S2 H 0.2912 0.4053 0.8062 0.116 Uiso 1 1 calc R . . H3S3 H 0.1694 0.3712 0.8100 0.116 Uiso 1 1 calc R . . C4S C 0.2536(6) 0.3794(2) 0.8927(3) 0.0700(15) Uiso 1 1 d . . . N1 N 0.2545(3) 0.96676(11) 0.86664(14) 0.0251(6) Uani 1 1 d . . . N2 N 0.4431(3) 0.98178(13) 0.78613(15) 0.0350(8) Uani 1 1 d . . . N3 N 0.1773(3) 1.05094(12) 0.80412(15) 0.0297(7) Uani 1 1 d . . . N4 N 0.1414(3) 0.92369(11) 0.76409(15) 0.0289(7) Uani 1 1 d . . . N5 N 0.2741(3) 1.00414(13) 0.66976(17) 0.0369(8) Uani 1 1 d . . . N1S N 0.2467(6) 0.2499(3) 0.6382(3) 0.1061(19) Uiso 1 1 d . . . N2S N 0.2556(6) 0.3802(3) 0.9500(3) 0.1054(19) Uiso 1 1 d . . . Ni1 Ni 0.25656(4) 0.985459(18) 0.76623(2) 0.02885(16) Uani 1 1 d . . . O1 O 0.6336(3) 0.97299(15) 0.73674(19) 0.0649(10) Uani 1 1 d . . . O2 O 0.1167(3) 1.13497(11) 0.78462(15) 0.0485(8) Uani 1 1 d . . . O3 O 0.0233(3) 0.86286(13) 0.70749(17) 0.0573(9) Uani 1 1 d . . . P1 P 0.76005(10) 0.19501(4) 0.86597(5) 0.0373(3) 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 C1 0.030(2) 0.0285(19) 0.0288(19) -0.0079(15) -0.0044(15) 0.0019(15) C2 0.036(2) 0.033(2) 0.040(2) -0.0009(18) -0.0081(18) -0.0070(17) C3 0.044(3) 0.030(2) 0.059(3) 0.001(2) -0.021(2) -0.0004(18) C4 0.044(3) 0.044(2) 0.050(3) -0.019(2) -0.017(2) 0.015(2) C5 0.029(2) 0.060(3) 0.034(2) -0.014(2) -0.0050(17) 0.0092(19) C6 0.030(2) 0.043(2) 0.0263(19) -0.0106(17) -0.0058(16) -0.0002(16) C7 0.032(2) 0.065(3) 0.036(2) -0.007(2) 0.0006(19) -0.004(2) C8 0.037(2) 0.066(3) 0.031(2) 0.007(2) 0.0011(18) -0.011(2) C9 0.077(4) 0.092(4) 0.049(3) 0.005(3) 0.020(3) -0.013(3) C10 0.140(7) 0.114(6) 0.064(4) 0.032(4) 0.044(4) -0.029(5) C11 0.116(6) 0.081(4) 0.074(4) 0.027(4) 0.020(4) -0.001(4) C12 0.069(3) 0.060(3) 0.056(3) 0.013(3) 0.002(3) -0.013(3) C13 0.044(3) 0.058(3) 0.042(2) 0.004(2) 0.005(2) -0.016(2) C14 0.0237(18) 0.0295(19) 0.0245(17) -0.0027(15) 0.0051(14) -0.0066(14) C15 0.0273(19) 0.034(2) 0.0278(18) 0.0013(16) 0.0012(15) -0.0033(15) C16 0.031(2) 0.040(2) 0.030(2) -0.0066(17) 0.0009(16) -0.0070(16) C17 0.042(2) 0.033(2) 0.035(2) -0.0086(17) 0.0077(18) -0.0117(17) C18 0.038(2) 0.0274(19) 0.034(2) 0.0025(16) 0.0048(17) -0.0005(16) C19 0.0248(19) 0.0314(19) 0.0286(19) -0.0004(15) 0.0073(15) -0.0020(14) C20 0.030(2) 0.037(2) 0.033(2) 0.0010(17) 0.0060(17) 0.0004(17) C21 0.035(2) 0.047(2) 0.034(2) 0.0060(18) 0.0018(18) 0.0151(19) C22 0.055(3) 0.051(3) 0.041(3) 0.014(2) -0.001(2) 0.009(2) C23 0.079(4) 0.073(4) 0.041(3) 0.020(3) -0.001(3) 0.024(3) C24 0.075(4) 0.075(4) 0.051(3) -0.004(3) -0.023(3) 0.021(3) C25 0.052(3) 0.079(4) 0.057(3) -0.011(3) -0.017(3) 0.008(3) C26 0.039(2) 0.050(3) 0.042(2) -0.001(2) -0.0080(19) 0.0068(19) C27 0.0236(18) 0.0227(17) 0.0309(19) 0.0008(15) 0.0008(15) -0.0008(14) C28 0.033(2) 0.0276(18) 0.0272(19) 0.0015(15) 0.0005(16) -0.0033(15) C29 0.032(2) 0.035(2) 0.035(2) 0.0033(17) 0.0065(17) -0.0012(16) C30 0.027(2) 0.033(2) 0.048(2) 0.0024(18) 0.0046(17) -0.0056(16) C31 0.032(2) 0.032(2) 0.040(2) -0.0034(17) -0.0007(17) -0.0051(16) C32 0.0283(19) 0.0236(18) 0.035(2) -0.0021(15) 0.0002(16) -0.0015(14) C33 0.031(2) 0.033(2) 0.040(2) -0.0064(18) -0.0036(17) -0.0012(16) C34 0.040(2) 0.0276(19) 0.038(2) -0.0108(17) -0.0037(18) 0.0029(16) C35 0.041(2) 0.048(2) 0.039(2) -0.0083(19) -0.0026(19) 0.0061(19) C36 0.041(3) 0.078(4) 0.057(3) -0.008(3) 0.003(2) 0.018(2) C37 0.056(3) 0.087(4) 0.048(3) -0.015(3) 0.013(2) 0.007(3) C38 0.059(3) 0.077(4) 0.034(2) -0.012(2) -0.004(2) 0.016(3) C39 0.046(3) 0.058(3) 0.042(2) -0.016(2) -0.008(2) 0.004(2) C40 0.049(3) 0.057(3) 0.032(2) 0.003(2) 0.002(2) 0.001(2) C41 0.109(5) 0.102(5) 0.049(3) 0.021(3) 0.028(3) 0.002(4) C42 0.035(2) 0.037(2) 0.037(2) 0.0058(18) 0.0048(17) 0.0056(17) C43 0.047(3) 0.047(3) 0.055(3) 0.021(2) 0.000(2) -0.003(2) C44 0.056(3) 0.050(3) 0.072(3) 0.016(3) 0.000(3) -0.015(2) C45 0.045(3) 0.056(3) 0.065(3) -0.001(3) -0.009(2) -0.004(2) C46 0.067(3) 0.045(3) 0.050(3) 0.009(2) -0.005(2) 0.004(2) C47 0.054(3) 0.033(2) 0.049(3) 0.011(2) -0.001(2) -0.003(2) C48 0.034(2) 0.032(2) 0.036(2) 0.0054(17) 0.0015(17) 0.0030(16) C49 0.031(2) 0.038(2) 0.044(2) 0.0036(18) 0.0067(18) 0.0039(17) C50 0.045(3) 0.043(2) 0.037(2) 0.0010(18) 0.0060(19) 0.0152(19) C51 0.044(2) 0.033(2) 0.037(2) 0.0023(17) 0.0005(19) 0.0031(18) C52 0.040(2) 0.044(2) 0.039(2) 0.0064(19) -0.0053(18) -0.0039(19) C53 0.030(2) 0.043(2) 0.038(2) 0.0024(18) -0.0011(17) 0.0039(17) C54 0.039(2) 0.048(3) 0.042(2) 0.014(2) -0.0028(19) 0.0045(19) C55 0.073(4) 0.052(3) 0.046(3) 0.012(2) -0.006(2) 0.000(2) C56 0.098(5) 0.071(4) 0.068(4) 0.034(3) -0.030(3) -0.007(3) C57 0.095(5) 0.124(6) 0.048(3) 0.038(4) 0.007(3) 0.025(4) C58 0.098(5) 0.110(5) 0.050(3) 0.020(3) 0.012(3) 0.030(4) C59 0.061(3) 0.083(4) 0.049(3) 0.019(3) 0.005(2) 0.021(3) C60 0.042(3) 0.037(2) 0.068(3) 0.016(2) 0.012(2) 0.0130(19) C61 0.072(4) 0.051(3) 0.076(4) 0.017(3) 0.032(3) 0.017(3) C62 0.113(6) 0.069(4) 0.118(6) 0.033(4) 0.070(5) 0.046(4) C63 0.081(5) 0.065(5) 0.200(11) 0.058(6) 0.075(7) 0.039(4) C64 0.048(4) 0.058(4) 0.212(10) 0.044(5) 0.017(5) 0.018(3) C65 0.040(3) 0.050(3) 0.148(6) 0.009(3) -0.003(3) 0.009(2) N1 0.0243(15) 0.0256(15) 0.0253(15) -0.0005(12) -0.0013(12) -0.0012(12) N2 0.0300(18) 0.049(2) 0.0263(16) 0.0005(15) 0.0019(14) 0.0003(14) N3 0.0307(17) 0.0328(16) 0.0257(16) 0.0020(13) 0.0019(13) 0.0019(13) N4 0.0292(16) 0.0289(16) 0.0286(16) -0.0039(13) -0.0024(13) -0.0031(13) N5 0.0356(19) 0.0423(19) 0.0328(19) -0.0028(15) 0.0002(15) 0.0002(15) Ni1 0.0312(3) 0.0311(3) 0.0242(3) -0.00106(19) -0.00053(19) -0.0017(2) O1 0.045(2) 0.080(2) 0.070(2) -0.0002(19) 0.0269(18) 0.0055(17) O2 0.065(2) 0.0358(16) 0.0451(17) 0.0048(13) -0.0001(15) 0.0128(14) O3 0.0447(18) 0.068(2) 0.059(2) -0.0331(17) 0.0071(15) -0.0198(16) P1 0.0356(6) 0.0342(5) 0.0422(6) 0.0089(5) 0.0046(5) 0.0052(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(5) . ? C1 C6 1.417(5) . ? C1 N1 1.461(5) . ? C2 C3 1.368(6) . ? C3 C4 1.367(7) . ? C4 C5 1.396(7) . ? C5 C6 1.383(6) . ? C6 N2 1.426(5) . ? C7 O1 1.251(6) . ? C7 N2 1.350(5) . ? C7 C8 1.489(7) . ? C8 C13 1.374(7) . ? C8 C9 1.394(7) . ? C9 C10 1.416(10) . ? C10 C11 1.357(10) . ? C11 C12 1.384(8) . ? C12 C13 1.393(7) . ? C14 C15 1.367(5) . ? C14 C19 1.425(5) . ? C14 N1 1.449(5) . ? C15 C16 1.386(5) . ? C16 C17 1.365(6) . ? C17 C18 1.395(6) . ? C18 C19 1.392(5) . ? C19 N3 1.406(5) . ? C20 O2 1.250(5) . ? C20 N3 1.345(5) . ? C20 C21 1.493(6) . ? C21 C26 1.386(6) . ? C21 C22 1.396(6) . ? C22 C23 1.373(7) . ? C23 C24 1.372(9) . ? C24 C25 1.383(8) . ? C25 C26 1.386(7) . ? C27 C28 1.386(5) . ? C27 C32 1.396(5) . ? C27 N1 1.461(4) . ? C28 C29 1.383(5) . ? C29 C30 1.386(6) . ? C30 C31 1.373(5) . ? C31 C32 1.407(5) . ? C32 N4 1.417(5) . ? C33 O3 1.263(5) . ? C33 N4 1.337(5) . ? C33 C34 1.495(6) . ? C34 C39 1.375(6) . ? C34 C35 1.401(6) . ? C35 C36 1.380(6) . ? C36 C37 1.381(7) . ? C37 C38 1.364(7) . ? C38 C39 1.392(6) . ? C40 N5 1.127(5) . ? C40 C41 1.473(7) . ? C42 C47 1.394(6) . ? C42 C43 1.409(6) . ? C42 P1 1.783(4) . ? C43 C44 1.351(7) . ? C44 C45 1.388(7) . ? C45 C46 1.376(7) . ? C46 C47 1.371(7) . ? C48 C53 1.389(6) . ? C48 C49 1.400(5) . ? C48 P1 1.786(4) . ? C49 C50 1.368(6) . ? C50 C51 1.389(6) . ? C51 C52 1.373(6) . ? C52 C53 1.356(6) . ? C54 C55 1.371(7) . ? C54 C59 1.412(7) . ? C54 P1 1.786(4) . ? C55 C56 1.388(7) . ? C56 C57 1.385(9) . ? C57 C58 1.389(9) . ? C58 C59 1.386(7) . ? C60 C61 1.371(8) . ? C60 C65 1.385(8) . ? C60 P1 1.809(4) . ? C61 C62 1.380(8) . ? C62 C63 1.341(13) . ? C63 C64 1.324(13) . ? C64 C65 1.389(9) . ? C1S C2S 1.438(9) . ? C2S N1S 1.108(8) . ? C3S C4S 1.347(9) . ? C4S N2S 1.155(8) . ? N1 Ni1 2.080(3) . ? N2 Ni1 2.078(3) . ? N3 Ni1 2.056(3) . ? N4 Ni1 2.039(3) . ? N5 Ni1 2.012(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 C2 C1 C6 121.0(4) . . ? C2 C1 N1 122.7(3) . . ? C6 C1 N1 116.3(3) . . ? C3 C2 C1 120.4(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 120.8(4) . . ? C6 C5 C4 120.7(4) . . ? C5 C6 C1 117.3(4) . . ? C5 C6 N2 128.3(4) . . ? C1 C6 N2 114.4(3) . . ? O1 C7 N2 126.2(4) . . ? O1 C7 C8 117.9(4) . . ? N2 C7 C8 115.9(4) . . ? C13 C8 C9 118.4(5) . . ? C13 C8 C7 123.4(4) . . ? C9 C8 C7 118.1(5) . . ? C8 C9 C10 118.3(6) . . ? C11 C10 C9 122.2(6) . . ? C10 C11 C12 119.5(6) . . ? C11 C12 C13 118.6(6) . . ? C8 C13 C12 122.8(4) . . ? C15 C14 C19 121.8(3) . . ? C15 C14 N1 122.6(3) . . ? C19 C14 N1 115.6(3) . . ? C14 C15 C16 120.9(4) . . ? C17 C16 C15 118.4(4) . . ? C16 C17 C18 121.8(4) . . ? C19 C18 C17 120.9(4) . . ? C18 C19 N3 128.2(3) . . ? C18 C19 C14 116.1(3) . . ? N3 C19 C14 115.5(3) . . ? O2 C20 N3 126.1(4) . . ? O2 C20 C21 118.0(4) . . ? N3 C20 C21 115.9(3) . . ? C26 C21 C22 118.3(4) . . ? C26 C21 C20 122.6(4) . . ? C22 C21 C20 119.2(4) . . ? C23 C22 C21 120.6(5) . . ? C24 C23 C22 120.6(5) . . ? C23 C24 C25 119.7(5) . . ? C24 C25 C26 119.8(5) . . ? C25 C26 C21 120.8(5) . . ? C28 C27 C32 122.3(3) . . ? C28 C27 N1 121.3(3) . . ? C32 C27 N1 116.4(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 118.4(4) . . ? C31 C30 C29 122.2(4) . . ? C30 C31 C32 120.3(4) . . ? C27 C32 C31 116.9(3) . . ? C27 C32 N4 115.3(3) . . ? C31 C32 N4 127.8(3) . . ? O3 C33 N4 127.7(4) . . ? O3 C33 C34 116.6(3) . . ? N4 C33 C34 115.6(3) . . ? C39 C34 C35 118.9(4) . . ? C39 C34 C33 120.6(4) . . ? C35 C34 C33 120.5(4) . . ? C36 C35 C34 120.1(4) . . ? C35 C36 C37 120.3(5) . . ? C38 C37 C36 119.7(5) . . ? C37 C38 C39 120.6(4) . . ? C34 C39 C38 120.3(4) . . ? N5 C40 C41 179.7(6) . . ? C47 C42 C43 117.7(4) . . ? C47 C42 P1 121.7(3) . . ? C43 C42 P1 120.3(3) . . ? C44 C43 C42 120.5(4) . . ? C43 C44 C45 121.1(5) . . ? C46 C45 C44 119.3(5) . . ? C47 C46 C45 120.1(4) . . ? C46 C47 C42 121.2(4) . . ? C53 C48 C49 119.5(4) . . ? C53 C48 P1 121.8(3) . . ? C49 C48 P1 118.6(3) . . ? C50 C49 C48 120.1(4) . . ? C49 C50 C51 119.7(4) . . ? C52 C51 C50 119.8(4) . . ? C53 C52 C51 121.4(4) . . ? C52 C53 C48 119.5(4) . . ? C55 C54 C59 120.5(4) . . ? C55 C54 P1 118.9(4) . . ? C59 C54 P1 120.5(3) . . ? C54 C55 C56 120.7(5) . . ? C57 C56 C55 119.4(5) . . ? C56 C57 C58 120.2(5) . . ? C59 C58 C57 120.9(6) . . ? C58 C59 C54 118.2(5) . . ? C61 C60 C65 120.4(5) . . ? C61 C60 P1 120.9(4) . . ? C65 C60 P1 118.8(4) . . ? C60 C61 C62 119.5(7) . . ? C63 C62 C61 119.9(8) . . ? C64 C63 C62 121.0(7) . . ? C63 C64 C65 122.0(8) . . ? C60 C65 C64 117.1(7) . . ? N1S C2S C1S 178.3(8) . . ? N2S C4S C3S 175.5(7) . . ? C14 N1 C27 114.3(3) . . ? C14 N1 C1 114.8(3) . . ? C27 N1 C1 114.4(3) . . ? C14 N1 Ni1 104.1(2) . . ? C27 N1 Ni1 105.4(2) . . ? C1 N1 Ni1 101.9(2) . . ? C7 N2 C6 120.8(4) . . ? C7 N2 Ni1 128.4(3) . . ? C6 N2 Ni1 103.8(2) . . ? C20 N3 C19 122.4(3) . . ? C20 N3 Ni1 126.1(2) . . ? C19 N3 Ni1 107.2(2) . . ? C33 N4 C32 121.5(3) . . ? C33 N4 Ni1 128.9(3) . . ? C32 N4 Ni1 109.1(2) . . ? C40 N5 Ni1 170.4(4) . . ? N5 Ni1 N4 103.27(13) . . ? N5 Ni1 N3 101.55(13) . . ? N4 Ni1 N3 113.45(12) . . ? N5 Ni1 N2 95.84(13) . . ? N4 Ni1 N2 124.93(13) . . ? N3 Ni1 N2 112.35(13) . . ? N5 Ni1 N1 175.14(13) . . ? N4 Ni1 N1 80.13(12) . . ? N3 Ni1 N1 80.01(11) . . ? N2 Ni1 N1 79.33(12) . . ? C42 P1 C54 110.9(2) . . ? C42 P1 C48 108.59(19) . . ? C54 P1 C48 111.7(2) . . ? C42 P1 C60 108.5(2) . . ? C54 P1 C60 107.5(2) . . ? C48 P1 C60 109.56(19) . . ? 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 C6 C1 C2 C3 -0.7(6) . . . . ? N1 C1 C2 C3 177.2(3) . . . . ? C1 C2 C3 C4 -0.2(6) . . . . ? C2 C3 C4 C5 1.3(6) . . . . ? C3 C4 C5 C6 -1.4(6) . . . . ? C4 C5 C6 C1 0.5(6) . . . . ? C4 C5 C6 N2 -177.4(4) . . . . ? C2 C1 C6 C5 0.5(5) . . . . ? N1 C1 C6 C5 -177.5(3) . . . . ? C2 C1 C6 N2 178.8(3) . . . . ? N1 C1 C6 N2 0.8(5) . . . . ? O1 C7 C8 C13 -158.7(4) . . . . ? N2 C7 C8 C13 18.6(6) . . . . ? O1 C7 C8 C9 19.3(7) . . . . ? N2 C7 C8 C9 -163.5(4) . . . . ? C13 C8 C9 C10 -3.4(8) . . . . ? C7 C8 C9 C10 178.5(6) . . . . ? C8 C9 C10 C11 3.6(12) . . . . ? C9 C10 C11 C12 -3.3(12) . . . . ? C10 C11 C12 C13 2.7(10) . . . . ? C9 C8 C13 C12 3.1(7) . . . . ? C7 C8 C13 C12 -178.9(4) . . . . ? C11 C12 C13 C8 -2.7(8) . . . . ? C19 C14 C15 C16 1.0(5) . . . . ? N1 C14 C15 C16 179.8(3) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 -0.9(6) . . . . ? C16 C17 C18 C19 -0.5(6) . . . . ? C17 C18 C19 N3 -174.2(3) . . . . ? C17 C18 C19 C14 2.0(5) . . . . ? C15 C14 C19 C18 -2.3(5) . . . . ? N1 C14 C19 C18 178.8(3) . . . . ? C15 C14 C19 N3 174.4(3) . . . . ? N1 C14 C19 N3 -4.5(4) . . . . ? O2 C20 C21 C26 -135.5(4) . . . . ? N3 C20 C21 C26 44.2(5) . . . . ? O2 C20 C21 C22 42.7(5) . . . . ? N3 C20 C21 C22 -137.6(4) . . . . ? C26 C21 C22 C23 -3.9(6) . . . . ? C20 C21 C22 C23 177.8(4) . . . . ? C21 C22 C23 C24 1.0(8) . . . . ? C22 C23 C24 C25 3.3(8) . . . . ? C23 C24 C25 C26 -4.7(8) . . . . ? C24 C25 C26 C21 1.7(7) . . . . ? C22 C21 C26 C25 2.5(6) . . . . ? C20 C21 C26 C25 -179.2(4) . . . . ? C32 C27 C28 C29 0.7(5) . . . . ? N1 C27 C28 C29 -179.6(3) . . . . ? C27 C28 C29 C30 0.8(6) . . . . ? C28 C29 C30 C31 -1.7(6) . . . . ? C29 C30 C31 C32 1.2(6) . . . . ? C28 C27 C32 C31 -1.2(5) . . . . ? N1 C27 C32 C31 179.0(3) . . . . ? C28 C27 C32 N4 177.6(3) . . . . ? N1 C27 C32 N4 -2.2(5) . . . . ? C30 C31 C32 C27 0.3(5) . . . . ? C30 C31 C32 N4 -178.3(4) . . . . ? O3 C33 C34 C39 45.0(6) . . . . ? N4 C33 C34 C39 -136.5(4) . . . . ? O3 C33 C34 C35 -132.2(4) . . . . ? N4 C33 C34 C35 46.2(5) . . . . ? C39 C34 C35 C36 1.8(6) . . . . ? C33 C34 C35 C36 179.0(4) . . . . ? C34 C35 C36 C37 -0.8(7) . . . . ? C35 C36 C37 C38 0.2(8) . . . . ? C36 C37 C38 C39 -0.7(8) . . . . ? C35 C34 C39 C38 -2.2(6) . . . . ? C33 C34 C39 C38 -179.5(4) . . . . ? C37 C38 C39 C34 1.7(8) . . . . ? C47 C42 C43 C44 0.6(7) . . . . ? P1 C42 C43 C44 174.5(4) . . . . ? C42 C43 C44 C45 -1.0(8) . . . . ? C43 C44 C45 C46 1.5(8) . . . . ? C44 C45 C46 C47 -1.5(7) . . . . ? C45 C46 C47 C42 1.1(7) . . . . ? C43 C42 C47 C46 -0.6(6) . . . . ? P1 C42 C47 C46 -174.4(4) . . . . ? C53 C48 C49 C50 0.0(6) . . . . ? P1 C48 C49 C50 -177.2(3) . . . . ? C48 C49 C50 C51 1.3(6) . . . . ? C49 C50 C51 C52 -2.3(6) . . . . ? C50 C51 C52 C53 2.0(6) . . . . ? C51 C52 C53 C48 -0.7(6) . . . . ? C49 C48 C53 C52 -0.3(6) . . . . ? P1 C48 C53 C52 176.8(3) . . . . ? C59 C54 C55 C56 -0.6(8) . . . . ? P1 C54 C55 C56 177.8(5) . . . . ? C54 C55 C56 C57 0.0(9) . . . . ? C55 C56 C57 C58 -1.0(11) . . . . ? C56 C57 C58 C59 2.5(12) . . . . ? C57 C58 C59 C54 -3.0(11) . . . . ? C55 C54 C59 C58 2.1(8) . . . . ? P1 C54 C59 C58 -176.3(5) . . . . ? C65 C60 C61 C62 3.1(7) . . . . ? P1 C60 C61 C62 -176.4(4) . . . . ? C60 C61 C62 C63 -3.4(9) . . . . ? C61 C62 C63 C64 2.8(11) . . . . ? C62 C63 C64 C65 -1.9(11) . . . . ? C61 C60 C65 C64 -2.1(8) . . . . ? P1 C60 C65 C64 177.4(4) . . . . ? C63 C64 C65 C60 1.5(9) . . . . ? C15 C14 N1 C27 98.5(4) . . . . ? C19 C14 N1 C27 -82.6(4) . . . . ? C15 C14 N1 C1 -36.6(4) . . . . ? C19 C14 N1 C1 142.3(3) . . . . ? C15 C14 N1 Ni1 -147.1(3) . . . . ? C19 C14 N1 Ni1 31.8(3) . . . . ? C28 C27 N1 C14 -39.1(4) . . . . ? C32 C27 N1 C14 140.6(3) . . . . ? C28 C27 N1 C1 96.1(4) . . . . ? C32 C27 N1 C1 -84.1(4) . . . . ? C28 C27 N1 Ni1 -152.8(3) . . . . ? C32 C27 N1 Ni1 27.0(3) . . . . ? C2 C1 N1 C14 103.1(4) . . . . ? C6 C1 N1 C14 -78.9(4) . . . . ? C2 C1 N1 C27 -31.9(5) . . . . ? C6 C1 N1 C27 146.1(3) . . . . ? C2 C1 N1 Ni1 -145.0(3) . . . . ? C6 C1 N1 Ni1 32.9(3) . . . . ? O1 C7 N2 C6 10.7(7) . . . . ? C8 C7 N2 C6 -166.3(3) . . . . ? O1 C7 N2 Ni1 -135.2(4) . . . . ? C8 C7 N2 Ni1 47.8(5) . . . . ? C5 C6 N2 C7 -9.5(6) . . . . ? C1 C6 N2 C7 172.5(4) . . . . ? C5 C6 N2 Ni1 143.7(4) . . . . ? C1 C6 N2 Ni1 -34.4(3) . . . . ? O2 C20 N3 C19 3.2(6) . . . . ? C21 C20 N3 C19 -176.6(3) . . . . ? O2 C20 N3 Ni1 -150.7(3) . . . . ? C21 C20 N3 Ni1 29.5(5) . . . . ? C18 C19 N3 C20 -8.0(6) . . . . ? C14 C19 N3 C20 175.8(3) . . . . ? C18 C19 N3 Ni1 150.1(3) . . . . ? C14 C19 N3 Ni1 -26.1(4) . . . . ? O3 C33 N4 C32 9.4(6) . . . . ? C34 C33 N4 C32 -168.9(3) . . . . ? O3 C33 N4 Ni1 -161.4(3) . . . . ? C34 C33 N4 Ni1 20.4(5) . . . . ? C27 C32 N4 C33 162.8(3) . . . . ? C31 C32 N4 C33 -18.6(6) . . . . ? C27 C32 N4 Ni1 -24.9(4) . . . . ? C31 C32 N4 Ni1 153.7(3) . . . . ? C41 C40 N5 Ni1 -112(100) . . . . ? C40 N5 Ni1 N4 -139(2) . . . . ? C40 N5 Ni1 N3 103(2) . . . . ? C40 N5 Ni1 N2 -11(2) . . . . ? C40 N5 Ni1 N1 -5(3) . . . . ? C33 N4 Ni1 N5 19.2(4) . . . . ? C32 N4 Ni1 N5 -152.5(2) . . . . ? C33 N4 Ni1 N3 128.2(3) . . . . ? C32 N4 Ni1 N3 -43.4(3) . . . . ? C33 N4 Ni1 N2 -87.8(4) . . . . ? C32 N4 Ni1 N2 100.6(2) . . . . ? C33 N4 Ni1 N1 -157.3(3) . . . . ? C32 N4 Ni1 N1 31.1(2) . . . . ? C20 N3 Ni1 N5 16.0(3) . . . . ? C19 N3 Ni1 N5 -141.1(2) . . . . ? C20 N3 Ni1 N4 -94.1(3) . . . . ? C19 N3 Ni1 N4 108.8(2) . . . . ? C20 N3 Ni1 N2 117.3(3) . . . . ? C19 N3 Ni1 N2 -39.8(3) . . . . ? C20 N3 Ni1 N1 -168.7(3) . . . . ? C19 N3 Ni1 N1 34.2(2) . . . . ? C7 N2 Ni1 N5 11.2(4) . . . . ? C6 N2 Ni1 N5 -139.1(2) . . . . ? C7 N2 Ni1 N4 121.9(4) . . . . ? C6 N2 Ni1 N4 -28.4(3) . . . . ? C7 N2 Ni1 N3 -93.8(4) . . . . ? C6 N2 Ni1 N3 115.8(2) . . . . ? C7 N2 Ni1 N1 -168.3(4) . . . . ? C6 N2 Ni1 N1 41.4(2) . . . . ? C14 N1 Ni1 N5 73.9(15) . . . . ? C27 N1 Ni1 N5 -165.5(14) . . . . ? C1 N1 Ni1 N5 -45.8(16) . . . . ? C14 N1 Ni1 N4 -151.4(2) . . . . ? C27 N1 Ni1 N4 -30.8(2) . . . . ? C1 N1 Ni1 N4 88.9(2) . . . . ? C14 N1 Ni1 N3 -35.2(2) . . . . ? C27 N1 Ni1 N3 85.4(2) . . . . ? C1 N1 Ni1 N3 -154.9(2) . . . . ? C14 N1 Ni1 N2 80.0(2) . . . . ? C27 N1 Ni1 N2 -159.4(2) . . . . ? C1 N1 Ni1 N2 -39.7(2) . . . . ? C47 C42 P1 C54 -154.6(3) . . . . ? C43 C42 P1 C54 31.7(4) . . . . ? C47 C42 P1 C48 -31.5(4) . . . . ? C43 C42 P1 C48 154.8(3) . . . . ? C47 C42 P1 C60 87.5(4) . . . . ? C43 C42 P1 C60 -86.2(4) . . . . ? C55 C54 P1 C42 -81.0(4) . . . . ? C59 C54 P1 C42 97.3(4) . . . . ? C55 C54 P1 C48 157.7(4) . . . . ? C59 C54 P1 C48 -24.0(5) . . . . ? C55 C54 P1 C60 37.4(5) . . . . ? C59 C54 P1 C60 -144.2(4) . . . . ? C53 C48 P1 C42 135.5(3) . . . . ? C49 C48 P1 C42 -47.3(4) . . . . ? C53 C48 P1 C54 -101.8(4) . . . . ? C49 C48 P1 C54 75.3(4) . . . . ? C53 C48 P1 C60 17.2(4) . . . . ? C49 C48 P1 C60 -165.6(3) . . . . ? C61 C60 P1 C42 -11.1(4) . . . . ? C65 C60 P1 C42 169.4(4) . . . . ? C61 C60 P1 C54 -131.1(4) . . . . ? C65 C60 P1 C54 49.4(4) . . . . ? C61 C60 P1 C48 107.3(4) . . . . ? C65 C60 P1 C48 -72.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 1.401 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.067