data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H34 Cd N4 O4' _chemical_formula_sum 'C41 H34 Cd N4 O4' _chemical_formula_weight 759.12 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.867(3) _cell_length_b 17.127(3) _cell_length_c 11.970(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.268(3) _cell_angle_gamma 90.00 _cell_volume 3452.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6042 _cell_measurement_theta_min 2.927 _cell_measurement_theta_max 27.483 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11384 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3975 _reflns_number_gt 3700 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+3.1068P] 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 3975 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Cd1 Cd 0.0000 0.315045(10) 0.7500 0.02029(8) Uani 1 2 d S . . O1 O -0.05835(10) 0.21868(9) 0.86105(16) 0.0428(4) Uani 1 1 d . . . O2 O -0.06855(9) 0.33946(9) 0.91762(13) 0.0315(3) Uani 1 1 d . . . N1 N 0.0000 0.45822(14) 0.7500 0.0282(5) Uani 1 2 d S . . N2 N 0.37366(10) 1.16330(11) 1.15707(16) 0.0291(4) Uani 1 1 d . . . N4 N 0.0000 0.95444(14) 0.7500 0.0316(6) Uani 1 2 d S . . C1 C -0.01495(17) 0.49931(13) 0.8411(2) 0.0406(6) Uani 1 1 d . . . H1 H -0.0258 0.4722 0.9058 0.049 Uiso 1 1 calc R . . C2 C -0.01526(17) 0.57990(13) 0.8448(2) 0.0407(6) Uani 1 1 d . . . H2 H -0.0257 0.6058 0.9106 0.049 Uiso 1 1 calc R . . C3 C 0.0000 0.62162(16) 0.7500 0.0260(6) Uani 1 2 d S . . C6 C 0.0000 0.70810(17) 0.7500 0.0261(6) Uani 1 2 d S . . C7 C 0.06557(13) 0.74982(13) 0.7179(2) 0.0348(5) Uani 1 1 d . . . H7 H 0.1101 0.7231 0.6959 0.042 Uiso 1 1 calc R . . C8 C 0.06565(14) 0.83070(13) 0.7182(2) 0.0364(5) Uani 1 1 d . . . H8 H 0.1101 0.8578 0.6968 0.044 Uiso 1 1 calc R . . C9 C 0.0000 0.87104(16) 0.7500 0.0259(6) Uani 1 2 d S . . C12 C 0.32364(13) 1.11170(13) 1.2003(2) 0.0320(5) Uani 1 1 d . . . H12 H 0.3332 1.0965 1.2744 0.038 Uiso 1 1 calc R . . C13 C 0.35665(14) 1.18528(12) 1.0518(2) 0.0324(5) Uani 1 1 d . . . H13 H 0.3892 1.2222 1.0206 0.039 Uiso 1 1 calc R . . C14 C 0.29314(14) 1.15624(14) 0.9863(2) 0.0342(5) Uani 1 1 d . . . H14 H 0.2843 1.1737 0.9131 0.041 Uiso 1 1 calc R . . C15 C 0.24230(12) 1.10104(12) 1.02914(18) 0.0265(4) Uani 1 1 d . . . C16 C 0.25909(13) 1.08024(13) 1.14083(19) 0.0309(5) Uani 1 1 d . . . H16 H 0.2264 1.0449 1.1752 0.037 Uiso 1 1 calc R . . C17 C 0.17615(12) 1.06581(12) 0.95972(18) 0.0269(4) Uani 1 1 d . . . C18 C 0.14599(13) 1.10099(12) 0.86076(19) 0.0276(4) Uani 1 1 d . . . H18 H 0.1656 1.1495 0.8408 0.033 Uiso 1 1 calc R . . C19 C 0.08793(12) 1.06588(12) 0.79174(18) 0.0274(4) Uani 1 1 d . . . H19 H 0.0697 1.0902 0.7258 0.033 Uiso 1 1 calc R . . C20 C 0.05667(12) 0.99359(11) 0.82137(18) 0.0260(4) Uani 1 1 d . . . C21 C 0.08377(13) 0.95924(12) 0.9220(2) 0.0318(5) Uani 1 1 d . . . H21 H 0.0619 0.9122 0.9441 0.038 Uiso 1 1 calc R . . C22 C 0.14279(13) 0.99440(13) 0.9891(2) 0.0315(5) Uani 1 1 d . . . H22 H 0.1608 0.9701 1.0553 0.038 Uiso 1 1 calc R . . C34 C -0.09071(13) 0.27005(12) 0.91714(18) 0.0282(4) Uani 1 1 d . . . C35 C -0.16380(13) 0.24758(12) 0.98050(19) 0.0295(5) Uani 1 1 d . . . H35 H -0.1468 0.2095 1.0380 0.035 Uiso 1 1 calc R . . C36 C -0.22596(13) 0.20782(13) 0.9007(2) 0.0331(5) Uani 1 1 d . . . H36A H -0.2416 0.2435 0.8405 0.040 Uiso 1 1 calc R . . H36B H -0.2025 0.1621 0.8678 0.040 Uiso 1 1 calc R . . C37 C -0.29930(14) 0.18329(12) 0.9607(2) 0.0329(5) Uani 1 1 d . . . H37A H -0.2847 0.1433 1.0155 0.040 Uiso 1 1 calc R . . H37B H -0.3382 0.1611 0.9069 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01457(11) 0.02533(11) 0.02099(12) 0.000 0.00122(8) 0.000 O1 0.0442(10) 0.0331(8) 0.0538(11) -0.0038(8) 0.0278(9) -0.0012(7) O2 0.0303(8) 0.0334(7) 0.0314(9) -0.0021(6) 0.0081(7) -0.0066(6) N1 0.0330(13) 0.0248(11) 0.0270(14) 0.000 0.0023(11) 0.000 N2 0.0198(8) 0.0377(9) 0.0294(10) -0.0015(8) -0.0019(7) -0.0016(7) N4 0.0296(13) 0.0229(11) 0.0405(16) 0.000 -0.0137(11) 0.000 C1 0.0646(17) 0.0302(11) 0.0275(13) 0.0009(9) 0.0085(12) -0.0049(11) C2 0.0689(17) 0.0286(10) 0.0252(12) -0.0027(9) 0.0093(12) -0.0025(11) C3 0.0263(14) 0.0242(13) 0.0272(16) 0.000 -0.0007(12) 0.000 C6 0.0295(15) 0.0256(13) 0.0229(15) 0.000 -0.0015(12) 0.000 C7 0.0281(11) 0.0303(10) 0.0468(14) -0.0036(10) 0.0085(10) 0.0016(8) C8 0.0282(12) 0.0298(10) 0.0516(16) -0.0010(10) 0.0061(11) -0.0053(9) C9 0.0260(14) 0.0229(12) 0.0278(16) 0.000 -0.0071(12) 0.000 C12 0.0242(10) 0.0438(12) 0.0277(12) 0.0015(9) -0.0015(9) -0.0034(9) C13 0.0270(11) 0.0377(12) 0.0319(13) 0.0035(9) -0.0033(9) -0.0086(8) C14 0.0314(12) 0.0432(12) 0.0271(12) 0.0064(10) -0.0069(9) -0.0081(10) C15 0.0208(10) 0.0312(10) 0.0272(11) -0.0002(8) -0.0019(8) 0.0002(8) C16 0.0236(10) 0.0389(11) 0.0301(12) 0.0022(9) 0.0004(9) -0.0048(9) C17 0.0231(10) 0.0293(10) 0.0277(11) -0.0005(8) -0.0037(8) -0.0004(8) C18 0.0263(10) 0.0255(9) 0.0306(12) 0.0005(8) -0.0015(9) -0.0049(8) C19 0.0264(10) 0.0274(9) 0.0276(11) 0.0022(8) -0.0052(8) 0.0001(8) C20 0.0233(9) 0.0236(9) 0.0302(11) -0.0024(8) -0.0075(8) 0.0015(7) C21 0.0313(11) 0.0252(9) 0.0378(13) 0.0046(9) -0.0075(10) -0.0033(8) C22 0.0307(11) 0.0326(10) 0.0298(12) 0.0053(9) -0.0093(9) -0.0012(9) C34 0.0284(10) 0.0316(10) 0.0253(11) 0.0010(8) 0.0070(9) -0.0020(8) C35 0.0312(11) 0.0288(10) 0.0296(12) 0.0021(8) 0.0111(9) -0.0013(8) C36 0.0330(11) 0.0337(10) 0.0340(13) -0.0044(9) 0.0135(10) -0.0031(9) C37 0.0323(12) 0.0309(11) 0.0367(13) -0.0051(9) 0.0121(10) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.3683(16) 2_556 ? Cd1 O1 2.3683(16) . ? Cd1 N2 2.3761(19) 8_465 ? Cd1 N2 2.3761(19) 7_567 ? Cd1 O2 2.4087(15) . ? Cd1 O2 2.4087(15) 2_556 ? Cd1 N1 2.452(2) . ? Cd1 C34 2.699(2) 2_556 ? O1 C34 1.251(3) . ? O2 C34 1.246(3) . ? N1 C1 1.334(3) . ? N1 C1 1.334(3) 2_556 ? N2 C13 1.330(3) . ? N2 C12 1.345(3) . ? N2 Cd1 2.3761(18) 7_567 ? N4 C20 1.414(2) . ? N4 C20 1.414(2) 2_556 ? N4 C9 1.428(4) . ? C1 C2 1.381(3) . ? C1 H1 0.9300 . ? C2 C3 1.377(3) . ? C2 H2 0.9300 . ? C3 C2 1.377(3) 2_556 ? C3 C6 1.481(4) . ? C6 C7 1.389(3) . ? C6 C7 1.389(3) 2_556 ? C7 C8 1.385(3) . ? C7 H7 0.9300 . ? C8 C9 1.377(3) . ? C8 H8 0.9300 . ? C9 C8 1.377(3) 2_556 ? C12 C16 1.376(3) . ? C12 H12 0.9300 . ? C13 C14 1.383(3) . ? C13 H13 0.9300 . ? C14 C15 1.393(3) . ? C14 H14 0.9300 . ? C15 C16 1.397(3) . ? C15 C17 1.481(3) . ? C16 H16 0.9300 . ? C17 C18 1.399(3) . ? C17 C22 1.399(3) . ? C18 C19 1.382(3) . ? C18 H18 0.9300 . ? C19 C20 1.399(3) . ? C19 H19 0.9300 . ? C20 C21 1.394(3) . ? C21 C22 1.381(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C34 C35 1.533(3) . ? C35 C37 1.528(3) 7_457 ? C35 C36 1.537(3) . ? C35 H35 0.9800 . ? C36 C37 1.525(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C35 1.528(3) 7_457 ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 91.64(8) 2_556 . ? O1 Cd1 N2 103.67(7) 2_556 8_465 ? O1 Cd1 N2 88.92(7) . 8_465 ? O1 Cd1 N2 88.92(7) 2_556 7_567 ? O1 Cd1 N2 103.67(7) . 7_567 ? N2 Cd1 N2 162.04(9) 8_465 7_567 ? O1 Cd1 O2 145.39(5) 2_556 . ? O1 Cd1 O2 54.47(5) . . ? N2 Cd1 O2 84.41(6) 8_465 . ? N2 Cd1 O2 92.48(6) 7_567 . ? O1 Cd1 O2 54.47(5) 2_556 2_556 ? O1 Cd1 O2 145.39(5) . 2_556 ? N2 Cd1 O2 92.48(6) 8_465 2_556 ? N2 Cd1 O2 84.41(6) 7_567 2_556 ? O2 Cd1 O2 160.01(7) . 2_556 ? O1 Cd1 N1 134.18(4) 2_556 . ? O1 Cd1 N1 134.18(4) . . ? N2 Cd1 N1 81.02(5) 8_465 . ? N2 Cd1 N1 81.02(5) 7_567 . ? O2 Cd1 N1 80.00(4) . . ? O2 Cd1 N1 80.00(4) 2_556 . ? O1 Cd1 C34 27.60(6) 2_556 2_556 ? O1 Cd1 C34 119.23(6) . 2_556 ? N2 Cd1 C34 103.22(7) 8_465 2_556 ? N2 Cd1 C34 81.98(7) 7_567 2_556 ? O2 Cd1 C34 170.48(6) . 2_556 ? O2 Cd1 C34 27.49(6) 2_556 2_556 ? N1 Cd1 C34 106.59(4) . 2_556 ? C34 O1 Cd1 91.09(12) . . ? C34 O2 Cd1 89.35(12) . . ? C1 N1 C1 116.3(3) . 2_556 ? C1 N1 Cd1 121.85(13) . . ? C1 N1 Cd1 121.85(13) 2_556 . ? C13 N2 C12 116.35(19) . . ? C13 N2 Cd1 122.57(15) . 7_567 ? C12 N2 Cd1 119.20(15) . 7_567 ? C20 N4 C20 123.4(2) . 2_556 ? C20 N4 C9 118.30(12) . . ? C20 N4 C9 118.30(12) 2_556 . ? N1 C1 C2 123.7(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C2 117.5(3) 2_556 . ? C2 C3 C6 121.25(14) 2_556 . ? C2 C3 C6 121.25(14) . . ? C7 C6 C7 118.1(3) . 2_556 ? C7 C6 C3 120.95(14) . . ? C7 C6 C3 120.95(14) 2_556 . ? C6 C7 C8 121.0(2) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C8 119.8(3) 2_556 . ? C8 C9 N4 120.11(13) 2_556 . ? C8 C9 N4 120.11(13) . . ? N2 C12 C16 123.6(2) . . ? N2 C12 H12 118.2 . . ? C16 C12 H12 118.2 . . ? N2 C13 C14 123.6(2) . . ? N2 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 120.6(2) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 115.4(2) . . ? C16 C15 C17 122.56(19) . . ? C14 C15 C17 122.0(2) . . ? C12 C16 C15 120.4(2) . . ? C12 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C22 117.21(19) . . ? C18 C17 C15 121.71(18) . . ? C22 C17 C15 121.0(2) . . ? C19 C18 C17 121.99(19) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 119.9(2) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 118.9(2) . . ? C21 C20 N4 119.93(19) . . ? C19 C20 N4 121.19(19) . . ? C22 C21 C20 120.6(2) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C17 121.4(2) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? O2 C34 O1 122.25(18) . . ? O2 C34 C35 119.13(18) . . ? O1 C34 C35 118.48(18) . . ? C37 C35 C34 113.17(17) 7_457 . ? C37 C35 C36 110.38(19) 7_457 . ? C34 C35 C36 110.07(18) . . ? C37 C35 H35 107.7 7_457 . ? C34 C35 H35 107.7 . . ? C36 C35 H35 107.7 . . ? C37 C36 C35 111.84(19) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C35 111.48(17) . 7_457 ? C36 C37 H37A 109.3 . . ? C35 C37 H37A 109.3 7_457 . ? C36 C37 H37B 109.3 . . ? C35 C37 H37B 109.3 7_457 . ? H37A C37 H37B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 O1 C34 -178.26(18) 2_556 . . . ? N2 Cd1 O1 C34 -74.61(15) 8_465 . . . ? N2 Cd1 O1 C34 92.45(15) 7_567 . . . ? O2 Cd1 O1 C34 9.29(13) . . . . ? O2 Cd1 O1 C34 -167.42(13) 2_556 . . . ? N1 Cd1 O1 C34 1.74(18) . . . . ? C34 Cd1 O1 C34 -179.18(8) 2_556 . . . ? O1 Cd1 O2 C34 -22.68(19) 2_556 . . . ? O1 Cd1 O2 C34 -9.32(13) . . . . ? N2 Cd1 O2 C34 83.36(14) 8_465 . . . ? N2 Cd1 O2 C34 -114.38(14) 7_567 . . . ? O2 Cd1 O2 C34 165.19(13) 2_556 . . . ? N1 Cd1 O2 C34 165.19(13) . . . . ? C34 Cd1 O2 C34 -60.3(4) 2_556 . . . ? O1 Cd1 N1 C1 -157.49(17) 2_556 . . . ? O1 Cd1 N1 C1 22.51(17) . . . . ? N2 Cd1 N1 C1 102.14(16) 8_465 . . . ? N2 Cd1 N1 C1 -77.86(16) 7_567 . . . ? O2 Cd1 N1 C1 16.28(16) . . . . ? O2 Cd1 N1 C1 -163.72(16) 2_556 . . . ? C34 Cd1 N1 C1 -156.65(16) 2_556 . . . ? O1 Cd1 N1 C1 22.51(17) 2_556 . . 2_556 ? O1 Cd1 N1 C1 -157.49(17) . . . 2_556 ? N2 Cd1 N1 C1 -77.86(16) 8_465 . . 2_556 ? N2 Cd1 N1 C1 102.14(16) 7_567 . . 2_556 ? O2 Cd1 N1 C1 -163.72(16) . . . 2_556 ? O2 Cd1 N1 C1 16.28(16) 2_556 . . 2_556 ? C34 Cd1 N1 C1 23.35(16) 2_556 . . 2_556 ? C1 N1 C1 C2 -0.2(2) 2_556 . . . ? Cd1 N1 C1 C2 179.8(2) . . . . ? N1 C1 C2 C3 0.5(4) . . . . ? C1 C2 C3 C2 -0.2(2) . . . 2_556 ? C1 C2 C3 C6 179.8(2) . . . . ? C2 C3 C6 C7 -55.34(19) 2_556 . . . ? C2 C3 C6 C7 124.66(19) . . . . ? C2 C3 C6 C7 124.66(19) 2_556 . . 2_556 ? C2 C3 C6 C7 -55.34(19) . . . 2_556 ? C7 C6 C7 C8 0.16(18) 2_556 . . . ? C3 C6 C7 C8 -179.84(18) . . . . ? C6 C7 C8 C9 -0.3(4) . . . . ? C7 C8 C9 C8 0.16(18) . . . 2_556 ? C7 C8 C9 N4 -179.84(18) . . . . ? C20 N4 C9 C8 118.15(17) . . . 2_556 ? C20 N4 C9 C8 -61.85(17) 2_556 . . 2_556 ? C20 N4 C9 C8 -61.85(17) . . . . ? C20 N4 C9 C8 118.15(17) 2_556 . . . ? C13 N2 C12 C16 1.8(3) . . . . ? Cd1 N2 C12 C16 -162.98(17) 7_567 . . . ? C12 N2 C13 C14 -2.0(3) . . . . ? Cd1 N2 C13 C14 162.21(19) 7_567 . . . ? N2 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 1.8(3) . . . . ? C13 C14 C15 C17 -176.9(2) . . . . ? N2 C12 C16 C15 0.2(3) . . . . ? C14 C15 C16 C12 -2.0(3) . . . . ? C17 C15 C16 C12 176.7(2) . . . . ? C16 C15 C17 C18 161.9(2) . . . . ? C14 C15 C17 C18 -19.4(3) . . . . ? C16 C15 C17 C22 -20.0(3) . . . . ? C14 C15 C17 C22 158.6(2) . . . . ? C22 C17 C18 C19 -2.6(3) . . . . ? C15 C17 C18 C19 175.59(19) . . . . ? C17 C18 C19 C20 1.1(3) . . . . ? C18 C19 C20 C21 1.5(3) . . . . ? C18 C19 C20 N4 -176.94(18) . . . . ? C20 N4 C20 C21 149.7(2) 2_556 . . . ? C9 N4 C20 C21 -30.3(2) . . . . ? C20 N4 C20 C19 -31.92(15) 2_556 . . . ? C9 N4 C20 C19 148.08(15) . . . . ? C19 C20 C21 C22 -2.6(3) . . . . ? N4 C20 C21 C22 175.82(19) . . . . ? C20 C21 C22 C17 1.2(3) . . . . ? C18 C17 C22 C21 1.4(3) . . . . ? C15 C17 C22 C21 -176.8(2) . . . . ? Cd1 O2 C34 O1 17.2(2) . . . . ? Cd1 O2 C34 C35 -158.35(19) . . . . ? Cd1 O1 C34 O2 -17.5(2) . . . . ? Cd1 O1 C34 C35 158.07(19) . . . . ? O2 C34 C35 C37 -0.6(3) . . . 7_457 ? O1 C34 C35 C37 -176.2(2) . . . 7_457 ? O2 C34 C35 C36 123.5(2) . . . . ? O1 C34 C35 C36 -52.2(3) . . . . ? C37 C35 C36 C37 -55.3(3) 7_457 . . . ? C34 C35 C36 C37 179.11(18) . . . . ? C35 C36 C37 C35 55.9(3) . . . 7_457 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.945 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.076 # === END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H78 Co2 N8 O9' _chemical_formula_sum 'C86 H78 Co2 N8 O9' _chemical_formula_weight 1485.42 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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0956(15) _cell_length_b 13.3473(15) _cell_length_c 21.610(2) _cell_angle_alpha 103.591(2) _cell_angle_beta 100.939(2) _cell_angle_gamma 91.078(2) _cell_volume 3596.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5226 _cell_measurement_theta_min 2.219 _cell_measurement_theta_max 26.155 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19173 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13730 _reflns_number_gt 9815 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.8800P] 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 13730 _refine_ls_number_parameters 970 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 1.0518(2) 1.3934(2) 0.22769(14) 0.0370(7) Uani 1 1 d . . . C2 C 0.9873(3) 1.4716(3) 0.24522(16) 0.0470(8) Uani 1 1 d . . . H2 H 0.9722 1.5194 0.2202 0.056 Uiso 1 1 calc R . . C3 C 0.9456(3) 1.4787(3) 0.29978(14) 0.0430(7) Uani 1 1 d . . . H3 H 0.9002 1.5300 0.3098 0.052 Uiso 1 1 calc R . . C4 C 1.0251(3) 1.3370(3) 0.32097(16) 0.0492(8) Uani 1 1 d . . . H4 H 1.0367 1.2892 0.3463 0.059 Uiso 1 1 calc R . . C5 C 1.0676(3) 1.3247(3) 0.26696(16) 0.0470(8) Uani 1 1 d . . . H5 H 1.1080 1.2691 0.2563 0.056 Uiso 1 1 calc R . . C6 C 1.2343(3) 1.7024(3) -0.11532(15) 0.0517(9) Uani 1 1 d . . . C7 C 1.3019(3) 1.7160(3) -0.15623(17) 0.0567(10) Uani 1 1 d . . . H7 H 1.3482 1.6659 -0.1670 0.068 Uiso 1 1 calc R . . C8 C 1.3007(4) 1.8016(3) -0.1804(2) 0.0637(10) Uani 1 1 d . . . H8 H 1.3494 1.8091 -0.2055 0.076 Uiso 1 1 calc R . . C9 C 1.1692(4) 1.8626(4) -0.1336(2) 0.0671(11) Uani 1 1 d . . . H9 H 1.1215 1.9126 -0.1261 0.080 Uiso 1 1 calc R . . C10 C 1.1655(4) 1.7805(3) -0.1049(2) 0.0654(11) Uani 1 1 d . . . H10 H 1.1173 1.7774 -0.0787 0.079 Uiso 1 1 calc R . . C11 C 1.5381(3) 1.0737(3) -0.06141(19) 0.0570(9) Uani 1 1 d . . . C12 C 1.6183(3) 1.0461(3) -0.0188(2) 0.0635(10) Uani 1 1 d . . . H12 H 1.6243 1.0752 0.0253 0.076 Uiso 1 1 calc R . . C13 C 1.6899(3) 0.9779(3) -0.0381(2) 0.0634(10) Uani 1 1 d . . . H13 H 1.7444 0.9649 -0.0072 0.076 Uiso 1 1 calc R . . C14 C 1.6095(3) 0.9539(4) -0.1424(2) 0.0752(13) Uani 1 1 d . . . H14 H 1.6059 0.9241 -0.1863 0.090 Uiso 1 1 calc R . . C15 C 1.5347(3) 1.0236(3) -0.1248(2) 0.0713(12) Uani 1 1 d . . . H15 H 1.4817 1.0358 -0.1569 0.086 Uiso 1 1 calc R . . C16 C 1.1998(3) 1.3763(3) 0.06477(15) 0.0427(7) Uani 1 1 d . . . C17 C 1.1786(3) 1.4713(3) 0.10148(16) 0.0512(9) Uani 1 1 d . . . H17 H 1.1966 1.5323 0.0912 0.061 Uiso 1 1 calc R . . C18 C 1.1305(3) 1.4738(3) 0.15353(17) 0.0489(8) Uani 1 1 d . . . H18 H 1.1162 1.5374 0.1777 0.059 Uiso 1 1 calc R . . C19 C 1.1032(2) 1.3860(2) 0.17081(14) 0.0368(7) Uani 1 1 d . . . C20 C 1.1281(3) 1.2945(3) 0.13533(16) 0.0485(8) Uani 1 1 d . . . H20 H 1.1139 1.2340 0.1474 0.058 Uiso 1 1 calc R . . C21 C 1.1743(3) 1.2882(3) 0.08149(15) 0.0456(8) Uani 1 1 d . . . H21 H 1.1875 1.2242 0.0572 0.055 Uiso 1 1 calc R . . C22 C 1.2438(3) 1.4525(3) -0.02194(15) 0.0449(8) Uani 1 1 d . . . C23 C 1.3323(3) 1.4913(3) -0.03717(17) 0.0504(8) Uani 1 1 d . . . H23 H 1.3960 1.4643 -0.0254 0.060 Uiso 1 1 calc R . . C24 C 1.3275(3) 1.5683(3) -0.06910(16) 0.0476(8) Uani 1 1 d . . . H24 H 1.3874 1.5899 -0.0809 0.057 Uiso 1 1 calc R . . C25 C 1.2349(3) 1.6155(3) -0.08468(15) 0.0467(8) Uani 1 1 d . . . C26 C 1.1480(3) 1.5763(3) -0.06900(18) 0.0555(9) Uani 1 1 d . . . H26 H 1.0849 1.6053 -0.0794 0.067 Uiso 1 1 calc R . . C27 C 1.1499(3) 1.4978(3) -0.03921(18) 0.0557(9) Uani 1 1 d . . . H27 H 1.0888 1.4736 -0.0301 0.067 Uiso 1 1 calc R . . C28 C 1.3198(3) 1.2955(3) -0.00519(16) 0.0457(8) Uani 1 1 d . . . C29 C 1.4004(3) 1.2754(3) 0.03944(18) 0.0551(9) Uani 1 1 d . . . H29 H 1.4079 1.3109 0.0827 0.066 Uiso 1 1 calc R . . C30 C 1.4704(3) 1.2045(3) 0.02228(18) 0.0559(9) Uani 1 1 d . . . H30 H 1.5245 1.1930 0.0540 0.067 Uiso 1 1 calc R . . C31 C 1.4623(3) 1.1494(3) -0.04165(17) 0.0497(8) Uani 1 1 d . . . C32 C 1.3824(3) 1.1698(3) -0.08575(18) 0.0569(9) Uani 1 1 d . . . H32 H 1.3744 1.1338 -0.1290 0.068 Uiso 1 1 calc R . . C33 C 1.3118(3) 1.2427(3) -0.06878(17) 0.0550(9) Uani 1 1 d . . . H33 H 1.2589 1.2558 -0.1007 0.066 Uiso 1 1 calc R . . C34 C 0.5054(3) 0.7537(2) 0.69118(14) 0.0423(8) Uani 1 1 d . . . C35 C 0.6029(3) 0.7950(3) 0.68664(17) 0.0478(8) Uani 1 1 d . . . H35 H 0.6639 0.7664 0.7020 0.057 Uiso 1 1 calc R . . C36 C 0.6072(3) 0.8769(3) 0.65967(15) 0.0444(8) Uani 1 1 d . C . H36 H 0.6724 0.9013 0.6564 0.053 Uiso 1 1 calc R . . C37 C 0.4331(3) 0.8883(2) 0.64473(14) 0.0396(7) Uani 1 1 d . C . H37 H 0.3743 0.9220 0.6318 0.048 Uiso 1 1 calc R . . C38 C 0.4196(3) 0.8050(3) 0.66974(16) 0.0438(8) Uani 1 1 d . . . H38 H 0.3532 0.7828 0.6724 0.053 Uiso 1 1 calc R . . C39 C 0.1002(3) 0.1319(3) 0.74036(17) 0.0564(9) Uani 1 1 d . . . C40 C 0.0000(3) 0.1623(3) 0.71530(18) 0.0562(9) Uani 1 1 d . . . H40 H -0.0063 0.2260 0.7050 0.067 Uiso 1 1 calc R . . C41 C -0.0875(4) 0.0976(3) 0.7062(2) 0.0674(11) Uani 1 1 d . . . H41 H -0.1520 0.1189 0.6896 0.081 Uiso 1 1 calc R . . C42 C 0.0093(4) -0.0231(4) 0.7397(2) 0.0721(12) Uani 1 1 d . . . H42 H 0.0131 -0.0895 0.7462 0.086 Uiso 1 1 calc R . . C43 C 0.0996(4) 0.0359(3) 0.7509(2) 0.0651(11) Uani 1 1 d . . . H43 H 0.1623 0.0098 0.7660 0.078 Uiso 1 1 calc R . . C44 C 0.8403(3) 0.2113(3) 0.8876(2) 0.0625(10) Uani 1 1 d . . . C45 C 0.8425(4) 0.1506(3) 0.9290(2) 0.0672(11) Uani 1 1 d . . . H45 H 0.7828 0.1394 0.9445 0.081 Uiso 1 1 calc R . . C46 C 0.9330(4) 0.1039(4) 0.9492(2) 0.0682(11) Uani 1 1 d . . . H46 H 0.9256 0.0559 0.9733 0.082 Uiso 1 1 calc R . . C47 C 1.0258(4) 0.1875(3) 0.9016(2) 0.0690(11) Uani 1 1 d . . . H47 H 1.0897 0.2035 0.8923 0.083 Uiso 1 1 calc R . . C48 C 0.9401(3) 0.2339(3) 0.8775(2) 0.0663(11) Uani 1 1 d . . . H48 H 0.9481 0.2820 0.8536 0.080 Uiso 1 1 calc R . . C49 C 0.4943(3) 0.6612(3) 0.71682(15) 0.0424(8) Uani 1 1 d . . . C50 C 0.4093(3) 0.5931(3) 0.69471(15) 0.0463(8) Uani 1 1 d . . . H50 H 0.3555 0.6074 0.6638 0.056 Uiso 1 1 calc R . . C51 C 0.3985(3) 0.5047(3) 0.71532(16) 0.0482(8) Uani 1 1 d . . . H51 H 0.3385 0.4609 0.6988 0.058 Uiso 1 1 calc R . . C52 C 0.4795(3) 0.4807(3) 0.76197(16) 0.0480(8) Uani 1 1 d . . . C53 C 0.5653(3) 0.5508(3) 0.78574(16) 0.0536(10) Uani 1 1 d . . . H53 H 0.6182 0.5382 0.8177 0.064 Uiso 1 1 calc R . . C54 C 0.5748(3) 0.6373(3) 0.76406(16) 0.0502(9) Uani 1 1 d . . . H54 H 0.6346 0.6813 0.7803 0.060 Uiso 1 1 calc R . . C55 C 0.3794(3) 0.3271(3) 0.77266(16) 0.0468(8) Uani 1 1 d . . . C56 C 0.2869(3) 0.3673(3) 0.78405(17) 0.0508(9) Uani 1 1 d . . . H56 H 0.2848 0.4383 0.7993 0.061 Uiso 1 1 calc R . . C57 C 0.1975(3) 0.3049(3) 0.77334(17) 0.0526(9) Uani 1 1 d . . . H57 H 0.1358 0.3340 0.7811 0.063 Uiso 1 1 calc R . . C58 C 0.1988(3) 0.1995(3) 0.75112(17) 0.0506(9) Uani 1 1 d . . . C59 C 0.2898(3) 0.1601(3) 0.74202(19) 0.0571(10) Uani 1 1 d . . . H59 H 0.2928 0.0888 0.7295 0.068 Uiso 1 1 calc R . . C60 C 0.3782(3) 0.2222(3) 0.7507(2) 0.0584(10) Uani 1 1 d . . . H60 H 0.4390 0.1924 0.7415 0.070 Uiso 1 1 calc R . . C61 C 0.7437(3) 0.2583(3) 0.86086(19) 0.0559(9) Uani 1 1 d . . . C62 C 0.7273(3) 0.2709(3) 0.79821(19) 0.0597(10) Uani 1 1 d . . . H62 H 0.7763 0.2495 0.7727 0.072 Uiso 1 1 calc R . . C63 C 0.6398(3) 0.3147(3) 0.7729(2) 0.0624(11) Uani 1 1 d . . . H63 H 0.6296 0.3218 0.7304 0.075 Uiso 1 1 calc R . . C64 C 0.5676(3) 0.3478(3) 0.81006(17) 0.0506(9) Uani 1 1 d . . . C65 C 0.5825(3) 0.3335(3) 0.87223(17) 0.0508(9) Uani 1 1 d . . . H65 H 0.5332 0.3545 0.8976 0.061 Uiso 1 1 calc R . . C66 C 0.6687(3) 0.2888(3) 0.89685(18) 0.0483(8) Uani 1 1 d . . . H66 H 0.6770 0.2789 0.9386 0.058 Uiso 1 1 calc R . . C67 C 0.7192(2) 1.3314(2) 0.56203(16) 0.0377(7) Uani 1 1 d . . . C69 C 0.6086(3) 1.4084(3) 0.48336(18) 0.0486(8) Uani 1 1 d . . . H69A H 0.5756 1.4730 0.4838 0.058 Uiso 1 1 calc R A 1 H69B H 0.6211 1.3805 0.4400 0.058 Uiso 1 1 calc R A 1 C70 C 0.5394(3) 1.3347(3) 0.50027(19) 0.0505(9) Uani 1 1 d . C . H70A H 0.5219 1.2729 0.4651 0.061 Uiso 1 1 calc R B 1 H70B H 0.4754 1.3658 0.5086 0.061 Uiso 1 1 calc R B 1 C72 C 0.8053(2) 1.4460(2) 0.50382(17) 0.0377(7) Uani 1 1 d . . . C68A C 0.7125(2) 1.4280(2) 0.53272(16) 0.0388(7) Uani 0.566(8) 1 d P C 1 H68A H 0.7098 1.4848 0.5658 0.047 Uiso 0.566(8) 1 d PR C 1 C71A C 0.6023(2) 1.3078(2) 0.56305(17) 0.0397(7) Uani 0.566(8) 1 d P C 1 C73A C 0.5577(5) 1.3840(5) 0.6113(4) 0.057(2) Uani 0.566(8) 1 d P C 1 H73A H 0.4859 1.3634 0.6083 0.085 Uiso 0.566(8) 1 calc PR C 1 H73B H 0.5623 1.4510 0.6025 0.085 Uiso 0.566(8) 1 calc PR C 1 H73C H 0.5960 1.3868 0.6543 0.085 Uiso 0.566(8) 1 calc PR C 1 C68B C 0.7125(2) 1.4280(2) 0.53272(16) 0.0388(7) Uani 0.434(8) 1 d P C 2 C71B C 0.6023(2) 1.3078(2) 0.56305(17) 0.0397(7) Uani 0.434(8) 1 d P C 2 H71B H 0.5841 1.3496 0.5978 0.048 Uiso 0.434(8) 1 d PR C 2 C73B C 0.6981(7) 1.5228(6) 0.5875(4) 0.047(2) Uani 0.434(8) 1 d P C 2 H73D H 0.6939 1.5836 0.5708 0.071 Uiso 0.434(8) 1 calc PR C 2 H73E H 0.7565 1.5320 0.6231 0.071 Uiso 0.434(8) 1 calc PR C 2 H73F H 0.6352 1.5112 0.6021 0.071 Uiso 0.434(8) 1 calc PR C 2 C74 C 0.7908(3) 1.3470(3) 0.62997(19) 0.0653(11) Uani 1 1 d . C . H74A H 0.7857 1.2857 0.6454 0.098 Uiso 1 1 calc R . . H74B H 0.7695 1.4044 0.6597 0.098 Uiso 1 1 calc R . . H74C H 0.8617 1.3607 0.6268 0.098 Uiso 1 1 calc R . . C75 C 0.7595(3) 1.2417(3) 0.51572(18) 0.0485(8) Uani 1 1 d . C . H75A H 0.8300 1.2592 0.5136 0.073 Uiso 1 1 calc R . . H75B H 0.7163 1.2294 0.4731 0.073 Uiso 1 1 calc R . . H75C H 0.7574 1.1804 0.5316 0.073 Uiso 1 1 calc R . . C76 C 0.5747(2) 1.1973(2) 0.56334(15) 0.0345(6) Uani 1 1 d . . . C77 C 0.7943(3) 0.7934(3) 0.47411(17) 0.0448(8) Uani 1 1 d . . . C79 C 0.8756(3) 0.9581(3) 0.54006(18) 0.0510(9) Uani 1 1 d . . . H79A H 0.8501 0.9707 0.5804 0.061 Uiso 1 1 calc R D 1 H79B H 0.9042 1.0229 0.5354 0.061 Uiso 1 1 calc R D 1 C80 C 0.9636(3) 0.8728(3) 0.53922(18) 0.0497(8) Uani 1 1 d . F . H80A H 1.0285 0.9003 0.5324 0.060 Uiso 1 1 calc R E 1 H80B H 0.9768 0.8506 0.5795 0.060 Uiso 1 1 calc R E 1 C82 C 0.6826(2) 0.9466(2) 0.49134(15) 0.0350(7) Uani 1 1 d . . . C78A C 0.7886(2) 0.9107(2) 0.48255(16) 0.0381(7) Uani 0.623(8) 1 d P F 1 H78A H 0.8056 0.9271 0.4462 0.046 Uiso 0.623(8) 1 d PR F 1 C81A C 0.9146(2) 0.7854(2) 0.48276(15) 0.0365(7) Uani 0.623(8) 1 d P F 1 C83A C 0.9331(5) 0.8009(5) 0.4182(3) 0.0544(19) Uani 0.623(8) 1 d P F 1 H83C H 0.8733 0.8292 0.3971 0.065 Uiso 0.623(8) 1 calc PR F 1 H83D H 0.9445 0.7357 0.3911 0.065 Uiso 0.623(8) 1 calc PR F 1 H83A H 0.9933 0.8477 0.4257 0.065 Uiso 0.623(8) 1 calc PR F 1 C78B C 0.7886(2) 0.9107(2) 0.48255(16) 0.0381(7) Uani 0.377(8) 1 d P F 2 C81B C 0.9146(2) 0.7854(2) 0.48276(15) 0.0365(7) Uani 0.377(8) 1 d P F 2 H81B H 0.9316 0.7961 0.4441 0.044 Uiso 0.377(8) 1 d PR F 2 C83B C 0.8228(7) 0.9427(9) 0.4246(5) 0.055(3) Uani 0.377(8) 1 d P F 2 H83E H 0.8975 0.9487 0.4318 0.066 Uiso 0.377(8) 1 calc PR F 2 H83F H 0.7960 1.0080 0.4210 0.066 Uiso 0.377(8) 1 calc PR F 2 H83B H 0.7961 0.8913 0.3853 0.066 Uiso 0.377(8) 1 calc PR F 2 C84 C 0.7329(4) 0.7319(3) 0.4070(2) 0.0755(14) Uani 1 1 d . F . H84D H 0.6929 0.6746 0.4124 0.113 Uiso 1 1 calc R . . H84E H 0.7808 0.7067 0.3793 0.113 Uiso 1 1 calc R . . H84F H 0.6868 0.7762 0.3877 0.113 Uiso 1 1 calc R . . C85 C 0.7534(3) 0.7557(3) 0.5282(2) 0.0590(10) Uani 1 1 d . F . H85A H 0.7957 0.7884 0.5697 0.089 Uiso 1 1 calc R . . H85B H 0.7567 0.6821 0.5207 0.089 Uiso 1 1 calc R . . H85C H 0.6825 0.7732 0.5276 0.089 Uiso 1 1 calc R . . C86 C 0.9423(2) 0.6774(2) 0.48761(13) 0.0294(6) Uani 1 1 d . . . Co1 Co 0.94547(3) 1.45598(3) 0.434814(18) 0.02907(10) Uani 1 1 d . . . Co2 Co 0.52928(3) 1.01970(3) 0.573016(19) 0.03072(10) Uani 1 1 d . . . N1 N 0.96729(19) 1.4160(2) 0.33836(12) 0.0351(5) Uani 1 1 d . C . N2 N 1.2341(3) 1.8753(3) -0.17033(17) 0.0676(9) Uani 1 1 d . . . N3 N 1.6824(3) 0.9295(3) -0.10097(17) 0.0645(9) Uani 1 1 d . . . N4 N 0.5245(2) 0.9247(2) 0.63758(11) 0.0378(6) Uani 1 1 d . . . N5 N -0.0836(3) 0.0083(3) 0.72006(19) 0.0741(10) Uani 1 1 d . . . N6 N 1.0208(3) 0.1171(3) 0.93979(17) 0.0651(9) Uani 1 1 d . . . N7 N 1.2494(2) 1.3732(2) 0.01020(14) 0.0515(7) Uani 1 1 d . . . N8 N 0.4746(3) 0.3921(2) 0.78642(15) 0.0516(7) Uani 1 1 d . . . O1 O 0.88863(17) 1.48717(18) 0.54271(12) 0.0473(6) Uani 1 1 d . . . O2 O 0.79697(18) 1.4186(2) 0.44097(12) 0.0516(6) Uani 1 1 d . C . O3 O 0.59089(18) 1.16850(17) 0.61537(10) 0.0420(5) Uani 1 1 d . C . O4 O 0.54026(17) 1.13220(15) 0.51095(10) 0.0364(5) Uani 1 1 d . . . O5 O 0.65919(16) 0.96448(17) 0.54555(10) 0.0381(5) Uani 1 1 d . F . O6 O 0.61912(16) 0.95194(15) 0.43854(10) 0.0334(4) Uani 1 1 d . . . O7 O 0.92088(17) 0.60421(16) 0.43731(10) 0.0371(5) Uani 1 1 d . . . O8 O 0.99528(16) 0.66869(15) 0.54094(9) 0.0345(4) Uani 1 1 d . . . O9 O 0.8175(2) 0.8871(2) 0.78924(15) 0.0742(8) Uani 1 1 d . . . H9B H 0.8379 0.9340 0.7728 0.089 Uiso 1 1 d R . . H9C H 0.7948 0.9148 0.8232 0.089 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0416(17) 0.0409(17) 0.0288(15) 0.0090(13) 0.0065(13) 0.0042(13) C2 0.059(2) 0.050(2) 0.0377(17) 0.0151(15) 0.0151(15) 0.0153(16) C3 0.051(2) 0.052(2) 0.0319(16) 0.0176(14) 0.0132(14) 0.0101(15) C4 0.066(2) 0.046(2) 0.0402(18) 0.0151(15) 0.0157(16) 0.0168(17) C5 0.071(2) 0.0374(18) 0.0401(17) 0.0154(14) 0.0198(16) 0.0173(16) C6 0.068(2) 0.059(2) 0.0287(16) 0.0158(16) 0.0054(16) 0.0139(18) C7 0.069(3) 0.064(2) 0.0391(19) 0.0138(17) 0.0135(17) 0.014(2) C8 0.075(3) 0.062(3) 0.061(2) 0.022(2) 0.020(2) 0.015(2) C9 0.070(3) 0.069(3) 0.067(3) 0.021(2) 0.015(2) 0.021(2) C10 0.078(3) 0.054(2) 0.069(3) 0.017(2) 0.022(2) 0.019(2) C11 0.068(3) 0.046(2) 0.057(2) 0.0078(17) 0.0161(19) 0.0093(18) C12 0.061(3) 0.059(2) 0.072(3) 0.011(2) 0.021(2) 0.016(2) C13 0.061(3) 0.068(3) 0.064(2) 0.016(2) 0.021(2) 0.013(2) C14 0.062(3) 0.078(3) 0.069(3) -0.011(2) 0.009(2) 0.016(2) C15 0.062(3) 0.063(3) 0.073(3) -0.016(2) 0.011(2) 0.014(2) C16 0.0443(19) 0.051(2) 0.0374(17) 0.0127(15) 0.0153(14) 0.0112(15) C17 0.076(3) 0.0415(19) 0.0429(18) 0.0153(15) 0.0225(18) 0.0046(17) C18 0.058(2) 0.0442(19) 0.0458(19) 0.0094(15) 0.0151(16) 0.0119(16) C19 0.0407(17) 0.0431(17) 0.0291(15) 0.0118(13) 0.0086(13) 0.0105(13) C20 0.066(2) 0.0425(19) 0.0427(18) 0.0132(15) 0.0219(17) 0.0076(16) C21 0.059(2) 0.0453(19) 0.0360(17) 0.0106(14) 0.0154(15) 0.0163(16) C22 0.050(2) 0.057(2) 0.0319(16) 0.0143(15) 0.0127(14) 0.0129(16) C23 0.056(2) 0.052(2) 0.049(2) 0.0139(16) 0.0217(17) 0.0167(17) C24 0.054(2) 0.053(2) 0.0400(18) 0.0138(16) 0.0148(16) 0.0124(16) C25 0.060(2) 0.048(2) 0.0324(16) 0.0106(14) 0.0089(15) 0.0118(16) C26 0.054(2) 0.063(2) 0.052(2) 0.0168(18) 0.0132(17) 0.0188(18) C27 0.050(2) 0.070(3) 0.053(2) 0.0221(19) 0.0150(17) 0.0181(18) C28 0.055(2) 0.050(2) 0.0382(17) 0.0168(15) 0.0165(15) 0.0120(16) C29 0.062(2) 0.064(2) 0.0402(18) 0.0102(17) 0.0127(17) 0.0171(19) C30 0.062(2) 0.060(2) 0.047(2) 0.0106(18) 0.0136(18) 0.0123(18) C31 0.065(2) 0.0398(19) 0.0464(19) 0.0118(15) 0.0151(17) 0.0075(16) C32 0.073(3) 0.057(2) 0.0402(19) 0.0069(17) 0.0150(18) 0.0108(19) C33 0.068(3) 0.065(2) 0.0349(18) 0.0145(17) 0.0133(17) 0.0145(19) C34 0.063(2) 0.0404(17) 0.0289(15) 0.0145(13) 0.0148(14) 0.0111(15) C35 0.047(2) 0.048(2) 0.0486(19) 0.0133(16) 0.0067(15) 0.0117(15) C36 0.0382(18) 0.058(2) 0.0388(17) 0.0197(15) 0.0035(14) 0.0035(15) C37 0.0498(19) 0.0416(17) 0.0349(16) 0.0156(13) 0.0178(14) 0.0160(14) C38 0.052(2) 0.0438(18) 0.0431(18) 0.0181(15) 0.0185(15) 0.0145(15) C39 0.070(3) 0.059(2) 0.0393(19) 0.0149(17) 0.0044(17) 0.0053(19) C40 0.065(2) 0.055(2) 0.052(2) 0.0134(17) 0.0185(18) 0.0116(18) C41 0.071(3) 0.062(3) 0.067(3) 0.012(2) 0.012(2) 0.003(2) C42 0.075(3) 0.066(3) 0.067(3) 0.022(2) -0.012(2) -0.010(2) C43 0.066(3) 0.056(2) 0.064(3) 0.016(2) -0.009(2) -0.004(2) C44 0.063(3) 0.064(3) 0.065(3) 0.024(2) 0.014(2) 0.017(2) C45 0.064(3) 0.071(3) 0.071(3) 0.025(2) 0.012(2) 0.015(2) C46 0.064(3) 0.075(3) 0.068(3) 0.024(2) 0.010(2) 0.009(2) C47 0.059(3) 0.068(3) 0.074(3) 0.009(2) 0.009(2) 0.001(2) C48 0.067(3) 0.065(3) 0.066(3) 0.008(2) 0.018(2) 0.007(2) C49 0.063(2) 0.0386(17) 0.0312(15) 0.0144(13) 0.0142(15) 0.0125(15) C50 0.061(2) 0.051(2) 0.0280(15) 0.0139(14) 0.0064(15) 0.0069(17) C51 0.065(2) 0.047(2) 0.0352(17) 0.0145(15) 0.0107(16) 0.0068(17) C52 0.076(3) 0.0384(18) 0.0345(17) 0.0144(14) 0.0154(16) 0.0115(17) C53 0.081(3) 0.043(2) 0.0339(17) 0.0162(15) -0.0042(17) 0.0118(18) C54 0.065(2) 0.050(2) 0.0345(17) 0.0180(15) -0.0017(16) 0.0030(17) C55 0.065(2) 0.0379(18) 0.0397(18) 0.0125(14) 0.0118(16) 0.0147(16) C56 0.067(2) 0.0407(19) 0.048(2) 0.0140(16) 0.0143(18) 0.0146(17) C57 0.074(3) 0.045(2) 0.0435(19) 0.0153(16) 0.0159(18) 0.0181(18) C58 0.070(2) 0.043(2) 0.0397(18) 0.0084(15) 0.0135(17) 0.0101(17) C59 0.068(3) 0.0367(19) 0.065(2) 0.0153(17) 0.004(2) 0.0130(18) C60 0.058(2) 0.040(2) 0.070(3) 0.0080(18) 0.0003(19) 0.0166(17) C61 0.068(3) 0.043(2) 0.061(2) 0.0132(17) 0.0206(19) 0.0166(17) C62 0.067(3) 0.064(2) 0.056(2) 0.0206(19) 0.0218(19) 0.023(2) C63 0.074(3) 0.062(3) 0.058(2) 0.022(2) 0.020(2) 0.021(2) C64 0.068(2) 0.0382(18) 0.047(2) 0.0105(15) 0.0144(17) 0.0170(17) C65 0.062(2) 0.051(2) 0.0423(19) 0.0179(16) 0.0108(16) 0.0086(17) C66 0.057(2) 0.0449(19) 0.049(2) 0.0182(16) 0.0165(17) 0.0133(16) C67 0.0359(17) 0.0330(16) 0.0456(18) 0.0115(14) 0.0097(14) -0.0016(13) C69 0.0318(17) 0.060(2) 0.057(2) 0.0190(18) 0.0089(15) 0.0062(15) C70 0.045(2) 0.0378(18) 0.068(2) 0.0210(17) 0.0002(17) -0.0007(15) C72 0.0340(17) 0.0269(15) 0.056(2) 0.0101(14) 0.0182(15) 0.0051(12) C68A 0.0335(16) 0.0327(16) 0.0540(19) 0.0124(14) 0.0157(14) 0.0050(12) C71A 0.0367(17) 0.0274(15) 0.055(2) 0.0102(14) 0.0083(14) 0.0053(12) C73A 0.050(4) 0.045(4) 0.072(5) 0.005(3) 0.018(3) 0.005(3) C68B 0.0335(16) 0.0327(16) 0.0540(19) 0.0124(14) 0.0157(14) 0.0050(12) C71B 0.0367(17) 0.0274(15) 0.055(2) 0.0102(14) 0.0083(14) 0.0053(12) C73B 0.056(5) 0.030(4) 0.059(5) 0.002(3) 0.029(4) 0.002(3) C74 0.060(3) 0.068(3) 0.056(2) 0.013(2) -0.0129(19) -0.003(2) C75 0.046(2) 0.0398(18) 0.064(2) 0.0143(16) 0.0176(17) 0.0183(15) C76 0.0348(16) 0.0362(16) 0.0384(16) 0.0119(13) 0.0183(13) 0.0011(12) C77 0.0385(18) 0.0395(18) 0.056(2) 0.0125(15) 0.0061(15) 0.0108(14) C79 0.048(2) 0.046(2) 0.056(2) 0.0048(16) 0.0112(17) 0.0027(16) C80 0.047(2) 0.0401(19) 0.059(2) 0.0116(16) 0.0039(17) -0.0016(15) C82 0.0409(17) 0.0285(15) 0.0402(17) 0.0128(13) 0.0135(14) 0.0060(12) C78A 0.0392(18) 0.0349(16) 0.0423(17) 0.0109(13) 0.0108(14) 0.0078(13) C81A 0.0366(17) 0.0341(16) 0.0468(18) 0.0192(14) 0.0158(14) 0.0089(13) C83A 0.072(4) 0.049(3) 0.047(3) 0.024(3) 0.011(3) -0.021(3) C78B 0.0392(18) 0.0349(16) 0.0423(17) 0.0109(13) 0.0108(14) 0.0078(13) C81B 0.0366(17) 0.0341(16) 0.0468(18) 0.0192(14) 0.0158(14) 0.0089(13) C83B 0.039(5) 0.086(8) 0.046(5) 0.016(5) 0.020(4) -0.005(5) C84 0.069(3) 0.060(3) 0.066(3) -0.021(2) -0.017(2) 0.016(2) C85 0.059(2) 0.050(2) 0.078(3) 0.024(2) 0.025(2) 0.0032(18) C86 0.0319(15) 0.0339(15) 0.0316(15) 0.0125(12) 0.0221(12) 0.0146(12) Co1 0.0320(2) 0.0322(2) 0.02758(19) 0.01308(16) 0.00961(15) 0.00579(16) Co2 0.0341(2) 0.0311(2) 0.0344(2) 0.01811(17) 0.01191(16) 0.00636(16) N1 0.0340(14) 0.0414(14) 0.0321(13) 0.0103(11) 0.0099(10) 0.0035(11) N2 0.073(2) 0.066(2) 0.065(2) 0.0179(18) 0.0129(18) 0.0161(18) N3 0.060(2) 0.065(2) 0.064(2) 0.0014(17) 0.0205(17) 0.0113(17) N4 0.0472(16) 0.0411(14) 0.0292(13) 0.0150(11) 0.0093(11) 0.0104(12) N5 0.069(3) 0.070(2) 0.077(3) 0.017(2) -0.001(2) -0.0051(19) N6 0.063(2) 0.071(2) 0.063(2) 0.0155(18) 0.0184(17) 0.0161(18) N7 0.061(2) 0.0593(19) 0.0405(15) 0.0181(14) 0.0177(14) 0.0142(15) N8 0.069(2) 0.0350(15) 0.0542(18) 0.0154(13) 0.0128(15) 0.0139(14) O1 0.0341(13) 0.0453(13) 0.0648(15) 0.0159(12) 0.0132(11) -0.0031(10) O2 0.0368(13) 0.0646(16) 0.0578(15) 0.0162(13) 0.0179(11) 0.0064(11) O3 0.0577(15) 0.0372(12) 0.0349(11) 0.0119(9) 0.0148(10) 0.0001(10) O4 0.0459(13) 0.0280(11) 0.0401(12) 0.0137(9) 0.0134(10) 0.0030(9) O5 0.0347(11) 0.0439(12) 0.0423(12) 0.0197(10) 0.0118(9) 0.0118(9) O6 0.0363(11) 0.0326(11) 0.0375(11) 0.0152(9) 0.0132(9) 0.0113(8) O7 0.0456(13) 0.0384(12) 0.0320(11) 0.0131(9) 0.0126(9) 0.0150(9) O8 0.0409(12) 0.0326(11) 0.0322(11) 0.0111(9) 0.0082(9) 0.0077(9) O9 0.073(2) 0.076(2) 0.078(2) 0.0233(16) 0.0180(16) 0.0154(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.382(4) . ? C1 C2 1.384(4) . ? C1 C19 1.494(4) . ? C2 C3 1.375(4) . ? C2 H2 0.9300 . ? C3 N1 1.312(3) . ? C3 H3 0.9300 . ? C4 N1 1.334(3) . ? C4 C5 1.363(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.397(5) . ? C6 C7 1.402(5) . ? C6 C25 1.464(5) . ? C7 C8 1.362(5) . ? C7 H7 0.9300 . ? C8 N2 1.334(4) . ? C8 H8 0.9300 . ? C9 N2 1.303(4) . ? C9 C10 1.384(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C15 1.368(5) . ? C11 C12 1.376(6) . ? C11 C31 1.478(5) . ? C12 C13 1.373(5) . ? C12 H12 0.9300 . ? C13 N3 1.343(4) . ? C13 H13 0.9300 . ? C14 N3 1.283(5) . ? C14 C15 1.407(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.362(5) . ? C16 C17 1.393(5) . ? C16 N7 1.443(3) . ? C17 C18 1.384(5) . ? C17 H17 0.9300 . ? C18 C19 1.371(5) . ? C18 H18 0.9300 . ? C19 C20 1.363(4) . ? C20 C21 1.396(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.386(5) . ? C22 N7 1.392(3) . ? C22 C27 1.406(5) . ? C23 C24 1.362(5) . ? C23 H23 0.9300 . ? C24 C25 1.398(5) . ? C24 H24 0.9300 . ? C25 C26 1.375(5) . ? C26 C27 1.351(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.364(5) . ? C28 C33 1.372(5) . ? C28 N7 1.424(3) . ? C29 C30 1.368(5) . ? C29 H29 0.9300 . ? C30 C31 1.387(5) . ? C30 H30 0.9300 . ? C31 C32 1.354(5) . ? C32 C33 1.389(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C38 1.388(4) . ? C34 C35 1.410(5) . ? C34 C49 1.484(3) . ? C35 C36 1.358(5) . ? C35 H35 0.9300 . ? C36 N4 1.334(3) . ? C36 H36 0.9300 . ? C37 N4 1.333(3) . ? C37 C38 1.368(4) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C43 1.352(4) . ? C39 C40 1.426(5) . ? C39 C58 1.510(4) . ? C40 C41 1.377(5) . ? C40 H40 0.9300 . ? C41 N5 1.294(6) . ? C41 H41 0.9300 . ? C42 N5 1.319(6) . ? C42 C43 1.358(6) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.337(6) . ? C44 C48 1.404(6) . ? C44 C61 1.501(5) . ? C45 C46 1.395(6) . ? C45 H45 0.9300 . ? C46 N6 1.221(5) . ? C46 H46 0.9300 . ? C47 C48 1.368(6) . ? C47 N6 1.397(6) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.360(5) . ? C49 C54 1.418(5) . ? C50 C51 1.369(5) . ? C50 H50 0.9300 . ? C51 C52 1.416(5) . ? C51 H51 0.9300 . ? C52 C53 1.385(5) . ? C52 N8 1.409(4) . ? C53 C54 1.355(5) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.368(5) . ? C55 C56 1.375(5) . ? C55 N8 1.446(5) . ? C56 C57 1.374(5) . ? C56 H56 0.9300 . ? C57 C58 1.377(5) . ? C57 H57 0.9300 . ? C58 C59 1.340(5) . ? C59 C60 1.369(6) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C66 1.375(5) . ? C61 C62 1.381(5) . ? C62 C63 1.375(5) . ? C62 H62 0.9300 . ? C63 C64 1.368(5) . ? C63 H63 0.9300 . ? C64 C65 1.379(5) . ? C64 N8 1.423(5) . ? C65 C66 1.364(5) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C75 1.542(4) . ? C67 C74 1.551(5) . ? C67 C68A 1.561(4) . ? C67 C71A 1.563(4) . ? C69 C70 1.478(5) . ? C69 C68A 1.537(5) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71A 1.569(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C72 O1 1.270(4) . ? C72 O2 1.304(4) . ? C72 C68A 1.507(4) . ? C68A H68A 0.9193 . ? C71A C73A 1.490(7) . ? C71A C76 1.514(4) . ? C71A H71B 0.8978 . ? C73A H73A 0.9600 . ? C73A H73B 0.9600 . ? C73A H73C 0.9600 . ? C73A H71B 0.6314 . ? C73B H68A 0.6459 . ? C73B H73D 0.9600 . ? C73B H73E 0.9600 . ? C73B H73F 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 O4 1.253(4) . ? C76 O3 1.254(4) . ? C76 Co2 2.499(3) . ? C77 C78A 1.538(4) . ? C77 C84 1.548(5) . ? C77 C85 1.552(5) . ? C77 C81A 1.559(4) . ? C79 C78A 1.519(5) . ? C79 C80 1.634(5) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81A 1.506(5) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C82 O5 1.237(4) . ? C82 O6 1.295(4) . ? C82 C78A 1.509(4) . ? C78A H78A 0.9276 . ? C81A C86 1.516(4) . ? C81A C83A 1.520(6) . ? C81A H81B 0.9454 . ? C83A H83C 0.9600 . ? C83A H83D 0.9600 . ? C83A H83A 0.9600 . ? C83A H81B 0.5817 . ? C83B H78A 0.6283 . ? C83B H83E 0.9600 . ? C83B H83F 0.9600 . ? C83B H83B 0.9600 . ? C84 H84D 0.9600 . ? C84 H84E 0.9600 . ? C84 H84F 0.9600 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 O8 1.260(3) . ? C86 O7 1.261(3) . ? Co1 O8 1.987(2) 2_776 ? Co1 O7 2.000(2) 1_565 ? Co1 O2 2.035(2) . ? Co1 N1 2.102(2) . ? Co1 O1 2.213(2) 2_786 ? Co1 Co1 2.8656(8) 2_786 ? Co2 O6 1.967(2) 2_676 ? Co2 O5 2.004(2) . ? Co2 O3 2.059(2) . ? Co2 N4 2.103(2) . ? Co2 O4 2.2553(19) . ? Co2 O4 2.410(2) 2_676 ? O1 Co1 2.213(2) 2_786 ? O4 Co2 2.410(2) 2_676 ? O6 Co2 1.967(2) 2_676 ? O7 Co1 2.000(2) 1_545 ? O8 Co1 1.987(2) 2_776 ? O9 H9B 0.8501 . ? O9 H9C 0.8500 . ? 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 C5 C1 C2 115.9(3) . . ? C5 C1 C19 122.4(3) . . ? C2 C1 C19 121.7(3) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? N1 C3 C2 122.8(3) . . ? N1 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? N1 C4 C5 121.5(3) . . ? N1 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C1 121.3(3) . . ? C4 C5 H5 119.4 . . ? C1 C5 H5 119.4 . . ? C10 C6 C7 114.2(3) . . ? C10 C6 C25 121.7(4) . . ? C7 C6 C25 124.0(3) . . ? C8 C7 C6 120.9(4) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N2 C8 C7 124.1(4) . . ? N2 C8 H8 117.9 . . ? C7 C8 H8 117.9 . . ? N2 C9 C10 125.2(4) . . ? N2 C9 H9 117.4 . . ? C10 C9 H9 117.4 . . ? C9 C10 C6 119.8(4) . . ? C9 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? C15 C11 C12 113.2(4) . . ? C15 C11 C31 122.6(4) . . ? C12 C11 C31 124.2(4) . . ? C13 C12 C11 123.5(4) . . ? C13 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? N3 C13 C12 121.1(4) . . ? N3 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? N3 C14 C15 123.2(4) . . ? N3 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C11 C15 C14 121.4(4) . . ? C11 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C21 C16 C17 119.3(3) . . ? C21 C16 N7 121.3(3) . . ? C17 C16 N7 119.3(3) . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 122.6(3) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C20 C19 C18 117.0(3) . . ? C20 C19 C1 122.8(3) . . ? C18 C19 C1 120.2(3) . . ? C19 C20 C21 122.3(3) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 119.7(3) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 N7 120.7(3) . . ? C23 C22 C27 117.2(3) . . ? N7 C22 C27 122.0(3) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 121.7(3) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C26 C25 C24 116.3(3) . . ? C26 C25 C6 123.5(3) . . ? C24 C25 C6 120.2(3) . . ? C27 C26 C25 123.1(4) . . ? C27 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C26 C27 C22 120.4(4) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C33 117.5(3) . . ? C29 C28 N7 123.4(3) . . ? C33 C28 N7 118.9(3) . . ? C28 C29 C30 121.8(3) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 121.2(4) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 116.7(3) . . ? C32 C31 C11 121.2(3) . . ? C30 C31 C11 122.1(4) . . ? C31 C32 C33 122.4(3) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C28 C33 C32 120.3(4) . . ? C28 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C38 C34 C35 115.7(3) . . ? C38 C34 C49 121.7(3) . . ? C35 C34 C49 122.6(3) . . ? C36 C35 C34 119.6(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N4 C36 C35 124.7(3) . . ? N4 C36 H36 117.7 . . ? C35 C36 H36 117.7 . . ? N4 C37 C38 124.7(3) . . ? N4 C37 H37 117.6 . . ? C38 C37 H37 117.6 . . ? C37 C38 C34 119.8(3) . . ? C37 C38 H38 120.1 . . ? C34 C38 H38 120.1 . . ? C43 C39 C40 114.3(3) . . ? C43 C39 C58 123.1(3) . . ? C40 C39 C58 122.6(3) . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? N5 C41 C40 122.5(4) . . ? N5 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? N5 C42 C43 123.8(4) . . ? N5 C42 H42 118.1 . . ? C43 C42 H42 118.1 . . ? C39 C43 C42 121.3(4) . . ? C39 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C44 C48 112.2(4) . . ? C45 C44 C61 123.4(4) . . ? C48 C44 C61 124.1(4) . . ? C44 C45 C46 120.9(4) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? N6 C46 C45 129.2(5) . . ? N6 C46 H46 115.4 . . ? C45 C46 H46 115.4 . . ? C48 C47 N6 122.4(4) . . ? C48 C47 H47 118.8 . . ? N6 C47 H47 118.8 . . ? C47 C48 C44 122.1(4) . . ? C47 C48 H48 118.9 . . ? C44 C48 H48 118.9 . . ? C50 C49 C54 116.7(3) . . ? C50 C49 C34 122.2(3) . . ? C54 C49 C34 121.1(3) . . ? C49 C50 C51 123.7(3) . . ? C49 C50 H50 118.2 . . ? C51 C50 H50 118.2 . . ? C50 C51 C52 119.4(4) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C53 C52 N8 119.5(3) . . ? C53 C52 C51 117.2(3) . . ? N8 C52 C51 123.3(3) . . ? C54 C53 C52 122.4(3) . . ? C54 C53 H53 118.8 . . ? C52 C53 H53 118.8 . . ? C53 C54 C49 120.6(4) . . ? C53 C54 H54 119.7 . . ? C49 C54 H54 119.7 . . ? C60 C55 C56 116.8(4) . . ? C60 C55 N8 121.5(3) . . ? C56 C55 N8 121.6(3) . . ? C57 C56 C55 121.4(3) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 120.4(4) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C59 C58 C57 118.1(4) . . ? C59 C58 C39 122.2(3) . . ? C57 C58 C39 119.7(3) . . ? C58 C59 C60 121.6(4) . . ? C58 C59 H59 119.2 . . ? C60 C59 H59 119.2 . . ? C55 C60 C59 121.5(4) . . ? C55 C60 H60 119.2 . . ? C59 C60 H60 119.2 . . ? C66 C61 C62 118.0(4) . . ? C66 C61 C44 121.9(4) . . ? C62 C61 C44 120.2(4) . . ? C63 C62 C61 121.1(4) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C64 C63 C62 120.1(4) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 119.0(4) . . ? C63 C64 N8 122.9(3) . . ? C65 C64 N8 118.1(3) . . ? C66 C65 C64 120.7(4) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C61 121.0(3) . . ? C65 C66 H66 119.5 . . ? C61 C66 H66 119.5 . . ? C75 C67 C74 107.3(3) . . ? C75 C67 C68A 109.4(3) . . ? C74 C67 C68A 115.5(3) . . ? C75 C67 C71A 110.6(3) . . ? C74 C67 C71A 112.5(3) . . ? C68A C67 C71A 101.5(2) . . ? C70 C69 C68A 109.5(3) . . ? C70 C69 H69A 109.8 . . ? C68A C69 H69A 109.8 . . ? C70 C69 H69B 109.8 . . ? C68A C69 H69B 109.8 . . ? H69A C69 H69B 108.2 . . ? C69 C70 C71A 105.8(3) . . ? C69 C70 H70A 110.6 . . ? C71A C70 H70A 110.6 . . ? C69 C70 H70B 110.6 . . ? C71A C70 H70B 110.6 . . ? H70A C70 H70B 108.7 . . ? O1 C72 O2 123.2(3) . . ? O1 C72 C68A 117.5(3) . . ? O2 C72 C68A 119.3(3) . . ? C72 C68A C69 113.7(3) . . ? C72 C68A C67 113.3(3) . . ? C69 C68A C67 104.3(3) . . ? C72 C68A H68A 107.8 . . ? C69 C68A H68A 109.9 . . ? C67 C68A H68A 107.6 . . ? C73A C71A C76 112.4(4) . . ? C73A C71A C67 115.4(4) . . ? C76 C71A C67 114.6(2) . . ? C73A C71A C70 97.4(4) . . ? C76 C71A C70 110.3(3) . . ? C67 C71A C70 104.9(3) . . ? C73A C71A H71B 10.9 . . ? C76 C71A H71B 108.2 . . ? C67 C71A H71B 110.5 . . ? C70 C71A H71B 108.3 . . ? C71A C73A H73A 109.5 . . ? C71A C73A H73B 109.5 . . ? H73A C73A H73B 109.5 . . ? C71A C73A H73C 109.5 . . ? H73A C73A H73C 109.5 . . ? H73B C73A H73C 109.5 . . ? C71A C73A H71B 15.6 . . ? H73A C73A H71B 115.4 . . ? H73B C73A H71B 117.8 . . ? H73C C73A H71B 93.9 . . ? H68A C73B H73D 109.1 . . ? H68A C73B H73E 103.8 . . ? H73D C73B H73E 109.5 . . ? H68A C73B H73F 115.3 . . ? H73D C73B H73F 109.5 . . ? H73E C73B H73F 109.5 . . ? C67 C74 H74A 109.5 . . ? C67 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C67 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C67 C75 H75A 109.5 . . ? C67 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C67 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O4 C76 O3 119.1(3) . . ? O4 C76 C71A 120.1(3) . . ? O3 C76 C71A 120.7(3) . . ? O4 C76 Co2 64.17(15) . . ? O3 C76 Co2 55.18(15) . . ? C71A C76 Co2 175.6(2) . . ? C78A C77 C84 112.0(3) . . ? C78A C77 C85 112.0(3) . . ? C84 C77 C85 109.0(3) . . ? C78A C77 C81A 99.9(3) . . ? C84 C77 C81A 113.6(3) . . ? C85 C77 C81A 110.2(3) . . ? C78A C79 C80 105.1(3) . . ? C78A C79 H79A 110.7 . . ? C80 C79 H79A 110.7 . . ? C78A C79 H79B 110.7 . . ? C80 C79 H79B 110.7 . . ? H79A C79 H79B 108.8 . . ? C81A C80 C79 103.0(3) . . ? C81A C80 H80A 111.2 . . ? C79 C80 H80A 111.2 . . ? C81A C80 H80B 111.2 . . ? C79 C80 H80B 111.2 . . ? H80A C80 H80B 109.1 . . ? O5 C82 O6 124.1(3) . . ? O5 C82 C78A 120.5(3) . . ? O6 C82 C78A 115.3(3) . . ? C82 C78A C79 113.6(3) . . ? C82 C78A C77 112.5(3) . . ? C79 C78A C77 104.7(3) . . ? C82 C78A H78A 110.3 . . ? C79 C78A H78A 107.5 . . ? C77 C78A H78A 107.8 . . ? C80 C81A C86 116.6(3) . . ? C80 C81A C83A 112.5(3) . . ? C86 C81A C83A 108.7(3) . . ? C80 C81A C77 106.7(3) . . ? C86 C81A C77 110.0(2) . . ? C83A C81A C77 101.2(3) . . ? C80 C81A H81B 109.6 . . ? C86 C81A H81B 107.9 . . ? C83A C81A H81B 4.4 . . ? C77 C81A H81B 105.4 . . ? C81A C83A H83C 109.5 . . ? C81A C83A H83D 109.5 . . ? H83C C83A H83D 109.5 . . ? C81A C83A H83A 109.5 . . ? H83C C83A H83A 109.5 . . ? H83D C83A H83A 109.5 . . ? C81A C83A H81B 7.2 . . ? H83C C83A H81B 115.5 . . ? H83D C83A H81B 109.5 . . ? H83A C83A H81B 103.1 . . ? H78A C83B H83E 113.7 . . ? H78A C83B H83F 110.2 . . ? H83E C83B H83F 109.5 . . ? H78A C83B H83B 104.4 . . ? H83E C83B H83B 109.5 . . ? H83F C83B H83B 109.5 . . ? C77 C84 H84D 109.5 . . ? C77 C84 H84E 109.5 . . ? H84D C84 H84E 109.5 . . ? C77 C84 H84F 109.5 . . ? H84D C84 H84F 109.5 . . ? H84E C84 H84F 109.5 . . ? C77 C85 H85A 109.5 . . ? C77 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C77 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O8 C86 O7 123.7(3) . . ? O8 C86 C81A 116.8(3) . . ? O7 C86 C81A 119.1(3) . . ? O8 Co1 O7 160.67(9) 2_776 1_565 ? O8 Co1 O2 95.33(9) 2_776 . ? O7 Co1 O2 94.39(10) 1_565 . ? O8 Co1 N1 96.00(9) 2_776 . ? O7 Co1 N1 95.84(9) 1_565 . ? O2 Co1 N1 111.78(10) . . ? O8 Co1 O1 82.90(9) 2_776 2_786 ? O7 Co1 O1 83.21(9) 1_565 2_786 ? O2 Co1 O1 164.22(10) . 2_786 ? N1 Co1 O1 83.99(10) . 2_786 ? O8 Co1 Co1 79.31(6) 2_776 2_786 ? O7 Co1 Co1 81.94(6) 1_565 2_786 ? O2 Co1 Co1 106.28(7) . 2_786 ? N1 Co1 Co1 141.92(7) . 2_786 ? O1 Co1 Co1 57.95(7) 2_786 2_786 ? O6 Co2 O5 156.13(9) 2_676 . ? O6 Co2 O3 98.04(9) 2_676 . ? O5 Co2 O3 96.35(9) . . ? O6 Co2 N4 96.11(9) 2_676 . ? O5 Co2 N4 94.80(9) . . ? O3 Co2 N4 115.33(9) . . ? O6 Co2 O4 84.86(8) 2_676 . ? O5 Co2 O4 86.01(8) . . ? O3 Co2 O4 59.93(8) . . ? N4 Co2 O4 175.27(9) . . ? O6 Co2 O4 81.29(8) 2_676 2_676 ? O5 Co2 O4 78.52(8) . 2_676 ? O3 Co2 O4 159.23(7) . 2_676 ? N4 Co2 O4 85.29(9) . 2_676 ? O4 Co2 O4 99.44(6) . 2_676 ? O6 Co2 C76 90.16(9) 2_676 . ? O5 Co2 C76 92.88(9) . . ? O3 Co2 C76 30.01(9) . . ? N4 Co2 C76 145.27(10) . . ? O4 Co2 C76 30.00(9) . . ? O4 Co2 C76 129.44(8) 2_676 . ? C3 N1 C4 118.5(2) . . ? C3 N1 Co1 121.51(16) . . ? C4 N1 Co1 118.36(15) . . ? C9 N2 C8 115.6(3) . . ? C14 N3 C13 117.5(3) . . ? C37 N4 C36 115.4(2) . . ? C37 N4 Co2 120.00(15) . . ? C36 N4 Co2 122.42(16) . . ? C41 N5 C42 117.6(4) . . ? C46 N6 C47 112.4(4) . . ? C22 N7 C28 117.7(2) . . ? C22 N7 C16 122.2(2) . . ? C28 N7 C16 119.3(2) . . ? C52 N8 C64 120.5(3) . . ? C52 N8 C55 121.5(3) . . ? C64 N8 C55 115.9(3) . . ? C72 O1 Co1 152.8(2) . 2_786 ? C72 O2 Co1 99.72(19) . . ? C76 O3 Co2 94.82(19) . . ? C76 O4 Co2 85.83(17) . . ? C76 O4 Co2 166.38(19) . 2_676 ? Co2 O4 Co2 80.56(6) . 2_676 ? C82 O5 Co2 129.6(2) . . ? C82 O6 Co2 128.32(19) . 2_676 ? C86 O7 Co1 124.91(18) . 1_545 ? C86 O8 Co1 129.33(19) . 2_776 ? H9B O9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.314 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.059 # === END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H30 N4 Ni O5' _chemical_formula_sum 'C41 H30 N4 Ni O5' _chemical_formula_weight 717.40 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 17.7338(19) _cell_length_b 9.9058(10) _cell_length_c 22.944(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.794(2) _cell_angle_gamma 90.00 _cell_volume 4028.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1920 _cell_measurement_theta_min 2.8605 _cell_measurement_theta_max 17.9285 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21832 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7080 _reflns_number_gt 4040 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^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 7080 _refine_ls_number_parameters 455 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.091 _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 0.94388(11) 0.0911(3) 1.00881(10) 0.0779(7) Uani 1 1 d U . . H1 H 0.9060 0.1537 1.0153 0.094 Uiso 1 1 calc R . . C2 C 0.93937(10) 0.0112(2) 0.95955(9) 0.0598(6) Uani 1 1 d U . . C3 C 0.99688(12) -0.0799(3) 0.95154(10) 0.0802(8) Uani 1 1 d . . . H3 H 0.9955 -0.1349 0.9187 0.096 Uiso 1 1 calc R . . C4 C 0.87449(10) 0.0173(2) 0.91703(9) 0.0616(7) Uani 1 1 d U . . C5 C 0.46492(11) 0.1177(2) 1.01455(9) 0.0685(7) Uani 1 1 d . . . H5 H 0.4420 0.1987 1.0243 0.082 Uiso 1 1 calc R . . C6 C 0.52747(12) 0.1192(2) 0.97910(10) 0.0716(8) Uani 1 1 d . . . H6 H 0.5452 0.2009 0.9650 0.086 Uiso 1 1 calc R . . C7 C 0.56322(10) 0.0012(2) 0.96478(8) 0.0514(6) Uani 1 1 d . . . C8 C 0.62908(10) 0.0029(2) 0.92526(8) 0.0525(5) Uani 1 1 d U . . C9 C 0.73144(11) 0.9256(2) 1.10542(10) 0.0691(7) Uani 1 1 d U . . C10 C 0.69948(16) 0.8051(3) 1.12190(11) 0.0979(9) Uani 1 1 d U . . H10 H 0.6771 0.7979 1.1579 0.117 Uiso 1 1 calc R . . C11 C 0.70078(16) 0.6956(3) 1.08500(11) 0.0987(9) Uani 1 1 d U . . H11 H 0.6792 0.6147 1.0964 0.118 Uiso 1 1 calc R . . C12 C 0.73391(12) 0.7037(2) 1.03075(10) 0.0685(6) Uani 1 1 d U . . C13 C 0.76170(13) 0.8263(2) 1.01501(10) 0.0775(8) Uani 1 1 d U . . H13 H 0.7820 0.8358 0.9783 0.093 Uiso 1 1 calc R . . C14 C 0.76082(13) 0.9366(2) 1.05146(10) 0.0809(8) Uani 1 1 d . . . H14 H 0.7803 1.0187 1.0392 0.097 Uiso 1 1 calc R . . C15 C 0.66793(11) 1.0756(2) 1.17327(10) 0.0757(7) Uani 1 1 d U . . C16 C 0.66839(12) 1.1063(3) 1.23224(10) 0.0770(8) Uani 1 1 d U . . H16 H 0.7136 1.1046 1.2539 0.092 Uiso 1 1 calc R . . C17 C 0.60322(12) 1.1390(2) 1.25882(10) 0.0769(8) Uani 1 1 d . . . H17 H 0.6048 1.1563 1.2987 0.092 Uiso 1 1 calc R . . C18 C 0.53491(11) 1.1473(2) 1.22842(10) 0.0740(8) Uani 1 1 d . . . C19 C 0.53526(12) 1.1178(3) 1.16899(11) 0.1058(10) Uani 1 1 d . . . H19 H 0.4903 1.1233 1.1471 0.127 Uiso 1 1 calc R . . C20 C 0.59894(12) 1.0815(3) 1.14226(11) 0.1109(10) Uani 1 1 d . . . H20 H 0.5969 1.0603 1.1028 0.133 Uiso 1 1 calc R . . C21 C 0.80582(11) 1.0793(2) 1.16690(9) 0.0654(7) Uani 1 1 d . . . C22 C 0.86252(13) 0.9878(3) 1.17582(12) 0.106 Uani 1 1 d . . . H22 H 0.8546 0.8980 1.1655 0.127 Uiso 1 1 calc R . . C23 C 0.93149(14) 1.0267(3) 1.19999(12) 0.112 Uani 1 1 d . . . H23 H 0.9693 0.9622 1.2049 0.134 Uiso 1 1 calc R . . C24 C 0.94594(11) 1.1559(2) 1.21685(10) 0.0695(7) Uani 1 1 d U . . C25 C 0.89073(12) 1.2469(2) 1.20299(11) 0.0846(9) Uani 1 1 d U . . H25 H 0.9002 1.3379 1.2101 0.102 Uiso 1 1 calc R . . C26 C 0.82100(13) 1.2106(3) 1.17883(11) 0.0880(9) Uani 1 1 d . . . H26 H 0.7847 1.2763 1.1708 0.106 Uiso 1 1 calc R . . C27 C 0.96356(11) 0.3165(2) 0.75802(10) 0.0683(7) Uani 1 1 d . . . C28 C 0.95717(13) 0.3363(3) 0.81742(11) 0.0880(9) Uani 1 1 d . . . H28 H 0.9972 0.3732 0.8392 0.106 Uiso 1 1 calc R . . C29 C 0.89152(13) 0.3014(3) 0.84437(11) 0.0831(8) Uani 1 1 d U . . H29 H 0.8891 0.3152 0.8844 0.100 Uiso 1 1 calc R . . C30 C 0.83836(11) 0.2308(3) 0.75973(9) 0.0721(7) Uani 1 1 d U . . H30 H 0.7973 0.1944 0.7390 0.087 Uiso 1 1 calc R . . C31 C 0.90154(12) 0.2612(3) 0.72886(10) 0.0832(9) Uani 1 1 d . . . H31 H 0.9025 0.2448 0.6890 0.100 Uiso 1 1 calc R . . C32 C 0.73689(12) 0.5855(2) 0.99140(9) 0.0672(7) Uani 1 1 d U . . C33 C 0.73961(15) 0.4538(2) 1.01269(10) 0.0846(8) Uani 1 1 d U . . H33 H 0.7399 0.4382 1.0527 0.102 Uiso 1 1 calc R . . C34 C 0.74180(14) 0.3476(2) 0.97494(10) 0.0744(8) Uani 1 1 d U . . H34 H 0.7424 0.2612 0.9907 0.089 Uiso 1 1 calc R . . C35 C 0.74201(14) 0.4828(2) 0.89726(10) 0.0817(9) Uani 1 1 d . . . H35 H 0.7435 0.4949 0.8571 0.098 Uiso 1 1 calc R . . C36 C 0.73873(15) 0.5971(2) 0.93176(10) 0.0858(9) Uani 1 1 d . . . H36 H 0.7378 0.6821 0.9145 0.103 Uiso 1 1 calc R . . N3A N 0.65293(6) 0.23013(13) 0.80423(5) 0.0602(6) Uani 0.5506(15) 1 d PG . 1 C37A C 0.59132(7) 0.14337(15) 0.80413(8) 0.0872(16) Uani 0.5506(15) 1 d PG . 1 H37A H 0.5944 0.0622 0.8244 0.105 Uiso 0.5506(15) 1 calc PR . 1 C38A C 0.52512(7) 0.1779(2) 0.77368(9) 0.0901(17) Uani 0.5506(15) 1 d PG . 1 H38A H 0.4839 0.1199 0.7736 0.108 Uiso 0.5506(15) 1 calc PR . 1 C39A C 0.52053(8) 0.2992(2) 0.74333(9) 0.0643(8) Uani 0.5506(15) 1 d PG . 1 C40A C 0.58213(10) 0.3860(2) 0.74343(9) 0.0667(12) Uani 0.5506(15) 1 d PGU . 1 H40A H 0.5791 0.4671 0.7231 0.080 Uiso 0.5506(15) 1 calc PR . 1 C41A C 0.64833(8) 0.35144(15) 0.77387(8) 0.0702(14) Uani 0.5506(15) 1 d PGU . 1 H41A H 0.6896 0.4095 0.7739 0.084 Uiso 0.5506(15) 1 calc PR . 1 N3B N 0.64997(6) 0.24849(14) 0.81480(5) 0.0602(6) Uani 0.4494(15) 1 d PG . 2 C37B C 0.63346(7) 0.18713(16) 0.76143(6) 0.086(2) Uani 0.4494(15) 1 d PG . 2 H37B H 0.6671 0.1256 0.7461 0.103 Uiso 0.4494(15) 1 calc PR . 2 C38B C 0.56664(9) 0.2177(2) 0.73099(7) 0.091(2) Uani 0.4494(15) 1 d PG . 2 H38B H 0.5556 0.1767 0.6953 0.109 Uiso 0.4494(15) 1 calc PR . 2 C39B C 0.51632(8) 0.3097(2) 0.75392(9) 0.0643(8) Uani 0.4494(15) 1 d PG . 2 C40B C 0.53283(8) 0.3710(2) 0.80729(10) 0.132(3) Uani 0.4494(15) 1 d PG . 2 H40B H 0.4992 0.4325 0.8226 0.159 Uiso 0.4494(15) 1 calc PR . 2 C41B C 0.59965(8) 0.34045(18) 0.83773(7) 0.133(3) Uani 0.4494(15) 1 d PG . 2 H41B H 0.6107 0.3815 0.8734 0.159 Uiso 0.4494(15) 1 calc PR . 2 N1 N 0.83134(9) 0.24906(18) 0.81630(7) 0.0626(5) Uani 1 1 d U . . N2 N 0.74319(9) 0.35855(17) 0.91724(7) 0.0589(5) Uani 1 1 d . . . N4 N 0.73411(9) 1.03866(19) 1.14458(8) 0.0745(6) Uani 1 1 d . . . Ni1 Ni 0.743153(13) 0.17728(3) 0.867026(11) 0.04964(8) Uani 1 1 d . . . O1 O 0.66281(7) 0.11383(14) 0.92187(6) 0.0606(4) Uani 1 1 d U . . O2 O 0.64425(7) -0.10232(15) 0.89790(6) 0.0634(4) Uani 1 1 d U . . O3 O 0.82616(7) 0.10983(15) 0.92531(6) 0.0591(4) Uani 1 1 d U . . O4 O 0.87177(8) -0.06428(18) 0.87691(7) 0.0931(6) Uani 1 1 d . . . O5 O 0.74510(6) -0.00654(12) 0.82299(5) 0.050 Uani 1 1 d . . . H5A H 0.7787 -0.0571 0.8387 0.075 Uiso 1 1 d R . . H5B H 0.7022 -0.0444 0.8250 0.075 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0477(11) 0.0910(16) 0.0941(13) -0.0221(11) -0.0126(11) 0.0266(11) C2 0.0385(10) 0.0704(14) 0.0701(12) -0.0018(10) -0.0033(10) 0.0052(10) C3 0.0584(12) 0.0955(19) 0.0859(15) -0.0279(14) -0.0120(12) 0.0228(13) C4 0.0426(10) 0.0757(14) 0.0663(13) -0.0063(12) -0.0004(10) 0.0062(9) C5 0.0551(11) 0.0595(14) 0.0922(15) -0.0087(13) 0.0234(11) -0.0028(11) C6 0.0631(12) 0.0558(14) 0.0975(16) -0.0015(13) 0.0289(12) -0.0106(11) C7 0.0428(10) 0.0545(13) 0.0570(11) -0.0084(10) 0.0041(9) -0.0090(10) C8 0.0409(9) 0.0613(10) 0.0554(11) -0.0009(9) 0.0046(9) -0.0048(8) C9 0.0505(11) 0.0753(13) 0.0816(14) -0.0288(12) 0.0057(11) -0.0036(10) C10 0.1200(19) 0.0948(15) 0.0808(16) -0.0257(14) 0.0349(15) -0.0230(14) C11 0.137(2) 0.0640(17) 0.0976(13) -0.0231(14) 0.0456(13) -0.0171(16) C12 0.0700(13) 0.0610(12) 0.0751(12) -0.0206(11) 0.0116(10) -0.0031(11) C13 0.0858(15) 0.0726(13) 0.0753(14) -0.0155(12) 0.0198(13) -0.0087(12) C14 0.0850(15) 0.0676(16) 0.0912(16) -0.0254(14) 0.0237(13) -0.0113(13) C15 0.0475(11) 0.0868(17) 0.0930(11) -0.0367(13) 0.0043(11) 0.0020(12) C16 0.0493(12) 0.0892(17) 0.0927(12) -0.0264(14) 0.0037(12) -0.0026(12) C17 0.0600(13) 0.0927(18) 0.0781(15) -0.0286(13) 0.0035(12) -0.0025(13) C18 0.0485(11) 0.0827(16) 0.0909(15) -0.0391(13) 0.0038(11) -0.0023(11) C19 0.0451(12) 0.178(3) 0.0942(17) -0.0620(17) 0.0002(12) 0.0070(15) C20 0.0475(13) 0.191(3) 0.0938(16) -0.0787(17) -0.0003(12) 0.0072(16) C21 0.0475(11) 0.0644(15) 0.0843(14) -0.0176(12) 0.0020(11) 0.0008(11) C22 0.086 0.062 0.165 -0.038 -0.057 0.010 C23 0.081 0.087 0.163 -0.049 -0.066 0.017 C24 0.0500(11) 0.0638(14) 0.0940(16) -0.0233(12) -0.0108(11) 0.0011(9) C25 0.0618(12) 0.0566(14) 0.134(2) -0.0146(15) -0.0234(13) -0.0055(10) C26 0.0573(13) 0.0682(17) 0.137(2) -0.0192(15) -0.0230(14) 0.0100(12) C27 0.0500(11) 0.0751(15) 0.0804(14) 0.0267(12) 0.0101(11) 0.0025(11) C28 0.0645(13) 0.100(2) 0.1002(18) -0.0073(16) 0.0173(13) -0.0252(13) C29 0.0719(12) 0.0968(19) 0.0814(15) -0.0126(14) 0.0152(11) -0.0284(12) C30 0.0499(11) 0.0977(18) 0.0684(10) 0.0189(13) -0.0033(10) -0.0100(12) C31 0.0496(12) 0.127(2) 0.0733(14) 0.0271(15) 0.0074(11) -0.0054(14) C32 0.0752(14) 0.0628(11) 0.0643(13) -0.0082(11) 0.0116(11) -0.0037(12) C33 0.125(2) 0.0698(11) 0.0595(13) -0.0049(9) 0.0148(14) 0.0056(16) C34 0.1041(17) 0.0516(13) 0.0676(13) -0.0018(10) 0.0052(13) 0.0037(13) C35 0.1240(19) 0.0612(16) 0.0602(13) -0.0025(13) 0.0063(14) 0.0056(15) C36 0.136(2) 0.0486(14) 0.0727(15) -0.0012(13) 0.0083(15) 0.0031(15) N3A 0.0541(10) 0.0637(13) 0.0627(12) -0.0039(11) 0.0000(9) 0.0063(10) C37A 0.068(2) 0.068(3) 0.122(3) 0.031(3) -0.042(2) -0.016(2) C38A 0.076(3) 0.054(3) 0.138(4) 0.027(3) -0.033(3) -0.011(2) C39A 0.0524(12) 0.0661(16) 0.0741(16) 0.0062(13) -0.0052(12) -0.0069(12) C40A 0.0477(15) 0.071(3) 0.081(2) 0.026(2) -0.0020(15) -0.0094(18) C41A 0.0396(15) 0.090(3) 0.081(3) 0.008(2) 0.0009(15) -0.0126(19) N3B 0.0541(10) 0.0637(13) 0.0627(12) -0.0039(11) 0.0000(9) 0.0063(10) C37B 0.062(3) 0.134(5) 0.061(3) 0.009(3) -0.007(3) 0.038(3) C38B 0.068(3) 0.136(5) 0.068(3) -0.003(3) -0.004(3) 0.046(3) C39B 0.0524(12) 0.0661(16) 0.0741(16) 0.0062(13) -0.0052(12) -0.0069(12) C40B 0.095(4) 0.098(5) 0.199(6) -0.049(5) -0.068(4) 0.039(4) C41B 0.082(4) 0.181(7) 0.133(5) -0.050(5) -0.041(4) 0.046(4) N1 0.0531(9) 0.0649(12) 0.0702(9) 0.0067(10) 0.0083(8) -0.0085(9) N2 0.0600(10) 0.0545(11) 0.0622(10) 0.0008(9) 0.0036(9) 0.0034(9) N4 0.0439(9) 0.0867(13) 0.0925(12) -0.0490(10) -0.0039(9) 0.0014(9) Ni1 0.03698(12) 0.05448(16) 0.05755(15) 0.00387(13) 0.00301(11) -0.00048(12) O1 0.0514(7) 0.0605(7) 0.0710(8) -0.0085(7) 0.0191(7) -0.0106(6) O2 0.0567(8) 0.0643(8) 0.0699(8) -0.0113(7) 0.0152(7) -0.0068(7) O3 0.0450(7) 0.0656(9) 0.0662(8) -0.0002(8) -0.0051(6) 0.0097(6) O4 0.0699(9) 0.1130(13) 0.0948(11) -0.0417(10) -0.0246(8) 0.0373(9) O5 0.039 0.050 0.060 -0.002 -0.003 0.001 _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 C3 1.373(3) 3_757 ? C1 C2 1.380(3) . ? C1 H1 0.9300 . ? C2 C3 1.379(3) . ? C2 C4 1.486(3) . ? C3 C1 1.373(3) 3_757 ? C3 H3 0.9300 . ? C4 O4 1.225(3) . ? C4 O3 1.273(2) . ? C5 C7 1.369(3) 3_657 ? C5 C6 1.396(3) . ? C5 H5 0.9300 . ? C6 C7 1.375(3) . ? C6 H6 0.9300 . ? C7 C5 1.369(3) 3_657 ? C7 C8 1.501(3) . ? C8 O2 1.251(2) . ? C8 O1 1.254(2) . ? C9 C14 1.363(3) . ? C9 C10 1.379(3) . ? C9 N4 1.436(3) . ? C10 C11 1.376(4) . ? C10 H10 0.9300 . ? C11 C12 1.395(3) . ? C11 H11 0.9300 . ? C12 C13 1.364(3) . ? C12 C32 1.480(3) . ? C13 C14 1.376(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.387(3) . ? C15 C20 1.397(3) . ? C15 N4 1.412(3) . ? C16 C17 1.362(3) . ? C16 H16 0.9300 . ? C17 C18 1.381(3) . ? C17 H17 0.9300 . ? C18 C19 1.395(3) . ? C18 C27 1.498(3) 4_576 ? C19 C20 1.350(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.354(3) . ? C21 C22 1.364(3) . ? C21 N4 1.414(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9300 . ? C23 C24 1.359(3) . ? C23 H23 0.9300 . ? C24 C25 1.361(3) . ? C24 C39A 1.505(12) 4_676 ? C24 C39B 1.527(11) 4_676 ? C25 C26 1.387(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C31 1.382(3) . ? C27 C28 1.385(3) . ? C27 C18 1.498(3) 4_675 ? C28 C29 1.379(3) . ? C28 H28 0.9300 . ? C29 N1 1.334(3) . ? C29 H29 0.9300 . ? C30 N1 1.320(3) . ? C30 C31 1.378(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C36 1.374(3) . ? C32 C33 1.394(3) . ? C33 C34 1.364(3) . ? C33 H33 0.9300 . ? C34 N2 1.329(3) . ? C34 H34 0.9300 . ? C35 N2 1.314(3) . ? C35 C36 1.383(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N3A C37A 1.3900 . ? N3A C41A 1.3900 . ? N3A Ni1 2.1831(11) . ? C37A C38A 1.3900 . ? C37A H37A 0.9300 . ? C38A C39A 1.3900 . ? C38A H38A 0.9300 . ? C39A C40A 1.3900 . ? C39A C24 1.505(2) 4_575 ? C40A C41A 1.3900 . ? C40A H40A 0.9300 . ? C41A H41A 0.9300 . ? N3B C37B 1.3900 . ? N3B C41B 1.3900 . ? N3B Ni1 2.1308(12) . ? C37B C38B 1.3900 . ? C37B H37B 0.9300 . ? C38B C39B 1.3900 . ? C38B H38B 0.9300 . ? C39B C40B 1.3900 . ? C39B C24 1.527(2) 4_575 ? C40B C41B 1.3900 . ? C40B H40B 0.9300 . ? C41B H41B 0.9300 . ? N1 Ni1 2.1023(17) . ? N2 Ni1 2.1334(17) . ? Ni1 O1 2.0299(13) . ? Ni1 O3 2.0684(13) . ? Ni1 O5 2.0833(13) . ? O5 H5A 0.8500 . ? O5 H5B 0.8502 . ? 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 C3 C1 C2 121.3(2) 3_757 . ? C3 C1 H1 119.3 3_757 . ? C2 C1 H1 119.3 . . ? C3 C2 C1 117.42(19) . . ? C3 C2 C4 119.99(19) . . ? C1 C2 C4 122.55(18) . . ? C1 C3 C2 121.2(2) 3_757 . ? C1 C3 H3 119.4 3_757 . ? C2 C3 H3 119.4 . . ? O4 C4 O3 125.20(18) . . ? O4 C4 C2 118.55(19) . . ? O3 C4 C2 116.25(18) . . ? C7 C5 C6 121.0(2) 3_657 . ? C7 C5 H5 119.5 3_657 . ? C6 C5 H5 119.5 . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C5 C7 C6 118.22(18) 3_657 . ? C5 C7 C8 121.21(18) 3_657 . ? C6 C7 C8 120.51(19) . . ? O2 C8 O1 126.06(17) . . ? O2 C8 C7 118.49(17) . . ? O1 C8 C7 115.43(17) . . ? C14 C9 C10 119.4(2) . . ? C14 C9 N4 120.0(2) . . ? C10 C9 N4 120.6(2) . . ? C11 C10 C9 119.9(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 121.3(2) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 116.9(2) . . ? C13 C12 C32 121.5(2) . . ? C11 C12 C32 121.5(2) . . ? C12 C13 C14 122.4(2) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C9 C14 C13 120.1(2) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C20 117.8(2) . . ? C16 C15 N4 122.17(19) . . ? C20 C15 N4 120.1(2) . . ? C17 C16 C15 120.7(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 122.1(2) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C19 116.8(2) . . ? C17 C18 C27 121.7(2) . 4_576 ? C19 C18 C27 121.53(19) . 4_576 ? C20 C19 C18 121.9(2) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C15 120.8(2) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? C26 C21 C22 117.8(2) . . ? C26 C21 N4 121.17(19) . . ? C22 C21 N4 121.0(2) . . ? C21 C22 C23 120.9(2) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 122.2(2) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 115.4(2) . . ? C23 C24 C39A 123.3(5) . 4_676 ? C25 C24 C39A 121.0(5) . 4_676 ? C23 C24 C39B 120.8(5) . 4_676 ? C25 C24 C39B 123.5(5) . 4_676 ? C39A C24 C39B 10.43(8) 4_676 4_676 ? C24 C25 C26 123.2(2) . . ? C24 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C21 C26 C25 120.0(2) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C31 C27 C28 116.4(2) . . ? C31 C27 C18 123.1(2) . 4_675 ? C28 C27 C18 120.6(2) . 4_675 ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? N1 C29 C28 123.7(2) . . ? N1 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? N1 C30 C31 125.4(2) . . ? N1 C30 H30 117.3 . . ? C31 C30 H30 117.3 . . ? C30 C31 C27 119.0(2) . . ? C30 C31 H31 120.5 . . ? C27 C31 H31 120.5 . . ? C36 C32 C33 115.2(2) . . ? C36 C32 C12 122.9(2) . . ? C33 C32 C12 121.90(19) . . ? C34 C33 C32 120.1(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? N2 C34 C33 124.9(2) . . ? N2 C34 H34 117.6 . . ? C33 C34 H34 117.6 . . ? N2 C35 C36 124.6(2) . . ? N2 C35 H35 117.7 . . ? C36 C35 H35 117.7 . . ? C32 C36 C35 120.3(2) . . ? C32 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C37A N3A C41A 120.0 . . ? C37A N3A Ni1 114.37(6) . . ? C41A N3A Ni1 124.63(6) . . ? C38A C37A N3A 120.0 . . ? C38A C37A H37A 120.0 . . ? N3A C37A H37A 120.0 . . ? C39A C38A C37A 120.0 . . ? C39A C38A H38A 120.0 . . ? C37A C38A H38A 120.0 . . ? C38A C39A C40A 120.0 . . ? C38A C39A C24 119.64(15) . 4_575 ? C40A C39A C24 119.91(15) . 4_575 ? C41A C40A C39A 120.0 . . ? C41A C40A H40A 120.0 . . ? C39A C40A H40A 120.0 . . ? C40A C41A N3A 120.0 . . ? C40A C41A H41A 120.0 . . ? N3A C41A H41A 120.0 . . ? C37B N3B C41B 120.0 . . ? C37B N3B Ni1 119.27(7) . . ? C41B N3B Ni1 119.99(6) . . ? C38B C37B N3B 120.0 . . ? C38B C37B H37B 120.0 . . ? N3B C37B H37B 120.0 . . ? C37B C38B C39B 120.0 . . ? C37B C38B H38B 120.0 . . ? C39B C38B H38B 120.0 . . ? C38B C39B C40B 120.0 . . ? C38B C39B C24 117.31(15) . 4_575 ? C40B C39B C24 122.61(16) . 4_575 ? C41B C40B C39B 120.0 . . ? C41B C40B H40B 120.0 . . ? C39B C40B H40B 120.0 . . ? C40B C41B N3B 120.0 . . ? C40B C41B H41B 120.0 . . ? N3B C41B H41B 120.0 . . ? C30 N1 C29 115.42(18) . . ? C30 N1 Ni1 126.34(14) . . ? C29 N1 Ni1 117.51(15) . . ? C35 N2 C34 115.04(19) . . ? C35 N2 Ni1 126.91(15) . . ? C34 N2 Ni1 118.01(14) . . ? C15 N4 C21 120.57(18) . . ? C15 N4 C9 118.83(17) . . ? C21 N4 C9 117.41(16) . . ? O1 Ni1 O3 89.90(5) . . ? O1 Ni1 O5 93.01(5) . . ? O3 Ni1 O5 90.51(5) . . ? O1 Ni1 N1 175.27(6) . . ? O3 Ni1 N1 86.59(6) . . ? O5 Ni1 N1 90.19(6) . . ? O1 Ni1 N3B 84.50(5) . . ? O3 Ni1 N3B 173.84(5) . . ? O5 Ni1 N3B 92.34(5) . . ? N1 Ni1 N3B 98.85(6) . . ? O1 Ni1 N2 85.08(6) . . ? O3 Ni1 N2 86.25(6) . . ? O5 Ni1 N2 176.24(6) . . ? N1 Ni1 N2 91.53(7) . . ? N3B Ni1 N2 90.70(6) . . ? O1 Ni1 N3A 88.24(5) . . ? O3 Ni1 N3A 175.02(5) . . ? O5 Ni1 N3A 84.97(5) . . ? N1 Ni1 N3A 95.51(6) . . ? N3B Ni1 N3A 8.1 . . ? N2 Ni1 N3A 98.19(6) . . ? C8 O1 Ni1 130.91(13) . . ? C4 O3 Ni1 127.22(13) . . ? Ni1 O5 H5A 109.4 . . ? Ni1 O5 H5B 109.3 . . ? H5A O5 H5B 109.5 . . ? 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 _platon_squeeze_void_content 1 0.000 0.000 0.500 174 46 ' ' 2 0.500 0.000 0.500 216 47 ' ' 3 0.000 0.500 1.000 216 47 ' ' 4 0.500 0.500 0.000 174 46 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.597 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.061 # === END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H36 N4 Ni O5' _chemical_formula_sum 'C41 H36 N4 Ni O5' _chemical_formula_weight 723.45 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' _symmetry_space_group_name_Hall '-P2yn' 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 17.005(2) _cell_length_b 10.5930(13) _cell_length_c 24.0013(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.215(3) _cell_angle_gamma 90.00 _cell_volume 4322.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 8623 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 27.616 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25240 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8483 _reflns_number_gt 6170 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.061 0.000 0.500 530 31 ' ' 2 1.082 0.500 0.000 530 31 ' ' _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^)+(0.0400P)^2^+1.5500P] 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 8483 _refine_ls_number_parameters 460 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _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 0.75723(18) -0.0419(3) 0.57388(12) 0.0440(7) Uani 1 1 d U . . H1 H 0.7630 -0.0174 0.6109 0.053 Uiso 1 1 calc R . . C2 C 0.75656(18) 0.0472(3) 0.53223(12) 0.0482(7) Uani 1 1 d . . . H2 H 0.7609 0.1321 0.5416 0.058 Uiso 1 1 calc R . . C3 C 0.74954(15) 0.0134(3) 0.47686(11) 0.0402(6) Uani 1 1 d . . . C4 C 0.74374(17) -0.1145(3) 0.46324(12) 0.0451(7) Uani 1 1 d . . . H4 H 0.7405 -0.1394 0.4261 0.054 Uiso 1 1 calc R . . C5 C 0.74287(18) -0.2035(3) 0.50484(11) 0.0465(7) Uani 1 1 d . . . H5 H 0.7379 -0.2884 0.4955 0.056 Uiso 1 1 calc R . . C6 C 0.75144(16) 0.1152(3) 0.43332(12) 0.0412(6) Uani 1 1 d . . . C7 C 0.81005(16) 0.2064(3) 0.43247(12) 0.0436(7) Uani 1 1 d . . . H7 H 0.8502 0.2039 0.4593 0.052 Uiso 1 1 calc R . . C8 C 0.81024(17) 0.3003(3) 0.39300(11) 0.0435(7) Uani 1 1 d . . . H8 H 0.8501 0.3604 0.3937 0.052 Uiso 1 1 calc R . . C9 C 0.75137(15) 0.3062(3) 0.35209(12) 0.0413(6) Uani 1 1 d . . . C10 C 0.69288(16) 0.2144(3) 0.35231(12) 0.0423(6) Uani 1 1 d . . . H10 H 0.6530 0.2170 0.3252 0.051 Uiso 1 1 calc R . . C11 C 0.69264(16) 0.1190(3) 0.39186(10) 0.0404(6) Uani 1 1 d . . . H11 H 0.6534 0.0578 0.3908 0.048 Uiso 1 1 calc R . . C12 C 1.14729(19) 0.7363(3) 0.22596(14) 0.0568(8) Uani 1 1 d U . . H12 H 1.1833 0.7823 0.2475 0.068 Uiso 1 1 calc R . . C13 C 1.08548(17) 0.6800(3) 0.25143(13) 0.0469(7) Uani 1 1 d U . . H13 H 1.0819 0.6839 0.2900 0.056 Uiso 1 1 calc R . . C14 C 1.02971(17) 0.6192(3) 0.22147(12) 0.0449(7) Uani 1 1 d U . . C15 C 1.03760(19) 0.6107(3) 0.16342(13) 0.0568(8) Uani 1 1 d . . . H15 H 0.9993 0.5695 0.1420 0.068 Uiso 1 1 calc R . . C16 C 1.10188(17) 0.6633(3) 0.13817(13) 0.0451(7) Uani 1 1 d . . . H16 H 1.1072 0.6555 0.0998 0.054 Uiso 1 1 calc R . . C17 C 0.96083(16) 0.5606(3) 0.25132(13) 0.0441(7) Uani 1 1 d . . . C18 C 0.94512(17) 0.4337(3) 0.24315(12) 0.0437(7) Uani 1 1 d . . . H18 H 0.9800 0.3837 0.2236 0.052 Uiso 1 1 calc R . . C19 C 0.87642(17) 0.3809(3) 0.26455(12) 0.0476(7) Uani 1 1 d . . . H19 H 0.8659 0.2956 0.2592 0.057 Uiso 1 1 calc R . . C20 C 0.82357(14) 0.4555(3) 0.29392(10) 0.0358(6) Uani 1 1 d . . . C21 C 0.83944(17) 0.5832(3) 0.30201(12) 0.0436(7) Uani 1 1 d . . . H21 H 0.8045 0.6335 0.3214 0.052 Uiso 1 1 calc R . . C22 C 0.90826(16) 0.6354(3) 0.28084(12) 0.0460(7) Uani 1 1 d . . . H22 H 0.9191 0.7206 0.2864 0.055 Uiso 1 1 calc R . . C23 C 0.41165(16) 0.6984(3) 0.13232(11) 0.0425(6) Uani 1 1 d . . . H23 H 0.4112 0.7166 0.0944 0.051 Uiso 1 1 calc R . . C24 C 0.47397(17) 0.6473(3) 0.15565(12) 0.0456(7) Uani 1 1 d . . . H24 H 0.5177 0.6316 0.1341 0.055 Uiso 1 1 calc R . . C25 C 0.47681(15) 0.6146(3) 0.21371(11) 0.0389(6) Uani 1 1 d . . . C26 C 0.40942(16) 0.6425(3) 0.24418(12) 0.0421(6) Uani 1 1 d . . . H26 H 0.4084 0.6229 0.2819 0.051 Uiso 1 1 calc R . . C27 C 0.34634(16) 0.6972(3) 0.21960(12) 0.0456(7) Uani 1 1 d . . . H27 H 0.3026 0.7157 0.2408 0.055 Uiso 1 1 calc R . . C28 C 0.54788(15) 0.5534(3) 0.23858(11) 0.0403(6) Uani 1 1 d . . . C29 C 0.61839(16) 0.5267(3) 0.20804(11) 0.0408(6) Uani 1 1 d . . . H29 H 0.6188 0.5445 0.1701 0.049 Uiso 1 1 calc R . . C30 C 0.68272(16) 0.4777(3) 0.23208(12) 0.0440(7) Uani 1 1 d . . . H30 H 0.7274 0.4632 0.2114 0.053 Uiso 1 1 calc R . . C31 C 0.68217(15) 0.4486(3) 0.28837(11) 0.0378(6) Uani 1 1 d . . . C32 C 0.61496(16) 0.4737(3) 0.32013(12) 0.0421(6) Uani 1 1 d . . . H32 H 0.6154 0.4555 0.3580 0.051 Uiso 1 1 calc R . . C33 C 0.54884(15) 0.5251(3) 0.29512(11) 0.0403(6) Uani 1 1 d . . . H33 H 0.5046 0.5411 0.3161 0.048 Uiso 1 1 calc R . . C34 C 0.62001(16) -0.4876(3) 0.58617(11) 0.0387(6) Uani 1 1 d . . . C35 C 0.58007(18) -0.5289(3) 0.48593(12) 0.0526(8) Uani 1 1 d . . . H35A H 0.6273 -0.5797 0.4832 0.063 Uiso 1 1 calc R . . H35B H 0.5896 -0.4462 0.4702 0.063 Uiso 1 1 calc R . . C36 C 0.55263(16) -0.5188(3) 0.54814(11) 0.0431(7) Uani 1 1 d . . . H36 H 0.5258 -0.5958 0.5599 0.052 Uiso 1 1 calc R . . C37 C 0.49414(17) -0.4029(3) 0.54450(13) 0.0473(7) Uani 1 1 d . . . H37A H 0.5149 -0.3348 0.5222 0.057 Uiso 1 1 calc R . . H37B H 0.4811 -0.3713 0.5811 0.057 Uiso 1 1 calc R . . C38 C 0.87307(17) -0.4947(3) 0.58284(12) 0.0435(7) Uani 1 1 d . . . C39 C 1.01771(13) -0.5055(3) 0.55990(12) 0.0492(7) Uani 1 1 d D . . H39A H 1.0270 -0.5549 0.5934 0.059 Uiso 1 1 calc R . . H39B H 1.0238 -0.4172 0.5697 0.059 Uiso 1 1 calc R . . C40 C 0.93624(13) -0.5273(3) 0.53959(11) 0.0407(6) Uani 1 1 d D . . H40 H 0.9316 -0.6181 0.5325 0.049 Uiso 1 1 calc R . . C41 C 0.92157(17) -0.4603(3) 0.48207(11) 0.0471(7) Uani 1 1 d . . . H41A H 0.8699 -0.4836 0.4675 0.057 Uiso 1 1 calc R . . H41B H 0.9220 -0.3696 0.4876 0.057 Uiso 1 1 calc R . . N1 N 0.74920(13) -0.1692(2) 0.56029(9) 0.0387(5) Uani 1 1 d U . . N2 N 1.15815(13) 0.7271(2) 0.16900(10) 0.0407(5) Uani 1 1 d U . . N3 N 0.34532(12) 0.7262(2) 0.16389(9) 0.0375(5) Uani 1 1 d . . . N4 N 0.75227(12) 0.4038(2) 0.31269(9) 0.0383(5) Uani 1 1 d . . . Ni1 Ni 0.749932(19) -0.31313(3) 0.622086(12) 0.03132(9) Uani 1 1 d U . . O1 O 0.66264(11) -0.3962(2) 0.57592(7) 0.0450(5) Uani 1 1 d . . . O2 O 0.62948(11) -0.56260(19) 0.62705(8) 0.0445(5) Uani 1 1 d . . . O3 O 0.83119(11) -0.40267(19) 0.57282(8) 0.0434(4) Uani 1 1 d U . . O4 O 0.87075(11) -0.56367(19) 0.62539(8) 0.0444(5) Uani 1 1 d . . . O1W O 0.75128(11) -0.46259(18) 0.68012(7) 0.0382(4) Uani 1 1 d U . . H1W4 H 0.7131 -0.5248 0.6696 0.046 Uiso 1 1 d R . . H1W6 H 0.8026 -0.5003 0.6807 0.046 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0569(18) 0.0364(13) 0.0385(15) -0.0035(12) -0.0037(13) -0.0054(13) C2 0.0584(19) 0.0437(17) 0.0429(16) -0.0016(13) 0.0085(13) 0.0080(14) C3 0.0357(14) 0.0453(16) 0.0390(14) 0.0062(12) -0.0164(11) -0.0127(12) C4 0.0541(18) 0.0429(17) 0.0380(15) -0.0026(12) -0.0022(12) 0.0033(13) C5 0.0597(18) 0.0420(17) 0.0374(15) 0.0002(12) -0.0104(13) 0.0115(14) C6 0.0362(14) 0.0390(15) 0.0491(16) 0.0102(12) 0.0151(12) 0.0070(12) C7 0.0409(15) 0.0396(16) 0.0500(16) -0.0103(13) -0.0065(12) 0.0041(12) C8 0.0489(16) 0.0421(16) 0.0397(15) -0.0055(12) 0.0059(12) -0.0113(13) C9 0.0323(14) 0.0439(16) 0.0482(15) 0.0071(13) 0.0103(11) 0.0077(12) C10 0.0370(15) 0.0424(16) 0.0473(16) -0.0025(13) -0.0096(12) 0.0056(12) C11 0.0455(16) 0.0453(16) 0.0306(13) -0.0107(12) 0.0088(11) -0.0112(13) C12 0.0523(19) 0.064(2) 0.0542(15) -0.0126(16) 0.0125(14) -0.0179(16) C13 0.0413(15) 0.0511(18) 0.0485(16) 0.0095(14) 0.0055(11) 0.0018(12) C14 0.0424(16) 0.0427(16) 0.0504(17) -0.0067(13) 0.0186(12) -0.0080(12) C15 0.0543(19) 0.065(2) 0.0513(18) -0.0093(16) 0.0072(14) -0.0211(16) C16 0.0465(16) 0.0415(17) 0.0474(16) 0.0064(13) 0.0070(12) 0.0050(13) C17 0.0376(15) 0.0386(16) 0.0568(18) -0.0091(13) 0.0146(12) -0.0029(12) C18 0.0433(16) 0.0384(16) 0.0499(16) -0.0096(13) 0.0151(12) -0.0026(12) C19 0.0486(17) 0.0405(16) 0.0544(18) -0.0170(13) 0.0148(13) -0.0108(13) C20 0.0306(13) 0.0407(15) 0.0359(14) -0.0069(11) 0.0003(10) -0.0079(11) C21 0.0433(16) 0.0431(16) 0.0451(16) -0.0111(13) 0.0169(12) -0.0038(13) C22 0.0386(15) 0.0428(16) 0.0571(18) -0.0129(14) 0.0131(13) -0.0111(13) C23 0.0414(15) 0.0517(17) 0.0343(14) 0.0060(12) -0.0032(11) -0.0083(13) C24 0.0374(15) 0.0589(19) 0.0409(15) -0.0051(13) 0.0064(11) 0.0130(13) C25 0.0315(14) 0.0401(15) 0.0444(15) -0.0119(12) -0.0182(11) -0.0051(11) C26 0.0356(14) 0.0506(17) 0.0399(15) 0.0143(13) -0.0048(11) -0.0081(12) C27 0.0371(14) 0.0565(19) 0.0435(16) -0.0027(14) 0.0077(12) 0.0084(13) C28 0.0297(14) 0.0499(17) 0.0406(15) -0.0096(12) -0.0144(11) -0.0072(12) C29 0.0367(15) 0.0520(17) 0.0336(14) 0.0013(12) -0.0023(11) -0.0083(13) C30 0.0396(16) 0.0467(17) 0.0458(16) -0.0137(13) 0.0032(12) -0.0012(13) C31 0.0313(13) 0.0379(15) 0.0441(15) -0.0022(12) -0.0044(11) -0.0053(11) C32 0.0399(15) 0.0476(17) 0.0387(14) -0.0005(12) -0.0043(11) -0.0066(13) C33 0.0318(14) 0.0458(16) 0.0434(15) -0.0022(12) 0.0048(11) -0.0059(12) C34 0.0362(14) 0.0394(15) 0.0398(15) -0.0090(12) -0.0142(11) 0.0076(12) C35 0.0519(18) 0.066(2) 0.0392(15) 0.0036(14) -0.0158(13) -0.0146(15) C36 0.0417(16) 0.0452(16) 0.0419(15) -0.0117(13) -0.0132(12) 0.0008(13) C37 0.0412(16) 0.0406(16) 0.0592(19) 0.0061(14) -0.0198(13) -0.0043(13) C38 0.0449(16) 0.0409(16) 0.0452(16) -0.0079(13) 0.0101(12) -0.0051(13) C39 0.0483(17) 0.0567(19) 0.0424(16) -0.0022(14) -0.0001(13) -0.0049(14) C40 0.0435(15) 0.0386(15) 0.0406(15) -0.0009(12) 0.0107(12) -0.0039(12) C41 0.0421(16) 0.0604(19) 0.0388(15) -0.0092(14) 0.0001(12) -0.0076(14) N1 0.0451(13) 0.0415(12) 0.0296(11) -0.0004(9) 0.0000(9) -0.0022(10) N2 0.0346(12) 0.0371(12) 0.0510(12) -0.0057(10) 0.0180(10) -0.0005(10) N3 0.0270(11) 0.0468(13) 0.0384(12) -0.0066(10) -0.0113(9) -0.0001(9) N4 0.0332(12) 0.0392(12) 0.0427(13) -0.0011(10) 0.0038(9) -0.0050(10) Ni1 0.03230(17) 0.03703(18) 0.02452(15) -0.00020(13) -0.00187(11) -0.00010(14) O1 0.0461(11) 0.0510(12) 0.0370(10) 0.0008(9) -0.0175(8) -0.0003(10) O2 0.0479(12) 0.0435(11) 0.0416(11) -0.0053(9) -0.0151(9) 0.0023(9) O3 0.0401(11) 0.0484(12) 0.0420(11) -0.0033(9) 0.0093(8) -0.0061(9) O4 0.0388(11) 0.0501(12) 0.0450(11) -0.0055(9) 0.0148(8) -0.0083(9) O1W 0.0393(10) 0.0491(10) 0.0258(9) 0.0037(7) -0.0062(7) -0.0016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.375(4) . ? C1 N1 1.393(3) . ? C1 H1 0.9300 . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.397(4) . ? C3 C6 1.502(4) . ? C4 C5 1.373(4) . ? C4 H4 0.9300 . ? C5 N1 1.382(3) . ? C5 H5 0.9300 . ? C6 C7 1.389(4) . ? C6 C11 1.396(4) . ? C7 C8 1.374(4) . ? C7 H7 0.9300 . ? C8 C9 1.389(4) . ? C8 H8 0.9300 . ? C9 C10 1.392(4) . ? C9 N4 1.401(3) . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.364(4) . ? C12 N2 1.387(4) . ? C12 H12 0.9300 . ? C13 C14 1.343(4) . ? C13 H13 0.9300 . ? C14 C15 1.405(4) . ? C14 C17 1.518(4) . ? C15 C16 1.379(4) . ? C15 H15 0.9300 . ? C16 N2 1.375(4) . ? C16 H16 0.9300 . ? C17 C18 1.384(4) . ? C17 C22 1.398(4) . ? C18 C19 1.402(4) . ? C18 H18 0.9300 . ? C19 C20 1.398(4) . ? C19 H19 0.9300 . ? C20 C21 1.392(4) . ? C20 N4 1.413(3) . ? C21 C22 1.400(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.306(4) . ? C23 N3 1.403(3) . ? C23 H23 0.9300 . ? C24 C25 1.436(4) . ? C24 H24 0.9300 . ? C25 C26 1.404(4) . ? C25 C28 1.485(4) . ? C26 C27 1.344(4) . ? C26 H26 0.9300 . ? C27 N3 1.372(3) . ? C27 H27 0.9300 . ? C28 C33 1.389(4) . ? C28 C29 1.446(4) . ? C29 C30 1.331(4) . ? C29 H29 0.9300 . ? C30 C31 1.386(4) . ? C30 H30 0.9300 . ? C31 N4 1.399(3) . ? C31 C32 1.412(4) . ? C32 C33 1.376(4) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 O1 1.238(3) . ? C34 O2 1.270(3) . ? C34 C36 1.487(3) . ? C35 C36 1.577(4) . ? C35 C37 1.615(4) 3_646 ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.581(4) . ? C36 H36 0.9800 . ? C37 C35 1.615(4) 3_646 ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O3 1.228(3) . ? C38 O4 1.257(3) . ? C38 C40 1.548(4) . ? C39 C40 1.4770(10) . ? C39 C41 1.502(4) 3_746 ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.568(4) . ? C40 H40 0.9800 . ? C41 C39 1.502(4) 3_746 ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N1 Ni1 2.127(2) . ? N2 Ni1 2.147(2) 4_665 ? N3 Ni1 2.102(2) 4_565 ? Ni1 O1 2.0336(18) . ? Ni1 O3 2.0680(19) . ? Ni1 N3 2.102(2) 4_666 ? Ni1 O1W 2.1085(18) . ? Ni1 N2 2.147(2) 4_566 ? O1W H1W4 0.9564 . ? O1W H1W6 0.9597 . ? 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 N1 119.7(3) . . ? C2 C1 H1 120.2 . . ? N1 C1 H1 120.2 . . ? C1 C2 C3 121.4(3) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 118.8(3) . . ? C2 C3 C6 118.8(3) . . ? C4 C3 C6 122.4(3) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 N1 121.2(3) . . ? C4 C5 H5 119.4 . . ? N1 C5 H5 119.4 . . ? C7 C6 C11 118.2(3) . . ? C7 C6 C3 122.4(3) . . ? C11 C6 C3 119.4(2) . . ? C8 C7 C6 121.8(3) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 120.5(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.1(3) . . ? C8 C9 N4 119.5(2) . . ? C10 C9 N4 122.4(2) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C6 119.8(3) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 N2 122.1(3) . . ? C13 C12 H12 119.0 . . ? N2 C12 H12 119.0 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 C17 119.1(3) . . ? C15 C14 C17 122.2(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? N2 C16 C15 120.8(3) . . ? N2 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C22 119.9(3) . . ? C18 C17 C14 118.6(2) . . ? C22 C17 C14 121.0(3) . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 119.6(2) . . ? C21 C20 N4 119.8(2) . . ? C19 C20 N4 120.5(2) . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C17 C22 C21 120.5(3) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 N3 120.6(2) . . ? C24 C23 H23 119.7 . . ? N3 C23 H23 119.7 . . ? C23 C24 C25 121.8(3) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 116.3(2) . . ? C26 C25 C28 123.3(2) . . ? C24 C25 C28 120.4(2) . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 N3 121.2(2) . . ? C26 C27 H27 119.4 . . ? N3 C27 H27 119.4 . . ? C33 C28 C29 117.4(2) . . ? C33 C28 C25 118.6(2) . . ? C29 C28 C25 123.9(2) . . ? C30 C29 C28 122.6(3) . . ? C30 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? C29 C30 C31 119.1(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 N4 117.3(2) . . ? C30 C31 C32 120.4(3) . . ? N4 C31 C32 122.1(2) . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C28 120.3(3) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? O1 C34 O2 125.3(2) . . ? O1 C34 C36 119.9(3) . . ? O2 C34 C36 114.8(3) . . ? C36 C35 C37 102.4(2) . 3_646 ? C36 C35 H35A 111.3 . . ? C37 C35 H35A 111.3 3_646 . ? C36 C35 H35B 111.3 . . ? C37 C35 H35B 111.3 3_646 . ? H35A C35 H35B 109.2 . . ? C34 C36 C35 110.9(2) . . ? C34 C36 C37 109.7(2) . . ? C35 C36 C37 101.5(2) . . ? C34 C36 H36 111.4 . . ? C35 C36 H36 111.4 . . ? C37 C36 H36 111.4 . . ? C36 C37 C35 99.4(2) . 3_646 ? C36 C37 H37A 111.9 . . ? C35 C37 H37A 111.9 3_646 . ? C36 C37 H37B 111.9 . . ? C35 C37 H37B 111.9 3_646 . ? H37A C37 H37B 109.6 . . ? O3 C38 O4 126.3(3) . . ? O3 C38 C40 117.0(3) . . ? O4 C38 C40 116.7(3) . . ? C40 C39 C41 113.2(2) . 3_746 ? C40 C39 H39A 108.9 . . ? C41 C39 H39A 108.9 3_746 . ? C40 C39 H39B 108.9 . . ? C41 C39 H39B 108.9 3_746 . ? H39A C39 H39B 107.7 . . ? C39 C40 C38 113.8(2) . . ? C39 C40 C41 110.5(2) . . ? C38 C40 C41 112.9(2) . . ? C39 C40 H40 106.3 . . ? C38 C40 H40 106.3 . . ? C41 C40 H40 106.3 . . ? C39 C41 C40 112.5(2) 3_746 . ? C39 C41 H41A 109.1 3_746 . ? C40 C41 H41A 109.1 . . ? C39 C41 H41B 109.1 3_746 . ? C40 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C5 N1 C1 119.1(2) . . ? C5 N1 Ni1 118.82(18) . . ? C1 N1 Ni1 122.09(17) . . ? C16 N2 C12 117.3(2) . . ? C16 N2 Ni1 115.59(18) . 4_665 ? C12 N2 Ni1 126.92(19) . 4_665 ? C27 N3 C23 119.1(2) . . ? C27 N3 Ni1 123.86(18) . 4_565 ? C23 N3 Ni1 117.07(17) . 4_565 ? C31 N4 C9 120.7(2) . . ? C31 N4 C20 117.7(2) . . ? C9 N4 C20 121.5(2) . . ? O1 Ni1 O3 88.79(8) . . ? O1 Ni1 N3 175.40(9) . 4_666 ? O3 Ni1 N3 87.46(8) . 4_666 ? O1 Ni1 O1W 91.88(7) . . ? O3 Ni1 O1W 92.02(8) . . ? N3 Ni1 O1W 90.93(8) 4_666 . ? O1 Ni1 N1 86.37(8) . . ? O3 Ni1 N1 85.65(8) . . ? N3 Ni1 N1 90.68(9) 4_666 . ? O1W Ni1 N1 177.11(8) . . ? O1 Ni1 N2 86.50(9) . 4_566 ? O3 Ni1 N2 175.29(8) . 4_566 ? N3 Ni1 N2 97.23(9) 4_666 4_566 ? O1W Ni1 N2 88.29(8) . 4_566 ? N1 Ni1 N2 93.89(9) . 4_566 ? C34 O1 Ni1 130.85(17) . . ? C38 O3 Ni1 130.09(18) . . ? Ni1 O1W H1W4 110.2 . . ? Ni1 O1W H1W6 108.7 . . ? H1W4 O1W H1W6 109.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.294 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.048 # === END