Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_address ; School of Chemistry F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email LINDOY@GMAIL.COM _publ_section_title ; Synthetic, structural, electrochemical and solvent extraction studies of neutral trinuclear Co(II), Ni(II), Cu(II) and Zn(II) metallocycles and tetrahedral tetranuclear Fe(III) species incorporating 1,4-aryl-linked bis-?-diketonato ligands ; loop_ _publ_author_name 'Leonard Lindoy' 'David J. Bray' 'Jack K. Clegg' 'Karsten Gloe' 'Kerstin Gloe' 'Katrina A. Jolliffe' ; G.A.Lawrance ; 'George V. Meehan' 'Marco Wenzel' data_lj112sad _database_code_depnum_ccdc_archive 'CCDC 665749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 O4' _chemical_formula_sum 'C20 H26 O4' _chemical_formula_weight 330.41 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.232(3) _cell_length_b 10.158(3) _cell_length_c 17.738(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1843.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2585 _cell_measurement_theta_min 2.296 _cell_measurement_theta_max 23.016 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.032 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.864765 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 46 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 16191 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2229 _reflns_number_gt 1380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0638P)^2^+0.4206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2229 _refine_ls_number_parameters 115 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 1.1406(2) 0.2276(2) 0.65174(16) 0.0588(7) Uani 1 1 d . . . H1A H 1.1454 0.2442 0.5974 0.088 Uiso 1 1 calc R . . H1B H 1.2262 0.1982 0.6700 0.088 Uiso 1 1 calc R . . H1C H 1.1156 0.3088 0.6779 0.088 Uiso 1 1 calc R . . C2 C 1.0289(3) 0.0967(3) 0.75208(14) 0.0642(7) Uani 1 1 d . . . H2A H 1.0061 0.1790 0.7777 0.096 Uiso 1 1 calc R . . H2B H 1.1130 0.0646 0.7711 0.096 Uiso 1 1 calc R . . H2C H 0.9611 0.0307 0.7618 0.096 Uiso 1 1 calc R . . C3 C 1.07942(19) -0.0059(2) 0.62845(13) 0.0507(6) Uani 1 1 d . . . H3A H 1.0176 -0.0759 0.6416 0.076 Uiso 1 1 calc R . . H3B H 1.1674 -0.0308 0.6450 0.076 Uiso 1 1 calc R . . H3C H 1.0793 0.0072 0.5737 0.076 Uiso 1 1 calc R . . C4 C 1.03903(17) 0.12123(17) 0.66723(10) 0.0327(4) Uani 1 1 d . A . C5 C 0.90640(16) 0.16932(16) 0.64128(10) 0.0279(4) Uani 1 1 d . . . C6 C 0.82083(15) 0.09840(15) 0.59744(10) 0.0274(4) Uani 1 1 d . A . H6 H 0.8455 0.0142 0.5790 0.033 Uiso 1 1 calc R . . C7 C 0.69586(16) 0.15039(16) 0.57954(9) 0.0272(4) Uani 1 1 d . . . C8 C 0.59660(15) 0.07136(15) 0.53775(9) 0.0253(4) Uani 1 1 d . . . C9 C 0.62667(16) -0.04644(16) 0.50199(10) 0.0307(4) Uani 1 1 d . . . H9 H 0.7138 -0.0787 0.5033 0.037 Uiso 1 1 calc R A . C10 C 0.53163(16) -0.11688(16) 0.46474(10) 0.0306(4) Uani 1 1 d . . . H10 H 0.5537 -0.1973 0.4405 0.037 Uiso 1 1 calc R . . O1 O 0.87529(13) 0.28646(12) 0.66679(8) 0.0395(4) Uani 1 1 d D A 1 H13 H 0.7949(13) 0.303(2) 0.6466(12) 0.059 Uiso 1 1 d D B 1 O2 O 0.66380(11) 0.26539(11) 0.59970(8) 0.0367(3) Uani 1 1 d . A . 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 0.0307(10) 0.0442(12) 0.102(2) 0.0033(13) -0.0113(12) -0.0074(9) C2 0.0644(16) 0.0782(17) 0.0500(13) 0.0077(12) -0.0166(12) 0.0162(14) C3 0.0286(10) 0.0493(13) 0.0742(16) -0.0171(11) -0.0130(10) 0.0083(9) C4 0.0277(9) 0.0319(9) 0.0384(10) -0.0018(8) -0.0080(8) -0.0027(7) C5 0.0261(9) 0.0254(9) 0.0322(9) 0.0008(7) 0.0011(7) -0.0030(7) C6 0.0234(8) 0.0249(8) 0.0338(9) -0.0026(7) -0.0003(7) -0.0009(6) C7 0.0264(8) 0.0262(8) 0.0289(9) 0.0008(7) 0.0001(7) -0.0025(7) C8 0.0221(8) 0.0254(8) 0.0284(9) 0.0022(7) -0.0011(6) -0.0017(7) C9 0.0212(8) 0.0315(9) 0.0393(10) -0.0037(8) -0.0028(7) 0.0029(7) C10 0.0263(9) 0.0269(9) 0.0385(10) -0.0049(7) -0.0013(7) 0.0024(7) O1 0.0333(7) 0.0308(7) 0.0545(9) -0.0099(6) -0.0101(6) 0.0014(6) O2 0.0286(6) 0.0268(6) 0.0545(8) -0.0060(6) -0.0059(6) 0.0012(5) _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 C4 1.524(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.529(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.520(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.514(2) . ? C5 O1 1.312(2) . ? C5 C6 1.375(2) . ? C6 C7 1.419(2) . ? C6 H6 0.9500 . ? C7 O2 1.265(2) . ? C7 C8 1.492(2) . ? C8 C9 1.389(2) . ? C8 C10 1.392(2) 5_656 ? C9 C10 1.376(2) . ? C9 H9 0.9500 . ? C10 C8 1.392(2) 5_656 ? C10 H10 0.9500 . ? O1 H13 0.913(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C3 112.34(15) . . ? C5 C4 C1 109.14(15) . . ? C3 C4 C1 109.56(17) . . ? C5 C4 C2 106.93(16) . . ? C3 C4 C2 108.98(18) . . ? C1 C4 C2 109.84(18) . . ? O1 C5 C6 121.04(15) . . ? O1 C5 C4 113.90(14) . . ? C6 C5 C4 125.02(15) . . ? C5 C6 C7 120.35(15) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? O2 C7 C6 120.93(15) . . ? O2 C7 C8 117.44(15) . . ? C6 C7 C8 121.62(15) . . ? C9 C8 C10 118.72(15) . 5_656 ? C9 C8 C7 122.67(15) . . ? C10 C8 C7 118.61(15) 5_656 . ? C10 C9 C8 120.71(15) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C8 120.57(16) . 5_656 ? C9 C10 H10 119.7 . . ? C8 C10 H10 119.7 5_656 . ? C5 O1 H13 104.7(14) . . ? 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 C3 C4 C5 O1 -172.36(16) . . . . ? C1 C4 C5 O1 -50.6(2) . . . . ? C2 C4 C5 O1 68.1(2) . . . . ? C3 C4 C5 C6 10.1(3) . . . . ? C1 C4 C5 C6 131.79(19) . . . . ? C2 C4 C5 C6 -109.4(2) . . . . ? O1 C5 C6 C7 -0.7(3) . . . . ? C4 C5 C6 C7 176.73(16) . . . . ? C5 C6 C7 O2 4.2(3) . . . . ? C5 C6 C7 C8 -174.67(15) . . . . ? O2 C7 C8 C9 169.04(16) . . . . ? C6 C7 C8 C9 -12.1(3) . . . . ? O2 C7 C8 C10 -11.7(2) . . . 5_656 ? C6 C7 C8 C10 167.16(16) . . . 5_656 ? C10 C8 C9 C10 0.0(3) 5_656 . . . ? C7 C8 C9 C10 179.29(16) . . . . ? C8 C9 C10 C8 0.0(3) . . . 5_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H13 O2 0.913(10) 1.625(13) 2.4790(18) 154(2) . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.234 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.041 # Attachment 'LJ222SADX.CIF' data_lj222sad _database_code_depnum_ccdc_archive 'CCDC 665750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C90 H102 N6 Ni3 O12), 3.5(C5 H5 N)' _chemical_formula_sum 'C107.50 H119.50 N9.50 Ni3 O12' _chemical_formula_weight 1912.76 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Intl_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9493(10) _cell_length_b 23.585(3) _cell_length_c 26.145(3) _cell_angle_alpha 104.688(8) _cell_angle_beta 93.275(8) _cell_angle_gamma 98.843(7) _cell_volume 5247.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3927 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 18.026 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2022 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 100(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 127447 _diffrn_reflns_av_R_equivalents 0.2848 _diffrn_reflns_av_sigmaI/netI 0.1526 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 22.00 _reflns_number_total 12860 _reflns_number_gt 6417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1690P)^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 SHELXL _refine_ls_extinction_coef 0.0032(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12860 _refine_ls_number_parameters 1048 _refine_ls_number_restraints 783 _refine_ls_R_factor_all 0.1943 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.2723 _refine_ls_wR_factor_gt 0.2253 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.956 _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 -0.1327(13) -0.2264(5) 0.2438(5) 0.067(3) Uani 1 1 d U . . H1A H -0.1375 -0.2659 0.2499 0.100 Uiso 1 1 calc R . . H1B H -0.1909 -0.2298 0.2099 0.100 Uiso 1 1 calc R . . H1C H -0.1759 -0.2007 0.2727 0.100 Uiso 1 1 calc R . . C2 C 0.0967(12) -0.2353(4) 0.1940(4) 0.047(3) Uani 1 1 d U . . H2A H 0.2001 -0.2160 0.1914 0.071 Uiso 1 1 calc R . . H2B H 0.0317 -0.2379 0.1618 0.071 Uiso 1 1 calc R . . H2C H 0.0989 -0.2755 0.1978 0.071 Uiso 1 1 calc R . . C3 C 0.1270(14) -0.2006(5) 0.2914(4) 0.063(3) Uani 1 1 d U . . H3A H 0.0863 -0.1783 0.3229 0.094 Uiso 1 1 calc R . . H3B H 0.2328 -0.1824 0.2907 0.094 Uiso 1 1 calc R . . H3C H 0.1227 -0.2419 0.2927 0.094 Uiso 1 1 calc R . . C4 C 0.0339(11) -0.1991(4) 0.2422(4) 0.036(2) Uani 1 1 d U . . C5 C 0.0306(10) -0.1360(4) 0.2348(4) 0.0328(9) Uani 1 1 d U . . C6 C 0.0839(10) -0.0855(4) 0.2784(4) 0.0328(9) Uani 1 1 d U . . H6 H 0.1116 -0.0924 0.3116 0.039 Uiso 1 1 calc R . . C7 C 0.0990(10) -0.0255(4) 0.2758(4) 0.0328(9) Uani 1 1 d U . . C8 C 0.1742(10) 0.0227(4) 0.3254(4) 0.031(2) Uani 1 1 d U . . C9 C 0.2664(12) 0.0145(4) 0.3652(4) 0.044(3) Uani 1 1 d U . . H9 H 0.2897 -0.0241 0.3623 0.053 Uiso 1 1 calc R . . C10 C 0.3273(11) 0.0596(4) 0.4094(4) 0.041(3) Uani 1 1 d U . . H10 H 0.3919 0.0519 0.4360 0.049 Uiso 1 1 calc R . . C11 C 0.2943(10) 0.1164(4) 0.4152(3) 0.026(2) Uani 1 1 d U . . C12 C 0.2085(11) 0.1260(4) 0.3742(4) 0.036(2) Uani 1 1 d U . . H12 H 0.1912 0.1653 0.3763 0.043 Uiso 1 1 calc R . . C13 C 0.1461(11) 0.0808(4) 0.3298(4) 0.037(2) Uani 1 1 d U . . H13 H 0.0849 0.0889 0.3024 0.044 Uiso 1 1 calc R . . C14 C 0.3483(10) 0.1675(4) 0.4648(3) 0.0314(9) Uani 1 1 d U . . C15 C 0.3693(10) 0.1543(4) 0.5131(3) 0.0314(9) Uani 1 1 d U . . H15 H 0.3629 0.1134 0.5119 0.038 Uiso 1 1 calc R . . C16 C 0.3994(10) 0.1956(4) 0.5644(3) 0.0314(9) Uani 1 1 d U . . C17 C 0.4102(11) 0.1725(4) 0.6135(3) 0.035(2) Uani 1 1 d U . . C18 C 0.5304(11) 0.1313(4) 0.6104(4) 0.043(3) Uani 1 1 d U . . H18A H 0.5473 0.1227 0.6448 0.065 Uiso 1 1 calc R . . H18B H 0.6260 0.1512 0.6015 0.065 Uiso 1 1 calc R . . H18C H 0.4940 0.0941 0.5829 0.065 Uiso 1 1 calc R . . C19 C 0.2560(11) 0.1381(4) 0.6196(4) 0.046(3) Uani 1 1 d U . . H19A H 0.1785 0.1632 0.6197 0.069 Uiso 1 1 calc R . . H19B H 0.2613 0.1267 0.6531 0.069 Uiso 1 1 calc R . . H19C H 0.2293 0.1022 0.5898 0.069 Uiso 1 1 calc R . . C20 C 0.4608(12) 0.2257(4) 0.6635(4) 0.044(3) Uani 1 1 d U . . H20A H 0.3871 0.2529 0.6668 0.066 Uiso 1 1 calc R . . H20B H 0.5611 0.2470 0.6600 0.066 Uiso 1 1 calc R . . H20C H 0.4662 0.2109 0.6953 0.066 Uiso 1 1 calc R . . C21 C 0.5215(11) 0.4746(5) 0.6368(4) 0.050(3) Uani 1 1 d U . . H21A H 0.5350 0.4376 0.6456 0.075 Uiso 1 1 calc R . . H21B H 0.5468 0.5080 0.6688 0.075 Uiso 1 1 calc R . . H21C H 0.5885 0.4813 0.6098 0.075 Uiso 1 1 calc R . . C22 C 0.3361(12) 0.5292(4) 0.6058(4) 0.043(3) Uani 1 1 d U . . H22A H 0.3612 0.5607 0.6391 0.065 Uiso 1 1 calc R . . H22B H 0.2299 0.5268 0.5925 0.065 Uiso 1 1 calc R . . H22C H 0.4027 0.5385 0.5794 0.065 Uiso 1 1 calc R . . C23 C 0.2532(11) 0.4538(4) 0.6555(4) 0.041(3) Uani 1 1 d U . . H23A H 0.2748 0.4174 0.6636 0.062 Uiso 1 1 calc R . . H23B H 0.1472 0.4475 0.6405 0.062 Uiso 1 1 calc R . . H23C H 0.2702 0.4864 0.6882 0.062 Uiso 1 1 calc R . . C24 C 0.3582(10) 0.4697(4) 0.6155(3) 0.031(2) Uani 1 1 d U . . C25 C 0.3276(10) 0.4177(4) 0.5634(3) 0.0318(9) Uani 1 1 d U . . C26 C 0.2984(10) 0.4258(4) 0.5145(3) 0.0318(9) Uani 1 1 d U . . H26 H 0.2996 0.4659 0.5137 0.038 Uiso 1 1 calc R . . C27 C 0.2664(10) 0.3832(4) 0.4645(3) 0.0318(9) Uani 1 1 d U . . C28 C 0.2130(10) 0.3974(4) 0.4153(3) 0.028(2) Uani 1 1 d U . . C29 C 0.2231(10) 0.3577(4) 0.3665(4) 0.034(2) Uani 1 1 d U . . H29 H 0.2672 0.3234 0.3656 0.041 Uiso 1 1 calc R . . C30 C 0.1703(11) 0.3675(4) 0.3196(4) 0.040(3) Uani 1 1 d U . . H30 H 0.1764 0.3393 0.2870 0.048 Uiso 1 1 calc R . . C31 C 0.1077(10) 0.4182(4) 0.3188(4) 0.032(2) Uani 1 1 d U . . C32 C 0.0933(10) 0.4578(4) 0.3683(4) 0.034(2) Uani 1 1 d U . . H32 H 0.0476 0.4919 0.3694 0.041 Uiso 1 1 calc R . . C33 C 0.1463(10) 0.4468(4) 0.4152(4) 0.033(2) Uani 1 1 d U . . H33 H 0.1365 0.4738 0.4482 0.040 Uiso 1 1 calc R . . C34 C 0.0619(11) 0.4286(4) 0.2670(4) 0.0360(9) Uani 1 1 d U . . C35 C 0.0842(10) 0.4879(4) 0.2627(4) 0.0360(9) Uani 1 1 d U . . H35 H 0.1174 0.5186 0.2945 0.043 Uiso 1 1 calc R . . C36 C 0.0618(11) 0.5053(4) 0.2159(4) 0.0360(9) Uani 1 1 d U A . C37 C 0.0987(11) 0.5723(4) 0.2163(4) 0.037(2) Uani 1 1 d U . . C38 C 0.179(3) 0.5786(14) 0.1699(11) 0.066(5) Uiso 0.50 1 d P A 1 H38A H 0.1126 0.5576 0.1373 0.099 Uiso 0.50 1 calc PR A 1 H38B H 0.2716 0.5614 0.1703 0.099 Uiso 0.50 1 calc PR A 1 H38C H 0.2051 0.6208 0.1712 0.099 Uiso 0.50 1 calc PR A 1 C39 C -0.063(3) 0.5926(11) 0.2104(10) 0.066(5) Uiso 0.50 1 d P A 1 H39A H -0.0472 0.6346 0.2101 0.099 Uiso 0.50 1 calc PR A 1 H39B H -0.1194 0.5875 0.2404 0.099 Uiso 0.50 1 calc PR A 1 H39C H -0.1206 0.5682 0.1771 0.099 Uiso 0.50 1 calc PR A 1 C40 C 0.182(3) 0.6097(11) 0.2632(10) 0.066(5) Uiso 0.50 1 d P A 1 H40A H 0.2248 0.6479 0.2569 0.099 Uiso 0.50 1 calc PR A 1 H40B H 0.2646 0.5908 0.2738 0.099 Uiso 0.50 1 calc PR A 1 H40C H 0.1147 0.6165 0.2916 0.099 Uiso 0.50 1 calc PR A 1 C38A C 0.264(2) 0.6043(10) 0.2528(8) 0.048(6) Uiso 0.50 1 d P A 2 H38D H 0.3381 0.5776 0.2448 0.072 Uiso 0.50 1 calc PR A 2 H38E H 0.2487 0.6124 0.2906 0.072 Uiso 0.50 1 calc PR A 2 H38F H 0.3018 0.6418 0.2443 0.072 Uiso 0.50 1 calc PR A 2 C39A C -0.020(3) 0.6008(10) 0.2429(9) 0.052(6) Uiso 0.50 1 d P A 2 H39D H 0.0041 0.6438 0.2473 0.077 Uiso 0.50 1 calc PR A 2 H39E H -0.0260 0.5930 0.2778 0.077 Uiso 0.50 1 calc PR A 2 H39F H -0.1178 0.5847 0.2213 0.077 Uiso 0.50 1 calc PR A 2 C40A C 0.121(2) 0.5794(10) 0.1611(8) 0.035(6) Uiso 0.50 1 d P A 2 H40D H 0.1296 0.6215 0.1617 0.052 Uiso 0.50 1 calc PR A 2 H40E H 0.0336 0.5562 0.1363 0.052 Uiso 0.50 1 calc PR A 2 H40F H 0.2139 0.5651 0.1495 0.052 Uiso 0.50 1 calc PR A 2 C41 C -0.1067(12) -0.1864(4) 0.0030(4) 0.055(3) Uani 1 1 d U . . H41A H -0.1144 -0.2028 0.0339 0.082 Uiso 1 1 calc R . . H41B H -0.0036 -0.1645 0.0044 0.082 Uiso 1 1 calc R . . H41C H -0.1287 -0.2190 -0.0297 0.082 Uiso 1 1 calc R . . C42 C -0.2174(14) -0.1217(5) -0.0464(4) 0.062(3) Uani 1 1 d U . . H42A H -0.2541 -0.1550 -0.0777 0.094 Uiso 1 1 calc R . . H42B H -0.1128 -0.1041 -0.0495 0.094 Uiso 1 1 calc R . . H42C H -0.2826 -0.0915 -0.0440 0.094 Uiso 1 1 calc R . . C43 C -0.3781(11) -0.1772(4) 0.0057(4) 0.054(3) Uani 1 1 d U . . H43A H -0.4028 -0.2120 -0.0252 0.081 Uiso 1 1 calc R . . H43B H -0.4523 -0.1508 0.0050 0.081 Uiso 1 1 calc R . . H43C H -0.3813 -0.1903 0.0383 0.081 Uiso 1 1 calc R . . C44 C -0.2214(11) -0.1443(4) 0.0038(4) 0.037(3) Uani 1 1 d U . . C45 C -0.1790(10) -0.0943(4) 0.0559(4) 0.0340(9) Uani 1 1 d U . . C46 C -0.1732(10) -0.0331(4) 0.0549(4) 0.0340(9) Uani 1 1 d U . . H46 H -0.1910 -0.0250 0.0216 0.041 Uiso 1 1 calc R . . C47 C -0.1424(10) 0.0154(4) 0.1009(4) 0.0340(9) Uani 1 1 d U . . C48 C -0.1624(10) 0.0770(4) 0.0978(3) 0.027(2) Uani 1 1 d U . . C49 C -0.2353(11) 0.0889(4) 0.0541(4) 0.037(2) Uani 1 1 d U . . H49 H -0.2771 0.0568 0.0243 0.044 Uiso 1 1 calc R . . C50 C -0.2481(11) 0.1457(4) 0.0532(4) 0.038(3) Uani 1 1 d U . . H50 H -0.3010 0.1526 0.0234 0.046 Uiso 1 1 calc R . . C51 C -0.1827(10) 0.1936(4) 0.0963(4) 0.034(2) Uani 1 1 d U . . C52 C -0.1138(11) 0.1829(4) 0.1407(4) 0.035(2) Uani 1 1 d U . . H52 H -0.0757 0.2149 0.1710 0.042 Uiso 1 1 calc R . . C53 C -0.1004(11) 0.1246(4) 0.1406(4) 0.040(3) Uani 1 1 d U . . H53 H -0.0479 0.1175 0.1704 0.048 Uiso 1 1 calc R . . C54 C -0.1832(11) 0.2589(4) 0.0966(4) 0.0356(9) Uani 1 1 d U A . C55 C -0.1964(10) 0.2749(4) 0.0491(4) 0.0356(9) Uani 1 1 d U . . H55 H -0.2133 0.2431 0.0175 0.043 Uiso 1 1 calc R . . C56 C -0.1875(11) 0.3322(4) 0.0422(4) 0.0356(9) Uani 1 1 d U A . C57 C -0.2067(11) 0.3432(4) -0.0137(4) 0.038(3) Uani 1 1 d DU . . C58 C -0.3439(19) 0.3704(8) -0.0168(6) 0.071(5) Uani 0.75 1 d PU B 1 H58A H -0.3389 0.4044 0.0143 0.106 Uiso 0.75 1 calc PR B 1 H58B H -0.4346 0.3409 -0.0175 0.106 Uiso 0.75 1 calc PR B 1 H58C H -0.3493 0.3840 -0.0492 0.106 Uiso 0.75 1 calc PR B 1 C59 C -0.070(2) 0.3874(9) -0.0177(7) 0.086(6) Uani 0.75 1 d PU B 1 H59A H -0.0753 0.3939 -0.0533 0.129 Uiso 0.75 1 calc PR B 1 H59B H 0.0228 0.3719 -0.0113 0.129 Uiso 0.75 1 calc PR B 1 H59C H -0.0688 0.4252 0.0090 0.129 Uiso 0.75 1 calc PR B 1 C60 C -0.215(2) 0.2880(7) -0.0586(6) 0.067(5) Uani 0.75 1 d PU B 1 H60A H -0.3045 0.2589 -0.0567 0.100 Uiso 0.75 1 calc PR B 1 H60B H -0.1232 0.2709 -0.0556 0.100 Uiso 0.75 1 calc PR B 1 H60C H -0.2245 0.2982 -0.0926 0.100 Uiso 0.75 1 calc PR B 1 C60A C -0.330(3) 0.2951(12) -0.0488(14) 0.063(8) Uiso 0.25 1 d PD B 2 H60D H -0.4278 0.2987 -0.0347 0.094 Uiso 0.25 1 calc PR B 2 H60E H -0.3054 0.2558 -0.0494 0.094 Uiso 0.25 1 calc PR B 2 H60F H -0.3349 0.2999 -0.0850 0.094 Uiso 0.25 1 calc PR B 2 C59A C -0.053(2) 0.3378(16) -0.0337(15) 0.063(8) Uiso 0.25 1 d PD B 2 H59D H -0.0376 0.3598 -0.0607 0.094 Uiso 0.25 1 calc PR B 2 H59E H -0.0488 0.2958 -0.0494 0.094 Uiso 0.25 1 calc PR B 2 H59F H 0.0266 0.3543 -0.0041 0.094 Uiso 0.25 1 calc PR B 2 C58A C -0.244(4) 0.4041(8) -0.0092(17) 0.063(8) Uiso 0.25 1 d PD B 2 H58D H -0.2006 0.4308 0.0254 0.094 Uiso 0.25 1 calc PR B 2 H58E H -0.3548 0.4016 -0.0124 0.094 Uiso 0.25 1 calc PR B 2 H58F H -0.2017 0.4197 -0.0376 0.094 Uiso 0.25 1 calc PR B 2 C61 C 0.2147(12) -0.1072(4) 0.1171(4) 0.043(3) Uani 1 1 d U . . H61 H 0.1578 -0.1439 0.1191 0.052 Uiso 1 1 calc R . . C62 C 0.3541(13) -0.1075(5) 0.0996(4) 0.057(3) Uani 1 1 d U . . H62 H 0.3931 -0.1436 0.0906 0.069 Uiso 1 1 calc R . . C63 C 0.4413(13) -0.0546(5) 0.0947(4) 0.060(3) Uani 1 1 d U . . H63 H 0.5407 -0.0533 0.0836 0.072 Uiso 1 1 calc R . . C64 C 0.3740(13) -0.0055(5) 0.1070(4) 0.057(3) Uani 1 1 d U . . H64 H 0.4238 0.0312 0.1022 0.069 Uiso 1 1 calc R . . C65 C 0.2344(12) -0.0089(5) 0.1261(4) 0.052(3) Uani 1 1 d U . . H65 H 0.1934 0.0267 0.1361 0.063 Uiso 1 1 calc R . . C66 C -0.3468(13) -0.1133(5) 0.2006(4) 0.057(3) Uani 1 1 d U . . H66 H -0.3194 -0.1488 0.1801 0.068 Uiso 1 1 calc R . . C67 C -0.4793(13) -0.1179(6) 0.2240(5) 0.065(3) Uani 1 1 d U . . H67 H -0.5405 -0.1556 0.2206 0.078 Uiso 1 1 calc R . . C68 C -0.5213(15) -0.0663(6) 0.2525(5) 0.072(4) Uani 1 1 d U . . H68 H -0.6140 -0.0677 0.2685 0.086 Uiso 1 1 calc R . . C69 C -0.4294(14) -0.0130(6) 0.2577(5) 0.067(3) Uani 1 1 d U . . H69 H -0.4553 0.0229 0.2783 0.080 Uiso 1 1 calc R . . C70 C -0.2974(13) -0.0120(5) 0.2324(4) 0.054(3) Uani 1 1 d U . . H70 H -0.2356 0.0253 0.2347 0.064 Uiso 1 1 calc R . . C71 C 0.6744(11) 0.3475(4) 0.5604(4) 0.037(2) Uani 1 1 d U . . H71 H 0.6353 0.3416 0.5920 0.044 Uiso 1 1 calc R . . C72 C 0.8237(12) 0.3740(4) 0.5633(5) 0.049(3) Uani 1 1 d U . . H72 H 0.8856 0.3868 0.5962 0.059 Uiso 1 1 calc R . . C73 C 0.8814(13) 0.3815(4) 0.5175(5) 0.053(3) Uani 1 1 d U . . H73 H 0.9844 0.3993 0.5181 0.064 Uiso 1 1 calc R . . C74 C 0.7874(12) 0.3628(4) 0.4706(4) 0.048(3) Uani 1 1 d U . . H74 H 0.8254 0.3671 0.4384 0.057 Uiso 1 1 calc R . . C75 C 0.6377(12) 0.3377(4) 0.4708(4) 0.039(3) Uani 1 1 d U . . H75 H 0.5732 0.3258 0.4385 0.046 Uiso 1 1 calc R . . C76 C 0.0162(12) 0.2380(4) 0.4764(4) 0.039(3) Uani 1 1 d U . . H76 H 0.0524 0.2378 0.4429 0.047 Uiso 1 1 calc R . . C77 C -0.1318(13) 0.2176(4) 0.4770(4) 0.046(3) Uani 1 1 d U . . H77 H -0.1979 0.2039 0.4450 0.056 Uiso 1 1 calc R . . C78 C -0.1848(13) 0.2172(4) 0.5247(4) 0.048(3) Uani 1 1 d U . . H78 H -0.2893 0.2034 0.5265 0.057 Uiso 1 1 calc R . . C79 C -0.0857(12) 0.2369(4) 0.5705(4) 0.045(3) Uani 1 1 d U . . H79 H -0.1203 0.2357 0.6040 0.054 Uiso 1 1 calc R . . C80 C 0.0618(12) 0.2580(4) 0.5668(4) 0.041(3) Uani 1 1 d U . . H80 H 0.1289 0.2728 0.5986 0.049 Uiso 1 1 calc R . . C81 C 0.1954(13) 0.3917(5) 0.0931(4) 0.049(3) Uani 1 1 d U . . H81 H 0.1488 0.4219 0.0839 0.059 Uiso 1 1 calc R . . C82 C 0.3292(13) 0.3807(5) 0.0713(4) 0.056(3) Uani 1 1 d U . . H82 H 0.3713 0.4013 0.0471 0.067 Uiso 1 1 calc R . . C83 C 0.3973(13) 0.3387(5) 0.0863(4) 0.055(3) Uani 1 1 d U . . H83 H 0.4905 0.3306 0.0729 0.067 Uiso 1 1 calc R . . C84 C 0.3354(12) 0.3075(5) 0.1203(4) 0.052(3) Uani 1 1 d U . . H84 H 0.3824 0.2781 0.1305 0.062 Uiso 1 1 calc R . . C85 C 0.1984(12) 0.3221(4) 0.1388(4) 0.043(3) Uani 1 1 d U . . H85 H 0.1529 0.3013 0.1622 0.052 Uiso 1 1 calc R . . C86 C -0.3385(12) 0.4482(4) 0.1732(4) 0.043(3) Uani 1 1 d U . . H86 H -0.2876 0.4696 0.1512 0.052 Uiso 1 1 calc R . . C87 C -0.4780(13) 0.4625(5) 0.1915(4) 0.055(3) Uani 1 1 d U . . H87 H -0.5224 0.4920 0.1803 0.067 Uiso 1 1 calc R . . C88 C -0.5478(13) 0.4339(5) 0.2250(4) 0.059(3) Uani 1 1 d U . . H88 H -0.6393 0.4438 0.2387 0.071 Uiso 1 1 calc R . . C89 C -0.4819(13) 0.3900(5) 0.2385(4) 0.052(3) Uani 1 1 d U . . H89 H -0.5291 0.3686 0.2613 0.063 Uiso 1 1 calc R . . C90 C -0.3501(12) 0.3772(5) 0.2195(4) 0.044(3) Uani 1 1 d U . . H90 H -0.3061 0.3471 0.2298 0.053 Uiso 1 1 calc R . . C91 C 0.8969(14) 0.0529(5) 0.4319(5) 0.066(3) Uani 1 1 d U . . H91 H 0.9605 0.0563 0.4045 0.079 Uiso 1 1 calc R . . C92 C 0.7437(18) 0.0295(6) 0.4205(6) 0.086(4) Uani 1 1 d U . . H92 H 0.7017 0.0188 0.3845 0.103 Uiso 1 1 calc R . . N7 N 0.6530(12) 0.0213(5) 0.4567(5) 0.074(3) Uani 1 1 d U . . C94 C 0.7139(14) 0.0370(5) 0.5053(5) 0.060(3) Uani 1 1 d U . . H94 H 0.6515 0.0296 0.5319 0.072 Uiso 1 1 calc R . . C95 C 0.8598(17) 0.0632(6) 0.5208(6) 0.080(4) Uani 1 1 d U . . H95 H 0.8973 0.0762 0.5574 0.096 Uiso 1 1 calc R . . C93 C 0.9509(15) 0.0703(6) 0.4826(6) 0.073(4) Uani 1 1 d U . . H93 H 1.0548 0.0880 0.4923 0.088 Uiso 1 1 calc R . . C96 C 0.7769(19) 0.1498(8) 0.3226(6) 0.093(5) Uani 1 1 d U . . H96 H 0.8049 0.1118 0.3189 0.111 Uiso 1 1 calc R . . N8 N 0.6430(16) 0.1579(7) 0.3436(5) 0.113(4) Uani 1 1 d U . . C97 C 0.5951(16) 0.2118(7) 0.3470(5) 0.079(4) Uani 1 1 d U . . H97 H 0.5008 0.2185 0.3602 0.095 Uiso 1 1 calc R . . C98 C 0.6857(18) 0.2553(7) 0.3310(5) 0.095(5) Uani 1 1 d U . . H98 H 0.6581 0.2932 0.3336 0.114 Uiso 1 1 calc R . . C99 C 0.8241(18) 0.2407(8) 0.3101(6) 0.105(5) Uani 1 1 d U . . H99 H 0.8883 0.2692 0.2976 0.126 Uiso 1 1 calc R . . C100 C 0.8656(16) 0.1868(7) 0.3079(5) 0.080(4) Uani 1 1 d U . . H100 H 0.9593 0.1780 0.2954 0.096 Uiso 1 1 calc R . . N9 N 0.4100(17) 0.2349(6) 0.2120(5) 0.100(4) Uani 1 1 d U . . C101 C 0.5139(17) 0.2051(8) 0.1989(6) 0.089(4) Uani 1 1 d U . . H101 H 0.5997 0.2236 0.1857 0.107 Uiso 1 1 calc R . . C102 C 0.512(2) 0.1495(8) 0.2022(6) 0.102(5) Uani 1 1 d U . . H102 H 0.5937 0.1291 0.1922 0.123 Uiso 1 1 calc R . . C103 C 0.290(2) 0.2093(9) 0.2315(7) 0.114(6) Uani 1 1 d U . . H103 H 0.2161 0.2324 0.2448 0.137 Uiso 1 1 calc R . . C104 C 0.272(2) 0.1531(10) 0.2330(7) 0.129(6) Uani 1 1 d U . . H104 H 0.1797 0.1342 0.2424 0.154 Uiso 1 1 calc R . . C105 C 0.389(2) 0.1234(7) 0.2204(6) 0.103(5) Uani 1 1 d U . . H105 H 0.3849 0.0843 0.2245 0.124 Uiso 1 1 calc R . . C106 C 0.5211(15) 0.6850(7) 0.1691(5) 0.077(8) Uiso 0.50 1 d PG . . H106 H 0.4502 0.6836 0.1946 0.092 Uiso 0.50 1 calc PR . . C107 C 0.5511(16) 0.7350(6) 0.1499(6) 0.048(6) Uiso 0.50 1 d PG . . H107 H 0.5007 0.7678 0.1623 0.057 Uiso 0.50 1 calc PR . . C108 C 0.6547(18) 0.7371(6) 0.1125(6) 0.079(8) Uiso 0.50 1 d PG . . H108 H 0.6752 0.7712 0.0994 0.095 Uiso 0.50 1 calc PR . . C109 C 0.7284(17) 0.6891(8) 0.0943(6) 0.101(10) Uiso 0.50 1 d PG . . H109 H 0.7992 0.6905 0.0687 0.121 Uiso 0.50 1 calc PR . . C110 C 0.6984(16) 0.6391(6) 0.1135(6) 0.069(7) Uiso 0.50 1 d PG . . H110 H 0.7487 0.6063 0.1010 0.083 Uiso 0.50 1 calc PR . . N10 N 0.5947(17) 0.6371(5) 0.1509(6) 0.075(6) Uiso 0.50 1 d PG . . N1 N 0.1524(8) -0.0585(3) 0.1316(3) 0.034(2) Uani 1 1 d U . . N2 N -0.2538(9) -0.0623(4) 0.2047(3) 0.042(2) Uani 1 1 d U . . N3 N 0.5807(8) 0.3296(3) 0.5150(3) 0.0322(19) Uani 1 1 d U . . N4 N 0.1179(9) 0.2590(3) 0.5201(3) 0.034(2) Uani 1 1 d U . . N5 N 0.1269(9) 0.3635(3) 0.1259(3) 0.037(2) Uani 1 1 d U . . N6 N -0.2788(9) 0.4054(3) 0.1866(3) 0.039(2) Uani 1 1 d U . . O1 O -0.0190(7) -0.1339(2) 0.1896(2) 0.0328(9) Uani 1 1 d U . . O2 O 0.0617(7) -0.0082(2) 0.2363(2) 0.0328(9) Uani 1 1 d U . . O3 O 0.3613(7) 0.2192(2) 0.4576(2) 0.0314(9) Uani 1 1 d U . . O4 O 0.4110(7) 0.2515(2) 0.5716(2) 0.0314(9) Uani 1 1 d U . . O5 O 0.3381(7) 0.3671(2) 0.5726(2) 0.0318(9) Uani 1 1 d U . . O6 O 0.2847(7) 0.3284(2) 0.4590(2) 0.0318(9) Uani 1 1 d U . . O7 O 0.0066(7) 0.3823(2) 0.2295(2) 0.0360(9) Uani 1 1 d U . . O8 O 0.0054(7) 0.4713(3) 0.1706(2) 0.0360(9) Uani 1 1 d U . . O9 O -0.1610(7) -0.1118(2) 0.0972(2) 0.0340(9) Uani 1 1 d U . . O10 O -0.0976(7) 0.0125(2) 0.1472(2) 0.0340(9) Uani 1 1 d U . . O11 O -0.1575(7) 0.2950(3) 0.1432(2) 0.0356(9) Uani 1 1 d U . . O12 O -0.1603(7) 0.3799(2) 0.0813(2) 0.0356(9) Uani 1 1 d U . . Ni1 Ni -0.05291(14) -0.06037(5) 0.16759(5) 0.0343(3) Uani 1 1 d U . . Ni2 Ni 0.35012(14) 0.29242(5) 0.51604(5) 0.0343(3) Uani 1 1 d U . . Ni3 Ni -0.07646(14) 0.38280(5) 0.15642(5) 0.0343(3) Uani 1 1 d U A . 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 0.074(7) 0.042(6) 0.087(7) 0.013(5) 0.032(6) 0.018(5) C2 0.059(6) 0.022(5) 0.060(6) 0.002(4) 0.018(5) 0.016(5) C3 0.080(7) 0.044(6) 0.060(6) 0.007(5) -0.005(6) 0.012(5) C4 0.042(6) 0.019(5) 0.041(5) -0.005(4) 0.011(4) 0.012(4) C5 0.0368(19) 0.0182(16) 0.0367(18) -0.0071(14) 0.0035(16) 0.0083(15) C6 0.0368(19) 0.0182(16) 0.0367(18) -0.0071(14) 0.0035(16) 0.0083(15) C7 0.0368(19) 0.0182(16) 0.0367(18) -0.0071(14) 0.0035(16) 0.0083(15) C8 0.037(5) 0.014(5) 0.037(5) -0.007(4) 0.005(4) 0.013(4) C9 0.064(6) 0.023(5) 0.041(5) -0.008(4) -0.005(5) 0.021(5) C10 0.053(6) 0.024(5) 0.038(5) -0.009(4) -0.005(5) 0.015(5) C11 0.029(5) 0.015(4) 0.027(5) -0.008(4) -0.005(4) 0.008(4) C12 0.044(6) 0.012(4) 0.040(5) -0.013(4) 0.000(5) 0.007(4) C13 0.050(6) 0.015(5) 0.036(5) -0.007(4) -0.008(4) 0.006(4) C14 0.0372(19) 0.0175(15) 0.0324(17) -0.0063(14) 0.0025(15) 0.0052(15) C15 0.0372(19) 0.0175(15) 0.0324(17) -0.0063(14) 0.0025(15) 0.0052(15) C16 0.0372(19) 0.0175(15) 0.0324(17) -0.0063(14) 0.0025(15) 0.0052(15) C17 0.042(6) 0.019(5) 0.035(5) -0.008(4) 0.004(4) 0.008(4) C18 0.046(6) 0.034(5) 0.046(5) 0.003(4) 0.001(5) 0.012(5) C19 0.048(6) 0.035(5) 0.054(6) 0.008(5) 0.013(5) 0.010(5) C20 0.058(6) 0.032(5) 0.036(5) -0.005(4) 0.003(5) 0.010(5) C21 0.044(6) 0.043(6) 0.045(6) -0.017(5) 0.001(5) 0.000(5) C22 0.057(6) 0.016(5) 0.042(5) -0.013(4) 0.003(5) -0.001(4) C23 0.046(6) 0.029(5) 0.043(5) -0.007(4) 0.006(5) 0.019(5) C24 0.033(5) 0.015(4) 0.038(5) -0.005(4) -0.002(4) 0.004(4) C25 0.036(2) 0.0182(16) 0.0343(18) -0.0064(15) 0.0018(15) 0.0069(16) C26 0.036(2) 0.0182(16) 0.0343(18) -0.0064(15) 0.0018(15) 0.0069(16) C27 0.036(2) 0.0182(16) 0.0343(18) -0.0064(15) 0.0018(15) 0.0069(16) C28 0.036(5) 0.015(4) 0.028(5) -0.003(4) 0.003(4) 0.004(4) C29 0.043(6) 0.019(5) 0.038(5) 0.000(4) -0.001(4) 0.011(4) C30 0.046(6) 0.022(5) 0.042(5) -0.011(4) 0.001(5) 0.010(4) C31 0.033(5) 0.021(5) 0.039(5) 0.001(4) 0.002(4) 0.008(4) C32 0.035(5) 0.019(5) 0.040(5) -0.007(4) 0.010(4) 0.008(4) C33 0.039(5) 0.021(5) 0.035(5) -0.004(4) 0.009(4) 0.006(4) C34 0.044(2) 0.0182(17) 0.040(2) -0.0039(14) 0.0037(17) 0.0071(16) C35 0.044(2) 0.0182(17) 0.040(2) -0.0039(14) 0.0037(17) 0.0071(16) C36 0.044(2) 0.0182(17) 0.040(2) -0.0039(14) 0.0037(17) 0.0071(16) C37 0.047(6) 0.017(5) 0.045(5) 0.001(4) 0.001(5) 0.011(4) C41 0.057(6) 0.036(6) 0.056(6) -0.018(5) 0.003(5) 0.016(5) C42 0.084(7) 0.042(6) 0.049(6) -0.011(5) 0.009(5) 0.012(5) C43 0.046(6) 0.040(6) 0.052(6) -0.031(5) 0.001(5) 0.006(5) C44 0.043(6) 0.016(5) 0.038(5) -0.015(4) -0.001(4) 0.004(4) C45 0.038(2) 0.0171(16) 0.0383(18) -0.0068(14) 0.0029(16) 0.0040(15) C46 0.038(2) 0.0171(16) 0.0383(18) -0.0068(14) 0.0029(16) 0.0040(15) C47 0.038(2) 0.0171(16) 0.0383(18) -0.0068(14) 0.0029(16) 0.0040(15) C48 0.030(5) 0.018(5) 0.030(5) -0.002(4) 0.007(4) 0.004(4) C49 0.041(6) 0.020(5) 0.039(5) -0.009(4) -0.005(4) 0.005(4) C50 0.042(6) 0.020(5) 0.040(5) -0.013(4) -0.012(4) 0.009(4) C51 0.032(5) 0.025(5) 0.039(5) -0.004(4) 0.011(4) 0.007(4) C52 0.051(6) 0.019(5) 0.031(5) -0.004(4) 0.003(4) 0.014(4) C53 0.051(6) 0.025(5) 0.034(5) -0.008(4) -0.001(4) 0.005(4) C54 0.041(2) 0.0198(17) 0.0390(19) -0.0061(14) 0.0022(17) 0.0084(16) C55 0.041(2) 0.0198(17) 0.0390(19) -0.0061(14) 0.0022(17) 0.0084(16) C56 0.041(2) 0.0198(17) 0.0390(19) -0.0061(14) 0.0022(17) 0.0084(16) C57 0.043(6) 0.030(5) 0.039(5) 0.000(4) 0.000(4) 0.017(5) C58 0.074(9) 0.086(9) 0.053(8) 0.010(7) -0.008(7) 0.032(7) C59 0.090(10) 0.092(9) 0.076(9) 0.033(8) 0.014(7) -0.003(8) C60 0.089(9) 0.067(8) 0.047(7) 0.011(6) 0.010(7) 0.029(7) C61 0.043(6) 0.031(5) 0.047(6) -0.007(4) 0.004(5) 0.010(5) C62 0.058(7) 0.045(6) 0.064(6) -0.002(5) 0.013(5) 0.017(5) C63 0.052(6) 0.048(6) 0.067(6) -0.011(5) 0.016(5) 0.010(5) C64 0.047(6) 0.040(6) 0.073(7) 0.001(5) 0.008(5) -0.002(5) C65 0.043(6) 0.032(6) 0.071(6) -0.005(5) 0.007(5) 0.005(5) C66 0.053(7) 0.048(6) 0.066(6) 0.007(5) -0.001(5) 0.014(5) C67 0.050(7) 0.069(7) 0.074(7) 0.015(6) 0.012(6) 0.007(6) C68 0.057(7) 0.088(8) 0.072(7) 0.019(6) 0.013(6) 0.022(6) C69 0.069(7) 0.063(7) 0.069(7) 0.004(6) 0.023(6) 0.029(6) C70 0.056(6) 0.038(6) 0.059(6) -0.006(5) 0.017(5) 0.010(5) C71 0.040(6) 0.022(5) 0.040(5) -0.007(4) 0.001(5) 0.008(4) C72 0.049(6) 0.023(5) 0.066(6) -0.006(5) 0.003(5) 0.004(5) C73 0.045(6) 0.026(5) 0.079(7) -0.002(5) 0.004(6) 0.007(5) C74 0.044(6) 0.038(6) 0.059(6) 0.007(5) 0.015(5) 0.011(5) C75 0.040(6) 0.027(5) 0.050(6) 0.004(4) 0.008(5) 0.019(5) C76 0.040(6) 0.025(5) 0.048(6) -0.001(4) 0.010(5) 0.010(5) C77 0.047(6) 0.033(5) 0.050(6) 0.000(5) -0.005(5) 0.003(5) C78 0.044(6) 0.033(5) 0.063(6) 0.008(5) -0.004(5) 0.007(5) C79 0.046(6) 0.043(6) 0.050(6) 0.015(5) 0.011(5) 0.014(5) C80 0.045(6) 0.032(5) 0.045(6) 0.006(4) 0.003(5) 0.015(5) C81 0.051(6) 0.043(6) 0.045(6) 0.002(5) 0.004(5) 0.003(5) C82 0.051(6) 0.061(7) 0.048(6) -0.001(5) 0.014(5) 0.004(6) C83 0.046(6) 0.050(6) 0.052(6) -0.018(5) 0.004(5) 0.008(5) C84 0.054(6) 0.028(5) 0.057(6) -0.023(5) 0.003(5) 0.020(5) C85 0.047(6) 0.032(5) 0.037(5) -0.014(4) -0.001(5) 0.004(5) C86 0.050(6) 0.030(5) 0.042(5) -0.008(4) -0.005(5) 0.013(5) C87 0.056(7) 0.033(6) 0.062(6) -0.022(5) -0.009(5) 0.026(5) C88 0.052(6) 0.057(7) 0.045(6) -0.029(5) 0.007(5) 0.009(6) C89 0.055(7) 0.048(6) 0.038(6) -0.014(5) 0.007(5) 0.002(5) C90 0.047(6) 0.032(5) 0.041(5) -0.009(5) -0.002(5) 0.005(5) C91 0.058(7) 0.056(7) 0.075(7) -0.001(6) 0.030(6) 0.003(6) C92 0.103(9) 0.073(8) 0.074(7) 0.008(6) -0.004(7) 0.015(7) N7 0.063(6) 0.061(6) 0.085(7) -0.001(5) 0.011(6) 0.006(5) C94 0.059(7) 0.051(6) 0.072(7) 0.021(6) 0.010(6) 0.008(6) C95 0.090(8) 0.066(7) 0.083(7) 0.021(6) 0.011(7) 0.004(6) C93 0.064(7) 0.067(7) 0.087(8) 0.014(6) 0.011(6) 0.015(6) C96 0.084(8) 0.092(8) 0.094(8) -0.002(7) 0.018(7) 0.035(7) N8 0.116(8) 0.111(8) 0.098(7) 0.005(6) -0.005(6) 0.021(7) C97 0.080(8) 0.078(8) 0.069(7) 0.001(6) 0.012(6) 0.012(7) C98 0.104(9) 0.076(8) 0.086(8) -0.010(6) 0.010(7) 0.015(7) C99 0.089(9) 0.115(9) 0.092(8) 0.018(7) 0.007(7) -0.022(7) C100 0.062(7) 0.081(8) 0.085(8) -0.001(6) 0.022(6) 0.008(7) N9 0.102(8) 0.074(7) 0.124(8) 0.031(6) 0.012(7) 0.008(6) C101 0.077(8) 0.094(8) 0.097(8) 0.029(7) 0.015(7) 0.007(7) C102 0.103(9) 0.104(9) 0.090(8) -0.002(7) 0.005(7) 0.035(8) C103 0.105(9) 0.126(10) 0.111(9) 0.017(8) 0.018(7) 0.042(8) C104 0.113(10) 0.141(10) 0.122(10) 0.046(8) -0.009(8) -0.020(8) C105 0.130(9) 0.071(8) 0.095(8) 0.015(7) -0.023(7) -0.002(8) N1 0.035(5) 0.024(4) 0.033(4) -0.009(3) 0.001(3) 0.003(4) N2 0.036(5) 0.033(5) 0.050(5) -0.004(4) 0.000(4) 0.013(4) N3 0.036(5) 0.009(4) 0.044(5) -0.009(3) 0.002(4) 0.008(3) N4 0.040(5) 0.016(4) 0.038(5) -0.011(3) -0.001(4) 0.009(4) N5 0.037(5) 0.025(4) 0.035(4) -0.016(4) -0.004(4) 0.006(4) N6 0.041(5) 0.024(4) 0.039(5) -0.017(4) -0.013(4) 0.010(4) O1 0.0368(19) 0.0182(16) 0.0367(18) -0.0071(14) 0.0035(16) 0.0083(15) O2 0.0368(19) 0.0182(16) 0.0367(18) -0.0071(14) 0.0035(16) 0.0083(15) O3 0.0372(19) 0.0175(15) 0.0324(17) -0.0063(14) 0.0025(15) 0.0052(15) O4 0.0372(19) 0.0175(15) 0.0324(17) -0.0063(14) 0.0025(15) 0.0052(15) O5 0.036(2) 0.0182(16) 0.0343(18) -0.0064(15) 0.0018(15) 0.0069(16) O6 0.036(2) 0.0182(16) 0.0343(18) -0.0064(15) 0.0018(15) 0.0069(16) O7 0.044(2) 0.0182(17) 0.040(2) -0.0039(14) 0.0037(17) 0.0071(16) O8 0.044(2) 0.0182(17) 0.040(2) -0.0039(14) 0.0037(17) 0.0071(16) O9 0.038(2) 0.0171(16) 0.0383(18) -0.0068(14) 0.0029(16) 0.0040(15) O10 0.038(2) 0.0171(16) 0.0383(18) -0.0068(14) 0.0029(16) 0.0040(15) O11 0.041(2) 0.0198(17) 0.0390(19) -0.0061(14) 0.0022(17) 0.0084(16) O12 0.041(2) 0.0198(17) 0.0390(19) -0.0061(14) 0.0022(17) 0.0084(16) Ni1 0.0431(5) 0.0118(4) 0.0380(5) -0.0115(3) 0.0009(3) 0.0063(3) Ni2 0.0431(5) 0.0118(4) 0.0380(5) -0.0115(3) 0.0009(3) 0.0063(3) Ni3 0.0431(5) 0.0118(4) 0.0380(5) -0.0115(3) 0.0009(3) 0.0063(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.538(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.523(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.504(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.552(12) . ? C5 O1 1.254(10) . ? C5 C6 1.420(12) . ? C6 C7 1.419(12) . ? C6 H6 0.9500 . ? C7 O2 1.250(10) . ? C7 C8 1.532(12) . ? C8 C9 1.361(12) . ? C8 C13 1.409(12) . ? C9 C10 1.375(13) . ? C9 H9 0.9500 . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 C12 1.369(12) . ? C11 C14 1.526(11) . ? C12 C13 1.382(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O3 1.269(10) . ? C14 C15 1.384(12) . ? C15 C16 1.426(12) . ? C15 H15 0.9500 . ? C16 O4 1.271(10) . ? C16 C17 1.522(12) . ? C17 C19 1.528(13) . ? C17 C18 1.547(12) . ? C17 C20 1.554(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.510(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.528(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.525(13) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.562(12) . ? C25 O5 1.291(10) . ? C25 C26 1.357(12) . ? C26 C27 1.416(12) . ? C26 H26 0.9500 . ? C27 O6 1.300(10) . ? C27 C28 1.479(12) . ? C28 C33 1.388(12) . ? C28 C29 1.397(12) . ? C29 C30 1.375(12) . ? C29 H29 0.9500 . ? C30 C31 1.400(12) . ? C30 H30 0.9500 . ? C31 C32 1.416(12) . ? C31 C34 1.482(12) . ? C32 C33 1.391(12) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O7 1.278(10) . ? C34 C35 1.416(12) . ? C35 C36 1.399(12) . ? C35 H35 0.9500 . ? C36 O8 1.276(10) . ? C36 C37 1.561(12) . ? C37 C40 1.41(2) . ? C37 C39A 1.46(2) . ? C37 C38 1.47(3) . ? C37 C40A 1.52(2) . ? C37 C39 1.60(3) . ? C37 C38A 1.67(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41 C44 1.533(13) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.537(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.505(13) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.542(12) . ? C45 O9 1.261(10) . ? C45 C46 1.442(12) . ? C46 C47 1.412(12) . ? C46 H46 0.9500 . ? C47 O10 1.277(10) . ? C47 C48 1.512(12) . ? C48 C53 1.385(12) . ? C48 C49 1.393(12) . ? C49 C50 1.368(12) . ? C49 H49 0.9500 . ? C50 C51 1.403(12) . ? C50 H50 0.9500 . ? C51 C52 1.380(12) . ? C51 C54 1.537(12) . ? C52 C53 1.399(12) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 O11 1.282(10) . ? C54 C55 1.391(12) . ? C55 C56 1.401(12) . ? C55 H55 0.9500 . ? C56 O12 1.293(10) . ? C56 C57 1.552(12) . ? C57 C58 1.479(16) . ? C57 C58A 1.503(10) . ? C57 C60 1.503(17) . ? C57 C59 1.507(18) . ? C57 C59A 1.510(10) . ? C57 C60A 1.521(10) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C60A H60D 0.9800 . ? C60A H60E 0.9800 . ? C60A H60F 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C61 N1 1.332(11) . ? C61 C62 1.353(13) . ? C61 H61 0.9500 . ? C62 C63 1.405(15) . ? C62 H62 0.9500 . ? C63 C64 1.364(15) . ? C63 H63 0.9500 . ? C64 C65 1.371(14) . ? C64 H64 0.9500 . ? C65 N1 1.326(12) . ? C65 H65 0.9500 . ? C66 N2 1.329(13) . ? C66 C67 1.367(15) . ? C66 H66 0.9500 . ? C67 C68 1.376(16) . ? C67 H67 0.9500 . ? C68 C69 1.363(16) . ? C68 H68 0.9500 . ? C69 C70 1.386(15) . ? C69 H69 0.9500 . ? C70 N2 1.351(12) . ? C70 H70 0.9500 . ? C71 N3 1.346(11) . ? C71 C72 1.375(13) . ? C71 H71 0.9500 . ? C72 C73 1.371(14) . ? C72 H72 0.9500 . ? C73 C74 1.378(14) . ? C73 H73 0.9500 . ? C74 C75 1.379(13) . ? C74 H74 0.9500 . ? C75 N3 1.335(11) . ? C75 H75 0.9500 . ? C76 C77 1.340(13) . ? C76 N4 1.354(12) . ? C76 H76 0.9500 . ? C77 C78 1.363(14) . ? C77 H77 0.9500 . ? C78 C79 1.380(14) . ? C78 H78 0.9500 . ? C79 C80 1.356(13) . ? C79 H79 0.9500 . ? C80 N4 1.352(12) . ? C80 H80 0.9500 . ? C81 N5 1.334(12) . ? C81 C82 1.388(14) . ? C81 H81 0.9500 . ? C82 C83 1.365(15) . ? C82 H82 0.9500 . ? C83 C84 1.377(15) . ? C83 H83 0.9500 . ? C84 C85 1.404(14) . ? C84 H84 0.9500 . ? C85 N5 1.344(12) . ? C85 H85 0.9500 . ? C86 N6 1.323(12) . ? C86 C87 1.420(14) . ? C86 H86 0.9500 . ? C87 C88 1.359(15) . ? C87 H87 0.9500 . ? C88 C89 1.377(15) . ? C88 H88 0.9500 . ? C89 C90 1.352(14) . ? C89 H89 0.9500 . ? C90 N6 1.348(12) . ? C90 H90 0.9500 . ? C91 C93 1.323(16) . ? C91 C92 1.382(17) . ? C91 H91 0.9500 . ? C92 N7 1.311(16) . ? C92 H92 0.9500 . ? N7 C94 1.291(14) . ? C94 C95 1.348(16) . ? C94 H94 0.9500 . ? C95 C93 1.351(16) . ? C95 H95 0.9500 . ? C93 H93 0.9500 . ? C96 C100 1.237(18) . ? C96 N8 1.367(17) . ? C96 H96 0.9500 . ? N8 C97 1.387(18) . ? C97 C98 1.373(18) . ? C97 H97 0.9500 . ? C98 C99 1.436(19) . ? C98 H98 0.9500 . ? C99 C100 1.37(2) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? N9 C101 1.261(17) . ? N9 C103 1.338(19) . ? C101 C102 1.33(2) . ? C101 H101 0.9500 . ? C102 C105 1.34(2) . ? C102 H102 0.9500 . ? C103 C104 1.32(2) . ? C103 H103 0.9500 . ? C104 C105 1.36(2) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.3900 . ? C106 N10 1.3900 . ? C106 H106 0.9500 . ? C107 C108 1.3900 . ? C107 H107 0.9500 . ? C108 C109 1.3900 . ? C108 H108 0.9500 . ? C109 C110 1.3900 . ? C109 H109 0.9500 . ? C110 N10 1.3900 . ? C110 H110 0.9500 . ? N1 Ni1 2.111(7) . ? N2 Ni1 2.091(8) . ? N3 Ni2 2.119(8) . ? N4 Ni2 2.125(8) . ? N5 Ni3 2.096(8) . ? N6 Ni3 2.105(8) . ? O1 Ni1 2.019(6) . ? O2 Ni1 2.018(6) . ? O3 Ni2 2.015(5) . ? O4 Ni2 2.030(6) . ? O5 Ni2 2.015(5) . ? O6 Ni2 1.997(6) . ? O7 Ni3 2.013(6) . ? O8 Ni3 2.033(6) . ? O9 Ni1 2.025(6) . ? O10 Ni1 2.012(6) . ? O11 Ni3 2.020(6) . ? O12 Ni3 2.043(6) . ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C2 108.4(8) . . ? C3 C4 C1 109.5(9) . . ? C2 C4 C1 109.7(8) . . ? C3 C4 C5 115.1(8) . . ? C2 C4 C5 108.3(8) . . ? C1 C4 C5 105.8(8) . . ? O1 C5 C6 124.8(8) . . ? O1 C5 C4 116.1(7) . . ? C6 C5 C4 119.1(8) . . ? C7 C6 C5 124.7(9) . . ? C7 C6 H6 117.6 . . ? C5 C6 H6 117.6 . . ? O2 C7 C6 126.3(8) . . ? O2 C7 C8 116.6(8) . . ? C6 C7 C8 117.1(8) . . ? C9 C8 C13 117.4(8) . . ? C9 C8 C7 125.9(8) . . ? C13 C8 C7 116.7(8) . . ? C8 C9 C10 122.9(9) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C9 C10 C11 120.0(9) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 117.7(8) . . ? C12 C11 C14 119.4(7) . . ? C10 C11 C14 123.0(8) . . ? C11 C12 C13 122.5(8) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C8 119.4(9) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? O3 C14 C15 126.2(8) . . ? O3 C14 C11 115.1(8) . . ? C15 C14 C11 118.6(8) . . ? C14 C15 C16 126.9(8) . . ? C14 C15 H15 116.6 . . ? C16 C15 H15 116.6 . . ? O4 C16 C15 123.1(8) . . ? O4 C16 C17 117.4(7) . . ? C15 C16 C17 119.5(8) . . ? C16 C17 C19 110.0(7) . . ? C16 C17 C18 111.4(7) . . ? C19 C17 C18 109.2(8) . . ? C16 C17 C20 109.5(7) . . ? C19 C17 C20 109.6(8) . . ? C18 C17 C20 107.1(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 C23 109.4(8) . . ? C21 C24 C22 108.9(8) . . ? C23 C24 C22 110.4(7) . . ? C21 C24 C25 106.8(7) . . ? C23 C24 C25 108.6(7) . . ? C22 C24 C25 112.6(7) . . ? O5 C25 C26 124.8(8) . . ? O5 C25 C24 111.9(7) . . ? C26 C25 C24 123.2(8) . . ? C25 C26 C27 129.5(9) . . ? C25 C26 H26 115.3 . . ? C27 C26 H26 115.3 . . ? O6 C27 C26 121.1(8) . . ? O6 C27 C28 115.6(7) . . ? C26 C27 C28 123.3(8) . . ? C33 C28 C29 118.0(8) . . ? C33 C28 C27 123.4(8) . . ? C29 C28 C27 118.5(8) . . ? C30 C29 C28 121.1(8) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 121.5(8) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C32 117.7(8) . . ? C30 C31 C34 119.3(8) . . ? C32 C31 C34 123.1(8) . . ? C33 C32 C31 119.8(8) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C28 C33 C32 121.9(8) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? O7 C34 C35 125.5(9) . . ? O7 C34 C31 116.3(8) . . ? C35 C34 C31 118.2(8) . . ? C36 C35 C34 125.8(9) . . ? C36 C35 H35 117.1 . . ? C34 C35 H35 117.1 . . ? O8 C36 C35 126.2(8) . . ? O8 C36 C37 113.2(8) . . ? C35 C36 C37 120.6(8) . . ? C40 C37 C39A 78.8(15) . . ? C40 C37 C38 110.0(18) . . ? C39A C37 C38 133.3(16) . . ? C40 C37 C40A 124.2(15) . . ? C39A C37 C40A 116.1(13) . . ? C40 C37 C36 114.5(12) . . ? C39A C37 C36 106.6(11) . . ? C38 C37 C36 110.0(13) . . ? C40A C37 C36 111.4(11) . . ? C40 C37 C39 108.3(16) . . ? C38 C37 C39 108.2(16) . . ? C36 C37 C39 105.5(11) . . ? C39A C37 C38A 107.3(14) . . ? C38 C37 C38A 86.3(15) . . ? C40A C37 C38A 105.3(12) . . ? C36 C37 C38A 110.0(10) . . ? C39 C37 C38A 133.9(14) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C37 C40A H40D 109.5 . . ? C37 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C37 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C44 C41 H41A 109.5 . . ? C44 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C44 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 H42A 109.5 . . ? C44 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C44 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C43 C44 C41 109.1(8) . . ? C43 C44 C42 109.7(8) . . ? C41 C44 C42 109.8(8) . . ? C43 C44 C45 108.1(8) . . ? C41 C44 C45 106.5(8) . . ? C42 C44 C45 113.6(8) . . ? O9 C45 C46 125.2(8) . . ? O9 C45 C44 115.0(8) . . ? C46 C45 C44 119.7(8) . . ? C47 C46 C45 123.7(9) . . ? C47 C46 H46 118.1 . . ? C45 C46 H46 118.1 . . ? O10 C47 C46 125.3(8) . . ? O10 C47 C48 114.2(7) . . ? C46 C47 C48 120.4(8) . . ? C53 C48 C49 118.3(8) . . ? C53 C48 C47 117.7(8) . . ? C49 C48 C47 124.0(8) . . ? C50 C49 C48 121.6(8) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C51 119.8(9) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 C50 119.7(9) . . ? C52 C51 C54 117.5(8) . . ? C50 C51 C54 122.8(8) . . ? C51 C52 C53 119.5(8) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C48 C53 C52 121.0(9) . . ? C48 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? O11 C54 C55 125.7(8) . . ? O11 C54 C51 113.6(8) . . ? C55 C54 C51 120.4(8) . . ? C54 C55 C56 127.8(8) . . ? C54 C55 H55 116.1 . . ? C56 C55 H55 116.1 . . ? O12 C56 C55 123.1(8) . . ? O12 C56 C57 114.9(8) . . ? C55 C56 C57 122.0(8) . . ? C58 C57 C60 111.2(11) . . ? C58 C57 C59 108.6(12) . . ? C60 C57 C59 108.5(11) . . ? C58A C57 C59A 111.8(10) . . ? C58A C57 C60A 111.2(9) . . ? C59A C57 C60A 110.7(9) . . ? C58 C57 C56 107.7(9) . . ? C58A C57 C56 110.2(17) . . ? C60 C57 C56 113.7(9) . . ? C59 C57 C56 107.0(9) . . ? C59A C57 C56 103.2(16) . . ? C60A C57 C56 109.6(17) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? C57 C60A H60D 109.5 . . ? C57 C60A H60E 109.5 . . ? H60D C60A H60E 109.5 . . ? C57 C60A H60F 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? C57 C59A H59D 109.5 . . ? C57 C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C57 C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C57 C58A H58D 109.5 . . ? C57 C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C57 C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? N1 C61 C62 123.9(10) . . ? N1 C61 H61 118.0 . . ? C62 C61 H61 118.0 . . ? C61 C62 C63 120.3(10) . . ? C61 C62 H62 119.8 . . ? C63 C62 H62 119.8 . . ? C64 C63 C62 115.6(11) . . ? C64 C63 H63 122.2 . . ? C62 C63 H63 122.2 . . ? C63 C64 C65 120.0(11) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? N1 C65 C64 124.6(10) . . ? N1 C65 H65 117.7 . . ? C64 C65 H65 117.7 . . ? N2 C66 C67 124.3(11) . . ? N2 C66 H66 117.8 . . ? C67 C66 H66 117.8 . . ? C66 C67 C68 117.9(12) . . ? C66 C67 H67 121.0 . . ? C68 C67 H67 121.0 . . ? C69 C68 C67 119.7(12) . . ? C69 C68 H68 120.2 . . ? C67 C68 H68 120.2 . . ? C68 C69 C70 118.9(11) . . ? C68 C69 H69 120.5 . . ? C70 C69 H69 120.5 . . ? N2 C70 C69 122.1(10) . . ? N2 C70 H70 119.0 . . ? C69 C70 H70 119.0 . . ? N3 C71 C72 123.3(10) . . ? N3 C71 H71 118.3 . . ? C72 C71 H71 118.3 . . ? C73 C72 C71 118.5(11) . . ? C73 C72 H72 120.7 . . ? C71 C72 H72 120.7 . . ? C72 C73 C74 118.8(11) . . ? C72 C73 H73 120.6 . . ? C74 C73 H73 120.6 . . ? C73 C74 C75 119.6(10) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? N3 C75 C74 122.1(10) . . ? N3 C75 H75 118.9 . . ? C74 C75 H75 118.9 . . ? C77 C76 N4 124.8(9) . . ? C77 C76 H76 117.6 . . ? N4 C76 H76 117.6 . . ? C76 C77 C78 118.2(10) . . ? C76 C77 H77 120.9 . . ? C78 C77 H77 120.9 . . ? C77 C78 C79 119.6(11) . . ? C77 C78 H78 120.2 . . ? C79 C78 H78 120.2 . . ? C80 C79 C78 118.7(10) . . ? C80 C79 H79 120.6 . . ? C78 C79 H79 120.6 . . ? N4 C80 C79 123.0(10) . . ? N4 C80 H80 118.5 . . ? C79 C80 H80 118.5 . . ? N5 C81 C82 125.4(11) . . ? N5 C81 H81 117.3 . . ? C82 C81 H81 117.3 . . ? C83 C82 C81 116.5(11) . . ? C83 C82 H82 121.8 . . ? C81 C82 H82 121.8 . . ? C82 C83 C84 122.2(11) . . ? C82 C83 H83 118.9 . . ? C84 C83 H83 118.9 . . ? C83 C84 C85 115.7(10) . . ? C83 C84 H84 122.2 . . ? C85 C84 H84 122.2 . . ? N5 C85 C84 124.9(10) . . ? N5 C85 H85 117.5 . . ? C84 C85 H85 117.5 . . ? N6 C86 C87 120.7(10) . . ? N6 C86 H86 119.6 . . ? C87 C86 H86 119.6 . . ? C88 C87 C86 119.8(11) . . ? C88 C87 H87 120.1 . . ? C86 C87 H87 120.1 . . ? C87 C88 C89 117.9(11) . . ? C87 C88 H88 121.0 . . ? C89 C88 H88 121.0 . . ? C90 C89 C88 120.2(11) . . ? C90 C89 H89 119.9 . . ? C88 C89 H89 119.9 . . ? N6 C90 C89 122.6(10) . . ? N6 C90 H90 118.7 . . ? C89 C90 H90 118.7 . . ? C93 C91 C92 116.9(12) . . ? C93 C91 H91 121.6 . . ? C92 C91 H91 121.6 . . ? N7 C92 C91 123.8(13) . . ? N7 C92 H92 118.1 . . ? C91 C92 H92 118.1 . . ? C94 N7 C92 116.3(12) . . ? N7 C94 C95 124.5(13) . . ? N7 C94 H94 117.7 . . ? C95 C94 H94 117.7 . . ? C94 C95 C93 117.6(14) . . ? C94 C95 H95 121.2 . . ? C93 C95 H95 121.2 . . ? C91 C93 C95 120.7(14) . . ? C91 C93 H93 119.6 . . ? C95 C93 H93 119.6 . . ? C100 C96 N8 126.7(16) . . ? C100 C96 H96 116.6 . . ? N8 C96 H96 116.6 . . ? C96 N8 C97 118.1(14) . . ? C98 C97 N8 119.1(14) . . ? C98 C97 H97 120.4 . . ? N8 C97 H97 120.4 . . ? C97 C98 C99 116.8(15) . . ? C97 C98 H98 121.6 . . ? C99 C98 H98 121.6 . . ? C100 C99 C98 121.4(15) . . ? C100 C99 H99 119.3 . . ? C98 C99 H99 119.3 . . ? C96 C100 C99 117.8(15) . . ? C96 C100 H100 121.1 . . ? C99 C100 H100 121.1 . . ? C101 N9 C103 117.7(15) . . ? N9 C101 C102 124.6(16) . . ? N9 C101 H101 117.7 . . ? C102 C101 H101 117.7 . . ? C101 C102 C105 117.4(16) . . ? C101 C102 H102 121.3 . . ? C105 C102 H102 121.3 . . ? C104 C103 N9 122.6(18) . . ? C104 C103 H103 118.7 . . ? N9 C103 H103 118.7 . . ? C103 C104 C105 117.4(19) . . ? C103 C104 H104 121.3 . . ? C105 C104 H104 121.3 . . ? C102 C105 C104 119.9(17) . . ? C102 C105 H105 120.1 . . ? C104 C105 H105 120.1 . . ? C107 C106 N10 120.0 . . ? C107 C106 H106 120.0 . . ? N10 C106 H106 120.0 . . ? C106 C107 C108 120.0 . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C107 C108 C109 120.0 . . ? C107 C108 H108 120.0 . . ? C109 C108 H108 120.0 . . ? C110 C109 C108 120.0 . . ? C110 C109 H109 120.0 . . ? C108 C109 H109 120.0 . . ? C109 C110 N10 120.0 . . ? C109 C110 H110 120.0 . . ? N10 C110 H110 120.0 . . ? C110 N10 C106 120.0 . . ? C65 N1 C61 115.4(9) . . ? C65 N1 Ni1 123.3(7) . . ? C61 N1 Ni1 121.1(7) . . ? C66 N2 C70 117.0(9) . . ? C66 N2 Ni1 121.2(7) . . ? C70 N2 Ni1 121.8(7) . . ? C75 N3 C71 117.6(9) . . ? C75 N3 Ni2 122.4(7) . . ? C71 N3 Ni2 120.0(7) . . ? C80 N4 C76 115.6(9) . . ? C80 N4 Ni2 121.8(7) . . ? C76 N4 Ni2 122.6(7) . . ? C81 N5 C85 115.4(9) . . ? C81 N5 Ni3 122.6(7) . . ? C85 N5 Ni3 122.0(7) . . ? C86 N6 C90 118.6(9) . . ? C86 N6 Ni3 119.9(8) . . ? C90 N6 Ni3 121.5(7) . . ? C5 O1 Ni1 126.7(5) . . ? C7 O2 Ni1 125.5(5) . . ? C14 O3 Ni2 123.0(5) . . ? C16 O4 Ni2 125.3(5) . . ? C25 O5 Ni2 124.3(5) . . ? C27 O6 Ni2 127.1(5) . . ? C34 O7 Ni3 125.3(6) . . ? C36 O8 Ni3 124.5(6) . . ? C45 O9 Ni1 124.8(5) . . ? C47 O10 Ni1 126.6(5) . . ? C54 O11 Ni3 123.2(6) . . ? C56 O12 Ni3 124.2(6) . . ? O10 Ni1 O2 89.9(2) . . ? O10 Ni1 O1 176.9(2) . . ? O2 Ni1 O1 90.4(2) . . ? O10 Ni1 O9 89.6(2) . . ? O2 Ni1 O9 177.8(3) . . ? O1 Ni1 O9 90.3(2) . . ? O10 Ni1 N2 88.1(3) . . ? O2 Ni1 N2 89.5(3) . . ? O1 Ni1 N2 88.8(3) . . ? O9 Ni1 N2 92.6(3) . . ? O10 Ni1 N1 92.6(3) . . ? O2 Ni1 N1 89.5(3) . . ? O1 Ni1 N1 90.5(3) . . ? O9 Ni1 N1 88.4(3) . . ? N2 Ni1 N1 178.8(3) . . ? O6 Ni2 O3 86.8(2) . . ? O6 Ni2 O5 91.3(2) . . ? O3 Ni2 O5 178.1(2) . . ? O6 Ni2 O4 177.0(2) . . ? O3 Ni2 O4 90.6(2) . . ? O5 Ni2 O4 91.3(2) . . ? O6 Ni2 N3 91.4(3) . . ? O3 Ni2 N3 93.0(2) . . ? O5 Ni2 N3 86.7(3) . . ? O4 Ni2 N3 90.4(3) . . ? O6 Ni2 N4 88.7(3) . . ? O3 Ni2 N4 89.8(3) . . ? O5 Ni2 N4 90.5(3) . . ? O4 Ni2 N4 89.7(3) . . ? N3 Ni2 N4 177.2(3) . . ? O7 Ni3 O11 87.9(2) . . ? O7 Ni3 O8 91.6(2) . . ? O11 Ni3 O8 179.4(2) . . ? O7 Ni3 O12 177.8(2) . . ? O11 Ni3 O12 90.2(2) . . ? O8 Ni3 O12 90.4(2) . . ? O7 Ni3 N5 90.8(3) . . ? O11 Ni3 N5 90.4(3) . . ? O8 Ni3 N5 89.8(3) . . ? O12 Ni3 N5 88.3(3) . . ? O7 Ni3 N6 90.0(3) . . ? O11 Ni3 N6 91.7(3) . . ? O8 Ni3 N6 88.2(3) . . ? O12 Ni3 N6 91.0(3) . . ? N5 Ni3 N6 177.9(3) . . ? 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 C3 C4 C5 O1 165.9(8) . . . . ? C2 C4 C5 O1 44.4(11) . . . . ? C1 C4 C5 O1 -73.1(10) . . . . ? C3 C4 C5 C6 -13.6(13) . . . . ? C2 C4 C5 C6 -135.0(9) . . . . ? C1 C4 C5 C6 107.5(10) . . . . ? O1 C5 C6 C7 -4.9(15) . . . . ? C4 C5 C6 C7 174.5(8) . . . . ? C5 C6 C7 O2 3.5(15) . . . . ? C5 C6 C7 C8 -173.7(8) . . . . ? O2 C7 C8 C9 -157.0(9) . . . . ? C6 C7 C8 C9 20.5(14) . . . . ? O2 C7 C8 C13 22.4(12) . . . . ? C6 C7 C8 C13 -160.1(8) . . . . ? C13 C8 C9 C10 2.4(16) . . . . ? C7 C8 C9 C10 -178.3(9) . . . . ? C8 C9 C10 C11 0.6(16) . . . . ? C9 C10 C11 C12 -4.0(14) . . . . ? C9 C10 C11 C14 175.6(9) . . . . ? C10 C11 C12 C13 4.6(15) . . . . ? C14 C11 C12 C13 -175.0(9) . . . . ? C11 C12 C13 C8 -1.6(15) . . . . ? C9 C8 C13 C12 -1.9(14) . . . . ? C7 C8 C13 C12 178.7(8) . . . . ? C12 C11 C14 O3 -25.9(12) . . . . ? C10 C11 C14 O3 154.5(9) . . . . ? C12 C11 C14 C15 150.1(9) . . . . ? C10 C11 C14 C15 -29.4(13) . . . . ? O3 C14 C15 C16 4.5(15) . . . . ? C11 C14 C15 C16 -171.1(8) . . . . ? C14 C15 C16 O4 -0.1(15) . . . . ? C14 C15 C16 C17 176.5(8) . . . . ? O4 C16 C17 C19 111.2(9) . . . . ? C15 C16 C17 C19 -65.6(10) . . . . ? O4 C16 C17 C18 -127.6(9) . . . . ? C15 C16 C17 C18 55.6(11) . . . . ? O4 C16 C17 C20 -9.3(11) . . . . ? C15 C16 C17 C20 173.9(8) . . . . ? C21 C24 C25 O5 64.3(10) . . . . ? C23 C24 C25 O5 -53.6(10) . . . . ? C22 C24 C25 O5 -176.3(8) . . . . ? C21 C24 C25 C26 -113.7(10) . . . . ? C23 C24 C25 C26 128.3(9) . . . . ? C22 C24 C25 C26 5.7(12) . . . . ? O5 C25 C26 C27 3.3(16) . . . . ? C24 C25 C26 C27 -178.9(9) . . . . ? C25 C26 C27 O6 -10.9(15) . . . . ? C25 C26 C27 C28 170.0(9) . . . . ? O6 C27 C28 C33 160.8(8) . . . . ? C26 C27 C28 C33 -20.0(14) . . . . ? O6 C27 C28 C29 -15.9(12) . . . . ? C26 C27 C28 C29 163.3(9) . . . . ? C33 C28 C29 C30 0.8(14) . . . . ? C27 C28 C29 C30 177.7(9) . . . . ? C28 C29 C30 C31 1.5(15) . . . . ? C29 C30 C31 C32 -3.2(14) . . . . ? C29 C30 C31 C34 176.0(9) . . . . ? C30 C31 C32 C33 2.5(13) . . . . ? C34 C31 C32 C33 -176.6(8) . . . . ? C29 C28 C33 C32 -1.4(14) . . . . ? C27 C28 C33 C32 -178.1(8) . . . . ? C31 C32 C33 C28 -0.3(14) . . . . ? C30 C31 C34 O7 35.6(13) . . . . ? C32 C31 C34 O7 -145.3(9) . . . . ? C30 C31 C34 C35 -143.5(9) . . . . ? C32 C31 C34 C35 35.6(13) . . . . ? O7 C34 C35 C36 -5.7(16) . . . . ? C31 C34 C35 C36 173.3(8) . . . . ? C34 C35 C36 O8 6.5(16) . . . . ? C34 C35 C36 C37 -176.9(9) . . . . ? O8 C36 C37 C40 -170.8(14) . . . . ? C35 C36 C37 C40 12.2(18) . . . . ? O8 C36 C37 C39A 104.2(13) . . . . ? C35 C36 C37 C39A -72.8(14) . . . . ? O8 C36 C37 C38 -46.3(16) . . . . ? C35 C36 C37 C38 136.7(15) . . . . ? O8 C36 C37 C40A -23.3(13) . . . . ? C35 C36 C37 C40A 159.6(11) . . . . ? O8 C36 C37 C39 70.2(13) . . . . ? C35 C36 C37 C39 -106.8(13) . . . . ? O8 C36 C37 C38A -139.7(11) . . . . ? C35 C36 C37 C38A 43.3(14) . . . . ? C43 C44 C45 O9 67.3(10) . . . . ? C41 C44 C45 O9 -49.9(11) . . . . ? C42 C44 C45 O9 -170.8(8) . . . . ? C43 C44 C45 C46 -108.5(10) . . . . ? C41 C44 C45 C46 134.4(9) . . . . ? C42 C44 C45 C46 13.5(12) . . . . ? O9 C45 C46 C47 1.7(15) . . . . ? C44 C45 C46 C47 177.0(8) . . . . ? C45 C46 C47 O10 9.4(15) . . . . ? C45 C46 C47 C48 -170.4(8) . . . . ? O10 C47 C48 C53 13.8(12) . . . . ? C46 C47 C48 C53 -166.4(9) . . . . ? O10 C47 C48 C49 -168.1(8) . . . . ? C46 C47 C48 C49 11.7(14) . . . . ? C53 C48 C49 C50 -0.9(14) . . . . ? C47 C48 C49 C50 -179.0(9) . . . . ? C48 C49 C50 C51 1.9(15) . . . . ? C49 C50 C51 C52 -3.8(14) . . . . ? C49 C50 C51 C54 175.9(9) . . . . ? C50 C51 C52 C53 4.5(14) . . . . ? C54 C51 C52 C53 -175.2(8) . . . . ? C49 C48 C53 C52 1.6(14) . . . . ? C47 C48 C53 C52 179.8(8) . . . . ? C51 C52 C53 C48 -3.5(14) . . . . ? C52 C51 C54 O11 -18.4(12) . . . . ? C50 C51 C54 O11 161.9(8) . . . . ? C52 C51 C54 C55 155.8(9) . . . . ? C50 C51 C54 C55 -23.9(14) . . . . ? O11 C54 C55 C56 -1.3(16) . . . . ? C51 C54 C55 C56 -174.9(9) . . . . ? C54 C55 C56 O12 2.2(16) . . . . ? C54 C55 C56 C57 -179.2(9) . . . . ? O12 C56 C57 C58 -64.8(12) . . . . ? C55 C56 C57 C58 116.5(12) . . . . ? O12 C56 C57 C58A -20.2(17) . . . . ? C55 C56 C57 C58A 161.1(16) . . . . ? O12 C56 C57 C60 171.6(10) . . . . ? C55 C56 C57 C60 -7.2(14) . . . . ? O12 C56 C57 C59 51.8(12) . . . . ? C55 C56 C57 C59 -126.9(12) . . . . ? O12 C56 C57 C59A 99.3(16) . . . . ? C55 C56 C57 C59A -79.5(17) . . . . ? O12 C56 C57 C60A -142.8(16) . . . . ? C55 C56 C57 C60A 38.4(18) . . . . ? N1 C61 C62 C63 -1.4(17) . . . . ? C61 C62 C63 C64 -2.0(16) . . . . ? C62 C63 C64 C65 4.2(17) . . . . ? C63 C64 C65 N1 -3.5(18) . . . . ? N2 C66 C67 C68 1.7(18) . . . . ? C66 C67 C68 C69 -1.6(18) . . . . ? C67 C68 C69 C70 2.2(19) . . . . ? C68 C69 C70 N2 -2.9(18) . . . . ? N3 C71 C72 C73 -1.3(14) . . . . ? C71 C72 C73 C74 0.6(14) . . . . ? C72 C73 C74 C75 0.8(14) . . . . ? C73 C74 C75 N3 -1.5(14) . . . . ? N4 C76 C77 C78 -0.6(15) . . . . ? C76 C77 C78 C79 -0.7(15) . . . . ? C77 C78 C79 C80 2.0(15) . . . . ? C78 C79 C80 N4 -2.1(15) . . . . ? N5 C81 C82 C83 -2.2(16) . . . . ? C81 C82 C83 C84 1.6(16) . . . . ? C82 C83 C84 C85 -0.5(15) . . . . ? C83 C84 C85 N5 -0.2(14) . . . . ? N6 C86 C87 C88 3.0(15) . . . . ? C86 C87 C88 C89 -2.3(15) . . . . ? C87 C88 C89 C90 1.3(15) . . . . ? C88 C89 C90 N6 -0.9(15) . . . . ? C93 C91 C92 N7 -3(2) . . . . ? C91 C92 N7 C94 1(2) . . . . ? C92 N7 C94 C95 3.2(19) . . . . ? N7 C94 C95 C93 -4(2) . . . . ? C92 C91 C93 C95 2.3(19) . . . . ? C94 C95 C93 C91 1(2) . . . . ? C100 C96 N8 C97 3(2) . . . . ? C96 N8 C97 C98 -2(2) . . . . ? N8 C97 C98 C99 2(2) . . . . ? C97 C98 C99 C100 -2(2) . . . . ? N8 C96 C100 C99 -3(3) . . . . ? C98 C99 C100 C96 3(2) . . . . ? C103 N9 C101 C102 1(3) . . . . ? N9 C101 C102 C105 1(3) . . . . ? C101 N9 C103 C104 -6(3) . . . . ? N9 C103 C104 C105 9(3) . . . . ? C101 C102 C105 C104 2(2) . . . . ? C103 C104 C105 C102 -7(3) . . . . ? N10 C106 C107 C108 0.0 . . . . ? C106 C107 C108 C109 0.0 . . . . ? C107 C108 C109 C110 0.0 . . . . ? C108 C109 C110 N10 0.0 . . . . ? C109 C110 N10 C106 0.0 . . . . ? C107 C106 N10 C110 0.0 . . . . ? C64 C65 N1 C61 0.1(15) . . . . ? C64 C65 N1 Ni1 174.4(8) . . . . ? C62 C61 N1 C65 2.4(14) . . . . ? C62 C61 N1 Ni1 -172.0(8) . . . . ? C67 C66 N2 C70 -2.3(16) . . . . ? C67 C66 N2 Ni1 179.6(8) . . . . ? C69 C70 N2 C66 2.8(16) . . . . ? C69 C70 N2 Ni1 -179.1(8) . . . . ? C74 C75 N3 C71 0.8(12) . . . . ? C74 C75 N3 Ni2 179.0(7) . . . . ? C72 C71 N3 C75 0.6(12) . . . . ? C72 C71 N3 Ni2 -177.6(7) . . . . ? C79 C80 N4 C76 0.9(13) . . . . ? C79 C80 N4 Ni2 -180.0(7) . . . . ? C77 C76 N4 C80 0.6(13) . . . . ? C77 C76 N4 Ni2 -178.6(7) . . . . ? C82 C81 N5 C85 1.5(14) . . . . ? C82 C81 N5 Ni3 -179.5(8) . . . . ? C84 C85 N5 C81 -0.3(13) . . . . ? C84 C85 N5 Ni3 -179.3(7) . . . . ? C87 C86 N6 C90 -2.5(13) . . . . ? C87 C86 N6 Ni3 177.6(7) . . . . ? C89 C90 N6 C86 1.5(14) . . . . ? C89 C90 N6 Ni3 -178.6(7) . . . . ? C6 C5 O1 Ni1 -5.2(13) . . . . ? C4 C5 O1 Ni1 175.4(5) . . . . ? C6 C7 O2 Ni1 7.6(13) . . . . ? C8 C7 O2 Ni1 -175.2(5) . . . . ? C15 C14 O3 Ni2 -20.1(12) . . . . ? C11 C14 O3 Ni2 155.6(6) . . . . ? C15 C16 O4 Ni2 12.6(12) . . . . ? C17 C16 O4 Ni2 -164.0(6) . . . . ? C26 C25 O5 Ni2 11.3(12) . . . . ? C24 C25 O5 Ni2 -166.7(5) . . . . ? C26 C27 O6 Ni2 2.3(12) . . . . ? C28 C27 O6 Ni2 -178.5(5) . . . . ? C35 C34 O7 Ni3 -4.7(13) . . . . ? C31 C34 O7 Ni3 176.2(5) . . . . ? C35 C36 O8 Ni3 3.3(13) . . . . ? C37 C36 O8 Ni3 -173.6(5) . . . . ? C46 C45 O9 Ni1 -21.6(12) . . . . ? C44 C45 O9 Ni1 162.9(6) . . . . ? C46 C47 O10 Ni1 1.8(13) . . . . ? C48 C47 O10 Ni1 -178.5(5) . . . . ? C55 C54 O11 Ni3 -16.7(12) . . . . ? C51 C54 O11 Ni3 157.2(6) . . . . ? C55 C56 O12 Ni3 15.2(12) . . . . ? C57 C56 O12 Ni3 -163.5(6) . . . . ? C47 O10 Ni1 O2 163.5(7) . . . . ? C47 O10 Ni1 O9 -14.4(7) . . . . ? C47 O10 Ni1 N2 -107.0(7) . . . . ? C47 O10 Ni1 N1 74.0(7) . . . . ? C7 O2 Ni1 O10 164.6(7) . . . . ? C7 O2 Ni1 O1 -12.3(7) . . . . ? C7 O2 Ni1 N2 76.5(7) . . . . ? C7 O2 Ni1 N1 -102.8(7) . . . . ? C5 O1 Ni1 O2 11.3(7) . . . . ? C5 O1 Ni1 O9 -170.8(7) . . . . ? C5 O1 Ni1 N2 -78.3(7) . . . . ? C5 O1 Ni1 N1 100.8(7) . . . . ? C45 O9 Ni1 O10 23.9(7) . . . . ? C45 O9 Ni1 O1 -159.2(7) . . . . ? C45 O9 Ni1 N2 112.0(7) . . . . ? C45 O9 Ni1 N1 -68.7(7) . . . . ? C66 N2 Ni1 O10 138.8(8) . . . . ? C70 N2 Ni1 O10 -39.2(8) . . . . ? C66 N2 Ni1 O2 -131.3(8) . . . . ? C70 N2 Ni1 O2 50.7(8) . . . . ? C66 N2 Ni1 O1 -41.0(8) . . . . ? C70 N2 Ni1 O1 141.0(8) . . . . ? C66 N2 Ni1 O9 49.2(8) . . . . ? C70 N2 Ni1 O9 -128.7(8) . . . . ? C65 N1 Ni1 O10 27.6(8) . . . . ? C61 N1 Ni1 O10 -158.4(7) . . . . ? C65 N1 Ni1 O2 -62.2(8) . . . . ? C61 N1 Ni1 O2 111.7(7) . . . . ? C65 N1 Ni1 O1 -152.6(8) . . . . ? C61 N1 Ni1 O1 21.4(7) . . . . ? C65 N1 Ni1 O9 117.1(8) . . . . ? C61 N1 Ni1 O9 -68.9(7) . . . . ? C27 O6 Ni2 O3 -172.4(7) . . . . ? C27 O6 Ni2 O5 7.3(7) . . . . ? C27 O6 Ni2 N3 -79.4(7) . . . . ? C27 O6 Ni2 N4 97.7(7) . . . . ? C14 O3 Ni2 O6 -155.1(7) . . . . ? C14 O3 Ni2 O4 23.3(7) . . . . ? C14 O3 Ni2 N3 113.7(7) . . . . ? C14 O3 Ni2 N4 -66.3(7) . . . . ? C25 O5 Ni2 O6 -13.9(7) . . . . ? C25 O5 Ni2 O4 167.7(7) . . . . ? C25 O5 Ni2 N3 77.4(7) . . . . ? C25 O5 Ni2 N4 -102.6(7) . . . . ? C16 O4 Ni2 O3 -20.2(7) . . . . ? C16 O4 Ni2 O5 160.1(7) . . . . ? C16 O4 Ni2 N3 -113.2(7) . . . . ? C16 O4 Ni2 N4 69.6(7) . . . . ? C75 N3 Ni2 O6 -32.3(6) . . . . ? C71 N3 Ni2 O6 145.8(6) . . . . ? C75 N3 Ni2 O3 54.6(6) . . . . ? C71 N3 Ni2 O3 -127.3(6) . . . . ? C75 N3 Ni2 O5 -123.5(6) . . . . ? C71 N3 Ni2 O5 54.6(6) . . . . ? C75 N3 Ni2 O4 145.2(6) . . . . ? C71 N3 Ni2 O4 -36.7(6) . . . . ? C80 N4 Ni2 O6 -141.4(7) . . . . ? C76 N4 Ni2 O6 37.7(7) . . . . ? C80 N4 Ni2 O3 131.7(7) . . . . ? C76 N4 Ni2 O3 -49.2(7) . . . . ? C80 N4 Ni2 O5 -50.2(7) . . . . ? C76 N4 Ni2 O5 128.9(7) . . . . ? C80 N4 Ni2 O4 41.2(7) . . . . ? C76 N4 Ni2 O4 -139.7(7) . . . . ? C34 O7 Ni3 O11 -169.8(7) . . . . ? C34 O7 Ni3 O8 10.0(7) . . . . ? C34 O7 Ni3 N5 99.9(7) . . . . ? C34 O7 Ni3 N6 -78.1(7) . . . . ? C54 O11 Ni3 O7 -155.0(7) . . . . ? C54 O11 Ni3 N5 -64.3(7) . . . . ? C54 O11 Ni3 N6 115.0(7) . . . . ? C36 O8 Ni3 O7 -9.3(7) . . . . ? C36 O8 Ni3 O12 171.6(7) . . . . ? C36 O8 Ni3 N5 -100.1(7) . . . . ? C36 O8 Ni3 N6 80.7(7) . . . . ? C56 O12 Ni3 O11 -23.6(7) . . . . ? C56 O12 Ni3 O8 156.5(7) . . . . ? C56 O12 Ni3 N5 66.7(7) . . . . ? C56 O12 Ni3 N6 -115.3(7) . . . . ? C81 N5 Ni3 O7 -135.0(7) . . . . ? C85 N5 Ni3 O7 43.9(7) . . . . ? C81 N5 Ni3 O11 137.2(7) . . . . ? C85 N5 Ni3 O11 -43.9(7) . . . . ? C81 N5 Ni3 O8 -43.4(7) . . . . ? C85 N5 Ni3 O8 135.5(7) . . . . ? C81 N5 Ni3 O12 47.0(7) . . . . ? C85 N5 Ni3 O12 -134.1(7) . . . . ? C86 N6 Ni3 O7 134.2(7) . . . . ? C90 N6 Ni3 O7 -45.8(7) . . . . ? C86 N6 Ni3 O11 -138.0(7) . . . . ? C90 N6 Ni3 O11 42.0(7) . . . . ? C86 N6 Ni3 O8 42.6(7) . . . . ? C90 N6 Ni3 O8 -137.4(7) . . . . ? C86 N6 Ni3 O12 -47.8(7) . . . . ? C90 N6 Ni3 O12 132.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.930 _refine_diff_density_min -1.526 _refine_diff_density_rms 0.120