####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cif5 _database_code_depnum_ccdc_archive 'CCDC 618416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H2mpeptea _chemical_melting_point ? _chemical_formula_moiety C27H25N9 _chemical_formula_sum 'C27 H25 N9' _chemical_formula_weight 475.56 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.578(3) _cell_length_b 25.708(5) _cell_length_c 10.673(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4823.1(16) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2708 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9795 _exptl_absorpt_correction_T_max 0.9835 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7380 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2708 _reflns_number_gt 2327 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0623P)^2^+3.2624P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 3(2) _refine_ls_number_reflns 2708 _refine_ls_number_parameters 164 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _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 N3 N -0.00513(9) 0.26729(6) 0.95458(17) 0.0317(4) Uani 1 1 d . . . N5 N 0.2500 0.2500 0.9339(2) 0.0296(5) Uani 1 2 d S . . N4 N 0.12538(9) 0.27688(7) 0.92287(16) 0.0345(4) Uani 1 1 d . . . N2 N -0.13653(9) 0.25474(6) 0.97946(18) 0.0357(4) Uani 1 1 d . . . H2A H -0.1794 0.2711 0.9895 0.043 Uiso 1 1 calc R . . C53 C 0.2500 0.2500 1.1914(3) 0.0363(6) Uani 1 2 d S . . H53A H 0.2500 0.2500 1.2795 0.044 Uiso 1 2 calc SR . . C35 C 0.05680(10) 0.29646(7) 0.97492(18) 0.0304(4) Uani 1 1 d . . . C33 C -0.01478(13) 0.36187(8) 1.0768(2) 0.0399(5) Uani 1 1 d . . . H33A H -0.0181 0.3941 1.1179 0.048 Uiso 1 1 calc R . . C52 C 0.18581(11) 0.26653(8) 1.12787(18) 0.0327(4) Uani 1 1 d . . . H52A H 0.1426 0.2785 1.1709 0.039 Uiso 1 1 calc R . . C32 C -0.07964(12) 0.33291(8) 1.0562(2) 0.0357(4) Uani 1 1 d . . . H32A H -0.1275 0.3451 1.0822 0.043 Uiso 1 1 calc R . . C51 C 0.18798(10) 0.26466(7) 0.99729(18) 0.0277(4) Uani 1 1 d . . . C15 C -0.14340(11) 0.20218(7) 0.9500(2) 0.0332(4) Uani 1 1 d . . . N1 N -0.21478(10) 0.18444(7) 0.96539(19) 0.0391(4) Uani 1 1 d . . . C31 C -0.07213(11) 0.28483(8) 0.99521(19) 0.0319(4) Uani 1 1 d . . . C14 C -0.08466(13) 0.17046(8) 0.9071(2) 0.0445(6) Uani 1 1 d . . . H14A H -0.0352 0.1837 0.8973 0.053 Uiso 1 1 calc R . . C34 C 0.05504(12) 0.34349(8) 1.0374(2) 0.0373(5) Uani 1 1 d . . . H34A H 0.0999 0.3624 1.0525 0.045 Uiso 1 1 calc R . . C13 C -0.10051(14) 0.11955(9) 0.8796(3) 0.0548(7) Uani 1 1 d . . . H13A H -0.0616 0.0974 0.8514 0.066 Uiso 1 1 calc R . . C12 C -0.17399(16) 0.10067(10) 0.8932(3) 0.0625(8) Uani 1 1 d . . . H12A H -0.1861 0.0659 0.8742 0.075 Uiso 1 1 calc R . . C11 C -0.22806(14) 0.13463(10) 0.9356(3) 0.0550(7) Uani 1 1 d . . . H11A H -0.2780 0.1222 0.9445 0.066 Uiso 1 1 calc R . . C4 C 0.12344(13) 0.25847(12) 0.7943(2) 0.0535(6) Uani 1 1 d . . . H4A H 0.1736 0.2463 0.7704 0.080 Uiso 1 1 calc R . . H4B H 0.1082 0.2867 0.7395 0.080 Uiso 1 1 calc R . . H4C H 0.0872 0.2302 0.7873 0.080 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 N3 0.0270(8) 0.0311(8) 0.0369(8) -0.0002(7) -0.0002(7) 0.0028(7) N5 0.0250(12) 0.0307(11) 0.0331(12) 0.000 0.000 -0.0024(9) N4 0.0258(9) 0.0430(9) 0.0347(9) -0.0077(8) -0.0020(7) 0.0046(7) N2 0.0235(8) 0.0345(9) 0.0491(10) -0.0029(8) 0.0011(8) 0.0037(7) C53 0.0400(16) 0.0389(15) 0.0298(13) 0.000 0.000 0.0039(12) C35 0.0264(9) 0.0318(10) 0.0330(10) 0.0014(8) -0.0029(8) 0.0006(7) C33 0.0417(12) 0.0314(10) 0.0467(13) -0.0077(9) -0.0022(10) 0.0055(9) C52 0.0310(10) 0.0321(10) 0.0350(11) -0.0025(8) 0.0034(8) 0.0026(8) C32 0.0272(9) 0.0372(10) 0.0425(11) -0.0026(9) 0.0002(9) 0.0096(8) C51 0.0236(9) 0.0234(8) 0.0361(10) -0.0004(8) -0.0004(7) -0.0040(7) C15 0.0285(10) 0.0339(10) 0.0373(10) 0.0019(8) -0.0044(8) 0.0005(8) N1 0.0280(9) 0.0351(9) 0.0541(11) -0.0007(8) 0.0022(8) 0.0001(7) C31 0.0280(10) 0.0340(10) 0.0338(10) 0.0031(8) -0.0040(8) 0.0003(7) C14 0.0319(11) 0.0358(11) 0.0658(16) -0.0023(11) -0.0004(10) 0.0018(9) C34 0.0323(11) 0.0343(11) 0.0454(13) -0.0031(9) -0.0027(9) -0.0005(8) C13 0.0404(14) 0.0380(12) 0.086(2) -0.0059(12) 0.0071(13) 0.0078(10) C12 0.0501(15) 0.0305(11) 0.107(2) -0.0115(13) 0.0058(15) -0.0021(11) C11 0.0374(12) 0.0384(12) 0.089(2) -0.0043(12) 0.0093(13) -0.0042(10) C4 0.0387(12) 0.0809(18) 0.0410(12) -0.0175(12) -0.0102(10) 0.0141(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C31 1.334(3) . ? N3 C35 1.340(2) . ? N5 C51 1.337(2) 14 ? N5 C51 1.337(2) . ? N4 C51 1.393(2) . ? N4 C35 1.420(2) . ? N4 C4 1.451(3) . ? N2 C31 1.381(2) . ? N2 C15 1.393(2) . ? N2 H2A 0.8700 . ? C53 C52 1.383(2) 14 ? C53 C52 1.383(2) . ? C53 H53A 0.9400 . ? C35 C34 1.381(3) . ? C33 C32 1.380(3) . ? C33 C34 1.381(3) . ? C33 H33A 0.9400 . ? C52 C51 1.395(3) . ? C52 H52A 0.9400 . ? C32 C31 1.403(3) . ? C32 H32A 0.9400 . ? C15 N1 1.345(3) . ? C15 C14 1.393(3) . ? N1 C11 1.340(3) . ? C14 C13 1.370(3) . ? C14 H14A 0.9400 . ? C34 H34A 0.9400 . ? C13 C12 1.388(4) . ? C13 H13A 0.9400 . ? C12 C11 1.368(4) . ? C12 H12A 0.9400 . ? C11 H11A 0.9400 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 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 C31 N3 C35 118.41(16) . . ? C51 N5 C51 119.2(2) 14 . ? C51 N4 C35 121.85(16) . . ? C51 N4 C4 118.93(17) . . ? C35 N4 C4 117.75(17) . . ? C31 N2 C15 129.93(17) . . ? C31 N2 H2A 115.0 . . ? C15 N2 H2A 115.0 . . ? C52 C53 C52 121.3(3) 14 . ? C52 C53 H53A 119.4 14 . ? C52 C53 H53A 119.4 . . ? N3 C35 C34 123.38(18) . . ? N3 C35 N4 115.35(16) . . ? C34 C35 N4 121.23(17) . . ? C32 C33 C34 120.1(2) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C53 C52 C51 117.2(2) . . ? C53 C52 H52A 121.4 . . ? C51 C52 H52A 121.4 . . ? C33 C32 C31 118.15(19) . . ? C33 C32 H32A 120.9 . . ? C31 C32 H32A 120.9 . . ? N5 C51 N4 114.79(17) . . ? N5 C51 C52 122.50(19) . . ? N4 C51 C52 122.70(17) . . ? N1 C15 N2 112.47(17) . . ? N1 C15 C14 122.22(19) . . ? N2 C15 C14 125.30(18) . . ? C11 N1 C15 117.23(18) . . ? N3 C31 N2 119.66(18) . . ? N3 C31 C32 122.12(18) . . ? N2 C31 C32 118.20(18) . . ? C13 C14 C15 118.6(2) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? C33 C34 C35 117.83(19) . . ? C33 C34 H34A 121.1 . . ? C35 C34 H34A 121.1 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C11 C12 C13 117.3(2) . . ? C11 C12 H12A 121.4 . . ? C13 C12 H12A 121.4 . . ? N1 C11 C12 124.6(2) . . ? N1 C11 H11A 117.7 . . ? C12 C11 H11A 117.7 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.234 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.041 data_cif7 _database_code_depnum_ccdc_archive 'CCDC 618417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(epeptea)2Cl2,4CH3OH,0.5H2O _chemical_melting_point ? _chemical_formula_moiety Ni3(C29H27N9)2Cl2,4CH3OH,0.5H2O _chemical_formula_sum 'C62 H70 Cl2 N18 Ni3 O4.50' _chemical_formula_weight 1386.39 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' Cl Cl 0.1484 0.1585 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.001(5) _cell_length_b 44.077(11) _cell_length_c 13.966(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.094(5) _cell_angle_gamma 90.00 _cell_volume 12799(5) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 17773 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 23.06 _exptl_crystal_description sheet _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5776 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8067 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50163 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 23.06 _reflns_number_total 17773 _reflns_number_gt 9840 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0583P)^2^+97.5218P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17773 _refine_ls_number_parameters 1631 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.20405(6) 0.42240(3) 0.81684(9) 0.0324(3) Uani 1 1 d . . . Ni2 Ni 0.17743(6) 0.37351(3) 0.75101(9) 0.0285(3) Uani 1 1 d . . . Ni3 Ni 0.15036(6) 0.32507(3) 0.68113(9) 0.0303(3) Uani 1 1 d . . . N1 N 0.2217(4) 0.43207(17) 0.6771(6) 0.038(2) Uani 1 1 d . . . N2 N 0.1592(4) 0.39047(16) 0.6260(6) 0.0327(19) Uani 1 1 d . . . N3 N 0.0992(4) 0.34855(16) 0.5725(5) 0.0321(19) Uani 1 1 d . . . N4 N 0.0378(4) 0.30452(18) 0.5247(6) 0.046(2) Uani 1 1 d . . . H4 H -0.0025 0.2992 0.5130 0.055 Uiso 1 1 calc R . . N5 N 0.1304(4) 0.28449(16) 0.6219(5) 0.0292(18) Uani 1 1 d . . . N6 N 0.2225(4) 0.26319(16) 0.7172(6) 0.034(2) Uani 1 1 d . . . H6 H 0.2534 0.2505 0.7105 0.041 Uiso 1 1 calc R . . N7 N 0.2066(4) 0.30830(16) 0.7999(5) 0.0306(19) Uani 1 1 d . . . N8 N 0.1950(4) 0.35482(16) 0.8742(5) 0.0292(18) Uani 1 1 d . . . N9 N 0.1820(4) 0.40171(17) 0.9433(6) 0.035(2) Uani 1 1 d . . . N10 N 0.2324(4) 0.33214(17) 0.6152(6) 0.036(2) Uani 1 1 d . . . N11 N 0.2640(4) 0.36842(16) 0.7332(6) 0.0322(19) Uani 1 1 d . . . N12 N 0.2945(4) 0.40591(16) 0.8470(6) 0.0320(19) Uani 1 1 d . . . N13 N 0.3220(4) 0.44421(18) 0.9619(6) 0.044(2) Uani 1 1 d . . . H13 H 0.3397 0.4459 1.0218 0.053 Uiso 1 1 calc R . . N14 N 0.2273(4) 0.46335(17) 0.8707(6) 0.036(2) Uani 1 1 d . . . N15 N 0.1319(4) 0.48444(18) 0.7818(7) 0.046(2) Uani 1 1 d . . . H15 H 0.1197 0.5007 0.7488 0.055 Uiso 1 1 calc R . . N16 N 0.1098(4) 0.43225(17) 0.7784(6) 0.036(2) Uani 1 1 d . . . N17 N 0.0921(3) 0.38018(16) 0.7698(5) 0.0290(18) Uani 1 1 d . . . N18 N 0.0723(4) 0.32865(17) 0.7575(5) 0.0328(19) Uani 1 1 d . . . C1 C 0.2633(5) 0.4540(2) 0.6564(8) 0.047(3) Uani 1 1 d . . . H1A H 0.2816 0.4666 0.7070 0.057 Uiso 1 1 calc R . . C2 C 0.2803(5) 0.4587(2) 0.5655(8) 0.050(3) Uani 1 1 d . . . H2A H 0.3086 0.4745 0.5555 0.060 Uiso 1 1 calc R . . C3 C 0.2559(5) 0.4406(2) 0.4905(8) 0.048(3) Uani 1 1 d . . . C4 C 0.2135(5) 0.4175(2) 0.5098(7) 0.042(3) Uani 1 1 d . . . H4A H 0.1968 0.4040 0.4604 0.051 Uiso 1 1 calc R . . C5 C 0.1962(5) 0.4144(2) 0.6024(7) 0.035(2) Uani 1 1 d . . . C6 C 0.2746(7) 0.4434(3) 0.3911(9) 0.077(4) Uani 1 1 d . . . H6A H 0.2365 0.4398 0.3433 0.093 Uiso 1 1 calc R . . H6B H 0.2892 0.4642 0.3822 0.093 Uiso 1 1 calc R . . C7 C 0.3241(9) 0.4228(4) 0.3733(12) 0.128(7) Uani 1 1 d . . . H7A H 0.3647 0.4291 0.4097 0.192 Uiso 1 1 calc R . . H7B H 0.3277 0.4227 0.3048 0.192 Uiso 1 1 calc R . . H7C H 0.3135 0.4025 0.3933 0.192 Uiso 1 1 calc R . . C8 C 0.1100(5) 0.3787(2) 0.5628(7) 0.035(2) Uani 1 1 d . . . C9 C 0.0701(5) 0.3954(2) 0.4952(8) 0.046(3) Uani 1 1 d . . . H9A H 0.0774 0.4163 0.4887 0.056 Uiso 1 1 calc R . . C10 C 0.0196(5) 0.3816(3) 0.4373(8) 0.053(3) Uani 1 1 d . . . H10A H -0.0076 0.3931 0.3919 0.063 Uiso 1 1 calc R . . C11 C 0.0097(5) 0.3517(2) 0.4461(8) 0.049(3) Uani 1 1 d . . . H11C H -0.0238 0.3419 0.4062 0.059 Uiso 1 1 calc R . . C12 C 0.0494(5) 0.3357(2) 0.5144(7) 0.037(3) Uani 1 1 d . . . C13 C 0.0805(5) 0.2809(2) 0.5505(8) 0.044(3) Uani 1 1 d . . . C14 C 0.0695(5) 0.2535(2) 0.5001(8) 0.056(3) Uani 1 1 d . . . H14A H 0.0333 0.2510 0.4528 0.067 Uiso 1 1 calc R . . C15 C 0.1126(6) 0.2305(2) 0.5217(8) 0.058(3) Uani 1 1 d . . . H15C H 0.1069 0.2122 0.4872 0.070 Uiso 1 1 calc R . . C16 C 0.1642(5) 0.2337(2) 0.5925(8) 0.050(3) Uani 1 1 d . . . H16A H 0.1941 0.2179 0.6069 0.060 Uiso 1 1 calc R . . C17 C 0.1710(5) 0.2613(2) 0.6432(7) 0.036(2) Uani 1 1 d . . . C18 C 0.2349(5) 0.2809(2) 0.7989(7) 0.034(2) Uani 1 1 d . . . C19 C 0.2758(5) 0.2699(2) 0.8768(8) 0.049(3) Uani 1 1 d . . . H19A H 0.2947 0.2506 0.8740 0.059 Uiso 1 1 calc R . . C20 C 0.2883(6) 0.2872(2) 0.9579(8) 0.049(3) Uani 1 1 d . . . H20A H 0.3152 0.2797 1.0122 0.059 Uiso 1 1 calc R . . C21 C 0.2622(5) 0.3154(2) 0.9608(7) 0.039(3) Uani 1 1 d . . . H21A H 0.2725 0.3276 1.0160 0.047 Uiso 1 1 calc R . . C22 C 0.2204(5) 0.3261(2) 0.8825(7) 0.035(2) Uani 1 1 d . . . C23 C 0.1812(5) 0.3711(2) 0.9544(7) 0.032(2) Uani 1 1 d . . . C24 C 0.1629(5) 0.3582(2) 1.0365(7) 0.042(3) Uani 1 1 d . . . H24A H 0.1623 0.3369 1.0420 0.051 Uiso 1 1 calc R . . C25 C 0.1457(6) 0.3755(3) 1.1096(8) 0.056(3) Uani 1 1 d . . . C26 C 0.1480(7) 0.4064(3) 1.0992(9) 0.069(4) Uani 1 1 d . . . H26A H 0.1382 0.4192 1.1491 0.083 Uiso 1 1 calc R . . C27 C 0.1647(6) 0.4188(2) 1.0149(8) 0.051(3) Uani 1 1 d . . . H27A H 0.1639 0.4400 1.0076 0.061 Uiso 1 1 calc R . . C28 C 0.1228(7) 0.3615(3) 1.1966(10) 0.082(4) Uani 1 1 d D . . H28A H 0.0844 0.3724 1.2104 0.098 Uiso 1 1 calc R . . H28B H 0.1105 0.3404 1.1819 0.098 Uiso 1 1 calc R . . C29 C 0.1719(10) 0.3622(5) 1.2839(13) 0.173(10) Uani 1 1 d D . . H29A H 0.2099 0.3513 1.2711 0.259 Uiso 1 1 calc R . . H29B H 0.1547 0.3527 1.3374 0.259 Uiso 1 1 calc R . . H29C H 0.1832 0.3831 1.3003 0.259 Uiso 1 1 calc R . . C30 C 0.2398(5) 0.3191(2) 0.5307(7) 0.036(2) Uani 1 1 d . . . H30A H 0.2074 0.3058 0.5027 0.044 Uiso 1 1 calc R . . C31 C 0.2913(5) 0.3238(2) 0.4828(7) 0.043(3) Uani 1 1 d . . . H31A H 0.2943 0.3138 0.4242 0.051 Uiso 1 1 calc R . . C32 C 0.3386(5) 0.3436(2) 0.5223(7) 0.044(3) Uani 1 1 d . . . C33 C 0.3320(4) 0.3585(2) 0.6073(7) 0.036(2) Uani 1 1 d . . . H33A H 0.3633 0.3725 0.6341 0.043 Uiso 1 1 calc R . . C34 C 0.2781(5) 0.3524(2) 0.6534(7) 0.031(2) Uani 1 1 d . . . C35 C 0.3971(6) 0.3494(3) 0.4692(9) 0.073(4) Uani 1 1 d . . . H35A H 0.3827 0.3593 0.4070 0.088 Uiso 1 1 calc R . . H35B H 0.4271 0.3632 0.5079 0.088 Uiso 1 1 calc R . . C36 C 0.4318(7) 0.3197(4) 0.4519(12) 0.115(7) Uani 1 1 d . . . H36A H 0.4523 0.3117 0.5132 0.172 Uiso 1 1 calc R . . H36B H 0.4642 0.3236 0.4102 0.172 Uiso 1 1 calc R . . H36C H 0.4009 0.3051 0.4212 0.172 Uiso 1 1 calc R . . C37 C 0.3113(5) 0.3798(2) 0.8024(7) 0.031(2) Uani 1 1 d . . . C38 C 0.3702(5) 0.3656(2) 0.8323(7) 0.038(3) Uani 1 1 d . . . H38A H 0.3810 0.3475 0.8030 0.045 Uiso 1 1 calc R . . C39 C 0.4120(5) 0.3784(3) 0.9051(7) 0.042(3) Uani 1 1 d . . . H39A H 0.4516 0.3689 0.9257 0.051 Uiso 1 1 calc R . . C40 C 0.3973(5) 0.4045(2) 0.9478(8) 0.044(3) Uani 1 1 d . . . H40A H 0.4264 0.4135 0.9969 0.052 Uiso 1 1 calc R . . C41 C 0.3377(5) 0.4176(2) 0.9168(7) 0.035(2) Uani 1 1 d . . . C42 C 0.2833(5) 0.4683(2) 0.9284(8) 0.043(3) Uani 1 1 d . . . C43 C 0.3041(5) 0.4972(2) 0.9573(8) 0.045(3) Uani 1 1 d . . . H43A H 0.3433 0.4998 0.9982 0.054 Uiso 1 1 calc R . . C44 C 0.2674(6) 0.5217(2) 0.9262(7) 0.049(3) Uani 1 1 d . . . H44A H 0.2816 0.5414 0.9446 0.058 Uiso 1 1 calc R . . C45 C 0.2091(6) 0.5176(2) 0.8672(8) 0.045(3) Uani 1 1 d . . . H45A H 0.1829 0.5343 0.8458 0.054 Uiso 1 1 calc R . . C46 C 0.1900(5) 0.4876(2) 0.8402(7) 0.044(3) Uani 1 1 d . . . C47 C 0.0889(5) 0.4604(2) 0.7652(8) 0.040(3) Uani 1 1 d . . . C48 C 0.0252(5) 0.4675(2) 0.7280(9) 0.051(3) Uani 1 1 d . . . H48A H 0.0124 0.4878 0.7172 0.062 Uiso 1 1 calc R . . C49 C -0.0172(5) 0.4449(3) 0.7081(9) 0.055(3) Uani 1 1 d . . . H49A H -0.0603 0.4492 0.6839 0.066 Uiso 1 1 calc R . . C50 C 0.0025(5) 0.4151(2) 0.7232(8) 0.047(3) Uani 1 1 d . . . H50A H -0.0269 0.3991 0.7091 0.056 Uiso 1 1 calc R . . C51 C 0.0666(4) 0.4090(2) 0.7596(7) 0.032(2) Uani 1 1 d . . . C52 C 0.0561(4) 0.3556(2) 0.7933(7) 0.031(2) Uani 1 1 d . . . C53 C 0.0093(5) 0.3575(2) 0.8555(7) 0.038(3) Uani 1 1 d . . . H53A H -0.0005 0.3765 0.8802 0.046 Uiso 1 1 calc R . . C54 C -0.0223(5) 0.3324(2) 0.8812(7) 0.037(3) Uani 1 1 d . . . C55 C -0.0076(5) 0.3049(2) 0.8399(7) 0.037(3) Uani 1 1 d . . . H55A H -0.0297 0.2871 0.8519 0.045 Uiso 1 1 calc R . . C56 C 0.0391(5) 0.30445(19) 0.7822(7) 0.035(2) Uani 1 1 d . . . H56A H 0.0491 0.2855 0.7572 0.042 Uiso 1 1 calc RD . . C57 C -0.0657(5) 0.3335(2) 0.9576(8) 0.049(3) Uani 1 1 d . . . H57A H -0.0862 0.3535 0.9560 0.059 Uiso 1 1 calc R . . H57B H -0.0997 0.3183 0.9426 0.059 Uiso 1 1 calc R . . C58 C -0.0323(8) 0.3279(4) 1.0543(11) 0.106(6) Uani 1 1 d . . . H58A H -0.0174 0.3071 1.0592 0.160 Uiso 1 1 calc R . . H58B H -0.0615 0.3315 1.1012 0.160 Uiso 1 1 calc R . . H58C H 0.0042 0.3415 1.0672 0.160 Uiso 1 1 calc R . . Ni4 Ni 0.67055(6) 0.39734(3) 0.58973(9) 0.0314(3) Uani 1 1 d . . . Ni5 Ni 0.67574(6) 0.37753(3) 0.75039(9) 0.0289(3) Uani 1 1 d . . . Ni6 Ni 0.68147(6) 0.35933(3) 0.91250(9) 0.0326(3) Uani 1 1 d . . . N19 N 0.7026(4) 0.43660(16) 0.6620(6) 0.0333(19) Uani 1 1 d . A . N20 N 0.6662(4) 0.41690(16) 0.7971(5) 0.0285(18) Uani 1 1 d . A . N21 N 0.6355(4) 0.39816(17) 0.9395(5) 0.0324(19) Uani 1 1 d . A . N22 N 0.6024(4) 0.3767(2) 1.0792(6) 0.051(2) Uani 1 1 d . A . H22 H 0.5671 0.3746 1.1044 0.062 Uiso 1 1 calc R . . N23 N 0.6876(4) 0.34364(18) 1.0483(6) 0.036(2) Uani 1 1 d . A . N24 N 0.7710(4) 0.30997(18) 1.0227(6) 0.041(2) Uani 1 1 d . A . H24 H 0.8075 0.3038 1.0541 0.050 Uiso 1 1 calc R . . N25 N 0.7271(4) 0.32284(17) 0.8631(6) 0.034(2) Uani 1 1 d . A . N26 N 0.6848(4) 0.33757(17) 0.7069(6) 0.035(2) Uani 1 1 d . A . N27 N 0.6432(4) 0.35314(17) 0.5517(6) 0.035(2) Uani 1 1 d . A . N28 N 0.5921(4) 0.34027(17) 0.8603(6) 0.0325(19) Uani 1 1 d . . . N29 N 0.5858(3) 0.37314(16) 0.7306(5) 0.0299(19) Uani 1 1 d . . . N30 N 0.5770(4) 0.40655(17) 0.6025(6) 0.034(2) Uani 1 1 d . . . N31 N 0.5691(4) 0.44130(19) 0.4712(6) 0.045(2) Uani 1 1 d . . . H31 H 0.5498 0.4582 0.4531 0.054 Uiso 1 1 calc R . . N32 N 0.6661(4) 0.41430(18) 0.4555(6) 0.035(2) Uani 1 1 d . . . N33 N 0.7589(4) 0.3869(2) 0.4284(6) 0.048(2) Uani 1 1 d . . . H33 H 0.7715 0.3770 0.3806 0.058 Uiso 1 1 calc R . . N34 N 0.7635(4) 0.38397(17) 0.5982(5) 0.0328(19) Uani 1 1 d . . . N35 N 0.7649(4) 0.38219(16) 0.7643(5) 0.0285(18) Uani 1 1 d . . . N36 N 0.7686(4) 0.38337(17) 0.9308(6) 0.0331(19) Uani 1 1 d . B . C59 C 0.7404(5) 0.4572(2) 0.6227(8) 0.047(3) Uani 1 1 d . . . H59A H 0.7456 0.4546 0.5574 0.056 Uiso 1 1 calc R . . C60 C 0.7705(6) 0.4806(3) 0.6695(8) 0.056(3) Uani 1 1 d . A . H60A H 0.7957 0.4936 0.6370 0.067 Uiso 1 1 calc R . . C61 C 0.7649(5) 0.4859(2) 0.7665(8) 0.046(3) Uani 1 1 d D . . C62 C 0.7253(5) 0.4648(2) 0.8124(7) 0.044(3) Uani 1 1 d D A . H62A H 0.7188 0.4673 0.8771 0.053 Uiso 1 1 calc R . . C63 C 0.6963(4) 0.43974(18) 0.7541(7) 0.032(2) Uani 1 1 d D . . C64 C 0.7989(6) 0.5105(3) 0.8274(9) 0.066(4) Uani 0.496(17) 1 d PD A 1 H64A H 0.8152 0.5255 0.7851 0.080 Uiso 0.496(17) 1 calc PR A 1 H64B H 0.7680 0.5208 0.8628 0.080 Uiso 0.496(17) 1 calc PR A 1 C65 C 0.8536(12) 0.4990(6) 0.898(2) 0.086(7) Uani 0.496(17) 1 d PD A 1 H65A H 0.8374 0.4851 0.9428 0.129 Uiso 0.496(17) 1 calc PR A 1 H65B H 0.8750 0.5159 0.9334 0.129 Uiso 0.496(17) 1 calc PR A 1 H65C H 0.8839 0.4884 0.8635 0.129 Uiso 0.496(17) 1 calc PR A 1 C64B C 0.7989(6) 0.5105(3) 0.8274(9) 0.066(4) Uani 0.504(17) 1 d P A 2 H64C H 0.7963 0.5063 0.8956 0.080 Uiso 0.504(17) 1 calc PR A 2 H64D H 0.7772 0.5299 0.8107 0.080 Uiso 0.504(17) 1 calc PR A 2 C65B C 0.8691(8) 0.5132(6) 0.813(2) 0.086(7) Uani 0.504(17) 1 d PD A 2 H65D H 0.8883 0.4931 0.8152 0.129 Uiso 0.504(17) 1 calc PR A 2 H65E H 0.8918 0.5255 0.8648 0.129 Uiso 0.504(17) 1 calc PR A 2 H65F H 0.8721 0.5226 0.7515 0.129 Uiso 0.504(17) 1 calc PR A 2 C66 C 0.6351(4) 0.4219(2) 0.8755(7) 0.032(2) Uani 1 1 d . . . C67 C 0.5997(5) 0.4483(2) 0.8891(7) 0.037(2) Uani 1 1 d . A . H67A H 0.5993 0.4647 0.8461 0.044 Uiso 1 1 calc R . . C68 C 0.5656(5) 0.4496(2) 0.9664(7) 0.041(3) Uani 1 1 d . . . H68A H 0.5410 0.4670 0.9754 0.049 Uiso 1 1 calc R A . C69 C 0.5672(5) 0.4260(2) 1.0303(8) 0.043(3) Uani 1 1 d . A . H69A H 0.5450 0.4272 1.0842 0.051 Uiso 1 1 calc R . . C70 C 0.6020(5) 0.4004(2) 1.0142(7) 0.037(2) Uani 1 1 d . . . C71 C 0.6506(5) 0.3554(2) 1.1109(8) 0.044(3) Uani 1 1 d . . . C72 C 0.6587(5) 0.3462(3) 1.2055(8) 0.064(4) Uani 1 1 d . A . H72A H 0.6333 0.3553 1.2479 0.076 Uiso 1 1 calc RD . . C73 C 0.7003(7) 0.3253(3) 1.2400(9) 0.074(4) Uani 1 1 d . . . H73A H 0.7035 0.3189 1.3047 0.089 Uiso 1 1 calc R A . C74 C 0.7397(6) 0.3129(3) 1.1771(8) 0.058(3) Uani 1 1 d . A . H74A H 0.7714 0.2984 1.1989 0.070 Uiso 1 1 calc R . . C75 C 0.7305(5) 0.3226(2) 1.0818(7) 0.042(3) Uani 1 1 d . . . C76 C 0.7657(5) 0.3051(2) 0.9235(7) 0.035(2) Uani 1 1 d . . . C77 C 0.8016(5) 0.2821(2) 0.8908(8) 0.045(3) Uani 1 1 d . A . H77A H 0.8279 0.2699 0.9354 0.054 Uiso 1 1 calc R . . C78 C 0.7991(5) 0.2770(2) 0.7939(8) 0.046(3) Uani 1 1 d . . . H78A H 0.8232 0.2612 0.7709 0.055 Uiso 1 1 calc R A . C79 C 0.7610(5) 0.2952(2) 0.7313(8) 0.042(3) Uani 1 1 d . A . H79A H 0.7597 0.2925 0.6643 0.050 Uiso 1 1 calc R . . C80 C 0.7237(5) 0.31773(19) 0.7661(7) 0.033(2) Uani 1 1 d . . . C81 C 0.6561(4) 0.3300(2) 0.6135(7) 0.032(2) Uani 1 1 d . . . C82 C 0.6392(5) 0.3003(2) 0.5841(8) 0.048(3) Uani 1 1 d . A . H82A H 0.6467 0.2841 0.6282 0.058 Uiso 1 1 calc R . . C83 C 0.6114(5) 0.2950(2) 0.4898(9) 0.049(3) Uani 1 1 d . . . C84 C 0.5976(5) 0.3189(3) 0.4294(8) 0.050(3) Uani 1 1 d . A . H84A H 0.5781 0.3158 0.3653 0.060 Uiso 1 1 calc R . . C85 C 0.6123(5) 0.3471(2) 0.4629(7) 0.041(3) Uani 1 1 d . . . H85A H 0.6001 0.3635 0.4214 0.049 Uiso 1 1 calc R A . C86 C 0.5978(7) 0.2628(3) 0.4543(10) 0.069(4) Uani 1 1 d . A . H86A H 0.5516 0.2605 0.4325 0.083 Uiso 1 1 calc R . . H86B H 0.6097 0.2486 0.5080 0.083 Uiso 1 1 calc R . . C87 C 0.6347(9) 0.2547(3) 0.3717(16) 0.147(9) Uani 1 1 d . . . H87A H 0.6246 0.2340 0.3510 0.221 Uiso 1 1 calc R A . H87B H 0.6805 0.2564 0.3934 0.221 Uiso 1 1 calc R . . H87C H 0.6225 0.2684 0.3180 0.221 Uiso 1 1 calc R . . C88 C 0.5667(5) 0.3168(2) 0.9070(8) 0.043(3) Uani 1 1 d . . . H88A H 0.5887 0.3102 0.9667 0.052 Uiso 1 1 calc R . . C89 C 0.5117(6) 0.3027(2) 0.8710(9) 0.053(3) Uani 1 1 d . . . H89A H 0.4954 0.2874 0.9080 0.064 Uiso 1 1 calc R . . C90 C 0.4783(5) 0.3099(2) 0.7807(9) 0.043(3) Uani 1 1 d . . . C91 C 0.5034(5) 0.3337(2) 0.7330(8) 0.038(3) Uani 1 1 d . . . H91A H 0.4833 0.3396 0.6715 0.046 Uiso 1 1 calc R . . C92 C 0.5591(5) 0.3490(2) 0.7762(7) 0.034(2) Uani 1 1 d . . . C93 C 0.4225(5) 0.2921(2) 0.7341(9) 0.058(3) Uani 1 1 d . . . H93A H 0.3963 0.3049 0.6864 0.070 Uiso 1 1 calc R . . H93B H 0.3958 0.2862 0.7832 0.070 Uiso 1 1 calc R . . C94 C 0.4427(9) 0.2641(4) 0.6849(18) 0.168(10) Uani 1 1 d . . . H94A H 0.4048 0.2532 0.6555 0.251 Uiso 1 1 calc R . . H94B H 0.4678 0.2512 0.7321 0.251 Uiso 1 1 calc R . . H94C H 0.4684 0.2699 0.6354 0.251 Uiso 1 1 calc R . . C95 C 0.5480(5) 0.3935(2) 0.6731(7) 0.030(2) Uani 1 1 d . . . C96 C 0.4865(5) 0.4013(2) 0.6888(7) 0.036(2) Uani 1 1 d . . . H96A H 0.4677 0.3923 0.7392 0.043 Uiso 1 1 calc R . . C97 C 0.4532(5) 0.4226(2) 0.6287(8) 0.049(3) Uani 1 1 d . . . H97A H 0.4117 0.4285 0.6387 0.059 Uiso 1 1 calc R . . C98 C 0.4803(5) 0.4351(2) 0.5551(8) 0.048(3) Uani 1 1 d . . . H98A H 0.4572 0.4489 0.5123 0.057 Uiso 1 1 calc R . . C99 C 0.5436(5) 0.4269(2) 0.5445(8) 0.039(3) Uani 1 1 d . . . C100 C 0.6196(5) 0.4344(2) 0.4201(7) 0.041(3) Uani 1 1 d . . . C101 C 0.6192(6) 0.4487(3) 0.3328(9) 0.062(4) Uani 1 1 d . . . H10B H 0.5875 0.4632 0.3118 0.075 Uiso 1 1 calc R . . C102 C 0.6650(7) 0.4417(3) 0.2773(8) 0.078(4) Uani 1 1 d . . . H10C H 0.6645 0.4510 0.2167 0.093 Uiso 1 1 calc R . . C103 C 0.7122(6) 0.4210(3) 0.3089(8) 0.063(4) Uani 1 1 d . . . H10D H 0.7441 0.4160 0.2706 0.076 Uiso 1 1 calc R . . C104 C 0.7117(5) 0.4077(2) 0.3999(7) 0.044(3) Uani 1 1 d . . . C105 C 0.7910(5) 0.3785(2) 0.5189(8) 0.044(3) Uani 1 1 d . . . C106 C 0.8513(6) 0.3658(3) 0.5245(9) 0.064(4) Uani 1 1 d . . . H10E H 0.8703 0.3633 0.4680 0.077 Uiso 1 1 calc R . . C107 C 0.8839(5) 0.3568(3) 0.6114(8) 0.054(3) Uani 1 1 d . . . H10F H 0.9238 0.3469 0.6147 0.064 Uiso 1 1 calc R . . C108 C 0.8572(5) 0.3623(2) 0.6942(7) 0.039(3) Uani 1 1 d . . . H10G H 0.8788 0.3566 0.7550 0.047 Uiso 1 1 calc R . . C109 C 0.7972(5) 0.3767(2) 0.6863(7) 0.032(2) Uani 1 1 d . . . C110 C 0.7986(5) 0.3908(2) 0.8544(7) 0.033(2) Uani 1 1 d . . . C111 C 0.8549(5) 0.4075(2) 0.8626(7) 0.039(3) Uani 1 1 d D B . H11D H 0.8736 0.4121 0.8072 0.047 Uiso 1 1 calc R . . C112 C 0.8850(5) 0.4177(2) 0.9571(6) 0.040(3) Uani 1 1 d D . . C113 C 0.8503(5) 0.4100(2) 1.0365(7) 0.044(3) Uani 1 1 d D B . H11E H 0.8659 0.4162 1.0999 0.052 Uiso 1 1 calc R . . C114 C 0.7951(5) 0.3937(2) 1.0179(7) 0.041(3) Uani 1 1 d . . . H11F H 0.7734 0.3893 1.0707 0.049 Uiso 1 1 calc R B . C115 C 0.9452(6) 0.4357(3) 0.9681(10) 0.075(4) Uani 0.553(18) 1 d PD B 1 H11A H 0.9523 0.4424 0.9035 0.090 Uiso 0.553(18) 1 calc PR B 1 H11B H 0.9807 0.4220 0.9920 0.090 Uiso 0.553(18) 1 calc PR B 1 C116 C 0.9499(14) 0.4628(6) 1.032(2) 0.118(9) Uani 0.553(18) 1 d PD B 1 H11G H 0.9247 0.4594 1.0844 0.177 Uiso 0.553(18) 1 calc PR B 1 H11H H 0.9336 0.4804 0.9953 0.177 Uiso 0.553(18) 1 calc PR B 1 H11I H 0.9945 0.4661 1.0592 0.177 Uiso 0.553(18) 1 calc PR B 1 C15B C 0.9452(6) 0.4357(3) 0.9681(10) 0.075(4) Uani 0.447(18) 1 d PD B 2 H15A H 0.9349 0.4570 0.9788 0.090 Uiso 0.447(18) 1 calc PR B 2 H15B H 0.9640 0.4345 0.9078 0.090 Uiso 0.447(18) 1 calc PR B 2 C16B C 0.9941(14) 0.4251(7) 1.050(2) 0.118(9) Uani 0.447(18) 1 d PD B 2 H16B H 1.0261 0.4408 1.0664 0.177 Uiso 0.447(18) 1 calc PR B 2 H16C H 1.0149 0.4068 1.0308 0.177 Uiso 0.447(18) 1 calc PR B 2 H16D H 0.9730 0.4207 1.1059 0.177 Uiso 0.447(18) 1 calc PR B 2 Cl1 Cl 0.31352(18) 0.20313(7) 0.7248(2) 0.0709(10) Uani 1 1 d . . . Cl2 Cl 0.43201(17) 0.46591(8) 1.1349(3) 0.0767(10) Uani 1 1 d . . . Cl3 Cl 0.0781(2) 0.55355(8) 0.7172(3) 0.0991(14) Uani 1 1 d . . . Cl4 Cl -0.07331(17) 0.28194(7) 0.3466(2) 0.0723(10) Uani 1 1 d . . . O1S O 0.8687(4) 0.27012(19) 1.1338(6) 0.072(3) Uani 1 1 d D . . H1S H 0.8906 0.2847 1.1574 0.108 Uiso 1 1 calc R . . C1S C 0.9096(9) 0.2469(4) 1.1105(12) 0.137(8) Uani 1 1 d D . . H1S1 H 0.9507 0.2484 1.1519 0.206 Uiso 1 1 calc R . . H1S2 H 0.9163 0.2489 1.0434 0.206 Uiso 1 1 calc R . . H1S3 H 0.8902 0.2273 1.1199 0.206 Uiso 1 1 calc R . . O2S O 0.8458(5) 0.3861(2) 0.2824(6) 0.084(3) Uani 1 1 d D . . H2S H 0.8654 0.4023 0.2782 0.126 Uiso 1 1 calc R . . C2S C 0.8777(6) 0.3630(3) 0.2425(9) 0.067(4) Uani 1 1 d D . . H2S1 H 0.9235 0.3671 0.2521 0.100 Uiso 1 1 calc R . . H2S2 H 0.8623 0.3616 0.1738 0.100 Uiso 1 1 calc R . . H2S3 H 0.8696 0.3439 0.2736 0.100 Uiso 1 1 calc R . . O3S O 0.4688(5) 0.4762(2) 0.3537(6) 0.088(3) Uani 1 1 d D . . H3S H 0.4504 0.4595 0.3474 0.132 Uiso 1 1 calc R . . C3S C 0.4253(7) 0.4981(3) 0.3699(10) 0.074(4) Uani 1 1 d D . . H3S1 H 0.4245 0.5001 0.4389 0.110 Uiso 1 1 calc R . . H3S2 H 0.3829 0.4924 0.3382 0.110 Uiso 1 1 calc R . . H3S3 H 0.4377 0.5173 0.3442 0.110 Uiso 1 1 calc R . . O4S O 0.5113(5) 0.3763(3) 1.2226(9) 0.134(5) Uani 1 1 d D . . H4S H 0.5336 0.3638 1.2569 0.201 Uiso 1 1 calc RD . . C4S C 0.4864(9) 0.3959(4) 1.2782(13) 0.126(7) Uani 1 1 d D . . H4S1 H 0.5202 0.4042 1.3254 0.189 Uiso 1 1 calc R . . H4S2 H 0.4549 0.3857 1.3115 0.189 Uiso 1 1 calc R . . H4S3 H 0.4657 0.4122 1.2387 0.189 Uiso 1 1 calc R . . O5S O 0.4599(6) 0.3185(3) 0.2033(9) 0.139(5) Uani 1 1 d D . . H5S H 0.4764 0.3039 0.2349 0.209 Uiso 1 1 calc R . . C5S C 0.4627(10) 0.3139(4) 0.1076(11) 0.140(8) Uani 1 1 d D . . H5S1 H 0.4525 0.3326 0.0723 0.210 Uiso 1 1 calc R . . H5S2 H 0.4320 0.2983 0.0831 0.210 Uiso 1 1 calc R . . H5S3 H 0.5057 0.3074 0.0992 0.210 Uiso 1 1 calc R . . O6S O 0.5669(5) 0.4967(3) 0.1525(8) 0.110(4) Uani 1 1 d D . . H6S H 0.5328 0.4874 0.1553 0.165 Uiso 1 1 calc R . . C6S C 0.5678(7) 0.5219(3) 0.2050(11) 0.092(5) Uani 1 1 d D . . H6S1 H 0.5432 0.5187 0.2580 0.138 Uiso 1 1 calc R . . H6S2 H 0.5490 0.5384 0.1647 0.138 Uiso 1 1 calc R . . H6S3 H 0.6119 0.5269 0.2307 0.138 Uiso 1 1 calc R . . O7S O 0.3442(16) 0.3635(4) 1.2203(17) 0.36(2) Uani 1 1 d D . . H7S H 0.3801 0.3556 1.2196 0.544 Uiso 1 1 calc R . . C7S C 0.3307(9) 0.3811(4) 1.1450(12) 0.117(6) Uani 1 1 d D . . H7S1 H 0.2845 0.3834 1.1299 0.176 Uiso 1 1 calc R . . H7S2 H 0.3475 0.3723 1.0901 0.176 Uiso 1 1 calc R . . H7S3 H 0.3502 0.4009 1.1591 0.176 Uiso 1 1 calc R . . O8S O 0.0579(10) 0.2186(3) 0.7552(13) 0.247(11) Uani 1 1 d D . . H8S H 0.0476 0.2367 0.7599 0.371 Uiso 1 1 calc RD . . C8S C 0.1146(12) 0.2133(5) 0.8143(19) 0.173(10) Uani 1 1 d D . . H8SB H 0.1487 0.2102 0.7752 0.259 Uiso 1 1 calc R . . H8SC H 0.1102 0.1953 0.8529 0.259 Uiso 1 1 calc R . . H8SD H 0.1250 0.2306 0.8566 0.259 Uiso 1 1 calc R . . O9S O 0.1387(12) 0.5390(6) 0.5270(18) 0.285(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0328(8) 0.0250(6) 0.0387(8) -0.0047(6) 0.0021(6) -0.0015(6) Ni2 0.0259(7) 0.0257(6) 0.0328(7) -0.0029(5) 0.0009(5) -0.0001(5) Ni3 0.0299(7) 0.0260(6) 0.0332(8) -0.0052(6) -0.0015(6) 0.0002(6) N1 0.044(5) 0.029(4) 0.043(6) -0.006(4) 0.004(4) -0.004(4) N2 0.032(5) 0.026(4) 0.038(5) -0.006(4) -0.005(4) -0.004(4) N3 0.033(5) 0.027(4) 0.035(5) -0.006(4) 0.000(4) 0.000(4) N4 0.031(5) 0.037(5) 0.064(6) -0.007(4) -0.011(4) 0.002(4) N5 0.028(5) 0.029(4) 0.029(5) -0.004(4) -0.003(4) 0.001(4) N6 0.034(5) 0.025(4) 0.041(5) -0.015(4) -0.006(4) 0.012(4) N7 0.034(5) 0.028(4) 0.029(5) -0.005(4) 0.001(4) -0.001(4) N8 0.031(5) 0.024(4) 0.032(5) -0.005(4) 0.000(4) -0.007(4) N9 0.036(5) 0.029(5) 0.040(5) -0.008(4) 0.007(4) 0.003(4) N10 0.040(5) 0.032(5) 0.036(5) -0.015(4) 0.005(4) 0.000(4) N11 0.024(5) 0.029(4) 0.042(5) -0.003(4) -0.001(4) -0.004(4) N12 0.032(5) 0.021(4) 0.042(5) -0.010(4) 0.002(4) -0.008(4) N13 0.045(6) 0.045(5) 0.038(5) -0.016(4) -0.014(4) -0.003(5) N14 0.034(5) 0.028(4) 0.046(6) -0.003(4) 0.004(4) -0.001(4) N15 0.046(6) 0.025(5) 0.064(7) 0.003(4) -0.001(5) 0.008(4) N16 0.034(5) 0.025(5) 0.048(6) -0.003(4) 0.004(4) 0.000(4) N17 0.027(5) 0.024(4) 0.034(5) -0.005(4) -0.001(4) -0.004(4) N18 0.031(5) 0.031(5) 0.033(5) -0.008(4) -0.006(4) -0.006(4) C1 0.037(7) 0.046(7) 0.059(8) -0.016(6) 0.007(6) -0.007(6) C2 0.056(8) 0.044(7) 0.052(8) 0.006(6) 0.013(6) -0.011(6) C3 0.051(7) 0.047(7) 0.049(8) 0.016(6) 0.019(6) 0.005(6) C4 0.043(7) 0.048(7) 0.034(6) 0.001(5) 0.002(5) 0.011(6) C5 0.034(6) 0.031(6) 0.040(7) 0.010(5) 0.004(5) 0.000(5) C6 0.081(11) 0.092(11) 0.066(10) 0.014(8) 0.033(8) -0.005(9) C7 0.140(18) 0.163(19) 0.092(14) 0.005(12) 0.053(13) -0.007(15) C8 0.031(6) 0.032(6) 0.044(7) -0.008(5) 0.006(5) -0.003(5) C9 0.042(7) 0.035(6) 0.057(8) 0.005(5) -0.015(6) 0.007(5) C10 0.047(7) 0.049(7) 0.054(8) 0.005(6) -0.024(6) 0.016(6) C11 0.044(7) 0.045(7) 0.052(7) 0.004(6) -0.020(6) 0.003(6) C12 0.043(7) 0.028(5) 0.038(6) -0.011(5) -0.001(5) 0.003(5) C13 0.029(6) 0.049(7) 0.052(7) -0.008(6) -0.002(6) 0.005(5) C14 0.052(8) 0.041(7) 0.063(8) -0.021(6) -0.033(6) -0.001(6) C15 0.077(9) 0.026(6) 0.060(8) -0.020(6) -0.029(7) 0.005(6) C16 0.054(8) 0.033(6) 0.060(8) -0.010(6) -0.005(6) 0.011(5) C17 0.039(6) 0.033(6) 0.035(6) -0.005(5) 0.004(5) 0.006(5) C18 0.042(6) 0.022(5) 0.039(7) 0.000(5) 0.008(5) 0.003(5) C19 0.060(8) 0.044(7) 0.040(7) -0.002(6) 0.000(6) 0.017(6) C20 0.070(8) 0.037(6) 0.036(7) 0.002(5) -0.004(6) 0.009(6) C21 0.047(7) 0.034(6) 0.034(6) -0.004(5) -0.002(5) 0.007(5) C22 0.032(6) 0.030(5) 0.042(7) 0.003(5) 0.008(5) 0.001(5) C23 0.037(6) 0.021(5) 0.036(6) -0.003(5) -0.003(5) -0.001(4) C24 0.054(7) 0.036(6) 0.039(7) -0.007(5) 0.015(6) -0.005(5) C25 0.079(9) 0.053(7) 0.042(7) -0.006(6) 0.024(7) -0.013(7) C26 0.100(11) 0.057(8) 0.058(9) -0.024(7) 0.035(8) -0.003(8) C27 0.069(8) 0.041(6) 0.046(7) -0.012(6) 0.016(6) 0.005(6) C28 0.099(12) 0.080(10) 0.071(10) -0.003(8) 0.031(9) -0.001(9) C29 0.18(2) 0.21(3) 0.123(19) 0.047(17) 0.013(17) -0.06(2) C30 0.029(6) 0.045(6) 0.033(6) -0.003(5) -0.006(5) 0.000(5) C31 0.047(7) 0.049(7) 0.031(6) -0.008(5) 0.002(5) 0.010(6) C32 0.046(7) 0.054(7) 0.033(6) -0.005(5) 0.011(5) 0.000(6) C33 0.024(6) 0.049(6) 0.033(6) -0.004(5) -0.004(5) -0.005(5) C34 0.032(6) 0.032(5) 0.027(6) 0.001(5) 0.000(5) 0.006(5) C35 0.059(9) 0.109(11) 0.056(9) -0.013(8) 0.026(7) -0.010(8) C36 0.049(9) 0.192(19) 0.105(13) -0.059(13) 0.020(9) 0.021(11) C37 0.030(6) 0.029(5) 0.036(6) 0.003(5) 0.006(5) -0.006(5) C38 0.029(6) 0.038(6) 0.047(7) -0.008(5) 0.009(5) 0.002(5) C39 0.019(6) 0.063(8) 0.042(7) 0.000(6) -0.004(5) 0.000(5) C40 0.030(6) 0.045(7) 0.052(7) 0.004(6) -0.010(5) -0.002(5) C41 0.043(7) 0.025(5) 0.039(6) -0.005(5) 0.010(5) -0.008(5) C42 0.049(7) 0.032(6) 0.048(7) -0.015(5) 0.003(6) -0.002(5) C43 0.058(8) 0.031(6) 0.043(7) -0.012(5) -0.005(6) -0.008(6) C44 0.076(9) 0.032(6) 0.036(7) -0.006(5) 0.004(6) -0.017(6) C45 0.065(8) 0.020(5) 0.049(7) -0.005(5) 0.011(6) 0.001(5) C46 0.045(7) 0.053(7) 0.035(7) -0.001(5) 0.004(6) 0.002(6) C47 0.039(7) 0.028(6) 0.053(7) -0.001(5) 0.009(5) 0.001(5) C48 0.041(7) 0.030(6) 0.084(9) 0.012(6) 0.011(6) 0.005(6) C49 0.024(6) 0.053(7) 0.086(10) 0.014(7) -0.003(6) -0.002(6) C50 0.036(7) 0.036(6) 0.067(8) 0.009(6) 0.005(6) -0.003(5) C51 0.020(5) 0.037(6) 0.040(6) 0.000(5) 0.005(5) 0.000(5) C52 0.028(6) 0.031(6) 0.031(6) 0.008(5) -0.005(5) 0.006(5) C53 0.034(6) 0.040(6) 0.043(7) 0.000(5) 0.010(5) 0.007(5) C54 0.029(6) 0.039(6) 0.045(7) 0.007(5) 0.010(5) 0.009(5) C55 0.038(6) 0.027(5) 0.047(7) 0.011(5) 0.009(5) -0.003(5) C56 0.042(7) 0.016(5) 0.043(7) -0.001(4) -0.009(5) -0.006(5) C57 0.045(7) 0.047(7) 0.062(8) 0.013(6) 0.025(6) 0.004(6) C58 0.091(12) 0.159(17) 0.075(12) 0.029(11) 0.035(10) 0.019(11) Ni4 0.0332(8) 0.0317(7) 0.0292(7) -0.0012(6) 0.0039(6) 0.0012(6) Ni5 0.0288(7) 0.0268(6) 0.0309(7) -0.0013(5) 0.0031(5) 0.0005(5) Ni6 0.0334(8) 0.0320(7) 0.0325(8) 0.0014(6) 0.0048(6) 0.0028(6) N19 0.038(5) 0.029(4) 0.034(5) 0.002(4) 0.007(4) 0.001(4) N20 0.029(5) 0.026(4) 0.032(5) -0.002(4) 0.008(4) -0.003(4) N21 0.036(5) 0.032(4) 0.028(5) 0.003(4) -0.001(4) -0.003(4) N22 0.050(6) 0.057(6) 0.052(6) 0.008(5) 0.027(5) 0.012(5) N23 0.036(5) 0.038(5) 0.035(5) 0.004(4) 0.008(4) 0.001(4) N24 0.040(5) 0.045(5) 0.038(6) 0.013(4) 0.001(4) 0.011(4) N25 0.037(5) 0.036(5) 0.031(5) 0.001(4) 0.010(4) -0.005(4) N26 0.029(5) 0.031(5) 0.045(6) 0.003(4) 0.005(4) 0.004(4) N27 0.034(5) 0.031(5) 0.038(5) 0.003(4) 0.000(4) 0.008(4) N28 0.023(5) 0.033(5) 0.042(5) 0.002(4) 0.008(4) 0.000(4) N29 0.020(4) 0.030(4) 0.040(5) -0.002(4) 0.003(4) -0.004(4) N30 0.038(5) 0.029(4) 0.031(5) 0.001(4) -0.005(4) 0.003(4) N31 0.060(6) 0.043(5) 0.033(5) 0.010(4) 0.010(5) 0.021(5) N32 0.038(5) 0.038(5) 0.030(5) -0.006(4) 0.005(4) -0.006(4) N33 0.052(6) 0.067(6) 0.025(5) -0.008(4) 0.003(4) 0.013(5) N34 0.038(5) 0.039(5) 0.022(5) -0.001(4) 0.006(4) -0.004(4) N35 0.036(5) 0.033(4) 0.016(4) 0.000(3) 0.003(4) 0.000(4) N36 0.036(5) 0.037(5) 0.025(5) 0.000(4) -0.002(4) 0.001(4) C59 0.063(8) 0.046(7) 0.033(6) -0.001(5) 0.015(6) -0.008(6) C60 0.068(9) 0.050(7) 0.052(8) -0.010(6) 0.015(7) -0.029(6) C61 0.048(7) 0.029(6) 0.061(8) -0.001(5) 0.003(6) -0.006(5) C62 0.044(7) 0.047(7) 0.042(7) -0.003(5) 0.009(5) -0.006(5) C63 0.030(6) 0.024(5) 0.040(7) 0.003(5) -0.002(5) 0.003(4) C64 0.088(10) 0.051(7) 0.061(9) -0.017(6) 0.016(8) -0.031(7) C65 0.087(16) 0.066(14) 0.100(19) -0.022(12) -0.011(15) -0.015(12) C64B 0.088(10) 0.051(7) 0.061(9) -0.017(6) 0.016(8) -0.031(7) C65B 0.087(16) 0.066(14) 0.100(19) -0.022(12) -0.011(15) -0.015(12) C66 0.025(6) 0.030(5) 0.039(6) -0.004(5) -0.007(5) -0.004(4) C67 0.046(7) 0.027(5) 0.034(6) -0.010(5) -0.003(5) 0.002(5) C68 0.036(6) 0.048(7) 0.036(6) -0.015(5) -0.006(5) 0.016(5) C69 0.037(6) 0.055(7) 0.037(7) 0.002(6) 0.007(5) 0.003(6) C70 0.034(6) 0.037(6) 0.041(7) 0.000(5) 0.010(5) 0.000(5) C71 0.049(7) 0.045(6) 0.037(7) 0.008(5) 0.007(6) 0.001(6) C72 0.088(10) 0.068(8) 0.040(8) 0.008(6) 0.027(7) 0.023(8) C73 0.106(12) 0.076(9) 0.049(8) 0.026(7) 0.035(8) 0.024(9) C74 0.067(9) 0.068(8) 0.044(8) 0.017(6) 0.022(7) 0.004(7) C75 0.048(7) 0.040(6) 0.039(7) 0.007(5) 0.011(6) 0.002(6) C76 0.038(6) 0.036(6) 0.029(6) 0.009(5) 0.000(5) 0.005(5) C77 0.050(7) 0.030(6) 0.051(8) 0.005(5) -0.005(6) 0.012(5) C78 0.046(7) 0.038(6) 0.053(8) 0.002(6) 0.002(6) 0.017(5) C79 0.049(7) 0.038(6) 0.037(6) 0.000(5) 0.002(5) 0.012(5) C80 0.033(6) 0.017(5) 0.048(7) -0.002(5) 0.007(5) 0.004(4) C81 0.031(6) 0.029(6) 0.035(6) -0.012(5) 0.000(5) -0.001(5) C82 0.057(8) 0.038(6) 0.049(8) 0.002(5) 0.006(6) 0.001(6) C83 0.048(7) 0.038(6) 0.059(8) -0.022(6) -0.005(6) -0.004(6) C84 0.047(7) 0.055(8) 0.044(7) -0.017(6) -0.001(6) -0.002(6) C85 0.041(7) 0.048(7) 0.031(6) -0.005(5) -0.001(5) 0.005(5) C86 0.083(10) 0.046(7) 0.077(10) -0.020(7) 0.001(8) -0.011(7) C87 0.154(18) 0.068(11) 0.24(2) -0.088(13) 0.096(17) -0.043(11) C88 0.040(7) 0.040(6) 0.050(7) 0.002(5) 0.005(6) -0.003(5) C89 0.048(8) 0.035(6) 0.079(10) 0.010(6) 0.018(7) 0.000(6) C90 0.045(7) 0.020(5) 0.065(8) 0.002(5) 0.006(6) -0.002(5) C91 0.032(6) 0.037(6) 0.045(7) -0.002(5) -0.001(5) 0.000(5) C92 0.042(7) 0.020(5) 0.041(7) 0.001(5) 0.010(5) 0.008(5) C93 0.048(7) 0.037(6) 0.084(10) -0.007(6) -0.008(7) -0.008(6) C94 0.114(16) 0.085(13) 0.29(3) -0.098(16) -0.008(17) -0.029(11) C95 0.030(6) 0.029(5) 0.031(6) 0.000(5) -0.001(5) 0.001(5) C96 0.030(6) 0.033(6) 0.043(7) 0.000(5) 0.001(5) -0.001(5) C97 0.037(7) 0.052(7) 0.058(8) 0.003(6) 0.004(6) 0.014(6) C98 0.050(7) 0.037(6) 0.054(8) 0.009(5) -0.001(6) 0.015(6) C99 0.040(7) 0.034(6) 0.045(7) -0.005(5) 0.010(5) 0.002(5) C100 0.050(7) 0.049(7) 0.023(6) 0.007(5) 0.001(5) -0.002(6) C101 0.054(8) 0.077(9) 0.060(9) 0.033(7) 0.020(7) 0.018(7) C102 0.095(11) 0.111(12) 0.030(7) 0.037(7) 0.019(7) 0.012(10) C103 0.065(9) 0.085(9) 0.042(8) 0.011(7) 0.019(7) 0.008(8) C104 0.048(7) 0.053(7) 0.031(6) 0.006(5) 0.006(5) 0.008(6) C105 0.034(7) 0.057(7) 0.040(7) -0.003(6) 0.005(5) 0.004(6) C106 0.046(8) 0.104(10) 0.045(8) -0.010(7) 0.013(6) 0.016(7) C107 0.031(6) 0.083(9) 0.047(8) 0.007(6) 0.007(6) 0.024(6) C108 0.029(6) 0.047(6) 0.039(7) -0.001(5) 0.000(5) 0.004(5) C109 0.029(6) 0.028(5) 0.039(6) 0.004(5) 0.002(5) -0.005(5) C110 0.038(6) 0.027(5) 0.035(6) 0.001(5) 0.005(5) 0.014(5) C111 0.042(7) 0.035(6) 0.042(7) 0.004(5) 0.007(5) -0.006(5) C112 0.038(6) 0.030(6) 0.048(7) -0.003(5) -0.005(5) -0.003(5) C113 0.054(8) 0.032(6) 0.041(7) -0.007(5) -0.005(6) -0.002(5) C114 0.046(7) 0.042(6) 0.034(7) -0.002(5) 0.007(5) -0.002(5) C115 0.066(9) 0.087(10) 0.067(9) -0.018(8) -0.004(7) -0.035(8) C116 0.10(2) 0.114(19) 0.15(2) -0.064(18) 0.044(17) -0.041(16) C15B 0.066(9) 0.087(10) 0.067(9) -0.018(8) -0.004(7) -0.035(8) C16B 0.10(2) 0.114(19) 0.15(2) -0.064(18) 0.044(17) -0.041(16) Cl1 0.106(3) 0.0572(19) 0.0469(19) 0.0002(15) 0.0019(18) 0.0319(19) Cl2 0.078(2) 0.075(2) 0.069(2) -0.0255(18) -0.0179(19) -0.0039(19) Cl3 0.129(4) 0.053(2) 0.104(3) -0.002(2) -0.026(3) 0.017(2) Cl4 0.080(2) 0.064(2) 0.064(2) -0.0066(17) -0.0213(18) -0.0179(18) O1S 0.070(6) 0.077(6) 0.065(6) 0.016(5) -0.003(5) 0.027(5) C1S 0.157(18) 0.158(18) 0.094(14) -0.012(12) 0.009(12) 0.102(15) O2S 0.097(7) 0.092(7) 0.073(7) -0.002(5) 0.047(6) 0.012(6) C2S 0.080(10) 0.067(8) 0.052(8) -0.002(7) 0.003(7) 0.006(8) O3S 0.106(8) 0.082(7) 0.073(7) 0.016(5) 0.000(6) 0.051(6) C3S 0.102(11) 0.047(8) 0.070(10) -0.006(7) 0.006(8) 0.002(8) O4S 0.131(11) 0.141(11) 0.151(11) -0.048(9) 0.098(9) -0.008(8) C4S 0.136(17) 0.114(15) 0.126(17) -0.026(13) 0.008(13) 0.001(13) O5S 0.140(11) 0.160(12) 0.126(11) -0.016(9) 0.045(9) -0.021(9) C5S 0.22(2) 0.132(16) 0.087(13) -0.031(12) 0.087(15) -0.052(15) O6S 0.100(9) 0.115(9) 0.117(9) -0.013(7) 0.022(7) 0.010(7) C6S 0.101(12) 0.080(10) 0.085(11) -0.032(9) -0.015(9) 0.028(9) O7S 0.63(5) 0.141(16) 0.25(2) 0.065(16) -0.17(3) -0.15(2) C7S 0.142(17) 0.111(14) 0.093(13) 0.018(11) -0.004(12) -0.038(13) O8S 0.20(2) 0.42(3) 0.133(16) -0.015(18) 0.041(14) -0.08(2) C8S 0.16(2) 0.16(2) 0.20(3) -0.021(19) 0.02(2) 0.008(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N14 1.989(8) . ? Ni1 N12 2.023(8) . ? Ni1 N16 2.023(8) . ? Ni1 N1 2.080(8) . ? Ni1 N9 2.097(8) . ? Ni1 Ni2 2.3785(17) . ? Ni2 N17 1.871(7) . ? Ni2 N11 1.883(7) . ? Ni2 N2 1.888(8) . ? Ni2 N8 1.897(7) . ? Ni2 Ni3 2.3825(17) . ? Ni3 N5 1.991(7) . ? Ni3 N3 2.017(8) . ? Ni3 N7 2.035(8) . ? Ni3 N18 2.083(8) . ? Ni3 N10 2.088(8) . ? N1 C5 1.352(12) . ? N1 C1 1.361(12) . ? N2 C8 1.365(12) . ? N2 C5 1.377(11) . ? N3 C12 1.355(12) . ? N3 C8 1.356(11) . ? N4 C13 1.389(12) . ? N4 C12 1.406(12) . ? N4 H4 0.8700 . ? N5 C17 1.338(11) . ? N5 C13 1.350(12) . ? N6 C18 1.377(12) . ? N6 C17 1.388(12) . ? N6 H6 0.8700 . ? N7 C18 1.346(11) . ? N7 C22 1.391(12) . ? N8 C22 1.372(11) . ? N8 C23 1.394(11) . ? N9 C27 1.341(12) . ? N9 C23 1.357(11) . ? N10 C30 1.340(12) . ? N10 C34 1.366(12) . ? N11 C37 1.379(12) . ? N11 C34 1.385(11) . ? N12 C41 1.336(12) . ? N12 C37 1.379(11) . ? N13 C42 1.377(13) . ? N13 C41 1.395(12) . ? N13 H13 0.8700 . ? N14 C42 1.348(13) . ? N14 C46 1.359(12) . ? N15 C46 1.376(13) . ? N15 C47 1.392(12) . ? N15 H15 0.8700 . ? N16 C47 1.320(12) . ? N16 C51 1.369(11) . ? N17 C51 1.378(11) . ? N17 C52 1.385(11) . ? N18 C56 1.347(11) . ? N18 C52 1.352(11) . ? C1 C2 1.382(14) . ? C1 H1A 0.9400 . ? C2 C3 1.359(15) . ? C2 H2A 0.9400 . ? C3 C4 1.404(14) . ? C3 C6 1.499(15) . ? C4 C5 1.398(13) . ? C4 H4A 0.9400 . ? C6 C7 1.43(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.384(14) . ? C9 C10 1.379(14) . ? C9 H9A 0.9400 . ? C10 C11 1.345(14) . ? C10 H10A 0.9400 . ? C11 C12 1.369(14) . ? C11 H11C 0.9400 . ? C13 C14 1.399(14) . ? C14 C15 1.365(14) . ? C14 H14A 0.9400 . ? C15 C16 1.367(14) . ? C15 H15C 0.9400 . ? C16 C17 1.404(13) . ? C16 H16A 0.9400 . ? C18 C19 1.378(14) . ? C19 C20 1.361(14) . ? C19 H19A 0.9400 . ? C20 C21 1.360(13) . ? C20 H20A 0.9400 . ? C21 C22 1.386(13) . ? C21 H21A 0.9400 . ? C23 C24 1.383(13) . ? C24 C25 1.364(14) . ? C24 H24A 0.9400 . ? C25 C26 1.373(15) . ? C25 C28 1.501(16) . ? C26 C27 1.387(15) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 C29 1.482(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C31 1.365(13) . ? C30 H30A 0.9400 . ? C31 C32 1.377(14) . ? C31 H31A 0.9400 . ? C32 C33 1.381(13) . ? C32 C35 1.544(14) . ? C33 C34 1.403(12) . ? C33 H33A 0.9400 . ? C35 C36 1.533(19) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C38 1.396(13) . ? C38 C39 1.368(13) . ? C38 H38A 0.9400 . ? C39 C40 1.348(14) . ? C39 H39A 0.9400 . ? C40 C41 1.392(14) . ? C40 H40A 0.9400 . ? C42 C43 1.388(13) . ? C43 C44 1.363(14) . ? C43 H43A 0.9400 . ? C44 C45 1.389(15) . ? C44 H44A 0.9400 . ? C45 C46 1.416(14) . ? C45 H45A 0.9400 . ? C47 C48 1.400(14) . ? C48 C49 1.338(14) . ? C48 H48A 0.9400 . ? C49 C50 1.383(14) . ? C49 H49A 0.9400 . ? C50 C51 1.396(13) . ? C50 H50A 0.9400 . ? C52 C53 1.403(13) . ? C53 C54 1.365(13) . ? C53 H53A 0.9400 . ? C54 C55 1.392(13) . ? C54 C57 1.498(13) . ? C55 C56 1.354(13) . ? C55 H55A 0.9400 . ? C56 H56A 0.9400 . ? C57 C58 1.452(17) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? Ni4 N32 2.009(8) . ? Ni4 N34 2.026(8) . ? Ni4 N30 2.039(8) . ? Ni4 N19 2.068(8) . ? Ni4 N27 2.079(8) . ? Ni4 Ni5 2.3959(18) . ? Ni5 N35 1.867(8) . ? Ni5 N20 1.874(7) . ? Ni5 N29 1.880(7) . ? Ni5 N26 1.882(8) . ? Ni5 Ni6 2.3889(18) . ? Ni6 N23 2.006(8) . ? Ni6 N21 2.027(8) . ? Ni6 N25 2.042(8) . ? Ni6 N28 2.091(8) . ? Ni6 N36 2.099(8) . ? N19 C63 1.319(11) . ? N19 C59 1.371(12) . ? N20 C66 1.370(11) . ? N20 C63 1.371(11) . ? N21 C70 1.341(12) . ? N21 C66 1.374(11) . ? N22 C70 1.385(12) . ? N22 C71 1.405(13) . ? N22 H22 0.8700 . ? N23 C75 1.331(12) . ? N23 C71 1.352(12) . ? N24 C75 1.383(12) . ? N24 C76 1.391(12) . ? N24 H24 0.8700 . ? N25 C76 1.338(12) . ? N25 C80 1.365(12) . ? N26 C80 1.388(12) . ? N26 C81 1.398(12) . ? N27 C81 1.338(12) . ? N27 C85 1.344(12) . ? N28 C92 1.334(12) . ? N28 C88 1.371(12) . ? N29 C95 1.379(11) . ? N29 C92 1.396(11) . ? N30 C99 1.340(12) . ? N30 C95 1.357(11) . ? N31 C99 1.375(12) . ? N31 C100 1.392(12) . ? N31 H31 0.8700 . ? N32 C104 1.347(12) . ? N32 C100 1.359(12) . ? N33 C104 1.368(13) . ? N33 C105 1.396(13) . ? N33 H33 0.8700 . ? N34 C105 1.342(12) . ? N34 C109 1.369(12) . ? N35 C109 1.382(11) . ? N35 C110 1.406(12) . ? N36 C114 1.344(12) . ? N36 C110 1.354(12) . ? C59 C60 1.331(14) . ? C59 H59A 0.9400 . ? C60 C61 1.396(14) . ? C60 H60A 0.9400 . ? C61 C62 1.452(8) . ? C61 C64 1.498(15) . ? C62 C63 1.456(8) . ? C62 H62A 0.9400 . ? C64 C65 1.493(10) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C65B H65D 0.9700 . ? C65B H65E 0.9700 . ? C65B H65F 0.9700 . ? C66 C67 1.408(13) . ? C67 C68 1.379(13) . ? C67 H67A 0.9400 . ? C68 C69 1.369(14) . ? C68 H68A 0.9400 . ? C69 C70 1.380(13) . ? C69 H69A 0.9400 . ? C71 C72 1.370(14) . ? C72 C73 1.314(15) . ? C72 H72A 0.9400 . ? C73 C74 1.400(15) . ? C73 H73A 0.9400 . ? C74 C75 1.387(14) . ? C74 H74A 0.9400 . ? C76 C77 1.378(13) . ? C77 C78 1.367(14) . ? C77 H77A 0.9400 . ? C78 C79 1.361(14) . ? C78 H78A 0.9400 . ? C79 C80 1.394(13) . ? C79 H79A 0.9400 . ? C81 C82 1.403(13) . ? C82 C83 1.384(14) . ? C82 H82A 0.9400 . ? C83 C84 1.355(15) . ? C83 C86 1.517(14) . ? C84 C85 1.349(14) . ? C84 H84A 0.9400 . ? C85 H85A 0.9400 . ? C86 C87 1.520(19) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C87 H87C 0.9700 . ? C88 C89 1.345(14) . ? C88 H88A 0.9400 . ? C89 C90 1.392(15) . ? C89 H89A 0.9400 . ? C90 C91 1.385(13) . ? C90 C93 1.482(14) . ? C91 C92 1.411(13) . ? C91 H91A 0.9400 . ? C93 C94 1.501(18) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C94 H94C 0.9700 . ? C95 C96 1.384(13) . ? C96 C97 1.381(14) . ? C96 H96A 0.9400 . ? C97 C98 1.359(14) . ? C97 H97A 0.9400 . ? C98 C99 1.403(14) . ? C98 H98A 0.9400 . ? C100 C101 1.371(14) . ? C101 C102 1.355(16) . ? C101 H10B 0.9400 . ? C102 C103 1.373(17) . ? C102 H10C 0.9400 . ? C103 C104 1.401(15) . ? C103 H10D 0.9400 . ? C105 C106 1.378(14) . ? C106 C107 1.366(15) . ? C106 H10E 0.9400 . ? C107 C108 1.376(14) . ? C107 H10F 0.9400 . ? C108 C109 1.400(13) . ? C108 H10G 0.9400 . ? C110 C111 1.381(13) . ? C111 C112 1.452(8) . ? C111 H11D 0.9400 . ? C112 C113 1.451(8) . ? C112 C115 1.481(14) . ? C113 C114 1.359(13) . ? C113 H11E 0.9400 . ? C114 H11F 0.9400 . ? C115 C116 1.489(10) . ? C115 H11A 0.9800 . ? C115 H11B 0.9800 . ? C116 H11G 0.9700 . ? C116 H11H 0.9700 . ? C116 H11I 0.9700 . ? C16B H16B 0.9700 . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? O1S C1S 1.405(12) . ? O1S H1S 0.8300 . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? O2S C2S 1.379(11) . ? O2S H2S 0.8300 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C2S H2S3 0.9700 . ? O3S C3S 1.369(11) . ? O3S H3S 0.8300 . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C3S H3S3 0.9700 . ? O4S C4S 1.318(13) . ? O4S H4S 0.8300 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? C4S H4S3 0.9700 . ? O5S C5S 1.362(13) . ? O5S H5S 0.8300 . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? C5S H5S3 0.9700 . ? O6S C6S 1.329(12) . ? O6S H6S 0.8300 . ? C6S H6S1 0.9700 . ? C6S H6S2 0.9700 . ? C6S H6S3 0.9700 . ? O7S C7S 1.308(15) . ? O7S H7S 0.8300 . ? C7S H7S1 0.9700 . ? C7S H7S2 0.9700 . ? C7S H7S3 0.9700 . ? O8S C8S 1.370(16) . ? O8S H8S 0.8300 . ? C8S H8SB 0.9700 . ? C8S H8SC 0.9700 . ? C8S H8SD 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 N14 Ni1 N12 94.3(3) . . ? N14 Ni1 N16 94.8(3) . . ? N12 Ni1 N16 170.9(3) . . ? N14 Ni1 N1 95.9(3) . . ? N12 Ni1 N1 89.0(3) . . ? N16 Ni1 N1 90.2(3) . . ? N14 Ni1 N9 98.5(3) . . ? N12 Ni1 N9 88.9(3) . . ? N16 Ni1 N9 89.6(3) . . ? N1 Ni1 N9 165.6(3) . . ? N14 Ni1 Ni2 179.2(2) . . ? N12 Ni1 Ni2 85.3(2) . . ? N16 Ni1 Ni2 85.6(2) . . ? N1 Ni1 Ni2 83.5(2) . . ? N9 Ni1 Ni2 82.2(2) . . ? N17 Ni2 N11 177.7(3) . . ? N17 Ni2 N2 89.7(3) . . ? N11 Ni2 N2 89.9(3) . . ? N17 Ni2 N8 90.5(3) . . ? N11 Ni2 N8 90.0(3) . . ? N2 Ni2 N8 177.6(3) . . ? N17 Ni2 Ni1 88.9(2) . . ? N11 Ni2 Ni1 88.9(2) . . ? N2 Ni2 Ni1 90.3(2) . . ? N8 Ni2 Ni1 92.2(2) . . ? N17 Ni2 Ni3 91.2(2) . . ? N11 Ni2 Ni3 91.1(2) . . ? N2 Ni2 Ni3 88.3(2) . . ? N8 Ni2 Ni3 89.3(2) . . ? Ni1 Ni2 Ni3 178.57(7) . . ? N5 Ni3 N3 95.1(3) . . ? N5 Ni3 N7 94.4(3) . . ? N3 Ni3 N7 170.4(3) . . ? N5 Ni3 N18 98.4(3) . . ? N3 Ni3 N18 88.4(3) . . ? N7 Ni3 N18 91.0(3) . . ? N5 Ni3 N10 95.1(3) . . ? N3 Ni3 N10 88.7(3) . . ? N7 Ni3 N10 89.7(3) . . ? N18 Ni3 N10 166.4(3) . . ? N5 Ni3 Ni2 178.3(2) . . ? N3 Ni3 Ni2 85.4(2) . . ? N7 Ni3 Ni2 85.1(2) . . ? N18 Ni3 Ni2 83.2(2) . . ? N10 Ni3 Ni2 83.3(2) . . ? C5 N1 C1 116.2(9) . . ? C5 N1 Ni1 120.2(6) . . ? C1 N1 Ni1 123.3(7) . . ? C8 N2 C5 122.5(8) . . ? C8 N2 Ni2 118.9(6) . . ? C5 N2 Ni2 118.5(6) . . ? C12 N3 C8 118.4(8) . . ? C12 N3 Ni3 121.4(6) . . ? C8 N3 Ni3 119.9(7) . . ? C13 N4 C12 130.2(9) . . ? C13 N4 H4 114.9 . . ? C12 N4 H4 114.9 . . ? C17 N5 C13 118.6(8) . . ? C17 N5 Ni3 120.3(6) . . ? C13 N5 Ni3 120.6(6) . . ? C18 N6 C17 133.4(8) . . ? C18 N6 H6 113.3 . . ? C17 N6 H6 113.3 . . ? C18 N7 C22 118.3(8) . . ? C18 N7 Ni3 121.5(6) . . ? C22 N7 Ni3 120.0(6) . . ? C22 N8 C23 122.0(8) . . ? C22 N8 Ni2 120.0(6) . . ? C23 N8 Ni2 117.9(6) . . ? C27 N9 C23 117.7(9) . . ? C27 N9 Ni1 119.9(7) . . ? C23 N9 Ni1 122.3(6) . . ? C30 N10 C34 117.5(8) . . ? C30 N10 Ni3 122.0(7) . . ? C34 N10 Ni3 120.3(6) . . ? C37 N11 C34 122.3(8) . . ? C37 N11 Ni2 118.6(6) . . ? C34 N11 Ni2 119.1(6) . . ? C41 N12 C37 117.4(8) . . ? C41 N12 Ni1 122.3(6) . . ? C37 N12 Ni1 119.9(6) . . ? C42 N13 C41 131.4(9) . . ? C42 N13 H13 114.3 . . ? C41 N13 H13 114.3 . . ? C42 N14 C46 118.5(9) . . ? C42 N14 Ni1 121.3(7) . . ? C46 N14 Ni1 119.8(7) . . ? C46 N15 C47 132.7(9) . . ? C46 N15 H15 113.6 . . ? C47 N15 H15 113.6 . . ? C47 N16 C51 118.5(8) . . ? C47 N16 Ni1 122.2(7) . . ? C51 N16 Ni1 119.2(6) . . ? C51 N17 C52 121.9(8) . . ? C51 N17 Ni2 119.7(6) . . ? C52 N17 Ni2 118.4(6) . . ? C56 N18 C52 115.8(8) . . ? C56 N18 Ni3 123.1(6) . . ? C52 N18 Ni3 120.9(6) . . ? N1 C1 C2 124.0(10) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C3 C2 C1 120.1(10) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 117.3(10) . . ? C2 C3 C6 123.1(11) . . ? C4 C3 C6 119.6(11) . . ? C5 C4 C3 120.2(10) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C5 N2 115.5(8) . . ? N1 C5 C4 122.2(9) . . ? N2 C5 C4 121.7(9) . . ? C7 C6 C3 113.6(12) . . ? C7 C6 H6A 108.8 . . ? C3 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? C3 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N2 115.5(9) . . ? N3 C8 C9 119.7(9) . . ? N2 C8 C9 124.7(9) . . ? C10 C9 C8 120.5(10) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 119.6(10) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 118.9(10) . . ? C10 C11 H11C 120.6 . . ? C12 C11 H11C 120.6 . . ? N3 C12 C11 122.9(9) . . ? N3 C12 N4 118.5(9) . . ? C11 C12 N4 118.5(9) . . ? N5 C13 N4 120.6(9) . . ? N5 C13 C14 122.0(9) . . ? N4 C13 C14 117.4(9) . . ? C15 C14 C13 118.1(10) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C14 C15 C16 121.1(10) . . ? C14 C15 H15C 119.5 . . ? C16 C15 H15C 119.5 . . ? C15 C16 C17 118.0(10) . . ? C15 C16 H16A 121.0 . . ? C17 C16 H16A 121.0 . . ? N5 C17 N6 121.6(8) . . ? N5 C17 C16 122.2(10) . . ? N6 C17 C16 116.2(9) . . ? N7 C18 N6 119.1(9) . . ? N7 C18 C19 122.4(9) . . ? N6 C18 C19 118.5(9) . . ? C20 C19 C18 119.0(10) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C21 C20 C19 120.4(10) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 120.1(10) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? N8 C22 C21 125.2(9) . . ? N8 C22 N7 114.7(8) . . ? C21 C22 N7 119.8(9) . . ? N9 C23 C24 120.9(9) . . ? N9 C23 N8 114.4(8) . . ? C24 C23 N8 124.5(8) . . ? C25 C24 C23 121.6(10) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C24 C25 C26 117.4(10) . . ? C24 C25 C28 121.7(11) . . ? C26 C25 C28 120.8(11) . . ? C25 C26 C27 119.8(10) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? N9 C27 C26 122.6(10) . . ? N9 C27 H27A 118.7 . . ? C26 C27 H27A 118.7 . . ? C29 C28 C25 113.1(14) . . ? C29 C28 H28A 109.0 . . ? C25 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 . . ? C25 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 C31 124.4(9) . . ? N10 C30 H30A 117.8 . . ? C31 C30 H30A 117.8 . . ? C30 C31 C32 118.5(9) . . ? C30 C31 H31A 120.8 . . ? C32 C31 H31A 120.8 . . ? C31 C32 C33 119.4(9) . . ? C31 C32 C35 119.5(10) . . ? C33 C32 C35 121.1(10) . . ? C32 C33 C34 119.3(9) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? N10 C34 N11 115.4(8) . . ? N10 C34 C33 120.9(8) . . ? N11 C34 C33 123.4(9) . . ? C36 C35 C32 111.2(11) . . ? C36 C35 H35A 109.4 . . ? C32 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C32 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N12 C37 N11 114.5(8) . . ? N12 C37 C38 120.8(9) . . ? N11 C37 C38 124.6(9) . . ? C39 C38 C37 119.0(9) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C40 C39 C38 121.2(10) . . ? C40 C39 H39A 119.4 . . ? C38 C39 H39A 119.4 . . ? C39 C40 C41 117.8(10) . . ? C39 C40 H40A 121.1 . . ? C41 C40 H40A 121.1 . . ? N12 C41 C40 123.8(9) . . ? N12 C41 N13 118.3(9) . . ? C40 C41 N13 117.9(9) . . ? N14 C42 N13 120.2(9) . . ? N14 C42 C43 122.3(10) . . ? N13 C42 C43 117.5(10) . . ? C44 C43 C42 119.7(11) . . ? C44 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C43 C44 C45 119.9(10) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C44 C45 C46 118.1(10) . . ? C44 C45 H45A 120.9 . . ? C46 C45 H45A 120.9 . . ? N14 C46 N15 121.9(9) . . ? N14 C46 C45 121.6(10) . . ? N15 C46 C45 116.6(10) . . ? N16 C47 N15 119.7(9) . . ? N16 C47 C48 122.9(9) . . ? N15 C47 C48 117.2(9) . . ? C49 C48 C47 118.9(10) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C48 C49 C50 119.9(10) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C49 C50 C51 119.3(10) . . ? C49 C50 H50A 120.3 . . ? C51 C50 H50A 120.3 . . ? N16 C51 N17 115.7(8) . . ? N16 C51 C50 120.3(9) . . ? N17 C51 C50 123.7(9) . . ? N18 C52 N17 115.2(8) . . ? N18 C52 C53 121.1(9) . . ? N17 C52 C53 123.6(9) . . ? C54 C53 C52 121.6(9) . . ? C54 C53 H53A 119.2 . . ? C52 C53 H53A 119.2 . . ? C53 C54 C55 116.9(9) . . ? C53 C54 C57 121.8(9) . . ? C55 C54 C57 121.0(9) . . ? C56 C55 C54 118.7(9) . . ? C56 C55 H55A 120.6 . . ? C54 C55 H55A 120.6 . . ? N18 C56 C55 125.9(9) . . ? N18 C56 H56A 117.1 . . ? C55 C56 H56A 117.1 . . ? C58 C57 C54 113.3(10) . . ? C58 C57 H57A 108.9 . . ? C54 C57 H57A 108.9 . . ? C58 C57 H57B 108.9 . . ? C54 C57 H57B 108.9 . . ? H57A C57 H57B 107.7 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N32 Ni4 N34 94.6(3) . . ? N32 Ni4 N30 95.1(3) . . ? N34 Ni4 N30 170.1(3) . . ? N32 Ni4 N19 96.5(3) . . ? N34 Ni4 N19 88.3(3) . . ? N30 Ni4 N19 92.4(3) . . ? N32 Ni4 N27 97.8(3) . . ? N34 Ni4 N27 88.4(3) . . ? N30 Ni4 N27 88.5(3) . . ? N19 Ni4 N27 165.5(3) . . ? N32 Ni4 Ni5 179.5(2) . . ? N34 Ni4 Ni5 85.6(2) . . ? N30 Ni4 Ni5 84.7(2) . . ? N19 Ni4 Ni5 83.0(2) . . ? N27 Ni4 Ni5 82.6(2) . . ? N35 Ni5 N20 91.0(3) . . ? N35 Ni5 N29 177.5(3) . . ? N20 Ni5 N29 89.5(3) . . ? N35 Ni5 N26 89.5(3) . . ? N20 Ni5 N26 178.4(3) . . ? N29 Ni5 N26 90.1(3) . . ? N35 Ni5 Ni6 91.3(2) . . ? N20 Ni5 Ni6 88.6(2) . . ? N29 Ni5 Ni6 91.2(2) . . ? N26 Ni5 Ni6 89.9(3) . . ? N35 Ni5 Ni4 88.3(2) . . ? N20 Ni5 Ni4 89.7(2) . . ? N29 Ni5 Ni4 89.3(2) . . ? N26 Ni5 Ni4 91.8(3) . . ? Ni6 Ni5 Ni4 178.23(7) . . ? N23 Ni6 N21 94.8(3) . . ? N23 Ni6 N25 94.5(3) . . ? N21 Ni6 N25 170.7(3) . . ? N23 Ni6 N28 97.2(3) . . ? N21 Ni6 N28 88.6(3) . . ? N25 Ni6 N28 90.4(3) . . ? N23 Ni6 N36 96.9(3) . . ? N21 Ni6 N36 88.9(3) . . ? N25 Ni6 N36 89.8(3) . . ? N28 Ni6 N36 165.8(3) . . ? N23 Ni6 Ni5 179.1(3) . . ? N21 Ni6 Ni5 86.0(2) . . ? N25 Ni6 Ni5 84.7(2) . . ? N28 Ni6 Ni5 83.2(2) . . ? N36 Ni6 Ni5 82.7(2) . . ? C63 N19 C59 117.7(8) . . ? C63 N19 Ni4 119.5(6) . . ? C59 N19 Ni4 121.7(6) . . ? C66 N20 C63 122.3(7) . . ? C66 N20 Ni5 120.8(6) . . ? C63 N20 Ni5 116.7(6) . . ? C70 N21 C66 119.5(8) . . ? C70 N21 Ni6 121.6(6) . . ? C66 N21 Ni6 118.7(6) . . ? C70 N22 C71 130.5(9) . . ? C70 N22 H22 114.8 . . ? C71 N22 H22 114.8 . . ? C75 N23 C71 117.6(9) . . ? C75 N23 Ni6 121.5(7) . . ? C71 N23 Ni6 120.9(7) . . ? C75 N24 C76 133.4(9) . . ? C75 N24 H24 113.3 . . ? C76 N24 H24 113.3 . . ? C76 N25 C80 118.2(8) . . ? C76 N25 Ni6 121.3(6) . . ? C80 N25 Ni6 120.3(6) . . ? C80 N26 C81 123.1(8) . . ? C80 N26 Ni5 118.4(6) . . ? C81 N26 Ni5 118.3(6) . . ? C81 N27 C85 118.1(8) . . ? C81 N27 Ni4 121.7(6) . . ? C85 N27 Ni4 120.2(7) . . ? C92 N28 C88 116.7(8) . . ? C92 N28 Ni6 121.3(6) . . ? C88 N28 Ni6 121.9(7) . . ? C95 N29 C92 121.7(8) . . ? C95 N29 Ni5 120.2(6) . . ? C92 N29 Ni5 118.1(6) . . ? C99 N30 C95 118.2(8) . . ? C99 N30 Ni4 120.6(7) . . ? C95 N30 Ni4 121.1(6) . . ? C99 N31 C100 133.3(8) . . ? C99 N31 H31 113.3 . . ? C100 N31 H31 113.3 . . ? C104 N32 C100 117.7(8) . . ? C104 N32 Ni4 120.9(7) . . ? C100 N32 Ni4 121.2(6) . . ? C104 N33 C105 132.8(9) . . ? C104 N33 H33 113.6 . . ? C105 N33 H33 113.6 . . ? C105 N34 C109 118.2(9) . . ? C105 N34 Ni4 121.8(7) . . ? C109 N34 Ni4 119.5(6) . . ? C109 N35 C110 120.8(8) . . ? C109 N35 Ni5 119.7(6) . . ? C110 N35 Ni5 119.6(6) . . ? C114 N36 C110 116.9(9) . . ? C114 N36 Ni6 121.6(7) . . ? C110 N36 Ni6 121.4(7) . . ? C60 C59 N19 125.3(10) . . ? C60 C59 H59A 117.4 . . ? N19 C59 H59A 117.4 . . ? C59 C60 C61 120.4(10) . . ? C59 C60 H60A 119.8 . . ? C61 C60 H60A 119.8 . . ? C60 C61 C62 117.0(9) . . ? C60 C61 C64 125.0(9) . . ? C62 C61 C64 118.0(9) . . ? C61 C62 C63 117.3(9) . . ? C61 C62 H62A 121.3 . . ? C63 C62 H62A 121.3 . . ? N19 C63 N20 117.8(7) . . ? N19 C63 C62 122.2(8) . . ? N20 C63 C62 119.8(8) . . ? C65 C64 C61 112.9(14) . . ? C65 C64 H64A 109.0 . . ? C61 C64 H64A 109.0 . . ? C65 C64 H64B 109.0 . . ? C61 C64 H64B 109.0 . . ? H64A C64 H64B 107.8 . . ? H65D C65B H65E 109.5 . . ? H65D C65B H65F 109.5 . . ? H65E C65B H65F 109.5 . . ? N20 C66 N21 116.0(8) . . ? N20 C66 C67 124.0(9) . . ? N21 C66 C67 119.7(9) . . ? C68 C67 C66 118.9(9) . . ? C68 C67 H67A 120.5 . . ? C66 C67 H67A 120.5 . . ? C69 C68 C67 120.7(9) . . ? C69 C68 H68A 119.7 . . ? C67 C68 H68A 119.7 . . ? C68 C69 C70 118.7(10) . . ? C68 C69 H69A 120.7 . . ? C70 C69 H69A 120.7 . . ? N21 C70 C69 122.4(9) . . ? N21 C70 N22 119.8(9) . . ? C69 C70 N22 117.7(9) . . ? N23 C71 C72 120.3(10) . . ? N23 C71 N22 120.4(9) . . ? C72 C71 N22 119.2(9) . . ? C73 C72 C71 123.2(10) . . ? C73 C72 H72A 118.4 . . ? C71 C72 H72A 118.4 . . ? C72 C73 C74 117.8(11) . . ? C72 C73 H73A 121.1 . . ? C74 C73 H73A 121.1 . . ? C75 C74 C73 117.8(11) . . ? C75 C74 H74A 121.1 . . ? C73 C74 H74A 121.1 . . ? N23 C75 N24 120.9(9) . . ? N23 C75 C74 123.3(10) . . ? N24 C75 C74 115.7(10) . . ? N25 C76 C77 122.2(9) . . ? N25 C76 N24 119.6(9) . . ? C77 C76 N24 118.3(9) . . ? C78 C77 C76 120.2(10) . . ? C78 C77 H77A 119.9 . . ? C76 C77 H77A 119.9 . . ? C79 C78 C77 118.4(10) . . ? C79 C78 H78A 120.8 . . ? C77 C78 H78A 120.8 . . ? C78 C79 C80 120.3(10) . . ? C78 C79 H79A 119.8 . . ? C80 C79 H79A 119.8 . . ? N25 C80 N26 115.5(8) . . ? N25 C80 C79 120.7(9) . . ? N26 C80 C79 123.6(9) . . ? N27 C81 N26 116.2(8) . . ? N27 C81 C82 120.2(9) . . ? N26 C81 C82 123.6(9) . . ? C83 C82 C81 119.5(10) . . ? C83 C82 H82A 120.2 . . ? C81 C82 H82A 120.2 . . ? C84 C83 C82 119.0(10) . . ? C84 C83 C86 120.6(11) . . ? C82 C83 C86 120.3(11) . . ? C85 C84 C83 118.8(11) . . ? C85 C84 H84A 120.6 . . ? C83 C84 H84A 120.6 . . ? N27 C85 C84 124.1(10) . . ? N27 C85 H85A 118.0 . . ? C84 C85 H85A 118.0 . . ? C83 C86 C87 112.1(11) . . ? C83 C86 H86A 109.2 . . ? C87 C86 H86A 109.2 . . ? C83 C86 H86B 109.2 . . ? C87 C86 H86B 109.2 . . ? H86A C86 H86B 107.9 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C89 C88 N28 122.9(11) . . ? C89 C88 H88A 118.6 . . ? N28 C88 H88A 118.6 . . ? C88 C89 C90 122.0(10) . . ? C88 C89 H89A 119.0 . . ? C90 C89 H89A 119.0 . . ? C91 C90 C89 115.6(10) . . ? C91 C90 C93 121.4(11) . . ? C89 C90 C93 122.9(10) . . ? C90 C91 C92 120.4(10) . . ? C90 C91 H91A 119.8 . . ? C92 C91 H91A 119.8 . . ? N28 C92 N29 115.4(9) . . ? N28 C92 C91 122.3(9) . . ? N29 C92 C91 122.2(9) . . ? C90 C93 C94 112.3(11) . . ? C90 C93 H93A 109.1 . . ? C94 C93 H93A 109.1 . . ? C90 C93 H93B 109.1 . . ? C94 C93 H93B 109.1 . . ? H93A C93 H93B 107.9 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? N30 C95 N29 114.7(8) . . ? N30 C95 C96 122.3(9) . . ? N29 C95 C96 122.9(9) . . ? C97 C96 C95 118.4(9) . . ? C97 C96 H96A 120.8 . . ? C95 C96 H96A 120.8 . . ? C98 C97 C96 120.4(10) . . ? C98 C97 H97A 119.8 . . ? C96 C97 H97A 119.8 . . ? C97 C98 C99 118.7(10) . . ? C97 C98 H98A 120.7 . . ? C99 C98 H98A 120.7 . . ? N30 C99 N31 122.2(9) . . ? N30 C99 C98 122.0(9) . . ? N31 C99 C98 115.8(10) . . ? N32 C100 C101 122.5(10) . . ? N32 C100 N31 121.0(8) . . ? C101 C100 N31 116.5(10) . . ? C102 C101 C100 119.3(11) . . ? C102 C101 H10B 120.4 . . ? C100 C101 H10B 120.4 . . ? C101 C102 C103 120.4(11) . . ? C101 C102 H10C 119.8 . . ? C103 C102 H10C 119.8 . . ? C102 C103 C104 118.2(11) . . ? C102 C103 H10D 120.9 . . ? C104 C103 H10D 120.9 . . ? N32 C104 N33 121.5(9) . . ? N32 C104 C103 121.9(10) . . ? N33 C104 C103 116.5(10) . . ? N34 C105 C106 121.7(10) . . ? N34 C105 N33 119.4(9) . . ? C106 C105 N33 118.8(10) . . ? C107 C106 C105 120.7(10) . . ? C107 C106 H10E 119.6 . . ? C105 C106 H10E 119.6 . . ? C106 C107 C108 118.8(10) . . ? C106 C107 H10F 120.6 . . ? C108 C107 H10F 120.6 . . ? C107 C108 C109 119.0(10) . . ? C107 C108 H10G 120.5 . . ? C109 C108 H10G 120.5 . . ? N34 C109 N35 114.8(8) . . ? N34 C109 C108 121.4(9) . . ? N35 C109 C108 123.5(9) . . ? N36 C110 C111 123.4(9) . . ? N36 C110 N35 114.1(9) . . ? C111 C110 N35 122.4(8) . . ? C110 C111 C112 120.0(9) . . ? C110 C111 H11D 120.0 . . ? C112 C111 H11D 120.0 . . ? C113 C112 C111 114.9(9) . . ? C113 C112 C115 124.0(9) . . ? C111 C112 C115 121.1(9) . . ? C114 C113 C112 119.0(9) . . ? C114 C113 H11E 120.5 . . ? C112 C113 H11E 120.5 . . ? N36 C114 C113 125.8(9) . . ? N36 C114 H11F 117.1 . . ? C113 C114 H11F 117.1 . . ? C112 C115 C116 118.3(15) . . ? C112 C115 H11A 107.7 . . ? C116 C115 H11A 107.7 . . ? C112 C115 H11B 107.7 . . ? C116 C115 H11B 107.7 . . ? H11A C115 H11B 107.1 . . ? H16B C16B H16C 109.5 . . ? H16B C16B H16D 109.5 . . ? H16C C16B H16D 109.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C3S O3S H3S 109.5 . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C4S O4S H4S 109.5 . . ? O4S C4S H4S1 109.5 . . ? O4S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? O4S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C5S O5S H5S 109.5 . . ? O5S C5S H5S1 109.5 . . ? O5S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? O5S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? C6S O6S H6S 109.5 . . ? O6S C6S H6S1 109.5 . . ? O6S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? O6S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C7S O7S H7S 109.5 . . ? O7S C7S H7S1 109.5 . . ? O7S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? O7S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C8S O8S H8S 109.5 . . ? O8S C8S H8SB 109.5 . . ? O8S C8S H8SC 109.5 . . ? H8SB C8S H8SC 109.5 . . ? O8S C8S H8SD 109.5 . . ? H8SB C8S H8SD 109.5 . . ? H8SC C8S H8SD 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.314 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.114 data_cif10 _database_code_depnum_ccdc_archive 'CCDC 618418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(epeptea)2(BPh4)2,3CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety Ni3(C29H27N9)2(BPh4)2,3CH2Cl2 _chemical_formula_sum 'C109 H100 B2 Cl6 N18 Ni3' _chemical_formula_weight 2072.52 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.186(4) _cell_length_b 15.723(3) _cell_length_c 28.092(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.041(3) _cell_angle_gamma 90.00 _cell_volume 10084(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 17735 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7958 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51917 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.1167 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17735 _reflns_number_gt 9880 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0930P)^2^+35.5885P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17735 _refine_ls_number_parameters 1309 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2625 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.21574(4) -0.12965(7) 0.53960(3) 0.0384(3) Uani 1 1 d . . . Ni2 Ni 0.24923(4) -0.05177(7) 0.47698(3) 0.0363(3) Uani 1 1 d . A . Ni3 Ni 0.28307(4) 0.02842(7) 0.41520(3) 0.0378(3) Uani 1 1 d . . . N1 N 0.3036(2) -0.1262(4) 0.57231(18) 0.0395(15) Uani 1 1 d . A . N2 N 0.3147(2) -0.0130(4) 0.52203(17) 0.0358(15) Uani 1 1 d . . . N3 N 0.3245(2) 0.1009(5) 0.47108(18) 0.0407(16) Uani 1 1 d . A . N4 N 0.3280(3) 0.2154(4) 0.41724(19) 0.0510(18) Uani 1 1 d . A . H4 H 0.3202 0.2695 0.4157 0.061 Uiso 1 1 calc R . . N5 N 0.3110(2) 0.0971(4) 0.36369(18) 0.0352(14) Uani 1 1 d . A . N6 N 0.2944(3) -0.0201(5) 0.30925(19) 0.0483(17) Uani 1 1 d . A . H6 H 0.3140 -0.0461 0.2899 0.058 Uiso 1 1 calc R . . N7 N 0.2362(2) -0.0537(4) 0.36817(18) 0.0437(17) Uani 1 1 d . A . N8 N 0.1847(2) -0.0871(5) 0.43009(18) 0.0453(17) Uani 1 1 d . . . N11 N 0.2053(3) 0.0418(5) 0.49178(19) 0.0472(17) Uani 1 1 d . . . N12 N 0.2029(3) -0.0129(5) 0.56768(19) 0.0440(16) Uani 1 1 d . A . N13 N 0.2065(3) -0.0753(5) 0.64549(19) 0.0501(18) Uani 1 1 d . A . H13 H 0.2235 -0.0649 0.6750 0.060 Uiso 1 1 calc R . . N14 N 0.1885(2) -0.1964(5) 0.59339(19) 0.0404(16) Uani 1 1 d . A . N15 N 0.1707(3) -0.3176(5) 0.5433(2) 0.057(2) Uani 1 1 d . A . H15 H 0.1427 -0.3550 0.5372 0.069 Uiso 1 1 calc R . . N16 N 0.2319(2) -0.2344(4) 0.50196(18) 0.0430(16) Uani 1 1 d . A . N17 N 0.2912(2) -0.1482(4) 0.46309(18) 0.0415(16) Uani 1 1 d . . . N18 N 0.3497(2) -0.0650(4) 0.42348(19) 0.0425(16) Uani 1 1 d . A . C11 C 0.3264(3) -0.1841(6) 0.6059(2) 0.048(2) Uani 1 1 d . . . H11 H 0.3023 -0.2290 0.6127 0.057 Uiso 1 1 calc R A . C12 C 0.3833(3) -0.1808(7) 0.6307(3) 0.061(3) Uani 1 1 d . A . H12 H 0.3970 -0.2216 0.6545 0.074 Uiso 1 1 calc R . . C13 C 0.4200(3) -0.1162(6) 0.6199(3) 0.062(3) Uani 1 1 d D . . C14 C 0.3972(3) -0.0582(6) 0.5849(3) 0.058(2) Uani 1 1 d . A . H14 H 0.4209 -0.0138 0.5770 0.069 Uiso 1 1 calc R . . C15 C 0.3384(3) -0.0645(5) 0.5607(2) 0.0389(18) Uani 1 1 d . A . C16 C 0.4827(3) -0.1113(9) 0.6444(4) 0.111(5) Uani 1 1 d D A . H16C H 0.5037 -0.1603 0.6342 0.133 Uiso 1 1 calc R . . H16D H 0.5001 -0.0599 0.6333 0.133 Uiso 1 1 calc R . . C17 C 0.4916(6) -0.1100(15) 0.6982(4) 0.201(10) Uani 1 1 d D . . H17A H 0.5313 -0.0917 0.7109 0.302 Uiso 1 1 calc R A . H17B H 0.4854 -0.1666 0.7101 0.302 Uiso 1 1 calc R . . H17C H 0.4640 -0.0708 0.7086 0.302 Uiso 1 1 calc R . . C31 C 0.3320(3) 0.0687(6) 0.5177(2) 0.0405(19) Uani 1 1 d . A . C32 C 0.3508(3) 0.1225(6) 0.5571(2) 0.051(2) Uani 1 1 d . . . H32 H 0.3548 0.1017 0.5889 0.062 Uiso 1 1 calc R A . C33 C 0.3634(4) 0.2057(6) 0.5488(2) 0.055(2) Uani 1 1 d . A . H33 H 0.3758 0.2419 0.5753 0.066 Uiso 1 1 calc R . . C34 C 0.3583(4) 0.2382(6) 0.5019(2) 0.055(2) Uani 1 1 d . . . H34 H 0.3679 0.2948 0.4958 0.066 Uiso 1 1 calc R A . C35 C 0.3379(3) 0.1810(6) 0.4646(2) 0.045(2) Uani 1 1 d . A . C51 C 0.3288(3) 0.1761(5) 0.3719(2) 0.0377(18) Uani 1 1 d . . . C52 C 0.3470(3) 0.2282(6) 0.3368(2) 0.048(2) Uani 1 1 d . A . H52 H 0.3579 0.2852 0.3434 0.058 Uiso 1 1 calc R . . C53 C 0.3482(4) 0.1923(6) 0.2917(3) 0.052(2) Uani 1 1 d . . . H53 H 0.3609 0.2245 0.2673 0.062 Uiso 1 1 calc R A . C54 C 0.3308(3) 0.1102(6) 0.2832(2) 0.049(2) Uani 1 1 d . A . H54 H 0.3319 0.0851 0.2530 0.059 Uiso 1 1 calc R . . C55 C 0.3118(3) 0.0643(5) 0.3189(2) 0.0368(18) Uani 1 1 d . . . C71 C 0.2515(3) -0.0710(5) 0.3247(2) 0.045(2) Uani 1 1 d . . . C72 C 0.2266(4) -0.1360(6) 0.2948(2) 0.056(2) Uani 1 1 d . A . H72 H 0.2379 -0.1455 0.2647 0.068 Uiso 1 1 calc R . . C73 C 0.1843(4) -0.1873(6) 0.3106(3) 0.064(3) Uani 1 1 d . . . H73 H 0.1671 -0.2325 0.2913 0.076 Uiso 1 1 calc R A . C74 C 0.1675(4) -0.1710(6) 0.3553(2) 0.056(2) Uani 1 1 d . A . H74 H 0.1386 -0.2042 0.3661 0.067 Uiso 1 1 calc R . . C75 C 0.1946(3) -0.1042(6) 0.3836(2) 0.046(2) Uani 1 1 d . A . N9 N 0.13474(15) -0.1186(5) 0.49234(13) 0.0502(18) Uani 0.31(3) 1 d PGD A 1 C91 C 0.1324(9) -0.0787(19) 0.4479(5) 0.035(3) Uani 0.31(3) 1 d PGD A 1 C92 C 0.0794(12) -0.073(2) 0.4161(7) 0.077(5) Uani 0.31(3) 1 d PGD A 1 H92 H 0.0778 -0.0457 0.3860 0.092 Uiso 0.31(3) 1 calc PR A 1 C93 C 0.0288(8) -0.106(2) 0.4288(10) 0.124(6) Uani 0.31(3) 1 d PGD A 1 C94 C 0.0312(4) -0.146(3) 0.4733(11) 0.064(6) Uani 0.31(3) 1 d PGD A 1 H94 H -0.0031 -0.1691 0.4819 0.076 Uiso 0.31(3) 1 calc PR A 1 C95 C 0.0841(6) -0.152(2) 0.5050(7) 0.045(4) Uani 0.31(3) 1 d PGD A 1 H95 H 0.0857 -0.1793 0.5351 0.054 Uiso 0.31(3) 1 calc PR A 1 C96 C -0.032(2) -0.103(5) 0.398(3) 0.32(2) Uani 0.31(3) 1 d PD A 1 H96A H -0.0613 -0.0981 0.4190 0.383 Uiso 0.31(3) 1 calc PR A 1 H96B H -0.0391 -0.1557 0.3793 0.383 Uiso 0.31(3) 1 calc PR A 1 C97 C -0.034(5) -0.027(8) 0.365(2) 0.27(2) Uani 0.31(3) 1 d PD A 1 H97A H -0.0743 -0.0165 0.3498 0.402 Uiso 0.31(3) 1 calc PR A 1 H97B H -0.0105 -0.0379 0.3402 0.402 Uiso 0.31(3) 1 calc PR A 1 H97C H -0.0188 0.0228 0.3835 0.402 Uiso 0.31(3) 1 calc PR A 1 N9B N 0.13474(15) -0.1186(5) 0.49234(13) 0.0502(18) Uani 0.69(3) 1 d PD A 2 C91B C 0.1314(4) -0.1098(11) 0.44270(16) 0.035(3) Uani 0.69(3) 1 d PD A 2 C92B C 0.0772(5) -0.0983(14) 0.4132(2) 0.077(5) Uani 0.69(3) 1 d PD A 2 H92B H 0.0750 -0.0919 0.3796 0.092 Uiso 0.69(3) 1 calc PR A 2 C93B C 0.0265(3) -0.0964(12) 0.4332(4) 0.124(6) Uani 0.69(3) 1 d PD A 2 C94B C 0.0301(2) -0.1024(15) 0.4830(5) 0.064(6) Uani 0.69(3) 1 d PD A 2 H94B H -0.0040 -0.0984 0.4967 0.076 Uiso 0.69(3) 1 calc PR A 2 C95B C 0.0842(3) -0.1143(13) 0.5125(3) 0.045(4) Uani 0.69(3) 1 d PD A 2 H95B H 0.0865 -0.1194 0.5461 0.054 Uiso 0.69(3) 1 calc PR A 2 C96B C -0.0322(10) -0.091(2) 0.4008(16) 0.32(2) Uani 0.69(3) 1 d PD A 2 H96C H -0.0634 -0.1037 0.4192 0.383 Uiso 0.69(3) 1 calc PR A 2 H96D H -0.0344 -0.1321 0.3744 0.383 Uiso 0.69(3) 1 calc PR A 2 C97B C -0.039(2) -0.001(3) 0.3806(10) 0.27(2) Uani 0.69(3) 1 d PD A 2 H97D H -0.0767 0.0039 0.3589 0.402 Uiso 0.69(3) 1 calc PR A 2 H97E H -0.0079 0.0116 0.3631 0.402 Uiso 0.69(3) 1 calc PR A 2 H97F H -0.0383 0.0393 0.4070 0.402 Uiso 0.69(3) 1 calc PR A 2 N10 N 0.20597(19) 0.0988(4) 0.41551(16) 0.0470(17) Uani 0.482(15) 1 d PGD A 1 C101 C 0.1777(7) 0.1306(10) 0.3714(3) 0.040(4) Uani 0.482(15) 1 d PGD A 1 H101 H 0.1953 0.1254 0.3438 0.048 Uiso 0.482(15) 1 calc PR A 1 C102 C 0.1236(8) 0.1701(14) 0.3681(8) 0.059(5) Uani 0.482(15) 1 d PGD A 1 H102 H 0.1045 0.1917 0.3383 0.071 Uiso 0.482(15) 1 calc PR A 1 C103 C 0.0976(7) 0.178(2) 0.4089(11) 0.098(6) Uani 0.482(15) 1 d PGD A 1 C104 C 0.1259(9) 0.146(2) 0.4531(9) 0.074(4) Uani 0.482(15) 1 d PGD A 1 H104 H 0.1083 0.1512 0.4807 0.089 Uiso 0.482(15) 1 calc PR A 1 C105 C 0.1800(8) 0.1065(14) 0.4563(4) 0.044(4) Uani 0.482(15) 1 d PGD A 1 C106 C 0.0352(6) 0.2040(17) 0.4083(10) 0.088(5) Uiso 0.482(15) 1 d PD A 1 H10A H 0.0141 0.1599 0.4229 0.106 Uiso 0.482(15) 1 calc PR A 1 H10B H 0.0151 0.2139 0.3751 0.106 Uiso 0.482(15) 1 calc PR A 1 C107 C 0.038(2) 0.286(2) 0.4377(18) 0.240(17) Uiso 0.482(15) 1 d PD A 1 H10C H -0.0009 0.3060 0.4388 0.360 Uiso 0.482(15) 1 calc PR A 1 H10D H 0.0594 0.3289 0.4227 0.360 Uiso 0.482(15) 1 calc PR A 1 H10E H 0.0589 0.2752 0.4703 0.360 Uiso 0.482(15) 1 calc PR A 1 N10B N 0.20597(19) 0.0988(4) 0.41551(16) 0.0470(17) Uani 0.518(15) 1 d PD A 2 C01B C 0.1844(7) 0.1562(9) 0.3791(4) 0.040(4) Uani 0.518(15) 1 d PD A 2 H01B H 0.2050 0.1657 0.3536 0.048 Uiso 0.518(15) 1 calc PR A 2 C02B C 0.1325(9) 0.1995(11) 0.3804(7) 0.059(5) Uani 0.518(15) 1 d PD A 2 H02B H 0.1172 0.2368 0.3552 0.071 Uiso 0.518(15) 1 calc PR A 2 C03B C 0.1031(9) 0.188(2) 0.4191(11) 0.098(6) Uani 0.518(15) 1 d PD A 2 C04B C 0.1254(9) 0.132(2) 0.4561(9) 0.074(4) Uani 0.518(15) 1 d PD A 2 H04B H 0.1062 0.1249 0.4826 0.089 Uiso 0.518(15) 1 calc PR A 2 C05B C 0.1762(7) 0.0861(14) 0.4538(5) 0.044(4) Uani 0.518(15) 1 d PD A 2 C06B C 0.0520(8) 0.2478(15) 0.4190(9) 0.088(5) Uiso 0.518(15) 1 d PD A 2 H06A H 0.0434 0.2520 0.4518 0.106 Uiso 0.518(15) 1 calc PR A 2 H06B H 0.0630 0.3046 0.4093 0.106 Uiso 0.518(15) 1 calc PR A 2 C07B C -0.0026(17) 0.219(3) 0.3851(15) 0.240(17) Uiso 0.518(15) 1 d PD A 2 H07A H -0.0341 0.2591 0.3867 0.360 Uiso 0.518(15) 1 calc PR A 2 H07B H -0.0139 0.1631 0.3946 0.360 Uiso 0.518(15) 1 calc PR A 2 H07C H 0.0052 0.2170 0.3523 0.360 Uiso 0.518(15) 1 calc PR A 2 C121 C 0.1985(3) 0.0584(6) 0.5398(2) 0.0396(19) Uani 1 1 d . A . C122 C 0.1930(4) 0.1372(6) 0.5586(3) 0.055(2) Uani 1 1 d . . . H122 H 0.1916 0.1852 0.5385 0.066 Uiso 1 1 calc R A . C123 C 0.1896(4) 0.1477(7) 0.6074(3) 0.059(2) Uani 1 1 d . A . H123 H 0.1855 0.2020 0.6203 0.071 Uiso 1 1 calc R . . C124 C 0.1922(3) 0.0753(6) 0.6363(3) 0.049(2) Uani 1 1 d . . . H124 H 0.1885 0.0795 0.6690 0.059 Uiso 1 1 calc R A . C125 C 0.2003(3) -0.0020(6) 0.6161(2) 0.047(2) Uani 1 1 d . A . C141 C 0.1915(3) -0.1598(6) 0.6380(2) 0.043(2) Uani 1 1 d . . . C142 C 0.1799(4) -0.2077(7) 0.6772(3) 0.056(2) Uani 1 1 d . A . H142 H 0.1829 -0.1828 0.7079 0.067 Uiso 1 1 calc R . . C143 C 0.1643(4) -0.2901(7) 0.6705(3) 0.063(3) Uani 1 1 d . . . H143 H 0.1558 -0.3224 0.6965 0.075 Uiso 1 1 calc R A . C144 C 0.1609(3) -0.3276(7) 0.6251(3) 0.059(2) Uani 1 1 d . A . H144 H 0.1498 -0.3848 0.6200 0.070 Uiso 1 1 calc R . . C145 C 0.1742(3) -0.2776(6) 0.5878(2) 0.043(2) Uani 1 1 d . . . C161 C 0.2044(3) -0.3086(6) 0.5058(2) 0.048(2) Uani 1 1 d . . . C162 C 0.2058(4) -0.3776(6) 0.4752(3) 0.055(2) Uani 1 1 d . A . H162 H 0.1863 -0.4287 0.4797 0.066 Uiso 1 1 calc R . . C163 C 0.2371(3) -0.3678(6) 0.4379(3) 0.052(2) Uani 1 1 d . . . H163 H 0.2380 -0.4124 0.4157 0.062 Uiso 1 1 calc R A . C164 C 0.2667(3) -0.2941(6) 0.4327(2) 0.049(2) Uani 1 1 d . A . H164 H 0.2882 -0.2885 0.4074 0.059 Uiso 1 1 calc R . . C165 C 0.2650(3) -0.2264(5) 0.4655(2) 0.0337(17) Uani 1 1 d . A . C181 C 0.3418(3) -0.1419(5) 0.4433(2) 0.0385(19) Uani 1 1 d . A . C182 C 0.3834(3) -0.2056(6) 0.4446(2) 0.048(2) Uani 1 1 d . . . H182 H 0.3782 -0.2565 0.4608 0.058 Uiso 1 1 calc R A . C183 C 0.4322(3) -0.1970(6) 0.4229(3) 0.051(2) Uani 1 1 d . A . C184 C 0.4392(4) -0.1174(7) 0.4017(3) 0.062(3) Uani 1 1 d . . . H184 H 0.4712 -0.1083 0.3859 0.075 Uiso 1 1 calc R A . C185 C 0.4000(4) -0.0532(7) 0.4038(3) 0.060(3) Uani 1 1 d . A . H185 H 0.4073 0.0006 0.3916 0.072 Uiso 1 1 calc R . . C186 C 0.4739(4) -0.2696(7) 0.4216(3) 0.067(3) Uani 1 1 d . . . H18A H 0.4858 -0.2920 0.4544 0.080 Uiso 1 1 calc R A . H18B H 0.5090 -0.2487 0.4104 0.080 Uiso 1 1 calc R . . C187 C 0.4466(4) -0.3415(7) 0.3882(3) 0.077(3) Uani 1 1 d . A . H18C H 0.4747 -0.3874 0.3888 0.116 Uiso 1 1 calc R . . H18D H 0.4359 -0.3201 0.3555 0.116 Uiso 1 1 calc R . . H18E H 0.4119 -0.3626 0.3992 0.116 Uiso 1 1 calc R . . B1 B 0.3341(4) 0.4599(6) 0.6416(3) 0.043(2) Uani 1 1 d . . . C201 C 0.2629(3) 0.4582(6) 0.6267(3) 0.053(2) Uani 1 1 d . . . C202 C 0.2255(4) 0.4548(8) 0.6607(3) 0.083(4) Uani 1 1 d . . . H202 H 0.2423 0.4586 0.6936 0.100 Uiso 1 1 calc R . . C203 C 0.1653(4) 0.4462(8) 0.6490(4) 0.094(4) Uani 1 1 d . . . H203 H 0.1422 0.4460 0.6734 0.113 Uiso 1 1 calc R . . C204 C 0.1392(5) 0.4379(9) 0.6009(5) 0.106(5) Uani 1 1 d . . . H204 H 0.0986 0.4292 0.5925 0.127 Uiso 1 1 calc R . . C205 C 0.1734(4) 0.4426(8) 0.5653(4) 0.091(4) Uani 1 1 d . . . H205 H 0.1560 0.4391 0.5325 0.110 Uiso 1 1 calc R . . C206 C 0.2331(4) 0.4523(6) 0.5781(3) 0.067(3) Uani 1 1 d . . . H206 H 0.2554 0.4553 0.5533 0.081 Uiso 1 1 calc R . . C207 C 0.3531(3) 0.5331(5) 0.6839(3) 0.045(2) Uani 1 1 d . . . C208 C 0.3190(4) 0.6051(6) 0.6874(3) 0.053(2) Uani 1 1 d . . . H208 H 0.2822 0.6085 0.6671 0.064 Uiso 1 1 calc R . . C209 C 0.3356(4) 0.6714(7) 0.7187(3) 0.063(3) Uani 1 1 d . . . H209 H 0.3112 0.7193 0.7183 0.076 Uiso 1 1 calc R . . C210 C 0.3883(4) 0.6682(7) 0.7510(3) 0.066(3) Uani 1 1 d . . . H210 H 0.4000 0.7132 0.7725 0.079 Uiso 1 1 calc R . . C211 C 0.4225(4) 0.5977(7) 0.7505(3) 0.076(3) Uani 1 1 d . . . H211 H 0.4577 0.5933 0.7727 0.091 Uiso 1 1 calc R . . C212 C 0.4061(4) 0.5323(6) 0.7177(3) 0.064(3) Uani 1 1 d . . . H212 H 0.4313 0.4854 0.7179 0.076 Uiso 1 1 calc R . . C213 C 0.3627(3) 0.4933(6) 0.5941(2) 0.044(2) Uani 1 1 d . . . C214 C 0.3519(4) 0.5749(7) 0.5763(3) 0.065(3) Uani 1 1 d . . . H214 H 0.3282 0.6102 0.5918 0.077 Uiso 1 1 calc R . . C215 C 0.3737(4) 0.6089(7) 0.5368(3) 0.073(3) Uani 1 1 d . . . H215 H 0.3655 0.6653 0.5269 0.087 Uiso 1 1 calc R . . C216 C 0.4072(4) 0.5574(8) 0.5131(3) 0.069(3) Uani 1 1 d . . . H216 H 0.4216 0.5780 0.4861 0.083 Uiso 1 1 calc R . . C217 C 0.4196(4) 0.4769(7) 0.5287(3) 0.063(3) Uani 1 1 d . . . H217 H 0.4433 0.4425 0.5127 0.076 Uiso 1 1 calc R . . C218 C 0.3974(3) 0.4441(6) 0.5686(3) 0.050(2) Uani 1 1 d . . . H218 H 0.4061 0.3877 0.5784 0.061 Uiso 1 1 calc R . . C219 C 0.3584(3) 0.3644(5) 0.6585(2) 0.0402(19) Uani 1 1 d . . . C220 C 0.4179(4) 0.3435(6) 0.6706(2) 0.049(2) Uani 1 1 d . . . H220 H 0.4455 0.3870 0.6693 0.059 Uiso 1 1 calc R . . C221 C 0.4389(4) 0.2628(6) 0.6842(3) 0.056(2) Uani 1 1 d . . . H221 H 0.4794 0.2526 0.6917 0.067 Uiso 1 1 calc R . . C222 C 0.3993(4) 0.1971(6) 0.6866(3) 0.056(2) Uani 1 1 d . . . H222 H 0.4127 0.1426 0.6968 0.068 Uiso 1 1 calc R . . C223 C 0.3404(4) 0.2128(6) 0.6738(3) 0.055(2) Uani 1 1 d . . . H223 H 0.3133 0.1684 0.6738 0.066 Uiso 1 1 calc R . . C224 C 0.3210(4) 0.2941(6) 0.6608(2) 0.048(2) Uani 1 1 d . . . H224 H 0.2804 0.3032 0.6531 0.058 Uiso 1 1 calc R . . B2 B 0.1895(3) 0.4652(5) 0.3016(2) 0.053(3) Uani 1 1 d D . . C225 C 0.1366(3) 0.5373(5) 0.3007(3) 0.077(3) Uani 0.15(2) 1 d PGD B 1 C226 C 0.116(2) 0.599(3) 0.3292(15) 0.098(6) Uani 0.15(2) 1 d PGD B 1 H226 H 0.1317 0.6021 0.3624 0.118 Uiso 0.15(2) 1 calc PR B 1 C227 C 0.073(3) 0.656(4) 0.309(3) 0.151(10) Uani 0.15(2) 1 d PGD B 1 H227 H 0.0597 0.6978 0.3279 0.181 Uiso 0.15(2) 1 calc PR B 1 C228 C 0.051(2) 0.652(4) 0.259(3) 0.143(11) Uani 0.15(2) 1 d PGD B 1 H228 H 0.0216 0.6901 0.2455 0.172 Uiso 0.15(2) 1 calc PR B 1 C229 C 0.071(2) 0.590(5) 0.2310(17) 0.124(7) Uani 0.15(2) 1 d PGD B 1 H229 H 0.0556 0.5868 0.1978 0.149 Uiso 0.15(2) 1 calc PR B 1 C230 C 0.1139(18) 0.533(3) 0.2516(5) 0.078(4) Uani 0.15(2) 1 d PGD B 1 H230 H 0.1276 0.4911 0.2324 0.093 Uiso 0.15(2) 1 calc PR B 1 C25B C 0.1366(3) 0.5373(5) 0.3007(3) 0.077(3) Uani 0.85(2) 1 d PD B 2 C26B C 0.1178(5) 0.5647(9) 0.3425(3) 0.098(6) Uani 0.85(2) 1 d PD B 2 H26B H 0.1328 0.5391 0.3724 0.118 Uiso 0.85(2) 1 calc PR B 2 C27B C 0.0768(7) 0.6297(11) 0.3403(6) 0.151(10) Uani 0.85(2) 1 d PD B 2 H27B H 0.0629 0.6465 0.3683 0.181 Uiso 0.85(2) 1 calc PR B 2 C28B C 0.0564(6) 0.6699(8) 0.2965(7) 0.143(11) Uani 0.85(2) 1 d PD B 2 H28B H 0.0317 0.7176 0.2954 0.172 Uiso 0.85(2) 1 calc PR B 2 C29B C 0.0726(5) 0.6395(9) 0.2543(5) 0.124(7) Uani 0.85(2) 1 d PD B 2 H29B H 0.0557 0.6625 0.2242 0.149 Uiso 0.85(2) 1 calc PR B 2 C30B C 0.1140(4) 0.5749(8) 0.2566(3) 0.078(4) Uani 0.85(2) 1 d PD B 2 H30B H 0.1267 0.5566 0.2283 0.093 Uiso 0.85(2) 1 calc PR B 2 C231 C 0.1685(10) 0.3772(11) 0.2703(8) 0.049(2) Uani 0.395(11) 1 d PGD B 1 C232 C 0.1089(9) 0.3593(10) 0.2639(6) 0.052(4) Uani 0.395(11) 1 d PGD B 1 H232 H 0.0823 0.4022 0.2687 0.062 Uiso 0.395(11) 1 calc PR B 1 C233 C 0.0888(8) 0.2781(12) 0.2504(7) 0.078(4) Uani 0.395(11) 1 d PGD B 1 H233 H 0.0485 0.2660 0.2460 0.094 Uiso 0.395(11) 1 calc PR B 1 C234 C 0.1282(11) 0.2147(8) 0.2432(8) 0.080(5) Uani 0.395(11) 1 d PGD B 1 H234 H 0.1146 0.1598 0.2341 0.096 Uiso 0.395(11) 1 calc PR B 1 C235 C 0.1878(10) 0.2326(13) 0.2497(9) 0.085(4) Uani 0.395(11) 1 d PGD B 1 H235 H 0.2145 0.1897 0.2449 0.102 Uiso 0.395(11) 1 calc PR B 1 C236 C 0.2079(7) 0.3138(17) 0.2632(10) 0.051(4) Uani 0.395(11) 1 d PGD B 1 H236 H 0.2482 0.3259 0.2675 0.061 Uiso 0.395(11) 1 calc PR B 1 C31B C 0.1619(7) 0.3752(8) 0.2719(5) 0.049(2) Uani 0.605(11) 1 d PD B 2 C32B C 0.1073(6) 0.3758(7) 0.2421(5) 0.052(4) Uani 0.605(11) 1 d PD B 2 H32B H 0.0833 0.4242 0.2408 0.062 Uiso 0.605(11) 1 calc PR B 2 C33B C 0.0882(5) 0.3049(8) 0.2142(6) 0.078(4) Uani 0.605(11) 1 d PD B 2 H33B H 0.0508 0.3046 0.1948 0.094 Uiso 0.605(11) 1 calc PR B 2 C34B C 0.1245(7) 0.2343(7) 0.2149(6) 0.080(5) Uani 0.605(11) 1 d PD B 2 H34B H 0.1123 0.1873 0.1950 0.096 Uiso 0.605(11) 1 calc PR B 2 C35B C 0.1788(7) 0.2334(10) 0.2450(7) 0.085(4) Uani 0.605(11) 1 d PD B 2 H35B H 0.2027 0.1849 0.2464 0.102 Uiso 0.605(11) 1 calc PR B 2 C36B C 0.1977(5) 0.3041(11) 0.2731(5) 0.051(4) Uani 0.605(11) 1 d PD B 2 H36B H 0.2348 0.3039 0.2930 0.061 Uiso 0.605(11) 1 calc PR B 2 C237 C 0.2432(3) 0.5133(6) 0.2795(3) 0.050(2) Uani 1 1 d D B . C238 C 0.2776(4) 0.4764(7) 0.2490(3) 0.064(3) Uani 1 1 d . . . H238 H 0.2686 0.4212 0.2371 0.077 Uiso 1 1 calc R B . C239 C 0.3252(4) 0.5197(8) 0.2357(4) 0.075(3) Uani 1 1 d . B . H239 H 0.3473 0.4932 0.2149 0.090 Uiso 1 1 calc R . . C240 C 0.3397(4) 0.5989(8) 0.2522(4) 0.075(3) Uani 1 1 d . . . H240 H 0.3717 0.6276 0.2431 0.089 Uiso 1 1 calc R B . C241 C 0.3063(4) 0.6374(7) 0.2831(3) 0.067(3) Uani 1 1 d . B . H241 H 0.3158 0.6923 0.2951 0.081 Uiso 1 1 calc R . . C242 C 0.2600(4) 0.5956(6) 0.2958(3) 0.059(2) Uani 1 1 d . . . H242 H 0.2381 0.6231 0.3164 0.070 Uiso 1 1 calc R B . C243 C 0.2156(3) 0.4337(5) 0.35796(17) 0.078(3) Uani 0.77(5) 1 d PGD B 1 C244 C 0.2749(3) 0.4408(12) 0.3771(5) 0.067(4) Uani 0.77(5) 1 d PGD B 1 H244 H 0.3013 0.4598 0.3576 0.081 Uiso 0.77(5) 1 calc PR B 1 C245 C 0.2950(6) 0.4199(13) 0.4253(5) 0.094(5) Uani 0.77(5) 1 d PGD B 1 H245 H 0.3351 0.4248 0.4382 0.113 Uiso 0.77(5) 1 calc PR B 1 C246 C 0.2559(8) 0.3919(15) 0.4542(2) 0.130(7) Uani 0.77(5) 1 d PGD B 1 H246 H 0.2696 0.3778 0.4867 0.155 Uiso 0.77(5) 1 calc PR B 1 C247 C 0.1967(7) 0.385(2) 0.4350(6) 0.137(10) Uani 0.77(5) 1 d PGD B 1 H247 H 0.1703 0.3658 0.4545 0.165 Uiso 0.77(5) 1 calc PR B 1 C248 C 0.1765(4) 0.4056(16) 0.3869(5) 0.116(7) Uani 0.77(5) 1 d PGD B 1 H248 H 0.1365 0.4008 0.3739 0.139 Uiso 0.77(5) 1 calc PR B 1 C43B C 0.2156(3) 0.4337(5) 0.35796(17) 0.078(3) Uani 0.23(5) 1 d PD B 2 C44B C 0.2703(9) 0.454(3) 0.3845(9) 0.067(4) Uani 0.23(5) 1 d PD B 2 H44B H 0.2967 0.4867 0.3705 0.081 Uiso 0.23(5) 1 calc PR B 2 C45B C 0.2859(14) 0.425(5) 0.4317(9) 0.094(5) Uani 0.23(5) 1 d PD B 2 H45B H 0.3221 0.4404 0.4502 0.113 Uiso 0.23(5) 1 calc PR B 2 C46B C 0.2479(16) 0.373(4) 0.4516(9) 0.130(7) Uani 0.23(5) 1 d PD B 2 H46B H 0.2574 0.3555 0.4841 0.155 Uiso 0.23(5) 1 calc PR B 2 C47B C 0.196(2) 0.346(4) 0.4233(13) 0.137(10) Uani 0.23(5) 1 d PD B 2 H47B H 0.1720 0.3057 0.4356 0.165 Uiso 0.23(5) 1 calc PR B 2 C48B C 0.1791(17) 0.378(4) 0.3769(13) 0.116(7) Uani 0.23(5) 1 d PD B 2 H48B H 0.1431 0.3613 0.3582 0.139 Uiso 0.23(5) 1 calc PR B 2 Cl1 Cl 0.4693(2) 0.3268(4) 0.41767(14) 0.1304(19) Uani 0.848(4) 1 d PD C 1 C1S C 0.4941(5) 0.3884(11) 0.3746(4) 0.128(6) Uani 0.848(4) 1 d PD C 1 H1S1 H 0.5204 0.3536 0.3589 0.154 Uiso 0.848(4) 1 calc PR C 1 H1S2 H 0.5174 0.4351 0.3912 0.154 Uiso 0.848(4) 1 calc PR C 1 Cl2 Cl 0.4415(2) 0.4316(4) 0.33012(19) 0.141(2) Uani 0.848(4) 1 d PD C 1 Cl1B Cl 0.4368(11) 0.414(2) 0.4041(8) 0.1304(19) Uani 0.152(4) 1 d PD C 2 C1SB C 0.4933(13) 0.400(7) 0.372(2) 0.128(6) Uani 0.152(4) 1 d PD C 2 H1S3 H 0.5237 0.3655 0.3921 0.154 Uiso 0.152(4) 1 calc PR C 2 H1S4 H 0.5104 0.4556 0.3678 0.154 Uiso 0.152(4) 1 calc PR C 2 Cl2B Cl 0.4755(11) 0.352(2) 0.3165(8) 0.141(2) Uani 0.152(4) 1 d PD C 2 Cl3 Cl 0.0784(6) -0.0394(11) 0.2625(4) 0.313(9) Uani 0.691(11) 1 d PD D 1 C2S C 0.0241(6) -0.0165(11) 0.2143(4) 0.119(7) Uani 0.691(11) 1 d PD D 1 H2S1 H 0.0265 0.0442 0.2069 0.143 Uiso 0.691(11) 1 calc PR D 1 H2S2 H -0.0138 -0.0260 0.2244 0.143 Uiso 0.691(11) 1 calc PR D 1 Cl4 Cl 0.0247(4) -0.0728(10) 0.1618(5) 0.257(7) Uani 0.691(11) 1 d PD D 1 Cl3B Cl 0.0753(14) 0.0182(19) 0.2776(11) 0.313(9) Uani 0.309(11) 1 d PD D 2 C2SB C 0.056(2) -0.0858(17) 0.2634(10) 0.119(7) Uani 0.309(11) 1 d PD D 2 H2S3 H 0.0885 -0.1224 0.2789 0.143 Uiso 0.309(11) 1 calc PR D 2 H2S4 H 0.0218 -0.0998 0.2775 0.143 Uiso 0.309(11) 1 calc PR D 2 Cl4B Cl 0.0414(10) -0.111(2) 0.2028(12) 0.257(7) Uani 0.309(11) 1 d PD D 2 Cl5 Cl 0.0419(3) -0.4281(6) 0.4779(4) 0.156(4) Uani 0.50 1 d PD . . C3S C 0.0407(7) -0.3261(10) 0.4553(11) 0.21(2) Uani 0.50 1 d PD . . H3S1 H 0.0707 -0.3219 0.4348 0.257 Uiso 0.50 1 calc PR . . H3S2 H 0.0519 -0.2870 0.4826 0.257 Uiso 0.50 1 calc PR . . Cl6 Cl -0.0247(6) -0.2916(7) 0.4223(6) 0.270(8) Uani 0.50 1 d PD . . Cl7 Cl 0.5261(7) -0.0517(8) 0.5028(6) 0.180(3) Uani 0.50 1 d PDU . . C4S C 0.4745(9) 0.0281(10) 0.4971(8) 0.101(5) Uani 0.50 1 d PDU . . H4S1 H 0.4706 0.0470 0.5297 0.121 Uiso 0.50 1 calc PR . . H4S2 H 0.4367 0.0037 0.4823 0.121 Uiso 0.50 1 calc PR . . Cl8 Cl 0.4870(5) 0.1165(7) 0.4641(4) 0.180(3) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0323(5) 0.0675(7) 0.0156(4) 0.0051(4) 0.0050(3) -0.0057(5) Ni2 0.0308(5) 0.0638(7) 0.0134(4) 0.0026(4) 0.0019(3) -0.0079(4) Ni3 0.0398(5) 0.0601(7) 0.0132(4) 0.0009(4) 0.0040(3) -0.0114(5) N1 0.034(3) 0.067(5) 0.017(3) 0.005(3) 0.004(2) -0.002(3) N2 0.031(3) 0.062(5) 0.013(3) 0.006(3) 0.000(2) -0.003(3) N3 0.040(3) 0.069(5) 0.013(3) -0.003(3) 0.005(2) -0.014(3) N4 0.075(5) 0.055(5) 0.022(3) 0.002(3) 0.006(3) -0.014(4) N5 0.038(3) 0.048(4) 0.018(3) -0.004(3) 0.003(2) -0.008(3) N6 0.059(4) 0.070(5) 0.020(3) -0.001(3) 0.017(3) -0.015(4) N7 0.037(3) 0.076(5) 0.015(3) 0.001(3) -0.001(2) -0.014(3) N8 0.035(3) 0.084(5) 0.015(3) 0.005(3) 0.000(2) -0.018(3) N11 0.037(3) 0.082(5) 0.021(3) 0.014(3) 0.002(2) -0.006(3) N12 0.040(4) 0.076(5) 0.016(3) 0.003(3) 0.007(2) 0.002(3) N13 0.053(4) 0.084(6) 0.013(3) 0.007(3) 0.004(3) 0.004(4) N14 0.031(3) 0.069(5) 0.020(3) -0.001(3) 0.001(2) -0.004(3) N15 0.055(4) 0.086(6) 0.031(3) 0.001(3) 0.010(3) -0.030(4) N16 0.034(3) 0.076(5) 0.019(3) 0.009(3) 0.005(2) -0.013(3) N17 0.032(3) 0.077(5) 0.015(3) 0.001(3) 0.002(2) -0.015(3) N18 0.035(3) 0.073(5) 0.020(3) 0.000(3) 0.007(2) -0.016(3) C11 0.042(4) 0.072(6) 0.027(4) 0.010(4) 0.004(3) 0.000(4) C12 0.044(5) 0.099(8) 0.035(4) 0.021(5) -0.007(4) 0.002(5) C13 0.045(5) 0.086(7) 0.051(5) 0.016(5) -0.007(4) -0.009(5) C14 0.038(4) 0.097(7) 0.034(4) 0.012(5) -0.004(3) -0.012(5) C15 0.034(4) 0.064(6) 0.019(3) 0.002(3) 0.005(3) -0.008(4) C16 0.054(6) 0.159(12) 0.102(9) 0.063(9) -0.031(6) -0.017(7) C17 0.076(9) 0.40(3) 0.107(12) -0.033(16) -0.037(8) -0.058(14) C31 0.040(4) 0.065(6) 0.017(3) 0.000(3) 0.008(3) -0.005(4) C32 0.056(5) 0.083(7) 0.014(3) -0.003(4) 0.002(3) -0.018(5) C33 0.064(5) 0.081(7) 0.019(4) -0.015(4) 0.004(3) -0.022(5) C34 0.071(6) 0.066(6) 0.027(4) -0.004(4) 0.005(4) -0.029(5) C35 0.052(5) 0.066(6) 0.017(3) 0.000(4) 0.003(3) -0.013(4) C51 0.038(4) 0.057(6) 0.016(3) 0.000(3) 0.001(3) -0.012(4) C52 0.061(5) 0.054(5) 0.028(4) 0.006(4) 0.003(3) -0.017(4) C53 0.067(5) 0.066(6) 0.025(4) 0.004(4) 0.013(4) -0.025(5) C54 0.057(5) 0.078(7) 0.013(3) 0.004(4) 0.009(3) -0.015(5) C55 0.036(4) 0.055(5) 0.018(3) 0.003(3) 0.003(3) -0.009(4) C71 0.054(5) 0.065(6) 0.015(3) 0.006(4) 0.003(3) -0.009(4) C72 0.066(6) 0.084(7) 0.017(3) -0.003(4) 0.005(3) -0.025(5) C73 0.077(6) 0.075(7) 0.032(4) -0.002(4) -0.009(4) -0.025(5) C74 0.067(5) 0.073(6) 0.023(4) 0.008(4) -0.006(4) -0.035(5) C75 0.035(4) 0.078(6) 0.023(3) 0.009(4) -0.004(3) -0.013(4) N9 0.033(3) 0.089(6) 0.028(3) 0.015(3) 0.004(3) -0.005(3) C91 0.033(4) 0.052(10) 0.019(4) -0.001(5) -0.001(3) -0.021(5) C92 0.041(5) 0.143(15) 0.039(5) 0.033(7) -0.016(4) -0.038(7) C93 0.029(5) 0.270(18) 0.064(7) 0.071(9) -0.014(5) -0.026(8) C94 0.037(5) 0.108(18) 0.047(8) 0.010(9) 0.009(4) -0.009(7) C95 0.040(5) 0.062(12) 0.033(5) 0.002(6) 0.005(4) -0.013(6) C96 0.063(9) 0.77(6) 0.119(13) 0.25(3) -0.006(8) 0.033(19) C97 0.075(15) 0.55(6) 0.17(3) -0.18(4) -0.02(2) 0.07(2) N9B 0.033(3) 0.089(6) 0.028(3) 0.015(3) 0.004(3) -0.005(3) C91B 0.033(4) 0.052(10) 0.019(4) -0.001(5) -0.001(3) -0.021(5) C92B 0.041(5) 0.143(15) 0.039(5) 0.033(7) -0.016(4) -0.038(7) C93B 0.029(5) 0.270(18) 0.064(7) 0.071(9) -0.014(5) -0.026(8) C94B 0.037(5) 0.108(18) 0.047(8) 0.010(9) 0.009(4) -0.009(7) C95B 0.040(5) 0.062(12) 0.033(5) 0.002(6) 0.005(4) -0.013(6) C96B 0.063(9) 0.77(6) 0.119(13) 0.25(3) -0.006(8) 0.033(19) C97B 0.075(15) 0.55(6) 0.17(3) -0.18(4) -0.02(2) 0.07(2) N10 0.046(4) 0.075(5) 0.019(3) 0.010(3) 0.002(3) -0.006(3) C101 0.052(6) 0.042(10) 0.021(5) -0.006(6) -0.008(4) -0.017(7) C102 0.054(8) 0.102(15) 0.013(10) 0.001(9) -0.015(5) 0.002(10) C103 0.066(7) 0.181(15) 0.050(12) 0.055(10) 0.018(7) 0.054(9) C104 0.056(6) 0.124(13) 0.044(5) 0.039(7) 0.018(4) 0.021(7) C105 0.041(5) 0.067(11) 0.023(4) 0.009(5) 0.000(3) -0.013(6) N10B 0.046(4) 0.075(5) 0.019(3) 0.010(3) 0.002(3) -0.006(3) C01B 0.052(6) 0.042(10) 0.021(5) -0.006(6) -0.008(4) -0.017(7) C02B 0.054(8) 0.102(15) 0.013(10) 0.001(9) -0.015(5) 0.002(10) C03B 0.066(7) 0.181(15) 0.050(12) 0.055(10) 0.018(7) 0.054(9) C04B 0.056(6) 0.124(13) 0.044(5) 0.039(7) 0.018(4) 0.021(7) C05B 0.041(5) 0.067(11) 0.023(4) 0.009(5) 0.000(3) -0.013(6) C121 0.029(4) 0.066(6) 0.025(4) 0.004(4) 0.009(3) 0.001(4) C122 0.057(5) 0.077(7) 0.033(4) 0.008(4) 0.015(4) 0.010(5) C123 0.052(5) 0.080(7) 0.045(5) 0.004(5) 0.011(4) 0.008(5) C124 0.043(4) 0.081(7) 0.025(4) 0.001(4) 0.013(3) 0.010(4) C125 0.032(4) 0.090(7) 0.020(3) 0.003(4) 0.007(3) 0.000(4) C141 0.034(4) 0.073(6) 0.022(4) 0.006(4) 0.007(3) -0.004(4) C142 0.060(5) 0.091(8) 0.019(4) 0.018(4) 0.012(3) 0.008(5) C143 0.069(6) 0.091(8) 0.033(4) 0.026(5) 0.020(4) 0.005(6) C144 0.054(5) 0.087(7) 0.035(4) 0.018(4) 0.009(4) -0.005(5) C145 0.037(4) 0.076(7) 0.018(3) 0.005(4) 0.007(3) -0.009(4) C161 0.041(4) 0.076(7) 0.025(4) 0.014(4) 0.005(3) -0.008(4) C162 0.062(5) 0.068(6) 0.034(4) 0.001(4) 0.005(4) -0.023(5) C163 0.056(5) 0.069(6) 0.031(4) -0.003(4) 0.006(4) -0.011(5) C164 0.049(5) 0.077(6) 0.023(4) -0.001(4) 0.015(3) -0.014(4) C165 0.032(4) 0.055(5) 0.014(3) 0.003(3) 0.003(3) -0.011(3) C181 0.035(4) 0.070(6) 0.010(3) 0.002(3) 0.003(3) -0.009(4) C182 0.043(4) 0.071(6) 0.029(4) 0.013(4) 0.003(3) -0.002(4) C183 0.041(4) 0.082(7) 0.032(4) 0.001(4) 0.010(3) -0.003(4) C184 0.036(5) 0.094(8) 0.063(6) 0.020(5) 0.026(4) 0.006(5) C185 0.045(5) 0.096(8) 0.042(5) 0.015(5) 0.011(4) -0.011(5) C186 0.039(5) 0.100(8) 0.062(6) 0.021(6) 0.014(4) 0.007(5) C187 0.068(6) 0.104(9) 0.062(6) -0.007(6) 0.021(5) 0.004(6) B1 0.048(5) 0.055(6) 0.027(4) 0.005(4) 0.010(4) -0.004(4) C201 0.045(5) 0.074(6) 0.041(4) 0.015(4) 0.006(4) -0.007(4) C202 0.046(5) 0.151(11) 0.052(5) 0.051(6) 0.008(4) -0.003(6) C203 0.045(6) 0.154(12) 0.087(8) 0.061(8) 0.019(5) 0.006(6) C204 0.048(6) 0.145(12) 0.118(10) 0.046(9) -0.007(7) -0.022(7) C205 0.061(7) 0.138(11) 0.068(7) 0.020(7) -0.008(5) -0.029(7) C206 0.051(5) 0.100(8) 0.046(5) 0.000(5) -0.006(4) -0.020(5) C207 0.042(4) 0.061(6) 0.032(4) 0.010(4) 0.010(3) -0.001(4) C208 0.056(5) 0.077(7) 0.027(4) 0.002(4) 0.010(4) 0.010(5) C209 0.076(6) 0.075(7) 0.041(5) 0.003(5) 0.019(4) 0.022(5) C210 0.070(6) 0.080(7) 0.046(5) -0.015(5) 0.004(5) 0.005(6) C211 0.066(6) 0.083(8) 0.067(6) -0.028(6) -0.018(5) 0.011(6) C212 0.055(5) 0.070(7) 0.061(6) -0.008(5) -0.002(4) 0.008(5) C213 0.037(4) 0.066(6) 0.027(4) 0.008(4) -0.001(3) -0.006(4) C214 0.073(6) 0.082(7) 0.041(5) 0.018(5) 0.016(4) 0.006(5) C215 0.085(7) 0.089(8) 0.045(5) 0.028(5) 0.014(5) 0.001(6) C216 0.072(6) 0.107(9) 0.031(4) 0.023(5) 0.019(4) -0.019(6) C217 0.058(6) 0.094(8) 0.038(4) -0.004(5) 0.011(4) -0.026(5) C218 0.058(5) 0.060(6) 0.034(4) 0.002(4) 0.008(4) -0.007(4) C219 0.047(4) 0.064(6) 0.011(3) -0.001(3) 0.009(3) -0.004(4) C220 0.053(5) 0.067(6) 0.028(4) 0.002(4) 0.005(3) 0.001(4) C221 0.054(5) 0.080(7) 0.034(4) -0.002(4) 0.008(4) 0.012(5) C222 0.084(7) 0.061(6) 0.024(4) 0.003(4) 0.011(4) 0.014(5) C223 0.069(6) 0.073(7) 0.025(4) -0.004(4) 0.013(4) -0.010(5) C224 0.052(5) 0.073(7) 0.019(3) 0.001(4) 0.005(3) -0.006(5) B2 0.045(5) 0.071(7) 0.041(5) -0.009(5) -0.003(4) -0.003(5) C225 0.043(5) 0.081(8) 0.105(8) -0.021(7) 0.008(5) -0.010(5) C226 0.052(6) 0.127(14) 0.118(11) -0.070(10) 0.020(7) -0.002(8) C227 0.116(15) 0.16(2) 0.20(3) -0.097(19) 0.101(18) -0.023(13) C228 0.066(10) 0.054(10) 0.32(3) -0.059(16) 0.059(18) -0.023(7) C229 0.081(11) 0.069(13) 0.23(2) -0.011(13) 0.056(12) -0.013(10) C230 0.043(6) 0.047(9) 0.147(12) 0.021(8) 0.027(7) 0.007(6) C25B 0.043(5) 0.081(8) 0.105(8) -0.021(7) 0.008(5) -0.010(5) C26B 0.052(6) 0.127(14) 0.118(11) -0.070(10) 0.020(7) -0.002(8) C27B 0.116(15) 0.16(2) 0.20(3) -0.097(19) 0.101(18) -0.023(13) C28B 0.066(10) 0.054(10) 0.32(3) -0.059(16) 0.059(18) -0.023(7) C29B 0.081(11) 0.069(13) 0.23(2) -0.011(13) 0.056(12) -0.013(10) C30B 0.043(6) 0.047(9) 0.147(12) 0.021(8) 0.027(7) 0.007(6) C231 0.055(6) 0.070(6) 0.020(4) 0.005(4) 0.006(4) -0.003(5) C232 0.058(6) 0.063(9) 0.034(9) 0.007(7) 0.005(8) -0.013(6) C233 0.063(8) 0.080(12) 0.085(11) 0.006(10) -0.005(9) -0.017(8) C234 0.118(12) 0.056(10) 0.066(11) -0.004(9) 0.015(12) -0.022(9) C235 0.112(11) 0.072(8) 0.076(8) -0.009(7) 0.033(7) 0.007(8) C236 0.069(7) 0.073(8) 0.013(8) 0.011(6) 0.014(6) 0.011(7) C31B 0.055(6) 0.070(6) 0.020(4) 0.005(4) 0.006(4) -0.003(5) C32B 0.058(6) 0.063(9) 0.034(9) 0.007(7) 0.005(8) -0.013(6) C33B 0.063(8) 0.080(12) 0.085(11) 0.006(10) -0.005(9) -0.017(8) C34B 0.118(12) 0.056(10) 0.066(11) -0.004(9) 0.015(12) -0.022(9) C35B 0.112(11) 0.072(8) 0.076(8) -0.009(7) 0.033(7) 0.007(8) C36B 0.069(7) 0.073(8) 0.013(8) 0.011(6) 0.014(6) 0.011(7) C237 0.040(4) 0.075(7) 0.031(4) -0.007(4) -0.005(3) 0.004(4) C238 0.051(5) 0.085(7) 0.051(5) -0.022(5) -0.001(4) 0.003(5) C239 0.062(6) 0.099(9) 0.069(6) -0.022(6) 0.023(5) 0.003(6) C240 0.057(6) 0.088(8) 0.081(7) 0.004(6) 0.016(5) -0.010(6) C241 0.060(6) 0.076(7) 0.067(6) -0.002(5) 0.014(5) -0.008(5) C242 0.051(5) 0.081(7) 0.043(5) -0.007(5) 0.003(4) 0.004(5) C243 0.078(7) 0.125(10) 0.033(5) -0.023(5) 0.012(5) -0.004(6) C244 0.079(7) 0.076(9) 0.038(6) -0.031(6) -0.013(5) 0.015(6) C245 0.120(11) 0.107(11) 0.044(7) -0.030(7) -0.014(7) 0.034(9) C246 0.199(18) 0.161(17) 0.023(5) -0.016(8) 0.003(8) 0.052(14) C247 0.159(15) 0.23(3) 0.024(8) -0.007(13) 0.024(9) 0.020(17) C248 0.106(10) 0.22(2) 0.026(7) -0.020(10) 0.027(6) -0.003(11) C43B 0.078(7) 0.125(10) 0.033(5) -0.023(5) 0.012(5) -0.004(6) C44B 0.079(7) 0.076(9) 0.038(6) -0.031(6) -0.013(5) 0.015(6) C45B 0.120(11) 0.107(11) 0.044(7) -0.030(7) -0.014(7) 0.034(9) C46B 0.199(18) 0.161(17) 0.023(5) -0.016(8) 0.003(8) 0.052(14) C47B 0.159(15) 0.23(3) 0.024(8) -0.007(13) 0.024(9) 0.020(17) C48B 0.106(10) 0.22(2) 0.026(7) -0.020(10) 0.027(6) -0.003(11) Cl1 0.112(3) 0.186(5) 0.088(3) -0.018(3) 0.001(2) -0.067(3) C1S 0.077(9) 0.142(14) 0.159(14) -0.018(11) 0.002(9) -0.032(9) Cl2 0.093(3) 0.167(5) 0.151(4) 0.021(4) -0.012(3) -0.032(3) Cl1B 0.112(3) 0.186(5) 0.088(3) -0.018(3) 0.001(2) -0.067(3) C1SB 0.077(9) 0.142(14) 0.159(14) -0.018(11) 0.002(9) -0.032(9) Cl2B 0.093(3) 0.167(5) 0.151(4) 0.021(4) -0.012(3) -0.032(3) Cl3 0.235(10) 0.50(3) 0.238(12) 0.229(14) 0.129(8) 0.214(13) C2S 0.098(13) 0.128(16) 0.144(17) 0.040(13) 0.061(12) 0.064(11) Cl4 0.125(6) 0.392(16) 0.251(14) -0.110(14) 0.030(8) 0.052(7) Cl3B 0.235(10) 0.50(3) 0.238(12) 0.229(14) 0.129(8) 0.214(13) C2SB 0.098(13) 0.128(16) 0.144(17) 0.040(13) 0.061(12) 0.064(11) Cl4B 0.125(6) 0.392(16) 0.251(14) -0.110(14) 0.030(8) 0.052(7) Cl5 0.087(5) 0.156(8) 0.203(9) 0.042(7) -0.037(5) -0.023(5) C3S 0.08(2) 0.23(4) 0.30(5) -0.17(4) -0.07(3) 0.05(2) Cl6 0.225(13) 0.174(11) 0.351(19) -0.012(12) -0.116(13) -0.075(10) Cl7 0.157(5) 0.214(7) 0.173(6) -0.001(5) 0.038(5) -0.004(5) C4S 0.081(9) 0.153(9) 0.057(8) -0.057(7) -0.018(8) -0.027(7) Cl8 0.157(5) 0.214(7) 0.173(6) -0.001(5) 0.038(5) -0.004(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 Ni1 N16 2.027(7) . ? Ni1 N14 2.030(6) . ? Ni1 N12 2.040(7) . ? Ni1 N1 2.084(5) . ? Ni1 N9 2.110(3) . ? Ni1 Ni2 2.3819(12) . ? Ni2 N11 1.876(7) . ? Ni2 N17 1.880(7) . ? Ni2 N8 1.896(5) . ? Ni2 N2 1.900(5) . ? Ni2 Ni3 2.3858(12) . ? Ni3 N5 2.001(6) . ? Ni3 N7 2.023(6) . ? Ni3 N3 2.040(6) . ? Ni3 N10 2.103(4) . ? Ni3 N18 2.115(7) . ? N1 C15 1.337(9) . ? N1 C11 1.351(9) . ? N2 C31 1.357(10) . ? N2 C15 1.389(9) . ? N3 C35 1.316(10) . ? N3 C31 1.387(8) . ? N4 C35 1.417(9) . ? N4 C51 1.420(9) . ? N4 H4 0.8700 . ? N5 C51 1.317(9) . ? N5 C55 1.362(8) . ? N6 C55 1.400(10) . ? N6 C71 1.403(9) . ? N6 H6 0.8700 . ? N7 C71 1.357(9) . ? N7 C75 1.377(9) . ? N8 C91B 1.390(11) . ? N8 C75 1.393(9) . ? N8 C91 1.40(2) . ? N11 C05B 1.352(15) . ? N11 C121 1.409(9) . ? N11 C105 1.472(17) . ? N12 C121 1.362(10) . ? N12 C125 1.382(8) . ? N13 C141 1.381(10) . ? N13 C125 1.411(10) . ? N13 H13 0.8700 . ? N14 C145 1.321(10) . ? N14 C141 1.370(9) . ? N15 C145 1.390(9) . ? N15 C161 1.422(9) . ? N15 H15 0.8700 . ? N16 C161 1.343(10) . ? N16 C165 1.389(8) . ? N17 C165 1.379(9) . ? N17 C181 1.385(9) . ? N18 C181 1.357(9) . ? N18 C185 1.387(9) . ? C11 C12 1.381(10) . ? C11 H11 0.9400 . ? C12 C13 1.393(12) . ? C12 H12 0.9400 . ? C13 C14 1.377(11) . ? C13 C16 1.496(5) . ? C14 C15 1.418(10) . ? C14 H14 0.9400 . ? C16 C17 1.490(9) . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C31 C32 1.402(10) . ? C32 C33 1.369(12) . ? C32 H32 0.9400 . ? C33 C34 1.399(10) . ? C33 H33 0.9400 . ? C34 C35 1.400(10) . ? C34 H34 0.9400 . ? C51 C52 1.401(10) . ? C52 C53 1.391(10) . ? C52 H52 0.9400 . ? C53 C54 1.361(11) . ? C53 H53 0.9400 . ? C54 C55 1.370(10) . ? C54 H54 0.9400 . ? C71 C72 1.382(11) . ? C72 C73 1.402(11) . ? C72 H72 0.9400 . ? C73 C74 1.401(11) . ? C73 H73 0.9400 . ? C74 C75 1.397(11) . ? C74 H74 0.9400 . ? N9 C91 1.3900 . ? N9 C95 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C92 H92 0.9400 . ? C93 C94 1.3900 . ? C93 C96 1.508(7) . ? C94 C95 1.3900 . ? C94 H94 0.9400 . ? C95 H95 0.9400 . ? C96 C97 1.521(7) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C97 H97C 0.9700 . ? C91B C92B 1.3902(10) . ? C92B C93B 1.3900(10) . ? C92B H92B 0.9400 . ? C93B C94B 1.3902(10) . ? C93B C96B 1.502(12) . ? C94B C95B 1.3899(10) . ? C94B H94B 0.9400 . ? C95B H95B 0.9400 . ? C96B C97B 1.524(7) . ? C96B H96C 0.9800 . ? C96B H96D 0.9800 . ? C97B H97D 0.9700 . ? C97B H97E 0.9700 . ? C97B H97F 0.9700 . ? N10 C101 1.3900 . ? N10 C105 1.3900 . ? C101 C102 1.3900 . ? C101 H101 0.9400 . ? C102 C103 1.3900 . ? C102 H102 0.9400 . ? C103 C104 1.3900 . ? C103 C106 1.502(10) . ? C104 C105 1.3900 . ? C104 H104 0.9400 . ? C106 C107 1.527(10) . ? C106 H10A 0.9800 . ? C106 H10B 0.9800 . ? C107 H10C 0.9700 . ? C107 H10D 0.9700 . ? C107 H10E 0.9700 . ? C01B C02B 1.3899(10) . ? C01B H01B 0.9400 . ? C02B C03B 1.3902(10) . ? C02B H02B 0.9400 . ? C03B C04B 1.3901(10) . ? C03B C06B 1.516(10) . ? C04B C05B 1.3900(10) . ? C04B H04B 0.9400 . ? C06B C07B 1.513(10) . ? C06B H06A 0.9800 . ? C06B H06B 0.9800 . ? C07B H07A 0.9700 . ? C07B H07B 0.9700 . ? C07B H07C 0.9700 . ? C121 C122 1.362(11) . ? C122 C123 1.396(11) . ? C122 H122 0.9400 . ? C123 C124 1.393(12) . ? C123 H123 0.9400 . ? C124 C125 1.368(12) . ? C124 H124 0.9400 . ? C141 C142 1.397(10) . ? C142 C143 1.349(13) . ? C142 H142 0.9400 . ? C143 C144 1.393(12) . ? C143 H143 0.9400 . ? C144 C145 1.387(10) . ? C144 H144 0.9400 . ? C161 C162 1.388(12) . ? C162 C163 1.385(11) . ? C162 H162 0.9400 . ? C163 C164 1.368(11) . ? C163 H163 0.9400 . ? C164 C165 1.413(10) . ? C164 H164 0.9400 . ? C181 C182 1.387(11) . ? C182 C183 1.382(10) . ? C182 H182 0.9400 . ? C183 C184 1.407(12) . ? C183 C186 1.499(12) . ? C184 C185 1.366(12) . ? C184 H184 0.9400 . ? C185 H185 0.9400 . ? C186 C187 1.534(13) . ? C186 H18A 0.9800 . ? C186 H18B 0.9800 . ? C187 H18C 0.9700 . ? C187 H18D 0.9700 . ? C187 H18E 0.9700 . ? B1 C201 1.632(12) . ? B1 C219 1.643(12) . ? B1 C207 1.657(12) . ? B1 C213 1.673(11) . ? C201 C202 1.398(11) . ? C201 C206 1.422(11) . ? C202 C203 1.384(12) . ? C202 H202 0.9400 . ? C203 C204 1.388(16) . ? C203 H203 0.9400 . ? C204 C205 1.380(16) . ? C204 H204 0.9400 . ? C205 C206 1.377(13) . ? C205 H205 0.9400 . ? C206 H206 0.9400 . ? C207 C208 1.395(11) . ? C207 C212 1.415(11) . ? C208 C209 1.377(12) . ? C208 H208 0.9400 . ? C209 C210 1.389(12) . ? C209 H209 0.9400 . ? C210 C211 1.365(13) . ? C210 H210 0.9400 . ? C211 C212 1.388(12) . ? C211 H211 0.9400 . ? C212 H212 0.9400 . ? C213 C214 1.385(12) . ? C213 C218 1.400(11) . ? C214 C215 1.401(12) . ? C214 H214 0.9400 . ? C215 C216 1.373(14) . ? C215 H215 0.9400 . ? C216 C217 1.352(13) . ? C216 H216 0.9400 . ? C217 C218 1.410(11) . ? C217 H217 0.9400 . ? C218 H218 0.9400 . ? C219 C220 1.402(10) . ? C219 C224 1.413(11) . ? C220 C221 1.389(12) . ? C220 H220 0.9400 . ? C221 C222 1.392(12) . ? C221 H221 0.9400 . ? C222 C223 1.372(12) . ? C222 H222 0.9400 . ? C223 C224 1.383(12) . ? C223 H223 0.9400 . ? C224 H224 0.9400 . ? B2 C231 1.665(6) . ? B2 C237 1.666(5) . ? B2 C225 1.667(5) . ? B2 C243 1.670(5) . ? B2 C31B 1.709(15) . ? C225 C226 1.3900 . ? C225 C230 1.3900 . ? C226 C227 1.3900 . ? C226 H226 0.9400 . ? C227 C228 1.3900 . ? C227 H227 0.9400 . ? C228 C229 1.3900 . ? C228 H228 0.9400 . ? C229 C230 1.3900 . ? C229 H229 0.9400 . ? C230 H230 0.9400 . ? C26B C27B 1.3900(19) . ? C26B H26B 0.9400 . ? C27B C28B 1.3905(19) . ? C27B H27B 0.9400 . ? C28B C29B 1.3904(19) . ? C28B H28B 0.9400 . ? C29B C30B 1.3898(19) . ? C29B H29B 0.9400 . ? C30B H30B 0.9400 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C232 H232 0.9400 . ? C233 C234 1.3900 . ? C233 H233 0.9400 . ? C234 C235 1.3900 . ? C234 H234 0.9400 . ? C235 C236 1.3900 . ? C235 H235 0.9400 . ? C236 H236 0.9400 . ? C31B C32B 1.3902(10) . ? C31B C36B 1.3902(10) . ? C32B C33B 1.3899(10) . ? C32B H32B 0.9400 . ? C33B C34B 1.3901(10) . ? C33B H33B 0.9400 . ? C34B C35B 1.3901(10) . ? C34B H34B 0.9400 . ? C35B C36B 1.3900(10) . ? C35B H35B 0.9400 . ? C36B H36B 0.9400 . ? C237 C238 1.395(11) . ? C237 C242 1.405(12) . ? C238 C239 1.402(13) . ? C238 H238 0.9400 . ? C239 C240 1.352(14) . ? C239 H239 0.9400 . ? C240 C241 1.399(13) . ? C240 H240 0.9400 . ? C241 C242 1.357(12) . ? C241 H241 0.9400 . ? C242 H242 0.9400 . ? C243 C244 1.3900 . ? C243 C248 1.3900 . ? C244 C245 1.3900 . ? C244 H244 0.9400 . ? C245 C246 1.3900 . ? C245 H245 0.9400 . ? C246 C247 1.3900 . ? C246 H246 0.9400 . ? C247 C248 1.3900 . ? C247 H247 0.9400 . ? C248 H248 0.9400 . ? C44B C45B 1.3902(10) . ? C44B H44B 0.9400 . ? C45B C46B 1.3902(10) . ? C45B H45B 0.9400 . ? C46B C47B 1.3902(11) . ? C46B H46B 0.9400 . ? C47B C48B 1.3903(10) . ? C47B H47B 0.9400 . ? C48B H48B 0.9400 . ? Cl1 C1S 1.725(6) . ? C1S Cl2 1.725(6) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? Cl1B C1SB 1.724(6) . ? C1SB Cl2B 1.724(6) . ? C1SB H1S3 0.9800 . ? C1SB H1S4 0.9800 . ? Cl3 C2S 1.719(7) . ? C2S Cl4 1.721(7) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? Cl3B C2SB 1.722(7) . ? C2SB Cl4B 1.722(7) . ? C2SB H2S3 0.9800 . ? C2SB H2S4 0.9800 . ? Cl5 C3S 1.722(7) . ? C3S Cl6 1.722(7) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? Cl7 C4S 0.37(3) 3_656 ? Cl7 Cl8 1.448(17) 3_656 ? Cl7 C4S 1.723(6) . ? Cl7 Cl7 2.02(3) 3_656 ? C4S Cl8 1.724(6) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? Cl8 Cl7 1.448(17) 3_656 ? 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 N16 Ni1 N14 94.5(3) . . ? N16 Ni1 N12 170.2(2) . . ? N14 Ni1 N12 95.3(3) . . ? N16 Ni1 N1 89.8(2) . . ? N14 Ni1 N1 95.3(2) . . ? N12 Ni1 N1 90.2(2) . . ? N16 Ni1 N9 87.9(2) . . ? N14 Ni1 N9 98.8(2) . . ? N12 Ni1 N9 89.7(2) . . ? N1 Ni1 N9 165.9(2) . . ? N16 Ni1 Ni2 85.34(17) . . ? N14 Ni1 Ni2 179.15(17) . . ? N12 Ni1 Ni2 84.93(17) . . ? N1 Ni1 Ni2 83.85(16) . . ? N9 Ni1 Ni2 82.06(13) . . ? N11 Ni2 N17 177.8(3) . . ? N11 Ni2 N8 89.5(3) . . ? N17 Ni2 N8 89.7(3) . . ? N11 Ni2 N2 90.1(3) . . ? N17 Ni2 N2 90.8(3) . . ? N8 Ni2 N2 177.6(3) . . ? N11 Ni2 Ni1 88.85(18) . . ? N17 Ni2 Ni1 89.19(18) . . ? N8 Ni2 Ni1 92.46(17) . . ? N2 Ni2 Ni1 89.91(17) . . ? N11 Ni2 Ni3 90.39(18) . . ? N17 Ni2 Ni3 91.57(18) . . ? N8 Ni2 Ni3 88.25(17) . . ? N2 Ni2 Ni3 89.37(17) . . ? Ni1 Ni2 Ni3 178.96(6) . . ? N5 Ni3 N7 94.4(2) . . ? N5 Ni3 N3 95.0(2) . . ? N7 Ni3 N3 170.6(2) . . ? N5 Ni3 N10 95.8(2) . . ? N7 Ni3 N10 88.7(2) . . ? N3 Ni3 N10 89.4(2) . . ? N5 Ni3 N18 97.6(2) . . ? N7 Ni3 N18 85.8(2) . . ? N3 Ni3 N18 93.8(2) . . ? N10 Ni3 N18 165.8(2) . . ? N5 Ni3 Ni2 179.23(19) . . ? N7 Ni3 Ni2 86.02(17) . . ? N3 Ni3 Ni2 84.60(17) . . ? N10 Ni3 Ni2 83.53(13) . . ? N18 Ni3 Ni2 83.06(16) . . ? C15 N1 C11 118.6(6) . . ? C15 N1 Ni1 119.8(5) . . ? C11 N1 Ni1 121.6(5) . . ? C31 N2 C15 122.7(6) . . ? C31 N2 Ni2 117.3(4) . . ? C15 N2 Ni2 119.6(5) . . ? C35 N3 C31 119.1(6) . . ? C35 N3 Ni3 121.2(4) . . ? C31 N3 Ni3 119.1(5) . . ? C35 N4 C51 130.7(7) . . ? C35 N4 H4 114.7 . . ? C51 N4 H4 114.7 . . ? C51 N5 C55 117.6(6) . . ? C51 N5 Ni3 121.0(4) . . ? C55 N5 Ni3 121.4(5) . . ? C55 N6 C71 132.5(7) . . ? C55 N6 H6 113.7 . . ? C71 N6 H6 113.7 . . ? C71 N7 C75 118.3(6) . . ? C71 N7 Ni3 121.4(5) . . ? C75 N7 Ni3 119.3(4) . . ? C91B N8 C75 119.3(6) . . ? C91B N8 C91 21.1(12) . . ? C75 N8 C91 130.5(9) . . ? C91B N8 Ni2 121.8(4) . . ? C75 N8 Ni2 118.0(4) . . ? C91 N8 Ni2 110.7(9) . . ? C05B N11 C121 122.4(9) . . ? C05B N11 C105 12.8(19) . . ? C121 N11 C105 114.9(7) . . ? C05B N11 Ni2 116.4(8) . . ? C121 N11 Ni2 120.9(5) . . ? C105 N11 Ni2 124.0(5) . . ? C121 N12 C125 116.9(7) . . ? C121 N12 Ni1 121.3(5) . . ? C125 N12 Ni1 121.8(6) . . ? C141 N13 C125 134.5(6) . . ? C141 N13 H13 112.8 . . ? C125 N13 H13 112.8 . . ? C145 N14 C141 119.1(6) . . ? C145 N14 Ni1 121.1(5) . . ? C141 N14 Ni1 119.4(6) . . ? C145 N15 C161 131.9(7) . . ? C145 N15 H15 114.1 . . ? C161 N15 H15 114.1 . . ? C161 N16 C165 118.0(7) . . ? C161 N16 Ni1 122.0(5) . . ? C165 N16 Ni1 119.2(5) . . ? C165 N17 C181 119.7(7) . . ? C165 N17 Ni2 117.4(4) . . ? C181 N17 Ni2 122.0(6) . . ? C181 N18 C185 117.8(7) . . ? C181 N18 Ni3 121.0(5) . . ? C185 N18 Ni3 120.8(6) . . ? N1 C11 C12 123.4(8) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 119.0(8) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 117.7(7) . . ? C14 C13 C16 121.1(8) . . ? C12 C13 C16 121.3(8) . . ? C13 C14 C15 121.0(8) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? N1 C15 N2 116.1(6) . . ? N1 C15 C14 120.3(7) . . ? N2 C15 C14 123.4(7) . . ? C17 C16 C13 114.8(9) . . ? C17 C16 H16C 108.6 . . ? C13 C16 H16C 108.6 . . ? C17 C16 H16D 108.6 . . ? C13 C16 H16D 108.6 . . ? H16C C16 H16D 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C31 N3 116.1(6) . . ? N2 C31 C32 123.9(6) . . ? N3 C31 C32 119.7(8) . . ? C33 C32 C31 119.3(7) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 121.5(7) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 115.7(8) . . ? C33 C34 H34 122.1 . . ? C35 C34 H34 122.1 . . ? N3 C35 C34 124.6(7) . . ? N3 C35 N4 119.4(6) . . ? C34 C35 N4 115.8(8) . . ? N5 C51 C52 123.6(6) . . ? N5 C51 N4 120.9(6) . . ? C52 C51 N4 115.5(7) . . ? C53 C52 C51 117.3(8) . . ? C53 C52 H52 121.3 . . ? C51 C52 H52 121.3 . . ? C54 C53 C52 119.5(7) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 119.7(7) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? N5 C55 C54 122.3(7) . . ? N5 C55 N6 119.3(6) . . ? C54 C55 N6 118.4(6) . . ? N7 C71 C72 123.3(7) . . ? N7 C71 N6 118.3(7) . . ? C72 C71 N6 118.5(6) . . ? C71 C72 C73 118.3(7) . . ? C71 C72 H72 120.9 . . ? C73 C72 H72 120.9 . . ? C74 C73 C72 119.9(8) . . ? C74 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? C75 C74 C73 118.6(7) . . ? C75 C74 H74 120.7 . . ? C73 C74 H74 120.7 . . ? N7 C75 N8 115.0(6) . . ? N7 C75 C74 121.7(7) . . ? N8 C75 C74 123.2(7) . . ? C91 N9 C95 120.0 . . ? C91 N9 Ni1 119.6(8) . . ? C95 N9 Ni1 120.4(8) . . ? C92 C91 N9 120.0 . . ? C92 C91 N8 120.1(11) . . ? N9 C91 N8 112.2(15) . . ? C91 C92 C93 120.0 . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 C96 114(4) . . ? C92 C93 C96 126(4) . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C94 C95 N9 120.0 . . ? C94 C95 H95 120.0 . . ? N9 C95 H95 120.0 . . ? C93 C96 C97 107.9(8) . . ? C93 C96 H96A 110.1 . . ? C97 C96 H96A 110.1 . . ? C93 C96 H96B 110.1 . . ? C97 C96 H96B 110.1 . . ? H96A C96 H96B 108.4 . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C92B C91B N8 124.4(7) . . ? C93B C92B C91B 120.03(13) . . ? C93B C92B H92B 120.0 . . ? C91B C92B H92B 120.0 . . ? C92B C93B C94B 119.99(13) . . ? C92B C93B C96B 120(2) . . ? C94B C93B C96B 120(2) . . ? C95B C94B C93B 119.91(13) . . ? C95B C94B H94B 120.0 . . ? C93B C94B H94B 120.0 . . ? C94B C95B H95B 120.0 . . ? C93B C96B C97B 107.9(10) . . ? C93B C96B H96C 110.1 . . ? C97B C96B H96C 110.1 . . ? C93B C96B H96D 110.1 . . ? C97B C96B H96D 110.1 . . ? H96C C96B H96D 108.4 . . ? C96B C97B H97D 109.5 . . ? C96B C97B H97E 109.5 . . ? H97D C97B H97E 109.5 . . ? C96B C97B H97F 109.5 . . ? H97D C97B H97F 109.5 . . ? H97E C97B H97F 109.5 . . ? C101 N10 C105 120.0 . . ? C101 N10 Ni3 117.0(7) . . ? C105 N10 Ni3 122.6(7) . . ? C102 C101 N10 120.0 . . ? C102 C101 H101 120.0 . . ? N10 C101 H101 120.0 . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C104 C103 C102 120.0 . . ? C104 C103 C106 114(2) . . ? C102 C103 C106 125(2) . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 N10 120.0 . . ? C104 C105 N11 127.1(10) . . ? N10 C105 N11 108.6(10) . . ? C103 C106 C107 106(3) . . ? C103 C106 H10A 110.6 . . ? C107 C106 H10A 110.6 . . ? C103 C106 H10B 110.6 . . ? C107 C106 H10B 110.6 . . ? H10A C106 H10B 108.8 . . ? C106 C107 H10C 109.5 . . ? C106 C107 H10D 109.5 . . ? H10C C107 H10D 109.5 . . ? C106 C107 H10E 109.5 . . ? H10C C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C02B C01B H01B 120.0 . . ? C01B C02B C03B 119.97(13) . . ? C01B C02B H02B 120.0 . . ? C03B C02B H02B 120.0 . . ? C04B C03B C02B 119.93(13) . . ? C04B C03B C06B 126(2) . . ? C02B C03B C06B 114(2) . . ? C05B C04B C03B 120.05(13) . . ? C05B C04B H04B 120.0 . . ? C03B C04B H04B 120.0 . . ? N11 C05B C04B 122.8(10) . . ? C07B C06B C03B 113(3) . . ? C07B C06B H06A 109.1 . . ? C03B C06B H06A 109.1 . . ? C07B C06B H06B 109.1 . . ? C03B C06B H06B 109.1 . . ? H06A C06B H06B 107.8 . . ? C06B C07B H07A 109.5 . . ? C06B C07B H07B 109.5 . . ? H07A C07B H07B 109.5 . . ? C06B C07B H07C 109.5 . . ? H07A C07B H07C 109.5 . . ? H07B C07B H07C 109.5 . . ? N12 C121 C122 121.9(6) . . ? N12 C121 N11 112.9(7) . . ? C122 C121 N11 125.0(7) . . ? C121 C122 C123 120.9(8) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C124 C123 C122 118.2(9) . . ? C124 C123 H123 120.9 . . ? C122 C123 H123 120.9 . . ? C125 C124 C123 118.6(7) . . ? C125 C124 H124 120.7 . . ? C123 C124 H124 120.7 . . ? C124 C125 N12 123.5(8) . . ? C124 C125 N13 119.3(6) . . ? N12 C125 N13 117.2(8) . . ? N14 C141 N13 121.0(7) . . ? N14 C141 C142 120.5(8) . . ? N13 C141 C142 118.5(7) . . ? C143 C142 C141 119.4(8) . . ? C143 C142 H142 120.3 . . ? C141 C142 H142 120.3 . . ? C142 C143 C144 120.4(8) . . ? C142 C143 H143 119.8 . . ? C144 C143 H143 119.8 . . ? C145 C144 C143 117.8(9) . . ? C145 C144 H144 121.1 . . ? C143 C144 H144 121.1 . . ? N14 C145 C144 122.8(7) . . ? N14 C145 N15 121.2(6) . . ? C144 C145 N15 116.0(8) . . ? N16 C161 C162 124.5(7) . . ? N16 C161 N15 118.4(8) . . ? C162 C161 N15 117.1(8) . . ? C163 C162 C161 117.0(8) . . ? C163 C162 H162 121.5 . . ? C161 C162 H162 121.5 . . ? C164 C163 C162 120.9(8) . . ? C164 C163 H163 119.5 . . ? C162 C163 H163 119.5 . . ? C163 C164 C165 119.8(7) . . ? C163 C164 H164 120.1 . . ? C165 C164 H164 120.1 . . ? N17 C165 N16 115.0(6) . . ? N17 C165 C164 125.2(6) . . ? N16 C165 C164 119.7(7) . . ? N18 C181 N17 114.4(7) . . ? N18 C181 C182 120.6(6) . . ? N17 C181 C182 124.9(7) . . ? C183 C182 C181 122.6(8) . . ? C183 C182 H182 118.7 . . ? C181 C182 H182 118.7 . . ? C182 C183 C184 115.8(8) . . ? C182 C183 C186 121.1(8) . . ? C184 C183 C186 123.0(7) . . ? C185 C184 C183 120.9(7) . . ? C185 C184 H184 119.6 . . ? C183 C184 H184 119.6 . . ? C184 C185 N18 122.0(9) . . ? C184 C185 H185 119.0 . . ? N18 C185 H185 119.0 . . ? C183 C186 C187 112.2(7) . . ? C183 C186 H18A 109.2 . . ? C187 C186 H18A 109.2 . . ? C183 C186 H18B 109.2 . . ? C187 C186 H18B 109.2 . . ? H18A C186 H18B 107.9 . . ? C186 C187 H18C 109.5 . . ? C186 C187 H18D 109.5 . . ? H18C C187 H18D 109.5 . . ? C186 C187 H18E 109.5 . . ? H18C C187 H18E 109.5 . . ? H18D C187 H18E 109.5 . . ? C201 B1 C219 109.8(7) . . ? C201 B1 C207 109.0(7) . . ? C219 B1 C207 113.1(6) . . ? C201 B1 C213 108.9(6) . . ? C219 B1 C213 110.7(6) . . ? C207 B1 C213 105.1(6) . . ? C202 C201 C206 113.5(8) . . ? C202 C201 B1 123.1(7) . . ? C206 C201 B1 123.2(7) . . ? C203 C202 C201 124.2(9) . . ? C203 C202 H202 117.9 . . ? C201 C202 H202 117.9 . . ? C202 C203 C204 119.3(10) . . ? C202 C203 H203 120.3 . . ? C204 C203 H203 120.3 . . ? C205 C204 C203 119.6(10) . . ? C205 C204 H204 120.2 . . ? C203 C204 H204 120.2 . . ? C206 C205 C204 119.6(10) . . ? C206 C205 H205 120.2 . . ? C204 C205 H205 120.2 . . ? C205 C206 C201 123.8(9) . . ? C205 C206 H206 118.1 . . ? C201 C206 H206 118.1 . . ? C208 C207 C212 113.4(8) . . ? C208 C207 B1 122.0(7) . . ? C212 C207 B1 124.4(7) . . ? C209 C208 C207 124.1(8) . . ? C209 C208 H208 118.0 . . ? C207 C208 H208 118.0 . . ? C208 C209 C210 120.5(9) . . ? C208 C209 H209 119.8 . . ? C210 C209 H209 119.8 . . ? C211 C210 C209 117.9(9) . . ? C211 C210 H210 121.0 . . ? C209 C210 H210 121.0 . . ? C210 C211 C212 121.1(9) . . ? C210 C211 H211 119.4 . . ? C212 C211 H211 119.4 . . ? C211 C212 C207 122.9(9) . . ? C211 C212 H212 118.6 . . ? C207 C212 H212 118.6 . . ? C214 C213 C218 114.2(7) . . ? C214 C213 B1 120.5(7) . . ? C218 C213 B1 125.3(7) . . ? C213 C214 C215 125.0(9) . . ? C213 C214 H214 117.5 . . ? C215 C214 H214 117.5 . . ? C216 C215 C214 118.1(10) . . ? C216 C215 H215 120.9 . . ? C214 C215 H215 120.9 . . ? C217 C216 C215 120.0(8) . . ? C217 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C216 C217 C218 120.9(9) . . ? C216 C217 H217 119.6 . . ? C218 C217 H217 119.6 . . ? C213 C218 C217 121.8(9) . . ? C213 C218 H218 119.1 . . ? C217 C218 H218 119.1 . . ? C220 C219 C224 113.0(8) . . ? C220 C219 B1 123.9(7) . . ? C224 C219 B1 123.1(7) . . ? C221 C220 C219 124.3(8) . . ? C221 C220 H220 117.8 . . ? C219 C220 H220 117.8 . . ? C220 C221 C222 119.3(8) . . ? C220 C221 H221 120.4 . . ? C222 C221 H221 120.4 . . ? C223 C222 C221 119.2(9) . . ? C223 C222 H222 120.4 . . ? C221 C222 H222 120.4 . . ? C222 C223 C224 119.9(9) . . ? C222 C223 H223 120.0 . . ? C224 C223 H223 120.0 . . ? C223 C224 C219 124.2(8) . . ? C223 C224 H224 117.9 . . ? C219 C224 H224 117.9 . . ? C231 B2 C237 110.4(9) . . ? C231 B2 C225 114.3(11) . . ? C237 B2 C225 106.4(6) . . ? C231 B2 C243 106.1(9) . . ? C237 B2 C243 108.5(5) . . ? C225 B2 C243 111.1(6) . . ? C231 B2 C31B 5.6(14) . . ? C237 B2 C31B 115.7(9) . . ? C225 B2 C31B 110.1(7) . . ? C243 B2 C31B 105.1(7) . . ? C226 C225 C230 120.0 . . ? C226 C225 B2 142(2) . . ? C230 C225 B2 97(2) . . ? C225 C226 C227 120.0 . . ? C225 C226 H226 120.0 . . ? C227 C226 H226 120.0 . . ? C226 C227 C228 120.0 . . ? C226 C227 H227 120.0 . . ? C228 C227 H227 120.0 . . ? C229 C228 C227 120.0 . . ? C229 C228 H228 120.0 . . ? C227 C228 H228 120.0 . . ? C230 C229 C228 120.0 . . ? C230 C229 H229 120.0 . . ? C228 C229 H229 120.0 . . ? C229 C230 C225 120.0 . . ? C229 C230 H230 120.0 . . ? C225 C230 H230 120.0 . . ? C27B C26B H26B 120.0 . . ? C26B C27B C28B 120.0(3) . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C29B C28B C27B 119.8(3) . . ? C29B C28B H28B 120.1 . . ? C27B C28B H28B 120.1 . . ? C30B C29B C28B 119.9(3) . . ? C30B C29B H29B 120.1 . . ? C28B C29B H29B 120.1 . . ? C29B C30B H30B 119.9 . . ? C232 C231 C236 120.0 . . ? C232 C231 B2 115.4(15) . . ? C236 C231 B2 122.2(15) . . ? C233 C232 C231 120.0 . . ? C233 C232 H232 120.0 . . ? C231 C232 H232 120.0 . . ? C232 C233 C234 120.0 . . ? C232 C233 H233 120.0 . . ? C234 C233 H233 120.0 . . ? C233 C234 C235 120.0 . . ? C233 C234 H234 120.0 . . ? C235 C234 H234 120.0 . . ? C234 C235 C236 120.0 . . ? C234 C235 H235 120.0 . . ? C236 C235 H235 120.0 . . ? C235 C236 C231 120.0 . . ? C235 C236 H236 120.0 . . ? C231 C236 H236 120.0 . . ? C32B C31B C36B 119.89(13) . . ? C32B C31B B2 120.8(9) . . ? C36B C31B B2 118.8(9) . . ? C33B C32B C31B 120.05(13) . . ? C33B C32B H32B 120.0 . . ? C31B C32B H32B 120.0 . . ? C32B C33B C34B 120.01(13) . . ? C32B C33B H33B 120.0 . . ? C34B C33B H33B 120.0 . . ? C35B C34B C33B 119.92(14) . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C36B C35B C34B 120.02(13) . . ? C36B C35B H35B 120.0 . . ? C34B C35B H35B 120.0 . . ? C35B C36B C31B 120.05(13) . . ? C35B C36B H36B 120.0 . . ? C31B C36B H36B 120.0 . . ? C238 C237 C242 115.3(8) . . ? C238 C237 B2 125.8(8) . . ? C242 C237 B2 118.7(7) . . ? C237 C238 C239 121.5(9) . . ? C237 C238 H238 119.3 . . ? C239 C238 H238 119.3 . . ? C240 C239 C238 121.2(9) . . ? C240 C239 H239 119.4 . . ? C238 C239 H239 119.4 . . ? C239 C240 C241 118.6(10) . . ? C239 C240 H240 120.7 . . ? C241 C240 H240 120.7 . . ? C242 C241 C240 120.2(10) . . ? C242 C241 H241 119.9 . . ? C240 C241 H241 119.9 . . ? C241 C242 C237 123.2(9) . . ? C241 C242 H242 118.4 . . ? C237 C242 H242 118.4 . . ? C244 C243 C248 120.0 . . ? C244 C243 B2 121.0(6) . . ? C248 C243 B2 118.9(6) . . ? C245 C244 C243 120.0 . . ? C245 C244 H244 120.0 . . ? C243 C244 H244 120.0 . . ? C244 C245 C246 120.0 . . ? C244 C245 H245 120.0 . . ? C246 C245 H245 120.0 . . ? C245 C246 C247 120.0 . . ? C245 C246 H246 120.0 . . ? C247 C246 H246 120.0 . . ? C248 C247 C246 120.0 . . ? C248 C247 H247 120.0 . . ? C246 C247 H247 120.0 . . ? C247 C248 C243 120.0 . . ? C247 C248 H248 120.0 . . ? C243 C248 H248 120.0 . . ? C45B C44B H44B 120.0 . . ? C46B C45B C44B 119.93(15) . . ? C46B C45B H45B 120.0 . . ? C44B C45B H45B 120.0 . . ? C47B C46B C45B 119.91(18) . . ? C47B C46B H46B 120.0 . . ? C45B C46B H46B 120.0 . . ? C46B C47B C48B 119.92(18) . . ? C46B C47B H47B 120.0 . . ? C48B C47B H47B 120.0 . . ? C47B C48B H48B 120.0 . . ? Cl1 C1S Cl2 116.7(6) . . ? Cl1 C1S H1S1 108.1 . . ? Cl2 C1S H1S1 108.1 . . ? Cl1 C1S H1S2 108.1 . . ? Cl2 C1S H1S2 108.1 . . ? H1S1 C1S H1S2 107.3 . . ? Cl1B C1SB Cl2B 116.4(8) . . ? Cl1B C1SB H1S3 108.2 . . ? Cl2B C1SB H1S3 108.2 . . ? Cl1B C1SB H1S4 108.2 . . ? Cl2B C1SB H1S4 108.2 . . ? H1S3 C1SB H1S4 107.3 . . ? Cl3 C2S Cl4 116.9(7) . . ? Cl3 C2S H2S1 108.1 . . ? Cl4 C2S H2S1 108.1 . . ? Cl3 C2S H2S2 108.1 . . ? Cl4 C2S H2S2 108.1 . . ? H2S1 C2S H2S2 107.3 . . ? Cl4B C2SB Cl3B 116.6(8) . . ? Cl4B C2SB H2S3 108.2 . . ? Cl3B C2SB H2S3 108.2 . . ? Cl4B C2SB H2S4 108.2 . . ? Cl3B C2SB H2S4 108.2 . . ? H2S3 C2SB H2S4 107.3 . . ? Cl5 C3S Cl6 116.6(8) . . ? Cl5 C3S H3S1 108.2 . . ? Cl6 C3S H3S1 108.2 . . ? Cl5 C3S H3S2 108.2 . . ? Cl6 C3S H3S2 108.2 . . ? H3S1 C3S H3S2 107.3 . . ? C4S Cl7 Cl8 133(5) 3_656 3_656 ? C4S Cl7 C4S 41(5) 3_656 . ? Cl8 Cl7 C4S 110.5(9) 3_656 . ? C4S Cl7 Cl7 34(4) 3_656 3_656 ? Cl8 Cl7 Cl7 115.2(13) 3_656 3_656 ? C4S Cl7 Cl7 7.0(9) . 3_656 ? Cl7 C4S Cl8 117.2(8) . . ? Cl7 C4S H4S1 108.0 . . ? Cl8 C4S H4S1 108.0 . . ? Cl7 C4S H4S2 108.0 . . ? Cl8 C4S H4S2 108.0 . . ? H4S1 C4S H4S2 107.2 . . ? Cl7 Cl8 C4S 9.0(13) 3_656 . ? 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 N1 Ni1 Ni3 N3 -48.3(3) . . . . ? N7 Ni3 Ni1 N9 -46.2(3) . . . . ? N10 Ni3 Ni1 N12 -47.5(2) . . . . ? N16 Ni1 Ni3 N18 -43.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.902 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.104 data_cif9 _database_code_depnum_ccdc_archive 'CCDC 618490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(mpeptea)2(BPh4)2,3CH3COCH3 _chemical_melting_point ? _chemical_formula_moiety Ni3(C27H23)2(BC24H20)2,3CH3COCH3 _chemical_formula_sum 'C111 H105 B2 N18 Ni3 O3' _chemical_formula_weight 1936.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.708(5) _cell_length_b 15.112(3) _cell_length_c 26.789(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.406(3) _cell_angle_gamma 90.00 _cell_volume 9816(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 17222 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4060 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9001 _exptl_absorpt_correction_T_max 0.9167 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50931 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17222 _reflns_number_gt 9779 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0706P)^2^+13.5516P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17222 _refine_ls_number_parameters 1214 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.15247(2) 0.41241(4) 0.10348(2) 0.03036(17) Uani 1 1 d . . . Ni3 Ni 0.30255(2) 0.60246(4) 0.12056(2) 0.03267(17) Uani 1 1 d . . . Ni2 Ni 0.22707(2) 0.50800(4) 0.11162(2) 0.02789(16) Uani 1 1 d . . . N1 N 0.24629(16) 0.6606(3) 0.05173(15) 0.0348(10) Uani 1 1 d . . . N2 N 0.19620(15) 0.5317(2) 0.03816(15) 0.0309(9) Uani 1 1 d . . . N3 N 0.14723(15) 0.4014(2) 0.02743(16) 0.0340(10) Uani 1 1 d . . . N4 N 0.10793(17) 0.2605(3) 0.02632(18) 0.0425(11) Uani 1 1 d . . . N5 N 0.08895(15) 0.3332(2) 0.09641(16) 0.0350(10) Uani 1 1 d . . . N6 N 0.07214(16) 0.4097(3) 0.16654(19) 0.0444(11) Uani 1 1 d . . . N7 N 0.16624(15) 0.4386(2) 0.18049(16) 0.0322(9) Uani 1 1 d . . . N8 N 0.25385(14) 0.4809(2) 0.18417(15) 0.0307(9) Uani 1 1 d . . . N9 N 0.34130(15) 0.5222(3) 0.18683(15) 0.0338(10) Uani 1 1 d . . . N10 N 0.21422(16) 0.3150(3) 0.12294(16) 0.0356(10) Uani 1 1 d . . . N11 N 0.26931(15) 0.4143(3) 0.09827(16) 0.0332(10) Uani 1 1 d . . . N12 N 0.32395(15) 0.5153(3) 0.07469(16) 0.0364(10) Uani 1 1 d . . . N13 N 0.36918(18) 0.6307(3) 0.04609(18) 0.0488(12) Uani 1 1 d . . . N14 N 0.36650(16) 0.6820(3) 0.12858(17) 0.0383(10) Uani 1 1 d . . . N15 N 0.36244(16) 0.7270(3) 0.21119(16) 0.0448(11) Uani 1 1 d . . . N16 N 0.27183(15) 0.6758(2) 0.16640(15) 0.0321(9) Uani 1 1 d . . . N17 N 0.18875(14) 0.6062(2) 0.12590(15) 0.0270(9) Uani 1 1 d . . . N18 N 0.10701(14) 0.5315(2) 0.08688(15) 0.0302(9) Uani 1 1 d . . . C1 C 0.1084(3) 0.1705(4) 0.0042(3) 0.0682(19) Uani 1 1 d . . . H1A H 0.0966 0.1277 0.0253 0.102 Uiso 1 1 calc R . . H1B H 0.1454 0.1562 0.0049 0.102 Uiso 1 1 calc R . . H1C H 0.0833 0.1688 -0.0320 0.102 Uiso 1 1 calc R . . C2 C 0.0260(2) 0.4434(4) 0.1823(3) 0.0675(19) Uani 1 1 d . . . H2A H -0.0087 0.4232 0.1572 0.101 Uiso 1 1 calc R . . H2B H 0.0267 0.5076 0.1827 0.101 Uiso 1 1 calc R . . H2C H 0.0295 0.4216 0.2173 0.101 Uiso 1 1 calc R . . C3 C 0.3771(3) 0.6636(5) -0.0027(3) 0.085(2) Uani 1 1 d . . . H3A H 0.3856 0.7263 0.0009 0.128 Uiso 1 1 calc R . . H3B H 0.3436 0.6542 -0.0325 0.128 Uiso 1 1 calc R . . H3C H 0.4073 0.6319 -0.0086 0.128 Uiso 1 1 calc R . . C4 C 0.4004(2) 0.7411(4) 0.2643(2) 0.0672(18) Uani 1 1 d . . . H4A H 0.4380 0.7390 0.2639 0.101 Uiso 1 1 calc R . . H4B H 0.3953 0.6952 0.2875 0.101 Uiso 1 1 calc R . . H4C H 0.3935 0.7985 0.2770 0.101 Uiso 1 1 calc R . . C11 C 0.2532(2) 0.7455(3) 0.0385(2) 0.0434(13) Uani 1 1 d . . . H11A H 0.2839 0.7770 0.0602 0.052 Uiso 1 1 calc R . . C12 C 0.2177(2) 0.7873(4) -0.0046(2) 0.0509(15) Uani 1 1 d . . . H12A H 0.2246 0.8453 -0.0134 0.061 Uiso 1 1 calc R . . C13 C 0.1715(2) 0.7415(4) -0.0348(2) 0.0526(15) Uani 1 1 d . . . H13A H 0.1459 0.7692 -0.0641 0.063 Uiso 1 1 calc R . . C14 C 0.1629(2) 0.6564(3) -0.0224(2) 0.0427(13) Uani 1 1 d . . . H14A H 0.1311 0.6255 -0.0427 0.051 Uiso 1 1 calc R . . C15 C 0.2021(2) 0.6155(3) 0.02116(19) 0.0326(11) Uani 1 1 d . . . C21 C 0.16822(19) 0.4658(3) 0.0042(2) 0.0344(12) Uani 1 1 d . . . C22 C 0.1637(2) 0.4592(4) -0.0490(2) 0.0447(13) Uani 1 1 d . . . H22A H 0.1782 0.5037 -0.0651 0.054 Uiso 1 1 calc R . . C23 C 0.1381(2) 0.3875(4) -0.0773(2) 0.0537(15) Uani 1 1 d . . . H23A H 0.1340 0.3832 -0.1134 0.064 Uiso 1 1 calc R . . C24 C 0.1183(2) 0.3216(4) -0.0536(2) 0.0525(15) Uani 1 1 d . . . H24A H 0.1009 0.2718 -0.0731 0.063 Uiso 1 1 calc R . . C25 C 0.1242(2) 0.3293(3) -0.0009(2) 0.0408(13) Uani 1 1 d . . . C31 C 0.0757(2) 0.2709(3) 0.0583(2) 0.0427(13) Uani 1 1 d . . . C32 C 0.0297(2) 0.2176(4) 0.0515(3) 0.0600(17) Uani 1 1 d . . . H32A H 0.0198 0.1742 0.0249 0.072 Uiso 1 1 calc R . . C33 C -0.0009(3) 0.2294(4) 0.0845(3) 0.0654(18) Uani 1 1 d . . . H33A H -0.0321 0.1939 0.0799 0.079 Uiso 1 1 calc R . . C34 C 0.0128(2) 0.2906(4) 0.1231(3) 0.0551(16) Uani 1 1 d . . . H34A H -0.0082 0.2974 0.1456 0.066 Uiso 1 1 calc R . . C35 C 0.0588(2) 0.3437(3) 0.1291(2) 0.0399(13) Uani 1 1 d . . . C41 C 0.1250(2) 0.4352(3) 0.2006(2) 0.0388(13) Uani 1 1 d . . . C42 C 0.1329(2) 0.4589(3) 0.2522(2) 0.0454(14) Uani 1 1 d . . . H42A H 0.1040 0.4550 0.2663 0.054 Uiso 1 1 calc R . . C43 C 0.1841(2) 0.4882(4) 0.2826(2) 0.0514(15) Uani 1 1 d . . . H43A H 0.1904 0.5040 0.3180 0.062 Uiso 1 1 calc R . . C44 C 0.2260(2) 0.4949(3) 0.2622(2) 0.0436(13) Uani 1 1 d . . . H44A H 0.2607 0.5167 0.2831 0.052 Uiso 1 1 calc R . . C45 C 0.21668(19) 0.4693(3) 0.2106(2) 0.0328(11) Uani 1 1 d . . . C51 C 0.31007(19) 0.4763(3) 0.2100(2) 0.0362(12) Uani 1 1 d . . . C52 C 0.3352(2) 0.4229(4) 0.2538(2) 0.0525(15) Uani 1 1 d . . . H52A H 0.3135 0.3904 0.2696 0.063 Uiso 1 1 calc R . . C53 C 0.3914(2) 0.4179(5) 0.2738(3) 0.0681(19) Uani 1 1 d . . . H53A H 0.4086 0.3826 0.3037 0.082 Uiso 1 1 calc R . . C54 C 0.4231(2) 0.4650(4) 0.2501(3) 0.0618(18) Uani 1 1 d . . . H54A H 0.4618 0.4623 0.2633 0.074 Uiso 1 1 calc R . . C55 C 0.39638(19) 0.5150(4) 0.2072(2) 0.0457(14) Uani 1 1 d . . . H55A H 0.4177 0.5465 0.1907 0.055 Uiso 1 1 calc R . . C61 C 0.2072(2) 0.2382(4) 0.1443(2) 0.0460(14) Uani 1 1 d . . . H61A H 0.1721 0.2256 0.1462 0.055 Uiso 1 1 calc R . . C62 C 0.2480(2) 0.1767(4) 0.1636(2) 0.0561(16) Uani 1 1 d . . . H62A H 0.2411 0.1231 0.1780 0.067 Uiso 1 1 calc R . . C63 C 0.2991(2) 0.1953(4) 0.1612(2) 0.0573(16) Uani 1 1 d . . . H63A H 0.3284 0.1552 0.1749 0.069 Uiso 1 1 calc R . . C64 C 0.3073(2) 0.2731(3) 0.1386(2) 0.0432(13) Uani 1 1 d . . . H64A H 0.3423 0.2862 0.1365 0.052 Uiso 1 1 calc R . . C65 C 0.26418(18) 0.3325(3) 0.1188(2) 0.0339(12) Uani 1 1 d . . . C71 C 0.30617(19) 0.4313(3) 0.0724(2) 0.0360(12) Uani 1 1 d . . . C72 C 0.3211(2) 0.3696(4) 0.0411(2) 0.0475(14) Uani 1 1 d . . . H72A H 0.3072 0.3117 0.0378 0.057 Uiso 1 1 calc R . . C73 C 0.3562(2) 0.3944(4) 0.0152(2) 0.0570(16) Uani 1 1 d . . . H73A H 0.3682 0.3523 -0.0044 0.068 Uiso 1 1 calc R . . C74 C 0.3742(2) 0.4802(4) 0.0175(2) 0.0531(15) Uani 1 1 d . . . H74A H 0.3982 0.4975 -0.0005 0.064 Uiso 1 1 calc R . . C75 C 0.3562(2) 0.5402(4) 0.0468(2) 0.0421(13) Uani 1 1 d . . . C81 C 0.3908(2) 0.6830(4) 0.0909(2) 0.0449(14) Uani 1 1 d . . . C82 C 0.4356(2) 0.7370(4) 0.0960(3) 0.0582(17) Uani 1 1 d . . . H82A H 0.4532 0.7370 0.0703 0.070 Uiso 1 1 calc R . . C83 C 0.4536(2) 0.7901(4) 0.1392(3) 0.0642(18) Uani 1 1 d . . . H83A H 0.4832 0.8288 0.1425 0.077 Uiso 1 1 calc R . . C84 C 0.4300(2) 0.7893(4) 0.1783(3) 0.0549(16) Uani 1 1 d . . . H84A H 0.4435 0.8255 0.2083 0.066 Uiso 1 1 calc R . . C85 C 0.3857(2) 0.7329(3) 0.1717(2) 0.0418(13) Uani 1 1 d . . . C91 C 0.3054(2) 0.7275(3) 0.2046(2) 0.0394(13) Uani 1 1 d . . . C92 C 0.2863(2) 0.7765(3) 0.2377(2) 0.0462(14) Uani 1 1 d . . . H92A H 0.3098 0.8149 0.2628 0.055 Uiso 1 1 calc R . . C93 C 0.2313(2) 0.7681(4) 0.2335(2) 0.0471(14) Uani 1 1 d . . . H93A H 0.2174 0.8007 0.2562 0.057 Uiso 1 1 calc R . . C94 C 0.1972(2) 0.7128(3) 0.1965(2) 0.0384(12) Uani 1 1 d . . . H94A H 0.1602 0.7057 0.1944 0.046 Uiso 1 1 calc R . . C95 C 0.21771(18) 0.6674(3) 0.16207(19) 0.0302(11) Uani 1 1 d . . . C101 C 0.13273(19) 0.6099(3) 0.10307(18) 0.0287(11) Uani 1 1 d . . . C102 C 0.1020(2) 0.6876(3) 0.0945(2) 0.0405(13) Uani 1 1 d . . . H10A H 0.1198 0.7422 0.1049 0.049 Uiso 1 1 calc R . . C103 C 0.0461(2) 0.6847(4) 0.0709(2) 0.0491(15) Uani 1 1 d . . . H10B H 0.0253 0.7372 0.0654 0.059 Uiso 1 1 calc R . . C104 C 0.0200(2) 0.6042(3) 0.0553(2) 0.0459(14) Uani 1 1 d . . . H10C H -0.0185 0.6004 0.0403 0.055 Uiso 1 1 calc R . . C105 C 0.05215(19) 0.5313(3) 0.06240(19) 0.0368(12) Uani 1 1 d . . . H10D H 0.0350 0.4771 0.0494 0.044 Uiso 1 1 calc R . . B1 B 0.0436(2) 0.9522(4) 0.1762(2) 0.0369(14) Uani 1 1 d . . . B2 B 0.4065(3) 1.0339(5) 0.3350(3) 0.0513(17) Uani 1 1 d . . . C111 C 0.0726(2) 0.9360(3) 0.1310(2) 0.0385(12) Uani 1 1 d . . . C112 C 0.0463(2) 0.9446(3) 0.0769(2) 0.0499(15) Uani 1 1 d . . . H11B H 0.0081 0.9550 0.0646 0.060 Uiso 1 1 calc R . . C113 C 0.0733(3) 0.9384(4) 0.0400(2) 0.0556(16) Uani 1 1 d . . . H11C H 0.0537 0.9445 0.0037 0.067 Uiso 1 1 calc R . . C114 C 0.1289(3) 0.9235(4) 0.0571(3) 0.0609(17) Uani 1 1 d . . . H11D H 0.1479 0.9204 0.0326 0.073 Uiso 1 1 calc R . . C115 C 0.1573(3) 0.9130(4) 0.1105(3) 0.0557(16) Uani 1 1 d . . . H11E H 0.1955 0.9022 0.1225 0.067 Uiso 1 1 calc R . . C116 C 0.1289(2) 0.9185(3) 0.1462(2) 0.0451(14) Uani 1 1 d . . . H11F H 0.1484 0.9101 0.1824 0.054 Uiso 1 1 calc R . . C121 C -0.0240(2) 0.9470(3) 0.1500(2) 0.0407(13) Uani 1 1 d . . . C122 C -0.0563(2) 0.8761(3) 0.15370(19) 0.0367(12) Uani 1 1 d . . . H12B H -0.0386 0.8261 0.1727 0.044 Uiso 1 1 calc R . . C123 C -0.1135(2) 0.8740(4) 0.1309(2) 0.0460(14) Uani 1 1 d . . . H12C H -0.1333 0.8238 0.1348 0.055 Uiso 1 1 calc R . . C124 C -0.1409(2) 0.9460(4) 0.1026(2) 0.0540(16) Uani 1 1 d . . . H12D H -0.1795 0.9458 0.0873 0.065 Uiso 1 1 calc R . . C125 C -0.1110(3) 1.0166(4) 0.0974(3) 0.078(2) Uani 1 1 d . . . H12E H -0.1289 1.0660 0.0778 0.094 Uiso 1 1 calc R . . C126 C -0.0542(3) 1.0167(4) 0.1207(3) 0.082(2) Uani 1 1 d . . . H12F H -0.0349 1.0673 0.1164 0.099 Uiso 1 1 calc R . . C131 C 0.0667(2) 0.8775(3) 0.2231(2) 0.0402(13) Uani 1 1 d . . . C132 C 0.0678(2) 0.7882(4) 0.2101(3) 0.0510(15) Uani 1 1 d . . . H13B H 0.0548 0.7718 0.1742 0.061 Uiso 1 1 calc R . . C133 C 0.0877(2) 0.7222(4) 0.2485(3) 0.0621(18) Uani 1 1 d . . . H13C H 0.0876 0.6628 0.2379 0.075 Uiso 1 1 calc R . . C134 C 0.1070(3) 0.7431(6) 0.3009(3) 0.075(2) Uani 1 1 d . . . H13D H 0.1201 0.6988 0.3266 0.091 Uiso 1 1 calc R . . C135 C 0.1069(2) 0.8314(6) 0.3153(3) 0.069(2) Uani 1 1 d . . . H13E H 0.1200 0.8474 0.3512 0.083 Uiso 1 1 calc R . . C136 C 0.0876(2) 0.8954(4) 0.2770(3) 0.0553(16) Uani 1 1 d . . . H13F H 0.0887 0.9547 0.2880 0.066 Uiso 1 1 calc R . . C141 C 0.0602(2) 1.0504(3) 0.2021(2) 0.0402(13) Uani 1 1 d . . . C142 C 0.0316(2) 1.0890(4) 0.2321(3) 0.0653(19) Uani 1 1 d . . . H14B H 0.0005 1.0594 0.2347 0.078 Uiso 1 1 calc R . . C143 C 0.0463(3) 1.1685(4) 0.2582(3) 0.075(2) Uani 1 1 d . . . H14C H 0.0252 1.1912 0.2779 0.090 Uiso 1 1 calc R . . C144 C 0.0912(2) 1.2148(4) 0.2558(2) 0.0581(16) Uani 1 1 d . . . H14D H 0.1020 1.2683 0.2742 0.070 Uiso 1 1 calc R . . C145 C 0.1196(2) 1.1795(4) 0.2252(2) 0.0518(15) Uani 1 1 d . . . H14E H 0.1503 1.2101 0.2222 0.062 Uiso 1 1 calc R . . C146 C 0.1042(2) 1.1001(3) 0.1989(2) 0.0398(13) Uani 1 1 d . . . H14F H 0.1245 1.0790 0.1778 0.048 Uiso 1 1 calc R . . C151 C 0.3409(2) 1.0188(4) 0.3265(2) 0.0533(15) Uani 1 1 d . . . C152 C 0.2988(3) 1.0180(4) 0.2781(3) 0.0649(18) Uani 1 1 d . . . H15A H 0.3077 1.0264 0.2472 0.078 Uiso 1 1 calc R . . C153 C 0.2451(3) 1.0054(5) 0.2737(4) 0.094(3) Uani 1 1 d . . . H15B H 0.2180 1.0061 0.2399 0.112 Uiso 1 1 calc R . . C154 C 0.2297(3) 0.9921(6) 0.3161(5) 0.105(3) Uani 1 1 d . . . H15C H 0.1926 0.9807 0.3122 0.126 Uiso 1 1 calc R . . C155 C 0.2688(3) 0.9955(6) 0.3651(4) 0.117(3) Uani 1 1 d . . . H15D H 0.2665 0.9401 0.3834 0.141 Uiso 1 1 calc R . . H15E H 0.2587 1.0434 0.3847 0.141 Uiso 1 1 calc R . . C156 C 0.3244(3) 1.0079(6) 0.3696(3) 0.094(3) Uani 1 1 d . . . H15F H 0.3512 1.0087 0.4035 0.113 Uiso 1 1 calc R . . C161 C 0.4411(2) 0.9420(4) 0.3536(2) 0.0517(15) Uani 1 1 d . . . C162 C 0.4221(3) 0.8698(5) 0.3738(3) 0.0716(19) Uani 1 1 d . . . H16A H 0.3865 0.8713 0.3763 0.086 Uiso 1 1 calc R . . C163 C 0.4542(4) 0.7953(5) 0.3904(3) 0.095(3) Uani 1 1 d . . . H16B H 0.4402 0.7473 0.4043 0.114 Uiso 1 1 calc R . . C164 C 0.5061(5) 0.7900(6) 0.3872(3) 0.104(3) Uani 1 1 d . . . H16C H 0.5270 0.7381 0.3977 0.125 Uiso 1 1 calc R . . C165 C 0.5276(3) 0.8616(7) 0.3683(3) 0.096(3) Uani 1 1 d . . . H16D H 0.5635 0.8597 0.3665 0.115 Uiso 1 1 calc R . . C166 C 0.4950(3) 0.9356(5) 0.3521(3) 0.0704(19) Uani 1 1 d . . . H16E H 0.5097 0.9843 0.3394 0.084 Uiso 1 1 calc R . . C171 C 0.4272(2) 1.1080(4) 0.3819(2) 0.0507(15) Uani 1 1 d . . . C172 C 0.4617(2) 1.0879(4) 0.4327(2) 0.0541(16) Uani 1 1 d . . . H17A H 0.4775 1.0312 0.4393 0.065 Uiso 1 1 calc R . . C173 C 0.4737(3) 1.1477(5) 0.4737(3) 0.0641(18) Uani 1 1 d . . . H17B H 0.4964 1.1304 0.5076 0.077 Uiso 1 1 calc R . . C174 C 0.4531(3) 1.2319(5) 0.4658(3) 0.076(2) Uani 1 1 d . . . H17C H 0.4619 1.2730 0.4938 0.091 Uiso 1 1 calc R . . C175 C 0.4192(3) 1.2548(5) 0.4160(4) 0.078(2) Uani 1 1 d . . . H17D H 0.4047 1.3124 0.4097 0.093 Uiso 1 1 calc R . . C176 C 0.4062(2) 1.1944(4) 0.3751(3) 0.0642(18) Uani 1 1 d . . . H17E H 0.3824 1.2118 0.3416 0.077 Uiso 1 1 calc R . . C181 C 0.4169(2) 1.0660(5) 0.2799(3) 0.0608(17) Uani 1 1 d . . . C182 C 0.4055(3) 1.0088(5) 0.2373(3) 0.086(2) Uani 1 1 d . . . H18A H 0.3900 0.9534 0.2399 0.104 Uiso 1 1 calc R . . C183 C 0.4160(4) 1.0295(6) 0.1904(3) 0.096(3) Uani 1 1 d . . . H18B H 0.4076 0.9885 0.1625 0.115 Uiso 1 1 calc R . . C184 C 0.4380(3) 1.1079(8) 0.1858(4) 0.095(3) Uani 1 1 d . . . H18C H 0.4450 1.1223 0.1545 0.114 Uiso 1 1 calc R . . C185 C 0.4500(3) 1.1669(7) 0.2262(4) 0.094(3) Uani 1 1 d . . . H18D H 0.4651 1.2222 0.2227 0.112 Uiso 1 1 calc R . . C186 C 0.4401(2) 1.1457(5) 0.2729(3) 0.076(2) Uani 1 1 d . . . H18E H 0.4495 1.1871 0.3007 0.092 Uiso 1 1 calc R . . O1 O 0.2927(3) 1.3671(5) 0.3690(3) 0.173(4) Uani 1 1 d D . . C1S C 0.2701(3) 1.2949(6) 0.3652(4) 0.106(3) Uani 1 1 d D . . C2S C 0.2496(4) 1.2524(6) 0.3158(4) 0.130(4) Uani 1 1 d D . . H2SA H 0.2561 1.2894 0.2889 0.196 Uiso 1 1 calc R . . H2SB H 0.2104 1.2422 0.3071 0.196 Uiso 1 1 calc R . . H2SC H 0.2684 1.1962 0.3174 0.196 Uiso 1 1 calc R . . C3S C 0.2659(4) 1.2577(8) 0.4116(4) 0.173(6) Uani 1 1 d D . . H3SA H 0.2823 1.2975 0.4410 0.260 Uiso 1 1 calc R . . H3SB H 0.2852 1.2015 0.4184 0.260 Uiso 1 1 calc R . . H3SC H 0.2274 1.2485 0.4074 0.260 Uiso 1 1 calc R . . O2 O 0.2632(6) 1.0456(15) 0.0421(9) 0.490(18) Uani 1 1 d D . . C4S C 0.3098(6) 1.0268(10) 0.0401(5) 0.44(3) Uani 1 1 d D . . C5S C 0.3487(6) 1.0877(9) 0.0344(6) 0.247(8) Uani 1 1 d D . . H5SA H 0.3331 1.1468 0.0304 0.370 Uiso 1 1 calc R . . H5SB H 0.3582 1.0726 0.0033 0.370 Uiso 1 1 calc R . . H5SC H 0.3815 1.0856 0.0655 0.370 Uiso 1 1 calc R . . C6S C 0.3244(6) 0.9377(9) 0.0512(8) 0.259(11) Uani 1 1 d D . . H6SA H 0.2929 0.9049 0.0535 0.389 Uiso 1 1 calc R . . H6SB H 0.3545 0.9334 0.0845 0.389 Uiso 1 1 calc R . . H6SC H 0.3360 0.9132 0.0231 0.389 Uiso 1 1 calc R . . O3 O 0.7316(6) 1.2190(11) 0.1240(6) 0.361(8) Uiso 1 1 d D . . C7S C 0.7122(6) 1.1433(11) 0.1108(6) 0.273(9) Uiso 1 1 d D . . C8S C 0.6615(7) 1.1074(12) 0.1086(8) 0.313(11) Uiso 1 1 d D . . H8SA H 0.6417 1.1496 0.1228 0.469 Uiso 1 1 calc R . . H8SB H 0.6675 1.0534 0.1292 0.469 Uiso 1 1 calc R . . H8SC H 0.6400 1.0944 0.0721 0.469 Uiso 1 1 calc R . . C9S C 0.7465(7) 1.0894(12) 0.0931(8) 0.307(10) Uiso 1 1 d D . . H9SA H 0.7807 1.1204 0.0969 0.460 Uiso 1 1 calc R . . H9SB H 0.7282 1.0748 0.0561 0.460 Uiso 1 1 calc R . . H9SC H 0.7546 1.0354 0.1139 0.460 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0265(3) 0.0276(3) 0.0378(4) -0.0007(3) 0.0117(3) 0.0014(3) Ni3 0.0302(3) 0.0364(4) 0.0341(4) -0.0006(3) 0.0144(3) -0.0026(3) Ni2 0.0268(3) 0.0281(3) 0.0305(4) -0.0008(3) 0.0119(3) 0.0023(3) N1 0.039(2) 0.037(2) 0.032(2) 0.001(2) 0.016(2) 0.000(2) N2 0.036(2) 0.027(2) 0.030(2) -0.0017(18) 0.0103(18) 0.0005(18) N3 0.030(2) 0.027(2) 0.043(3) -0.007(2) 0.0092(19) 0.0000(18) N4 0.044(3) 0.024(2) 0.057(3) -0.008(2) 0.014(2) 0.000(2) N5 0.031(2) 0.026(2) 0.045(3) 0.002(2) 0.009(2) 0.0023(18) N6 0.033(2) 0.046(3) 0.063(3) -0.002(2) 0.028(2) 0.000(2) N7 0.031(2) 0.028(2) 0.040(3) 0.0065(19) 0.015(2) 0.0049(18) N8 0.027(2) 0.034(2) 0.032(2) 0.0019(18) 0.0119(18) 0.0008(17) N9 0.027(2) 0.040(2) 0.036(2) -0.002(2) 0.0112(19) 0.0017(18) N10 0.036(2) 0.029(2) 0.043(3) 0.000(2) 0.015(2) 0.0043(19) N11 0.031(2) 0.033(2) 0.039(3) 0.0023(19) 0.0166(19) 0.0022(18) N12 0.033(2) 0.037(3) 0.042(3) -0.001(2) 0.018(2) -0.0003(19) N13 0.051(3) 0.056(3) 0.048(3) 0.000(2) 0.028(2) -0.014(2) N14 0.035(2) 0.044(3) 0.038(3) 0.007(2) 0.014(2) 0.002(2) N15 0.036(2) 0.060(3) 0.031(3) -0.004(2) 0.002(2) -0.017(2) N16 0.032(2) 0.029(2) 0.034(2) 0.0006(19) 0.0102(19) -0.0013(18) N17 0.026(2) 0.026(2) 0.029(2) -0.0013(18) 0.0100(17) 0.0000(17) N18 0.025(2) 0.031(2) 0.033(2) -0.0014(18) 0.0079(18) 0.0029(17) C1 0.081(5) 0.040(4) 0.077(5) -0.018(3) 0.018(4) 0.006(3) C2 0.052(4) 0.080(5) 0.086(5) 0.003(4) 0.044(4) 0.010(3) C3 0.087(5) 0.102(6) 0.080(5) 0.024(5) 0.045(4) -0.005(4) C4 0.060(4) 0.081(5) 0.053(4) -0.010(4) 0.008(3) -0.017(4) C11 0.051(3) 0.038(3) 0.048(4) -0.001(3) 0.025(3) -0.004(3) C12 0.068(4) 0.037(3) 0.051(4) 0.008(3) 0.023(3) 0.000(3) C13 0.065(4) 0.048(4) 0.042(4) 0.013(3) 0.015(3) 0.010(3) C14 0.047(3) 0.044(3) 0.034(3) 0.001(3) 0.009(3) 0.001(3) C15 0.039(3) 0.033(3) 0.029(3) -0.004(2) 0.015(2) 0.002(2) C21 0.033(3) 0.030(3) 0.039(3) -0.003(2) 0.012(2) 0.000(2) C22 0.053(3) 0.050(3) 0.034(3) -0.009(3) 0.019(3) -0.003(3) C23 0.067(4) 0.054(4) 0.042(4) -0.015(3) 0.020(3) -0.002(3) C24 0.059(4) 0.046(4) 0.052(4) -0.019(3) 0.017(3) -0.001(3) C25 0.034(3) 0.035(3) 0.051(4) -0.008(3) 0.011(3) 0.004(2) C31 0.043(3) 0.026(3) 0.051(4) 0.005(3) 0.005(3) -0.003(2) C32 0.064(4) 0.047(4) 0.061(4) -0.001(3) 0.010(3) -0.025(3) C33 0.064(4) 0.066(4) 0.061(5) 0.012(4) 0.014(4) -0.028(3) C34 0.045(3) 0.060(4) 0.062(4) 0.009(3) 0.021(3) -0.011(3) C35 0.032(3) 0.035(3) 0.052(4) 0.010(3) 0.014(3) -0.001(2) C41 0.036(3) 0.035(3) 0.052(4) 0.004(3) 0.024(3) 0.002(2) C42 0.049(3) 0.047(3) 0.051(4) 0.006(3) 0.032(3) 0.002(3) C43 0.063(4) 0.060(4) 0.039(3) 0.000(3) 0.028(3) -0.005(3) C44 0.042(3) 0.049(3) 0.043(3) -0.001(3) 0.018(3) -0.007(3) C45 0.034(3) 0.031(3) 0.036(3) 0.007(2) 0.015(2) 0.004(2) C51 0.035(3) 0.035(3) 0.038(3) -0.002(2) 0.013(2) 0.003(2) C52 0.043(3) 0.059(4) 0.052(4) 0.023(3) 0.012(3) 0.002(3) C53 0.040(3) 0.088(5) 0.065(4) 0.034(4) 0.002(3) 0.015(3) C54 0.026(3) 0.073(4) 0.077(5) 0.024(4) 0.005(3) 0.003(3) C55 0.026(3) 0.053(4) 0.057(4) 0.005(3) 0.012(3) 0.002(3) C61 0.041(3) 0.047(3) 0.052(4) 0.009(3) 0.018(3) 0.005(3) C62 0.049(3) 0.040(3) 0.083(5) 0.020(3) 0.026(3) 0.012(3) C63 0.051(4) 0.045(4) 0.075(5) 0.016(3) 0.020(3) 0.020(3) C64 0.034(3) 0.042(3) 0.056(4) 0.004(3) 0.019(3) 0.009(2) C65 0.028(3) 0.037(3) 0.037(3) -0.008(2) 0.012(2) 0.003(2) C71 0.028(3) 0.043(3) 0.037(3) 0.002(2) 0.011(2) 0.008(2) C72 0.047(3) 0.049(3) 0.055(4) -0.013(3) 0.028(3) 0.001(3) C73 0.053(4) 0.070(4) 0.057(4) -0.016(3) 0.031(3) 0.003(3) C74 0.050(3) 0.077(4) 0.046(4) -0.007(3) 0.032(3) -0.006(3) C75 0.038(3) 0.053(4) 0.043(3) -0.003(3) 0.024(3) -0.003(3) C81 0.038(3) 0.042(3) 0.061(4) 0.005(3) 0.025(3) -0.004(3) C82 0.055(4) 0.052(4) 0.086(5) -0.012(4) 0.047(4) -0.014(3) C83 0.054(4) 0.051(4) 0.098(5) -0.015(4) 0.041(4) -0.021(3) C84 0.049(3) 0.048(4) 0.072(4) -0.013(3) 0.025(3) -0.017(3) C85 0.039(3) 0.040(3) 0.045(4) 0.002(3) 0.013(3) -0.003(2) C91 0.040(3) 0.038(3) 0.036(3) 0.000(3) 0.008(3) -0.010(2) C92 0.049(3) 0.042(3) 0.042(3) -0.011(3) 0.007(3) -0.005(3) C93 0.050(3) 0.044(3) 0.049(4) -0.012(3) 0.019(3) 0.005(3) C94 0.033(3) 0.040(3) 0.041(3) -0.006(3) 0.010(2) 0.004(2) C95 0.031(3) 0.026(3) 0.032(3) 0.004(2) 0.009(2) 0.004(2) C101 0.035(3) 0.025(3) 0.027(3) 0.001(2) 0.012(2) 0.003(2) C102 0.045(3) 0.033(3) 0.037(3) -0.001(2) 0.005(3) 0.003(2) C103 0.045(3) 0.042(3) 0.048(4) -0.003(3) -0.001(3) 0.017(3) C104 0.030(3) 0.045(3) 0.050(4) -0.008(3) -0.003(3) 0.010(3) C105 0.032(3) 0.034(3) 0.037(3) -0.001(2) 0.002(2) 0.002(2) B1 0.038(3) 0.028(3) 0.047(4) 0.001(3) 0.017(3) 0.002(3) B2 0.043(4) 0.060(4) 0.049(4) 0.004(4) 0.014(3) 0.003(3) C111 0.042(3) 0.023(3) 0.050(4) -0.001(2) 0.014(3) 0.000(2) C112 0.054(3) 0.038(3) 0.054(4) 0.006(3) 0.013(3) -0.009(3) C113 0.078(5) 0.045(4) 0.041(4) -0.007(3) 0.016(3) -0.019(3) C114 0.094(5) 0.047(4) 0.059(5) -0.008(3) 0.048(4) -0.005(4) C115 0.063(4) 0.046(4) 0.068(5) 0.002(3) 0.035(4) 0.006(3) C116 0.056(3) 0.036(3) 0.048(4) -0.002(3) 0.023(3) 0.002(3) C121 0.044(3) 0.034(3) 0.047(3) 0.005(3) 0.019(3) 0.005(2) C122 0.043(3) 0.037(3) 0.032(3) -0.003(2) 0.014(2) 0.000(2) C123 0.046(3) 0.052(4) 0.044(3) -0.008(3) 0.020(3) -0.008(3) C124 0.038(3) 0.072(4) 0.049(4) -0.013(3) 0.011(3) 0.005(3) C125 0.052(4) 0.055(4) 0.110(6) 0.023(4) 0.004(4) 0.023(3) C126 0.057(4) 0.038(4) 0.138(7) 0.029(4) 0.014(4) 0.003(3) C131 0.033(3) 0.043(3) 0.050(4) 0.007(3) 0.022(3) 0.000(2) C132 0.050(3) 0.042(3) 0.069(4) 0.010(3) 0.029(3) 0.007(3) C133 0.057(4) 0.042(4) 0.099(6) 0.020(4) 0.042(4) 0.008(3) C134 0.054(4) 0.091(6) 0.083(6) 0.040(5) 0.026(4) 0.014(4) C135 0.047(4) 0.108(6) 0.047(4) 0.023(4) 0.008(3) 0.002(4) C136 0.044(3) 0.059(4) 0.061(4) 0.008(3) 0.015(3) -0.004(3) C141 0.040(3) 0.037(3) 0.050(3) 0.000(3) 0.023(3) 0.006(2) C142 0.058(4) 0.060(4) 0.097(5) -0.025(4) 0.051(4) -0.016(3) C143 0.072(4) 0.063(4) 0.113(6) -0.039(4) 0.060(4) -0.010(4) C144 0.070(4) 0.045(4) 0.068(4) -0.012(3) 0.033(4) -0.003(3) C145 0.056(3) 0.051(4) 0.054(4) -0.009(3) 0.025(3) -0.017(3) C146 0.041(3) 0.038(3) 0.044(3) -0.002(3) 0.020(3) 0.000(2) C151 0.044(3) 0.058(4) 0.055(4) 0.000(3) 0.011(3) 0.003(3) C152 0.060(4) 0.054(4) 0.066(5) 0.005(3) 0.001(4) -0.004(3) C153 0.056(5) 0.061(5) 0.126(8) -0.003(5) -0.021(5) -0.014(4) C154 0.035(4) 0.090(6) 0.174(11) 0.006(7) 0.011(6) -0.014(4) C155 0.075(6) 0.122(8) 0.169(10) -0.003(7) 0.059(7) -0.014(5) C156 0.050(4) 0.157(8) 0.076(5) 0.012(5) 0.024(4) -0.018(5) C161 0.049(3) 0.064(4) 0.038(3) 0.001(3) 0.009(3) 0.003(3) C162 0.073(5) 0.069(5) 0.060(5) 0.014(4) 0.006(4) 0.002(4) C163 0.119(7) 0.067(5) 0.080(6) 0.002(4) 0.006(5) 0.013(5) C164 0.140(9) 0.086(7) 0.067(6) 0.005(5) 0.010(6) 0.065(6) C165 0.077(5) 0.136(8) 0.063(5) 0.001(5) 0.008(4) 0.053(6) C166 0.060(4) 0.088(5) 0.065(5) 0.010(4) 0.023(4) 0.017(4) C171 0.038(3) 0.061(4) 0.059(4) 0.011(3) 0.025(3) 0.000(3) C172 0.056(4) 0.056(4) 0.060(4) 0.001(3) 0.033(3) -0.003(3) C173 0.073(4) 0.065(5) 0.066(5) 0.004(4) 0.038(4) -0.003(4) C174 0.071(5) 0.088(6) 0.085(6) -0.021(5) 0.046(5) -0.030(4) C175 0.068(5) 0.057(5) 0.119(7) -0.007(5) 0.046(5) -0.005(4) C176 0.052(4) 0.060(4) 0.082(5) 0.008(4) 0.024(4) 0.001(3) C181 0.049(4) 0.079(5) 0.056(4) 0.021(4) 0.019(3) 0.021(3) C182 0.140(7) 0.071(5) 0.062(5) 0.021(4) 0.052(5) 0.046(5) C183 0.135(7) 0.090(6) 0.076(6) 0.023(5) 0.054(5) 0.061(6) C184 0.083(6) 0.136(9) 0.080(7) 0.037(6) 0.046(5) 0.048(6) C185 0.044(4) 0.143(8) 0.093(6) 0.055(6) 0.021(4) -0.002(5) C186 0.046(4) 0.113(6) 0.069(5) 0.025(4) 0.016(3) -0.011(4) O1 0.195(8) 0.097(5) 0.153(7) 0.014(5) -0.040(6) -0.005(5) C1S 0.071(5) 0.062(6) 0.152(10) -0.010(6) -0.005(6) 0.008(4) C2S 0.117(8) 0.104(7) 0.141(9) -0.009(7) 0.003(7) -0.016(6) C3S 0.132(9) 0.236(15) 0.172(12) 0.103(11) 0.078(9) 0.049(9) O2 0.251(17) 0.72(4) 0.54(3) -0.29(3) 0.182(19) -0.22(2) C4S 0.46(4) 0.75(7) 0.113(14) -0.12(3) 0.09(2) -0.49(5) C5S 0.199(16) 0.28(2) 0.225(19) 0.024(15) 0.026(14) -0.010(15) C6S 0.185(16) 0.29(2) 0.24(2) 0.018(17) -0.021(14) -0.123(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 1.982(4) . ? Ni1 N3 2.004(4) . ? Ni1 N7 2.013(4) . ? Ni1 N10 2.100(4) . ? Ni1 N18 2.111(4) . ? Ni1 Ni2 2.3527(9) . ? Ni3 N14 1.990(4) . ? Ni3 N12 1.999(4) . ? Ni3 N16 2.001(4) . ? Ni3 N9 2.107(4) . ? Ni3 N1 2.119(4) . ? Ni3 Ni2 2.3560(9) . ? Ni2 N8 1.879(4) . ? Ni2 N17 1.889(4) . ? Ni2 N11 1.890(4) . ? Ni2 N2 1.895(4) . ? N1 C15 1.344(6) . ? N1 C11 1.358(6) . ? N2 C15 1.372(6) . ? N2 C21 1.379(6) . ? N3 C25 1.347(6) . ? N3 C21 1.359(6) . ? N4 C31 1.385(7) . ? N4 C25 1.411(7) . ? N4 C1 1.485(6) . ? N5 C31 1.347(6) . ? N5 C35 1.359(6) . ? N6 C35 1.374(7) . ? N6 C41 1.416(6) . ? N6 C2 1.477(6) . ? N7 C41 1.339(6) . ? N7 C45 1.361(6) . ? N8 C45 1.377(6) . ? N8 C51 1.381(6) . ? N9 C55 1.342(6) . ? N9 C51 1.357(6) . ? N10 C61 1.331(6) . ? N10 C65 1.351(6) . ? N11 C71 1.372(6) . ? N11 C65 1.377(6) . ? N12 C75 1.342(6) . ? N12 C71 1.344(6) . ? N13 C81 1.390(7) . ? N13 C75 1.409(7) . ? N13 C3 1.474(7) . ? N14 C85 1.338(6) . ? N14 C81 1.352(6) . ? N15 C85 1.379(7) . ? N15 C91 1.417(6) . ? N15 C4 1.449(7) . ? N16 C91 1.347(6) . ? N16 C95 1.363(6) . ? N17 C101 1.366(6) . ? N17 C95 1.367(6) . ? N18 C105 1.343(6) . ? N18 C101 1.355(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C11 C12 1.365(7) . ? C11 H11A 0.9400 . ? C12 C13 1.380(8) . ? C12 H12A 0.9400 . ? C13 C14 1.366(7) . ? C13 H13A 0.9400 . ? C14 C15 1.406(7) . ? C14 H14A 0.9400 . ? C21 C22 1.394(7) . ? C22 C23 1.361(7) . ? C22 H22A 0.9400 . ? C23 C24 1.366(8) . ? C23 H23A 0.9400 . ? C24 C25 1.374(7) . ? C24 H24A 0.9400 . ? C31 C32 1.391(7) . ? C32 C33 1.376(8) . ? C32 H32A 0.9400 . ? C33 C34 1.344(8) . ? C33 H33A 0.9400 . ? C34 C35 1.392(7) . ? C34 H34A 0.9400 . ? C41 C42 1.378(7) . ? C42 C43 1.369(7) . ? C42 H42A 0.9400 . ? C43 C44 1.364(7) . ? C43 H43A 0.9400 . ? C44 C45 1.378(7) . ? C44 H44A 0.9400 . ? C51 C52 1.394(7) . ? C52 C53 1.367(7) . ? C52 H52A 0.9400 . ? C53 C54 1.383(8) . ? C53 H53A 0.9400 . ? C54 C55 1.357(7) . ? C54 H54A 0.9400 . ? C55 H55A 0.9400 . ? C61 C62 1.368(7) . ? C61 H61A 0.9400 . ? C62 C63 1.366(8) . ? C62 H62A 0.9400 . ? C63 C64 1.369(7) . ? C63 H63A 0.9400 . ? C64 C65 1.388(6) . ? C64 H64A 0.9400 . ? C71 C72 1.390(7) . ? C72 C73 1.358(7) . ? C72 H72A 0.9400 . ? C73 C74 1.371(8) . ? C73 H73A 0.9400 . ? C74 C75 1.376(7) . ? C74 H74A 0.9400 . ? C81 C82 1.381(7) . ? C82 C83 1.356(8) . ? C82 H82A 0.9400 . ? C83 C84 1.373(8) . ? C83 H83A 0.9400 . ? C84 C85 1.388(7) . ? C84 H84A 0.9400 . ? C91 C92 1.367(7) . ? C92 C93 1.385(7) . ? C92 H92A 0.9400 . ? C93 C94 1.369(7) . ? C93 H93A 0.9400 . ? C94 C95 1.386(6) . ? C94 H94A 0.9400 . ? C101 C102 1.391(6) . ? C102 C103 1.367(7) . ? C102 H10A 0.9400 . ? C103 C104 1.384(7) . ? C103 H10B 0.9400 . ? C104 C105 1.352(7) . ? C104 H10C 0.9400 . ? C105 H10D 0.9400 . ? B1 C141 1.633(8) . ? B1 C111 1.639(8) . ? B1 C131 1.646(8) . ? B1 C121 1.647(7) . ? B2 C171 1.634(9) . ? B2 C161 1.635(9) . ? B2 C151 1.641(8) . ? B2 C181 1.660(9) . ? C111 C112 1.385(7) . ? C111 C116 1.391(7) . ? C112 C113 1.389(8) . ? C112 H11B 0.9400 . ? C113 C114 1.366(8) . ? C113 H11C 0.9400 . ? C114 C115 1.382(8) . ? C114 H11D 0.9400 . ? C115 C116 1.387(7) . ? C115 H11E 0.9400 . ? C116 H11F 0.9400 . ? C121 C122 1.379(7) . ? C121 C126 1.386(7) . ? C122 C123 1.393(7) . ? C122 H12B 0.9400 . ? C123 C124 1.378(8) . ? C123 H12C 0.9400 . ? C124 C125 1.348(8) . ? C124 H12D 0.9400 . ? C125 C126 1.385(8) . ? C125 H12E 0.9400 . ? C126 H12F 0.9400 . ? C131 C136 1.389(8) . ? C131 C132 1.396(7) . ? C132 C133 1.402(8) . ? C132 H13B 0.9400 . ? C133 C134 1.361(9) . ? C133 H13C 0.9400 . ? C134 C135 1.390(10) . ? C134 H13D 0.9400 . ? C135 C136 1.377(8) . ? C135 H13E 0.9400 . ? C136 H13F 0.9400 . ? C141 C142 1.384(7) . ? C141 C146 1.386(7) . ? C142 C143 1.378(8) . ? C142 H14B 0.9400 . ? C143 C144 1.369(8) . ? C143 H14C 0.9400 . ? C144 C145 1.373(7) . ? C144 H14D 0.9400 . ? C145 C146 1.382(7) . ? C145 H14E 0.9400 . ? C146 H14F 0.9400 . ? C151 C156 1.366(9) . ? C151 C152 1.384(8) . ? C152 C153 1.360(10) . ? C152 H15A 0.9400 . ? C153 C154 1.335(12) . ? C153 H15B 0.9400 . ? C154 C155 1.365(12) . ? C154 H15C 0.9400 . ? C155 C156 1.405(9) . ? C155 H15D 0.9800 . ? C155 H15E 0.9800 . ? C156 H15F 0.9400 . ? C161 C162 1.379(8) . ? C161 C166 1.403(8) . ? C162 C163 1.380(10) . ? C162 H16A 0.9400 . ? C163 C164 1.368(12) . ? C163 H16B 0.9400 . ? C164 C165 1.385(12) . ? C164 H16C 0.9400 . ? C165 C166 1.379(10) . ? C165 H16D 0.9400 . ? C166 H16E 0.9400 . ? C171 C172 1.388(8) . ? C171 C176 1.402(8) . ? C172 C173 1.376(8) . ? C172 H17A 0.9400 . ? C173 C174 1.367(9) . ? C173 H17B 0.9400 . ? C174 C175 1.374(10) . ? C174 H17C 0.9400 . ? C175 C176 1.379(9) . ? C175 H17D 0.9400 . ? C176 H17E 0.9400 . ? C181 C182 1.382(9) . ? C181 C186 1.384(9) . ? C182 C183 1.406(10) . ? C182 H18A 0.9400 . ? C183 C184 1.336(11) . ? C183 H18B 0.9400 . ? C184 C185 1.356(11) . ? C184 H18C 0.9400 . ? C185 C186 1.395(10) . ? C185 H18D 0.9400 . ? C186 H18E 0.9400 . ? O1 C1S 1.225(9) . ? C1S C3S 1.401(8) . ? C1S C2S 1.404(7) . ? C2S H2SA 0.9700 . ? C2S H2SB 0.9700 . ? C2S H2SC 0.9700 . ? C3S H3SA 0.9700 . ? C3S H3SB 0.9700 . ? C3S H3SC 0.9700 . ? O2 C4S 1.249(12) . ? C4S C6S 1.403(9) . ? C4S C5S 1.404(9) . ? C5S H5SA 0.9700 . ? C5S H5SB 0.9700 . ? C5S H5SC 0.9700 . ? C6S H6SA 0.9700 . ? C6S H6SB 0.9700 . ? C6S H6SC 0.9700 . ? O3 C7S 1.250(11) . ? C7S C8S 1.395(9) . ? C7S C9S 1.396(9) . ? C8S H8SA 0.9700 . ? C8S H8SB 0.9700 . ? C8S H8SC 0.9700 . ? C9S H9SA 0.9700 . ? C9S H9SB 0.9700 . ? C9S H9SC 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 N5 Ni1 N3 94.46(16) . . ? N5 Ni1 N7 94.33(16) . . ? N3 Ni1 N7 171.08(16) . . ? N5 Ni1 N10 97.54(15) . . ? N3 Ni1 N10 89.08(15) . . ? N7 Ni1 N10 91.30(15) . . ? N5 Ni1 N18 96.53(15) . . ? N3 Ni1 N18 90.63(15) . . ? N7 Ni1 N18 86.83(15) . . ? N10 Ni1 N18 165.91(15) . . ? N5 Ni1 Ni2 179.25(12) . . ? N3 Ni1 Ni2 85.55(11) . . ? N7 Ni1 Ni2 85.64(11) . . ? N10 Ni1 Ni2 83.21(11) . . ? N18 Ni1 Ni2 82.72(10) . . ? N14 Ni3 N12 94.48(17) . . ? N14 Ni3 N16 94.56(16) . . ? N12 Ni3 N16 170.90(16) . . ? N14 Ni3 N9 96.58(15) . . ? N12 Ni3 N9 89.38(16) . . ? N16 Ni3 N9 88.52(15) . . ? N14 Ni3 N1 98.28(16) . . ? N12 Ni3 N1 89.18(16) . . ? N16 Ni3 N1 90.58(15) . . ? N9 Ni3 N1 165.13(15) . . ? N14 Ni3 Ni2 179.65(13) . . ? N12 Ni3 Ni2 85.65(11) . . ? N16 Ni3 Ni2 85.31(11) . . ? N9 Ni3 Ni2 83.09(10) . . ? N1 Ni3 Ni2 82.04(11) . . ? N8 Ni2 N17 89.91(16) . . ? N8 Ni2 N11 89.78(17) . . ? N17 Ni2 N11 176.46(16) . . ? N8 Ni2 N2 176.61(16) . . ? N17 Ni2 N2 89.74(16) . . ? N11 Ni2 N2 90.78(16) . . ? N8 Ni2 Ni1 88.22(11) . . ? N17 Ni2 Ni1 92.12(11) . . ? N11 Ni2 Ni1 91.39(12) . . ? N2 Ni2 Ni1 88.42(12) . . ? N8 Ni2 Ni3 91.19(11) . . ? N17 Ni2 Ni3 88.34(11) . . ? N11 Ni2 Ni3 88.15(12) . . ? N2 Ni2 Ni3 92.17(12) . . ? Ni1 Ni2 Ni3 179.26(4) . . ? C15 N1 C11 118.5(4) . . ? C15 N1 Ni3 121.0(3) . . ? C11 N1 Ni3 120.5(4) . . ? C15 N2 C21 122.6(4) . . ? C15 N2 Ni2 117.7(3) . . ? C21 N2 Ni2 119.7(3) . . ? C25 N3 C21 119.2(4) . . ? C25 N3 Ni1 120.6(3) . . ? C21 N3 Ni1 120.2(3) . . ? C31 N4 C25 125.3(4) . . ? C31 N4 C1 115.8(4) . . ? C25 N4 C1 115.2(5) . . ? C31 N5 C35 121.0(4) . . ? C31 N5 Ni1 119.2(3) . . ? C35 N5 Ni1 119.8(3) . . ? C35 N6 C41 128.4(4) . . ? C35 N6 C2 115.4(4) . . ? C41 N6 C2 114.4(5) . . ? C41 N7 C45 120.0(4) . . ? C41 N7 Ni1 120.7(3) . . ? C45 N7 Ni1 118.9(3) . . ? C45 N8 C51 121.7(4) . . ? C45 N8 Ni2 118.8(3) . . ? C51 N8 Ni2 119.5(3) . . ? C55 N9 C51 118.5(4) . . ? C55 N9 Ni3 121.9(3) . . ? C51 N9 Ni3 119.6(3) . . ? C61 N10 C65 118.3(4) . . ? C61 N10 Ni1 121.2(3) . . ? C65 N10 Ni1 120.2(3) . . ? C71 N11 C65 123.0(4) . . ? C71 N11 Ni2 119.5(3) . . ? C65 N11 Ni2 117.3(3) . . ? C75 N12 C71 120.2(4) . . ? C75 N12 Ni3 120.3(3) . . ? C71 N12 Ni3 119.4(3) . . ? C81 N13 C75 124.6(5) . . ? C81 N13 C3 116.2(5) . . ? C75 N13 C3 116.2(5) . . ? C85 N14 C81 120.6(4) . . ? C85 N14 Ni3 119.6(3) . . ? C81 N14 Ni3 119.7(4) . . ? C85 N15 C91 126.6(4) . . ? C85 N15 C4 114.9(4) . . ? C91 N15 C4 117.0(5) . . ? C91 N16 C95 119.8(4) . . ? C91 N16 Ni3 120.2(3) . . ? C95 N16 Ni3 119.7(3) . . ? C101 N17 C95 122.3(4) . . ? C101 N17 Ni2 119.0(3) . . ? C95 N17 Ni2 118.5(3) . . ? C105 N18 C101 118.7(4) . . ? C105 N18 Ni1 121.2(3) . . ? C101 N18 Ni1 120.0(3) . . ? N4 C1 H1A 109.5 . . ? N4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N6 C2 H2A 109.5 . . ? N6 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N6 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N13 C3 H3A 109.5 . . ? N13 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N13 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N15 C4 H4A 109.5 . . ? N15 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N15 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C11 C12 123.3(5) . . ? N1 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C11 C12 C13 117.8(5) . . ? C11 C12 H12A 121.1 . . ? C13 C12 H12A 121.1 . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 119.0(5) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? N1 C15 N2 115.5(4) . . ? N1 C15 C14 120.7(4) . . ? N2 C15 C14 123.6(4) . . ? N3 C21 N2 114.5(4) . . ? N3 C21 C22 120.4(5) . . ? N2 C21 C22 125.0(5) . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N3 C25 C24 121.7(5) . . ? N3 C25 N4 117.0(5) . . ? C24 C25 N4 121.2(5) . . ? N5 C31 N4 119.7(4) . . ? N5 C31 C32 119.6(5) . . ? N4 C31 C32 120.7(5) . . ? C33 C32 C31 118.9(6) . . ? C33 C32 H32A 120.5 . . ? C31 C32 H32A 120.5 . . ? C34 C33 C32 121.5(6) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 118.8(6) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? N5 C35 N6 119.8(4) . . ? N5 C35 C34 120.1(5) . . ? N6 C35 C34 120.0(5) . . ? N7 C41 C42 121.4(5) . . ? N7 C41 N6 118.1(5) . . ? C42 C41 N6 120.4(5) . . ? C43 C42 C41 118.2(5) . . ? C43 C42 H42A 120.9 . . ? C41 C42 H42A 120.9 . . ? C44 C43 C42 121.2(5) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C43 C44 C45 118.8(5) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? N7 C45 N8 115.2(4) . . ? N7 C45 C44 120.3(4) . . ? N8 C45 C44 124.1(4) . . ? N9 C51 N8 115.2(4) . . ? N9 C51 C52 120.2(4) . . ? N8 C51 C52 124.4(5) . . ? C53 C52 C51 119.6(5) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? C52 C53 C54 120.0(6) . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 117.8(5) . . ? C55 C54 H54A 121.1 . . ? C53 C54 H54A 121.1 . . ? N9 C55 C54 123.9(5) . . ? N9 C55 H55A 118.1 . . ? C54 C55 H55A 118.1 . . ? N10 C61 C62 123.9(5) . . ? N10 C61 H61A 118.0 . . ? C62 C61 H61A 118.0 . . ? C63 C62 C61 118.1(5) . . ? C63 C62 H62A 120.9 . . ? C61 C62 H62A 120.9 . . ? C62 C63 C64 119.3(5) . . ? C62 C63 H63A 120.4 . . ? C64 C63 H63A 120.4 . . ? C63 C64 C65 120.2(5) . . ? C63 C64 H64A 119.9 . . ? C65 C64 H64A 119.9 . . ? N10 C65 N11 115.4(4) . . ? N10 C65 C64 120.1(5) . . ? N11 C65 C64 124.3(4) . . ? N12 C71 N11 115.8(4) . . ? N12 C71 C72 120.2(5) . . ? N11 C71 C72 123.7(5) . . ? C73 C72 C71 119.1(5) . . ? C73 C72 H72A 120.5 . . ? C71 C72 H72A 120.5 . . ? C72 C73 C74 120.7(5) . . ? C72 C73 H73A 119.7 . . ? C74 C73 H73A 119.7 . . ? C73 C74 C75 118.4(5) . . ? C73 C74 H74A 120.8 . . ? C75 C74 H74A 120.8 . . ? N12 C75 C74 121.3(5) . . ? N12 C75 N13 118.2(4) . . ? C74 C75 N13 120.5(5) . . ? N14 C81 C82 120.6(5) . . ? N14 C81 N13 119.2(4) . . ? C82 C81 N13 120.2(5) . . ? C83 C82 C81 118.1(6) . . ? C83 C82 H82A 120.9 . . ? C81 C82 H82A 120.9 . . ? C82 C83 C84 122.2(5) . . ? C82 C83 H83A 118.9 . . ? C84 C83 H83A 118.9 . . ? C83 C84 C85 117.5(6) . . ? C83 C84 H84A 121.2 . . ? C85 C84 H84A 121.2 . . ? N14 C85 N15 119.7(4) . . ? N14 C85 C84 120.9(5) . . ? N15 C85 C84 119.3(5) . . ? N16 C91 C92 122.0(5) . . ? N16 C91 N15 117.8(5) . . ? C92 C91 N15 120.2(5) . . ? C91 C92 C93 118.3(5) . . ? C91 C92 H92A 120.8 . . ? C93 C92 H92A 120.8 . . ? C94 C93 C92 120.4(5) . . ? C94 C93 H93A 119.8 . . ? C92 C93 H93A 119.8 . . ? C93 C94 C95 119.3(5) . . ? C93 C94 H94A 120.3 . . ? C95 C94 H94A 120.3 . . ? N16 C95 N17 115.0(4) . . ? N16 C95 C94 120.0(4) . . ? N17 C95 C94 124.6(4) . . ? N18 C101 N17 115.9(4) . . ? N18 C101 C102 119.7(4) . . ? N17 C101 C102 124.4(4) . . ? C103 C102 C101 120.1(5) . . ? C103 C102 H10A 120.0 . . ? C101 C102 H10A 120.0 . . ? C102 C103 C104 119.8(5) . . ? C102 C103 H10B 120.1 . . ? C104 C103 H10B 120.1 . . ? C105 C104 C103 117.6(5) . . ? C105 C104 H10C 121.2 . . ? C103 C104 H10C 121.2 . . ? N18 C105 C104 124.0(5) . . ? N18 C105 H10D 118.0 . . ? C104 C105 H10D 118.0 . . ? C141 B1 C111 109.4(4) . . ? C141 B1 C131 108.8(4) . . ? C111 B1 C131 109.0(4) . . ? C141 B1 C121 108.3(4) . . ? C111 B1 C121 110.7(4) . . ? C131 B1 C121 110.7(4) . . ? C171 B2 C161 110.1(5) . . ? C171 B2 C151 105.1(5) . . ? C161 B2 C151 110.8(5) . . ? C171 B2 C181 112.1(5) . . ? C161 B2 C181 106.6(5) . . ? C151 B2 C181 112.2(5) . . ? C112 C111 C116 115.2(5) . . ? C112 C111 B1 125.0(5) . . ? C116 C111 B1 119.6(5) . . ? C111 C112 C113 123.4(6) . . ? C111 C112 H11B 118.3 . . ? C113 C112 H11B 118.3 . . ? C114 C113 C112 119.1(6) . . ? C114 C113 H11C 120.4 . . ? C112 C113 H11C 120.4 . . ? C113 C114 C115 120.1(6) . . ? C113 C114 H11D 120.0 . . ? C115 C114 H11D 120.0 . . ? C114 C115 C116 119.2(6) . . ? C114 C115 H11E 120.4 . . ? C116 C115 H11E 120.4 . . ? C115 C116 C111 122.9(6) . . ? C115 C116 H11F 118.5 . . ? C111 C116 H11F 118.5 . . ? C122 C121 C126 113.2(5) . . ? C122 C121 B1 125.5(5) . . ? C126 C121 B1 121.2(5) . . ? C121 C122 C123 123.9(5) . . ? C121 C122 H12B 118.1 . . ? C123 C122 H12B 118.1 . . ? C124 C123 C122 119.8(5) . . ? C124 C123 H12C 120.1 . . ? C122 C123 H12C 120.1 . . ? C125 C124 C123 118.5(5) . . ? C125 C124 H12D 120.8 . . ? C123 C124 H12D 120.8 . . ? C124 C125 C126 120.3(6) . . ? C124 C125 H12E 119.8 . . ? C126 C125 H12E 119.8 . . ? C125 C126 C121 124.3(6) . . ? C125 C126 H12F 117.9 . . ? C121 C126 H12F 117.9 . . ? C136 C131 C132 114.5(5) . . ? C136 C131 B1 125.2(5) . . ? C132 C131 B1 120.3(5) . . ? C131 C132 C133 122.5(6) . . ? C131 C132 H13B 118.8 . . ? C133 C132 H13B 118.8 . . ? C134 C133 C132 120.7(6) . . ? C134 C133 H13C 119.7 . . ? C132 C133 H13C 119.7 . . ? C133 C134 C135 118.4(7) . . ? C133 C134 H13D 120.8 . . ? C135 C134 H13D 120.8 . . ? C136 C135 C134 120.0(7) . . ? C136 C135 H13E 120.0 . . ? C134 C135 H13E 120.0 . . ? C135 C136 C131 123.8(6) . . ? C135 C136 H13F 118.1 . . ? C131 C136 H13F 118.1 . . ? C142 C141 C146 114.3(5) . . ? C142 C141 B1 121.0(5) . . ? C146 C141 B1 124.7(4) . . ? C143 C142 C141 123.5(5) . . ? C143 C142 H14B 118.3 . . ? C141 C142 H14B 118.3 . . ? C144 C143 C142 121.1(6) . . ? C144 C143 H14C 119.5 . . ? C142 C143 H14C 119.5 . . ? C143 C144 C145 116.9(6) . . ? C143 C144 H14D 121.5 . . ? C145 C144 H14D 121.5 . . ? C144 C145 C146 121.5(5) . . ? C144 C145 H14E 119.2 . . ? C146 C145 H14E 119.2 . . ? C145 C146 C141 122.6(5) . . ? C145 C146 H14F 118.7 . . ? C141 C146 H14F 118.7 . . ? C156 C151 C152 115.1(6) . . ? C156 C151 B2 119.5(6) . . ? C152 C151 B2 125.4(6) . . ? C153 C152 C151 122.6(7) . . ? C153 C152 H15A 118.7 . . ? C151 C152 H15A 118.7 . . ? C154 C153 C152 121.7(8) . . ? C154 C153 H15B 119.1 . . ? C152 C153 H15B 119.1 . . ? C153 C154 C155 118.8(8) . . ? C153 C154 H15C 120.6 . . ? C155 C154 H15C 120.6 . . ? C154 C155 C156 119.3(9) . . ? C154 C155 H15D 107.5 . . ? C156 C155 H15D 107.5 . . ? C154 C155 H15E 107.5 . . ? C156 C155 H15E 107.5 . . ? H15D C155 H15E 107.0 . . ? C151 C156 C155 122.5(8) . . ? C151 C156 H15F 118.8 . . ? C155 C156 H15F 118.8 . . ? C162 C161 C166 116.1(6) . . ? C162 C161 B2 124.2(6) . . ? C166 C161 B2 119.6(6) . . ? C161 C162 C163 121.3(7) . . ? C161 C162 H16A 119.3 . . ? C163 C162 H16A 119.3 . . ? C164 C163 C162 121.3(9) . . ? C164 C163 H16B 119.4 . . ? C162 C163 H16B 119.4 . . ? C163 C164 C165 119.6(8) . . ? C163 C164 H16C 120.2 . . ? C165 C164 H16C 120.2 . . ? C166 C165 C164 118.2(8) . . ? C166 C165 H16D 120.9 . . ? C164 C165 H16D 120.9 . . ? C165 C166 C161 123.4(7) . . ? C165 C166 H16E 118.3 . . ? C161 C166 H16E 118.3 . . ? C172 C171 C176 115.1(6) . . ? C172 C171 B2 122.8(5) . . ? C176 C171 B2 121.7(6) . . ? C173 C172 C171 122.6(6) . . ? C173 C172 H17A 118.7 . . ? C171 C172 H17A 118.7 . . ? C174 C173 C172 121.1(7) . . ? C174 C173 H17B 119.4 . . ? C172 C173 H17B 119.5 . . ? C173 C174 C175 118.1(7) . . ? C173 C174 H17C 120.9 . . ? C175 C174 H17C 120.9 . . ? C174 C175 C176 120.9(7) . . ? C174 C175 H17D 119.5 . . ? C176 C175 H17D 119.5 . . ? C175 C176 C171 122.1(7) . . ? C175 C176 H17E 118.9 . . ? C171 C176 H17E 118.9 . . ? C182 C181 C186 114.6(7) . . ? C182 C181 B2 119.9(6) . . ? C186 C181 B2 125.3(6) . . ? C181 C182 C183 123.2(8) . . ? C181 C182 H18A 118.4 . . ? C183 C182 H18A 118.4 . . ? C184 C183 C182 119.5(9) . . ? C184 C183 H18B 120.2 . . ? C182 C183 H18B 120.2 . . ? C183 C184 C185 120.0(9) . . ? C183 C184 H18C 120.0 . . ? C185 C184 H18C 120.0 . . ? C184 C185 C186 120.3(9) . . ? C184 C185 H18D 119.9 . . ? C186 C185 H18D 119.9 . . ? C181 C186 C185 122.4(8) . . ? C181 C186 H18E 118.8 . . ? C185 C186 H18E 118.8 . . ? O1 C1S C3S 117.1(9) . . ? O1 C1S C2S 120.4(9) . . ? C3S C1S C2S 122.5(9) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C3S H3SA 109.5 . . ? C1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O2 C4S C6S 113.8(13) . . ? O2 C4S C5S 125.7(13) . . ? C6S C4S C5S 120.1(11) . . ? C4S C5S H5SA 109.5 . . ? C4S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C4S C6S H6SA 109.5 . . ? C4S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C4S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? O3 C7S C8S 130.3(14) . . ? O3 C7S C9S 113.1(13) . . ? C8S C7S C9S 116.5(13) . . ? C7S C8S H8SA 109.5 . . ? C7S C8S H8SB 109.5 . . ? H8SA C8S H8SB 109.5 . . ? C7S C8S H8SC 109.5 . . ? H8SA C8S H8SC 109.5 . . ? H8SB C8S H8SC 109.5 . . ? C7S C9S H9SA 109.5 . . ? C7S C9S H9SB 109.5 . . ? H9SA C9S H9SB 109.5 . . ? C7S C9S H9SC 109.5 . . ? H9SA C9S H9SC 109.5 . . ? H9SB C9S H9SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.888 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.085 data_cif8 _database_code_depnum_ccdc_archive 'CCDC 618491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(mpeptea)2(PF6)2,0.75CH3COCH3,0.5H2O _chemical_melting_point ? _chemical_formula_moiety Ni3(C27H23N18)2(PF6)2,0.75CH3COCH3,0.5H2O _chemical_formula_sum 'C56.25 H50.50 F12 N18 Ni3 O1.25 P2' _chemical_formula_weight 1464.72 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.986(7) _cell_length_b 14.116(7) _cell_length_c 31.151(15) _cell_angle_alpha 85.761(8) _cell_angle_beta 78.517(8) _cell_angle_gamma 80.128(9) _cell_volume 5933(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 37864 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8620 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37863 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20609 _reflns_number_gt 13021 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0720P)^2^+18.7066P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20609 _refine_ls_number_parameters 1765 _refine_ls_number_restraints 5841 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.159 _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 Ni1 Ni 0.49318(6) -0.16372(6) 0.35006(2) 0.0240(2) Uani 1 1 d . . . Ni2 Ni 0.63388(6) -0.26558(6) 0.36582(2) 0.02070(19) Uani 1 1 d . . . Ni3 Ni 0.77410(6) -0.36866(6) 0.38173(3) 0.0242(2) Uani 1 1 d . . . Ni4 Ni 0.71178(7) 0.18786(6) 0.11181(3) 0.0288(2) Uani 1 1 d . . . Ni5 Ni 0.85077(6) 0.24061(6) 0.12896(2) 0.0244(2) Uani 1 1 d . . . Ni6 Ni 0.98770(7) 0.29140(6) 0.14823(3) 0.0277(2) Uani 1 1 d . . . N1 N 0.6724(4) -0.4676(4) 0.39798(16) 0.0258(12) Uani 1 1 d . . . N2 N 0.5487(4) -0.3365(4) 0.40504(16) 0.0240(12) Uani 1 1 d . . . N3 N 0.4260(4) -0.2038(4) 0.40964(17) 0.0261(12) Uani 1 1 d . . . N4 N 0.3193(4) -0.0556(4) 0.41201(18) 0.0336(14) Uani 1 1 d . . . N5 N 0.3736(4) -0.0801(4) 0.33624(17) 0.0310(13) Uani 1 1 d . . . N6 N 0.4327(5) -0.1095(4) 0.26009(19) 0.0392(15) Uani 1 1 d . . . N7 N 0.5770(4) -0.1381(4) 0.29159(16) 0.0269(12) Uani 1 1 d . . . N8 N 0.7111(4) -0.1890(4) 0.32576(16) 0.0257(12) Uani 1 1 d . . . N9 N 0.8431(4) -0.2463(4) 0.35924(17) 0.0276(12) Uani 1 1 d . . . N10 N 0.4680(4) -0.2899(4) 0.32377(17) 0.0284(13) Uani 1 1 d . . . N11 N 0.6337(4) -0.3465(4) 0.32014(16) 0.0258(12) Uani 1 1 d . . . N12 N 0.8002(4) -0.4021(4) 0.31822(17) 0.0273(12) Uani 1 1 d . . . N13 N 0.9709(4) -0.4353(4) 0.3208(2) 0.0376(15) Uani 1 1 d . . . N14 N 0.8928(4) -0.4550(4) 0.39496(18) 0.0300(13) Uani 1 1 d . . . N15 N 0.8100(4) -0.4695(4) 0.46917(18) 0.0338(14) Uani 1 1 d . . . N16 N 0.7313(4) -0.3207(4) 0.44260(16) 0.0239(12) Uani 1 1 d . . . N17 N 0.6423(4) -0.1900(4) 0.41186(16) 0.0230(12) Uani 1 1 d . . . N18 N 0.5496(4) -0.0624(4) 0.38112(17) 0.0263(12) Uani 1 1 d . . . N19 N 0.9355(4) 0.4206(4) 0.11586(16) 0.0287(13) Uani 1 1 d . . . N20 N 0.8462(4) 0.3341(4) 0.08263(16) 0.0293(13) Uani 1 1 d . . . N21 N 0.7587(4) 0.2416(4) 0.05106(17) 0.0311(13) Uani 1 1 d . . . N22 N 0.6788(5) 0.1308(4) 0.02390(19) 0.0412(16) Uani 1 1 d . . . N23 N 0.5930(4) 0.1461(4) 0.09787(18) 0.0348(14) Uani 1 1 d . . . N24 N 0.5118(5) 0.1588(4) 0.1730(2) 0.0413(15) Uani 1 1 d . . . N25 N 0.6825(4) 0.1414(4) 0.17503(17) 0.0302(13) Uani 1 1 d . . . N26 N 0.8485(4) 0.1454(4) 0.17452(16) 0.0274(13) Uani 1 1 d . . . N27 N 1.0129(4) 0.1489(4) 0.17326(17) 0.0301(13) Uani 1 1 d . . . N28 N 0.8153(4) 0.0617(4) 0.09632(17) 0.0320(13) Uani 1 1 d . . . N29 N 0.9396(4) 0.1535(4) 0.09075(17) 0.0296(13) Uani 1 1 d . . . N30 N 1.0610(4) 0.2455(4) 0.08987(17) 0.0326(14) Uani 1 1 d . . . N31 N 1.1680(5) 0.3586(5) 0.0899(2) 0.0423(16) Uani 1 1 d . . . N32 N 1.1038(4) 0.3326(4) 0.16526(18) 0.0326(14) Uani 1 1 d . . . N33 N 1.0363(5) 0.3001(4) 0.24004(18) 0.0385(15) Uani 1 1 d . . . N34 N 0.8976(4) 0.3261(4) 0.20548(16) 0.0276(13) Uani 1 1 d . . . N35 N 0.7700(4) 0.3293(4) 0.16795(16) 0.0257(12) Uani 1 1 d . . . N36 N 0.6404(4) 0.3270(4) 0.13243(17) 0.0297(13) Uani 1 1 d . . . C11 C 0.7025(5) -0.5632(5) 0.3960(2) 0.0298(15) Uani 1 1 d . . . H11A H 0.7707 -0.5862 0.3898 0.036 Uiso 1 1 calc R . . C12 C 0.6387(6) -0.6288(5) 0.4025(2) 0.0368(18) Uani 1 1 d . . . H12A H 0.6625 -0.6950 0.4002 0.044 Uiso 1 1 calc R . . C13 C 0.5382(6) -0.5949(5) 0.4125(2) 0.0435(19) Uani 1 1 d . . . H13A H 0.4928 -0.6384 0.4176 0.052 Uiso 1 1 calc R . . C14 C 0.5052(5) -0.4987(5) 0.4150(2) 0.0338(16) Uani 1 1 d . . . H14A H 0.4371 -0.4750 0.4215 0.041 Uiso 1 1 calc R . . C15 C 0.5749(5) -0.4350(5) 0.4075(2) 0.0265(15) Uani 1 1 d . . . C21 C 0.4631(5) -0.2878(5) 0.4286(2) 0.0252(14) Uani 1 1 d . . . C22 C 0.4206(5) -0.3155(5) 0.4713(2) 0.0314(16) Uani 1 1 d . . . H22A H 0.4452 -0.3746 0.4843 0.038 Uiso 1 1 calc R . . C23 C 0.3427(5) -0.2550(5) 0.4936(2) 0.0396(18) Uani 1 1 d . . . H23A H 0.3126 -0.2730 0.5221 0.048 Uiso 1 1 calc R . . C24 C 0.3082(5) -0.1682(6) 0.4748(2) 0.0384(18) Uani 1 1 d . . . H24A H 0.2559 -0.1256 0.4904 0.046 Uiso 1 1 calc R . . C25 C 0.3516(5) -0.1445(5) 0.4325(2) 0.0307(16) Uani 1 1 d . . . C31 C 0.3018(5) -0.0433(5) 0.3689(2) 0.0331(16) Uani 1 1 d . . . C32 C 0.2135(6) 0.0084(5) 0.3608(3) 0.045(2) Uani 1 1 d . . . H32A H 0.1634 0.0330 0.3839 0.054 Uiso 1 1 calc R . . C33 C 0.2011(6) 0.0227(6) 0.3180(3) 0.053(2) Uani 1 1 d . . . H33A H 0.1415 0.0575 0.3117 0.064 Uiso 1 1 calc R . . C34 C 0.2739(6) -0.0129(6) 0.2846(3) 0.049(2) Uani 1 1 d . . . H34A H 0.2650 -0.0017 0.2554 0.059 Uiso 1 1 calc R . . C35 C 0.3614(6) -0.0656(5) 0.2937(2) 0.0374(18) Uani 1 1 d . . . C41 C 0.5363(6) -0.1187(5) 0.2558(2) 0.0354(17) Uani 1 1 d . . . C42 C 0.5948(6) -0.1122(6) 0.2143(2) 0.045(2) Uani 1 1 d . . . H42A H 0.5658 -0.0973 0.1894 0.054 Uiso 1 1 calc R . . C43 C 0.6944(7) -0.1280(6) 0.2106(2) 0.047(2) Uani 1 1 d . . . H43A H 0.7343 -0.1228 0.1827 0.056 Uiso 1 1 calc R . . C44 C 0.7393(6) -0.1514(5) 0.2467(2) 0.0378(18) Uani 1 1 d . . . H44A H 0.8085 -0.1636 0.2436 0.045 Uiso 1 1 calc R . . C45 C 0.6771(5) -0.1562(5) 0.2881(2) 0.0297(16) Uani 1 1 d . . . C51 C 0.8019(5) -0.1792(5) 0.3329(2) 0.0275(15) Uani 1 1 d . . . C52 C 0.8501(6) -0.1008(5) 0.3161(2) 0.0398(18) Uani 1 1 d . . . H52A H 0.8202 -0.0525 0.2984 0.048 Uiso 1 1 calc R . . C53 C 0.9403(7) -0.0949(6) 0.3255(3) 0.053(2) Uani 1 1 d . . . H53A H 0.9729 -0.0432 0.3138 0.064 Uiso 1 1 calc R . . C54 C 0.9834(6) -0.1645(6) 0.3521(3) 0.051(2) Uani 1 1 d . . . H54A H 1.0456 -0.1621 0.3588 0.061 Uiso 1 1 calc R . . C55 C 0.9312(5) -0.2381(5) 0.3685(2) 0.0370(17) Uani 1 1 d . . . H55A H 0.9590 -0.2854 0.3873 0.044 Uiso 1 1 calc R . . C61 C 0.3779(6) -0.3015(6) 0.3177(2) 0.0412(18) Uani 1 1 d . . . H61A H 0.3237 -0.2543 0.3281 0.049 Uiso 1 1 calc R . . C62 C 0.3604(6) -0.3775(6) 0.2972(3) 0.055(2) Uani 1 1 d . . . H62A H 0.2967 -0.3820 0.2929 0.066 Uiso 1 1 calc R . . C63 C 0.4402(6) -0.4474(6) 0.2831(3) 0.052(2) Uani 1 1 d . . . H63A H 0.4313 -0.5006 0.2688 0.062 Uiso 1 1 calc R . . C64 C 0.5321(6) -0.4399(5) 0.2898(2) 0.0377(18) Uani 1 1 d . . . H64A H 0.5858 -0.4889 0.2811 0.045 Uiso 1 1 calc R . . C65 C 0.5458(5) -0.3585(5) 0.3098(2) 0.0288(15) Uani 1 1 d . . . C71 C 0.7240(5) -0.3838(5) 0.2962(2) 0.0279(15) Uani 1 1 d . . . C72 C 0.7423(6) -0.3909(5) 0.2506(2) 0.0348(17) Uani 1 1 d . . . H72A H 0.6903 -0.3777 0.2350 0.042 Uiso 1 1 calc R . . C73 C 0.8374(6) -0.4173(5) 0.2296(2) 0.043(2) Uani 1 1 d . . . H73A H 0.8503 -0.4243 0.1991 0.052 Uiso 1 1 calc R . . C74 C 0.9154(6) -0.4342(5) 0.2517(2) 0.044(2) Uani 1 1 d . . . H74A H 0.9808 -0.4515 0.2368 0.053 Uiso 1 1 calc R . . C75 C 0.8937(5) -0.4246(5) 0.2968(2) 0.0339(17) Uani 1 1 d . . . C81 C 0.9713(5) -0.4786(5) 0.3630(2) 0.0360(17) Uani 1 1 d . . . C82 C 1.0516(6) -0.5409(6) 0.3714(3) 0.048(2) Uani 1 1 d . . . H82A H 1.1060 -0.5576 0.3487 0.058 Uiso 1 1 calc R . . C83 C 1.0533(6) -0.5789(6) 0.4126(3) 0.051(2) Uani 1 1 d . . . H83A H 1.1086 -0.6226 0.4183 0.061 Uiso 1 1 calc R . . C84 C 0.9749(5) -0.5542(5) 0.4461(3) 0.0419(19) Uani 1 1 d . . . H84A H 0.9763 -0.5787 0.4749 0.050 Uiso 1 1 calc R . . C85 C 0.8940(5) -0.4921(5) 0.4361(2) 0.0332(16) Uani 1 1 d . . . C91 C 0.7537(5) -0.3781(5) 0.4772(2) 0.0281(15) Uani 1 1 d . . . C92 C 0.7193(5) -0.3481(5) 0.5195(2) 0.0344(17) Uani 1 1 d . . . H92A H 0.7364 -0.3874 0.5434 0.041 Uiso 1 1 calc R . . C93 C 0.6598(5) -0.2600(5) 0.5264(2) 0.0355(17) Uani 1 1 d . . . H93A H 0.6370 -0.2389 0.5551 0.043 Uiso 1 1 calc R . . C94 C 0.6335(5) -0.2026(5) 0.4915(2) 0.0308(16) Uani 1 1 d . . . H94A H 0.5917 -0.1431 0.4960 0.037 Uiso 1 1 calc R . . C95 C 0.6708(5) -0.2353(4) 0.4492(2) 0.0255(14) Uani 1 1 d . . . C101 C 0.6139(5) -0.0922(5) 0.4081(2) 0.0266(15) Uani 1 1 d . . . C102 C 0.6543(5) -0.0268(5) 0.4281(2) 0.0344(17) Uani 1 1 d . . . H10A H 0.7003 -0.0488 0.4463 0.041 Uiso 1 1 calc R . . C103 C 0.6255(6) 0.0699(5) 0.4207(2) 0.0414(19) Uani 1 1 d . . . H10B H 0.6515 0.1149 0.4340 0.050 Uiso 1 1 calc R . . C104 C 0.5575(5) 0.1011(5) 0.3935(2) 0.0362(17) Uani 1 1 d . . . H10C H 0.5362 0.1671 0.3884 0.043 Uiso 1 1 calc R . . C105 C 0.5226(5) 0.0335(5) 0.3744(2) 0.0339(17) Uani 1 1 d . . . H10D H 0.4777 0.0545 0.3556 0.041 Uiso 1 1 calc R . . C111 C 0.9634(5) 0.5038(5) 0.1224(2) 0.0352(17) Uani 1 1 d . . . H11B H 1.0049 0.5038 0.1428 0.042 Uiso 1 1 calc R . . C112 C 0.9339(6) 0.5903(5) 0.1006(2) 0.046(2) Uani 1 1 d . . . H11C H 0.9566 0.6470 0.1052 0.055 Uiso 1 1 calc R . . C113 C 0.8706(7) 0.5898(6) 0.0724(3) 0.051(2) Uani 1 1 d . . . H11D H 0.8472 0.6476 0.0580 0.061 Uiso 1 1 calc R . . C114 C 0.8409(6) 0.5049(5) 0.0647(2) 0.0436(19) Uani 1 1 d . . . H11E H 0.7981 0.5044 0.0450 0.052 Uiso 1 1 calc R . . C115 C 0.8753(5) 0.4200(5) 0.0867(2) 0.0303(16) Uani 1 1 d . . . C121 C 0.8210(5) 0.3077(5) 0.0449(2) 0.0317(16) Uani 1 1 d . . . C122 C 0.8620(6) 0.3389(6) 0.0028(2) 0.0405(18) Uani 1 1 d . . . H12B H 0.9054 0.3842 -0.0015 0.049 Uiso 1 1 calc R . . C123 C 0.8369(6) 0.3012(6) -0.0324(2) 0.047(2) Uani 1 1 d . . . H12C H 0.8619 0.3229 -0.0610 0.057 Uiso 1 1 calc R . . C124 C 0.7758(7) 0.2325(6) -0.0263(2) 0.049(2) Uani 1 1 d . . . H12D H 0.7607 0.2059 -0.0504 0.058 Uiso 1 1 calc R . . C125 C 0.7371(6) 0.2034(5) 0.0160(2) 0.0361(17) Uani 1 1 d . . . C131 C 0.5908(6) 0.1314(5) 0.0557(3) 0.0419(19) Uani 1 1 d . . . C132 C 0.5069(7) 0.1133(7) 0.0432(3) 0.064(3) Uani 1 1 d . . . H13B H 0.5050 0.1082 0.0134 0.076 Uiso 1 1 calc R . . C133 C 0.4255(7) 0.1029(8) 0.0755(4) 0.070(3) Uani 1 1 d . . . H13C H 0.3677 0.0893 0.0679 0.084 Uiso 1 1 calc R . . C134 C 0.4289(6) 0.1125(7) 0.1189(3) 0.057(2) Uani 1 1 d . . . H13D H 0.3751 0.1021 0.1411 0.069 Uiso 1 1 calc R . . C135 C 0.5134(6) 0.1378(5) 0.1293(3) 0.0405(18) Uani 1 1 d . . . C141 C 0.5894(6) 0.1373(5) 0.1964(2) 0.0375(18) Uani 1 1 d . . . C142 C 0.5692(6) 0.1163(6) 0.2411(2) 0.047(2) Uani 1 1 d . . . H14B H 0.5045 0.1108 0.2556 0.056 Uiso 1 1 calc R . . C143 C 0.6460(6) 0.1035(6) 0.2640(2) 0.048(2) Uani 1 1 d . . . H14C H 0.6330 0.0906 0.2945 0.057 Uiso 1 1 calc R . . C144 C 0.7404(6) 0.1095(5) 0.2430(2) 0.0376(18) Uani 1 1 d . . . H14D H 0.7924 0.1003 0.2587 0.045 Uiso 1 1 calc R . . C145 C 0.7583(5) 0.1292(5) 0.1980(2) 0.0302(16) Uani 1 1 d . . . C151 C 0.9365(6) 0.1004(5) 0.1846(2) 0.0322(16) Uani 1 1 d . . . C152 C 0.9499(6) 0.0051(5) 0.2024(2) 0.045(2) Uani 1 1 d . . . H15A H 0.8957 -0.0278 0.2111 0.053 Uiso 1 1 calc R . . C153 C 1.0421(7) -0.0385(6) 0.2066(3) 0.056(2) Uani 1 1 d . . . H15B H 1.0521 -0.1013 0.2190 0.067 Uiso 1 1 calc R . . C154 C 1.1215(7) 0.0103(6) 0.1927(3) 0.061(3) Uani 1 1 d . . . H15C H 1.1863 -0.0197 0.1942 0.074 Uiso 1 1 calc R . . C155 C 1.1034(6) 0.1026(6) 0.1769(2) 0.0405(18) Uani 1 1 d . . . H15D H 1.1571 0.1360 0.1680 0.049 Uiso 1 1 calc R . . C161 C 0.7859(6) -0.0250(5) 0.0983(2) 0.0373(18) Uani 1 1 d . . . H16A H 0.7177 -0.0268 0.1035 0.045 Uiso 1 1 calc R . . C162 C 0.8489(7) -0.1099(6) 0.0933(2) 0.048(2) Uani 1 1 d . . . H16B H 0.8251 -0.1686 0.0946 0.057 Uiso 1 1 calc R . . C163 C 0.9497(7) -0.1070(6) 0.0861(3) 0.051(2) Uani 1 1 d . . . H16C H 0.9953 -0.1646 0.0831 0.061 Uiso 1 1 calc R . . C164 C 0.9829(6) -0.0206(5) 0.0835(2) 0.0410(19) Uani 1 1 d . . . H16D H 1.0510 -0.0184 0.0782 0.049 Uiso 1 1 calc R . . C165 C 0.9139(5) 0.0647(5) 0.0887(2) 0.0313(16) Uani 1 1 d . . . C171 C 1.0291(5) 0.1777(5) 0.0703(2) 0.0332(16) Uani 1 1 d . . . C172 C 1.0822(6) 0.1425(6) 0.0298(2) 0.043(2) Uani 1 1 d . . . H17A H 1.0593 0.0970 0.0155 0.052 Uiso 1 1 calc R . . C173 C 1.1683(6) 0.1767(6) 0.0119(2) 0.051(2) Uani 1 1 d . . . H17B H 1.2067 0.1516 -0.0144 0.062 Uiso 1 1 calc R . . C174 C 1.1992(6) 0.2469(6) 0.0315(2) 0.048(2) Uani 1 1 d . . . H17C H 1.2575 0.2708 0.0187 0.058 Uiso 1 1 calc R . . C175 C 1.1432(6) 0.2816(5) 0.0704(2) 0.0378(18) Uani 1 1 d . . . C181 C 1.1758(6) 0.3606(5) 0.1341(2) 0.0384(18) Uani 1 1 d . . . C182 C 1.2552(6) 0.3941(6) 0.1451(3) 0.054(2) Uani 1 1 d . . . H18A H 1.3053 0.4136 0.1231 0.065 Uiso 1 1 calc R . . C183 C 1.2592(6) 0.3983(6) 0.1883(3) 0.056(2) Uani 1 1 d . . . H18B H 1.3118 0.4219 0.1963 0.067 Uiso 1 1 calc R . . C184 C 1.1866(6) 0.3683(6) 0.2200(3) 0.049(2) Uani 1 1 d . . . H18C H 1.1896 0.3702 0.2498 0.059 Uiso 1 1 calc R . . C185 C 1.1082(6) 0.3348(5) 0.2079(2) 0.0381(18) Uani 1 1 d . . . C191 C 0.9333(6) 0.3206(5) 0.2427(2) 0.0351(17) Uani 1 1 d . . . C192 C 0.8709(6) 0.3325(6) 0.2830(2) 0.044(2) Uani 1 1 d . . . H19A H 0.8965 0.3312 0.3088 0.053 Uiso 1 1 calc R . . C193 C 0.7705(7) 0.3464(6) 0.2847(2) 0.048(2) Uani 1 1 d . . . H19B H 0.7274 0.3547 0.3119 0.057 Uiso 1 1 calc R . . C194 C 0.7320(6) 0.3486(5) 0.2471(2) 0.0378(18) Uani 1 1 d . . . H19C H 0.6634 0.3562 0.2485 0.045 Uiso 1 1 calc R . . C195 C 0.7974(5) 0.3390(4) 0.2071(2) 0.0271(15) Uani 1 1 d . . . C201 C 0.6790(5) 0.3731(5) 0.1591(2) 0.0287(15) Uani 1 1 d . . . C202 C 0.6317(6) 0.4632(5) 0.1748(2) 0.0419(19) Uani 1 1 d . . . H20A H 0.6589 0.4951 0.1937 0.050 Uiso 1 1 calc R . . C203 C 0.5459(6) 0.5035(6) 0.1619(3) 0.049(2) Uani 1 1 d . . . H20B H 0.5130 0.5635 0.1724 0.058 Uiso 1 1 calc R . . C204 C 0.5068(6) 0.4577(6) 0.1338(3) 0.047(2) Uani 1 1 d . . . H20C H 0.4478 0.4857 0.1247 0.057 Uiso 1 1 calc R . . C205 C 0.5563(5) 0.3693(5) 0.1194(2) 0.0390(18) Uani 1 1 d . . . H20D H 0.5306 0.3376 0.0998 0.047 Uiso 1 1 calc R . . C1 C 0.2688(6) 0.0212(6) 0.4417(3) 0.049(2) Uani 1 1 d . . . H1A H 0.2857 0.0062 0.4704 0.074 Uiso 1 1 calc R . . H1B H 0.1978 0.0265 0.4441 0.074 Uiso 1 1 calc R . . H1C H 0.2894 0.0818 0.4302 0.074 Uiso 1 1 calc R . . C2 C 0.3965(7) -0.1325(7) 0.2213(3) 0.065(3) Uani 1 1 d . . . H2A H 0.3249 -0.1243 0.2278 0.098 Uiso 1 1 calc R . . H2B H 0.4230 -0.1987 0.2140 0.098 Uiso 1 1 calc R . . H2C H 0.4178 -0.0898 0.1968 0.098 Uiso 1 1 calc R . . C3 C 1.0680(6) -0.4176(6) 0.2959(3) 0.055(2) Uani 1 1 d . . . H3A H 1.1154 -0.4267 0.3154 0.082 Uiso 1 1 calc R . . H3B H 1.0622 -0.3522 0.2836 0.082 Uiso 1 1 calc R . . H3C H 1.0904 -0.4624 0.2725 0.082 Uiso 1 1 calc R . . C4 C 0.7975(6) -0.5417(6) 0.5055(3) 0.048(2) Uani 1 1 d . . . H4A H 0.7384 -0.5195 0.5267 0.072 Uiso 1 1 calc R . . H4B H 0.8545 -0.5511 0.5196 0.072 Uiso 1 1 calc R . . H4C H 0.7912 -0.6021 0.4943 0.072 Uiso 1 1 calc R . . C5 C 0.6887(7) 0.0653(6) -0.0125(3) 0.062(3) Uani 1 1 d . . . H5A H 0.7507 0.0686 -0.0327 0.093 Uiso 1 1 calc R . . H5B H 0.6342 0.0847 -0.0279 0.093 Uiso 1 1 calc R . . H5C H 0.6878 -0.0001 -0.0006 0.093 Uiso 1 1 calc R . . C6 C 0.4148(6) 0.1886(7) 0.1996(3) 0.064(3) Uani 1 1 d . . . H6A H 0.4219 0.2010 0.2289 0.095 Uiso 1 1 calc R . . H6B H 0.3752 0.1380 0.2011 0.095 Uiso 1 1 calc R . . H6C H 0.3825 0.2468 0.1865 0.095 Uiso 1 1 calc R . . C7 C 1.2190(7) 0.4267(7) 0.0599(3) 0.067(3) Uani 1 1 d . . . H7A H 1.2095 0.4198 0.0304 0.100 Uiso 1 1 calc R . . H7B H 1.2890 0.4137 0.0607 0.100 Uiso 1 1 calc R . . H7C H 1.1921 0.4918 0.0688 0.100 Uiso 1 1 calc R . . C8 C 1.0692(7) 0.2589(6) 0.2807(3) 0.056(2) Uani 1 1 d . . . H8A H 1.1408 0.2470 0.2758 0.084 Uiso 1 1 calc R . . H8B H 1.0442 0.1989 0.2892 0.084 Uiso 1 1 calc R . . H8C H 1.0440 0.3039 0.3040 0.084 Uiso 1 1 calc R . . P1 P 0.3298(9) 0.2959(8) 0.3342(3) 0.0439(10) Uani 0.491(7) 1 d PD A 1 F1 F 0.2226(10) 0.2802(13) 0.3572(5) 0.110(5) Uani 0.491(7) 1 d PD A 1 F2 F 0.4343(9) 0.3121(14) 0.3101(7) 0.141(7) Uani 0.491(7) 1 d PD A 1 F3 F 0.3256(14) 0.2234(9) 0.2991(5) 0.099(5) Uani 0.491(7) 1 d PD A 1 F4 F 0.3728(16) 0.2097(13) 0.3631(6) 0.150(8) Uani 0.491(7) 1 d PD A 1 F5 F 0.3316(18) 0.3667(14) 0.3701(5) 0.131(6) Uani 0.491(7) 1 d PD A 1 F6 F 0.2835(10) 0.3818(7) 0.3063(4) 0.093(3) Uani 0.491(7) 1 d PD A 1 P1B P 0.3439(9) 0.2870(8) 0.3310(3) 0.0439(10) Uani 0.509(7) 1 d PD A 2 F1B F 0.2315(9) 0.2919(13) 0.3292(5) 0.110(5) Uani 0.509(7) 1 d PD A 2 F2B F 0.4547(10) 0.2803(14) 0.3329(6) 0.141(7) Uani 0.509(7) 1 d PD A 2 F3B F 0.3657(13) 0.1863(8) 0.3098(5) 0.099(5) Uani 0.509(7) 1 d PD A 2 F4B F 0.3249(16) 0.2335(15) 0.3773(4) 0.150(8) Uani 0.509(7) 1 d PD A 2 F5B F 0.3200(17) 0.3857(12) 0.3534(5) 0.131(6) Uani 0.509(7) 1 d PD A 2 F6B F 0.3611(11) 0.3386(8) 0.2847(3) 0.093(3) Uani 0.509(7) 1 d PD A 2 P2 P 0.9185(4) 0.1636(4) 0.40683(19) 0.0478(7) Uani 0.753(7) 1 d PD B 1 F7 F 0.9673(8) 0.0987(8) 0.3674(3) 0.107(3) Uani 0.753(7) 1 d PD B 1 F8 F 0.8737(7) 0.2299(7) 0.4471(3) 0.101(3) Uani 0.753(7) 1 d PD B 1 F9 F 1.0137(6) 0.1359(9) 0.4270(3) 0.131(5) Uani 0.753(7) 1 d PD B 1 F10 F 0.9590(9) 0.2528(6) 0.3811(3) 0.118(5) Uani 0.753(7) 1 d PD B 1 F11 F 0.8227(6) 0.1935(7) 0.3873(3) 0.125(4) Uani 0.753(7) 1 d PD B 1 F12 F 0.8706(7) 0.0793(6) 0.4332(3) 0.108(3) Uani 0.753(7) 1 d PD B 1 P2B P 0.9267(12) 0.1659(12) 0.4087(6) 0.0478(7) Uani 0.247(7) 1 d PD B 2 F7B F 0.949(2) 0.108(2) 0.3660(7) 0.107(3) Uani 0.247(7) 1 d PD B 2 F8B F 0.904(2) 0.224(2) 0.4515(7) 0.101(3) Uani 0.247(7) 1 d PD B 2 F9B F 1.0335(13) 0.192(2) 0.3983(9) 0.131(5) Uani 0.247(7) 1 d PD B 2 F10B F 0.890(2) 0.2596(16) 0.3828(8) 0.118(5) Uani 0.247(7) 1 d PD B 2 F11B F 0.8191(13) 0.143(2) 0.4195(10) 0.125(4) Uani 0.247(7) 1 d PD B 2 F12B F 0.963(2) 0.0731(15) 0.4353(8) 0.108(3) Uani 0.247(7) 1 d PD B 2 P3 P 1.1844(4) 0.6856(4) 0.16854(17) 0.0848(10) Uani 0.806(7) 1 d PD C 1 F13 F 1.2513(10) 0.7575(7) 0.1767(5) 0.257(10) Uani 0.806(7) 1 d PD C 1 F14 F 1.1150(6) 0.6152(7) 0.1621(4) 0.167(6) Uani 0.806(7) 1 d PD C 1 F15 F 1.2305(9) 0.6118(6) 0.2021(3) 0.146(5) Uani 0.806(7) 1 d PD C 1 F16 F 1.2661(7) 0.6375(8) 0.1309(3) 0.155(5) Uani 0.806(7) 1 d PD C 1 F17 F 1.1417(8) 0.7602(6) 0.1351(2) 0.138(4) Uani 0.806(7) 1 d PD C 1 F18 F 1.1005(10) 0.7293(7) 0.2062(3) 0.228(9) Uani 0.806(7) 1 d PD C 1 P3B P 1.1913(16) 0.6813(15) 0.1669(6) 0.0848(10) Uani 0.194(7) 1 d PD C 2 F13B F 1.230(3) 0.764(2) 0.1355(11) 0.257(10) Uani 0.194(7) 1 d PD C 2 F14B F 1.151(2) 0.599(2) 0.1981(11) 0.167(6) Uani 0.194(7) 1 d PD C 2 F15B F 1.183(3) 0.745(2) 0.2069(9) 0.146(5) Uani 0.194(7) 1 d PD C 2 F16B F 1.2998(17) 0.638(3) 0.1714(12) 0.155(5) Uani 0.194(7) 1 d PD C 2 F17B F 1.201(3) 0.618(2) 0.1268(9) 0.138(4) Uani 0.194(7) 1 d PD C 2 F18B F 1.083(2) 0.724(2) 0.1625(12) 0.228(9) Uani 0.194(7) 1 d PD C 2 P4 P 1.4317(15) 0.1217(16) -0.0788(6) 0.122(2) Uani 0.219(6) 1 d PD D 1 F19 F 1.365(3) 0.070(3) -0.0413(10) 0.213(7) Uani 0.219(6) 1 d PD D 1 F20 F 1.501(3) 0.172(3) -0.1161(11) 0.357(16) Uani 0.219(6) 1 d PD D 1 F21 F 1.414(3) 0.054(2) -0.1130(10) 0.177(6) Uani 0.219(6) 1 d PD D 1 F22 F 1.524(2) 0.047(3) -0.0700(14) 0.52(3) Uani 0.219(6) 1 d PD D 1 F23 F 1.452(3) 0.188(3) -0.0445(12) 0.260(9) Uani 0.219(6) 1 d PD D 1 F24 F 1.341(3) 0.196(3) -0.0875(16) 0.59(3) Uani 0.219(6) 1 d PD D 1 P4B P 1.4225(4) 0.2109(5) -0.08636(16) 0.122(2) Uani 0.781(6) 1 d PD D 2 F19B F 1.3827(10) 0.1447(9) -0.0472(4) 0.213(7) Uani 0.781(6) 1 d PD D 2 F20B F 1.4679(14) 0.2718(9) -0.1272(4) 0.357(16) Uani 0.781(6) 1 d PD D 2 F21B F 1.4552(10) 0.1165(6) -0.1115(4) 0.177(6) Uani 0.781(6) 1 d PD D 2 F22B F 1.5225(8) 0.1992(14) -0.0695(5) 0.52(3) Uani 0.781(6) 1 d PD D 2 F23B F 1.3841(11) 0.3050(8) -0.0593(5) 0.260(9) Uani 0.781(6) 1 d PD D 2 F24B F 1.3222(9) 0.2278(13) -0.1036(6) 0.59(3) Uani 0.781(6) 1 d PD D 2 O1 O 1.0257(16) 0.6981(9) 0.4577(5) 0.165(8) Uani 0.89(3) 1 d PD E 1 C1S C 1.0037(8) 0.7834(8) 0.4653(4) 0.057(3) Uani 0.89(3) 1 d PD E 1 C2S C 0.9060(8) 0.8207(15) 0.4854(5) 0.104(6) Uani 0.89(3) 1 d PD E 1 H2SA H 0.8677 0.7687 0.4925 0.156 Uiso 0.89(3) 1 calc PR E 1 H2SB H 0.8763 0.8673 0.4654 0.156 Uiso 0.89(3) 1 calc PR E 1 H2SC H 0.9071 0.8518 0.5120 0.156 Uiso 0.89(3) 1 calc PR E 1 C3S C 1.0731(13) 0.8467(17) 0.4524(7) 0.183(12) Uani 0.89(3) 1 d PD E 1 H3SA H 1.1359 0.8108 0.4386 0.275 Uiso 0.89(3) 1 calc PR E 1 H3SB H 1.0818 0.8772 0.4779 0.275 Uiso 0.89(3) 1 calc PR E 1 H3SC H 1.0494 0.8955 0.4317 0.275 Uiso 0.89(3) 1 calc PR E 1 O1B O 1.078(9) 0.709(8) 0.438(3) 0.165(8) Uani 0.11(3) 1 d PD E 2 C1SB C 1.019(6) 0.774(7) 0.457(3) 0.057(3) Uani 0.11(3) 1 d PD E 2 C2SB C 0.933(8) 0.753(12) 0.485(4) 0.104(6) Uani 0.11(3) 1 d PD E 2 H2SD H 0.9327 0.6836 0.4867 0.156 Uiso 0.11(3) 1 calc PR E 2 H2SE H 0.8753 0.7853 0.4740 0.156 Uiso 0.11(3) 1 calc PR E 2 H2SF H 0.9299 0.7740 0.5145 0.156 Uiso 0.11(3) 1 calc PR E 2 C3SB C 1.038(11) 0.869(7) 0.452(6) 0.183(12) Uani 0.11(3) 1 d PD E 2 H3SD H 1.1090 0.8686 0.4449 0.275 Uiso 0.11(3) 1 calc PR E 2 H3SE H 1.0097 0.9032 0.4781 0.275 Uiso 0.11(3) 1 calc PR E 2 H3SF H 1.0090 0.9008 0.4274 0.275 Uiso 0.11(3) 1 calc PR E 2 O2 O 1.6785(10) 0.0780(10) -0.1230(3) 0.171(5) Uani 1 1 d . . . O3 O 1.458(2) 0.4095(17) 0.0325(9) 0.191(11) Uiso 0.50 1 d PD . . C4S C 1.435(2) 0.4736(19) 0.0056(10) 0.51(7) Uiso 0.50 1 d PD . . C5S C 1.431(2) 0.5716(18) 0.0133(11) 0.145(12) Uiso 0.50 1 d PD . . H5SA H 1.4600 0.5767 0.0386 0.218 Uiso 0.50 1 calc PR . . H5SB H 1.3624 0.6030 0.0188 0.218 Uiso 0.50 1 calc PR . . H5SC H 1.4670 0.6023 -0.0122 0.218 Uiso 0.50 1 calc PR . . C6S C 1.405(7) 0.447(4) -0.0317(18) 0.55(7) Uiso 0.50 1 d PD . . H6SA H 1.4166 0.3771 -0.0328 0.818 Uiso 0.50 1 calc PR . . H6SB H 1.4429 0.4738 -0.0579 0.818 Uiso 0.50 1 calc PR . . H6SC H 1.3353 0.4707 -0.0302 0.818 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0283(5) 0.0228(4) 0.0200(4) -0.0008(3) -0.0046(4) -0.0019(4) Ni2 0.0252(4) 0.0194(4) 0.0162(4) -0.0003(3) -0.0005(3) -0.0043(3) Ni3 0.0245(5) 0.0234(4) 0.0223(4) -0.0007(3) -0.0003(3) -0.0021(4) Ni4 0.0367(5) 0.0274(5) 0.0221(4) -0.0005(3) -0.0048(4) -0.0062(4) Ni5 0.0340(5) 0.0222(4) 0.0151(4) 0.0009(3) -0.0025(3) -0.0025(4) Ni6 0.0357(5) 0.0283(5) 0.0190(4) 0.0014(3) -0.0051(4) -0.0061(4) N1 0.031(3) 0.021(3) 0.023(3) 0.004(2) -0.001(2) -0.002(2) N2 0.025(3) 0.025(3) 0.019(3) 0.002(2) 0.002(2) -0.005(2) N3 0.024(3) 0.029(3) 0.024(3) -0.005(2) -0.002(2) -0.003(2) N4 0.030(3) 0.032(3) 0.035(3) -0.007(3) -0.002(3) 0.001(3) N5 0.038(3) 0.029(3) 0.028(3) -0.003(2) -0.008(3) -0.006(3) N6 0.048(4) 0.044(4) 0.029(3) -0.003(3) -0.016(3) -0.006(3) N7 0.035(3) 0.023(3) 0.021(3) 0.000(2) -0.002(2) -0.005(2) N8 0.032(3) 0.021(3) 0.024(3) 0.002(2) -0.004(2) -0.009(2) N9 0.029(3) 0.023(3) 0.030(3) -0.006(2) 0.001(2) -0.007(2) N10 0.034(3) 0.025(3) 0.027(3) 0.001(2) -0.007(3) -0.007(3) N11 0.032(3) 0.024(3) 0.020(3) -0.003(2) 0.000(2) -0.004(2) N12 0.032(3) 0.022(3) 0.025(3) -0.005(2) 0.005(3) -0.007(2) N13 0.022(3) 0.039(4) 0.047(4) -0.009(3) 0.008(3) -0.003(3) N14 0.026(3) 0.026(3) 0.034(3) 0.002(2) 0.000(3) -0.002(2) N15 0.037(4) 0.030(3) 0.035(3) 0.006(3) -0.012(3) -0.003(3) N16 0.021(3) 0.023(3) 0.026(3) 0.001(2) -0.002(2) -0.003(2) N17 0.030(3) 0.018(3) 0.021(3) -0.003(2) -0.006(2) -0.001(2) N18 0.028(3) 0.022(3) 0.027(3) -0.002(2) -0.001(2) -0.001(2) N19 0.037(3) 0.027(3) 0.019(3) 0.002(2) -0.001(2) -0.006(3) N20 0.040(3) 0.026(3) 0.021(3) 0.003(2) -0.006(3) -0.004(3) N21 0.044(4) 0.029(3) 0.021(3) 0.001(2) -0.010(3) -0.004(3) N22 0.056(4) 0.039(4) 0.034(3) -0.006(3) -0.015(3) -0.010(3) N23 0.044(4) 0.031(3) 0.030(3) -0.006(3) -0.007(3) -0.006(3) N24 0.039(4) 0.040(4) 0.042(4) -0.005(3) 0.003(3) -0.007(3) N25 0.044(4) 0.021(3) 0.025(3) -0.002(2) -0.003(3) -0.008(3) N26 0.037(3) 0.023(3) 0.021(3) 0.003(2) -0.004(2) -0.004(3) N27 0.039(4) 0.032(3) 0.020(3) 0.000(2) -0.009(3) -0.001(3) N28 0.046(4) 0.028(3) 0.023(3) -0.003(2) -0.006(3) -0.005(3) N29 0.040(4) 0.027(3) 0.020(3) -0.004(2) 0.000(3) -0.005(3) N30 0.032(3) 0.037(3) 0.026(3) 0.002(3) -0.003(3) -0.002(3) N31 0.042(4) 0.046(4) 0.039(4) 0.011(3) -0.002(3) -0.018(3) N32 0.040(4) 0.029(3) 0.031(3) 0.000(2) -0.011(3) -0.006(3) N33 0.055(4) 0.040(4) 0.025(3) 0.003(3) -0.019(3) -0.008(3) N34 0.042(4) 0.024(3) 0.018(3) 0.000(2) -0.004(2) -0.009(3) N35 0.032(3) 0.026(3) 0.016(3) -0.003(2) 0.001(2) -0.002(2) N36 0.037(3) 0.024(3) 0.024(3) 0.003(2) -0.001(3) -0.004(3) C11 0.040(4) 0.026(4) 0.022(3) 0.001(3) -0.005(3) -0.003(3) C12 0.055(5) 0.020(4) 0.032(4) 0.004(3) -0.004(4) -0.006(3) C13 0.055(5) 0.033(4) 0.040(4) 0.006(3) 0.004(4) -0.019(4) C14 0.033(4) 0.032(4) 0.035(4) -0.003(3) 0.004(3) -0.011(3) C15 0.032(4) 0.029(4) 0.019(3) 0.004(3) -0.004(3) -0.008(3) C21 0.023(4) 0.030(4) 0.023(3) -0.003(3) -0.003(3) -0.007(3) C22 0.031(4) 0.035(4) 0.025(3) 0.002(3) -0.002(3) -0.004(3) C23 0.041(5) 0.047(5) 0.025(4) -0.002(3) 0.005(3) -0.006(4) C24 0.031(4) 0.052(5) 0.028(4) -0.010(3) 0.000(3) 0.001(4) C25 0.026(4) 0.037(4) 0.031(4) -0.004(3) -0.007(3) -0.006(3) C31 0.032(4) 0.030(4) 0.036(4) -0.003(3) -0.006(3) -0.002(3) C32 0.038(5) 0.037(4) 0.057(5) 0.004(4) -0.008(4) 0.002(4) C33 0.037(5) 0.049(5) 0.071(6) 0.019(4) -0.021(5) 0.004(4) C34 0.045(5) 0.054(5) 0.049(5) 0.015(4) -0.024(4) -0.002(4) C35 0.048(5) 0.031(4) 0.038(4) 0.004(3) -0.019(4) -0.009(3) C41 0.053(5) 0.028(4) 0.027(4) 0.000(3) -0.014(3) -0.003(3) C42 0.061(6) 0.049(5) 0.021(4) 0.005(3) -0.009(4) -0.001(4) C43 0.069(6) 0.044(5) 0.023(4) 0.001(3) 0.003(4) -0.012(4) C44 0.043(5) 0.042(4) 0.026(4) 0.002(3) 0.007(3) -0.017(4) C45 0.042(4) 0.022(4) 0.025(3) 0.000(3) -0.002(3) -0.010(3) C51 0.031(4) 0.022(3) 0.027(3) -0.001(3) 0.002(3) -0.005(3) C52 0.047(5) 0.037(4) 0.035(4) 0.004(3) 0.000(4) -0.018(4) C53 0.062(6) 0.046(5) 0.058(5) 0.006(4) -0.009(5) -0.033(4) C54 0.041(5) 0.061(6) 0.054(5) -0.004(4) -0.005(4) -0.022(4) C55 0.034(4) 0.037(4) 0.041(4) -0.005(3) -0.004(3) -0.008(3) C61 0.038(5) 0.045(5) 0.043(4) -0.006(4) -0.010(4) -0.008(4) C62 0.046(5) 0.055(6) 0.073(6) -0.019(5) -0.019(5) -0.013(4) C63 0.054(6) 0.049(5) 0.060(5) -0.022(4) -0.008(4) -0.022(4) C64 0.046(5) 0.028(4) 0.038(4) -0.011(3) 0.001(4) -0.010(3) C65 0.033(4) 0.027(4) 0.025(3) -0.002(3) -0.003(3) -0.004(3) C71 0.036(4) 0.024(4) 0.022(3) -0.006(3) 0.003(3) -0.008(3) C72 0.052(5) 0.030(4) 0.024(3) -0.004(3) -0.003(3) -0.012(3) C73 0.056(5) 0.043(5) 0.024(4) -0.009(3) 0.010(4) -0.008(4) C74 0.040(5) 0.040(5) 0.043(4) -0.007(4) 0.018(4) -0.003(4) C75 0.036(4) 0.025(4) 0.034(4) -0.001(3) 0.010(3) -0.006(3) C81 0.027(4) 0.034(4) 0.046(4) -0.006(3) -0.004(3) -0.004(3) C82 0.027(4) 0.049(5) 0.064(6) -0.016(4) -0.004(4) 0.006(4) C83 0.033(5) 0.045(5) 0.076(6) -0.009(4) -0.021(4) 0.007(4) C84 0.036(4) 0.040(4) 0.051(5) 0.001(4) -0.018(4) 0.002(4) C85 0.029(4) 0.032(4) 0.040(4) 0.000(3) -0.008(3) -0.008(3) C91 0.027(4) 0.031(4) 0.028(4) 0.005(3) -0.010(3) -0.006(3) C92 0.034(4) 0.044(4) 0.025(4) 0.007(3) -0.007(3) -0.006(3) C93 0.039(4) 0.050(5) 0.017(3) -0.008(3) -0.002(3) -0.007(4) C94 0.033(4) 0.033(4) 0.025(3) -0.008(3) 0.001(3) -0.005(3) C95 0.027(4) 0.023(3) 0.029(3) 0.000(3) -0.006(3) -0.008(3) C101 0.030(4) 0.024(4) 0.023(3) -0.004(3) -0.002(3) -0.001(3) C102 0.037(4) 0.030(4) 0.037(4) -0.002(3) -0.010(3) -0.004(3) C103 0.053(5) 0.034(4) 0.041(4) -0.006(3) -0.007(4) -0.015(4) C104 0.042(4) 0.025(4) 0.038(4) -0.003(3) 0.001(3) -0.005(3) C105 0.039(4) 0.025(4) 0.032(4) 0.003(3) 0.001(3) 0.000(3) C111 0.039(4) 0.035(4) 0.030(4) -0.003(3) 0.002(3) -0.009(3) C112 0.066(6) 0.031(4) 0.040(4) 0.006(3) -0.006(4) -0.014(4) C113 0.079(6) 0.029(4) 0.043(5) 0.014(3) -0.011(4) -0.008(4) C114 0.060(5) 0.032(4) 0.039(4) 0.012(3) -0.014(4) -0.007(4) C115 0.039(4) 0.028(4) 0.021(3) 0.003(3) 0.003(3) -0.007(3) C121 0.039(4) 0.031(4) 0.020(3) 0.003(3) -0.003(3) 0.002(3) C122 0.054(5) 0.044(5) 0.020(3) 0.001(3) 0.000(3) -0.009(4) C123 0.069(6) 0.049(5) 0.019(4) 0.004(3) -0.007(4) -0.004(4) C124 0.075(6) 0.054(5) 0.019(4) -0.007(3) -0.014(4) -0.008(5) C125 0.047(5) 0.033(4) 0.029(4) -0.003(3) -0.013(3) -0.001(3) C131 0.050(5) 0.035(4) 0.046(5) -0.003(3) -0.022(4) -0.008(4) C132 0.070(7) 0.074(7) 0.059(6) -0.009(5) -0.033(5) -0.020(5) C133 0.046(6) 0.081(7) 0.088(8) -0.008(6) -0.024(6) -0.012(5) C134 0.038(5) 0.073(6) 0.064(6) -0.012(5) -0.004(4) -0.019(5) C135 0.038(5) 0.034(4) 0.050(5) -0.004(3) -0.007(4) -0.006(3) C141 0.046(5) 0.023(4) 0.038(4) 0.000(3) 0.003(4) -0.006(3) C142 0.047(5) 0.043(5) 0.040(4) 0.003(4) 0.014(4) -0.007(4) C143 0.061(6) 0.046(5) 0.027(4) 0.003(3) 0.009(4) -0.006(4) C144 0.057(5) 0.028(4) 0.025(4) 0.004(3) -0.004(4) -0.003(4) C145 0.043(4) 0.022(4) 0.023(3) -0.004(3) 0.001(3) -0.007(3) C151 0.045(5) 0.028(4) 0.022(3) -0.001(3) -0.006(3) -0.001(3) C152 0.060(5) 0.030(4) 0.041(4) 0.010(3) -0.012(4) -0.004(4) C153 0.078(7) 0.031(5) 0.061(6) 0.014(4) -0.029(5) -0.001(5) C154 0.066(6) 0.045(5) 0.075(6) 0.000(5) -0.042(5) 0.016(5) C155 0.039(5) 0.048(5) 0.036(4) -0.001(3) -0.017(4) -0.002(4) C161 0.056(5) 0.037(4) 0.021(3) -0.005(3) -0.007(3) -0.012(4) C162 0.073(6) 0.030(4) 0.039(4) -0.006(3) -0.004(4) -0.010(4) C163 0.070(6) 0.030(4) 0.045(5) -0.012(4) 0.002(4) 0.005(4) C164 0.050(5) 0.033(4) 0.035(4) -0.006(3) 0.000(4) 0.001(4) C165 0.042(5) 0.033(4) 0.015(3) -0.001(3) -0.003(3) -0.002(3) C171 0.037(4) 0.034(4) 0.027(4) 0.004(3) -0.007(3) -0.002(3) C172 0.055(5) 0.049(5) 0.020(3) -0.004(3) 0.002(3) -0.002(4) C173 0.055(6) 0.063(6) 0.025(4) -0.001(4) 0.011(4) -0.002(5) C174 0.040(5) 0.061(6) 0.036(4) 0.007(4) 0.004(4) -0.004(4) C175 0.043(5) 0.041(4) 0.026(4) 0.005(3) -0.006(3) -0.002(4) C181 0.040(5) 0.034(4) 0.040(4) 0.005(3) -0.011(4) -0.002(3) C182 0.034(5) 0.058(6) 0.072(6) -0.003(5) -0.013(4) -0.012(4) C183 0.042(5) 0.060(6) 0.075(6) -0.009(5) -0.026(5) -0.013(4) C184 0.051(5) 0.049(5) 0.053(5) -0.012(4) -0.025(4) -0.001(4) C185 0.048(5) 0.027(4) 0.041(4) -0.001(3) -0.019(4) 0.000(3) C191 0.060(5) 0.022(4) 0.025(4) -0.001(3) -0.012(3) -0.008(3) C192 0.067(6) 0.047(5) 0.020(4) -0.003(3) -0.009(4) -0.013(4) C193 0.068(6) 0.048(5) 0.023(4) -0.006(3) 0.001(4) -0.009(4) C194 0.050(5) 0.030(4) 0.028(4) -0.005(3) 0.005(3) -0.005(3) C195 0.041(4) 0.017(3) 0.022(3) 0.002(3) -0.002(3) -0.006(3) C201 0.037(4) 0.022(3) 0.025(3) -0.001(3) 0.002(3) -0.006(3) C202 0.052(5) 0.030(4) 0.043(4) -0.009(3) -0.011(4) 0.000(4) C203 0.047(5) 0.029(4) 0.063(5) -0.008(4) -0.002(4) 0.005(4) C204 0.036(5) 0.037(5) 0.063(5) 0.004(4) -0.005(4) 0.003(4) C205 0.034(4) 0.039(4) 0.045(4) 0.007(3) -0.006(4) -0.013(4) C1 0.049(5) 0.039(5) 0.053(5) -0.018(4) 0.004(4) -0.001(4) C2 0.084(7) 0.075(7) 0.047(5) -0.014(5) -0.043(5) -0.001(5) C3 0.034(5) 0.057(6) 0.064(6) -0.007(4) 0.017(4) -0.011(4) C4 0.057(5) 0.041(5) 0.045(5) 0.015(4) -0.012(4) -0.009(4) C5 0.089(7) 0.054(6) 0.049(5) -0.020(4) -0.023(5) -0.010(5) C6 0.040(5) 0.069(6) 0.070(6) -0.005(5) 0.009(5) 0.004(5) C7 0.069(7) 0.076(7) 0.054(5) 0.018(5) 0.005(5) -0.036(5) C8 0.078(7) 0.056(5) 0.037(4) 0.008(4) -0.028(4) -0.001(5) P1 0.039(3) 0.053(2) 0.0371(15) -0.0088(14) -0.0148(16) 0.0119(17) F1 0.064(5) 0.099(7) 0.153(17) -0.013(12) 0.004(9) 0.003(5) F2 0.059(7) 0.128(14) 0.23(2) -0.001(12) -0.024(9) -0.006(8) F3 0.134(14) 0.061(9) 0.085(8) -0.021(7) 0.028(7) -0.018(8) F4 0.23(2) 0.150(12) 0.084(11) 0.025(10) -0.072(14) -0.036(13) F5 0.204(11) 0.112(9) 0.088(13) -0.052(9) -0.026(10) -0.033(8) F6 0.138(11) 0.071(7) 0.075(7) 0.022(5) -0.042(7) -0.020(6) P1B 0.039(3) 0.053(2) 0.0371(15) -0.0088(14) -0.0148(16) 0.0119(17) F1B 0.064(5) 0.099(7) 0.153(17) -0.013(12) 0.004(9) 0.003(5) F2B 0.059(7) 0.128(14) 0.23(2) -0.001(12) -0.024(9) -0.006(8) F3B 0.134(14) 0.061(9) 0.085(8) -0.021(7) 0.028(7) -0.018(8) F4B 0.23(2) 0.150(12) 0.084(11) 0.025(10) -0.072(14) -0.036(13) F5B 0.204(11) 0.112(9) 0.088(13) -0.052(9) -0.026(10) -0.033(8) F6B 0.138(11) 0.071(7) 0.075(7) 0.022(5) -0.042(7) -0.020(6) P2 0.0387(16) 0.0529(14) 0.0439(13) 0.0005(11) 0.0062(11) -0.0030(11) F7 0.104(7) 0.114(6) 0.099(5) -0.062(5) 0.007(4) -0.012(5) F8 0.119(9) 0.098(5) 0.066(4) -0.018(4) 0.037(5) -0.014(5) F9 0.060(5) 0.231(15) 0.099(8) -0.043(9) -0.036(6) 0.027(7) F10 0.202(14) 0.122(7) 0.050(4) 0.001(4) 0.003(7) -0.118(9) F11 0.087(6) 0.118(9) 0.172(11) 0.027(7) -0.064(7) 0.007(6) F12 0.127(8) 0.082(6) 0.110(6) 0.033(5) -0.004(7) -0.045(7) P2B 0.0387(16) 0.0529(14) 0.0439(13) 0.0005(11) 0.0062(11) -0.0030(11) F7B 0.104(7) 0.114(6) 0.099(5) -0.062(5) 0.007(4) -0.012(5) F8B 0.119(9) 0.098(5) 0.066(4) -0.018(4) 0.037(5) -0.014(5) F9B 0.060(5) 0.231(15) 0.099(8) -0.043(9) -0.036(6) 0.027(7) F10B 0.202(14) 0.122(7) 0.050(4) 0.001(4) 0.003(7) -0.118(9) F11B 0.087(6) 0.118(9) 0.172(11) 0.027(7) -0.064(7) 0.007(6) F12B 0.127(8) 0.082(6) 0.110(6) 0.033(5) -0.004(7) -0.045(7) P3 0.149(3) 0.0591(18) 0.0501(16) -0.0011(13) -0.0171(19) -0.029(2) F13 0.41(2) 0.140(11) 0.33(2) 0.076(12) -0.26(2) -0.175(14) F14 0.086(7) 0.172(11) 0.263(16) -0.089(11) -0.021(8) -0.062(7) F15 0.279(15) 0.088(6) 0.079(6) 0.016(5) -0.063(8) -0.025(8) F16 0.131(9) 0.194(12) 0.099(7) 0.024(8) 0.026(7) 0.020(8) F17 0.202(11) 0.137(8) 0.056(5) -0.003(5) -0.043(6) 0.044(8) F18 0.42(2) 0.073(7) 0.109(8) 0.000(6) 0.097(12) 0.025(10) P3B 0.149(3) 0.0591(18) 0.0501(16) -0.0011(13) -0.0171(19) -0.029(2) F13B 0.41(2) 0.140(11) 0.33(2) 0.076(12) -0.26(2) -0.175(14) F14B 0.086(7) 0.172(11) 0.263(16) -0.089(11) -0.021(8) -0.062(7) F15B 0.279(15) 0.088(6) 0.079(6) 0.016(5) -0.063(8) -0.025(8) F16B 0.131(9) 0.194(12) 0.099(7) 0.024(8) 0.026(7) 0.020(8) F17B 0.202(11) 0.137(8) 0.056(5) -0.003(5) -0.043(6) 0.044(8) F18B 0.42(2) 0.073(7) 0.109(8) 0.000(6) 0.097(12) 0.025(10) P4 0.095(4) 0.181(7) 0.086(3) -0.030(4) -0.010(3) -0.007(4) F19 0.185(14) 0.171(14) 0.33(2) 0.074(14) -0.098(14) -0.135(12) F20 0.67(5) 0.144(14) 0.173(14) 0.063(11) 0.10(2) -0.08(2) F21 0.253(16) 0.061(7) 0.235(15) 0.042(9) -0.094(13) -0.042(8) F22 0.160(14) 1.13(10) 0.197(17) 0.26(4) -0.074(13) 0.00(3) F23 0.253(19) 0.217(18) 0.26(2) -0.070(15) -0.007(15) 0.077(15) F24 0.141(14) 0.71(5) 1.00(7) -0.61(6) -0.18(3) 0.02(2) P4B 0.095(4) 0.181(7) 0.086(3) -0.030(4) -0.010(3) -0.007(4) F19B 0.185(14) 0.171(14) 0.33(2) 0.074(14) -0.098(14) -0.135(12) F20B 0.67(5) 0.144(14) 0.173(14) 0.063(11) 0.10(2) -0.08(2) F21B 0.253(16) 0.061(7) 0.235(15) 0.042(9) -0.094(13) -0.042(8) F22B 0.160(14) 1.13(10) 0.197(17) 0.26(4) -0.074(13) 0.00(3) F23B 0.253(19) 0.217(18) 0.26(2) -0.070(15) -0.007(15) 0.077(15) F24B 0.141(14) 0.71(5) 1.00(7) -0.61(6) -0.18(3) 0.02(2) O1 0.30(2) 0.106(8) 0.066(9) -0.024(7) -0.091(11) 0.097(11) C1S 0.067(8) 0.060(7) 0.046(7) 0.009(5) -0.023(6) -0.006(6) C2S 0.060(8) 0.136(17) 0.121(11) -0.083(11) 0.004(8) -0.025(9) C3S 0.106(16) 0.41(3) 0.076(10) 0.068(15) -0.048(12) -0.15(2) O1B 0.30(2) 0.106(8) 0.066(9) -0.024(7) -0.091(11) 0.097(11) C1SB 0.067(8) 0.060(7) 0.046(7) 0.009(5) -0.023(6) -0.006(6) C2SB 0.060(8) 0.136(17) 0.121(11) -0.083(11) 0.004(8) -0.025(9) C3SB 0.106(16) 0.41(3) 0.076(10) 0.068(15) -0.048(12) -0.15(2) O2 0.238(14) 0.214(13) 0.077(6) 0.019(7) -0.018(8) -0.103(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 1.977(6) . ? Ni1 N3 1.995(5) . ? Ni1 N7 2.005(5) . ? Ni1 N18 2.121(5) . ? Ni1 N10 2.124(5) . ? Ni1 Ni2 2.3433(14) . ? Ni2 N17 1.883(5) . ? Ni2 N8 1.886(5) . ? Ni2 N2 1.888(5) . ? Ni2 N11 1.890(5) . ? Ni2 Ni3 2.3474(14) . ? Ni3 N14 1.979(5) . ? Ni3 N16 2.003(5) . ? Ni3 N12 2.015(5) . ? Ni3 N1 2.126(6) . ? Ni3 N9 2.128(5) . ? Ni4 N23 1.989(6) . ? Ni4 N21 2.013(5) . ? Ni4 N25 2.014(5) . ? Ni4 N28 2.113(6) . ? Ni4 N36 2.128(5) . ? Ni4 Ni5 2.3638(15) . ? Ni5 N35 1.875(5) . ? Ni5 N26 1.880(5) . ? Ni5 N20 1.885(5) . ? Ni5 N29 1.892(5) . ? Ni5 Ni6 2.3525(15) . ? Ni6 N32 1.992(6) . ? Ni6 N30 1.994(6) . ? Ni6 N34 2.008(5) . ? Ni6 N27 2.101(6) . ? Ni6 N19 2.107(5) . ? N1 C15 1.342(8) . ? N1 C11 1.345(8) . ? N2 C21 1.372(8) . ? N2 C15 1.376(8) . ? N3 C25 1.337(8) . ? N3 C21 1.354(8) . ? N4 C31 1.406(9) . ? N4 C25 1.411(9) . ? N4 C1 1.469(9) . ? N5 C31 1.343(9) . ? N5 C35 1.364(8) . ? N6 C35 1.394(9) . ? N6 C41 1.412(10) . ? N6 C2 1.475(9) . ? N7 C41 1.341(8) . ? N7 C45 1.363(9) . ? N8 C51 1.364(8) . ? N8 C45 1.373(8) . ? N9 C51 1.337(8) . ? N9 C55 1.345(9) . ? N10 C65 1.350(8) . ? N10 C61 1.351(9) . ? N11 C65 1.370(8) . ? N11 C71 1.373(8) . ? N12 C75 1.341(8) . ? N12 C71 1.359(8) . ? N13 C81 1.409(9) . ? N13 C75 1.412(9) . ? N13 C3 1.475(9) . ? N14 C81 1.339(9) . ? N14 C85 1.350(9) . ? N15 C91 1.404(8) . ? N15 C85 1.407(9) . ? N15 C4 1.471(9) . ? N16 C95 1.353(8) . ? N16 C91 1.354(8) . ? N17 C101 1.372(8) . ? N17 C95 1.381(8) . ? N18 C101 1.347(8) . ? N18 C105 1.354(8) . ? N19 C111 1.342(9) . ? N19 C115 1.358(8) . ? N20 C115 1.366(9) . ? N20 C121 1.384(8) . ? N21 C125 1.359(8) . ? N21 C121 1.362(9) . ? N22 C125 1.394(9) . ? N22 C131 1.417(10) . ? N22 C5 1.485(9) . ? N23 C135 1.343(9) . ? N23 C131 1.351(9) . ? N24 C141 1.404(10) . ? N24 C135 1.410(10) . ? N24 C6 1.453(10) . ? N25 C141 1.348(9) . ? N25 C145 1.373(9) . ? N26 C151 1.369(9) . ? N26 C145 1.373(9) . ? N27 C151 1.341(9) . ? N27 C155 1.343(9) . ? N28 C161 1.350(9) . ? N28 C165 1.360(9) . ? N29 C165 1.370(9) . ? N29 C171 1.374(9) . ? N30 C171 1.351(9) . ? N30 C175 1.351(9) . ? N31 C181 1.406(9) . ? N31 C175 1.408(10) . ? N31 C7 1.463(10) . ? N32 C181 1.344(9) . ? N32 C185 1.344(9) . ? N33 C185 1.397(10) . ? N33 C191 1.407(10) . ? N33 C8 1.479(9) . ? N34 C191 1.344(8) . ? N34 C195 1.374(9) . ? N35 C195 1.371(8) . ? N35 C201 1.385(8) . ? N36 C201 1.336(8) . ? N36 C205 1.349(9) . ? C11 C12 1.370(10) . ? C11 H11A 0.9400 . ? C12 C13 1.385(11) . ? C12 H12A 0.9400 . ? C13 C14 1.361(10) . ? C13 H13A 0.9400 . ? C14 C15 1.412(9) . ? C14 H14A 0.9400 . ? C21 C22 1.400(9) . ? C22 C23 1.367(9) . ? C22 H22A 0.9400 . ? C23 C24 1.373(10) . ? C23 H23A 0.9400 . ? C24 C25 1.378(10) . ? C24 H24A 0.9400 . ? C31 C32 1.382(10) . ? C32 C33 1.375(11) . ? C32 H32A 0.9400 . ? C33 C34 1.361(12) . ? C33 H33A 0.9400 . ? C34 C35 1.389(10) . ? C34 H34A 0.9400 . ? C41 C42 1.391(10) . ? C42 C43 1.356(11) . ? C42 H42A 0.9400 . ? C43 C44 1.387(10) . ? C43 H43A 0.9400 . ? C44 C45 1.411(9) . ? C44 H44A 0.9400 . ? C51 C52 1.408(9) . ? C52 C53 1.369(11) . ? C52 H52A 0.9400 . ? C53 C54 1.374(12) . ? C53 H53A 0.9400 . ? C54 C55 1.381(11) . ? C54 H54A 0.9400 . ? C55 H55A 0.9400 . ? C61 C62 1.368(11) . ? C61 H61A 0.9400 . ? C62 C63 1.380(11) . ? C62 H62A 0.9400 . ? C63 C64 1.364(11) . ? C63 H63A 0.9400 . ? C64 C65 1.407(9) . ? C64 H64A 0.9400 . ? C71 C72 1.397(9) . ? C72 C73 1.363(10) . ? C72 H72A 0.9400 . ? C73 C74 1.381(11) . ? C73 H73A 0.9400 . ? C74 C75 1.389(10) . ? C74 H74A 0.9400 . ? C81 C82 1.359(10) . ? C82 C83 1.358(12) . ? C82 H82A 0.9400 . ? C83 C84 1.370(11) . ? C83 H83A 0.9400 . ? C84 C85 1.381(9) . ? C84 H84A 0.9400 . ? C91 C92 1.382(9) . ? C92 C93 1.377(10) . ? C92 H92A 0.9400 . ? C93 C94 1.379(9) . ? C93 H93A 0.9400 . ? C94 C95 1.397(9) . ? C94 H94A 0.9400 . ? C101 C102 1.401(9) . ? C102 C103 1.371(10) . ? C102 H10A 0.9400 . ? C103 C104 1.393(10) . ? C103 H10B 0.9400 . ? C104 C105 1.366(10) . ? C104 H10C 0.9400 . ? C105 H10D 0.9400 . ? C111 C112 1.392(10) . ? C111 H11B 0.9400 . ? C112 C113 1.368(11) . ? C112 H11C 0.9400 . ? C113 C114 1.387(11) . ? C113 H11D 0.9400 . ? C114 C115 1.395(9) . ? C114 H11E 0.9400 . ? C121 C122 1.393(9) . ? C122 C123 1.384(10) . ? C122 H12B 0.9400 . ? C123 C124 1.378(11) . ? C123 H12C 0.9400 . ? C124 C125 1.383(10) . ? C124 H12D 0.9400 . ? C131 C132 1.377(11) . ? C132 C133 1.381(13) . ? C132 H13B 0.9400 . ? C133 C134 1.380(13) . ? C133 H13C 0.9400 . ? C134 C135 1.394(11) . ? C134 H13D 0.9400 . ? C141 C142 1.385(10) . ? C142 C143 1.386(11) . ? C142 H14B 0.9400 . ? C143 C144 1.366(11) . ? C143 H14C 0.9400 . ? C144 C145 1.391(9) . ? C144 H14D 0.9400 . ? C151 C152 1.413(10) . ? C152 C153 1.359(11) . ? C152 H15A 0.9400 . ? C153 C154 1.386(13) . ? C153 H15B 0.9400 . ? C154 C155 1.360(11) . ? C154 H15C 0.9400 . ? C155 H15D 0.9400 . ? C161 C162 1.359(10) . ? C161 H16A 0.9400 . ? C162 C163 1.391(12) . ? C162 H16B 0.9400 . ? C163 C164 1.368(11) . ? C163 H16C 0.9400 . ? C164 C165 1.406(10) . ? C164 H16D 0.9400 . ? C171 C172 1.409(10) . ? C172 C173 1.373(11) . ? C172 H17A 0.9400 . ? C173 C174 1.373(12) . ? C173 H17B 0.9400 . ? C174 C175 1.377(10) . ? C174 H17C 0.9400 . ? C181 C182 1.388(11) . ? C182 C183 1.366(12) . ? C182 H18A 0.9400 . ? C183 C184 1.368(12) . ? C183 H18B 0.9400 . ? C184 C185 1.391(11) . ? C184 H18C 0.9400 . ? C191 C192 1.382(10) . ? C192 C193 1.375(11) . ? C192 H19A 0.9400 . ? C193 C194 1.378(10) . ? C193 H19B 0.9400 . ? C194 C195 1.392(9) . ? C194 H19C 0.9400 . ? C201 C202 1.402(9) . ? C202 C203 1.359(11) . ? C202 H20A 0.9400 . ? C203 C204 1.371(11) . ? C203 H20B 0.9400 . ? C204 C205 1.378(10) . ? C204 H20C 0.9400 . ? C205 H20D 0.9400 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? P1 F2 1.551(7) . ? P1 F5 1.561(6) . ? P1 F6 1.563(6) . ? P1 F4 1.567(6) . ? P1 F3 1.568(6) . ? P1 F1 1.571(6) . ? P1B F2B 1.549(7) . ? P1B F5B 1.560(7) . ? P1B F6B 1.561(7) . ? P1B F3B 1.568(7) . ? P1B F1B 1.573(7) . ? P1B F4B 1.574(7) . ? P2 F7 1.559(6) . ? P2 F11 1.560(6) . ? P2 F9 1.563(6) . ? P2 F12 1.565(6) . ? P2 F10 1.569(6) . ? P2 F8 1.581(6) . ? P2B F7B 1.561(7) . ? P2B F12B 1.561(7) . ? P2B F11B 1.562(7) . ? P2B F9B 1.562(7) . ? P2B F10B 1.563(7) . ? P2B F8B 1.569(7) . ? P3 F14 1.551(6) . ? P3 F17 1.555(6) . ? P3 F13 1.558(6) . ? P3 F18 1.563(6) . ? P3 F16 1.568(6) . ? P3 F15 1.572(6) . ? P3B F17B 1.561(7) . ? P3B F13B 1.562(7) . ? P3B F15B 1.562(7) . ? P3B F14B 1.563(7) . ? P3B F18B 1.563(7) . ? P3B F16B 1.567(7) . ? P4 F21 1.560(7) . ? P4 F19 1.561(7) . ? P4 F24 1.561(7) . ? P4 F23 1.565(7) . ? P4 F20 1.567(7) . ? P4 F22 1.572(7) . ? P4B F21B 1.550(7) . ? P4B F19B 1.552(7) . ? P4B F22B 1.568(7) . ? P4B F20B 1.570(7) . ? P4B F24B 1.574(7) . ? P4B F23B 1.581(7) . ? O1 C1S 1.220(7) . ? C1S C3S 1.411(7) . ? C1S C2S 1.412(7) . ? C2S H2SA 0.9700 . ? C2S H2SB 0.9700 . ? C2S H2SC 0.9700 . ? C3S H3SA 0.9700 . ? C3S H3SB 0.9700 . ? C3S H3SC 0.9700 . ? O1B C1SB 1.232(8) . ? C1SB C3SB 1.407(8) . ? C1SB C2SB 1.407(8) . ? C2SB H2SD 0.9700 . ? C2SB H2SE 0.9700 . ? C2SB H2SF 0.9700 . ? C3SB H3SD 0.9700 . ? C3SB H3SE 0.9700 . ? C3SB H3SF 0.9700 . ? O3 C4S 1.236(8) . ? O3 C5S 1.93(4) 2_865 ? C4S C6S 1.406(6) . ? C4S C5S 1.411(10) . ? C4S C5S 1.87(5) 2_865 ? C5S C4S 1.87(5) 2_865 ? C5S O3 1.93(4) 2_865 ? C5S H5SA 0.9700 . ? C5S H5SB 0.9700 . ? C5S H5SC 0.9700 . ? C6S H6SA 0.9700 . ? C6S H6SB 0.9700 . ? C6S H6SC 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 N5 Ni1 N3 94.1(2) . . ? N5 Ni1 N7 94.1(2) . . ? N3 Ni1 N7 171.7(2) . . ? N5 Ni1 N18 98.9(2) . . ? N3 Ni1 N18 87.2(2) . . ? N7 Ni1 N18 92.8(2) . . ? N5 Ni1 N10 95.9(2) . . ? N3 Ni1 N10 90.6(2) . . ? N7 Ni1 N10 87.2(2) . . ? N18 Ni1 N10 165.1(2) . . ? N5 Ni1 Ni2 178.78(17) . . ? N3 Ni1 Ni2 85.89(15) . . ? N7 Ni1 Ni2 85.93(16) . . ? N18 Ni1 Ni2 82.33(14) . . ? N10 Ni1 Ni2 82.84(15) . . ? N17 Ni2 N8 89.9(2) . . ? N17 Ni2 N2 90.3(2) . . ? N8 Ni2 N2 176.0(2) . . ? N17 Ni2 N11 176.1(2) . . ? N8 Ni2 N11 89.8(2) . . ? N2 Ni2 N11 90.3(2) . . ? N17 Ni2 Ni1 92.49(15) . . ? N8 Ni2 Ni1 88.01(17) . . ? N2 Ni2 Ni1 87.99(16) . . ? N11 Ni2 Ni1 91.38(16) . . ? N17 Ni2 Ni3 87.73(15) . . ? N8 Ni2 Ni3 92.40(17) . . ? N2 Ni2 Ni3 91.61(16) . . ? N11 Ni2 Ni3 88.40(16) . . ? Ni1 Ni2 Ni3 179.54(5) . . ? N14 Ni3 N16 94.2(2) . . ? N14 Ni3 N12 94.4(2) . . ? N16 Ni3 N12 171.3(2) . . ? N14 Ni3 N1 98.0(2) . . ? N16 Ni3 N1 89.0(2) . . ? N12 Ni3 N1 90.7(2) . . ? N14 Ni3 N9 97.3(2) . . ? N16 Ni3 N9 92.0(2) . . ? N12 Ni3 N9 86.1(2) . . ? N1 Ni3 N9 164.5(2) . . ? N14 Ni3 Ni2 179.66(19) . . ? N16 Ni3 Ni2 85.85(15) . . ? N12 Ni3 Ni2 85.53(16) . . ? N1 Ni3 Ni2 82.29(14) . . ? N9 Ni3 Ni2 82.32(15) . . ? N23 Ni4 N21 95.3(2) . . ? N23 Ni4 N25 93.4(2) . . ? N21 Ni4 N25 171.2(2) . . ? N23 Ni4 N28 99.2(2) . . ? N21 Ni4 N28 88.5(2) . . ? N25 Ni4 N28 90.6(2) . . ? N23 Ni4 N36 96.2(2) . . ? N21 Ni4 N36 90.9(2) . . ? N25 Ni4 N36 87.7(2) . . ? N28 Ni4 N36 164.6(2) . . ? N23 Ni4 Ni5 178.76(17) . . ? N21 Ni4 Ni5 84.82(17) . . ? N25 Ni4 Ni5 86.40(17) . . ? N28 Ni4 Ni5 82.06(17) . . ? N36 Ni4 Ni5 82.59(16) . . ? N35 Ni5 N26 89.8(2) . . ? N35 Ni5 N20 90.1(2) . . ? N26 Ni5 N20 176.6(2) . . ? N35 Ni5 N29 176.2(2) . . ? N26 Ni5 N29 90.1(2) . . ? N20 Ni5 N29 90.3(2) . . ? N35 Ni5 Ni6 87.63(17) . . ? N26 Ni5 Ni6 90.86(17) . . ? N20 Ni5 Ni6 92.50(18) . . ? N29 Ni5 Ni6 88.59(18) . . ? N35 Ni5 Ni4 91.60(17) . . ? N26 Ni5 Ni4 87.59(17) . . ? N20 Ni5 Ni4 89.04(18) . . ? N29 Ni5 Ni4 92.17(18) . . ? Ni6 Ni5 Ni4 178.28(5) . . ? N32 Ni6 N30 94.9(2) . . ? N32 Ni6 N34 93.8(2) . . ? N30 Ni6 N34 171.0(2) . . ? N32 Ni6 N27 96.4(2) . . ? N30 Ni6 N27 88.4(2) . . ? N34 Ni6 N27 88.4(2) . . ? N32 Ni6 N19 98.2(2) . . ? N30 Ni6 N19 87.7(2) . . ? N34 Ni6 N19 93.3(2) . . ? N27 Ni6 N19 165.1(2) . . ? N32 Ni6 Ni5 179.06(17) . . ? N30 Ni6 Ni5 85.42(17) . . ? N34 Ni6 Ni5 85.87(16) . . ? N27 Ni6 Ni5 82.71(16) . . ? N19 Ni6 Ni5 82.69(16) . . ? C15 N1 C11 118.3(6) . . ? C15 N1 Ni3 119.9(4) . . ? C11 N1 Ni3 121.6(5) . . ? C21 N2 C15 123.6(5) . . ? C21 N2 Ni2 118.7(4) . . ? C15 N2 Ni2 117.7(4) . . ? C25 N3 C21 119.9(6) . . ? C25 N3 Ni1 120.7(4) . . ? C21 N3 Ni1 119.1(4) . . ? C31 N4 C25 125.0(6) . . ? C31 N4 C1 115.9(6) . . ? C25 N4 C1 115.6(6) . . ? C31 N5 C35 120.3(6) . . ? C31 N5 Ni1 119.8(4) . . ? C35 N5 Ni1 119.7(5) . . ? C35 N6 C41 126.7(6) . . ? C35 N6 C2 116.2(6) . . ? C41 N6 C2 116.2(6) . . ? C41 N7 C45 120.8(6) . . ? C41 N7 Ni1 120.4(5) . . ? C45 N7 Ni1 117.9(4) . . ? C51 N8 C45 123.5(6) . . ? C51 N8 Ni2 118.9(4) . . ? C45 N8 Ni2 117.1(4) . . ? C51 N9 C55 118.9(6) . . ? C51 N9 Ni3 119.7(4) . . ? C55 N9 Ni3 121.3(5) . . ? C65 N10 C61 118.3(6) . . ? C65 N10 Ni1 119.0(4) . . ? C61 N10 Ni1 122.5(5) . . ? C65 N11 C71 123.0(5) . . ? C65 N11 Ni2 119.8(4) . . ? C71 N11 Ni2 116.9(4) . . ? C75 N12 C71 120.9(6) . . ? C75 N12 Ni3 119.4(5) . . ? C71 N12 Ni3 118.5(4) . . ? C81 N13 C75 127.2(6) . . ? C81 N13 C3 115.4(6) . . ? C75 N13 C3 116.2(6) . . ? C81 N14 C85 119.8(6) . . ? C81 N14 Ni3 120.2(5) . . ? C85 N14 Ni3 120.0(5) . . ? C91 N15 C85 126.5(6) . . ? C91 N15 C4 115.6(6) . . ? C85 N15 C4 115.6(6) . . ? C95 N16 C91 120.3(5) . . ? C95 N16 Ni3 119.3(4) . . ? C91 N16 Ni3 120.0(4) . . ? C101 N17 C95 122.4(5) . . ? C101 N17 Ni2 118.5(4) . . ? C95 N17 Ni2 118.9(4) . . ? C101 N18 C105 118.1(6) . . ? C101 N18 Ni1 120.5(4) . . ? C105 N18 Ni1 121.4(5) . . ? C111 N19 C115 118.8(6) . . ? C111 N19 Ni6 121.0(5) . . ? C115 N19 Ni6 120.1(4) . . ? C115 N20 C121 123.9(5) . . ? C115 N20 Ni5 118.7(4) . . ? C121 N20 Ni5 117.2(4) . . ? C125 N21 C121 120.3(6) . . ? C125 N21 Ni4 119.4(5) . . ? C121 N21 Ni4 119.9(4) . . ? C125 N22 C131 125.8(6) . . ? C125 N22 C5 116.4(7) . . ? C131 N22 C5 114.4(7) . . ? C135 N23 C131 119.9(7) . . ? C135 N23 Ni4 120.9(5) . . ? C131 N23 Ni4 119.1(5) . . ? C141 N24 C135 127.6(6) . . ? C141 N24 C6 115.0(7) . . ? C135 N24 C6 116.1(7) . . ? C141 N25 C145 119.9(6) . . ? C141 N25 Ni4 121.7(5) . . ? C145 N25 Ni4 117.5(5) . . ? C151 N26 C145 123.2(5) . . ? C151 N26 Ni5 118.5(5) . . ? C145 N26 Ni5 118.2(4) . . ? C151 N27 C155 118.2(6) . . ? C151 N27 Ni6 119.1(4) . . ? C155 N27 Ni6 122.6(5) . . ? C161 N28 C165 118.2(6) . . ? C161 N28 Ni4 121.0(5) . . ? C165 N28 Ni4 120.4(4) . . ? C165 N29 C171 123.6(6) . . ? C165 N29 Ni5 116.7(5) . . ? C171 N29 Ni5 119.3(5) . . ? C171 N30 C175 120.3(6) . . ? C171 N30 Ni6 120.0(5) . . ? C175 N30 Ni6 119.7(5) . . ? C181 N31 C175 125.5(6) . . ? C181 N31 C7 115.5(7) . . ? C175 N31 C7 116.1(7) . . ? C181 N32 C185 120.4(6) . . ? C181 N32 Ni6 119.8(5) . . ? C185 N32 Ni6 119.8(5) . . ? C185 N33 C191 126.8(6) . . ? C185 N33 C8 115.9(6) . . ? C191 N33 C8 115.3(6) . . ? C191 N34 C195 120.1(6) . . ? C191 N34 Ni6 120.7(5) . . ? C195 N34 Ni6 118.2(4) . . ? C195 N35 C201 121.9(5) . . ? C195 N35 Ni5 118.3(4) . . ? C201 N35 Ni5 119.3(4) . . ? C201 N36 C205 119.3(6) . . ? C201 N36 Ni4 119.5(4) . . ? C205 N36 Ni4 121.2(5) . . ? N1 C11 C12 123.3(7) . . ? N1 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 118.2(7) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 118.9(7) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? N1 C15 N2 115.4(6) . . ? N1 C15 C14 121.3(6) . . ? N2 C15 C14 123.0(6) . . ? N3 C21 N2 115.4(5) . . ? N3 C21 C22 120.4(6) . . ? N2 C21 C22 123.9(6) . . ? C23 C22 C21 118.6(6) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C22 C23 C24 120.5(7) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C23 C24 C25 118.7(7) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N3 C25 C24 121.7(6) . . ? N3 C25 N4 117.6(6) . . ? C24 C25 N4 120.7(6) . . ? N5 C31 C32 121.6(7) . . ? N5 C31 N4 118.6(6) . . ? C32 C31 N4 119.8(7) . . ? C33 C32 C31 118.1(8) . . ? C33 C32 H32A 120.9 . . ? C31 C32 H32A 120.9 . . ? C34 C33 C32 120.8(7) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 119.9(7) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? N5 C35 C34 119.3(7) . . ? N5 C35 N6 120.4(6) . . ? C34 C35 N6 120.1(7) . . ? N7 C41 C42 121.0(7) . . ? N7 C41 N6 119.4(6) . . ? C42 C41 N6 119.5(6) . . ? C43 C42 C41 118.7(7) . . ? C43 C42 H42A 120.7 . . ? C41 C42 H42A 120.7 . . ? C42 C43 C44 122.0(7) . . ? C42 C43 H43A 119.0 . . ? C44 C43 H43A 119.0 . . ? C43 C44 C45 117.3(7) . . ? C43 C44 H44A 121.3 . . ? C45 C44 H44A 121.3 . . ? N7 C45 N8 116.1(6) . . ? N7 C45 C44 120.1(6) . . ? N8 C45 C44 123.3(7) . . ? N9 C51 N8 116.6(6) . . ? N9 C51 C52 119.9(6) . . ? N8 C51 C52 123.5(6) . . ? C53 C52 C51 120.1(7) . . ? C53 C52 H52A 120.0 . . ? C51 C52 H52A 120.0 . . ? C52 C53 C54 120.2(8) . . ? C52 C53 H53A 119.9 . . ? C54 C53 H53A 119.9 . . ? C53 C54 C55 116.9(8) . . ? C53 C54 H54A 121.5 . . ? C55 C54 H54A 121.5 . . ? N9 C55 C54 124.1(7) . . ? N9 C55 H55A 118.0 . . ? C54 C55 H55A 118.0 . . ? N10 C61 C62 124.1(7) . . ? N10 C61 H61A 117.9 . . ? C62 C61 H61A 117.9 . . ? C61 C62 C63 117.2(8) . . ? C61 C62 H62A 121.4 . . ? C63 C62 H62A 121.4 . . ? C64 C63 C62 120.6(7) . . ? C64 C63 H63A 119.7 . . ? C62 C63 H63A 119.7 . . ? C63 C64 C65 119.6(7) . . ? C63 C64 H64A 120.2 . . ? C65 C64 H64A 120.2 . . ? N10 C65 N11 115.5(6) . . ? N10 C65 C64 120.2(6) . . ? N11 C65 C64 124.1(6) . . ? N12 C71 N11 116.0(5) . . ? N12 C71 C72 120.0(6) . . ? N11 C71 C72 123.4(6) . . ? C73 C72 C71 118.4(7) . . ? C73 C72 H72A 120.8 . . ? C71 C72 H72A 120.8 . . ? C72 C73 C74 121.9(7) . . ? C72 C73 H73A 119.0 . . ? C74 C73 H73A 119.0 . . ? C73 C74 C75 117.6(7) . . ? C73 C74 H74A 121.2 . . ? C75 C74 H74A 121.2 . . ? N12 C75 C74 121.1(7) . . ? N12 C75 N13 118.7(6) . . ? C74 C75 N13 120.1(7) . . ? N14 C81 C82 120.7(7) . . ? N14 C81 N13 119.0(6) . . ? C82 C81 N13 120.2(7) . . ? C83 C82 C81 119.9(8) . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C82 C83 C84 120.5(7) . . ? C82 C83 H83A 119.7 . . ? C84 C83 H83A 119.7 . . ? C83 C84 C85 117.8(7) . . ? C83 C84 H84A 121.1 . . ? C85 C84 H84A 121.1 . . ? N14 C85 C84 121.2(7) . . ? N14 C85 N15 119.5(6) . . ? C84 C85 N15 119.3(6) . . ? N16 C91 C92 120.5(6) . . ? N16 C91 N15 118.6(6) . . ? C92 C91 N15 120.8(6) . . ? C93 C92 C91 119.4(6) . . ? C93 C92 H92A 120.3 . . ? C91 C92 H92A 120.3 . . ? C92 C93 C94 120.6(6) . . ? C92 C93 H93A 119.7 . . ? C94 C93 H93A 119.7 . . ? C93 C94 C95 118.2(6) . . ? C93 C94 H94A 120.9 . . ? C95 C94 H94A 120.9 . . ? N16 C95 N17 114.7(5) . . ? N16 C95 C94 121.0(6) . . ? N17 C95 C94 124.0(6) . . ? N18 C101 N17 115.4(6) . . ? N18 C101 C102 121.7(6) . . ? N17 C101 C102 122.8(6) . . ? C103 C102 C101 118.9(6) . . ? C103 C102 H10A 120.5 . . ? C101 C102 H10A 120.5 . . ? C102 C103 C104 119.7(7) . . ? C102 C103 H10B 120.2 . . ? C104 C103 H10B 120.2 . . ? C105 C104 C103 118.3(7) . . ? C105 C104 H10C 120.8 . . ? C103 C104 H10C 120.8 . . ? N18 C105 C104 123.3(7) . . ? N18 C105 H10D 118.4 . . ? C104 C105 H10D 118.4 . . ? N19 C111 C112 123.2(7) . . ? N19 C111 H11B 118.4 . . ? C112 C111 H11B 118.4 . . ? C113 C112 C111 117.6(7) . . ? C113 C112 H11C 121.2 . . ? C111 C112 H11C 121.2 . . ? C112 C113 C114 120.5(7) . . ? C112 C113 H11D 119.8 . . ? C114 C113 H11D 119.8 . . ? C113 C114 C115 119.0(7) . . ? C113 C114 H11E 120.5 . . ? C115 C114 H11E 120.5 . . ? N19 C115 N20 116.2(6) . . ? N19 C115 C114 120.7(6) . . ? N20 C115 C114 123.0(6) . . ? N21 C121 N20 115.3(6) . . ? N21 C121 C122 120.9(6) . . ? N20 C121 C122 123.6(7) . . ? C123 C122 C121 118.0(8) . . ? C123 C122 H12B 121.0 . . ? C121 C122 H12B 121.0 . . ? C124 C123 C122 121.3(7) . . ? C124 C123 H12C 119.4 . . ? C122 C123 H12C 119.4 . . ? C123 C124 C125 118.8(7) . . ? C123 C124 H12D 120.6 . . ? C125 C124 H12D 120.6 . . ? N21 C125 C124 120.8(7) . . ? N21 C125 N22 118.2(6) . . ? C124 C125 N22 120.9(7) . . ? N23 C131 C132 122.0(8) . . ? N23 C131 N22 118.8(6) . . ? C132 C131 N22 119.2(7) . . ? C131 C132 C133 118.1(9) . . ? C131 C132 H13B 120.9 . . ? C133 C132 H13B 120.9 . . ? C134 C133 C132 120.2(9) . . ? C134 C133 H13C 119.9 . . ? C132 C133 H13C 119.9 . . ? C133 C134 C135 119.0(9) . . ? C133 C134 H13D 120.5 . . ? C135 C134 H13D 120.5 . . ? N23 C135 C134 120.5(7) . . ? N23 C135 N24 120.8(7) . . ? C134 C135 N24 118.6(7) . . ? N25 C141 C142 121.0(7) . . ? N25 C141 N24 119.0(6) . . ? C142 C141 N24 119.9(7) . . ? C141 C142 C143 118.7(8) . . ? C141 C142 H14B 120.6 . . ? C143 C142 H14B 120.6 . . ? C144 C143 C142 120.9(7) . . ? C144 C143 H14C 119.5 . . ? C142 C143 H14C 119.5 . . ? C143 C144 C145 118.8(7) . . ? C143 C144 H14D 120.6 . . ? C145 C144 H14D 120.6 . . ? N26 C145 N25 116.0(6) . . ? N26 C145 C144 123.2(7) . . ? N25 C145 C144 120.6(7) . . ? N27 C151 N26 116.2(6) . . ? N27 C151 C152 120.9(7) . . ? N26 C151 C152 122.7(7) . . ? C153 C152 C151 119.1(8) . . ? C153 C152 H15A 120.4 . . ? C151 C152 H15A 120.4 . . ? C152 C153 C154 119.7(8) . . ? C152 C153 H15B 120.2 . . ? C154 C153 H15B 120.2 . . ? C155 C154 C153 118.3(8) . . ? C155 C154 H15C 120.9 . . ? C153 C154 H15C 120.9 . . ? N27 C155 C154 123.7(8) . . ? N27 C155 H15D 118.2 . . ? C154 C155 H15D 118.2 . . ? N28 C161 C162 124.0(8) . . ? N28 C161 H16A 118.0 . . ? C162 C161 H16A 118.0 . . ? C161 C162 C163 117.8(8) . . ? C161 C162 H16B 121.1 . . ? C163 C162 H16B 121.1 . . ? C164 C163 C162 120.1(8) . . ? C164 C163 H16C 119.9 . . ? C162 C163 H16C 119.9 . . ? C163 C164 C165 119.3(8) . . ? C163 C164 H16D 120.3 . . ? C165 C164 H16D 120.3 . . ? N28 C165 N29 115.8(6) . . ? N28 C165 C164 120.5(7) . . ? N29 C165 C164 123.4(7) . . ? N30 C171 N29 115.4(6) . . ? N30 C171 C172 120.4(7) . . ? N29 C171 C172 124.0(7) . . ? C173 C172 C171 118.0(8) . . ? C173 C172 H17A 121.0 . . ? C171 C172 H17A 121.0 . . ? C172 C173 C174 121.2(7) . . ? C172 C173 H17B 119.4 . . ? C174 C173 H17B 119.4 . . ? C173 C174 C175 118.8(8) . . ? C173 C174 H17C 120.6 . . ? C175 C174 H17C 120.6 . . ? N30 C175 C174 121.2(7) . . ? N30 C175 N31 118.2(6) . . ? C174 C175 N31 120.6(7) . . ? N32 C181 C182 121.0(7) . . ? N32 C181 N31 118.8(7) . . ? C182 C181 N31 120.2(7) . . ? C183 C182 C181 118.9(8) . . ? C183 C182 H18A 120.5 . . ? C181 C182 H18A 120.5 . . ? C182 C183 C184 120.0(8) . . ? C182 C183 H18B 120.0 . . ? C184 C183 H18B 120.0 . . ? C183 C184 C185 119.6(8) . . ? C183 C184 H18C 120.2 . . ? C185 C184 H18C 120.2 . . ? N32 C185 C184 120.1(8) . . ? N32 C185 N33 120.1(6) . . ? C184 C185 N33 119.7(7) . . ? N34 C191 C192 121.2(7) . . ? N34 C191 N33 118.4(6) . . ? C192 C191 N33 120.3(6) . . ? C193 C192 C191 118.7(7) . . ? C193 C192 H19A 120.6 . . ? C191 C192 H19A 120.6 . . ? C192 C193 C194 121.2(7) . . ? C192 C193 H19B 119.4 . . ? C194 C193 H19B 119.4 . . ? C193 C194 C195 118.3(7) . . ? C193 C194 H19C 120.9 . . ? C195 C194 H19C 120.9 . . ? N35 C195 N34 114.9(5) . . ? N35 C195 C194 124.2(7) . . ? N34 C195 C194 120.4(6) . . ? N36 C201 N35 116.1(6) . . ? N36 C201 C202 120.9(6) . . ? N35 C201 C202 122.9(6) . . ? C203 C202 C201 118.7(7) . . ? C203 C202 H20A 120.6 . . ? C201 C202 H20A 120.6 . . ? C202 C203 C204 120.7(7) . . ? C202 C203 H20B 119.6 . . ? C204 C203 H20B 119.6 . . ? C203 C204 C205 118.2(7) . . ? C203 C204 H20C 120.9 . . ? C205 C204 H20C 120.9 . . ? N36 C205 C204 122.0(7) . . ? N36 C205 H20D 119.0 . . ? C204 C205 H20D 119.0 . . ? N4 C1 H1A 109.5 . . ? N4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N6 C2 H2A 109.5 . . ? N6 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N6 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N13 C3 H3A 109.5 . . ? N13 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N13 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N15 C4 H4A 109.5 . . ? N15 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N15 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N22 C5 H5A 109.5 . . ? N22 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N22 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N24 C6 H6A 109.5 . . ? N24 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N24 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N31 C7 H7A 109.5 . . ? N31 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N31 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N33 C8 H8A 109.5 . . ? N33 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N33 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F2 P1 F5 90.9(7) . . ? F2 P1 F6 89.4(6) . . ? F5 P1 F6 89.9(6) . . ? F2 P1 F4 92.4(7) . . ? F5 P1 F4 89.8(7) . . ? F6 P1 F4 178.2(8) . . ? F2 P1 F3 90.6(7) . . ? F5 P1 F3 178.3(8) . . ? F6 P1 F3 90.7(6) . . ? F4 P1 F3 89.5(7) . . ? F2 P1 F1 178.1(8) . . ? F5 P1 F1 90.3(7) . . ? F6 P1 F1 89.1(6) . . ? F4 P1 F1 89.1(7) . . ? F3 P1 F1 88.2(6) . . ? F2B P1B F5B 90.4(7) . . ? F2B P1B F6B 90.5(6) . . ? F5B P1B F6B 90.9(6) . . ? F2B P1B F3B 90.4(7) . . ? F5B P1B F3B 178.1(8) . . ? F6B P1B F3B 90.8(6) . . ? F2B P1B F1B 179.1(8) . . ? F5B P1B F1B 90.3(7) . . ? F6B P1B F1B 90.1(6) . . ? F3B P1B F1B 88.9(6) . . ? F2B P1B F4B 90.5(7) . . ? F5B P1B F4B 90.0(7) . . ? F6B P1B F4B 178.7(8) . . ? F3B P1B F4B 88.3(6) . . ? F1B P1B F4B 88.9(7) . . ? F7 P2 F11 91.1(5) . . ? F7 P2 F9 90.1(5) . . ? F11 P2 F9 178.6(6) . . ? F7 P2 F12 91.9(5) . . ? F11 P2 F12 88.6(5) . . ? F9 P2 F12 91.9(6) . . ? F7 P2 F10 90.8(5) . . ? F11 P2 F10 88.3(5) . . ? F9 P2 F10 91.2(6) . . ? F12 P2 F10 175.9(6) . . ? F7 P2 F8 177.4(5) . . ? F11 P2 F8 91.2(5) . . ? F9 P2 F8 87.6(5) . . ? F12 P2 F8 89.2(5) . . ? F10 P2 F8 88.2(4) . . ? F7B P2B F12B 90.5(8) . . ? F7B P2B F11B 90.7(8) . . ? F12B P2B F11B 90.3(8) . . ? F7B P2B F9B 90.3(8) . . ? F12B P2B F9B 90.6(8) . . ? F11B P2B F9B 178.7(10) . . ? F7B P2B F10B 90.4(8) . . ? F12B P2B F10B 179.0(10) . . ? F11B P2B F10B 89.4(8) . . ? F9B P2B F10B 89.7(8) . . ? F7B P2B F8B 179.7(10) . . ? F12B P2B F8B 89.8(8) . . ? F11B P2B F8B 89.5(8) . . ? F9B P2B F8B 89.5(8) . . ? F10B P2B F8B 89.3(8) . . ? F14 P3 F17 91.1(6) . . ? F14 P3 F13 177.8(7) . . ? F17 P3 F13 89.4(5) . . ? F14 P3 F18 87.3(6) . . ? F17 P3 F18 89.9(5) . . ? F13 P3 F18 90.5(6) . . ? F14 P3 F16 90.1(6) . . ? F17 P3 F16 90.9(5) . . ? F13 P3 F16 92.1(6) . . ? F18 P3 F16 177.3(6) . . ? F14 P3 F15 90.6(5) . . ? F17 P3 F15 178.2(7) . . ? F13 P3 F15 89.0(5) . . ? F18 P3 F15 90.8(5) . . ? F16 P3 F15 88.5(5) . . ? F17B P3B F13B 90.2(8) . . ? F17B P3B F15B 179.3(10) . . ? F13B P3B F15B 89.5(8) . . ? F17B P3B F14B 89.6(8) . . ? F13B P3B F14B 179.5(10) . . ? F15B P3B F14B 90.8(8) . . ? F17B P3B F18B 89.9(8) . . ? F13B P3B F18B 90.4(8) . . ? F15B P3B F18B 90.8(8) . . ? F14B P3B F18B 89.2(8) . . ? F17B P3B F16B 89.9(8) . . ? F13B P3B F16B 90.2(8) . . ? F15B P3B F16B 89.4(8) . . ? F14B P3B F16B 90.2(8) . . ? F18B P3B F16B 179.4(11) . . ? F21 P4 F19 90.7(8) . . ? F21 P4 F24 90.4(8) . . ? F19 P4 F24 91.0(8) . . ? F21 P4 F23 178.6(9) . . ? F19 P4 F23 89.8(8) . . ? F24 P4 F23 90.9(8) . . ? F21 P4 F20 89.5(8) . . ? F19 P4 F20 178.8(10) . . ? F24 P4 F20 90.2(8) . . ? F23 P4 F20 90.0(8) . . ? F21 P4 F22 89.8(8) . . ? F19 P4 F22 89.3(8) . . ? F24 P4 F22 179.6(11) . . ? F23 P4 F22 88.9(8) . . ? F20 P4 F22 89.5(8) . . ? F21B P4B F19B 84.6(6) . . ? F21B P4B F22B 92.3(7) . . ? F19B P4B F22B 89.1(6) . . ? F21B P4B F20B 91.8(6) . . ? F19B P4B F20B 176.1(8) . . ? F22B P4B F20B 89.4(7) . . ? F21B P4B F24B 89.8(6) . . ? F19B P4B F24B 92.8(7) . . ? F22B P4B F24B 177.4(8) . . ? F20B P4B F24B 88.9(7) . . ? F21B P4B F23B 176.9(7) . . ? F19B P4B F23B 92.8(6) . . ? F22B P4B F23B 89.4(7) . . ? F20B P4B F23B 90.8(6) . . ? F24B P4B F23B 88.6(6) . . ? O1 C1S C3S 120.9(11) . . ? O1 C1S C2S 119.7(10) . . ? C3S C1S C2S 119.3(12) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C3S H3SA 109.5 . . ? C1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O1B C1SB C3SB 119.7(15) . . ? O1B C1SB C2SB 120.0(15) . . ? C3SB C1SB C2SB 120.3(19) . . ? C1SB C2SB H2SD 109.5 . . ? C1SB C2SB H2SE 109.5 . . ? H2SD C2SB H2SE 109.5 . . ? C1SB C2SB H2SF 109.5 . . ? H2SD C2SB H2SF 109.5 . . ? H2SE C2SB H2SF 109.5 . . ? C1SB C3SB H3SD 109.5 . . ? C1SB C3SB H3SE 109.5 . . ? H3SD C3SB H3SE 109.5 . . ? C1SB C3SB H3SF 109.5 . . ? H3SD C3SB H3SF 109.5 . . ? H3SE C3SB H3SF 109.5 . . ? C4S O3 C5S 68(2) . 2_865 ? O3 C4S C6S 118.0(15) . . ? O3 C4S C5S 121.3(14) . . ? C6S C4S C5S 120.5(19) . . ? O3 C4S C5S 74(2) . 2_865 ? C6S C4S C5S 95(3) . 2_865 ? C5S C4S C5S 104(2) . 2_865 ? C4S C5S C4S 76(2) . 2_865 ? C4S C5S O3 95(2) . 2_865 ? C4S C5S O3 38.0(8) 2_865 2_865 ? C4S C5S H5SA 109.5 . . ? C4S C5S H5SA 75.7 2_865 . ? O3 C5S H5SA 99.1 2_865 . ? C4S C5S H5SB 109.5 . . ? C4S C5S H5SB 170.1 2_865 . ? O3 C5S H5SB 132.1 2_865 . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? C4S C5S H5SC 60.6 2_865 . ? O3 C5S H5SC 22.8 2_865 . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C4S C6S H6SA 109.5 . . ? C4S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C4S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.173 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.104