# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_sk_sk_013_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 N O3' _chemical_formula_sum 'C17 H19 N O3' _chemical_formula_weight 285.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' _symmetry_space_group_name_Hall 'P 2yb' _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7736(4) _cell_length_b 6.5159(2) _cell_length_c 11.9527(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.729(2) _cell_angle_gamma 90.00 _cell_volume 732.69(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4906 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 35.81 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.078 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.989 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'SADABS; BRUKER, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4218 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3008 _reflns_number_gt 2927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(1) _refine_ls_number_reflns 3008 _refine_ls_number_parameters 192 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.003 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 C2 C -0.28173(12) 0.2557(2) 0.45094(11) 0.0166(2) Uani 1 1 d . . . H2 H -0.3473 0.3422 0.4022 0.020 Uiso 1 1 calc R . . C1 C -0.21762(12) 0.31571(19) 0.56293(11) 0.0157(2) Uani 1 1 d . . . C6 C -0.00076(11) -0.15436(19) 0.67213(10) 0.0149(2) Uani 1 1 d . . . H6 H 0.0111 -0.2832 0.6426 0.018 Uiso 1 1 calc R . . C5 C -0.08781(11) -0.00864(19) 0.59661(10) 0.0150(2) Uani 1 1 d . . . C4 C -0.15464(12) -0.0669(2) 0.47987(11) 0.0170(3) Uani 1 1 d . . . H4 H -0.1341 -0.1933 0.4521 0.020 Uiso 1 1 calc R . . C11 C 0.38252(12) 0.0960(2) 0.82963(10) 0.0187(3) Uani 1 1 d . . . H11 H 0.3080 0.1843 0.8304 0.022 Uiso 1 1 calc R . . C10 C 0.38774(12) -0.0991(2) 0.87916(10) 0.0167(2) Uani 1 1 d . . . C9 C 0.27895(12) -0.1684(2) 0.94079(11) 0.0180(3) Uani 1 1 d . . . H9A H 0.2507 -0.0504 0.9788 0.022 Uiso 1 1 calc R . . H9B H 0.3239 -0.2658 1.0009 0.022 Uiso 1 1 calc R . . C7 C 0.14430(12) -0.26832(19) 0.86182(10) 0.0150(2) Uani 1 1 d . . . H7 H 0.1725 -0.3796 0.8176 0.018 Uiso 1 1 calc R . . C8 C 0.05303(12) -0.3582(2) 0.93696(11) 0.0174(2) Uani 1 1 d . . . H8A H 0.1017 -0.4762 0.9790 0.021 Uiso 1 1 calc R . . H8B H 0.0443 -0.2563 0.9938 0.021 Uiso 1 1 calc R . . C15 C 0.50011(12) -0.2295(2) 0.87541(10) 0.0196(3) Uani 1 1 d . . . H15 H 0.5037 -0.3608 0.9065 0.024 Uiso 1 1 calc R . . C14 C 0.60707(13) -0.1660(2) 0.82584(12) 0.0243(3) Uani 1 1 d . . . H14 H 0.6819 -0.2536 0.8250 0.029 Uiso 1 1 calc R . . C3 C -0.24932(12) 0.0634(2) 0.40836(10) 0.0173(3) Uani 1 1 d . . . H3 H -0.2924 0.0258 0.3318 0.021 Uiso 1 1 calc R . . C12 C 0.48855(14) 0.1592(2) 0.77895(11) 0.0220(3) Uani 1 1 d . . . H12 H 0.4839 0.2890 0.7458 0.026 Uiso 1 1 calc R . . C13 C 0.60083(13) 0.0296(2) 0.77761(11) 0.0245(3) Uani 1 1 d . . . H13 H 0.6717 0.0733 0.7446 0.029 Uiso 1 1 calc R . . C16 C -0.37418(13) 0.5980(2) 0.55453(11) 0.0214(3) Uani 1 1 d . . . H16A H -0.4528 0.5055 0.5459 0.032 Uiso 1 1 calc R . . H16B H -0.3689 0.6424 0.4792 0.032 Uiso 1 1 calc R . . H16C H -0.3874 0.7149 0.5994 0.032 Uiso 1 1 calc R . . C17 C -0.11271(11) 0.18833(19) 0.64136(10) 0.0142(2) Uani 1 1 d . . . O2 O -0.04896(9) 0.24619(14) 0.74568(7) 0.0186(2) Uani 1 1 d . . . O3 O -0.08430(8) -0.41853(15) 0.87245(8) 0.0199(2) Uani 1 1 d . . . H3A H -0.0780 -0.5101 0.8271 0.030 Uiso 1 1 calc R . . O1 O -0.24522(9) 0.49534(14) 0.61279(8) 0.0208(2) Uani 1 1 d . . . N1 N 0.06311(10) -0.11590(16) 0.78056(9) 0.0154(2) Uani 1 1 d . . . H1 H 0.0573 0.0064 0.8060 0.018 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 C2 0.0138(5) 0.0187(6) 0.0168(5) 0.0056(5) 0.0036(4) 0.0003(4) C1 0.0139(5) 0.0139(5) 0.0201(6) 0.0012(5) 0.0062(4) -0.0019(4) C6 0.0130(5) 0.0161(5) 0.0164(6) -0.0006(4) 0.0057(4) -0.0003(4) C5 0.0122(5) 0.0175(6) 0.0154(6) 0.0014(5) 0.0041(4) -0.0004(4) C4 0.0170(5) 0.0192(6) 0.0160(6) -0.0012(5) 0.0066(4) -0.0001(4) C11 0.0170(5) 0.0214(6) 0.0166(6) -0.0022(5) 0.0029(4) 0.0019(5) C10 0.0144(5) 0.0228(6) 0.0114(5) -0.0018(5) 0.0009(4) -0.0007(5) C9 0.0160(5) 0.0243(6) 0.0130(5) -0.0001(5) 0.0027(4) 0.0000(5) C7 0.0150(5) 0.0147(5) 0.0144(5) 0.0003(5) 0.0026(4) 0.0030(4) C8 0.0180(5) 0.0171(6) 0.0174(5) -0.0007(5) 0.0053(4) 0.0001(4) C15 0.0188(5) 0.0228(6) 0.0154(5) 0.0012(5) 0.0015(4) 0.0033(5) C14 0.0160(5) 0.0364(8) 0.0199(6) -0.0040(6) 0.0037(4) 0.0052(5) C3 0.0170(5) 0.0229(6) 0.0124(5) 0.0014(5) 0.0046(4) -0.0022(5) C12 0.0266(6) 0.0223(6) 0.0162(5) -0.0006(5) 0.0041(5) -0.0052(5) C13 0.0182(5) 0.0385(8) 0.0176(6) -0.0025(6) 0.0063(4) -0.0052(5) C16 0.0201(6) 0.0200(6) 0.0236(6) 0.0010(5) 0.0049(5) 0.0057(5) C17 0.0120(5) 0.0161(6) 0.0147(5) 0.0017(4) 0.0040(4) -0.0029(4) O2 0.0197(4) 0.0164(4) 0.0171(4) -0.0023(4) 0.0007(3) 0.0017(3) O3 0.0165(4) 0.0187(4) 0.0251(5) -0.0041(4) 0.0066(3) 0.0000(3) O1 0.0210(4) 0.0168(4) 0.0211(5) -0.0001(4) -0.0004(3) 0.0063(3) N1 0.0154(4) 0.0136(5) 0.0161(5) 0.0004(4) 0.0026(4) 0.0024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C1 1.3721(17) . ? C2 C3 1.4205(18) . ? C1 O1 1.3730(15) . ? C1 C17 1.4484(16) . ? C6 N1 1.3013(15) . ? C6 C5 1.4226(16) . ? C5 C4 1.4226(16) . ? C5 C17 1.4363(17) . ? C4 C3 1.3706(17) . ? C11 C12 1.3967(18) . ? C11 C10 1.3977(19) . ? C10 C15 1.3986(17) . ? C10 C9 1.5171(17) . ? C9 C7 1.5407(15) . ? C7 N1 1.4634(15) . ? C7 C8 1.5426(16) . ? C8 O3 1.4105(14) . ? C15 C14 1.3967(18) . ? C14 C13 1.394(2) . ? C12 C13 1.388(2) . ? C16 O1 1.4300(14) . ? C17 O2 1.2899(14) . ? 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 C1 C2 C3 120.91(11) . . ? C2 C1 O1 125.09(11) . . ? C2 C1 C17 121.61(11) . . ? O1 C1 C17 113.30(10) . . ? N1 C6 C5 123.11(11) . . ? C6 C5 C4 118.74(11) . . ? C6 C5 C17 119.51(10) . . ? C4 C5 C17 121.65(11) . . ? C3 C4 C5 119.95(12) . . ? C12 C11 C10 120.36(12) . . ? C11 C10 C15 118.54(12) . . ? C11 C10 C9 121.76(11) . . ? C15 C10 C9 119.65(11) . . ? C10 C9 C7 115.02(9) . . ? N1 C7 C9 109.83(10) . . ? N1 C7 C8 110.42(9) . . ? C9 C7 C8 109.66(9) . . ? O3 C8 C7 113.72(10) . . ? C14 C15 C10 121.21(13) . . ? C13 C14 C15 119.51(12) . . ? C4 C3 C2 120.10(11) . . ? C13 C12 C11 120.52(13) . . ? C14 C13 C12 119.84(12) . . ? O2 C17 C5 122.34(11) . . ? O2 C17 C1 121.99(11) . . ? C5 C17 C1 115.64(10) . . ? C1 O1 C16 115.99(10) . . ? C6 N1 C7 123.90(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.242 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 900846' ####################################################################### # # 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_sk_sk_099_m1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H60 N4 Ni4 O16, 4(C2 H3 N)' _chemical_formula_sum 'C68 H72 N8 Ni4 O16' _chemical_formula_weight 1492.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4(1)/a ' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+3/4' 'y+1/4, -x+1/4, z+1/4' '-x, -y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+5/4' 'y+3/4, -x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' '-x, -y, -z' 'y-1/4, -x-3/4, -z-3/4' '-y-1/4, x-1/4, -z-1/4' 'x, y-1/2, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z-1/4' '-y+1/4, x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' _cell_length_a 24.030(3) _cell_length_b 24.030(3) _cell_length_c 15.0512(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8691(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3112 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 21.97 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.14 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15773 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.78 _reflns_number_total 4148 _reflns_number_gt 2345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4148 _refine_ls_number_parameters 215 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 0.053763(19) 0.288393(19) 1.05457(3) 0.03740(18) Uani 1 1 d . . . O1 O 0.13292(10) 0.26639(11) 1.05518(16) 0.0484(7) Uani 1 1 d . . . O2 O 0.23293(13) 0.24664(17) 1.1053(2) 0.0898(12) Uani 1 1 d . . . O3 O -0.02905(9) 0.29567(10) 1.05787(14) 0.0372(6) Uani 1 1 d . . . O4 O 0.06987(14) 0.37513(13) 1.0856(2) 0.0538(8) Uani 1 1 d D . . N1 N 0.06013(13) 0.31225(13) 0.92388(19) 0.0413(8) Uani 1 1 d . . . C1 C 0.17153(17) 0.28964(19) 1.0085(3) 0.0540(11) Uani 1 1 d . . . C2 C 0.16144(18) 0.3234(2) 0.9333(3) 0.0623(12) Uani 1 1 d . . . C3 C 0.2075(2) 0.3496(3) 0.8913(4) 0.101(2) Uani 1 1 d . . . H3 H 0.2011 0.3728 0.8430 0.121 Uiso 1 1 calc R . . C4 C 0.2600(3) 0.3420(4) 0.9193(5) 0.134(3) Uani 1 1 d . . . H4A H 0.2892 0.3604 0.8912 0.161 Uiso 1 1 calc R . . C5 C 0.2708(2) 0.3064(3) 0.9907(4) 0.117(2) Uani 1 1 d . . . H5 H 0.3073 0.2998 1.0084 0.140 Uiso 1 1 calc R . . C6 C 0.22737(19) 0.2814(3) 1.0344(3) 0.0774(15) Uani 1 1 d . . . C7 C 0.2878(2) 0.2341(3) 1.1357(4) 0.125(3) Uani 1 1 d . . . H7A H 0.3098 0.2208 1.0868 0.187 Uiso 1 1 calc R . . H7B H 0.2860 0.2060 1.1809 0.187 Uiso 1 1 calc R . . H7C H 0.3045 0.2672 1.1597 0.187 Uiso 1 1 calc R . . C8 C 0.10726(19) 0.33079(19) 0.8951(3) 0.0576(12) Uani 1 1 d . . . H8 H 0.1059 0.3515 0.8430 0.069 Uiso 1 1 calc R . . C9 C 0.01299(17) 0.31937(15) 0.8675(2) 0.0433(9) Uani 1 1 d . . . C10 C 0.0188(2) 0.31565(17) 0.7753(3) 0.0551(11) Uani 1 1 d . . . H10 H 0.0536 0.3085 0.7509 0.066 Uiso 1 1 calc R . . C11 C -0.0268(2) 0.3226(2) 0.7198(3) 0.0694(14) Uani 1 1 d . . . H11 H -0.0220 0.3220 0.6585 0.083 Uiso 1 1 calc R . . C12 C -0.0781(2) 0.3301(2) 0.7544(3) 0.0712(14) Uani 1 1 d . . . H12 H -0.1087 0.3342 0.7172 0.085 Uiso 1 1 calc R . . C13 C -0.08484(19) 0.33168(17) 0.8456(3) 0.0581(11) Uani 1 1 d . . . H13 H -0.1204 0.3359 0.8689 0.070 Uiso 1 1 calc R . . C14 C -0.04004(16) 0.32709(16) 0.9034(2) 0.0443(10) Uani 1 1 d . . . C15 C -0.05202(17) 0.33673(16) 1.0009(2) 0.0461(10) Uani 1 1 d . . . H15A H -0.0373 0.3728 1.0178 0.055 Uiso 1 1 calc R . . H15B H -0.0920 0.3377 1.0095 0.055 Uiso 1 1 calc R . . N2 N 0.8799(3) 0.5339(3) 0.0237(5) 0.1581(17) Uani 1 1 d . . . C16 C 0.8325(3) 0.4606(3) 0.1189(5) 0.1581(17) Uani 1 1 d . . . H16A H 0.8605 0.4406 0.1515 0.237 Uiso 1 1 calc R . . H16B H 0.8120 0.4350 0.0825 0.237 Uiso 1 1 calc R . . H16C H 0.8077 0.4785 0.1597 0.237 Uiso 1 1 calc R . . C17 C 0.8592(4) 0.5024(4) 0.0625(6) 0.1581(17) Uani 1 1 d . . . H4W1 H 0.041(3) 0.387(3) 1.113(4) 0.14(3) Uiso 1 1 d . . . H4W2 H 0.065(3) 0.399(2) 1.045(4) 0.18(4) Uiso 1 1 d 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 0.0375(3) 0.0416(3) 0.0331(3) 0.0025(2) 0.0005(2) -0.0015(2) O1 0.0309(14) 0.0663(18) 0.0480(15) 0.0084(14) 0.0016(12) -0.0033(13) O2 0.044(2) 0.134(3) 0.092(3) 0.021(2) -0.0083(18) 0.008(2) O3 0.0360(14) 0.0428(14) 0.0328(13) 0.0046(11) 0.0000(11) 0.0030(11) O4 0.062(2) 0.0471(18) 0.0521(18) 0.0030(15) 0.0040(16) -0.0072(15) N1 0.0468(19) 0.0445(18) 0.0326(17) 0.0020(14) 0.0009(14) 0.0003(15) C1 0.038(2) 0.069(3) 0.055(3) 0.000(2) 0.003(2) -0.006(2) C2 0.048(3) 0.086(3) 0.052(3) 0.012(2) 0.009(2) -0.013(2) C3 0.068(4) 0.156(6) 0.079(4) 0.037(4) 0.012(3) -0.033(4) C4 0.060(4) 0.225(9) 0.118(5) 0.060(6) 0.019(4) -0.022(5) C5 0.034(3) 0.206(8) 0.111(5) 0.023(5) 0.011(3) -0.016(4) C6 0.044(3) 0.114(5) 0.074(3) 0.004(3) 0.000(3) -0.001(3) C7 0.045(3) 0.184(7) 0.145(6) 0.022(5) -0.030(4) 0.030(4) C8 0.061(3) 0.069(3) 0.042(2) 0.016(2) 0.009(2) -0.002(2) C9 0.060(3) 0.034(2) 0.036(2) 0.0032(17) -0.0002(19) 0.0041(18) C10 0.072(3) 0.050(3) 0.044(2) 0.0042(19) 0.001(2) 0.002(2) C11 0.104(4) 0.073(3) 0.032(2) -0.002(2) -0.011(3) 0.013(3) C12 0.085(4) 0.074(4) 0.054(3) -0.001(2) -0.024(3) 0.006(3) C13 0.060(3) 0.059(3) 0.055(3) 0.011(2) -0.009(2) 0.003(2) C14 0.050(2) 0.046(2) 0.037(2) 0.0047(18) -0.0082(19) 0.0008(19) C15 0.049(2) 0.043(2) 0.046(2) 0.0079(19) -0.0014(19) 0.0111(19) N2 0.148(4) 0.157(5) 0.169(4) 0.083(3) 0.008(3) -0.015(3) C16 0.148(4) 0.157(5) 0.169(4) 0.083(3) 0.008(3) -0.015(3) C17 0.148(4) 0.157(5) 0.169(4) 0.083(3) 0.008(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.974(2) . ? Ni1 O3 1.998(2) . ? Ni1 N1 2.055(3) . ? Ni1 O3 2.092(2) 10_568 ? Ni1 O3 2.106(2) 4 ? Ni1 O4 2.171(3) . ? O1 C1 1.291(4) . ? O2 C6 1.361(6) . ? O2 C7 1.427(5) . ? O3 C15 1.419(4) . ? O3 Ni1 2.092(2) 15_557 ? O3 Ni1 2.106(2) 4 ? O4 H4W1 0.86(6) . ? O4 H4W2 0.84(2) . ? N1 C8 1.292(5) . ? N1 C9 1.426(5) . ? C1 C6 1.411(6) . ? C1 C2 1.413(6) . ? C2 C3 1.423(6) . ? C2 C8 1.435(6) . ? C3 C4 1.342(8) . ? C3 H3 0.9300 . ? C4 C5 1.397(8) . ? C4 H4A 0.9300 . ? C5 C6 1.374(7) . ? C5 H5 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8 0.9300 . ? C9 C10 1.397(5) . ? C9 C14 1.397(5) . ? C10 C11 1.387(6) . ? C10 H10 0.9300 . ? C11 C12 1.351(6) . ? C11 H11 0.9300 . ? C12 C13 1.383(6) . ? C12 H12 0.9300 . ? C13 C14 1.389(5) . ? C13 H13 0.9300 . ? C14 C15 1.513(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? N2 C17 1.078(8) . ? C16 C17 1.464(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O3 169.36(10) . . ? O1 Ni1 N1 90.42(12) . . ? O3 Ni1 N1 94.22(11) . . ? O1 Ni1 O3 93.22(10) . 10_568 ? O3 Ni1 O3 83.81(10) . 10_568 ? N1 Ni1 O3 169.92(11) . 10_568 ? O1 Ni1 O3 90.84(10) . 4 ? O3 Ni1 O3 78.61(10) . 4 ? N1 Ni1 O3 108.14(11) . 4 ? O3 Ni1 O3 81.23(9) 10_568 4 ? O1 Ni1 O4 94.84(12) . . ? O3 Ni1 O4 95.05(11) . . ? N1 Ni1 O4 85.70(12) . . ? O3 Ni1 O4 84.63(11) 10_568 . ? O3 Ni1 O4 165.03(11) 4 . ? C1 O1 Ni1 125.0(3) . . ? C6 O2 C7 118.1(4) . . ? C15 O3 Ni1 115.7(2) . . ? C15 O3 Ni1 119.4(2) . 15_557 ? Ni1 O3 Ni1 98.03(9) . 15_557 ? C15 O3 Ni1 122.9(2) . 4 ? Ni1 O3 Ni1 101.32(10) . 4 ? Ni1 O3 Ni1 94.72(9) 15_557 4 ? Ni1 O4 H4W1 105(4) . . ? Ni1 O4 H4W2 117(5) . . ? H4W1 O4 H4W2 92(6) . . ? C8 N1 C9 117.1(3) . . ? C8 N1 Ni1 118.9(3) . . ? C9 N1 Ni1 123.0(2) . . ? O1 C1 C6 118.2(4) . . ? O1 C1 C2 124.1(4) . . ? C6 C1 C2 117.7(4) . . ? C1 C2 C3 118.5(4) . . ? C1 C2 C8 123.2(4) . . ? C3 C2 C8 118.3(4) . . ? C4 C3 C2 122.1(6) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? O2 C6 C5 124.7(5) . . ? O2 C6 C1 113.3(4) . . ? C5 C6 C1 121.9(5) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C2 128.2(4) . . ? N1 C8 H8 115.9 . . ? C2 C8 H8 115.9 . . ? C10 C9 C14 119.0(4) . . ? C10 C9 N1 120.3(4) . . ? C14 C9 N1 120.6(3) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.2(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 121.9(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C9 118.4(4) . . ? C13 C14 C15 116.6(4) . . ? C9 C14 C15 124.7(3) . . ? O3 C15 C14 113.9(3) . . ? O3 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? O3 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C16 177.3(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.78 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.504 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.064 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.294 0.193 -0.187 2706.6 -27.0 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 900847' ####################################################################### # # 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_sk_sk_100_1_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H40 N8 Ni4 O20' _chemical_formula_sum 'C56 H40 N8 Ni4 O20' _chemical_formula_weight 1379.72 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cc ' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 23.8710(19) _cell_length_b 15.5094(13) _cell_length_c 19.9409(19) _cell_angle_alpha 90.00 _cell_angle_beta 107.492(5) _cell_angle_gamma 90.00 _cell_volume 7041.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.09 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.74 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816.0 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.617 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32858 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.17 _reflns_number_total 9581 _reflns_number_gt 8246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.081(12) _refine_ls_number_reflns 9581 _refine_ls_number_parameters 793 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.006 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 0.90889(3) 0.33686(4) 0.47148(4) 0.04108(17) Uani 1 1 d . . . Ni2 Ni 0.96500(3) 0.22190(4) 0.59902(3) 0.03753(17) Uani 1 1 d . . . Ni3 Ni 1.01560(3) 0.21662(4) 0.47373(3) 0.03891(17) Uani 1 1 d . . . Ni4 Ni 0.89194(3) 0.13964(4) 0.45459(3) 0.03765(16) Uani 1 1 d . . . O4 O 0.88591(16) 0.2331(2) 0.52655(19) 0.0352(9) Uani 1 1 d . . . O6 O 0.99409(16) 0.3056(2) 0.5337(2) 0.0359(8) Uani 1 1 d . . . O5 O 1.01978(17) 0.1250(2) 0.4064(2) 0.0528(10) Uani 1 1 d . . . N3 N 1.0712(2) 0.2941(3) 0.4390(2) 0.0434(10) Uani 1 1 d . . . O2 O 0.92840(16) 0.2426(2) 0.4131(2) 0.0378(9) Uani 1 1 d . . . O13 O 0.7792(3) 0.7665(3) 0.4164(4) 0.111(2) Uani 1 1 d . . . O1 O 0.90038(18) 0.4255(2) 0.5403(2) 0.0513(10) Uani 1 1 d . . . O12 O 0.91192(16) 0.0604(2) 0.3738(2) 0.0505(10) Uani 1 1 d . . . O7 O 0.81179(16) 0.1637(2) 0.39065(19) 0.0423(9) Uani 1 1 d . . . N4 N 0.86492(18) 0.0246(3) 0.4865(2) 0.0420(11) Uani 1 1 d . . . O19 O 0.6172(3) -0.0588(4) 0.1922(3) 0.107(2) Uani 1 1 d . . . O3 O 1.04600(15) 0.1985(3) 0.6580(2) 0.0454(9) Uani 1 1 d . . . O15 O 1.1696(3) 0.2437(4) 0.9763(3) 0.105(2) Uani 1 1 d . . . N2 N 0.93145(19) 0.1600(3) 0.6694(2) 0.0407(10) Uani 1 1 d . . . O9 O 0.81778(18) 0.3389(2) 0.4073(2) 0.0550(11) Uani 1 1 d . . . C41 C 1.0610(2) 0.4176(3) 0.5128(3) 0.0426(13) Uani 1 1 d . . . O18 O 1.2343(3) 0.1013(4) 0.2945(4) 0.132(3) Uani 1 1 d D . . N1 N 0.9184(2) 0.4330(3) 0.4052(2) 0.0460(11) Uani 1 1 d . . . C47 C 0.7358(2) -0.0403(4) 0.3459(3) 0.0451(13) Uani 1 1 d . . . H47 H 0.7348 -0.0955 0.3638 0.054 Uiso 1 1 calc R . . O8 O 0.97307(15) 0.1323(2) 0.5226(2) 0.0362(9) Uani 1 1 d . . . C22 C 0.8745(2) 0.1273(3) 0.6544(3) 0.0411(12) Uani 1 1 d . . . C29 C 1.0594(2) 0.1129(3) 0.3772(3) 0.0400(12) Uani 1 1 d . . . C34 C 1.1049(2) 0.1753(3) 0.3799(3) 0.0504(14) Uani 1 1 d . . . C35 C 1.1073(3) 0.2602(4) 0.4096(3) 0.0496(14) Uani 1 1 d . . . H35 H 1.1386 0.2947 0.4074 0.060 Uiso 1 1 calc R . . C36 C 1.0796(2) 0.3848(3) 0.4574(3) 0.0460(13) Uani 1 1 d . . . C40 C 1.0692(3) 0.5056(3) 0.5264(3) 0.0562(15) Uani 1 1 d . . . H40 H 1.0557 0.5295 0.5615 0.067 Uiso 1 1 calc R . . C39 C 1.0963(3) 0.5589(4) 0.4902(4) 0.0675(18) Uani 1 1 d . . . H39 H 1.1036 0.6163 0.5032 0.081 Uiso 1 1 calc R . . C38 C 1.1123(3) 0.5262(4) 0.4350(4) 0.073(2) Uani 1 1 d . . . H38 H 1.1288 0.5621 0.4086 0.088 Uiso 1 1 calc R . . C37 C 1.1039(3) 0.4398(4) 0.4186(4) 0.0621(17) Uani 1 1 d . . . H37 H 1.1147 0.4179 0.3809 0.075 Uiso 1 1 calc R . . C42 C 1.0380(3) 0.3675(4) 0.5643(3) 0.0493(14) Uani 1 1 d . . . H42A H 1.0707 0.3382 0.5973 0.059 Uiso 1 1 calc R . . H42B H 1.0221 0.4081 0.5909 0.059 Uiso 1 1 calc R . . C33 C 1.1477(3) 0.1534(4) 0.3490(5) 0.078(2) Uani 1 1 d . . . H33 H 1.1780 0.1920 0.3510 0.093 Uiso 1 1 calc R . . C32 C 1.1462(3) 0.0767(5) 0.3158(5) 0.079(2) Uani 1 1 d . . . N7 N 1.1919(4) 0.0567(6) 0.2839(6) 0.153(4) Uani 1 1 d D . . C31 C 1.1018(3) 0.0168(4) 0.3115(4) 0.0675(19) Uani 1 1 d . . . H31 H 1.1008 -0.0348 0.2874 0.081 Uiso 1 1 calc R . . C30 C 1.0617(3) 0.0340(4) 0.3416(4) 0.0610(17) Uani 1 1 d . . . H30 H 1.0330 -0.0073 0.3397 0.073 Uiso 1 1 calc R . . O11 O 1.09497(16) 0.1797(3) 0.5543(2) 0.0526(10) Uani 1 1 d . . . C14 C 0.9115(3) 0.2580(4) 0.3405(3) 0.0511(15) Uani 1 1 d . . . H14A H 0.8694 0.2679 0.3241 0.061 Uiso 1 1 calc R . . H14B H 0.9196 0.2068 0.3170 0.061 Uiso 1 1 calc R . . C13 C 0.9428(3) 0.3353(3) 0.3196(3) 0.0486(14) Uani 1 1 d . . . C8 C 0.9435(3) 0.4188(3) 0.3481(3) 0.0461(13) Uani 1 1 d . . . C7 C 0.8923(3) 0.5058(4) 0.4027(3) 0.0556(16) Uani 1 1 d . . . H7 H 0.8872 0.5398 0.3629 0.067 Uiso 1 1 calc R . . C6 C 0.8702(3) 0.5387(3) 0.4587(3) 0.0507(15) Uani 1 1 d . . . C5 C 0.8402(3) 0.6161(3) 0.4453(4) 0.0600(16) Uani 1 1 d . . . H5 H 0.8344 0.6420 0.4017 0.072 Uiso 1 1 calc R . . C4 C 0.8188(3) 0.6559(4) 0.4930(4) 0.0655(18) Uani 1 1 d . . . N5 N 0.7865(3) 0.7365(4) 0.4746(5) 0.085(2) Uani 1 1 d . . . O14 O 0.7657(3) 0.7674(4) 0.5189(4) 0.126(3) Uani 1 1 d . . . C3 C 0.8295(3) 0.6229(4) 0.5593(5) 0.078(2) Uani 1 1 d . . . H3 H 0.8162 0.6519 0.5924 0.094 Uiso 1 1 calc R . . C2 C 0.8605(3) 0.5456(4) 0.5774(4) 0.0684(19) Uani 1 1 d . . . H2 H 0.8699 0.5244 0.6231 0.082 Uiso 1 1 calc R . . C1 C 0.8778(3) 0.4994(4) 0.5241(3) 0.0495(14) Uani 1 1 d . . . C9 C 0.9696(3) 0.4852(4) 0.3239(3) 0.0589(16) Uani 1 1 d . . . H9A H 0.9716 0.5399 0.3436 0.071 Uiso 1 1 calc R . . C10 C 0.9935(3) 0.4691(5) 0.2679(4) 0.073(2) Uani 1 1 d . . . H10 H 1.0116 0.5142 0.2515 0.088 Uiso 1 1 calc R . . C11 C 0.9911(3) 0.3947(5) 0.2391(4) 0.0714(19) Uani 1 1 d . . . H11A H 1.0053 0.3865 0.2009 0.086 Uiso 1 1 calc R . . C12 C 0.9663(3) 0.3252(4) 0.2670(3) 0.0610(16) Uani 1 1 d . . . H12A H 0.9663 0.2705 0.2480 0.073 Uiso 1 1 calc R . . C43 C 0.7767(2) 0.1048(3) 0.3586(3) 0.0372(12) Uani 1 1 d . . . C44 C 0.7338(2) 0.1258(3) 0.2938(3) 0.0443(13) Uani 1 1 d . . . H44 H 0.7328 0.1813 0.2759 0.053 Uiso 1 1 calc R . . C45 C 0.6945(2) 0.0669(4) 0.2577(3) 0.0521(14) Uani 1 1 d . . . H45 H 0.6664 0.0823 0.2158 0.062 Uiso 1 1 calc R . . C46 C 0.6961(2) -0.0174(4) 0.2836(3) 0.0438(13) Uani 1 1 d . . . C48 C 0.7781(2) 0.0184(3) 0.3829(3) 0.0391(12) Uani 1 1 d . . . C49 C 0.8197(2) -0.0135(3) 0.4466(3) 0.0409(12) Uani 1 1 d . . . H49 H 0.8126 -0.0687 0.4603 0.049 Uiso 1 1 calc R . . C50 C 0.8997(2) -0.0206(3) 0.5487(3) 0.0442(13) Uani 1 1 d . . . C55 C 0.9591(2) -0.0075(3) 0.5736(3) 0.0443(13) Uani 1 1 d . . . C54 C 0.9906(3) -0.0518(4) 0.6352(4) 0.0647(18) Uani 1 1 d . . . H54 H 1.0308 -0.0432 0.6544 0.078 Uiso 1 1 calc R . . C53 C 0.9610(3) -0.1085(5) 0.6674(4) 0.085(2) Uani 1 1 d . . . H53 H 0.9818 -0.1360 0.7089 0.102 Uiso 1 1 calc R . . C52 C 0.9048(3) -0.1238(4) 0.6403(4) 0.0681(19) Uani 1 1 d . . . H52 H 0.8867 -0.1649 0.6607 0.082 Uiso 1 1 calc R . . C51 C 0.8719(3) -0.0783(3) 0.5808(3) 0.0517(14) Uani 1 1 d . . . H51 H 0.8316 -0.0870 0.5629 0.062 Uiso 1 1 calc R . . C56 C 0.9947(3) 0.0471(3) 0.5400(3) 0.0465(13) Uani 1 1 d . . . H56A H 1.0345 0.0506 0.5716 0.056 Uiso 1 1 calc R . . H56B H 0.9966 0.0186 0.4974 0.056 Uiso 1 1 calc R . . N8 N 0.6527(2) -0.0812(4) 0.2464(3) 0.0647(14) Uani 1 1 d . . . O20 O 0.6532(2) -0.1515(3) 0.2714(3) 0.0904(16) Uani 1 1 d . . . C15 C 1.0616(2) 0.2010(3) 0.7246(3) 0.0449(13) Uani 1 1 d . . . C20 C 1.0225(2) 0.1866(3) 0.7661(3) 0.0434(13) Uani 1 1 d . . . C19 C 1.0430(2) 0.1933(3) 0.8367(3) 0.0520(15) Uani 1 1 d . . . H19 H 1.0171 0.1853 0.8629 0.062 Uiso 1 1 calc R . . C18 C 1.1007(3) 0.2116(4) 0.8714(3) 0.0526(15) Uani 1 1 d . . . N6 N 1.1208(3) 0.2173(4) 0.9478(3) 0.0670(15) Uani 1 1 d . . . O16 O 1.0884(3) 0.1959(5) 0.9802(3) 0.1007(17) Uani 1 1 d . . . C17 C 1.1397(3) 0.2250(4) 0.8343(4) 0.0577(17) Uani 1 1 d . . . H17 H 1.1788 0.2377 0.8578 0.069 Uiso 1 1 calc R . . C16 C 1.1213(3) 0.2197(4) 0.7632(3) 0.0570(16) Uani 1 1 d . . . H16 H 1.1484 0.2284 0.7387 0.068 Uiso 1 1 calc R . . C21 C 0.9613(2) 0.1627(3) 0.7357(3) 0.0424(13) Uani 1 1 d . . . H21 H 0.9412 0.1476 0.7672 0.051 Uiso 1 1 calc R . . C27 C 0.8293(2) 0.1615(3) 0.5942(3) 0.0482(14) Uani 1 1 d . . . C26 C 0.7737(2) 0.1240(4) 0.5801(3) 0.0568(16) Uani 1 1 d . . . H26 H 0.7439 0.1446 0.5419 0.068 Uiso 1 1 calc R . . C25 C 0.7606(3) 0.0591(4) 0.6189(4) 0.0661(18) Uani 1 1 d . . . H25 H 0.7226 0.0374 0.6075 0.079 Uiso 1 1 calc R . . C24 C 0.8038(3) 0.0262(4) 0.6750(4) 0.0658(18) Uani 1 1 d . . . H24 H 0.7955 -0.0190 0.7011 0.079 Uiso 1 1 calc R . . C23 C 0.8594(2) 0.0603(4) 0.6923(3) 0.0549(15) Uani 1 1 d . . . H23 H 0.8881 0.0378 0.7308 0.066 Uiso 1 1 calc R . . C28 C 0.8367(2) 0.2375(4) 0.5537(3) 0.0438(13) Uani 1 1 d . . . H28A H 0.8012 0.2451 0.5146 0.053 Uiso 1 1 calc R . . H28B H 0.8411 0.2880 0.5835 0.053 Uiso 1 1 calc R . . O10 O 0.95628(18) 0.3377(2) 0.6568(2) 0.0521(10) Uani 1 1 d . . . O17 O 1.1811(5) -0.0056(6) 0.2423(7) 0.243(7) Uani 1 1 d 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 0.0551(4) 0.0264(3) 0.0436(4) 0.0023(3) 0.0175(3) 0.0043(3) Ni2 0.0427(4) 0.0323(4) 0.0393(4) 0.0027(3) 0.0149(3) -0.0016(3) Ni3 0.0450(4) 0.0280(3) 0.0471(4) -0.0034(3) 0.0191(3) -0.0041(3) Ni4 0.0431(3) 0.0263(3) 0.0432(4) 0.0011(3) 0.0124(3) 0.0000(3) O4 0.0418(19) 0.035(2) 0.030(2) 0.0059(15) 0.0128(17) 0.0085(15) O6 0.0432(18) 0.0282(17) 0.0394(19) 0.0008(18) 0.0171(15) -0.0089(17) O5 0.055(2) 0.038(2) 0.075(3) -0.0190(19) 0.036(2) -0.0162(18) N3 0.055(3) 0.027(2) 0.053(3) -0.006(2) 0.023(2) -0.0078(19) O2 0.046(2) 0.0306(19) 0.036(2) 0.0077(16) 0.0101(17) 0.0035(16) O13 0.149(6) 0.042(3) 0.151(6) 0.035(3) 0.062(5) 0.041(3) O1 0.078(3) 0.036(2) 0.042(2) 0.0005(17) 0.022(2) 0.0114(19) O12 0.059(2) 0.041(2) 0.054(3) -0.0056(18) 0.021(2) -0.0035(17) O7 0.045(2) 0.0312(19) 0.045(2) 0.0048(16) 0.0033(17) 0.0032(16) N4 0.041(2) 0.029(2) 0.055(3) 0.015(2) 0.014(2) 0.0048(19) O19 0.102(4) 0.125(5) 0.066(4) 0.013(3) -0.019(3) -0.045(4) O3 0.0365(19) 0.056(2) 0.044(3) 0.0054(19) 0.0124(18) -0.0057(17) O15 0.087(4) 0.127(5) 0.075(4) -0.035(3) -0.013(3) -0.008(3) N2 0.044(2) 0.036(2) 0.039(3) 0.007(2) 0.009(2) 0.0016(19) O9 0.058(2) 0.041(2) 0.056(3) 0.0079(18) 0.003(2) 0.0047(17) C41 0.060(3) 0.030(3) 0.044(3) -0.005(2) 0.024(3) -0.008(2) O18 0.124(5) 0.094(4) 0.227(8) -0.025(5) 0.128(6) -0.020(4) N1 0.060(3) 0.025(2) 0.054(3) 0.004(2) 0.019(2) 0.007(2) C47 0.049(3) 0.043(3) 0.049(3) -0.003(3) 0.023(3) -0.008(2) O8 0.037(2) 0.0222(17) 0.050(2) -0.0010(15) 0.0132(18) 0.0030(13) C22 0.039(3) 0.047(3) 0.038(3) 0.009(2) 0.014(2) 0.003(2) C29 0.040(3) 0.039(3) 0.044(3) -0.003(2) 0.018(2) -0.005(2) C34 0.052(3) 0.034(3) 0.069(4) -0.009(3) 0.025(3) -0.002(2) C35 0.063(4) 0.042(3) 0.049(4) -0.003(3) 0.025(3) -0.016(3) C36 0.053(3) 0.034(3) 0.051(3) 0.001(2) 0.014(3) -0.013(2) C40 0.078(4) 0.030(3) 0.068(4) -0.004(3) 0.034(3) -0.005(3) C39 0.090(5) 0.031(3) 0.086(5) -0.012(3) 0.034(4) -0.016(3) C38 0.107(5) 0.035(3) 0.092(5) -0.001(3) 0.050(5) -0.019(3) C37 0.080(4) 0.040(3) 0.080(5) -0.008(3) 0.046(4) -0.020(3) C42 0.056(3) 0.040(3) 0.053(4) -0.009(3) 0.019(3) -0.006(3) C33 0.070(4) 0.038(4) 0.141(7) -0.009(4) 0.056(5) -0.014(3) C32 0.084(5) 0.066(5) 0.110(6) -0.035(4) 0.066(5) -0.012(4) N7 0.158(8) 0.097(6) 0.274(12) -0.093(7) 0.173(9) -0.061(5) C31 0.077(4) 0.047(4) 0.095(5) -0.023(3) 0.051(4) -0.009(3) C30 0.056(3) 0.051(4) 0.080(5) -0.032(3) 0.027(3) -0.023(3) O11 0.047(2) 0.045(2) 0.066(3) -0.0031(19) 0.0162(19) 0.0002(18) C14 0.065(4) 0.040(3) 0.049(4) -0.006(3) 0.019(3) 0.001(3) C13 0.067(4) 0.034(3) 0.051(4) 0.004(3) 0.027(3) 0.008(3) C8 0.063(3) 0.031(3) 0.042(3) 0.013(2) 0.014(3) 0.009(2) C7 0.074(4) 0.033(3) 0.069(4) 0.001(3) 0.034(4) -0.003(3) C6 0.065(4) 0.020(3) 0.063(4) -0.003(2) 0.013(3) 0.003(2) C5 0.078(4) 0.028(3) 0.082(5) -0.003(3) 0.035(4) 0.012(3) C4 0.075(4) 0.039(3) 0.087(5) 0.004(3) 0.031(4) 0.009(3) N5 0.077(4) 0.039(3) 0.149(7) -0.007(4) 0.046(5) 0.008(3) O14 0.148(6) 0.073(4) 0.189(7) -0.003(4) 0.102(6) 0.051(4) C3 0.090(5) 0.053(4) 0.102(6) -0.033(4) 0.046(5) 0.010(4) C2 0.094(5) 0.048(4) 0.066(4) -0.009(3) 0.028(4) 0.015(3) C1 0.065(4) 0.032(3) 0.058(4) -0.001(3) 0.030(3) 0.003(3) C9 0.069(4) 0.039(3) 0.075(4) 0.005(3) 0.030(3) 0.006(3) C10 0.087(5) 0.064(5) 0.076(5) 0.023(4) 0.035(4) -0.007(4) C11 0.096(5) 0.063(5) 0.064(5) 0.005(4) 0.036(4) -0.002(4) C12 0.096(5) 0.046(4) 0.046(4) -0.003(3) 0.029(4) -0.002(3) C43 0.040(3) 0.030(3) 0.044(3) 0.006(2) 0.017(2) 0.004(2) C44 0.048(3) 0.037(3) 0.044(3) 0.007(2) 0.009(3) 0.011(2) C45 0.043(3) 0.065(4) 0.045(3) 0.008(3) 0.009(3) 0.007(3) C46 0.035(3) 0.048(3) 0.047(3) 0.002(2) 0.011(2) -0.007(2) C48 0.036(3) 0.036(3) 0.047(3) 0.000(2) 0.014(2) -0.003(2) C49 0.043(3) 0.024(2) 0.059(4) 0.003(2) 0.020(3) -0.006(2) C50 0.047(3) 0.028(3) 0.054(3) 0.001(2) 0.009(3) 0.000(2) C55 0.052(3) 0.034(3) 0.041(3) 0.006(2) 0.005(3) -0.007(2) C54 0.062(4) 0.040(3) 0.080(5) 0.018(3) 0.002(3) -0.013(3) C53 0.097(6) 0.061(4) 0.075(5) 0.037(4) -0.009(4) -0.010(4) C52 0.074(4) 0.059(4) 0.063(4) 0.024(3) 0.009(4) -0.026(3) C51 0.058(3) 0.045(3) 0.050(4) 0.010(3) 0.014(3) -0.007(3) C56 0.044(3) 0.031(3) 0.065(4) -0.001(3) 0.018(3) 0.006(2) N8 0.058(3) 0.075(4) 0.054(3) 0.004(3) 0.008(3) -0.012(3) O20 0.094(4) 0.069(3) 0.091(4) -0.003(3) 0.001(3) -0.032(3) C15 0.048(3) 0.029(3) 0.058(4) 0.004(3) 0.017(3) -0.003(2) C20 0.051(3) 0.038(3) 0.037(3) 0.004(2) 0.007(3) -0.004(2) C19 0.052(3) 0.040(3) 0.062(4) 0.001(3) 0.015(3) 0.004(3) C18 0.059(4) 0.052(4) 0.042(3) 0.003(3) 0.008(3) -0.003(3) N6 0.068(4) 0.064(4) 0.065(4) -0.008(3) 0.014(3) 0.000(3) O16 0.092(4) 0.144(5) 0.060(3) 0.008(3) 0.013(3) -0.007(4) C17 0.043(3) 0.051(4) 0.073(5) 0.002(3) 0.009(3) -0.010(3) C16 0.042(3) 0.074(4) 0.053(4) 0.010(3) 0.012(3) -0.012(3) C21 0.051(3) 0.034(3) 0.051(4) 0.006(2) 0.029(3) 0.000(2) C27 0.040(3) 0.043(3) 0.059(4) 0.009(3) 0.010(3) -0.002(2) C26 0.042(3) 0.076(4) 0.050(4) 0.004(3) 0.010(3) 0.006(3) C25 0.052(4) 0.066(4) 0.078(5) 0.008(4) 0.016(3) -0.005(3) C24 0.060(4) 0.060(4) 0.082(5) 0.019(4) 0.028(4) -0.017(3) C23 0.045(3) 0.060(4) 0.063(4) 0.012(3) 0.022(3) -0.002(3) C28 0.033(3) 0.051(3) 0.051(4) 0.011(3) 0.018(3) 0.010(2) O10 0.062(2) 0.042(2) 0.054(2) -0.0017(18) 0.020(2) -0.0025(18) O17 0.262(11) 0.140(7) 0.446(18) -0.165(10) 0.286(13) -0.089(7) _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 O1 1.996(4) . ? Ni1 O2 2.008(4) . ? Ni1 N1 2.050(5) . ? Ni1 O6 2.096(4) . ? Ni1 O4 2.111(4) . ? Ni1 O9 2.167(4) . ? Ni2 O3 1.971(4) . ? Ni2 O4 2.011(4) . ? Ni2 N2 2.052(4) . ? Ni2 O6 2.099(3) . ? Ni2 O8 2.114(4) . ? Ni2 O10 2.178(4) . ? Ni3 O5 1.978(4) . ? Ni3 O6 1.992(4) . ? Ni3 N3 2.058(4) . ? Ni3 O8 2.070(4) . ? Ni3 O2 2.108(4) . ? Ni3 O11 2.161(4) . ? Ni4 O7 1.990(3) . ? Ni4 O8 2.006(3) . ? Ni4 N4 2.063(4) . ? Ni4 O4 2.075(4) . ? Ni4 O2 2.103(4) . ? Ni4 O12 2.189(4) . ? O4 C28 1.436(6) . ? O6 C42 1.416(6) . ? O5 C29 1.263(6) . ? N3 C35 1.292(7) . ? N3 C36 1.451(6) . ? O2 C14 1.402(7) . ? O13 N5 1.213(10) . ? O1 C1 1.267(7) . ? O7 C43 1.274(6) . ? N4 C49 1.277(7) . ? N4 C50 1.449(7) . ? O19 N8 1.206(7) . ? O3 C15 1.268(7) . ? O15 N6 1.206(8) . ? N2 C21 1.299(7) . ? N2 C22 1.396(7) . ? C41 C40 1.393(7) . ? C41 C36 1.405(8) . ? C41 C42 1.518(8) . ? O18 N7 1.191(8) . ? N1 C7 1.284(7) . ? N1 C8 1.454(7) . ? C47 C46 1.364(7) . ? C47 C48 1.395(7) . ? C47 H47 0.9300 . ? O8 C56 1.424(6) . ? C22 C23 1.395(8) . ? C22 C27 1.452(7) . ? C29 C30 1.423(8) . ? C29 C34 1.445(7) . ? C34 C33 1.385(9) . ? C34 C35 1.439(8) . ? C35 H35 0.9300 . ? C36 C37 1.389(8) . ? C40 C39 1.380(9) . ? C40 H40 0.9300 . ? C39 C38 1.366(10) . ? C39 H39 0.9300 . ? C38 C37 1.380(8) . ? C38 H38 0.9300 . ? C37 H37 0.9300 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C33 C32 1.357(9) . ? C33 H33 0.9300 . ? C32 C31 1.392(9) . ? C32 N7 1.452(9) . ? N7 O17 1.248(9) . ? C31 C30 1.303(8) . ? C31 H31 0.9300 . ? C30 H30 0.9300 . ? C14 C13 1.537(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C13 C12 1.338(8) . ? C13 C8 1.412(7) . ? C8 C9 1.364(8) . ? C7 C6 1.462(8) . ? C7 H7 0.9300 . ? C6 C5 1.383(7) . ? C6 C1 1.401(8) . ? C5 C4 1.355(9) . ? C5 H5 0.9300 . ? C4 C3 1.368(10) . ? C4 N5 1.457(9) . ? N5 O14 1.233(9) . ? C3 C2 1.398(9) . ? C3 H3 0.9300 . ? C2 C1 1.442(8) . ? C2 H2 0.9300 . ? C9 C10 1.421(9) . ? C9 H9A 0.9300 . ? C10 C11 1.283(10) . ? C10 H10 0.9300 . ? C11 C12 1.423(9) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C43 C48 1.421(7) . ? C43 C44 1.425(7) . ? C44 C45 1.352(8) . ? C44 H44 0.9300 . ? C45 C46 1.402(8) . ? C45 H45 0.9300 . ? C46 N8 1.464(8) . ? C48 C49 1.445(7) . ? C49 H49 0.9300 . ? C50 C51 1.379(7) . ? C50 C55 1.370(7) . ? C55 C54 1.411(8) . ? C55 C56 1.494(8) . ? C54 C53 1.398(9) . ? C54 H54 0.9300 . ? C53 C52 1.308(9) . ? C53 H53 0.9300 . ? C52 C51 1.402(8) . ? C52 H52 0.9300 . ? C51 H51 0.9300 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? N8 O20 1.198(7) . ? C15 C20 1.439(8) . ? C15 C16 1.432(8) . ? C20 C19 1.350(8) . ? C20 C21 1.450(7) . ? C19 C18 1.372(8) . ? C19 H19 0.9300 . ? C18 C17 1.369(9) . ? C18 N6 1.456(9) . ? N6 O16 1.194(8) . ? C17 C16 1.354(9) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? C21 H21 0.9300 . ? C27 C26 1.396(8) . ? C27 C28 1.470(7) . ? C26 C25 1.362(9) . ? C26 H26 0.9300 . ? C25 C24 1.371(9) . ? C25 H25 0.9300 . ? C24 C23 1.372(8) . ? C24 H24 0.9300 . ? C23 H23 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 171.53(15) . . ? O1 Ni1 N1 89.82(15) . . ? O2 Ni1 N1 93.76(17) . . ? O1 Ni1 O6 91.90(16) . . ? O2 Ni1 O6 79.74(14) . . ? N1 Ni1 O6 105.90(16) . . ? O1 Ni1 O4 94.07(15) . . ? O2 Ni1 O4 83.59(13) . . ? N1 Ni1 O4 170.45(17) . . ? O6 Ni1 O4 82.72(13) . . ? O1 Ni1 O9 96.00(16) . . ? O2 Ni1 O9 92.01(15) . . ? N1 Ni1 O9 83.97(17) . . ? O6 Ni1 O9 167.41(13) . . ? O4 Ni1 O9 86.95(14) . . ? O3 Ni2 O4 170.18(17) . . ? O3 Ni2 N2 91.17(16) . . ? O4 Ni2 N2 93.26(16) . . ? O3 Ni2 O6 92.05(15) . . ? O4 Ni2 O6 85.12(15) . . ? N2 Ni2 O6 169.62(16) . . ? O3 Ni2 O8 91.35(15) . . ? O4 Ni2 O8 78.93(14) . . ? N2 Ni2 O8 108.97(16) . . ? O6 Ni2 O8 80.82(14) . . ? O3 Ni2 O10 93.95(16) . . ? O4 Ni2 O10 95.19(15) . . ? N2 Ni2 O10 84.51(16) . . ? O6 Ni2 O10 85.42(14) . . ? O8 Ni2 O10 165.42(14) . . ? O5 Ni3 O6 168.52(16) . . ? O5 Ni3 N3 91.28(16) . . ? O6 Ni3 N3 96.07(15) . . ? O5 Ni3 O8 89.87(15) . . ? O6 Ni3 O8 84.46(14) . . ? N3 Ni3 O8 169.79(17) . . ? O5 Ni3 O2 89.49(16) . . ? O6 Ni3 O2 79.82(15) . . ? N3 Ni3 O2 108.71(16) . . ? O8 Ni3 O2 81.44(14) . . ? O5 Ni3 O11 95.90(16) . . ? O6 Ni3 O11 93.64(15) . . ? N3 Ni3 O11 83.97(17) . . ? O8 Ni3 O11 85.82(14) . . ? O2 Ni3 O11 166.16(15) . . ? O7 Ni4 O8 172.26(14) . . ? O7 Ni4 N4 91.73(15) . . ? O8 Ni4 N4 94.03(15) . . ? O7 Ni4 O4 93.38(14) . . ? O8 Ni4 O4 79.97(14) . . ? N4 Ni4 O4 107.34(17) . . ? O7 Ni4 O2 92.16(14) . . ? O8 Ni4 O2 83.06(14) . . ? N4 Ni4 O2 169.48(16) . . ? O4 Ni4 O2 82.18(14) . . ? O7 Ni4 O12 90.81(15) . . ? O8 Ni4 O12 94.92(15) . . ? N4 Ni4 O12 84.18(16) . . ? O4 Ni4 O12 167.60(14) . . ? O2 Ni4 O12 86.00(14) . . ? C28 O4 Ni2 115.6(3) . . ? C28 O4 Ni4 121.9(3) . . ? Ni2 O4 Ni4 101.02(15) . . ? C28 O4 Ni1 122.0(3) . . ? Ni2 O4 Ni1 96.03(15) . . ? Ni4 O4 Ni1 95.16(15) . . ? C42 O6 Ni3 115.9(3) . . ? C42 O6 Ni1 124.0(3) . . ? Ni3 O6 Ni1 100.60(17) . . ? C42 O6 Ni2 119.5(3) . . ? Ni3 O6 Ni2 97.88(13) . . ? Ni1 O6 Ni2 93.87(14) . . ? C29 O5 Ni3 128.1(3) . . ? C35 N3 C36 116.6(4) . . ? C35 N3 Ni3 120.0(3) . . ? C36 N3 Ni3 122.4(4) . . ? C14 O2 Ni1 115.5(3) . . ? C14 O2 Ni4 120.6(3) . . ? Ni1 O2 Ni4 97.45(17) . . ? C14 O2 Ni3 123.6(4) . . ? Ni1 O2 Ni3 99.69(16) . . ? Ni4 O2 Ni3 94.78(14) . . ? C1 O1 Ni1 124.8(4) . . ? C43 O7 Ni4 123.2(3) . . ? C49 N4 C50 118.0(4) . . ? C49 N4 Ni4 119.5(3) . . ? C50 N4 Ni4 122.1(3) . . ? C15 O3 Ni2 123.1(3) . . ? C21 N2 C22 115.6(5) . . ? C21 N2 Ni2 118.2(3) . . ? C22 N2 Ni2 125.3(4) . . ? C40 C41 C36 116.7(5) . . ? C40 C41 C42 115.3(5) . . ? C36 C41 C42 127.7(5) . . ? C7 N1 C8 114.4(5) . . ? C7 N1 Ni1 121.2(4) . . ? C8 N1 Ni1 123.1(3) . . ? C46 C47 C48 120.4(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C56 O8 Ni4 115.1(3) . . ? C56 O8 Ni3 120.5(3) . . ? Ni4 O8 Ni3 99.01(16) . . ? C56 O8 Ni2 122.7(4) . . ? Ni4 O8 Ni2 99.88(14) . . ? Ni3 O8 Ni2 95.05(13) . . ? N2 C22 C23 123.3(5) . . ? N2 C22 C27 118.6(4) . . ? C23 C22 C27 118.0(5) . . ? O5 C29 C30 120.3(5) . . ? O5 C29 C34 122.8(5) . . ? C30 C29 C34 116.9(5) . . ? C33 C34 C35 117.6(5) . . ? C33 C34 C29 117.9(5) . . ? C35 C34 C29 124.4(5) . . ? N3 C35 C34 127.6(5) . . ? N3 C35 H35 116.2 . . ? C34 C35 H35 116.2 . . ? C37 C36 C41 119.9(5) . . ? C37 C36 N3 120.3(5) . . ? C41 C36 N3 119.8(5) . . ? C39 C40 C41 123.0(6) . . ? C39 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C38 C39 C40 119.2(6) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C39 C38 C37 119.6(6) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C37 C36 121.4(6) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? O6 C42 C41 115.3(5) . . ? O6 C42 H42A 108.4 . . ? C41 C42 H42A 108.4 . . ? O6 C42 H42B 108.4 . . ? C41 C42 H42B 108.4 . . ? H42A C42 H42B 107.5 . . ? C32 C33 C34 121.1(6) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C33 C32 C31 121.6(6) . . ? C33 C32 N7 119.2(6) . . ? C31 C32 N7 119.2(6) . . ? O18 N7 O17 124.1(7) . . ? O18 N7 C32 120.5(7) . . ? O17 N7 C32 115.2(7) . . ? C30 C31 C32 119.1(6) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C31 C30 C29 123.4(5) . . ? C31 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? O2 C14 C13 113.6(5) . . ? O2 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? O2 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C12 C13 C8 117.7(5) . . ? C12 C13 C14 118.3(5) . . ? C8 C13 C14 123.7(5) . . ? C9 C8 C13 120.1(5) . . ? C9 C8 N1 120.1(5) . . ? C13 C8 N1 119.7(5) . . ? N1 C7 C6 124.0(6) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C5 C6 C1 118.1(6) . . ? C5 C6 C7 116.1(6) . . ? C1 C6 C7 125.7(5) . . ? C4 C5 C6 122.9(6) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C4 C3 120.5(6) . . ? C5 C4 N5 119.8(7) . . ? C3 C4 N5 119.7(7) . . ? O13 N5 O14 124.4(7) . . ? O13 N5 C4 118.9(7) . . ? O14 N5 C4 116.7(8) . . ? C4 C3 C2 120.1(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C2 C1 118.8(7) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? O1 C1 C6 123.9(5) . . ? O1 C1 C2 117.1(5) . . ? C6 C1 C2 119.0(5) . . ? C8 C9 C10 118.7(6) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 120.7 . . ? C11 C10 C9 122.4(6) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 118.2(7) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C13 C12 C11 122.7(6) . . ? C13 C12 H12A 118.6 . . ? C11 C12 H12A 118.6 . . ? O7 C43 C48 124.1(5) . . ? O7 C43 C44 118.4(4) . . ? C48 C43 C44 117.5(5) . . ? C45 C44 C43 121.6(5) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 119.7(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 120.9(5) . . ? C47 C46 N8 118.6(5) . . ? C45 C46 N8 120.4(5) . . ? C47 C48 C43 119.8(5) . . ? C47 C48 C49 116.0(5) . . ? C43 C48 C49 124.2(4) . . ? N4 C49 C48 128.2(5) . . ? N4 C49 H49 115.9 . . ? C48 C49 H49 115.9 . . ? C51 C50 C55 121.2(5) . . ? C51 C50 N4 118.7(5) . . ? C55 C50 N4 120.2(5) . . ? C50 C55 C54 117.7(5) . . ? C50 C55 C56 126.1(5) . . ? C54 C55 C56 116.2(5) . . ? C53 C54 C55 119.8(6) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C52 C53 C54 121.4(6) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C53 C52 C51 120.1(6) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C50 C51 C52 119.7(5) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? O8 C56 C55 114.9(4) . . ? O8 C56 H56A 108.5 . . ? C55 C56 H56A 108.6 . . ? O8 C56 H56B 108.5 . . ? C55 C56 H56B 108.5 . . ? H56A C56 H56B 107.5 . . ? O20 N8 O19 123.5(6) . . ? O20 N8 C46 119.2(5) . . ? O19 N8 C46 117.3(6) . . ? O3 C15 C20 124.1(5) . . ? O3 C15 C16 120.1(5) . . ? C20 C15 C16 115.8(5) . . ? C19 C20 C15 119.5(5) . . ? C19 C20 C21 117.4(5) . . ? C15 C20 C21 123.0(5) . . ? C20 C19 C18 122.4(6) . . ? C20 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? C17 C18 C19 120.2(6) . . ? C17 C18 N6 119.5(6) . . ? C19 C18 N6 120.3(6) . . ? O16 N6 O15 122.0(7) . . ? O16 N6 C18 119.1(6) . . ? O15 N6 C18 118.8(7) . . ? C16 C17 C18 119.8(6) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C16 C15 122.2(6) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? N2 C21 C20 127.5(5) . . ? N2 C21 H21 116.2 . . ? C20 C21 H21 116.2 . . ? C26 C27 C22 116.1(5) . . ? C26 C27 C28 119.1(5) . . ? C22 C27 C28 124.4(5) . . ? C25 C26 C27 124.0(6) . . ? C25 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C24 C23 119.6(6) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C23 C22 122.7(6) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? O4 C28 C27 114.6(4) . . ? O4 C28 H28A 108.6 . . ? C27 C28 H28A 108.6 . . ? O4 C28 H28B 108.6 . . ? C27 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.17 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.626 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.060 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.098 0.250 0.035 939.5 229.0 2 0.185 -0.250 0.623 939.5 229.0 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 900849' ####################################################################### # # 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_sk_sk_100m_b_b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H54 N8 Ni4 O20, 4(C2 H3 N)' _chemical_formula_sum 'C67 H66 N12 Ni4 O20' _chemical_formula_weight 1594.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.4300(19) _cell_length_b 15.9077(11) _cell_length_c 35.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.4970(10) _cell_angle_gamma 90.00 _cell_volume 13887.1(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.78 _exptl_crystal_description block _exptl_crystal_colour green-brown _exptl_crystal_size_max 0.453 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.176 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6592 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details 'SADABS; BRUKER, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53896 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.00 _reflns_number_total 15133 _reflns_number_gt 12952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+153.5005P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15133 _refine_ls_number_parameters 921 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.815 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.22851(3) 0.32682(5) 0.84721(2) 0.01271(18) Uani 1 1 d . . . Ni2 Ni 0.33257(3) 0.32723(5) 0.92121(2) 0.01306(18) Uani 1 1 d . . . Ni3 Ni 0.33125(3) 0.40862(5) 0.83908(2) 0.01286(18) Uani 1 1 d . . . Ni4 Ni 0.27339(3) 0.49587(5) 0.89209(2) 0.01315(18) Uani 1 1 d . . . N3 N 0.4047(2) 0.2661(3) 0.93380(16) 0.0153(11) Uani 1 1 d . . . N7 N 0.2078(2) 0.5507(3) 0.89958(16) 0.0161(11) Uani 1 1 d . . . O3 O 0.0363(2) -0.0551(3) 0.80521(17) 0.0288(12) Uani 1 1 d . . . N13 N 0.1489(2) 0.3557(3) 0.82324(16) 0.0152(11) Uani 1 1 d . . . O13 O 0.29281(18) 0.6028(3) 0.87072(14) 0.0181(9) Uani 1 1 d . . . O19 O 0.33627(19) 0.5365(3) 0.81928(15) 0.0186(10) Uani 1 1 d . . . O17 O 0.2223(2) 0.2725(3) 0.78939(15) 0.0206(10) Uani 1 1 d D . . O5 O 0.35027(19) 0.3700(3) 0.97749(14) 0.0197(10) Uani 1 1 d . . . O18 O 0.2999(2) 0.2121(3) 0.93361(15) 0.0189(10) Uani 1 1 d . . . O1 O 0.21200(18) 0.2184(3) 0.86935(14) 0.0175(9) Uani 1 1 d . . . O20 O 0.3137(2) 0.5261(3) 0.95704(15) 0.0203(10) Uani 1 1 d . . . N5 N 0.4105(2) 0.3949(3) 0.84384(16) 0.0144(10) Uani 1 1 d . . . O11 O 0.46232(19) 0.2669(3) 0.69301(15) 0.0230(10) Uani 1 1 d . . . C58 C 0.3815(3) 0.5800(5) 0.8141(3) 0.0302(17) Uani 1 1 d . . . H58A H 0.4116 0.5766 0.8388 0.045 Uiso 1 1 calc R . . H58B H 0.3724 0.6379 0.8077 0.045 Uiso 1 1 calc R . . H58C H 0.3907 0.5544 0.7925 0.045 Uiso 1 1 calc R . . C22 C 0.4223(3) 0.2289(4) 0.9028(2) 0.0171(13) Uani 1 1 d . . . N12 N 0.1836(4) 0.5119(6) 0.1784(3) 0.067(3) Uani 1 1 d . . . C67 C 0.2252(4) 0.4860(5) 0.1947(3) 0.040(2) Uani 1 1 d . . . C66 C 0.2782(4) 0.4522(5) 0.2160(3) 0.0361(19) Uani 1 1 d . . . H66A H 0.2778 0.3924 0.2126 0.054 Uiso 1 1 calc R . . H66B H 0.2880 0.4654 0.2443 0.054 Uiso 1 1 calc R . . H66C H 0.3038 0.4767 0.2053 0.054 Uiso 1 1 calc R . . O7 O 0.5085(2) 0.2869(5) 1.14963(17) 0.0457(9) Uani 1 1 d . . . C59 C 0.2944(4) 0.5578(6) 0.9880(3) 0.0373(19) Uani 1 1 d . . . H59A H 0.2853 0.6161 0.9830 0.056 Uiso 1 1 calc R . . H59B H 0.3219 0.5518 1.0139 0.056 Uiso 1 1 calc R . . H59C H 0.2632 0.5267 0.9878 0.056 Uiso 1 1 calc R . . C52 C 0.0713(3) 0.4986(5) 0.9017(3) 0.0317(18) Uani 1 1 d . . . H52 H 0.0383 0.5251 0.8965 0.038 Uiso 1 1 calc R . . C57 C 0.2991(3) 0.1768(5) 0.9707(2) 0.0316(17) Uani 1 1 d . . . H57A H 0.3352 0.1660 0.9880 0.047 Uiso 1 1 calc R . . H57B H 0.2792 0.1251 0.9654 0.047 Uiso 1 1 calc R . . H57C H 0.2823 0.2155 0.9838 0.047 Uiso 1 1 calc R . . O4 O -0.0131(2) 0.0562(3) 0.78622(17) 0.0302(12) Uani 1 1 d . . . C33 C 0.4142(3) 0.3305(4) 0.7448(2) 0.0161(12) Uani 1 1 d . . . H33 H 0.4514 0.3338 0.7529 0.019 Uiso 1 1 calc R . . C56 C 0.2246(3) 0.3726(4) 0.9314(2) 0.0168(13) Uani 1 1 d . . . H56A H 0.2461 0.3932 0.9579 0.020 Uiso 1 1 calc R . . H56B H 0.2176 0.3135 0.9343 0.020 Uiso 1 1 calc R . . C48 C 0.2456(3) 0.6927(4) 0.9017(2) 0.0188(13) Uani 1 1 d . . . C10 C 0.0563(3) 0.5383(5) 0.7912(2) 0.0251(15) Uani 1 1 d . . . H10 H 0.0215 0.5524 0.7896 0.030 Uiso 1 1 calc R . . C18 C 0.4690(4) 0.2937(7) 1.0802(3) 0.0457(9) Uani 1 1 d . . . C24 C 0.4949(3) 0.1864(4) 0.8794(2) 0.0242(15) Uani 1 1 d . . . H24 H 0.5315 0.1815 0.8840 0.029 Uiso 1 1 calc R . . O15 O 0.2909(3) 0.9805(3) 0.91477(18) 0.0361(7) Uani 1 1 d . . . C8 C 0.1293(3) 0.4379(4) 0.80891(19) 0.0169(13) Uani 1 1 d . . . C14 C 0.2186(3) 0.4791(4) 0.7984(2) 0.0167(13) Uani 1 1 d . . . C41 C 0.4462(3) 0.4598(4) 0.9121(2) 0.0174(13) Uani 1 1 d . . . O12 O 0.3876(2) 0.2725(4) 0.64256(17) 0.0393(15) Uani 1 1 d . . . C1 C 0.1690(3) 0.1744(4) 0.8536(2) 0.0169(13) Uani 1 1 d . . . C31 C 0.3292(3) 0.2991(4) 0.6930(2) 0.0194(13) Uani 1 1 d . . . H31 H 0.3101 0.2823 0.6666 0.023 Uiso 1 1 calc R . . C55 C 0.1714(3) 0.4191(4) 0.9181(2) 0.0179(13) Uani 1 1 d . . . C34 C 0.3878(3) 0.3519(4) 0.77210(19) 0.0147(12) Uani 1 1 d . . . C9 C 0.0778(3) 0.4615(4) 0.8071(2) 0.0218(14) Uani 1 1 d . . . H9 H 0.0575 0.4248 0.8168 0.026 Uiso 1 1 calc R . . C13 C 0.1619(3) 0.4959(4) 0.79759(19) 0.0165(12) Uani 1 1 d . . . C2 C 0.1685(3) 0.0880(4) 0.8643(2) 0.0202(14) Uani 1 1 d . . . H2 H 0.1988 0.0649 0.8833 0.024 Uiso 1 1 calc R . . C11 C 0.0869(3) 0.5942(4) 0.7777(2) 0.0242(15) Uani 1 1 d . . . H11 H 0.0724 0.6451 0.7660 0.029 Uiso 1 1 calc R . . C3 C 0.1245(3) 0.0379(4) 0.8473(2) 0.0212(14) Uani 1 1 d . . . H3A H 0.1254 -0.0187 0.8541 0.025 Uiso 1 1 calc R . . C17 C 0.4277(4) 0.3445(7) 1.0830(3) 0.0457(9) Uani 1 1 d . . . H17 H 0.4272 0.3623 1.1082 0.055 Uiso 1 1 calc R . . N6 N 0.4137(2) 0.2800(4) 0.67884(18) 0.0218(12) Uani 1 1 d . . . C39 C 0.5423(3) 0.4564(5) 0.9493(2) 0.0241(15) Uani 1 1 d . . . H39 H 0.5710 0.4708 0.9722 0.029 Uiso 1 1 calc R . . C38 C 0.5508(3) 0.4111(4) 0.9181(2) 0.0222(14) Uani 1 1 d . . . H38 H 0.5852 0.3943 0.9200 0.027 Uiso 1 1 calc R . . C7 C 0.1135(3) 0.2961(4) 0.8131(2) 0.0182(13) Uani 1 1 d . . . H7 H 0.0795 0.3111 0.7960 0.022 Uiso 1 1 calc R . . N4 N 0.5116(3) 0.2674(6) 1.1168(2) 0.0457(9) Uani 1 1 d . . . C51 C 0.1137(3) 0.5416(4) 0.8963(2) 0.0234(15) Uani 1 1 d . . . H51 H 0.1088 0.5965 0.8867 0.028 Uiso 1 1 calc R . . C30 C 0.3027(3) 0.3189(4) 0.7194(2) 0.0189(13) Uani 1 1 d . . . H30 H 0.2655 0.3145 0.7108 0.023 Uiso 1 1 calc R . . C45 C 0.3060(4) 0.8266(5) 0.8861(3) 0.0361(7) Uani 1 1 d . . . H45 H 0.3252 0.8714 0.8808 0.043 Uiso 1 1 calc R . . C16 C 0.3880(3) 0.3682(4) 1.0487(2) 0.0208(14) Uani 1 1 d . . . H16 H 0.3603 0.4019 1.0508 0.025 Uiso 1 1 calc R . . C23 C 0.4769(3) 0.2194(4) 0.9090(2) 0.0211(14) Uani 1 1 d . . . H23 H 0.5018 0.2356 0.9336 0.025 Uiso 1 1 calc R . . N14 N 0.0307(2) 0.0217(4) 0.80256(19) 0.0225(12) Uani 1 1 d . . . C53 C 0.0778(3) 0.4159(5) 0.9147(3) 0.0305(17) Uani 1 1 d . . . H53 H 0.0493 0.3868 0.9185 0.037 Uiso 1 1 calc R . . C32 C 0.3853(3) 0.3045(4) 0.7061(2) 0.0177(13) Uani 1 1 d . . . C42 C 0.3934(3) 0.4941(4) 0.9134(2) 0.0168(13) Uani 1 1 d . . . C4 C 0.0781(3) 0.0730(4) 0.8197(2) 0.0196(14) Uani 1 1 d . . . C29 C 0.3306(3) 0.3457(4) 0.75956(19) 0.0150(12) Uani 1 1 d . . . C44 C 0.3128(3) 0.7468(4) 0.8739(2) 0.0217(14) Uani 1 1 d . . . H44 H 0.3368 0.7381 0.8599 0.026 Uiso 1 1 calc R . . C20 C 0.4296(3) 0.2875(4) 1.0074(2) 0.0180(13) Uani 1 1 d . . . O8 O 0.5490(2) 0.2251(5) 1.11354(17) 0.0457(9) Uani 1 1 d . . . C47 C 0.2394(4) 0.7746(5) 0.9142(3) 0.0361(7) Uani 1 1 d . . . H47 H 0.2150 0.7855 0.9275 0.043 Uiso 1 1 calc R . . C21 C 0.4350(3) 0.2527(4) 0.9709(2) 0.0183(13) Uani 1 1 d . . . H21 H 0.4637 0.2162 0.9745 0.022 Uiso 1 1 calc R . . C35 C 0.4231(3) 0.3779(4) 0.8120(2) 0.0154(12) Uani 1 1 d . . . C28 C 0.3243(3) 0.2153(4) 0.8541(2) 0.0163(13) Uani 1 1 d . . . C15 C 0.3877(3) 0.3428(4) 1.0095(2) 0.0171(13) Uani 1 1 d . . . C49 C 0.2088(3) 0.6304(4) 0.9078(2) 0.0185(13) Uani 1 1 d . . . H49 H 0.1833 0.6496 0.9187 0.022 Uiso 1 1 calc R . . C27 C 0.3846(3) 0.2053(4) 0.8652(2) 0.0166(13) Uani 1 1 d . . . C5 C 0.0758(3) 0.1568(4) 0.8090(2) 0.0200(14) Uani 1 1 d . . . H5 H 0.0443 0.1790 0.7909 0.024 Uiso 1 1 calc R . . C12 C 0.1392(3) 0.5732(4) 0.7819(2) 0.0212(14) Uani 1 1 d . . . H12 H 0.1601 0.6120 0.7739 0.025 Uiso 1 1 calc R . . N8 N 0.2614(3) 0.9238(4) 0.9188(2) 0.0361(7) Uani 1 1 d . . . C40 C 0.4909(3) 0.4794(4) 0.9459(2) 0.0209(14) Uani 1 1 d . . . H40 H 0.4856 0.5094 0.9670 0.025 Uiso 1 1 calc R . . O16 O 0.2243(3) 0.9369(3) 0.93192(18) 0.0361(7) Uani 1 1 d . . . C37 C 0.5077(3) 0.3913(4) 0.8843(2) 0.0186(13) Uani 1 1 d . . . C43 C 0.2845(3) 0.6773(4) 0.8819(2) 0.0179(13) Uani 1 1 d . . . C50 C 0.1644(3) 0.5036(4) 0.9050(2) 0.0176(13) Uani 1 1 d . . . C19 C 0.4700(3) 0.2646(5) 1.0435(2) 0.0220(14) Uani 1 1 d . . . H19 H 0.4977 0.2295 1.0426 0.026 Uiso 1 1 calc R . . C26 C 0.4020(3) 0.1714(4) 0.8358(2) 0.0228(14) Uani 1 1 d . . . H18A H 0.3772 0.1555 0.8111 0.027 Uiso 1 1 calc RD . . C6 C 0.1209(3) 0.2086(4) 0.8254(2) 0.0178(13) Uani 1 1 d . . . C46 C 0.2696(4) 0.8391(5) 0.9066(3) 0.0361(7) Uani 1 1 d . . . C36 C 0.4548(3) 0.4160(4) 0.87990(19) 0.0158(12) Uani 1 1 d . . . C54 C 0.1272(3) 0.3768(5) 0.9222(2) 0.0239(15) Uani 1 1 d . . . H54 H 0.1309 0.3207 0.9302 0.029 Uiso 1 1 calc R . . C25 C 0.4580(3) 0.1605(4) 0.8429(2) 0.0251(15) Uani 1 1 d . . . H25 H 0.4697 0.1362 0.8232 0.030 Uiso 1 1 calc R . . O2 O 0.25223(17) 0.4410(3) 0.83466(13) 0.0132(8) Uani 1 1 d . . . O10 O 0.34741(17) 0.4424(3) 0.89701(13) 0.0138(9) Uani 1 1 d . . . O14 O 0.25511(17) 0.3798(3) 0.90514(13) 0.0136(9) Uani 1 1 d . . . O6 O 0.30935(17) 0.2974(3) 0.86251(13) 0.0141(9) Uani 1 1 d . . . O9 O 0.30363(17) 0.3636(3) 0.78337(13) 0.0163(9) Uani 1 1 d . . . C60 C 0.3949(4) 0.7103(6) 0.9786(3) 0.039(2) Uani 1 1 d . . . H60A H 0.3728 0.6641 0.9650 0.059 Uiso 1 1 calc R . . H60B H 0.4302 0.6902 0.9936 0.059 Uiso 1 1 calc R . . H60C H 0.3972 0.7509 0.9590 0.059 Uiso 1 1 calc R . . C61 C 0.3713(5) 0.7492(7) 1.0061(4) 0.055(3) Uani 1 1 d . . . C62 C 0.4422(5) 0.9514(8) 0.9623(5) 0.084(2) Uani 1 1 d . . . C63 C 0.4203(5) 1.0201(8) 0.9321(5) 0.084(2) Uani 1 1 d . . . H63A H 0.4488 1.0574 0.9322 0.127 Uiso 1 1 calc R . . H63B H 0.3934 1.0507 0.9392 0.127 Uiso 1 1 calc R . . H63C H 0.4046 0.9961 0.9056 0.127 Uiso 1 1 calc R . . N9 N 0.4604(4) 0.8973(6) 0.9829(4) 0.084(2) Uani 1 1 d . . . N10 N 0.3517(6) 0.7791(9) 1.0274(4) 0.108(5) Uani 1 1 d . . . C64 C 0.5653(5) 0.0740(8) 0.1860(4) 0.065(3) Uani 1 1 d . . . H64A H 0.5697 0.0604 0.1606 0.098 Uiso 1 1 calc R . . H64B H 0.5292 0.0926 0.1814 0.098 Uiso 1 1 calc R . . H64C H 0.5726 0.0251 0.2030 0.098 Uiso 1 1 calc R . . C65 C 0.6019(6) 0.1393(9) 0.2053(4) 0.076(4) Uani 1 1 d . . . N11 N 0.6332(5) 0.1897(8) 0.2220(4) 0.086(4) Uani 1 1 d . . . H20 H 0.325(3) 0.486(5) 0.964(3) 0.02(2) Uiso 1 1 d . . . H42A H 0.400(3) 0.508(4) 0.942(2) 0.008(16) Uiso 1 1 d . . . H42B H 0.386(3) 0.549(5) 0.899(2) 0.020(19) Uiso 1 1 d . . . H14A H 0.217(3) 0.444(5) 0.775(2) 0.013(17) Uiso 1 1 d . . . H14B H 0.234(3) 0.533(5) 0.795(2) 0.02(2) Uiso 1 1 d . . . H19A H 0.322(3) 0.561(5) 0.832(2) 0.014(19) Uiso 1 1 d . . . H28A H 0.312(3) 0.179(5) 0.869(2) 0.015(18) Uiso 1 1 d . . . H28B H 0.308(3) 0.204(5) 0.824(2) 0.017(19) Uiso 1 1 d . . . H18B H 0.271(4) 0.204(5) 0.917(3) 0.02(2) Uiso 1 1 d . . . H37 H 0.517(3) 0.359(5) 0.864(2) 0.018(19) Uiso 1 1 d . . . H35 H 0.458(3) 0.382(5) 0.811(2) 0.015(18) Uiso 1 1 d . . . H17A H 0.243(4) 0.303(6) 0.783(3) 0.07(4) Uiso 1 1 d D . . H17B H 0.196(2) 0.277(6) 0.7690(17) 0.03(3) Uiso 1 1 d 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 0.0114(4) 0.0129(4) 0.0138(4) 0.0003(3) 0.0042(3) 0.0004(3) Ni2 0.0133(4) 0.0136(4) 0.0123(4) 0.0003(3) 0.0044(3) 0.0026(3) Ni3 0.0116(4) 0.0152(4) 0.0121(4) -0.0010(3) 0.0045(3) -0.0003(3) Ni4 0.0134(4) 0.0120(4) 0.0145(4) 0.0000(3) 0.0052(3) 0.0016(3) N3 0.015(3) 0.014(3) 0.018(3) 0.000(2) 0.006(2) 0.002(2) N7 0.014(3) 0.017(3) 0.017(3) 0.002(2) 0.005(2) 0.003(2) O3 0.030(3) 0.020(3) 0.041(3) -0.005(2) 0.018(3) -0.009(2) N13 0.013(3) 0.016(3) 0.017(3) 0.001(2) 0.006(2) 0.000(2) O13 0.018(2) 0.014(2) 0.023(2) 0.0008(18) 0.009(2) 0.0014(17) O19 0.017(2) 0.019(2) 0.023(3) 0.0019(19) 0.011(2) -0.0010(18) O17 0.017(2) 0.025(3) 0.018(2) -0.005(2) 0.003(2) -0.005(2) O5 0.024(2) 0.021(2) 0.014(2) 0.0010(18) 0.0053(19) 0.0071(19) O18 0.019(3) 0.020(2) 0.017(2) 0.0046(18) 0.005(2) 0.0007(19) O1 0.015(2) 0.015(2) 0.021(2) 0.0013(17) 0.0045(19) -0.0012(17) O20 0.023(3) 0.018(3) 0.020(3) -0.003(2) 0.008(2) 0.004(2) N5 0.012(2) 0.015(3) 0.015(3) -0.001(2) 0.003(2) -0.0001(19) O11 0.018(2) 0.025(3) 0.030(3) -0.004(2) 0.014(2) -0.0005(19) C58 0.024(4) 0.026(4) 0.046(5) 0.004(3) 0.018(4) -0.003(3) C22 0.021(3) 0.013(3) 0.019(3) 0.004(2) 0.010(3) 0.005(2) N12 0.054(6) 0.060(6) 0.081(7) 0.027(5) 0.012(5) 0.005(5) C67 0.052(6) 0.030(4) 0.041(5) 0.002(4) 0.020(4) -0.007(4) C66 0.044(5) 0.035(4) 0.034(5) -0.008(3) 0.019(4) -0.003(4) O7 0.0312(17) 0.081(3) 0.0194(14) 0.0005(15) 0.0007(13) 0.0154(16) C59 0.043(5) 0.039(5) 0.030(4) -0.001(3) 0.011(4) 0.006(4) C52 0.020(4) 0.032(4) 0.047(5) 0.008(4) 0.017(3) 0.010(3) C57 0.041(5) 0.031(4) 0.023(4) 0.008(3) 0.010(3) -0.005(3) O4 0.019(3) 0.032(3) 0.041(3) -0.005(2) 0.012(2) -0.006(2) C33 0.012(3) 0.016(3) 0.020(3) -0.001(2) 0.005(2) 0.000(2) C56 0.020(3) 0.014(3) 0.019(3) 0.003(2) 0.010(3) 0.003(2) C48 0.021(3) 0.016(3) 0.017(3) 0.001(2) 0.003(3) 0.004(2) C10 0.015(3) 0.025(4) 0.031(4) -0.003(3) 0.002(3) 0.008(3) C18 0.0312(17) 0.081(3) 0.0194(14) 0.0005(15) 0.0007(13) 0.0154(16) C24 0.021(4) 0.022(3) 0.034(4) 0.006(3) 0.016(3) 0.007(3) O15 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C8 0.016(3) 0.017(3) 0.016(3) 0.001(2) 0.003(2) 0.004(2) C14 0.017(3) 0.018(3) 0.015(3) 0.003(2) 0.005(3) 0.001(2) C41 0.016(3) 0.018(3) 0.018(3) 0.002(2) 0.004(3) 0.000(2) O12 0.028(3) 0.070(4) 0.021(3) -0.016(3) 0.009(2) -0.006(3) C1 0.019(3) 0.017(3) 0.017(3) -0.003(2) 0.010(3) -0.001(2) C31 0.019(3) 0.025(3) 0.013(3) -0.005(2) 0.004(3) -0.003(3) C55 0.018(3) 0.020(3) 0.017(3) 0.000(2) 0.008(3) 0.003(3) C34 0.016(3) 0.014(3) 0.016(3) 0.000(2) 0.006(2) 0.000(2) C9 0.015(3) 0.024(3) 0.027(4) 0.002(3) 0.007(3) 0.002(3) C13 0.015(3) 0.017(3) 0.014(3) 0.000(2) 0.001(2) 0.001(2) C2 0.020(3) 0.018(3) 0.023(3) 0.001(3) 0.008(3) 0.001(3) C11 0.026(4) 0.016(3) 0.025(4) 0.000(3) 0.002(3) 0.006(3) C3 0.023(4) 0.016(3) 0.029(4) 0.001(3) 0.014(3) -0.003(3) C17 0.0312(17) 0.081(3) 0.0194(14) 0.0005(15) 0.0007(13) 0.0154(16) N6 0.025(3) 0.024(3) 0.020(3) -0.007(2) 0.011(3) -0.006(2) C39 0.017(3) 0.031(4) 0.020(3) 0.000(3) 0.001(3) -0.003(3) C38 0.015(3) 0.027(4) 0.022(3) 0.004(3) 0.003(3) 0.002(3) C7 0.014(3) 0.020(3) 0.021(3) 0.003(3) 0.006(3) 0.001(2) N4 0.0312(17) 0.081(3) 0.0194(14) 0.0005(15) 0.0007(13) 0.0154(16) C51 0.021(3) 0.020(3) 0.031(4) 0.004(3) 0.011(3) 0.006(3) C30 0.013(3) 0.023(3) 0.019(3) -0.003(3) 0.003(3) -0.001(2) C45 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C16 0.022(3) 0.023(3) 0.018(3) -0.002(3) 0.007(3) 0.001(3) C23 0.021(3) 0.019(3) 0.023(4) 0.005(3) 0.008(3) 0.004(3) N14 0.022(3) 0.022(3) 0.029(3) -0.004(2) 0.015(3) -0.007(2) C53 0.020(4) 0.032(4) 0.044(5) 0.010(3) 0.018(3) 0.001(3) C32 0.021(3) 0.017(3) 0.016(3) -0.003(2) 0.009(3) -0.001(2) C42 0.015(3) 0.018(3) 0.017(3) -0.005(2) 0.005(3) 0.000(2) C4 0.017(3) 0.021(3) 0.025(4) -0.005(3) 0.012(3) -0.008(3) C29 0.015(3) 0.014(3) 0.015(3) 0.001(2) 0.005(2) 0.002(2) C44 0.018(3) 0.022(3) 0.025(4) 0.001(3) 0.007(3) -0.001(3) C20 0.016(3) 0.020(3) 0.018(3) 0.002(2) 0.005(3) -0.001(2) O8 0.0312(17) 0.081(3) 0.0194(14) 0.0005(15) 0.0007(13) 0.0154(16) C47 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C21 0.017(3) 0.017(3) 0.020(3) 0.003(2) 0.005(3) 0.004(2) C35 0.013(3) 0.017(3) 0.017(3) 0.000(2) 0.006(3) -0.002(2) C28 0.018(3) 0.013(3) 0.018(3) -0.002(2) 0.007(3) 0.003(2) C15 0.019(3) 0.015(3) 0.016(3) 0.002(2) 0.004(3) -0.003(2) C49 0.021(3) 0.018(3) 0.017(3) 0.002(2) 0.007(3) 0.007(3) C27 0.018(3) 0.012(3) 0.021(3) 0.002(2) 0.008(3) 0.002(2) C5 0.017(3) 0.022(3) 0.022(3) 0.001(3) 0.008(3) -0.002(3) C12 0.022(3) 0.018(3) 0.021(3) 0.002(3) 0.003(3) -0.001(3) N8 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C40 0.021(3) 0.025(3) 0.015(3) -0.002(3) 0.004(3) -0.001(3) O16 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C37 0.017(3) 0.021(3) 0.018(3) 0.002(3) 0.006(3) 0.003(3) C43 0.016(3) 0.018(3) 0.018(3) 0.001(2) 0.004(3) 0.004(2) C50 0.016(3) 0.021(3) 0.018(3) 0.000(2) 0.009(3) 0.003(3) C19 0.016(3) 0.027(4) 0.021(3) 0.002(3) 0.003(3) 0.002(3) C26 0.029(4) 0.019(3) 0.023(4) -0.001(3) 0.012(3) 0.001(3) C6 0.016(3) 0.017(3) 0.021(3) 0.002(2) 0.007(3) -0.001(2) C46 0.0502(19) 0.0201(13) 0.0416(17) -0.0017(12) 0.0201(14) 0.0017(12) C36 0.017(3) 0.015(3) 0.014(3) 0.002(2) 0.004(2) -0.002(2) C54 0.026(4) 0.022(3) 0.027(4) 0.006(3) 0.012(3) 0.005(3) C25 0.030(4) 0.020(3) 0.033(4) 0.000(3) 0.021(3) 0.006(3) O2 0.011(2) 0.016(2) 0.013(2) 0.0022(16) 0.0039(17) 0.0012(16) O10 0.013(2) 0.015(2) 0.012(2) -0.0015(16) 0.0032(17) 0.0004(17) O14 0.015(2) 0.014(2) 0.014(2) 0.0011(16) 0.0072(18) 0.0018(16) O6 0.015(2) 0.012(2) 0.017(2) -0.0013(16) 0.0066(18) 0.0015(16) O9 0.011(2) 0.024(2) 0.015(2) -0.0032(18) 0.0054(18) -0.0012(17) C60 0.037(5) 0.044(5) 0.032(5) 0.002(4) 0.004(4) -0.005(4) C61 0.058(7) 0.051(6) 0.058(7) -0.013(5) 0.022(5) -0.011(5) C62 0.059(4) 0.044(4) 0.134(7) 0.014(4) 0.011(4) 0.001(3) C63 0.059(4) 0.044(4) 0.134(7) 0.014(4) 0.011(4) 0.001(3) N9 0.059(4) 0.044(4) 0.134(7) 0.014(4) 0.011(4) 0.001(3) N10 0.135(12) 0.105(10) 0.121(11) -0.062(9) 0.091(10) -0.029(9) C64 0.045(6) 0.060(7) 0.080(9) 0.007(6) 0.007(6) -0.009(5) C65 0.077(9) 0.068(8) 0.067(8) 0.013(7) 0.001(7) -0.006(7) N11 0.090(9) 0.088(9) 0.064(7) 0.006(6) 0.003(6) -0.018(7) _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 O1 1.999(5) . ? Ni1 O2 2.018(4) . ? Ni1 N13 2.041(5) . ? Ni1 O6 2.075(4) . ? Ni1 O14 2.091(4) . ? Ni1 O17 2.158(5) . ? Ni2 O5 1.989(5) . ? Ni2 O6 1.997(4) . ? Ni2 N3 2.053(5) . ? Ni2 O14 2.106(4) . ? Ni2 O10 2.110(4) . ? Ni2 O18 2.131(5) . ? Ni3 O9 1.976(4) . ? Ni3 O10 2.003(4) . ? Ni3 N5 2.057(5) . ? Ni3 O2 2.106(4) . ? Ni3 O6 2.111(4) . ? Ni3 O19 2.168(5) . ? Ni4 O13 1.994(5) . ? Ni4 O14 2.000(4) . ? Ni4 N7 2.034(5) . ? Ni4 O10 2.087(4) . ? Ni4 O2 2.091(4) . ? Ni4 O20 2.220(5) . ? N3 C21 1.298(9) . ? N3 C22 1.444(8) . ? N7 C49 1.298(8) . ? N7 C50 1.436(8) . ? O3 N14 1.231(8) . ? N13 C7 1.295(8) . ? N13 C8 1.433(8) . ? O13 C43 1.289(8) . ? O19 C58 1.445(8) . ? O19 H19A 0.78(8) . ? O17 H17A 0.83(3) . ? O17 H17B 0.81(2) . ? O5 C15 1.299(8) . ? O18 C57 1.423(8) . ? O18 H18B 0.79(9) . ? O1 C1 1.290(8) . ? O20 C59 1.435(9) . ? O20 H20 0.71(9) . ? N5 C35 1.296(8) . ? N5 C36 1.447(8) . ? O11 N6 1.231(8) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C22 C23 1.395(9) . ? C22 C27 1.411(9) . ? N12 C67 1.134(13) . ? C67 C66 1.452(13) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? O7 N4 1.222(9) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C52 C51 1.381(10) . ? C52 C53 1.383(11) . ? C52 H52 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? O4 N14 1.235(8) . ? C33 C32 1.381(9) . ? C33 C34 1.399(9) . ? C33 H33 0.9300 . ? C56 O14 1.417(7) . ? C56 C55 1.519(9) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C48 C47 1.401(10) . ? C48 C43 1.442(9) . ? C48 C49 1.452(10) . ? C10 C9 1.384(10) . ? C10 C11 1.386(11) . ? C10 H10 0.9300 . ? C18 C19 1.378(11) . ? C18 C17 1.387(13) . ? C18 N4 1.456(11) . ? C24 C23 1.380(10) . ? C24 C25 1.387(11) . ? C24 H24 0.9300 . ? O15 N8 1.231(9) . ? C8 C9 1.393(9) . ? C8 C13 1.406(9) . ? C14 O2 1.419(7) . ? C14 C13 1.513(9) . ? C14 H14A 0.99(7) . ? C14 H14B 0.97(8) . ? C41 C40 1.401(9) . ? C41 C36 1.408(9) . ? C41 C42 1.514(9) . ? O12 N6 1.233(8) . ? C1 C2 1.427(9) . ? C1 C6 1.432(9) . ? C31 C30 1.370(9) . ? C31 C32 1.400(9) . ? C31 H31 0.9300 . ? C55 C54 1.397(10) . ? C55 C50 1.411(9) . ? C34 C29 1.431(9) . ? C34 C35 1.457(9) . ? C9 H9 0.9300 . ? C13 C12 1.399(9) . ? C2 C3 1.371(10) . ? C2 H2 0.9300 . ? C11 C12 1.382(10) . ? C11 H11 0.9300 . ? C3 C4 1.399(10) . ? C3 H3A 0.9300 . ? C17 C16 1.359(11) . ? C17 H17 0.9300 . ? N6 C32 1.451(8) . ? C39 C40 1.371(10) . ? C39 C38 1.389(10) . ? C39 H39 0.9300 . ? C38 C37 1.377(10) . ? C38 H38 0.9300 . ? C7 C6 1.451(9) . ? C7 H7 0.9300 . ? N4 O8 1.232(9) . ? C51 C50 1.407(9) . ? C51 H51 0.9300 . ? C30 C29 1.419(9) . ? C30 H30 0.9300 . ? C45 C44 1.370(10) . ? C45 C46 1.395(12) . ? C45 H45 0.9300 . ? C16 C15 1.427(9) . ? C16 H16 0.9300 . ? C23 H23 0.9300 . ? N14 C4 1.446(8) . ? C53 C54 1.389(10) . ? C53 H53 0.9300 . ? C42 O10 1.420(8) . ? C42 H42A 1.00(7) . ? C42 H42B 1.01(8) . ? C4 C5 1.382(9) . ? C29 O9 1.297(8) . ? C44 C43 1.414(9) . ? C44 H44 0.9300 . ? C20 C19 1.404(9) . ? C20 C15 1.435(9) . ? C20 C21 1.443(9) . ? C47 C46 1.379(12) . ? C47 H47 0.9300 . ? C21 H21 0.9300 . ? C35 H35 0.95(7) . ? C28 O6 1.423(7) . ? C28 C27 1.517(9) . ? C28 H28A 0.92(8) . ? C28 H28B 1.00(8) . ? C49 H49 0.9300 . ? C27 C26 1.371(9) . ? C5 C6 1.406(9) . ? C5 H5 0.9300 . ? C12 H12 0.9300 . ? N8 O16 1.231(9) . ? N8 C46 1.452(10) . ? C40 H40 0.9300 . ? C37 C36 1.410(9) . ? C37 H37 0.97(8) . ? C19 H19 0.9300 . ? C26 C25 1.428(10) . ? C26 H18A 0.9300 . ? C54 H54 0.9300 . ? C25 H25 0.9300 . ? C60 C61 1.450(14) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 N10 1.144(14) . ? C62 N9 1.124(16) . ? C62 C63 1.496(18) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.426(17) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 N11 1.160(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 170.33(19) . . ? O1 Ni1 N13 91.5(2) . . ? O2 Ni1 N13 93.45(19) . . ? O1 Ni1 O6 92.55(18) . . ? O2 Ni1 O6 83.75(17) . . ? N13 Ni1 O6 171.2(2) . . ? O1 Ni1 O14 90.98(18) . . ? O2 Ni1 O14 79.66(17) . . ? N13 Ni1 O14 105.98(19) . . ? O6 Ni1 O14 81.74(17) . . ? O1 Ni1 O17 93.47(19) . . ? O2 Ni1 O17 95.05(18) . . ? N13 Ni1 O17 87.7(2) . . ? O6 Ni1 O17 84.33(18) . . ? O14 Ni1 O17 165.55(18) . . ? O5 Ni2 O6 172.79(18) . . ? O5 Ni2 N3 93.1(2) . . ? O6 Ni2 N3 93.04(19) . . ? O5 Ni2 O14 90.87(18) . . ? O6 Ni2 O14 83.21(17) . . ? N3 Ni2 O14 174.6(2) . . ? O5 Ni2 O10 95.02(18) . . ? O6 Ni2 O10 80.03(17) . . ? N3 Ni2 O10 102.34(19) . . ? O14 Ni2 O10 80.94(17) . . ? O5 Ni2 O18 94.0(2) . . ? O6 Ni2 O18 89.98(18) . . ? N3 Ni2 O18 87.7(2) . . ? O14 Ni2 O18 88.37(18) . . ? O10 Ni2 O18 166.12(18) . . ? O9 Ni3 O10 169.05(18) . . ? O9 Ni3 N5 94.15(19) . . ? O10 Ni3 N5 94.54(19) . . ? O9 Ni3 O2 89.18(17) . . ? O10 Ni3 O2 83.09(17) . . ? N5 Ni3 O2 171.89(19) . . ? O9 Ni3 O6 91.25(18) . . ? O10 Ni3 O6 79.89(17) . . ? N5 Ni3 O6 106.50(19) . . ? O2 Ni3 O6 80.78(17) . . ? O9 Ni3 O19 93.76(19) . . ? O10 Ni3 O19 93.27(19) . . ? N5 Ni3 O19 87.5(2) . . ? O2 Ni3 O19 84.94(17) . . ? O6 Ni3 O19 164.80(18) . . ? O13 Ni4 O14 170.35(18) . . ? O13 Ni4 N7 91.1(2) . . ? O14 Ni4 N7 94.9(2) . . ? O13 Ni4 O10 91.54(18) . . ? O14 Ni4 O10 84.06(17) . . ? N7 Ni4 O10 168.5(2) . . ? O13 Ni4 O2 90.82(18) . . ? O14 Ni4 O2 80.05(17) . . ? N7 Ni4 O2 109.7(2) . . ? O10 Ni4 O2 81.48(16) . . ? O13 Ni4 O20 96.0(2) . . ? O14 Ni4 O20 92.02(19) . . ? N7 Ni4 O20 85.0(2) . . ? O10 Ni4 O20 83.58(18) . . ? O2 Ni4 O20 163.71(18) . . ? C21 N3 C22 116.2(5) . . ? C21 N3 Ni2 120.8(4) . . ? C22 N3 Ni2 122.8(4) . . ? C49 N7 C50 116.1(6) . . ? C49 N7 Ni4 119.4(5) . . ? C50 N7 Ni4 123.1(4) . . ? C7 N13 C8 115.3(5) . . ? C7 N13 Ni1 119.9(5) . . ? C8 N13 Ni1 123.5(4) . . ? C43 O13 Ni4 125.4(4) . . ? C58 O19 Ni3 129.1(4) . . ? C58 O19 H19A 115(6) . . ? Ni3 O19 H19A 101(6) . . ? Ni1 O17 H17A 100(8) . . ? Ni1 O17 H17B 124(7) . . ? H17A O17 H17B 99(10) . . ? C15 O5 Ni2 127.1(4) . . ? C57 O18 Ni2 131.0(5) . . ? C57 O18 H18B 106(6) . . ? Ni2 O18 H18B 111(6) . . ? C1 O1 Ni1 125.2(4) . . ? C59 O20 Ni4 133.0(5) . . ? C59 O20 H20 106(7) . . ? Ni4 O20 H20 99(7) . . ? C35 N5 C36 115.8(5) . . ? C35 N5 Ni3 120.0(4) . . ? C36 N5 Ni3 123.5(4) . . ? O19 C58 H58A 109.5 . . ? O19 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O19 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C23 C22 C27 119.2(6) . . ? C23 C22 N3 120.2(6) . . ? C27 C22 N3 120.6(6) . . ? N12 C67 C66 179.1(11) . . ? C67 C66 H66A 109.5 . . ? C67 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C67 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O20 C59 H59A 109.5 . . ? O20 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O20 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C51 C52 C53 119.9(7) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? O18 C57 H57A 109.5 . . ? O18 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O18 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C32 C33 C34 120.4(6) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? O14 C56 C55 115.5(5) . . ? O14 C56 H56A 108.4 . . ? C55 C56 H56A 108.4 . . ? O14 C56 H56B 108.4 . . ? C55 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? C47 C48 C43 119.0(7) . . ? C47 C48 C49 115.8(7) . . ? C43 C48 C49 125.1(6) . . ? C9 C10 C11 119.7(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C19 C18 C17 121.5(8) . . ? C19 C18 N4 118.3(8) . . ? C17 C18 N4 120.1(8) . . ? C23 C24 C25 119.5(7) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C9 C8 C13 119.4(6) . . ? C9 C8 N13 119.6(6) . . ? C13 C8 N13 120.9(6) . . ? O2 C14 C13 114.4(5) . . ? O2 C14 H14A 110(4) . . ? C13 C14 H14A 108(4) . . ? O2 C14 H14B 109(5) . . ? C13 C14 H14B 107(5) . . ? H14A C14 H14B 107(6) . . ? C40 C41 C36 118.0(6) . . ? C40 C41 C42 114.9(6) . . ? C36 C41 C42 127.0(6) . . ? O1 C1 C2 119.6(6) . . ? O1 C1 C6 122.8(6) . . ? C2 C1 C6 117.6(6) . . ? C30 C31 C32 119.1(6) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C54 C55 C50 118.0(6) . . ? C54 C55 C56 117.0(6) . . ? C50 C55 C56 124.8(6) . . ? C33 C34 C29 119.3(6) . . ? C33 C34 C35 114.7(6) . . ? C29 C34 C35 126.0(6) . . ? C10 C9 C8 121.3(7) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C12 C13 C8 117.8(6) . . ? C12 C13 C14 117.1(6) . . ? C8 C13 C14 125.0(6) . . ? C3 C2 C1 121.8(7) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C16 C17 C18 119.5(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? O11 N6 O12 123.2(6) . . ? O11 N6 C32 118.7(6) . . ? O12 N6 C32 118.0(6) . . ? C40 C39 C38 118.9(6) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C37 C38 C39 119.5(6) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? N13 C7 C6 127.4(6) . . ? N13 C7 H7 116.3 . . ? C6 C7 H7 116.3 . . ? O7 N4 O8 122.3(7) . . ? O7 N4 C18 118.6(7) . . ? O8 N4 C18 119.1(7) . . ? C52 C51 C50 121.0(7) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C31 C30 C29 121.8(6) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C44 C45 C46 118.7(8) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? C17 C16 C15 121.8(7) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C24 C23 C22 121.5(7) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? O3 N14 O4 123.1(6) . . ? O3 N14 C4 117.5(6) . . ? O4 N14 C4 119.3(6) . . ? C52 C53 C54 119.6(7) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C33 C32 C31 121.2(6) . . ? C33 C32 N6 119.3(6) . . ? C31 C32 N6 119.4(6) . . ? O10 C42 C41 116.9(5) . . ? O10 C42 H42A 112(4) . . ? C41 C42 H42A 106(4) . . ? O10 C42 H42B 108(4) . . ? C41 C42 H42B 109(4) . . ? H42A C42 H42B 106(6) . . ? C5 C4 C3 121.5(6) . . ? C5 C4 N14 118.5(6) . . ? C3 C4 N14 120.0(6) . . ? O9 C29 C30 119.4(6) . . ? O9 C29 C34 122.6(6) . . ? C30 C29 C34 118.0(6) . . ? C45 C44 C43 121.9(7) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C19 C20 C15 118.7(6) . . ? C19 C20 C21 115.3(6) . . ? C15 C20 C21 126.0(6) . . ? C46 C47 C48 119.7(8) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? N3 C21 C20 127.8(6) . . ? N3 C21 H21 116.1 . . ? C20 C21 H21 116.1 . . ? N5 C35 C34 128.2(6) . . ? N5 C35 H35 125(5) . . ? C34 C35 H35 107(4) . . ? O6 C28 C27 112.6(5) . . ? O6 C28 H28A 107(5) . . ? C27 C28 H28A 109(5) . . ? O6 C28 H28B 109(4) . . ? C27 C28 H28B 108(4) . . ? H28A C28 H28B 112(6) . . ? O5 C15 C16 119.6(6) . . ? O5 C15 C20 122.5(6) . . ? C16 C15 C20 117.8(6) . . ? N7 C49 C48 126.9(6) . . ? N7 C49 H49 116.6 . . ? C48 C49 H49 116.6 . . ? C26 C27 C22 119.8(6) . . ? C26 C27 C28 115.9(6) . . ? C22 C27 C28 124.3(6) . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C11 C12 C13 122.4(7) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? O16 N8 O15 122.2(7) . . ? O16 N8 C46 118.9(7) . . ? O15 N8 C46 118.9(7) . . ? C39 C40 C41 123.1(7) . . ? C39 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C38 C37 C36 122.3(6) . . ? C38 C37 H37 115(5) . . ? C36 C37 H37 123(5) . . ? O13 C43 C44 120.3(6) . . ? O13 C43 C48 121.5(6) . . ? C44 C43 C48 118.2(6) . . ? C51 C50 C55 119.4(6) . . ? C51 C50 N7 119.4(6) . . ? C55 C50 N7 121.1(6) . . ? C18 C19 C20 120.5(7) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C27 C26 C25 120.4(7) . . ? C27 C26 H18A 119.8 . . ? C25 C26 H18A 119.8 . . ? C5 C6 C1 119.8(6) . . ? C5 C6 C7 115.4(6) . . ? C1 C6 C7 124.8(6) . . ? C47 C46 C45 122.4(8) . . ? C47 C46 N8 118.7(8) . . ? C45 C46 N8 118.8(7) . . ? C41 C36 C37 118.1(6) . . ? C41 C36 N5 120.9(6) . . ? C37 C36 N5 121.0(6) . . ? C53 C54 C55 122.0(7) . . ? C53 C54 H54 119.0 . . ? C55 C54 H54 119.0 . . ? C24 C25 C26 119.6(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C14 O2 Ni1 115.6(4) . . ? C14 O2 Ni4 124.7(4) . . ? Ni1 O2 Ni4 99.72(18) . . ? C14 O2 Ni3 118.7(4) . . ? Ni1 O2 Ni3 97.83(18) . . ? Ni4 O2 Ni3 95.23(17) . . ? C42 O10 Ni3 115.5(4) . . ? C42 O10 Ni4 116.7(4) . . ? Ni3 O10 Ni4 98.55(18) . . ? C42 O10 Ni2 126.1(4) . . ? Ni3 O10 Ni2 99.70(18) . . ? Ni4 O10 Ni2 95.28(17) . . ? C56 O14 Ni4 117.2(4) . . ? C56 O14 Ni1 121.2(4) . . ? Ni4 O14 Ni1 100.29(18) . . ? C56 O14 Ni2 120.5(4) . . ? Ni4 O14 Ni2 98.05(18) . . ? Ni1 O14 Ni2 94.68(17) . . ? C28 O6 Ni2 114.8(4) . . ? C28 O6 Ni1 119.1(4) . . ? Ni2 O6 Ni1 98.55(18) . . ? C28 O6 Ni3 123.8(4) . . ? Ni2 O6 Ni3 99.89(18) . . ? Ni1 O6 Ni3 95.91(18) . . ? C29 O9 Ni3 127.9(4) . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N10 C61 C60 178.6(14) . . ? N9 C62 C63 174.6(19) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.4 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N11 C65 C64 176.8(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.1 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 900850' ####################################################################### # # 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_sk_sk_213b_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 N4 Ni4 O16' _chemical_formula_sum 'C56 H84 N4 Ni4 O16' _chemical_formula_weight 1304.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3328(17) _cell_length_b 16.1942(19) _cell_length_c 16.976(2) _cell_angle_alpha 71.996(2) _cell_angle_beta 68.484(2) _cell_angle_gamma 66.013(2) _cell_volume 3289.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9561 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 33.17 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.432 _exptl_crystal_size_mid 0.321 _exptl_crystal_size_min 0.235 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.756 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51553 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.00 _reflns_number_total 14351 _reflns_number_gt 12302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.9407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14351 _refine_ls_number_parameters 753 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 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 0.339086(13) 0.255825(12) 0.332629(11) 0.01275(4) Uani 1 1 d . . . Ni2 Ni 0.316830(14) 0.125079(12) 0.250039(11) 0.01520(5) Uani 1 1 d . . . Ni3 Ni 0.115042(14) 0.275482(12) 0.343726(11) 0.01393(5) Uani 1 1 d . . . Ni4 Ni 0.253755(14) 0.327901(12) 0.166488(11) 0.01454(5) Uani 1 1 d . . . N4 N 0.29518(9) 0.44026(8) 0.12916(7) 0.0158(2) Uani 1 1 d . . . O10 O 0.31591(8) 0.29580(7) 0.05079(6) 0.0195(2) Uani 1 1 d . . . O11 O 0.39901(11) 0.22193(8) -0.08376(7) 0.0366(3) Uani 1 1 d . . . O3 O 0.38241(7) 0.22655(7) 0.21476(6) 0.01495(19) Uani 1 1 d . . . N1 N 0.45148(9) 0.31444(8) 0.27877(8) 0.0157(2) Uani 1 1 d . . . O2 O 0.17597(8) 0.37265(7) 0.57846(6) 0.0213(2) Uani 1 1 d . . . O1 O 0.28450(8) 0.30690(7) 0.43869(6) 0.0158(2) Uani 1 1 d . . . O16 O 0.10195(9) 0.41653(8) 0.14967(7) 0.0233(2) Uani 1 1 d . . . O15 O 0.08207(8) 0.32286(7) 0.45825(7) 0.0190(2) Uani 1 1 d . . . O7 O -0.01287(8) 0.36052(7) 0.30665(6) 0.0190(2) Uani 1 1 d . . . O8 O -0.14932(8) 0.47392(8) 0.22355(7) 0.0256(2) Uani 1 1 d . . . O4 O 0.43047(8) 0.02217(7) 0.29335(6) 0.0196(2) Uani 1 1 d . . . O5 O 0.58896(9) -0.08876(7) 0.35171(7) 0.0283(3) Uani 1 1 d . . . O14 O 0.38184(9) 0.11260(8) 0.11567(7) 0.0236(2) Uani 1 1 d D . . O13 O 0.45602(9) 0.13030(8) 0.37251(8) 0.0295(3) Uani 1 1 d . . . O9 O 0.24680(7) 0.17503(6) 0.36798(6) 0.01432(19) Uani 1 1 d . . . N2 N 0.23289(10) 0.04626(9) 0.26487(8) 0.0191(3) Uani 1 1 d . . . O6 O 0.18651(8) 0.22734(7) 0.22578(6) 0.0163(2) Uani 1 1 d . . . O12 O 0.21063(7) 0.35586(6) 0.28448(6) 0.01454(19) Uani 1 1 d . . . C36 C 0.21842(11) 0.12202(10) 0.45107(9) 0.0166(3) Uani 1 1 d . . . H36A H 0.2083 0.1546 0.4944 0.020 Uiso 1 1 calc R . . H36B H 0.2756 0.0640 0.4570 0.020 Uiso 1 1 calc R . . C22 C 0.13521(12) 0.09666(11) 0.23670(10) 0.0218(3) Uani 1 1 d . . . H22 H 0.0751 0.1033 0.2888 0.026 Uiso 1 1 calc R . . C24 C 0.11687(15) 0.04664(13) 0.18211(11) 0.0322(4) Uani 1 1 d . . . H24 H 0.1029 -0.0090 0.2201 0.039 Uiso 1 1 calc R . . C25 C 0.21305(17) 0.01604(15) 0.10653(12) 0.0433(5) Uani 1 1 d . . . H25A H 0.1966 -0.0142 0.0753 0.065 Uiso 1 1 calc R . . H25B H 0.2725 -0.0258 0.1279 0.065 Uiso 1 1 calc R . . H25C H 0.2306 0.0688 0.0689 0.065 Uiso 1 1 calc R . . C26 C 0.01798(17) 0.10656(15) 0.15175(14) 0.0444(5) Uani 1 1 d . . . H26A H 0.0320 0.1581 0.1089 0.067 Uiso 1 1 calc R . . H26B H -0.0399 0.1283 0.1998 0.067 Uiso 1 1 calc R . . H26C H -0.0004 0.0710 0.1274 0.067 Uiso 1 1 calc R . . C23 C 0.13688(12) 0.19457(11) 0.18906(10) 0.0209(3) Uani 1 1 d . . . H23A H 0.1750 0.1936 0.1287 0.025 Uiso 1 1 calc R . . H23B H 0.0646 0.2360 0.1924 0.025 Uiso 1 1 calc R . . C47 C 0.34928(11) 0.46626(10) 0.05300(9) 0.0186(3) Uani 1 1 d . . . H47 H 0.3616 0.5214 0.0424 0.022 Uiso 1 1 calc R . . C45 C 0.39312(11) 0.41744(10) -0.01814(9) 0.0178(3) Uani 1 1 d . . . C40 C 0.37505(11) 0.33652(10) -0.01511(9) 0.0174(3) Uani 1 1 d . . . C41 C 0.42469(13) 0.29725(10) -0.09107(10) 0.0227(3) Uani 1 1 d . . . C42 C 0.49024(13) 0.33348(11) -0.16324(10) 0.0263(3) Uani 1 1 d . . . H42 H 0.5227 0.3054 -0.2112 0.032 Uiso 1 1 calc R . . C43 C 0.50809(13) 0.41259(11) -0.16454(10) 0.0268(3) Uani 1 1 d . . . H43 H 0.5529 0.4370 -0.2131 0.032 Uiso 1 1 calc R . . C44 C 0.45940(12) 0.45404(11) -0.09402(10) 0.0238(3) Uani 1 1 d . . . H44 H 0.4702 0.5076 -0.0960 0.029 Uiso 1 1 calc R . . C46 C 0.4376(3) 0.18366(18) -0.15880(14) 0.0771(10) Uani 1 1 d . . . H46A H 0.4178 0.2311 -0.2060 0.116 Uiso 1 1 calc R . . H46B H 0.4075 0.1369 -0.1487 0.116 Uiso 1 1 calc R . . H46C H 0.5136 0.1571 -0.1726 0.116 Uiso 1 1 calc R . . C48 C 0.25971(11) 0.49182(10) 0.19929(9) 0.0179(3) Uani 1 1 d . . . H48 H 0.3223 0.4782 0.2181 0.021 Uiso 1 1 calc R . . C49 C 0.18075(11) 0.45212(9) 0.27655(9) 0.0167(3) Uani 1 1 d . . . H49A H 0.1787 0.4655 0.3292 0.020 Uiso 1 1 calc R . . H49B H 0.1100 0.4815 0.2686 0.020 Uiso 1 1 calc R . . C50 C 0.21577(13) 0.59753(10) 0.17128(10) 0.0262(3) Uani 1 1 d . . . H50 H 0.2746 0.6170 0.1286 0.031 Uiso 1 1 calc R . . C52 C 0.18014(16) 0.64441(12) 0.24791(12) 0.0394(5) Uani 1 1 d . . . H52A H 0.1655 0.7095 0.2279 0.059 Uiso 1 1 calc R . . H52B H 0.2355 0.6202 0.2761 0.059 Uiso 1 1 calc R . . H52C H 0.1170 0.6329 0.2879 0.059 Uiso 1 1 calc R . . C51 C 0.12735(14) 0.62875(12) 0.12830(11) 0.0363(4) Uani 1 1 d . . . H51A H 0.0686 0.6100 0.1682 0.054 Uiso 1 1 calc R . . H51B H 0.1534 0.6013 0.0783 0.054 Uiso 1 1 calc R . . H51C H 0.1043 0.6946 0.1113 0.054 Uiso 1 1 calc R . . C10 C 0.49067(11) 0.21880(10) 0.17603(9) 0.0179(3) Uani 1 1 d . . . H10A H 0.5079 0.2215 0.1146 0.021 Uiso 1 1 calc R . . H10B H 0.5349 0.1598 0.2003 0.021 Uiso 1 1 calc R . . C9 C 0.51442(11) 0.29659(10) 0.19071(9) 0.0172(3) Uani 1 1 d . . . H9 H 0.4864 0.3521 0.1507 0.021 Uiso 1 1 calc R . . C11 C 0.63447(12) 0.27979(12) 0.16864(10) 0.0263(3) Uani 1 1 d . . . H11 H 0.6419 0.3357 0.1729 0.032 Uiso 1 1 calc R . . C12 C 0.68990(14) 0.20063(14) 0.22956(13) 0.0399(5) Uani 1 1 d . . . H12A H 0.6857 0.1443 0.2259 0.060 Uiso 1 1 calc R . . H12B H 0.6560 0.2114 0.2875 0.060 Uiso 1 1 calc R . . H12C H 0.7631 0.1960 0.2139 0.060 Uiso 1 1 calc R . . C13 C 0.68842(15) 0.26627(15) 0.07483(12) 0.0415(5) Uani 1 1 d . . . H13A H 0.7594 0.2680 0.0577 0.062 Uiso 1 1 calc R . . H13B H 0.6487 0.3145 0.0381 0.062 Uiso 1 1 calc R . . H13C H 0.6909 0.2078 0.0700 0.062 Uiso 1 1 calc R . . C8 C 0.46332(11) 0.37006(10) 0.31099(9) 0.0174(3) Uani 1 1 d . . . H8 H 0.5184 0.3937 0.2793 0.021 Uiso 1 1 calc R . . C6 C 0.39870(11) 0.39974(10) 0.39246(9) 0.0177(3) Uani 1 1 d . . . C1 C 0.31402(11) 0.36813(9) 0.44975(9) 0.0155(3) Uani 1 1 d . . . C2 C 0.25688(11) 0.40600(10) 0.52642(9) 0.0183(3) Uani 1 1 d . . . C3 C 0.28329(12) 0.46956(11) 0.54475(11) 0.0244(3) Uani 1 1 d . . . H3 H 0.2451 0.4924 0.5955 0.029 Uiso 1 1 calc R . . C4 C 0.36719(13) 0.49986(12) 0.48748(11) 0.0288(4) Uani 1 1 d . . . H4 H 0.3848 0.5428 0.5000 0.035 Uiso 1 1 calc R . . C5 C 0.42296(12) 0.46594(11) 0.41321(11) 0.0242(3) Uani 1 1 d . . . H5 H 0.4783 0.4867 0.3752 0.029 Uiso 1 1 calc R . . C7 C 0.12926(14) 0.39309(13) 0.66339(10) 0.0308(4) Uani 1 1 d . . . H7A H 0.1838 0.3733 0.6917 0.046 Uiso 1 1 calc R . . H7B H 0.0788 0.3615 0.6957 0.046 Uiso 1 1 calc R . . H7C H 0.0938 0.4582 0.6599 0.046 Uiso 1 1 calc R . . C56 C 0.07360(16) 0.44134(16) 0.07248(12) 0.0440(5) Uani 1 1 d . . . H56A H 0.1307 0.4549 0.0249 0.066 Uiso 1 1 calc R . . H56B H 0.0108 0.4947 0.0749 0.066 Uiso 1 1 calc R . . H56C H 0.0599 0.3914 0.0649 0.066 Uiso 1 1 calc R . . C55 C -0.01265(12) 0.39075(11) 0.49312(11) 0.0260(3) Uani 1 1 d . . . H55A H -0.0132 0.4502 0.4583 0.039 Uiso 1 1 calc R . . H55B H -0.0162 0.3901 0.5509 0.039 Uiso 1 1 calc R . . H55C H -0.0728 0.3780 0.4938 0.039 Uiso 1 1 calc R . . C27 C -0.10140(11) 0.34312(10) 0.32790(9) 0.0171(3) Uani 1 1 d . . . C32 C -0.12667(11) 0.26836(10) 0.39129(9) 0.0182(3) Uani 1 1 d . . . C31 C -0.22947(12) 0.26232(11) 0.41358(10) 0.0224(3) Uani 1 1 d . . . H31 H -0.2463 0.2144 0.4565 0.027 Uiso 1 1 calc R . . C30 C -0.30413(12) 0.32463(12) 0.37385(11) 0.0261(3) Uani 1 1 d . . . H30 H -0.3714 0.3198 0.3903 0.031 Uiso 1 1 calc R . . C29 C -0.27911(12) 0.39612(11) 0.30800(10) 0.0237(3) Uani 1 1 d . . . H29 H -0.3291 0.4376 0.2793 0.028 Uiso 1 1 calc R . . C28 C -0.18089(12) 0.40502(10) 0.28574(10) 0.0203(3) Uani 1 1 d . . . C33 C -0.22681(14) 0.54218(13) 0.18283(13) 0.0370(4) Uani 1 1 d . . . H33A H -0.2472 0.5140 0.1526 0.055 Uiso 1 1 calc R . . H33B H -0.1974 0.5880 0.1428 0.055 Uiso 1 1 calc R . . H33C H -0.2880 0.5706 0.2257 0.055 Uiso 1 1 calc R . . C34 C -0.05315(11) 0.19444(10) 0.43528(9) 0.0180(3) Uani 1 1 d . . . H34 H -0.0794 0.1505 0.4774 0.022 Uiso 1 1 calc R . . N3 N 0.04467(9) 0.18408(8) 0.42152(7) 0.0163(2) Uani 1 1 d . . . C35 C 0.11501(11) 0.10305(10) 0.46629(9) 0.0174(3) Uani 1 1 d . . . H35 H 0.1349 0.0516 0.4379 0.021 Uiso 1 1 calc R . . C37 C 0.06240(13) 0.07266(10) 0.56295(10) 0.0226(3) Uani 1 1 d . . . H37 H 0.0058 0.0516 0.5662 0.027 Uiso 1 1 calc R . . C38 C 0.01143(14) 0.15008(12) 0.61448(10) 0.0300(4) Uani 1 1 d . . . H38A H -0.0184 0.1265 0.6738 0.045 Uiso 1 1 calc R . . H38B H -0.0437 0.1982 0.5915 0.045 Uiso 1 1 calc R . . H38C H 0.0644 0.1742 0.6106 0.045 Uiso 1 1 calc R . . C39 C 0.14295(14) -0.00903(12) 0.60285(11) 0.0323(4) Uani 1 1 d . . . H39A H 0.1948 0.0111 0.6075 0.049 Uiso 1 1 calc R . . H39B H 0.1778 -0.0547 0.5670 0.049 Uiso 1 1 calc R . . H39C H 0.1071 -0.0350 0.6592 0.049 Uiso 1 1 calc R . . C21 C 0.25725(13) -0.03973(11) 0.29775(9) 0.0223(3) Uani 1 1 d . . . H21 H 0.2111 -0.0691 0.3023 0.027 Uiso 1 1 calc R . . C19 C 0.34992(13) -0.09550(10) 0.32849(9) 0.0218(3) Uani 1 1 d . . . C14 C 0.42967(12) -0.06219(10) 0.32464(9) 0.0197(3) Uani 1 1 d . . . C15 C 0.51653(13) -0.12670(11) 0.35693(10) 0.0245(3) Uani 1 1 d . . . C20 C 0.68321(16) -0.15038(13) 0.37532(15) 0.0457(5) Uani 1 1 d . . . H20A H 0.6646 -0.1805 0.4344 0.069 Uiso 1 1 calc R . . H20B H 0.7281 -0.1165 0.3685 0.069 Uiso 1 1 calc R . . H20C H 0.7204 -0.1956 0.3390 0.069 Uiso 1 1 calc R . . C16 C 0.52438(15) -0.21784(11) 0.38983(10) 0.0310(4) Uani 1 1 d . . . H16 H 0.5819 -0.2584 0.4106 0.037 Uiso 1 1 calc R . . C17 C 0.44534(16) -0.24928(11) 0.39193(11) 0.0343(4) Uani 1 1 d . . . H17 H 0.4507 -0.3108 0.4136 0.041 Uiso 1 1 calc R . . C18 C 0.36106(15) -0.18974(11) 0.36230(10) 0.0299(4) Uani 1 1 d . . . H18 H 0.3091 -0.2113 0.3642 0.036 Uiso 1 1 calc R . . C54 C 0.48981(17) 0.06393(15) 0.08100(13) 0.0478(5) Uani 1 1 d D . . H54A H 0.5280 0.0485 0.1225 0.072 Uiso 1 1 calc R . . H54B H 0.5194 0.1016 0.0297 0.072 Uiso 1 1 calc RD . . H54C H 0.4956 0.0086 0.0672 0.072 Uiso 1 1 calc RD . . C53 C 0.52398(16) 0.10898(12) 0.42175(13) 0.0353(4) Uani 1 1 d . . . H53A H 0.5267 0.1647 0.4282 0.053 Uiso 1 1 calc R . . H53B H 0.5939 0.0725 0.3937 0.053 Uiso 1 1 calc R . . H53C H 0.4985 0.0749 0.4775 0.053 Uiso 1 1 calc R . . H15M H 0.1340(16) 0.3284(13) 0.4619(12) 0.032(5) Uiso 1 1 d . . . H13M H 0.4590(16) 0.0883(15) 0.3557(13) 0.040(6) Uiso 1 1 d . . . H16M H 0.0530(16) 0.4070(14) 0.1915(13) 0.036(6) Uiso 1 1 d . . . H14M H 0.3656(16) 0.1640(11) 0.0887(13) 0.041(6) Uiso 1 1 d 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 0.01226(9) 0.01384(9) 0.01234(9) -0.00227(7) -0.00317(7) -0.00489(7) Ni2 0.01887(10) 0.01470(9) 0.01378(9) -0.00148(7) -0.00574(7) -0.00705(7) Ni3 0.01320(9) 0.01594(9) 0.01252(9) 0.00022(7) -0.00414(7) -0.00629(7) Ni4 0.01621(9) 0.01589(9) 0.01119(9) 0.00014(7) -0.00371(7) -0.00705(7) N4 0.0153(6) 0.0155(6) 0.0142(6) -0.0015(5) -0.0034(5) -0.0043(5) O10 0.0245(6) 0.0221(5) 0.0130(5) -0.0003(4) -0.0031(4) -0.0128(4) O11 0.0635(9) 0.0302(6) 0.0172(6) -0.0065(5) 0.0010(6) -0.0259(6) O3 0.0140(5) 0.0168(5) 0.0135(5) -0.0028(4) -0.0025(4) -0.0058(4) N1 0.0120(6) 0.0159(6) 0.0169(6) -0.0025(5) -0.0032(5) -0.0037(5) O2 0.0187(5) 0.0258(6) 0.0178(5) -0.0088(4) -0.0015(4) -0.0055(4) O1 0.0169(5) 0.0175(5) 0.0147(5) -0.0042(4) -0.0036(4) -0.0074(4) O16 0.0187(6) 0.0307(6) 0.0159(5) 0.0045(5) -0.0068(4) -0.0083(5) O15 0.0146(5) 0.0241(5) 0.0195(5) -0.0074(4) -0.0029(4) -0.0068(4) O7 0.0156(5) 0.0213(5) 0.0204(5) 0.0005(4) -0.0071(4) -0.0077(4) O8 0.0199(6) 0.0285(6) 0.0265(6) 0.0024(5) -0.0126(5) -0.0063(5) O4 0.0252(6) 0.0145(5) 0.0195(5) -0.0021(4) -0.0082(4) -0.0057(4) O5 0.0337(6) 0.0212(6) 0.0295(6) -0.0009(5) -0.0188(5) -0.0024(5) O14 0.0317(6) 0.0218(6) 0.0176(5) -0.0033(5) -0.0054(5) -0.0107(5) O13 0.0314(7) 0.0180(6) 0.0485(8) -0.0118(5) -0.0286(6) 0.0023(5) O9 0.0163(5) 0.0156(5) 0.0112(5) 0.0007(4) -0.0046(4) -0.0072(4) N2 0.0257(7) 0.0220(6) 0.0131(6) -0.0030(5) -0.0044(5) -0.0123(5) O6 0.0183(5) 0.0200(5) 0.0143(5) 0.0002(4) -0.0070(4) -0.0101(4) O12 0.0154(5) 0.0135(5) 0.0141(5) -0.0006(4) -0.0041(4) -0.0056(4) C36 0.0189(7) 0.0166(7) 0.0127(7) 0.0015(5) -0.0046(5) -0.0072(6) C22 0.0251(8) 0.0295(8) 0.0176(7) -0.0039(6) -0.0052(6) -0.0164(7) C24 0.0428(10) 0.0391(10) 0.0302(9) -0.0062(8) -0.0140(8) -0.0256(9) C25 0.0618(13) 0.0502(12) 0.0335(10) -0.0187(9) -0.0160(9) -0.0233(11) C26 0.0500(12) 0.0604(13) 0.0450(12) -0.0042(10) -0.0252(10) -0.0334(11) C23 0.0240(8) 0.0265(8) 0.0184(7) -0.0029(6) -0.0091(6) -0.0125(6) C47 0.0188(7) 0.0168(7) 0.0192(7) -0.0009(6) -0.0045(6) -0.0075(6) C45 0.0163(7) 0.0202(7) 0.0145(7) 0.0001(6) -0.0040(5) -0.0063(6) C40 0.0165(7) 0.0198(7) 0.0132(7) 0.0012(6) -0.0059(5) -0.0051(6) C41 0.0288(8) 0.0205(7) 0.0169(7) -0.0022(6) -0.0047(6) -0.0088(6) C42 0.0295(9) 0.0271(8) 0.0159(7) -0.0053(6) 0.0002(6) -0.0078(7) C43 0.0262(8) 0.0309(9) 0.0177(7) -0.0007(6) 0.0018(6) -0.0137(7) C44 0.0250(8) 0.0239(8) 0.0207(8) -0.0002(6) -0.0026(6) -0.0128(7) C46 0.147(3) 0.0585(15) 0.0316(11) -0.0234(11) 0.0170(14) -0.0664(18) C48 0.0185(7) 0.0155(7) 0.0174(7) -0.0032(6) -0.0027(6) -0.0053(6) C49 0.0171(7) 0.0144(7) 0.0152(7) -0.0017(5) -0.0031(5) -0.0040(5) C50 0.0295(9) 0.0141(7) 0.0237(8) -0.0020(6) 0.0032(7) -0.0066(6) C52 0.0494(12) 0.0206(8) 0.0362(10) -0.0111(8) 0.0069(9) -0.0123(8) C51 0.0326(10) 0.0217(8) 0.0295(9) 0.0043(7) -0.0017(7) 0.0026(7) C10 0.0137(7) 0.0201(7) 0.0166(7) -0.0056(6) 0.0003(5) -0.0050(6) C9 0.0143(7) 0.0180(7) 0.0160(7) -0.0021(6) -0.0019(5) -0.0051(6) C11 0.0159(8) 0.0349(9) 0.0291(9) -0.0117(7) 0.0020(6) -0.0124(7) C12 0.0183(8) 0.0519(12) 0.0491(12) -0.0249(10) -0.0131(8) 0.0034(8) C13 0.0280(10) 0.0594(13) 0.0333(10) -0.0168(9) 0.0120(8) -0.0232(9) C8 0.0138(7) 0.0179(7) 0.0207(7) -0.0012(6) -0.0053(6) -0.0069(6) C6 0.0157(7) 0.0169(7) 0.0223(7) -0.0045(6) -0.0084(6) -0.0037(6) C1 0.0140(7) 0.0138(6) 0.0185(7) -0.0033(5) -0.0084(6) -0.0008(5) C2 0.0142(7) 0.0183(7) 0.0212(7) -0.0054(6) -0.0072(6) -0.0010(6) C3 0.0228(8) 0.0240(8) 0.0280(8) -0.0142(7) -0.0084(7) -0.0013(6) C4 0.0285(9) 0.0268(8) 0.0403(10) -0.0162(8) -0.0106(7) -0.0097(7) C5 0.0211(8) 0.0243(8) 0.0321(9) -0.0084(7) -0.0065(7) -0.0107(6) C7 0.0293(9) 0.0392(10) 0.0207(8) -0.0144(7) 0.0004(7) -0.0083(8) C56 0.0348(10) 0.0656(14) 0.0254(9) 0.0043(9) -0.0152(8) -0.0139(10) C55 0.0201(8) 0.0280(8) 0.0278(8) -0.0124(7) -0.0042(6) -0.0030(7) C27 0.0153(7) 0.0217(7) 0.0165(7) -0.0088(6) -0.0031(5) -0.0056(6) C32 0.0164(7) 0.0227(7) 0.0172(7) -0.0081(6) -0.0024(6) -0.0071(6) C31 0.0186(8) 0.0269(8) 0.0242(8) -0.0096(6) -0.0006(6) -0.0112(6) C30 0.0150(7) 0.0351(9) 0.0333(9) -0.0130(7) -0.0048(6) -0.0101(7) C29 0.0167(7) 0.0309(8) 0.0266(8) -0.0104(7) -0.0102(6) -0.0035(6) C28 0.0193(7) 0.0239(8) 0.0191(7) -0.0079(6) -0.0054(6) -0.0058(6) C33 0.0299(9) 0.0376(10) 0.0391(10) 0.0064(8) -0.0213(8) -0.0065(8) C34 0.0193(7) 0.0207(7) 0.0158(7) -0.0045(6) -0.0007(6) -0.0112(6) N3 0.0185(6) 0.0172(6) 0.0134(6) -0.0020(5) -0.0037(5) -0.0073(5) C35 0.0201(7) 0.0163(7) 0.0148(7) -0.0004(5) -0.0048(6) -0.0071(6) C37 0.0266(8) 0.0227(8) 0.0170(7) 0.0030(6) -0.0038(6) -0.0136(7) C38 0.0355(10) 0.0337(9) 0.0146(7) -0.0010(7) -0.0005(7) -0.0137(8) C39 0.0394(10) 0.0260(9) 0.0257(9) 0.0080(7) -0.0095(7) -0.0141(8) C21 0.0288(8) 0.0250(8) 0.0163(7) -0.0070(6) 0.0012(6) -0.0164(7) C19 0.0311(9) 0.0177(7) 0.0135(7) -0.0043(6) -0.0001(6) -0.0097(6) C14 0.0293(8) 0.0151(7) 0.0114(7) -0.0051(5) -0.0029(6) -0.0047(6) C15 0.0333(9) 0.0206(8) 0.0159(7) -0.0045(6) -0.0070(6) -0.0045(7) C20 0.0425(12) 0.0329(10) 0.0581(13) 0.0064(9) -0.0321(10) -0.0040(9) C16 0.0441(10) 0.0189(8) 0.0210(8) -0.0002(6) -0.0116(7) -0.0021(7) C17 0.0538(12) 0.0167(8) 0.0230(8) 0.0009(7) -0.0043(8) -0.0114(8) C18 0.0408(10) 0.0225(8) 0.0231(8) -0.0032(7) 0.0003(7) -0.0161(7) C54 0.0529(13) 0.0436(12) 0.0369(11) -0.0204(9) -0.0098(10) 0.0007(10) C53 0.0483(11) 0.0255(9) 0.0407(10) -0.0013(8) -0.0316(9) -0.0070(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.9746(10) . ? Ni1 N1 1.9895(12) . ? Ni1 O3 2.0123(10) . ? Ni1 O9 2.0399(9) . ? Ni1 O12 2.1313(10) . ? Ni1 O13 2.1473(11) . ? Ni2 O4 1.9709(10) . ? Ni2 N2 1.9920(12) . ? Ni2 O6 2.0072(10) . ? Ni2 O3 2.0438(10) . ? Ni2 O9 2.1302(10) . ? Ni2 O14 2.1645(11) . ? Ni3 O7 1.9778(10) . ? Ni3 N3 1.9951(12) . ? Ni3 O9 2.0102(10) . ? Ni3 O12 2.0525(9) . ? Ni3 O6 2.1159(10) . ? Ni3 O15 2.1319(10) . ? Ni4 O10 1.9730(10) . ? Ni4 N4 1.9887(12) . ? Ni4 O12 2.0060(10) . ? Ni4 O6 2.0360(10) . ? Ni4 O16 2.1305(11) . ? Ni4 O3 2.1406(10) . ? N4 C47 1.2819(18) . ? N4 C48 1.4827(18) . ? O10 C40 1.3069(17) . ? O11 C41 1.3699(19) . ? O11 C46 1.416(2) . ? O3 C10 1.4142(16) . ? N1 C8 1.2791(18) . ? N1 C9 1.4827(17) . ? O2 C2 1.3710(18) . ? O2 C7 1.4295(18) . ? O1 C1 1.3085(16) . ? O16 C56 1.406(2) . ? O16 H16M 0.82(2) . ? O15 C55 1.4147(18) . ? O15 H15M 0.81(2) . ? O7 C27 1.3084(17) . ? O8 C28 1.3770(18) . ? O8 C33 1.4234(19) . ? O4 C14 1.3070(17) . ? O5 C15 1.371(2) . ? O5 C20 1.427(2) . ? O14 C54 1.411(2) . ? O14 H14M 0.801(15) . ? O13 C53 1.3830(19) . ? O13 H13M 0.80(2) . ? O9 C36 1.4165(16) . ? N2 C21 1.280(2) . ? N2 C22 1.475(2) . ? O6 C23 1.4188(16) . ? O12 C49 1.4147(16) . ? C36 C35 1.5486(19) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C22 C23 1.547(2) . ? C22 C24 1.549(2) . ? C22 H22 0.9800 . ? C24 C26 1.525(3) . ? C24 C25 1.527(3) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C47 C45 1.452(2) . ? C47 H47 0.9300 . ? C45 C44 1.415(2) . ? C45 C40 1.418(2) . ? C40 C41 1.428(2) . ? C41 C42 1.374(2) . ? C42 C43 1.397(2) . ? C42 H42 0.9300 . ? C43 C44 1.369(2) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C48 C50 1.547(2) . ? C48 C49 1.5478(19) . ? C48 H48 0.9800 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.524(3) . ? C50 C52 1.529(2) . ? C50 H50 0.9800 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C10 C9 1.539(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 C11 1.544(2) . ? C9 H9 0.9800 . ? C11 C12 1.516(3) . ? C11 C13 1.535(2) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C8 C6 1.453(2) . ? C8 H8 0.9300 . ? C6 C1 1.419(2) . ? C6 C5 1.422(2) . ? C1 C2 1.430(2) . ? C2 C3 1.379(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9300 . ? C4 C5 1.365(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C27 C32 1.421(2) . ? C27 C28 1.429(2) . ? C32 C31 1.417(2) . ? C32 C34 1.449(2) . ? C31 C30 1.360(2) . ? C31 H31 0.9300 . ? C30 C29 1.401(2) . ? C30 H30 0.9300 . ? C29 C28 1.373(2) . ? C29 H29 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N3 1.2812(18) . ? C34 H34 0.9300 . ? N3 C35 1.4785(18) . ? C35 C37 1.5487(19) . ? C35 H35 0.9800 . ? C37 C39 1.523(2) . ? C37 C38 1.528(2) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C21 C19 1.447(2) . ? C21 H21 0.9300 . ? C19 C18 1.418(2) . ? C19 C14 1.424(2) . ? C14 C15 1.425(2) . ? C15 C16 1.380(2) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C16 C17 1.404(3) . ? C16 H16 0.9300 . ? C17 C18 1.357(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 93.81(4) . . ? O1 Ni1 O3 169.90(4) . . ? N1 Ni1 O3 83.32(4) . . ? O1 Ni1 O9 98.79(4) . . ? N1 Ni1 O9 166.41(4) . . ? O3 Ni1 O9 85.09(4) . . ? O1 Ni1 O12 91.56(4) . . ? N1 Ni1 O12 102.16(4) . . ? O3 Ni1 O12 79.64(4) . . ? O9 Ni1 O12 82.66(4) . . ? O1 Ni1 O13 98.26(4) . . ? N1 Ni1 O13 88.96(5) . . ? O3 Ni1 O13 91.38(4) . . ? O9 Ni1 O13 84.23(4) . . ? O12 Ni1 O13 164.67(4) . . ? O4 Ni2 N2 93.96(5) . . ? O4 Ni2 O6 170.71(4) . . ? N2 Ni2 O6 82.97(5) . . ? O4 Ni2 O3 98.84(4) . . ? N2 Ni2 O3 166.31(5) . . ? O6 Ni2 O3 85.11(4) . . ? O4 Ni2 O9 92.97(4) . . ? N2 Ni2 O9 102.23(4) . . ? O6 Ni2 O9 79.19(4) . . ? O3 Ni2 O9 82.03(4) . . ? O4 Ni2 O14 97.68(4) . . ? N2 Ni2 O14 87.94(4) . . ? O6 Ni2 O14 90.99(4) . . ? O3 Ni2 O14 85.56(4) . . ? O9 Ni2 O14 164.75(4) . . ? O7 Ni3 N3 94.17(5) . . ? O7 Ni3 O9 169.82(4) . . ? N3 Ni3 O9 83.02(4) . . ? O7 Ni3 O12 98.65(4) . . ? N3 Ni3 O12 165.67(4) . . ? O9 Ni3 O12 85.40(4) . . ? O7 Ni3 O6 91.75(4) . . ? N3 Ni3 O6 103.50(4) . . ? O9 Ni3 O6 79.47(4) . . ? O12 Ni3 O6 82.55(4) . . ? O7 Ni3 O15 98.96(4) . . ? N3 Ni3 O15 85.22(4) . . ? O9 Ni3 O15 90.58(4) . . ? O12 Ni3 O15 86.49(4) . . ? O6 Ni3 O15 165.71(4) . . ? O10 Ni4 N4 94.04(4) . . ? O10 Ni4 O12 172.34(4) . . ? N4 Ni4 O12 83.42(4) . . ? O10 Ni4 O6 97.51(4) . . ? N4 Ni4 O6 167.38(4) . . ? O12 Ni4 O6 85.75(4) . . ? O10 Ni4 O16 96.77(4) . . ? N4 Ni4 O16 86.76(5) . . ? O12 Ni4 O16 90.31(4) . . ? O6 Ni4 O16 86.85(4) . . ? O10 Ni4 O3 93.99(4) . . ? N4 Ni4 O3 102.35(4) . . ? O12 Ni4 O3 79.56(4) . . ? O6 Ni4 O3 81.95(4) . . ? O16 Ni4 O3 165.38(4) . . ? C47 N4 C48 121.91(12) . . ? C47 N4 Ni4 124.65(10) . . ? C48 N4 Ni4 113.41(9) . . ? C40 O10 Ni4 124.83(9) . . ? C41 O11 C46 116.53(14) . . ? C10 O3 Ni1 108.30(8) . . ? C10 O3 Ni2 127.42(8) . . ? Ni1 O3 Ni2 97.24(4) . . ? C10 O3 Ni4 124.68(8) . . ? Ni1 O3 Ni4 100.14(4) . . ? Ni2 O3 Ni4 93.31(4) . . ? C8 N1 C9 121.52(12) . . ? C8 N1 Ni1 124.90(10) . . ? C9 N1 Ni1 113.20(9) . . ? C2 O2 C7 116.75(12) . . ? C1 O1 Ni1 124.93(9) . . ? C56 O16 Ni4 124.91(11) . . ? C56 O16 H16M 111.0(14) . . ? Ni4 O16 H16M 112.4(14) . . ? C55 O15 Ni3 125.05(9) . . ? C55 O15 H15M 111.7(14) . . ? Ni3 O15 H15M 111.8(14) . . ? C27 O7 Ni3 124.60(9) . . ? C28 O8 C33 116.56(12) . . ? C14 O4 Ni2 125.12(10) . . ? C15 O5 C20 116.81(13) . . ? C54 O14 Ni2 121.93(11) . . ? C54 O14 H14M 110.6(15) . . ? Ni2 O14 H14M 105.8(15) . . ? C53 O13 Ni1 132.81(11) . . ? C53 O13 H13M 115.4(15) . . ? Ni1 O13 H13M 111.8(15) . . ? C36 O9 Ni3 108.77(8) . . ? C36 O9 Ni1 125.61(8) . . ? Ni3 O9 Ni1 97.07(4) . . ? C36 O9 Ni2 125.63(8) . . ? Ni3 O9 Ni2 100.37(4) . . ? Ni1 O9 Ni2 93.72(4) . . ? C21 N2 C22 121.45(13) . . ? C21 N2 Ni2 124.78(11) . . ? C22 N2 Ni2 113.75(9) . . ? C23 O6 Ni2 108.71(9) . . ? C23 O6 Ni4 126.23(9) . . ? Ni2 O6 Ni4 97.66(4) . . ? C23 O6 Ni3 124.60(9) . . ? Ni2 O6 Ni3 100.95(4) . . ? Ni4 O6 Ni3 93.39(4) . . ? C49 O12 Ni4 108.33(8) . . ? C49 O12 Ni3 127.58(8) . . ? Ni4 O12 Ni3 96.24(4) . . ? C49 O12 Ni1 125.08(8) . . ? Ni4 O12 Ni1 100.65(4) . . ? Ni3 O12 Ni1 92.98(4) . . ? O9 C36 C35 111.15(11) . . ? O9 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? O9 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? N2 C22 C23 108.55(11) . . ? N2 C22 C24 114.06(13) . . ? C23 C22 C24 112.07(13) . . ? N2 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C24 C22 H22 107.3 . . ? C26 C24 C25 111.24(16) . . ? C26 C24 C22 110.05(15) . . ? C25 C24 C22 113.55(14) . . ? C26 C24 H24 107.2 . . ? C25 C24 H24 107.2 . . ? C22 C24 H24 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C23 C22 110.97(12) . . ? O6 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? O6 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N4 C47 C45 125.90(13) . . ? N4 C47 H47 117.1 . . ? C45 C47 H47 117.1 . . ? C44 C45 C40 119.44(13) . . ? C44 C45 C47 116.17(13) . . ? C40 C45 C47 124.38(13) . . ? O10 C40 C45 125.50(13) . . ? O10 C40 C41 117.52(13) . . ? C45 C40 C41 116.98(13) . . ? O11 C41 C42 124.82(14) . . ? O11 C41 C40 113.00(13) . . ? C42 C41 C40 122.18(14) . . ? C41 C42 C43 119.93(14) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 119.73(14) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 121.69(14) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? O11 C46 H46A 109.5 . . ? O11 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O11 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N4 C48 C50 114.10(12) . . ? N4 C48 C49 108.08(11) . . ? C50 C48 C49 113.42(12) . . ? N4 C48 H48 106.9 . . ? C50 C48 H48 106.9 . . ? C49 C48 H48 106.9 . . ? O12 C49 C48 111.16(11) . . ? O12 C49 H49A 109.4 . . ? C48 C49 H49A 109.4 . . ? O12 C49 H49B 109.4 . . ? C48 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C51 C50 C52 111.40(15) . . ? C51 C50 C48 113.18(14) . . ? C52 C50 C48 110.24(13) . . ? C51 C50 H50 107.2 . . ? C52 C50 H50 107.2 . . ? C48 C50 H50 107.2 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O3 C10 C9 110.93(11) . . ? O3 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? N1 C9 C10 108.28(11) . . ? N1 C9 C11 115.37(12) . . ? C10 C9 C11 113.21(12) . . ? N1 C9 H9 106.5 . . ? C10 C9 H9 106.5 . . ? C11 C9 H9 106.5 . . ? C12 C11 C13 111.03(15) . . ? C12 C11 C9 113.91(14) . . ? C13 C11 C9 109.62(13) . . ? C12 C11 H11 107.3 . . ? C13 C11 H11 107.3 . . ? C9 C11 H11 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C8 C6 126.01(13) . . ? N1 C8 H8 117.0 . . ? C6 C8 H8 117.0 . . ? C1 C6 C5 119.59(13) . . ? C1 C6 C8 124.19(12) . . ? C5 C6 C8 116.21(13) . . ? O1 C1 C6 125.58(13) . . ? O1 C1 C2 117.42(12) . . ? C6 C1 C2 116.99(12) . . ? O2 C2 C3 124.43(13) . . ? O2 C2 C1 113.78(12) . . ? C3 C2 C1 121.79(14) . . ? C2 C3 C4 120.40(14) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.52(14) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.71(14) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O16 C56 H56A 109.5 . . ? O16 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O16 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O15 C55 H55A 109.5 . . ? O15 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O15 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O7 C27 C32 125.41(13) . . ? O7 C27 C28 117.91(13) . . ? C32 C27 C28 116.67(13) . . ? C31 C32 C27 119.52(14) . . ? C31 C32 C34 115.92(13) . . ? C27 C32 C34 124.55(13) . . ? C30 C31 C32 121.79(15) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C30 C29 119.64(14) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C28 C29 C30 120.13(15) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C28 O8 124.70(14) . . ? C29 C28 C27 122.10(14) . . ? O8 C28 C27 113.19(12) . . ? O8 C33 H33A 109.5 . . ? O8 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O8 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C32 125.99(13) . . ? N3 C34 H34 117.0 . . ? C32 C34 H34 117.0 . . ? C34 N3 C35 121.84(12) . . ? C34 N3 Ni3 124.43(10) . . ? C35 N3 Ni3 113.68(9) . . ? N3 C35 C37 114.48(12) . . ? N3 C35 C36 108.44(11) . . ? C37 C35 C36 112.69(12) . . ? N3 C35 H35 106.9 . . ? C37 C35 H35 106.9 . . ? C36 C35 H35 106.9 . . ? C39 C37 C38 111.01(14) . . ? C39 C37 C35 109.83(13) . . ? C38 C37 C35 113.73(12) . . ? C39 C37 H37 107.3 . . ? C38 C37 H37 107.3 . . ? C35 C37 H37 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C21 C19 126.08(14) . . ? N2 C21 H21 117.0 . . ? C19 C21 H21 117.0 . . ? C18 C19 C14 119.33(15) . . ? C18 C19 C21 116.36(14) . . ? C14 C19 C21 124.29(13) . . ? O4 C14 C19 125.59(14) . . ? O4 C14 C15 117.32(14) . . ? C19 C14 C15 117.09(13) . . ? O5 C15 C16 124.76(15) . . ? O5 C15 C14 113.30(13) . . ? C16 C15 C14 121.94(16) . . ? O5 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C16 C17 119.89(16) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 119.85(15) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 121.90(16) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? O14 C54 H54A 109.5 . . ? O14 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O14 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O13 C53 H53A 109.5 . . ? O13 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O13 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.426 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.049 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 498.0 7.5 2 0.222 0.667 0.405 7.3 -0.2 3 0.778 0.333 0.595 7.3 -0.2 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 900851' ####################################################################### # # 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_sk_086_4_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 N4 Ni4 O16' _chemical_formula_sum 'C72 H74 N4 Ni4 O16' _chemical_formula_weight 1486.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8226(12) _cell_length_b 15.9005(13) _cell_length_c 17.7741(14) _cell_angle_alpha 85.655(2) _cell_angle_beta 66.2790(10) _cell_angle_gamma 72.521(2) _cell_volume 3653.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9790 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.79 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.109 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47893 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.83 _reflns_number_total 12513 _reflns_number_gt 11704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+125.5299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12513 _refine_ls_number_parameters 592 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.1272 _refine_ls_wR_factor_ref 0.2784 _refine_ls_wR_factor_gt 0.2762 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 C28 C 0.8677(3) 0.0616(3) 0.4422(3) 0.0537(13) Uani 1 1 d G A 4 C29 C 0.8938(3) -0.0237(3) 0.4680(3) 0.0537(13) Uani 1 1 d G A 4 H29 H 0.9076 -0.0333 0.5151 0.064 Uiso 1 1 calc R A 4 C30 C 0.8992(4) -0.0946(3) 0.4235(3) 0.0537(13) Uani 1 1 d G A 4 H30 H 0.9167 -0.1516 0.4408 0.064 Uiso 1 1 calc R A 4 C31 C 0.8786(4) -0.0802(4) 0.3532(3) 0.0537(13) Uani 1 1 d G A 4 H31 H 0.8823 -0.1276 0.3234 0.064 Uiso 1 1 calc R A 4 C32 C 0.8525(4) 0.0051(4) 0.3273(3) 0.0537(13) Uani 1 1 d G A 4 H32 H 0.8387 0.0147 0.2802 0.064 Uiso 1 1 calc R A 4 C33 C 0.8471(4) 0.0759(4) 0.3718(3) 0.0537(13) Uani 1 1 d G A 4 H33 H 0.8296 0.1330 0.3545 0.064 Uiso 1 1 calc R A 4 C62 C 0.8946(4) 0.2347(4) 0.8063(4) 0.078(2) Uani 1 1 d G A 4 H62 H 0.9628 0.2070 0.7634 0.094 Uiso 1 1 calc R A 4 C63 C 0.8885(4) 0.3209(4) 0.7825(4) 0.078(2) Uani 1 1 d G A 4 H63 H 0.8713 0.3401 0.7379 0.094 Uiso 1 1 calc R A 4 C64 C 0.9079(4) 0.3782(4) 0.8253(4) 0.078(2) Uani 1 1 d G A 4 H64 H 0.9038 0.4358 0.8093 0.094 Uiso 1 1 calc R A 4 C65 C 0.9336(5) 0.3493(5) 0.8919(4) 0.078(2) Uani 1 1 d G A 4 H65 H 0.9467 0.3877 0.9205 0.094 Uiso 1 1 calc R A 4 C66 C 0.9398(4) 0.2632(5) 0.9157(4) 0.078(2) Uani 1 1 d G A 4 H66 H 0.9570 0.2439 0.9603 0.094 Uiso 1 1 calc R A 4 C67 C 0.9203(4) 0.2059(4) 0.8729(4) 0.078(2) Uani 1 1 d G A 4 H67 H 0.9244 0.1482 0.8889 0.094 Uiso 1 1 calc R A 4 C11 C 0.1565(4) 0.5459(4) 0.7768(4) 0.103(3) Uani 1 1 d GD A 4 C12 C 0.1491(4) 0.6331(3) 0.7901(4) 0.103(3) Uani 1 1 d GD A 4 H12 H 0.1589 0.6492 0.8349 0.123 Uiso 1 1 calc R A 4 C13 C 0.1272(5) 0.6964(4) 0.7366(5) 0.103(3) Uani 1 1 d GD A 4 H13 H 0.1223 0.7548 0.7455 0.123 Uiso 1 1 calc R A 4 C14 C 0.1127(5) 0.6725(4) 0.6696(5) 0.103(3) Uani 1 1 d GD A 4 H14 H 0.0980 0.7148 0.6338 0.123 Uiso 1 1 calc R A 4 C15 C 0.1200(4) 0.5852(4) 0.6563(4) 0.103(3) Uani 1 1 d GD A 4 H15 H 0.1103 0.5692 0.6115 0.123 Uiso 1 1 calc R A 4 C16 C 0.1419(4) 0.5219(4) 0.7098(4) 0.103(3) Uani 1 1 d GD A 4 H16 H 0.1468 0.4635 0.7009 0.123 Uiso 1 1 calc R A 4 C45 C 0.1669(3) 0.0837(4) 0.9439(3) 0.090(2) Uani 1 1 d GD A 4 H45 H 0.2296 0.0405 0.9446 0.107 Uiso 1 1 calc R A 4 C46 C 0.1509(3) 0.1490(4) 1.0000(3) 0.090(2) Uani 1 1 d GD A 4 H46 H 0.1683 0.2013 0.9864 0.107 Uiso 1 1 calc R A 4 C47 C 0.1029(4) 0.1224(5) 1.0826(3) 0.090(2) Uani 1 1 d GD A 4 H47 H 0.1012 0.1523 1.1264 0.107 Uiso 1 1 calc R A 4 C48 C 0.0604(4) 0.0555(5) 1.0983(4) 0.090(2) Uani 1 1 d GD A 4 H48 H 0.0319 0.0387 1.1519 0.107 Uiso 1 1 calc R A 4 C49 C 0.0597(4) 0.0117(5) 1.0334(4) 0.090(2) Uani 1 1 d GD A 4 C50 C 0.1059(4) 0.0309(5) 0.9545(4) 0.090(2) Uani 1 1 d GD A 4 C1 C 0.4603(12) 0.1127(8) 1.1431(7) 0.051(4) Uani 1 1 d . B 4 H1A H 0.4367 0.1516 1.1903 0.077 Uiso 1 1 calc R B 4 H1B H 0.5318 0.0808 1.1280 0.077 Uiso 1 1 calc R B 4 H1C H 0.4206 0.0717 1.1560 0.077 Uiso 1 1 calc R B 4 C2 C 0.3526(8) 0.2192(6) 1.0886(6) 0.020(2) Uani 1 1 d . B 4 C3 C 0.2651(9) 0.2268(7) 1.1604(6) 0.028(2) Uani 1 1 d . B 4 H3 H 0.2679 0.1905 1.2034 0.033 Uiso 1 1 calc R B 4 C4 C 0.1715(9) 0.2903(9) 1.1674(7) 0.036(3) Uani 1 1 d . B 4 H4 H 0.1128 0.2971 1.2158 0.043 Uiso 1 1 calc R B 4 C5 C 0.1673(9) 0.3409(10) 1.1039(7) 0.038(3) Uani 1 1 d . B 4 H5 H 0.1053 0.3829 1.1100 0.045 Uiso 1 1 calc R B 4 C6 C 0.2535(8) 0.3327(7) 1.0282(6) 0.024(2) Uani 1 1 d . B 4 C7 C 0.3511(7) 0.2697(6) 1.0195(6) 0.017(2) Uani 1 1 d . B 4 C8 C 0.2376(8) 0.3850(9) 0.9639(7) 0.039(3) Uani 1 1 d . B 4 H8 H 0.1743 0.4282 0.9779 0.047 Uiso 1 1 calc R B 4 C10 C 0.1813(15) 0.5094(14) 0.8566(15) 0.103(3) Uani 1 1 d D A 4 C17 C 0.3743(8) 0.4252(8) 0.7455(7) 0.0336(16) Uani 1 1 d . A 4 H17A H 0.3547 0.4322 0.6990 0.040 Uiso 1 1 calc R A 4 H17B H 0.4048 0.4713 0.7453 0.040 Uiso 1 1 calc R A 4 C18 C 0.6282(14) 0.6230(11) 0.8233(10) 0.063(3) Uani 1 1 d . C 4 H18A H 0.6840 0.6052 0.8411 0.095 Uiso 1 1 calc R C 4 H18B H 0.5639 0.6420 0.8703 0.095 Uiso 1 1 calc R C 4 H18C H 0.6362 0.6707 0.7872 0.095 Uiso 1 1 calc R C 4 C19 C 0.7184(8) 0.5109(7) 0.7154(6) 0.0217(9) Uani 1 1 d . B 4 C20 C 0.8059(8) 0.5386(7) 0.6871(6) 0.0217(9) Uani 1 1 d . B 4 H20 H 0.8062 0.5875 0.7125 0.026 Uiso 1 1 calc R B 4 C21 C 0.8948(8) 0.4924(7) 0.6194(6) 0.0217(9) Uani 1 1 d . B 4 H21 H 0.9533 0.5116 0.5994 0.026 Uiso 1 1 calc R B 4 C22 C 0.8949(8) 0.4196(7) 0.5835(6) 0.0217(9) Uani 1 1 d . B 4 H22 H 0.9537 0.3898 0.5389 0.026 Uiso 1 1 calc R B 4 C23 C 0.8066(8) 0.3881(7) 0.6128(6) 0.0217(9) Uani 1 1 d . B 4 C24 C 0.7143(8) 0.4358(7) 0.6783(6) 0.0217(9) Uani 1 1 d . B 4 C25 C 0.8177(8) 0.3082(8) 0.5718(6) 0.024(2) Uani 1 1 d . B 4 H25 H 0.8794 0.2850 0.5268 0.029 Uiso 1 1 calc R B 4 C26 C 0.7681(11) 0.1841(9) 0.5469(9) 0.0537(13) Uani 1 1 d . A 4 C27 C 0.8564(11) 0.1439(9) 0.4879(9) 0.0537(13) Uani 1 1 d . A 4 H27 H 0.9124 0.1657 0.4739 0.064 Uiso 1 1 calc R A 4 C34 C 0.6697(11) 0.1611(10) 0.5717(9) 0.0537(13) Uani 1 1 d . A 4 H34A H 0.6379 0.1853 0.5335 0.064 Uiso 1 1 calc R A 4 H34B H 0.6849 0.0974 0.5685 0.064 Uiso 1 1 calc R A 4 C35 C 0.4601(9) 0.4043(7) 0.3867(6) 0.026(2) Uani 1 1 d . D 4 H35A H 0.4403 0.3744 0.3537 0.039 Uiso 1 1 calc R D 4 H35B H 0.5310 0.4026 0.3576 0.039 Uiso 1 1 calc R D 4 H35C H 0.4176 0.4647 0.3978 0.039 Uiso 1 1 calc R D 4 C36 C 0.3521(7) 0.3542(6) 0.5092(6) 0.0149(19) Uani 1 1 d . B 4 C37 C 0.2651(8) 0.3872(6) 0.4929(7) 0.023(2) Uani 1 1 d . B 4 H37 H 0.2679 0.4214 0.4477 0.028 Uiso 1 1 calc R B 4 C38 C 0.1723(8) 0.3701(6) 0.5436(7) 0.027(2) Uani 1 1 d . B 4 H38 H 0.1150 0.3901 0.5303 0.032 Uiso 1 1 calc R B 4 C39 C 0.1665(8) 0.3234(6) 0.6128(7) 0.022(2) Uani 1 1 d . B 4 H39 H 0.1045 0.3130 0.6465 0.027 Uiso 1 1 calc R B 4 C40 C 0.2514(7) 0.2914(6) 0.6341(6) 0.0170(19) Uani 1 1 d . B 4 C41 C 0.3485(7) 0.3056(6) 0.5809(6) 0.0151(19) Uani 1 1 d . B 4 C42 C 0.2351(7) 0.2474(6) 0.7112(7) 0.019(2) Uani 1 1 d . B 4 H42 H 0.1713 0.2374 0.7386 0.023 Uiso 1 1 calc R B 4 C43 C 0.2735(8) 0.1762(8) 0.8239(7) 0.0336(16) Uani 1 1 d . A 4 H43 H 0.2312 0.2254 0.8649 0.040 Uiso 1 1 calc R A 4 C44 C 0.2124(17) 0.1182(16) 0.8448(13) 0.090(2) Uani 1 1 d . A 4 H44A H 0.2521 0.0657 0.8084 0.107 Uiso 1 1 calc R A 4 H44B H 0.1530 0.1462 0.8317 0.107 Uiso 1 1 calc R A 4 C51 C 0.3713(8) 0.1398(7) 0.8425(6) 0.020(2) Uani 1 1 d . A 4 H51A H 0.3515 0.1447 0.9014 0.024 Uiso 1 1 calc R A 4 H51B H 0.4019 0.0776 0.8253 0.024 Uiso 1 1 calc R A 4 C52 C 0.6208(9) -0.1783(7) 0.5878(8) 0.031(3) Uani 1 1 d . E 4 H52A H 0.6735 -0.1842 0.5332 0.046 Uiso 1 1 calc R E 4 H52B H 0.5546 -0.1645 0.5851 0.046 Uiso 1 1 calc R E 4 H52C H 0.6333 -0.2328 0.6145 0.046 Uiso 1 1 calc R E 4 C53 C 0.7116(8) -0.1188(6) 0.6427(6) 0.019(2) Uani 1 1 d . B 4 C54 C 0.7970(8) -0.1929(6) 0.6162(6) 0.020(2) Uani 1 1 d . B 4 H54 H 0.7957 -0.2403 0.5895 0.024 Uiso 1 1 calc R B 4 C55 C 0.8849(7) -0.1972(6) 0.6293(6) 0.020(2) Uani 1 1 d . B 4 H55 H 0.9414 -0.2477 0.6126 0.024 Uiso 1 1 calc R B 4 C56 C 0.8873(7) -0.1255(6) 0.6674(6) 0.018(2) Uani 1 1 d . B 4 H56 H 0.9461 -0.1284 0.6760 0.022 Uiso 1 1 calc R B 4 C57 C 0.8032(7) -0.0483(6) 0.6933(5) 0.0142(18) Uani 1 1 d . B 4 C58 C 0.7090(7) -0.0449(6) 0.6854(5) 0.0148(19) Uani 1 1 d . B 4 C59 C 0.8173(7) 0.0245(6) 0.7273(6) 0.0166(19) Uani 1 1 d . B 4 H59 H 0.8792 0.0147 0.7332 0.020 Uiso 1 1 calc R B 4 C60 C 0.7732(15) 0.1718(13) 0.7835(14) 0.078(2) Uani 1 1 d . A 4 H60 H 0.8076 0.1976 0.7320 0.094 Uiso 1 1 calc R A 4 C68 C 0.6745(8) 0.2487(6) 0.8218(6) 0.021(2) Uani 1 1 d . . . H68A H 0.6426 0.2417 0.8805 0.025 Uiso 1 1 calc R A 4 H68B H 0.6923 0.3036 0.8142 0.025 Uiso 1 1 calc R A 4 C69 C 0.4822(14) 0.4528(11) 0.9303(10) 0.063(3) Uani 1 1 d . B . H69A H 0.4248 0.4425 0.9762 0.095 Uiso 1 1 calc R . . H69B H 0.4751 0.5149 0.9285 0.095 Uiso 1 1 calc R . . H69C H 0.5451 0.4215 0.9362 0.095 Uiso 1 1 calc R . . C70 C 0.6248(9) 0.3941(8) 0.4953(6) 0.028(2) Uani 1 1 d . B . H70A H 0.6797 0.4111 0.4994 0.042 Uiso 1 1 calc R . . H70B H 0.5834 0.4426 0.4766 0.042 Uiso 1 1 calc R . . H70C H 0.6534 0.3443 0.4568 0.042 Uiso 1 1 calc R . . C71 C 0.4713(11) 0.0596(8) 0.5861(7) 0.037(3) Uani 1 1 d . B . H71A H 0.4123 0.0985 0.5787 0.056 Uiso 1 1 calc R . . H71B H 0.4670 0.0002 0.5897 0.056 Uiso 1 1 calc R . . H71C H 0.5330 0.0622 0.5401 0.056 Uiso 1 1 calc R . . C72 C 0.6261(8) 0.0413(6) 0.9295(6) 0.022(2) Uani 1 1 d . B . H72A H 0.6835 -0.0009 0.8895 0.034 Uiso 1 1 calc R . . H72B H 0.5856 0.0107 0.9720 0.034 Uiso 1 1 calc R . . H72C H 0.6511 0.0768 0.9532 0.034 Uiso 1 1 calc R . . N1 N 0.3012(6) 0.3792(5) 0.8887(5) 0.0166(12) Uani 1 1 d . . . N2 N 0.7500(6) 0.2662(5) 0.5920(5) 0.0176(17) Uani 1 1 d . . . N3 N 0.2992(6) 0.2210(5) 0.7454(5) 0.0166(12) Uani 1 1 d . . . N4 N 0.7513(6) 0.1017(5) 0.7502(4) 0.0125(15) Uani 1 1 d . . . Ni1 Ni 0.44778(9) 0.30562(7) 0.84716(7) 0.0118(3) Uani 1 1 d . A . Ni2 Ni 0.60478(9) 0.31314(7) 0.67425(7) 0.0112(3) Uani 1 1 d . A . Ni3 Ni 0.44486(8) 0.22157(7) 0.69304(7) 0.0106(3) Uani 1 1 d . B . Ni4 Ni 0.60447(9) 0.13215(7) 0.76291(7) 0.0113(3) Uani 1 1 d . A . O1 O 0.4480(6) 0.1630(5) 1.0761(4) 0.0299(18) Uani 1 1 d . . . O2 O 0.4360(5) 0.2582(4) 0.9558(4) 0.0159(13) Uani 1 1 d . . . O3 O 0.4469(5) 0.3425(4) 0.7375(4) 0.0129(13) Uani 1 1 d . . . O4 O 0.6287(6) 0.5499(5) 0.7805(5) 0.0267(16) Uani 1 1 d . . . O5 O 0.6284(5) 0.4173(4) 0.7062(4) 0.0155(13) Uani 1 1 d . . . O6 O 0.5993(5) 0.1940(4) 0.6526(4) 0.0130(13) Uani 1 1 d . . . O7 O 0.4471(5) 0.3617(5) 0.4627(4) 0.0226(15) Uani 1 1 d . . . O8 O 0.4330(5) 0.2751(4) 0.5921(4) 0.0147(13) Uani 1 1 d . . . O9 O 0.4463(5) 0.1848(4) 0.8024(4) 0.0139(13) Uani 1 1 d . . . O10 O 0.6225(6) -0.1090(4) 0.6336(4) 0.0229(15) Uani 1 1 d . . . O11 O 0.6243(5) 0.0184(4) 0.7134(4) 0.0161(14) Uani 1 1 d . . . O12 O 0.6029(5) 0.2535(4) 0.7865(4) 0.0155(13) Uani 1 1 d . A . O13 O 0.4844(6) 0.4244(5) 0.8611(4) 0.0270(16) Uani 1 1 d . . . O14 O 0.5620(5) 0.3708(4) 0.5746(4) 0.0176(14) Uani 1 1 d . . . O15 O 0.4738(5) 0.0855(4) 0.6590(4) 0.0179(14) Uani 1 1 d . . . O16 O 0.5645(5) 0.0959(4) 0.8910(4) 0.0168(14) Uani 1 1 d . . . C61 C 0.8503(15) 0.1523(14) 0.8145(14) 0.078(2) Uani 1 1 d . . . C9 C 0.2772(8) 0.4348(8) 0.8261(7) 0.0336(16) Uani 1 1 d D A . H9 H 0.2490 0.3954 0.8083 0.040 Uiso 1 1 calc R F 4 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 C28 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C29 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C30 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C31 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C32 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C33 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C62 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C63 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C64 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C65 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C66 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C67 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C11 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C12 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C13 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C14 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C15 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C16 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C45 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C46 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C47 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C48 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C49 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C50 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C1 0.075(10) 0.029(7) 0.015(6) 0.007(5) -0.004(6) 0.011(6) C2 0.029(5) 0.015(5) 0.017(5) 0.001(4) -0.003(4) -0.016(4) C3 0.039(6) 0.033(6) 0.012(5) -0.002(4) 0.001(4) -0.027(5) C4 0.026(6) 0.064(8) 0.023(6) 0.001(5) -0.005(5) -0.027(6) C5 0.016(5) 0.077(9) 0.015(5) -0.007(6) 0.000(4) -0.014(6) C6 0.016(5) 0.034(6) 0.016(5) -0.005(4) -0.002(4) -0.006(4) C7 0.017(5) 0.019(5) 0.012(4) -0.008(4) 0.003(4) -0.010(4) C8 0.011(5) 0.070(9) 0.021(6) -0.010(6) -0.005(4) 0.011(5) C10 0.076(5) 0.096(6) 0.138(8) 0.011(6) -0.075(5) 0.016(5) C17 0.021(3) 0.042(4) 0.023(3) 0.002(3) -0.008(3) 0.010(3) C18 0.079(8) 0.059(7) 0.059(7) -0.018(6) -0.019(6) -0.039(6) C19 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C20 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C21 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C22 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C23 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C24 0.028(2) 0.027(2) 0.020(2) 0.0067(17) -0.0110(18) -0.0192(18) C25 0.014(5) 0.045(6) 0.017(5) -0.006(4) 0.002(4) -0.022(5) C26 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C27 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C34 0.047(3) 0.041(2) 0.054(3) -0.023(2) 0.005(2) -0.015(2) C35 0.035(6) 0.033(6) 0.016(5) 0.008(4) -0.016(5) -0.012(5) C36 0.016(5) 0.013(4) 0.018(5) -0.002(4) -0.010(4) -0.001(4) C37 0.033(6) 0.011(4) 0.029(5) -0.003(4) -0.024(5) 0.005(4) C38 0.026(6) 0.014(5) 0.049(7) -0.001(5) -0.029(5) 0.004(4) C39 0.016(5) 0.019(5) 0.037(6) 0.000(4) -0.016(5) -0.004(4) C40 0.016(5) 0.014(4) 0.024(5) 0.002(4) -0.009(4) -0.007(4) C41 0.014(5) 0.010(4) 0.024(5) -0.006(4) -0.014(4) 0.003(4) C42 0.015(5) 0.013(5) 0.036(6) 0.002(4) -0.015(4) -0.006(4) C43 0.021(3) 0.042(4) 0.023(3) 0.002(3) -0.008(3) 0.010(3) C44 0.071(5) 0.103(6) 0.091(6) 0.010(5) -0.016(4) -0.045(5) C51 0.025(5) 0.023(5) 0.018(5) 0.012(4) -0.010(4) -0.015(4) C52 0.038(6) 0.018(5) 0.044(7) -0.005(5) -0.025(6) -0.005(5) C53 0.023(5) 0.016(5) 0.013(5) 0.004(4) -0.004(4) -0.007(4) C54 0.029(5) 0.011(4) 0.014(5) -0.001(4) -0.005(4) -0.002(4) C55 0.014(5) 0.015(5) 0.021(5) -0.003(4) 0.002(4) 0.000(4) C56 0.010(4) 0.023(5) 0.015(5) 0.002(4) 0.002(4) -0.004(4) C57 0.014(4) 0.018(5) 0.007(4) 0.003(3) -0.001(3) -0.006(4) C58 0.014(5) 0.014(4) 0.012(4) 0.005(4) -0.003(4) -0.001(4) C59 0.017(5) 0.018(5) 0.014(5) 0.002(4) -0.008(4) -0.003(4) C60 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C68 0.023(5) 0.018(5) 0.025(5) 0.003(4) -0.012(4) -0.009(4) C69 0.079(8) 0.059(7) 0.059(7) -0.018(6) -0.019(6) -0.039(6) C70 0.030(6) 0.034(6) 0.019(5) 0.003(4) 0.000(4) -0.024(5) C71 0.059(8) 0.028(6) 0.034(6) -0.010(5) -0.036(6) 0.002(6) C72 0.027(5) 0.017(5) 0.016(5) 0.006(4) -0.007(4) -0.001(4) N1 0.015(3) 0.019(3) 0.012(3) -0.004(2) -0.004(2) -0.002(2) N2 0.020(4) 0.021(4) 0.013(4) 0.000(3) -0.005(3) -0.010(3) N3 0.015(3) 0.019(3) 0.012(3) -0.004(2) -0.004(2) -0.002(2) N4 0.016(4) 0.013(4) 0.008(3) 0.006(3) -0.005(3) -0.006(3) Ni1 0.0106(6) 0.0117(6) 0.0095(6) -0.0004(4) -0.0014(4) -0.0019(4) Ni2 0.0117(6) 0.0126(6) 0.0096(5) 0.0003(4) -0.0026(4) -0.0060(4) Ni3 0.0078(5) 0.0131(6) 0.0111(6) 0.0012(4) -0.0037(4) -0.0036(4) Ni4 0.0116(6) 0.0100(5) 0.0124(6) -0.0001(4) -0.0059(5) -0.0019(4) O1 0.040(5) 0.018(4) 0.014(3) 0.005(3) -0.002(3) 0.003(3) O2 0.016(3) 0.019(3) 0.011(3) 0.003(3) -0.002(3) -0.007(3) O3 0.012(3) 0.012(3) 0.013(3) 0.001(2) -0.004(3) -0.002(2) O4 0.029(4) 0.023(4) 0.033(4) -0.009(3) -0.014(3) -0.008(3) O5 0.019(3) 0.017(3) 0.016(3) 0.003(3) -0.009(3) -0.011(3) O6 0.013(3) 0.014(3) 0.011(3) -0.001(2) -0.003(3) -0.004(3) O7 0.020(4) 0.032(4) 0.018(3) 0.014(3) -0.011(3) -0.009(3) O8 0.011(3) 0.015(3) 0.021(3) 0.000(3) -0.009(3) -0.002(3) O9 0.010(3) 0.016(3) 0.012(3) 0.000(3) 0.000(2) -0.006(3) O10 0.029(4) 0.014(3) 0.030(4) -0.005(3) -0.018(3) -0.002(3) O11 0.017(3) 0.017(3) 0.020(3) 0.008(3) -0.011(3) -0.010(3) O12 0.016(3) 0.015(3) 0.014(3) 0.001(3) -0.005(3) -0.004(3) O13 0.032(4) 0.026(4) 0.020(4) -0.009(3) -0.003(3) -0.012(3) O14 0.016(3) 0.025(4) 0.014(3) 0.005(3) -0.008(3) -0.008(3) O15 0.020(3) 0.017(3) 0.021(3) -0.005(3) -0.010(3) -0.007(3) O16 0.021(3) 0.019(3) 0.012(3) 0.004(3) -0.010(3) -0.003(3) C61 0.070(4) 0.084(5) 0.111(6) 0.005(4) -0.057(4) -0.038(4) C9 0.021(3) 0.042(4) 0.023(3) 0.002(3) -0.008(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C28 C29 1.3900 . ? C28 C33 1.3900 . ? C28 C27 1.524(14) . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C62 C63 1.3900 . ? C62 C67 1.3901 . ? C62 C61 1.607(19) . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C11 C10 1.63(2) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C45 C50 1.3616 . ? C45 C46 1.3956 . ? C45 C44 1.73(2) . ? C46 C47 1.4452 . ? C47 C48 1.3496 . ? C48 C49 1.3978 . ? C49 C50 1.3472 . ? C1 O1 1.427(13) . ? C2 O1 1.367(13) . ? C2 C3 1.387(14) . ? C2 C7 1.419(14) . ? C3 C4 1.413(18) . ? C4 C5 1.347(18) . ? C5 C6 1.415(14) . ? C6 C8 1.417(16) . ? C6 C7 1.446(14) . ? C7 O2 1.283(11) . ? C8 N1 1.279(14) . ? C10 C9 1.479(15) . ? C17 O3 1.401(12) . ? C17 C9 1.545(15) . ? C18 O4 1.433(15) . ? C19 O4 1.366(13) . ? C19 C20 1.383(14) . ? C19 C24 1.436(14) . ? C20 C21 1.415(15) . ? C21 C22 1.363(14) . ? C22 C23 1.428(13) . ? C23 C24 1.425(15) . ? C23 C25 1.446(14) . ? C24 O5 1.283(12) . ? C25 N2 1.288(12) . ? C26 C27 1.310(19) . ? C26 N2 1.481(15) . ? C26 C34 1.49(2) . ? C34 O6 1.417(14) . ? C35 O7 1.433(11) . ? C36 O7 1.353(12) . ? C36 C37 1.376(13) . ? C36 C41 1.428(13) . ? C37 C38 1.404(16) . ? C38 C39 1.374(15) . ? C39 C40 1.398(13) . ? C40 C41 1.444(13) . ? C40 C42 1.456(14) . ? C41 O8 1.291(11) . ? C42 N3 1.278(12) . ? C43 C44 1.41(2) . ? C43 N3 1.476(14) . ? C43 C51 1.550(14) . ? C51 O9 1.422(11) . ? C52 O10 1.431(12) . ? C53 O10 1.356(12) . ? C53 C54 1.387(14) . ? C53 C58 1.428(13) . ? C54 C55 1.394(15) . ? C55 C56 1.387(14) . ? C56 C57 1.406(13) . ? C57 C58 1.445(13) . ? C57 C59 1.450(13) . ? C58 O11 1.285(11) . ? C59 N4 1.290(12) . ? C60 C61 1.41(2) . ? C60 N4 1.472(19) . ? C60 C68 1.53(2) . ? C68 O12 1.418(12) . ? C69 O13 1.327(16) . ? C70 O14 1.437(11) . ? C71 O15 1.406(12) . ? C72 O16 1.411(11) . ? N1 C9 1.459(13) . ? N1 Ni1 1.988(8) . ? N2 Ni2 1.999(8) . ? N3 Ni3 1.980(8) . ? N4 Ni4 2.002(8) . ? Ni1 O2 1.979(6) . ? Ni1 O3 1.996(6) . ? Ni1 O12 2.032(6) . ? Ni1 O9 2.143(6) . ? Ni1 O13 2.172(7) . ? Ni2 O5 1.959(6) . ? Ni2 O6 1.993(6) . ? Ni2 O3 2.065(6) . ? Ni2 O12 2.136(6) . ? Ni2 O14 2.165(6) . ? Ni3 O8 1.977(6) . ? Ni3 O9 1.993(6) . ? Ni3 O6 2.018(6) . ? Ni3 O3 2.147(6) . ? Ni3 O15 2.159(6) . ? Ni4 O11 1.962(6) . ? Ni4 O12 1.997(6) . ? Ni4 O9 2.068(6) . ? Ni4 O6 2.144(6) . ? Ni4 O16 2.188(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 C28 C33 120.0 . . ? C29 C28 C27 124.1(7) . . ? C33 C28 C27 115.9(7) . . ? C28 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C28 120.0 . . ? C63 C62 C67 120.0 . . ? C63 C62 C61 146.7(7) . . ? C67 C62 C61 88.7(7) . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C62 120.0 . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 95.6(9) . . ? C16 C11 C10 144.4(9) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C50 C45 C46 126.1 . . ? C50 C45 C44 112.8(7) . . ? C46 C45 C44 110.3(8) . . ? C45 C46 C47 109.1 . . ? C48 C47 C46 122.1 . . ? C47 C48 C49 119.6 . . ? C50 C49 C48 121.7 . . ? C49 C50 C45 113.8 . . ? O1 C2 C3 124.5(10) . . ? O1 C2 C7 112.9(8) . . ? C3 C2 C7 122.6(10) . . ? C2 C3 C4 119.2(10) . . ? C5 C4 C3 120.0(10) . . ? C4 C5 C6 122.6(12) . . ? C5 C6 C8 117.4(10) . . ? C5 C6 C7 118.9(10) . . ? C8 C6 C7 123.7(9) . . ? O2 C7 C2 118.1(9) . . ? O2 C7 C6 125.3(9) . . ? C2 C7 C6 116.6(8) . . ? N1 C8 C6 126.9(10) . . ? C9 C10 C11 106.6(15) . . ? O3 C17 C9 111.1(9) . . ? O4 C19 C20 124.9(9) . . ? O4 C19 C24 113.0(8) . . ? C20 C19 C24 122.1(10) . . ? C19 C20 C21 119.8(9) . . ? C22 C21 C20 120.0(9) . . ? C21 C22 C23 121.4(10) . . ? C24 C23 C22 119.9(9) . . ? C24 C23 C25 124.0(9) . . ? C22 C23 C25 116.2(9) . . ? O5 C24 C23 125.5(9) . . ? O5 C24 C19 117.8(9) . . ? C23 C24 C19 116.7(9) . . ? N2 C25 C23 125.9(9) . . ? C27 C26 N2 123.4(13) . . ? C27 C26 C34 125.8(13) . . ? N2 C26 C34 110.4(10) . . ? C26 C27 C28 120.3(12) . . ? O6 C34 C26 112.1(11) . . ? O7 C36 C37 126.5(9) . . ? O7 C36 C41 112.9(8) . . ? C37 C36 C41 120.6(9) . . ? C36 C37 C38 121.0(9) . . ? C39 C38 C37 119.6(9) . . ? C38 C39 C40 121.7(10) . . ? C39 C40 C41 119.2(9) . . ? C39 C40 C42 117.2(9) . . ? C41 C40 C42 123.6(8) . . ? O8 C41 C36 117.7(9) . . ? O8 C41 C40 124.5(9) . . ? C36 C41 C40 117.7(8) . . ? N3 C42 C40 126.9(9) . . ? C44 C43 N3 123.1(13) . . ? C44 C43 C51 112.7(13) . . ? N3 C43 C51 109.4(9) . . ? C43 C44 C45 120.2(16) . . ? O9 C51 C43 113.0(8) . . ? O10 C53 C54 125.0(9) . . ? O10 C53 C58 113.2(8) . . ? C54 C53 C58 121.8(9) . . ? C53 C54 C55 120.8(9) . . ? C56 C55 C54 119.3(9) . . ? C55 C56 C57 121.7(9) . . ? C56 C57 C58 119.7(9) . . ? C56 C57 C59 116.7(8) . . ? C58 C57 C59 123.6(8) . . ? O11 C58 C53 118.1(8) . . ? O11 C58 C57 125.5(9) . . ? C53 C58 C57 116.4(8) . . ? N4 C59 C57 125.6(9) . . ? C61 C60 N4 121.5(17) . . ? C61 C60 C68 120.5(17) . . ? N4 C60 C68 110.1(12) . . ? O12 C68 C60 112.1(10) . . ? C8 N1 C9 123.2(9) . . ? C8 N1 Ni1 124.1(7) . . ? C9 N1 Ni1 112.3(6) . . ? C25 N2 C26 122.4(9) . . ? C25 N2 Ni2 124.0(7) . . ? C26 N2 Ni2 113.0(7) . . ? C42 N3 C43 121.6(9) . . ? C42 N3 Ni3 124.0(7) . . ? C43 N3 Ni3 113.9(6) . . ? C59 N4 C60 121.5(10) . . ? C59 N4 Ni4 124.4(6) . . ? C60 N4 Ni4 113.2(9) . . ? O2 Ni1 N1 93.8(3) . . ? O2 Ni1 O3 171.6(3) . . ? N1 Ni1 O3 83.5(3) . . ? O2 Ni1 O12 97.6(3) . . ? N1 Ni1 O12 166.6(3) . . ? O3 Ni1 O12 86.1(2) . . ? O2 Ni1 O9 92.4(3) . . ? N1 Ni1 O9 104.0(3) . . ? O3 Ni1 O9 80.6(2) . . ? O12 Ni1 O9 82.6(2) . . ? O2 Ni1 O13 98.0(3) . . ? N1 Ni1 O13 86.7(3) . . ? O3 Ni1 O13 89.8(3) . . ? O12 Ni1 O13 84.7(3) . . ? O9 Ni1 O13 164.6(3) . . ? O5 Ni2 O6 168.5(3) . . ? O5 Ni2 N2 93.6(3) . . ? O6 Ni2 N2 82.2(3) . . ? O5 Ni2 O3 100.5(3) . . ? O6 Ni2 O3 85.2(2) . . ? N2 Ni2 O3 164.0(3) . . ? O5 Ni2 O12 91.1(3) . . ? O6 Ni2 O12 79.8(2) . . ? N2 Ni2 O12 105.5(3) . . ? O3 Ni2 O12 81.8(2) . . ? O5 Ni2 O14 96.8(3) . . ? O6 Ni2 O14 93.8(3) . . ? N2 Ni2 O14 88.5(3) . . ? O3 Ni2 O14 82.5(2) . . ? O12 Ni2 O14 163.5(2) . . ? O8 Ni3 N3 94.4(3) . . ? O8 Ni3 O9 171.8(3) . . ? N3 Ni3 O9 83.8(3) . . ? O8 Ni3 O6 96.7(3) . . ? N3 Ni3 O6 166.1(3) . . ? O9 Ni3 O6 86.3(2) . . ? O8 Ni3 O3 92.3(2) . . ? N3 Ni3 O3 105.5(3) . . ? O9 Ni3 O3 80.6(2) . . ? O6 Ni3 O3 82.5(2) . . ? O8 Ni3 O15 98.3(3) . . ? N3 Ni3 O15 83.7(3) . . ? O9 Ni3 O15 89.4(3) . . ? O6 Ni3 O15 86.3(2) . . ? O3 Ni3 O15 165.4(2) . . ? O11 Ni4 O12 166.7(3) . . ? O11 Ni4 N4 93.6(3) . . ? O12 Ni4 N4 82.7(3) . . ? O11 Ni4 O9 100.1(3) . . ? O12 Ni4 O9 85.4(3) . . ? N4 Ni4 O9 164.5(3) . . ? O11 Ni4 O6 89.3(2) . . ? O12 Ni4 O6 79.5(2) . . ? N4 Ni4 O6 106.2(3) . . ? O9 Ni4 O6 81.3(2) . . ? O11 Ni4 O16 98.8(3) . . ? O12 Ni4 O16 93.8(3) . . ? N4 Ni4 O16 87.9(3) . . ? O9 Ni4 O16 82.9(2) . . ? O6 Ni4 O16 163.3(2) . . ? C2 O1 C1 117.9(9) . . ? C7 O2 Ni1 124.8(6) . . ? C17 O3 Ni1 110.3(6) . . ? C17 O3 Ni2 126.4(6) . . ? Ni1 O3 Ni2 96.9(3) . . ? C17 O3 Ni3 125.7(7) . . ? Ni1 O3 Ni3 99.3(3) . . ? Ni2 O3 Ni3 92.2(2) . . ? C19 O4 C18 116.5(10) . . ? C24 O5 Ni2 126.2(6) . . ? C34 O6 Ni2 110.4(7) . . ? C34 O6 Ni3 124.1(8) . . ? Ni2 O6 Ni3 98.4(3) . . ? C34 O6 Ni4 124.9(8) . . ? Ni2 O6 Ni4 100.2(3) . . ? Ni3 O6 Ni4 93.8(2) . . ? C36 O7 C35 116.9(8) . . ? C41 O8 Ni3 125.6(6) . . ? C51 O9 Ni3 110.0(5) . . ? C51 O9 Ni4 126.6(6) . . ? Ni3 O9 Ni4 96.9(3) . . ? C51 O9 Ni1 125.5(6) . . ? Ni3 O9 Ni1 99.5(3) . . ? Ni4 O9 Ni1 92.3(2) . . ? C53 O10 C52 116.5(8) . . ? C58 O11 Ni4 126.2(6) . . ? C68 O12 Ni4 110.0(5) . . ? C68 O12 Ni1 123.7(6) . . ? Ni4 O12 Ni1 97.8(3) . . ? C68 O12 Ni2 126.1(6) . . ? Ni4 O12 Ni2 100.3(3) . . ? Ni1 O12 Ni2 93.6(3) . . ? C69 O13 Ni1 124.8(9) . . ? C70 O14 Ni2 129.5(6) . . ? C71 O15 Ni3 122.9(6) . . ? C72 O16 Ni4 130.5(6) . . ? C60 C61 C62 110.5(16) . . ? N1 C9 C10 115.8(12) . . ? N1 C9 C17 111.4(8) . . ? C10 C9 C17 128.7(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.1 _refine_diff_density_min -2.1 _refine_diff_density_rms 0.221 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.021 0.343 0.026 10.4 -0.2 2 -0.021 0.657 0.974 10.4 0.2 3 0.323 0.769 0.836 209.0 28.6 4 0.677 0.231 0.164 209.1 31.2 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 956882'