Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name S.Brooker _publ_contact_author_address ; Chemistry Department University of Otago PO Box 56 Dunedin 9001 NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; A [2 2] nickel(II) grid and a copper(II) square result from differing binding modes of a pyrazine-based diamide ligand ; loop_ _publ_author_name 'S. Brooker' 'Kevin J. Berry' 'John F. Boas' 'Peter D. W. Boyd' 'Keith A. Hunter' ; G.B.Jameson ; 'Julia Klingele' 'Boujemaa Moubaraki' 'Keith Murray' 'John Pilbrow' # Attachment 'CUL6SA_squeeze_edited_finalNov06_Rev.cif' data_cul6sa_squeeze _database_code_depnum_ccdc_archive 'CCDC 296868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H76 B4 Cu4 F16 N24 O8' _chemical_formula_weight 2103.04 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 16.152(3) _cell_length_b 16.152(3) _cell_length_c 17.855(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4658(2) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6040 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.25 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; The calculated molar mass, density and absorption coefficient pertain to a formula inferred from microanalysis, which does not include solvate species. A disordered pyridyl group, disordered BF4- anions and unidentified solvate species were not included in the structural model. Final refinements were made with data subjected to SQUEEZE. See "_refine_special_details" below. ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 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 9277 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.1752 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 24.69 _reflns_number_total 3910 _reflns_number_gt 2014 _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 'XP in SHELXTL' _computing_publication_material 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. The overall apparent thermal motion is quite high, leading to a rapid drop-off in intensity at moderate resolution. Refinement died with R1 =0.096, with badly disordered non-coordinated pyridyl, solvent and BF4- moieties. The non-coordinated pyridyl group occupied two different sites with approximately equal occupancy, with substantial librational motions in each site about the methylene linker groups. In addition these sites were alternately occupied by a BF4- counter ion. in view of the serious disorder which could not be properly modelled, the structure was subjected, therefore, to SQUEEZE (AL Spek (1990) Acta Cryst A46, C34), which calculated a void volume of 2,497 A^3^ and 768 electrons per unit cell (I-centring led to SQUEEZE apparently mis-reporting the electron density by a factor of two ie. as 384 electrons; this error was clearly seen by comparison of calc. e count with calc. void volume). Methylene carbon C26 was eliminated for the accurate calculation calculation of the void volume of the attached pyridyl side chain and electron density in the void volume, but this carbon was readily apparent in the subsequent difference Fourier map and was accordingly reincluded in the model. Metrical parameters of the copper complex had improved internal consistency as a result of proper treatment of the disordered components of the structure. Inversion twinning was apparent (minor component 0.195 (32)). ; _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^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(3) _refine_ls_number_reflns 3910 _refine_ls_number_parameters 195 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.005 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 Cu1 Cu 0.45990(6) 0.29998(5) 0.24034(4) 0.0458(3) Uani 1 1 d . . . N1 N 0.5648(3) 0.2342(3) 0.2579(3) 0.0401(14) Uani 1 1 d . . . C2 C 0.6121(6) 0.2198(5) 0.1966(5) 0.050(2) Uani 1 1 d . . . C3 C 0.6795(6) 0.1678(5) 0.1994(4) 0.046(2) Uani 1 1 d . . . N2 N 0.6966(4) 0.1309(4) 0.2664(4) 0.0491(17) Uani 1 1 d . . . C4 C 0.6542(5) 0.1464(5) 0.3250(4) 0.046(2) Uani 1 1 d . . . H4A H 0.6684 0.1205 0.3710 0.055 Uiso 1 1 calc R . . C5 C 0.5889(6) 0.1993(6) 0.3225(4) 0.054(3) Uani 1 1 d . . . H5A H 0.5597 0.2117 0.3673 0.064 Uiso 1 1 calc R . . C6 C 0.5767(6) 0.2684(5) 0.1289(4) 0.050(2) Uani 1 1 d U . . O1 O 0.6176(4) 0.2745(4) 0.0685(3) 0.0742(18) Uani 1 1 d . . . N3 N 0.5048(4) 0.3013(4) 0.1423(3) 0.0417(16) Uani 1 1 d . . . C7 C 0.4705(6) 0.3499(6) 0.0795(5) 0.072(3) Uani 1 1 d . . . H7A H 0.4705 0.3160 0.0333 0.086 Uiso 1 1 calc R . . H7B H 0.5051 0.3995 0.0707 0.086 Uiso 1 1 calc R . . C8 C 0.3812(5) 0.3764(6) 0.0987(4) 0.056(2) Uani 1 1 d . . . H8A H 0.3560 0.4018 0.0537 0.068 Uiso 1 1 calc R . . H8B H 0.3486 0.3264 0.1112 0.068 Uiso 1 1 calc R . . C9 C 0.3751(5) 0.4365(5) 0.1625(5) 0.053(2) Uani 1 1 d . . . C10 C 0.3401(5) 0.5144(7) 0.1558(5) 0.066(3) Uani 1 1 d . . . H10A H 0.3197 0.5327 0.1088 0.080 Uiso 1 1 calc R . . C11 C 0.3351(5) 0.5649(6) 0.2166(6) 0.068(3) Uani 1 1 d . . . H11A H 0.3094 0.6176 0.2127 0.082 Uiso 1 1 calc R . . C12 C 0.3673(5) 0.5394(6) 0.2832(5) 0.060(3) Uani 1 1 d . . . H12A H 0.3665 0.5743 0.3260 0.072 Uiso 1 1 calc R . . C13 C 0.4007(5) 0.4618(6) 0.2859(5) 0.053(2) Uani 1 1 d . . . H13A H 0.4206 0.4431 0.3330 0.063 Uiso 1 1 calc R . . N4 N 0.4073(3) 0.4121(4) 0.2302(4) 0.0421(16) Uani 1 1 d . . . O2 O 0.7883(3) 0.0794(3) 0.1560(3) 0.0456(14) Uani 1 1 d . . . N5 N 0.7371(5) 0.1715(5) 0.0754(4) 0.079(3) Uani 1 1 d . . . H5C H 0.7001 0.2098 0.0651 0.095 Uiso 1 1 calc R . . C26 C 0.7396(5) 0.1374(6) 0.1399(4) 0.047(2) Uani 1 1 d U . . C27 C 0.789(2) 0.1487(18) 0.0268(16) 0.134(10) Uiso 0.50 1 d P . . 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 Cu1 0.0602(7) 0.0490(6) 0.0281(5) 0.0068(5) 0.0026(5) 0.0002(5) N1 0.062(4) 0.044(3) 0.015(3) 0.005(3) 0.002(3) 0.000(3) C2 0.060(7) 0.038(5) 0.051(6) 0.004(4) -0.009(5) -0.001(5) C3 0.056(6) 0.054(6) 0.027(5) -0.001(4) -0.013(4) -0.001(5) N2 0.067(4) 0.051(4) 0.030(4) 0.001(3) 0.002(4) -0.016(3) C4 0.046(6) 0.070(6) 0.022(5) 0.007(4) -0.003(4) 0.016(5) C5 0.061(6) 0.078(7) 0.023(5) -0.021(4) 0.016(4) -0.021(6) C6 0.082(6) 0.051(5) 0.016(4) 0.016(3) 0.003(4) 0.009(4) O1 0.085(5) 0.083(5) 0.054(4) 0.019(3) 0.011(3) 0.041(4) N3 0.046(4) 0.042(4) 0.037(4) 0.012(3) 0.005(3) 0.010(3) C7 0.085(7) 0.081(7) 0.050(5) 0.026(5) 0.005(5) 0.005(6) C8 0.041(6) 0.084(7) 0.044(5) 0.017(5) -0.001(4) 0.006(5) C9 0.051(6) 0.043(6) 0.066(7) 0.003(5) 0.022(5) 0.011(5) C10 0.060(6) 0.088(8) 0.051(6) 0.030(6) 0.015(5) 0.015(5) C11 0.057(6) 0.052(6) 0.094(8) 0.007(6) 0.015(5) 0.021(4) C12 0.059(6) 0.066(7) 0.055(6) 0.001(5) 0.009(5) 0.009(5) C13 0.061(6) 0.053(6) 0.044(6) 0.013(5) 0.009(4) 0.010(5) N4 0.040(4) 0.056(4) 0.030(4) -0.008(4) 0.003(3) -0.008(3) O2 0.047(3) 0.052(4) 0.037(3) -0.002(2) -0.006(3) 0.001(3) N5 0.080(6) 0.120(7) 0.036(4) 0.032(4) 0.042(4) 0.050(5) C26 0.055(5) 0.069(5) 0.016(4) 0.006(4) -0.009(4) 0.001(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 Cu1 N3 1.895(6) . ? Cu1 O2 1.966(5) 8_545 ? Cu1 N4 2.009(6) . ? Cu1 N1 2.024(6) . ? Cu1 N2 2.226(7) 8_545 ? N1 C5 1.342(10) . ? N1 C2 1.355(10) . ? C2 C3 1.375(12) . ? C2 C6 1.551(11) . ? C3 N2 1.365(9) . ? C3 C26 1.521(11) . ? N2 C4 1.275(9) . ? N2 Cu1 2.226(7) 7 ? C4 C5 1.358(12) . ? C6 O1 1.268(9) . ? C6 N3 1.299(9) . ? N3 C7 1.476(9) . ? C7 C8 1.542(12) . ? C8 C9 1.499(11) . ? C9 N4 1.375(10) . ? C9 C10 1.385(11) . ? C10 C11 1.360(12) . ? C11 C12 1.360(12) . ? C12 C13 1.366(11) . ? C13 N4 1.282(9) . ? O2 C26 1.256(9) . ? O2 Cu1 1.966(5) 7 ? N5 C27 1.26(3) . ? N5 C26 1.278(9) . ? 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 N3 Cu1 O2 174.0(2) . 8_545 ? N3 Cu1 N4 93.9(3) . . ? O2 Cu1 N4 92.0(2) 8_545 . ? N3 Cu1 N1 80.1(3) . . ? O2 Cu1 N1 94.3(2) 8_545 . ? N4 Cu1 N1 147.2(2) . . ? N3 Cu1 N2 102.1(3) . 8_545 ? O2 Cu1 N2 76.5(2) 8_545 8_545 ? N4 Cu1 N2 113.1(2) . 8_545 ? N1 Cu1 N2 99.6(2) . 8_545 ? C5 N1 C2 117.2(6) . . ? C5 N1 Cu1 126.6(5) . . ? C2 N1 Cu1 116.0(5) . . ? N1 C2 C3 121.5(7) . . ? N1 C2 C6 109.5(7) . . ? C3 C2 C6 129.0(8) . . ? N2 C3 C2 117.3(7) . . ? N2 C3 C26 110.0(7) . . ? C2 C3 C26 132.6(7) . . ? C4 N2 C3 121.7(7) . . ? C4 N2 Cu1 125.2(6) . 7 ? C3 N2 Cu1 113.1(5) . 7 ? N2 C4 C5 120.9(7) . . ? N1 C5 C4 121.3(7) . . ? O1 C6 N3 126.2(7) . . ? O1 C6 C2 120.6(8) . . ? N3 C6 C2 113.2(7) . . ? C6 N3 C7 114.4(6) . . ? C6 N3 Cu1 120.5(5) . . ? C7 N3 Cu1 124.3(5) . . ? N3 C7 C8 109.3(6) . . ? C9 C8 C7 114.2(7) . . ? N4 C9 C10 119.3(8) . . ? N4 C9 C8 117.3(7) . . ? C10 C9 C8 123.4(9) . . ? C11 C10 C9 120.0(8) . . ? C10 C11 C12 119.6(8) . . ? C11 C12 C13 117.3(9) . . ? N4 C13 C12 125.5(8) . . ? C13 N4 C9 118.1(7) . . ? C13 N4 Cu1 122.0(6) . . ? C9 N4 Cu1 119.8(5) . . ? C26 O2 Cu1 121.1(5) . 7 ? C27 N5 C26 118.2(15) . . ? O2 C26 N5 123.2(8) . . ? O2 C26 C3 118.7(7) . . ? N5 C26 C3 118.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C5 -177.8(6) . . . . ? O2 Cu1 N1 C5 0.0(6) 8_545 . . . ? N4 Cu1 N1 C5 100.3(7) . . . . ? N2 Cu1 N1 C5 -77.0(6) 8_545 . . . ? N3 Cu1 N1 C2 -2.6(5) . . . . ? O2 Cu1 N1 C2 175.1(5) 8_545 . . . ? N4 Cu1 N1 C2 -84.5(7) . . . . ? N2 Cu1 N1 C2 98.1(5) 8_545 . . . ? C5 N1 C2 C3 3.4(11) . . . . ? Cu1 N1 C2 C3 -172.2(6) . . . . ? C5 N1 C2 C6 -177.4(6) . . . . ? Cu1 N1 C2 C6 7.0(8) . . . . ? N1 C2 C3 N2 0.4(12) . . . . ? C6 C2 C3 N2 -178.7(7) . . . . ? N1 C2 C3 C26 176.3(8) . . . . ? C6 C2 C3 C26 -2.7(15) . . . . ? C2 C3 N2 C4 -2.8(11) . . . . ? C26 C3 N2 C4 -179.6(7) . . . . ? C2 C3 N2 Cu1 174.7(6) . . . 7 ? C26 C3 N2 Cu1 -2.1(8) . . . 7 ? C3 N2 C4 C5 1.3(12) . . . . ? Cu1 N2 C4 C5 -175.9(6) 7 . . . ? C2 N1 C5 C4 -5.0(11) . . . . ? Cu1 N1 C5 C4 170.1(6) . . . . ? N2 C4 C5 N1 2.8(13) . . . . ? N1 C2 C6 O1 169.3(7) . . . . ? C3 C2 C6 O1 -11.6(13) . . . . ? N1 C2 C6 N3 -9.6(9) . . . . ? C3 C2 C6 N3 169.5(8) . . . . ? O1 C6 N3 C7 -0.3(12) . . . . ? C2 C6 N3 C7 178.5(7) . . . . ? O1 C6 N3 Cu1 -170.5(7) . . . . ? C2 C6 N3 Cu1 8.3(9) . . . . ? O2 Cu1 N3 C6 -25(3) 8_545 . . . ? N4 Cu1 N3 C6 143.9(6) . . . . ? N1 Cu1 N3 C6 -3.6(6) . . . . ? N2 Cu1 N3 C6 -101.4(6) 8_545 . . . ? O2 Cu1 N3 C7 166(2) 8_545 . . . ? N4 Cu1 N3 C7 -25.3(6) . . . . ? N1 Cu1 N3 C7 -172.8(6) . . . . ? N2 Cu1 N3 C7 89.4(6) 8_545 . . . ? C6 N3 C7 C8 173.2(7) . . . . ? Cu1 N3 C7 C8 -17.0(10) . . . . ? N3 C7 C8 C9 66.5(10) . . . . ? C7 C8 C9 N4 -58.3(10) . . . . ? C7 C8 C9 C10 120.7(9) . . . . ? N4 C9 C10 C11 -2.5(12) . . . . ? C8 C9 C10 C11 178.6(8) . . . . ? C9 C10 C11 C12 2.3(13) . . . . ? C10 C11 C12 C13 -2.4(13) . . . . ? C11 C12 C13 N4 3.0(14) . . . . ? C12 C13 N4 C9 -3.2(13) . . . . ? C12 C13 N4 Cu1 178.6(6) . . . . ? C10 C9 N4 C13 2.8(11) . . . . ? C8 C9 N4 C13 -178.2(7) . . . . ? C10 C9 N4 Cu1 -179.0(6) . . . . ? C8 C9 N4 Cu1 0.0(9) . . . . ? N3 Cu1 N4 C13 -146.4(6) . . . . ? O2 Cu1 N4 C13 32.4(6) 8_545 . . . ? N1 Cu1 N4 C13 -68.6(8) . . . . ? N2 Cu1 N4 C13 108.6(6) 8_545 . . . ? N3 Cu1 N4 C9 35.4(6) . . . . ? O2 Cu1 N4 C9 -145.7(5) 8_545 . . . ? N1 Cu1 N4 C9 113.2(6) . . . . ? N2 Cu1 N4 C9 -69.6(6) 8_545 . . . ? Cu1 O2 C26 N5 171.4(6) 7 . . . ? Cu1 O2 C26 C3 -9.6(9) 7 . . . ? C27 N5 C26 O2 -4(2) . . . . ? C27 N5 C26 C3 177.2(17) . . . . ? N2 C3 C26 O2 7.3(10) . . . . ? C2 C3 C26 O2 -168.9(8) . . . . ? N2 C3 C26 N5 -173.7(8) . . . . ? C2 C3 C26 N5 10.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.281 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.069 # Attachment 'H2L6CUfinalNov06.CIF' data_h2l6cu _database_code_depnum_ccdc_archive 'CCDC 296869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21.50 H22 B1.50 Cu F6 N6.75 O2.13' _chemical_formula_weight 602.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9483(2) _cell_length_b 14.1741(2) _cell_length_c 26.0046(2) _cell_angle_alpha 82.3380(10) _cell_angle_beta 86.1350(10) _cell_angle_gamma 87.7230(10) _cell_volume 5081.28(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6588 _cell_measurement_theta_min 0.79 _cell_measurement_theta_max 25.11 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2446 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17828 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 25.11 _reflns_number_total 17828 _reflns_number_gt 14155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 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^)+(0.1235P)^2^+16.5502P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17828 _refine_ls_number_parameters 1480 _refine_ls_number_restraints 339 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1976 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.66880(5) 0.79131(5) 0.29076(3) 0.02623(19) Uani 1 1 d . . . Cu2 Cu 0.93333(5) 0.37169(5) 0.24775(3) 0.02904(19) Uani 1 1 d . . . Cu3 Cu 0.50529(5) 0.13397(5) 0.24052(2) 0.02472(18) Uani 1 1 d . . . Cu4 Cu 0.24920(5) 0.56974(5) 0.23954(2) 0.02487(18) Uani 1 1 d . . . N1 N 0.5445(3) 0.7441(3) 0.26824(18) 0.0270(10) Uani 1 1 d . . . N2 N 0.5969(3) 0.7757(4) 0.35648(18) 0.0295(11) Uani 1 1 d . . . N3 N 0.7627(4) 0.8788(4) 0.31308(19) 0.0301(11) Uani 1 1 d . . . N4 N 0.3837(3) 0.6555(3) 0.24795(18) 0.0277(10) Uani 1 1 d . . . N5 N 0.3093(4) 0.6384(4) 0.38316(19) 0.0340(12) Uani 1 1 d . . . H5C H 0.3558 0.6755 0.3920 0.041 Uiso 1 1 d . . . N6 N 0.3209(5) 0.6462(4) 0.5431(2) 0.0504(16) Uani 1 1 d . . . O1 O 0.4533(3) 0.7359(3) 0.39995(16) 0.0394(11) Uani 1 1 d . . . O2 O 0.2537(3) 0.5814(3) 0.31488(15) 0.0278(9) Uani 1 1 d . . . C1 C 0.5307(4) 0.7292(4) 0.2200(2) 0.0305(13) Uani 1 1 d . . . H1 H 0.5768 0.7489 0.1925 0.037 Uiso 1 1 calc R . . C2 C 0.4487(4) 0.6846(5) 0.2102(2) 0.0317(13) Uani 1 1 d . . . H2 H 0.4387 0.6747 0.1755 0.038 Uiso 1 1 calc R . . C3 C 0.3972(4) 0.6711(4) 0.2975(2) 0.0257(12) Uani 1 1 d . . . C4 C 0.4793(4) 0.7175(4) 0.3080(2) 0.0252(12) Uani 1 1 d . . . C5 C 0.5090(4) 0.7439(4) 0.3600(2) 0.0272(12) Uani 1 1 d . . . C6 C 0.6346(5) 0.8028(5) 0.4038(2) 0.0321(13) Uani 1 1 d . . . H6A H 0.6071 0.7620 0.4347 0.038 Uiso 1 1 calc R . . H6B H 0.6153 0.8698 0.4072 0.038 Uiso 1 1 calc R . . C7 C 0.7433(5) 0.7920(4) 0.4014(2) 0.0339(14) Uani 1 1 d . . . H7A H 0.7657 0.7977 0.4361 0.041 Uiso 1 1 calc R . . H7B H 0.7619 0.7272 0.3933 0.041 Uiso 1 1 calc R . . C8 C 0.7941(4) 0.8638(4) 0.3617(2) 0.0319(13) Uani 1 1 d . . . C9 C 0.8706(5) 0.9147(5) 0.3746(3) 0.0423(16) Uani 1 1 d . . . H9 H 0.8936 0.9023 0.4084 0.051 Uiso 1 1 calc R . . C10 C 0.9126(5) 0.9824(5) 0.3386(3) 0.0459(17) Uani 1 1 d . . . H10 H 0.9654 1.0163 0.3472 0.055 Uiso 1 1 calc R . . C11 C 0.8776(5) 1.0011(5) 0.2897(3) 0.0417(16) Uani 1 1 d . . . H11 H 0.9042 1.0494 0.2646 0.050 Uiso 1 1 calc R . . C12 C 0.8026(5) 0.9473(4) 0.2783(3) 0.0354(14) Uani 1 1 d . . . H12 H 0.7785 0.9594 0.2446 0.043 Uiso 1 1 calc R . . C13 C 0.3158(4) 0.6280(4) 0.3336(2) 0.0269(12) Uani 1 1 d . . . C14 C 0.2288(5) 0.5982(5) 0.4173(2) 0.0392(15) Uani 1 1 d . . . H14A H 0.2353 0.5279 0.4216 0.047 Uiso 1 1 calc R . . H14B H 0.1677 0.6169 0.4009 0.047 Uiso 1 1 calc R . . C15 C 0.2255(5) 0.6323(5) 0.4705(2) 0.0385(15) Uani 1 1 d . . . H15A H 0.2308 0.7024 0.4653 0.046 Uiso 1 1 calc R . . H15B H 0.1616 0.6179 0.4882 0.046 Uiso 1 1 calc R . . C16 C 0.3016(5) 0.5906(5) 0.5067(2) 0.0365(14) Uani 1 1 d . . . C17 C 0.3442(5) 0.5018(5) 0.5072(3) 0.0450(17) Uani 1 1 d . . . H17 H 0.3306 0.4630 0.4817 0.054 Uiso 1 1 calc R . . C18 C 0.4074(6) 0.4685(5) 0.5450(3) 0.0513(19) Uani 1 1 d . . . H18 H 0.4377 0.4073 0.5451 0.062 Uiso 1 1 calc R . . C19 C 0.4261(6) 0.5246(6) 0.5828(3) 0.055(2) Uani 1 1 d . . . H19 H 0.4677 0.5023 0.6095 0.066 Uiso 1 1 calc R . . C20 C 0.3830(7) 0.6125(6) 0.5801(3) 0.059(2) Uani 1 1 d . . . H20 H 0.3966 0.6524 0.6051 0.070 Uiso 1 1 calc R . . N7 N 0.8669(3) 0.4915(3) 0.27179(18) 0.0256(10) Uani 1 1 d . . . N8 N 0.9566(3) 0.4593(3) 0.1858(2) 0.0298(11) Uani 1 1 d . . . N9 N 1.0341(4) 0.2738(4) 0.2277(2) 0.0365(12) Uani 1 1 d . . . N10 N 0.7640(3) 0.6538(3) 0.28998(17) 0.0265(10) Uani 1 1 d . . . N11 N 0.8558(4) 0.7627(3) 0.16654(19) 0.0320(11) Uani 1 1 d . . . H11C H 0.9005 0.7109 0.1599 0.038 Uiso 1 1 d . . . N12 N 0.8443(4) 0.6795(4) 0.0463(2) 0.0394(13) Uani 1 1 d . . . O3 O 0.9666(3) 0.6175(3) 0.15545(18) 0.0392(11) Uani 1 1 d . . . O4 O 0.7320(3) 0.7996(3) 0.22081(15) 0.0288(9) Uani 1 1 d . . . C21 C 0.8162(4) 0.4958(4) 0.3165(2) 0.0306(13) Uani 1 1 d . . . H21 H 0.8147 0.4418 0.3424 0.037 Uiso 1 1 calc R . . C22 C 0.7653(5) 0.5788(4) 0.3256(2) 0.0316(13) Uani 1 1 d . . . H22 H 0.7308 0.5813 0.3581 0.038 Uiso 1 1 calc R . . C23 C 0.8161(4) 0.6512(4) 0.2445(2) 0.0227(11) Uani 1 1 d . . . C24 C 0.8709(4) 0.5688(4) 0.2351(2) 0.0244(11) Uani 1 1 d . . . C25 C 0.9360(4) 0.5506(4) 0.1878(2) 0.0296(13) Uani 1 1 d . . . C26 C 1.0180(5) 0.4355(5) 0.1413(3) 0.0393(15) Uani 1 1 d . . . H26A H 1.0853 0.4505 0.1459 0.047 Uiso 1 1 calc R . . H26B H 0.9974 0.4745 0.1092 0.047 Uiso 1 1 calc R . . C27 C 1.0124(5) 0.3302(5) 0.1357(3) 0.0417(16) Uani 1 1 d . . . H27A H 0.9440 0.3140 0.1361 0.050 Uiso 1 1 calc R . . H27B H 1.0433 0.3192 0.1015 0.050 Uiso 1 1 calc R . . C28 C 1.0597(5) 0.2640(5) 0.1777(3) 0.0403(16) Uani 1 1 d . . . C29 C 1.1259(6) 0.1934(5) 0.1650(4) 0.056(2) Uani 1 1 d . . . H29 H 1.1429 0.1871 0.1296 0.067 Uiso 1 1 calc R . . C30 C 1.1669(7) 0.1323(6) 0.2042(5) 0.078(3) Uani 1 1 d . . . H30 H 1.2109 0.0826 0.1961 0.093 Uiso 1 1 calc R . . C31 C 1.1428(6) 0.1450(6) 0.2543(4) 0.069(3) Uani 1 1 d . . . H31 H 1.1719 0.1055 0.2818 0.083 Uiso 1 1 calc R . . C32 C 1.0760(5) 0.2151(5) 0.2656(4) 0.0519(19) Uani 1 1 d . . . H32 H 1.0592 0.2223 0.3009 0.062 Uiso 1 1 calc R . . C33 C 0.7993(4) 0.7435(4) 0.2083(2) 0.0248(12) Uani 1 1 d . . . C34 C 0.8452(5) 0.8518(4) 0.1311(2) 0.0368(14) Uani 1 1 d . . . H34A H 0.9071 0.8847 0.1262 0.044 Uiso 1 1 calc R . . H34B H 0.7965 0.8944 0.1464 0.044 Uiso 1 1 calc R . . C35 C 0.8147(5) 0.8309(5) 0.0790(3) 0.0392(15) Uani 1 1 d . . . H35A H 0.7491 0.8056 0.0835 0.047 Uiso 1 1 calc R . . H35B H 0.8127 0.8909 0.0547 0.047 Uiso 1 1 calc R . . C36 C 0.8825(5) 0.7596(5) 0.0559(2) 0.0352(14) Uani 1 1 d . . . C37 C 0.9803(5) 0.7758(5) 0.0465(2) 0.0415(16) Uani 1 1 d . . . H37 H 1.0059 0.8334 0.0538 0.050 Uiso 1 1 calc R . . C38 C 1.0398(5) 0.7077(6) 0.0264(3) 0.0456(17) Uani 1 1 d . . . H38 H 1.1069 0.7169 0.0204 0.055 Uiso 1 1 calc R . . C39 C 1.0000(6) 0.6265(6) 0.0155(3) 0.055(2) Uani 1 1 d . . . H39 H 1.0389 0.5790 0.0009 0.066 Uiso 1 1 calc R . . C40 C 0.9019(5) 0.6144(6) 0.0260(3) 0.0493(18) Uani 1 1 d . . . H40 H 0.8748 0.5578 0.0184 0.059 Uiso 1 1 calc R . . N13 N 0.6341(3) 0.1991(3) 0.23441(17) 0.0233(10) Uani 1 1 d . . . N14 N 0.5463(4) 0.0962(3) 0.30995(18) 0.0271(10) Uani 1 1 d . . . N15 N 0.4111(3) 0.0292(3) 0.24555(19) 0.0289(11) Uani 1 1 d . . . N16 N 0.8015(3) 0.2925(3) 0.23656(18) 0.0257(10) Uani 1 1 d . . . N17 N 0.8156(4) 0.1900(4) 0.3686(2) 0.0402(13) Uani 1 1 d . . . H17C H 0.7626 0.1526 0.3737 0.048 Uiso 1 1 d . . . N18 N 0.6966(6) 0.1622(4) 0.4787(2) 0.0501(16) Uani 1 1 d . . . H18C H 0.7118 0.2270 0.4690 0.060 Uiso 1 1 d . . . O5 O 0.6698(3) 0.0899(3) 0.36325(16) 0.0371(10) Uani 1 1 d . . . O6 O 0.9011(3) 0.2975(3) 0.31609(16) 0.0315(9) Uani 1 1 d . . . C41 C 0.6675(4) 0.2555(4) 0.1933(2) 0.0277(12) Uani 1 1 d . . . H41 H 0.6329 0.2640 0.1627 0.033 Uiso 1 1 calc R . . C42 C 0.7523(4) 0.3026(4) 0.1940(2) 0.0281(12) Uani 1 1 d . . . H42 H 0.7757 0.3424 0.1639 0.034 Uiso 1 1 calc R . . C43 C 0.7684(4) 0.2355(4) 0.2792(2) 0.0244(11) Uani 1 1 d . . . C44 C 0.6827(4) 0.1858(4) 0.2786(2) 0.0240(11) Uani 1 1 d . . . C45 C 0.6318(4) 0.1190(4) 0.3211(2) 0.0262(12) Uani 1 1 d . . . C46 C 0.4911(5) 0.0358(5) 0.3499(2) 0.0321(13) Uani 1 1 d . . . H46A H 0.4977 0.0577 0.3841 0.039 Uiso 1 1 calc R . . H46B H 0.5172 -0.0304 0.3517 0.039 Uiso 1 1 calc R . . C47 C 0.3856(5) 0.0380(4) 0.3389(2) 0.0330(13) Uani 1 1 d . . . H47A H 0.3491 0.0041 0.3693 0.040 Uiso 1 1 calc R . . H47B H 0.3614 0.1050 0.3342 0.040 Uiso 1 1 calc R . . C48 C 0.3676(4) -0.0066(4) 0.2915(2) 0.0309(13) Uani 1 1 d . . . C49 C 0.3080(5) -0.0835(5) 0.2949(3) 0.0425(16) Uani 1 1 d . . . H49 H 0.2790 -0.1097 0.3275 0.051 Uiso 1 1 calc R . . C50 C 0.2912(5) -0.1216(5) 0.2499(3) 0.0473(18) Uani 1 1 d . . . H50 H 0.2488 -0.1729 0.2513 0.057 Uiso 1 1 calc R . . C51 C 0.3359(5) -0.0850(5) 0.2034(3) 0.0413(16) Uani 1 1 d . . . H51 H 0.3257 -0.1108 0.1724 0.050 Uiso 1 1 calc R . . C52 C 0.3952(5) -0.0107(4) 0.2026(3) 0.0350(14) Uani 1 1 d . . . H52 H 0.4269 0.0141 0.1705 0.042 Uiso 1 1 calc R . . C53 C 0.8333(4) 0.2409(4) 0.3235(2) 0.0280(12) Uani 1 1 d . . . C54 C 0.8752(6) 0.1987(6) 0.4129(3) 0.058(2) Uani 1 1 d . . . H54A H 0.8557 0.2577 0.4279 0.069 Uiso 1 1 calc R . . H54B H 0.9436 0.2035 0.4002 0.069 Uiso 1 1 calc R . . C55 C 0.8644(7) 0.1151(6) 0.4542(3) 0.064(2) Uani 1 1 d . . . H55A H 0.8920 0.0580 0.4398 0.077 Uiso 1 1 calc R . . H55B H 0.9034 0.1256 0.4832 0.077 Uiso 1 1 calc R . . C56 C 0.7656(7) 0.0941(6) 0.4757(2) 0.054(2) Uani 1 1 d . . . C57 C 0.7367(10) -0.0008(7) 0.4957(3) 0.081(3) Uani 1 1 d . . . H57 H 0.7800 -0.0535 0.4927 0.097 Uiso 1 1 calc R . . C58 C 0.6484(10) -0.0147(7) 0.5186(3) 0.083(4) Uani 1 1 d . . . H58 H 0.6307 -0.0770 0.5333 0.099 Uiso 1 1 calc R . . C59 C 0.5842(10) 0.0595(7) 0.5210(4) 0.084(3) Uani 1 1 d . . . H59 H 0.5217 0.0491 0.5372 0.101 Uiso 1 1 calc R . . C60 C 0.6091(8) 0.1465(6) 0.5005(3) 0.064(2) Uani 1 1 d . . . H60 H 0.5638 0.1981 0.5016 0.076 Uiso 1 1 calc R . . N19 N 0.3150(3) 0.4390(3) 0.24697(17) 0.0236(10) Uani 1 1 d . . . N20 N 0.2557(3) 0.5465(3) 0.16814(18) 0.0253(10) Uani 1 1 d . . . N21 N 0.1518(3) 0.6779(3) 0.22850(19) 0.0276(10) Uani 1 1 d . . . N22 N 0.4129(3) 0.2680(3) 0.24793(17) 0.0247(10) Uani 1 1 d . . . N23 N 0.3784(3) 0.2767(3) 0.11337(17) 0.0266(10) Uani 1 1 d . . . H23C H 0.3388 0.3329 0.1109 0.032 Uiso 1 1 d . . . N24 N 0.3451(4) 0.3659(4) -0.05378(19) 0.0334(11) Uani 1 1 d . . . H24C H 0.2740 0.3495 -0.0574 0.040 Uiso 1 1 d . . . O7 O 0.2833(3) 0.4348(3) 0.11260(15) 0.0316(9) Uani 1 1 d . . . O8 O 0.4694(3) 0.1836(3) 0.16865(14) 0.0269(8) Uani 1 1 d . . . C61 C 0.3474(4) 0.3946(4) 0.2907(2) 0.0291(13) Uani 1 1 d . . . H61 H 0.3366 0.4226 0.3219 0.035 Uiso 1 1 calc R . . C62 C 0.3969(4) 0.3079(4) 0.2916(2) 0.0301(13) Uani 1 1 d . . . H62 H 0.4194 0.2766 0.3233 0.036 Uiso 1 1 calc R . . C63 C 0.3812(4) 0.3123(4) 0.2031(2) 0.0211(11) Uani 1 1 d . . . C64 C 0.3298(4) 0.4000(4) 0.2019(2) 0.0234(11) Uani 1 1 d . . . C65 C 0.2870(4) 0.4633(4) 0.1564(2) 0.0234(11) Uani 1 1 d . . . C66 C 0.2149(4) 0.6139(4) 0.1261(2) 0.0281(12) Uani 1 1 d . . . H66A H 0.1473 0.5984 0.1224 0.034 Uiso 1 1 calc R . . H66B H 0.2516 0.6077 0.0927 0.034 Uiso 1 1 calc R . . C67 C 0.2192(4) 0.7161(4) 0.1384(2) 0.0308(13) Uani 1 1 d . . . H67A H 0.2858 0.7279 0.1462 0.037 Uiso 1 1 calc R . . H67B H 0.2035 0.7604 0.1071 0.037 Uiso 1 1 calc R . . C68 C 0.1523(4) 0.7384(4) 0.1834(2) 0.0295(13) Uani 1 1 d . . . C69 C 0.0943(5) 0.8206(5) 0.1793(3) 0.0369(14) Uani 1 1 d . . . H69 H 0.0962 0.8631 0.1477 0.044 Uiso 1 1 calc R . . C70 C 0.0338(5) 0.8409(5) 0.2211(3) 0.0443(16) Uani 1 1 d . . . H70 H -0.0042 0.8983 0.2190 0.053 Uiso 1 1 calc R . . C71 C 0.0295(5) 0.7754(5) 0.2664(3) 0.0423(16) Uani 1 1 d . . . H71 H -0.0141 0.7856 0.2950 0.051 Uiso 1 1 calc R . . C72 C 0.0897(4) 0.6959(5) 0.2688(2) 0.0341(14) Uani 1 1 d . . . H72 H 0.0878 0.6519 0.2997 0.041 Uiso 1 1 calc R . . C73 C 0.4129(4) 0.2539(4) 0.1591(2) 0.0221(11) Uani 1 1 d . . . C74 C 0.3977(5) 0.2140(4) 0.0725(2) 0.0344(14) Uani 1 1 d . . . H74A H 0.3754 0.1492 0.0856 0.041 Uiso 1 1 calc R . . H74B H 0.4677 0.2094 0.0637 0.041 Uiso 1 1 calc R . . C75 C 0.3461(5) 0.2532(5) 0.0241(2) 0.0347(14) Uani 1 1 d . . . H75A H 0.3353 0.1995 0.0047 0.042 Uiso 1 1 calc R . . H75B H 0.2821 0.2787 0.0354 0.042 Uiso 1 1 calc R . . C76 C 0.3955(4) 0.3299(4) -0.0127(2) 0.0309(13) Uani 1 1 d . . . C77 C 0.4880(5) 0.3608(5) -0.0103(3) 0.0416(16) Uani 1 1 d . . . H77 H 0.5247 0.3374 0.0184 0.050 Uiso 1 1 calc R . . C78 C 0.5267(5) 0.4260(6) -0.0500(3) 0.0492(18) Uani 1 1 d . . . H78 H 0.5898 0.4477 -0.0483 0.059 Uiso 1 1 calc R . . C79 C 0.4740(6) 0.4594(5) -0.0920(3) 0.0499(18) Uani 1 1 d . . . H79 H 0.5009 0.5025 -0.1199 0.060 Uiso 1 1 calc R . . C80 C 0.3816(6) 0.4291(5) -0.0927(3) 0.0464(17) Uani 1 1 d . . . H80 H 0.3434 0.4529 -0.1208 0.056 Uiso 1 1 calc R . . B1 B 0.5952(4) 0.4737(4) 0.2531(2) 0.0345(16) Uani 1 1 d D . . F11 F 0.5425(4) 0.5243(3) 0.28674(17) 0.0648(14) Uani 1 1 d D . . F12 F 0.5337(3) 0.4437(3) 0.21788(16) 0.0576(12) Uani 1 1 d D . . F13 F 0.6654(3) 0.5220(4) 0.22601(17) 0.0658(14) Uani 1 1 d D . . F14 F 0.6313(3) 0.3916(3) 0.28288(16) 0.0584(12) Uani 1 1 d D . . B2 B 0.5052(6) 0.1384(5) -0.0760(3) 0.047(2) Uani 1 1 d D . . F21 F 0.5335(9) 0.0525(7) -0.0923(5) 0.200(5) Uani 1 1 d D . . F22 F 0.5093(10) 0.1207(7) -0.0224(3) 0.191(5) Uani 1 1 d D . . F23 F 0.4310(7) 0.1757(7) -0.0977(3) 0.166(4) Uani 1 1 d D . . F24 F 0.5755(8) 0.2051(8) -0.0944(4) 0.193(5) Uani 1 1 d D . . B3 B 0.1914(9) 0.0203(11) 0.0578(4) 0.053(3) Uani 0.73 1 d P A 1 F31 F 0.1612(5) 0.1161(4) 0.0501(2) 0.0535(15) Uani 0.73 1 d P A 1 F32 F 0.1145(8) -0.0356(6) 0.0652(5) 0.133(5) Uani 0.73 1 d P A 1 F33 F 0.2491(10) 0.0027(10) 0.0166(3) 0.181(7) Uani 0.73 1 d P A 1 F34 F 0.2391(7) 0.0035(7) 0.1017(3) 0.097(3) Uani 0.73 1 d P A 1 B3' B -0.0663(9) 0.5529(9) 0.4344(5) 0.044(7) Uani 0.27 1 d PD B 2 F35 F -0.0516(9) 0.6065(8) 0.3878(4) 0.038(3) Uani 0.27 1 d PD B 2 F36 F -0.1110(8) 0.4666(8) 0.4266(4) 0.037(3) Uani 0.27 1 d PD B 2 F37 F 0.0078(9) 0.5344(9) 0.4611(5) 0.047(4) Uani 0.27 1 d PD B 2 F38 F -0.1377(11) 0.6009(10) 0.4633(7) 0.078(6) Uani 0.27 1 d PD B 2 B4 B 0.3552(6) 0.2824(5) 0.4345(3) 0.073(3) Uani 1 1 d D . . F41 F 0.3515(4) 0.3703(3) 0.40812(16) 0.0710(15) Uani 1 1 d D C . F42 F 0.4204(8) 0.2238(6) 0.4087(3) 0.078(3) Uani 0.61 1 d PD C 1 F43 F 0.2794(7) 0.2491(10) 0.4586(6) 0.145(6) Uani 0.61 1 d PD C 1 F44 F 0.4196(8) 0.2956(7) 0.4765(3) 0.099(3) Uani 0.61 1 d PD C 1 F45 F 0.2968(11) 0.2323(9) 0.4003(5) 0.099(3) Uani 0.39 1 d PD C 2 F46 F 0.3160(12) 0.2612(9) 0.4789(3) 0.078(3) Uani 0.39 1 d PD C 2 F47 F 0.4417(10) 0.2326(14) 0.4241(8) 0.145(6) Uani 0.39 1 d PD C 2 B5 B 0.1248(6) -0.1238(7) 0.3996(3) 0.081(4) Uani 1 1 d D . . F51 F 0.2154(4) -0.1347(5) 0.4146(2) 0.0845(17) Uani 1 1 d D D . F52 F 0.0792(12) -0.0436(10) 0.4213(7) 0.141(6) Uani 0.53 1 d PD D 1 F53 F 0.1072(9) -0.1287(18) 0.3529(4) 0.132(6) Uani 0.53 1 d PD D 1 F54 F 0.0719(9) -0.1993(11) 0.4306(8) 0.158(6) Uani 0.53 1 d PD D 1 F55 F 0.1302(11) -0.0354(13) 0.3635(8) 0.158(6) Uani 0.47 1 d PD D 2 F56 F 0.0959(13) -0.1926(12) 0.3786(9) 0.141(6) Uani 0.47 1 d PD D 2 F57 F 0.0556(8) -0.0954(17) 0.4367(5) 0.132(6) Uani 0.47 1 d PD D 2 B6 B 0.7293(5) 0.3565(6) 0.0506(3) 0.068(3) Uani 1 1 d D . . F61 F 0.6461(3) 0.3442(4) 0.07949(15) 0.0613(13) Uani 1 1 d D E . F62 F 0.7888(7) 0.2748(7) 0.0700(4) 0.083(3) Uani 0.56 1 d PD E 1 F63 F 0.7374(8) 0.3832(12) 0.0032(3) 0.131(6) Uani 0.56 1 d PD E 1 F64 F 0.7820(7) 0.4248(7) 0.0757(4) 0.087(2) Uani 0.56 1 d PD E 1 F65 F 0.7285(9) 0.2818(8) 0.0158(5) 0.087(2) Uani 0.44 1 d PD E 2 F66 F 0.7253(10) 0.4353(7) 0.0185(5) 0.083(3) Uani 0.44 1 d PD E 2 F67 F 0.8139(7) 0.3385(16) 0.0737(4) 0.131(6) Uani 0.44 1 d PD E 2 N600 N 0.8685(7) 0.0965(6) 0.1699(3) 0.083(3) Uani 1 1 d . . . C600 C 0.8940(7) 0.0992(6) 0.1280(4) 0.060(2) Uani 1 1 d . . . C601 C 0.9239(8) 0.1040(8) 0.0740(4) 0.084(3) Uani 1 1 d . . . H60A H 0.8672 0.1056 0.0535 0.101 Uiso 1 1 calc R . . H60B H 0.9647 0.0480 0.0683 0.101 Uiso 1 1 calc R . . H60C H 0.9603 0.1618 0.0631 0.101 Uiso 1 1 calc R . . N610 N 0.6234(7) -0.0004(9) 0.1915(6) 0.104(4) Uani 1 1 d . . . C610 C 0.6363(9) 0.0264(10) 0.1493(8) 0.092(5) Uani 1 1 d . . . C611 C 0.6516(9) 0.0629(9) 0.0963(8) 0.118(6) Uani 1 1 d . . . H61A H 0.5900 0.0700 0.0800 0.142 Uiso 1 1 calc R . . H61B H 0.6945 0.0191 0.0788 0.142 Uiso 1 1 calc R . . H61C H 0.6811 0.1252 0.0933 0.142 Uiso 1 1 calc R . . N620 N 0.0952(6) 0.4510(6) 0.2899(4) 0.076(2) Uani 1 1 d . . . C620 C 0.0933(7) 0.4210(6) 0.3319(6) 0.073(3) Uani 1 1 d . . . C621 C 0.0916(10) 0.3837(9) 0.3859(6) 0.119(5) Uani 1 1 d . . . H62A H 0.0913 0.4365 0.4067 0.143 Uiso 1 1 calc R . . H62B H 0.1487 0.3425 0.3925 0.143 Uiso 1 1 calc R . . H62C H 0.0337 0.3468 0.3954 0.143 Uiso 1 1 calc R . . O70 O 0.1165(13) 0.1444(10) 0.3924(8) 0.111(6) Uani 0.50 1 d P . . H70C H 0.1715 0.1707 0.3962 0.133 Uiso 0.50 1 d P . . H70D H 0.1133 0.0844 0.4155 0.133 Uiso 0.50 1 d P . . 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 Cu1 0.0288(4) 0.0312(4) 0.0203(4) -0.0080(3) -0.0046(3) 0.0006(3) Cu2 0.0297(4) 0.0243(4) 0.0327(4) -0.0011(3) -0.0049(3) 0.0019(3) Cu3 0.0315(4) 0.0263(4) 0.0174(3) -0.0030(3) -0.0080(3) -0.0024(3) Cu4 0.0306(4) 0.0287(4) 0.0170(3) -0.0081(3) -0.0059(3) 0.0034(3) N1 0.027(2) 0.034(3) 0.022(2) -0.010(2) -0.0066(19) 0.002(2) N2 0.031(3) 0.039(3) 0.021(2) -0.010(2) -0.008(2) -0.003(2) N3 0.030(3) 0.032(3) 0.030(3) -0.008(2) -0.004(2) 0.001(2) N4 0.030(3) 0.034(3) 0.021(2) -0.010(2) -0.009(2) 0.005(2) N5 0.042(3) 0.043(3) 0.020(2) -0.012(2) -0.003(2) -0.012(2) N6 0.079(5) 0.042(3) 0.034(3) -0.009(3) -0.021(3) -0.001(3) O1 0.040(2) 0.060(3) 0.022(2) -0.019(2) 0.0003(18) -0.015(2) O2 0.030(2) 0.035(2) 0.0210(19) -0.0125(17) -0.0040(16) -0.0014(17) C1 0.030(3) 0.042(3) 0.019(3) -0.007(2) -0.001(2) 0.001(3) C2 0.033(3) 0.047(4) 0.016(3) -0.010(2) -0.004(2) 0.002(3) C3 0.032(3) 0.028(3) 0.019(3) -0.009(2) -0.006(2) 0.005(2) C4 0.031(3) 0.026(3) 0.019(3) -0.007(2) -0.006(2) 0.005(2) C5 0.034(3) 0.029(3) 0.020(3) -0.007(2) -0.005(2) 0.000(2) C6 0.043(3) 0.041(3) 0.016(3) -0.010(2) -0.009(2) -0.006(3) C7 0.043(4) 0.035(3) 0.027(3) -0.008(3) -0.014(3) 0.001(3) C8 0.029(3) 0.034(3) 0.035(3) -0.010(3) -0.007(3) 0.004(2) C9 0.039(4) 0.050(4) 0.040(4) -0.011(3) -0.011(3) -0.003(3) C10 0.038(4) 0.049(4) 0.055(4) -0.014(3) -0.010(3) -0.007(3) C11 0.041(4) 0.034(3) 0.051(4) -0.012(3) 0.005(3) -0.003(3) C12 0.044(4) 0.029(3) 0.034(3) -0.008(3) -0.001(3) -0.001(3) C13 0.031(3) 0.029(3) 0.022(3) -0.007(2) -0.004(2) 0.004(2) C14 0.042(4) 0.053(4) 0.025(3) -0.013(3) 0.001(3) -0.016(3) C15 0.045(4) 0.049(4) 0.023(3) -0.011(3) -0.001(3) -0.003(3) C16 0.047(4) 0.038(3) 0.025(3) -0.006(3) -0.001(3) -0.006(3) C17 0.057(4) 0.045(4) 0.034(4) -0.012(3) 0.003(3) -0.007(3) C18 0.062(5) 0.043(4) 0.045(4) 0.006(3) 0.004(4) 0.002(3) C19 0.068(5) 0.056(5) 0.040(4) 0.005(4) -0.015(4) -0.006(4) C20 0.083(6) 0.055(5) 0.041(4) -0.010(4) -0.024(4) -0.001(4) N7 0.029(2) 0.023(2) 0.025(2) -0.0029(19) -0.007(2) 0.0002(19) N8 0.029(3) 0.027(3) 0.033(3) -0.005(2) 0.002(2) 0.002(2) N9 0.029(3) 0.028(3) 0.053(3) -0.004(2) -0.006(2) 0.002(2) N10 0.033(3) 0.030(3) 0.018(2) -0.0048(19) -0.0053(19) -0.004(2) N11 0.040(3) 0.027(3) 0.026(3) 0.001(2) 0.003(2) 0.005(2) N12 0.037(3) 0.042(3) 0.038(3) -0.005(2) -0.006(2) 0.004(2) O3 0.041(3) 0.028(2) 0.044(3) 0.002(2) 0.015(2) 0.0026(19) O4 0.034(2) 0.028(2) 0.024(2) -0.0032(16) -0.0048(17) 0.0039(17) C21 0.038(3) 0.028(3) 0.026(3) 0.000(2) -0.011(3) 0.000(2) C22 0.044(4) 0.033(3) 0.018(3) -0.005(2) -0.001(2) -0.003(3) C23 0.022(3) 0.025(3) 0.022(3) -0.003(2) -0.005(2) -0.004(2) C24 0.022(3) 0.026(3) 0.025(3) -0.002(2) -0.006(2) -0.004(2) C25 0.027(3) 0.031(3) 0.031(3) -0.003(3) -0.003(2) 0.002(2) C26 0.044(4) 0.033(3) 0.038(4) -0.002(3) 0.013(3) 0.005(3) C27 0.039(4) 0.040(4) 0.046(4) -0.012(3) 0.006(3) 0.002(3) C28 0.029(3) 0.031(3) 0.061(5) -0.009(3) 0.005(3) 0.001(3) C29 0.051(5) 0.042(4) 0.076(6) -0.020(4) 0.009(4) 0.005(3) C30 0.062(6) 0.049(5) 0.119(9) -0.012(5) -0.002(6) 0.030(4) C31 0.055(5) 0.056(5) 0.093(7) 0.004(5) -0.014(5) 0.028(4) C32 0.041(4) 0.038(4) 0.074(6) 0.001(4) -0.012(4) 0.011(3) C33 0.029(3) 0.026(3) 0.020(3) -0.006(2) -0.005(2) -0.001(2) C34 0.051(4) 0.027(3) 0.030(3) 0.001(3) 0.003(3) 0.001(3) C35 0.043(4) 0.043(4) 0.030(3) 0.001(3) -0.004(3) 0.007(3) C36 0.040(4) 0.044(4) 0.022(3) 0.000(3) -0.005(3) -0.001(3) C37 0.047(4) 0.049(4) 0.028(3) -0.005(3) -0.001(3) -0.005(3) C38 0.040(4) 0.061(5) 0.035(4) -0.004(3) 0.001(3) 0.000(3) C39 0.059(5) 0.057(5) 0.050(5) -0.015(4) 0.002(4) 0.016(4) C40 0.049(4) 0.050(4) 0.052(4) -0.018(4) -0.006(3) 0.002(3) N13 0.030(2) 0.023(2) 0.018(2) -0.0034(18) -0.0062(19) 0.0017(19) N14 0.034(3) 0.028(2) 0.020(2) -0.0018(19) -0.006(2) -0.004(2) N15 0.032(3) 0.028(3) 0.029(3) -0.006(2) -0.010(2) -0.001(2) N16 0.026(2) 0.027(2) 0.024(2) -0.0033(19) -0.0010(19) 0.0019(19) N17 0.047(3) 0.045(3) 0.030(3) 0.002(2) -0.019(2) -0.014(3) N18 0.093(5) 0.034(3) 0.025(3) -0.006(2) -0.011(3) -0.006(3) O5 0.041(2) 0.045(3) 0.024(2) 0.0096(19) -0.0155(18) -0.010(2) O6 0.033(2) 0.029(2) 0.034(2) -0.0007(17) -0.0134(18) -0.0061(18) C41 0.030(3) 0.034(3) 0.019(3) -0.003(2) -0.005(2) 0.000(2) C42 0.032(3) 0.033(3) 0.019(3) 0.000(2) -0.002(2) 0.001(2) C43 0.030(3) 0.023(3) 0.021(3) -0.004(2) -0.006(2) 0.003(2) C44 0.029(3) 0.023(3) 0.021(3) -0.005(2) -0.005(2) 0.005(2) C45 0.036(3) 0.024(3) 0.018(3) -0.001(2) -0.005(2) 0.001(2) C46 0.041(3) 0.036(3) 0.019(3) 0.001(2) -0.006(2) -0.009(3) C47 0.040(3) 0.033(3) 0.026(3) -0.002(2) 0.000(3) -0.006(3) C48 0.030(3) 0.026(3) 0.038(3) -0.003(3) -0.011(3) -0.001(2) C49 0.048(4) 0.034(3) 0.046(4) 0.005(3) -0.013(3) -0.011(3) C50 0.056(4) 0.027(3) 0.063(5) -0.006(3) -0.031(4) -0.009(3) C51 0.052(4) 0.030(3) 0.046(4) -0.009(3) -0.022(3) -0.002(3) C52 0.041(4) 0.033(3) 0.034(3) -0.011(3) -0.017(3) 0.005(3) C53 0.033(3) 0.023(3) 0.028(3) -0.001(2) -0.009(2) 0.003(2) C54 0.070(5) 0.059(5) 0.047(4) 0.000(4) -0.033(4) -0.021(4) C55 0.089(7) 0.069(5) 0.039(4) -0.005(4) -0.035(4) -0.008(5) C56 0.099(7) 0.051(4) 0.013(3) -0.005(3) -0.016(3) 0.001(4) C57 0.162(11) 0.050(5) 0.032(4) -0.010(4) -0.009(6) 0.009(6) C58 0.153(11) 0.052(5) 0.039(5) -0.003(4) 0.030(6) -0.027(6) C59 0.134(10) 0.067(6) 0.047(5) -0.009(5) 0.029(6) -0.016(6) C60 0.102(7) 0.060(5) 0.028(4) -0.007(4) 0.006(4) -0.014(5) N19 0.031(2) 0.026(2) 0.015(2) -0.0057(18) -0.0036(18) 0.0009(19) N20 0.030(2) 0.027(2) 0.020(2) -0.0038(19) -0.0061(19) 0.0002(19) N21 0.027(2) 0.029(3) 0.030(3) -0.012(2) -0.006(2) 0.000(2) N22 0.032(3) 0.026(2) 0.017(2) -0.0047(18) -0.0053(19) -0.0008(19) N23 0.034(3) 0.030(3) 0.017(2) -0.0071(19) -0.0076(19) 0.006(2) N24 0.037(3) 0.041(3) 0.022(3) -0.004(2) -0.007(2) 0.005(2) O7 0.045(2) 0.035(2) 0.0173(19) -0.0089(17) -0.0126(17) 0.0118(18) O8 0.033(2) 0.029(2) 0.0202(19) -0.0078(16) -0.0069(16) 0.0042(17) C61 0.039(3) 0.031(3) 0.018(3) -0.007(2) -0.005(2) 0.000(3) C62 0.041(3) 0.034(3) 0.016(3) -0.006(2) -0.007(2) 0.001(3) C63 0.027(3) 0.023(3) 0.015(2) -0.002(2) -0.005(2) -0.004(2) C64 0.027(3) 0.028(3) 0.017(3) -0.006(2) -0.004(2) -0.002(2) C65 0.022(3) 0.030(3) 0.019(3) -0.005(2) -0.005(2) 0.001(2) C66 0.034(3) 0.031(3) 0.019(3) 0.000(2) -0.005(2) 0.003(2) C67 0.031(3) 0.033(3) 0.028(3) -0.001(2) -0.007(2) 0.000(2) C68 0.033(3) 0.027(3) 0.030(3) -0.007(2) -0.007(2) -0.001(2) C69 0.041(4) 0.035(3) 0.037(4) -0.009(3) -0.011(3) 0.005(3) C70 0.049(4) 0.039(4) 0.047(4) -0.016(3) -0.010(3) 0.011(3) C71 0.038(4) 0.058(4) 0.035(4) -0.023(3) -0.003(3) 0.010(3) C72 0.034(3) 0.043(4) 0.028(3) -0.012(3) -0.004(3) -0.002(3) C73 0.025(3) 0.025(3) 0.018(3) -0.006(2) -0.004(2) -0.004(2) C74 0.048(4) 0.034(3) 0.023(3) -0.013(3) -0.009(3) 0.007(3) C75 0.046(4) 0.044(4) 0.017(3) -0.008(3) -0.007(3) -0.005(3) C76 0.040(3) 0.035(3) 0.019(3) -0.010(2) -0.006(2) 0.005(3) C77 0.041(4) 0.049(4) 0.037(4) -0.013(3) -0.008(3) 0.000(3) C78 0.037(4) 0.056(5) 0.056(5) -0.014(4) 0.003(3) -0.005(3) C79 0.053(4) 0.045(4) 0.048(4) -0.002(3) 0.011(4) -0.003(3) C80 0.059(5) 0.045(4) 0.034(4) 0.000(3) -0.007(3) 0.003(3) B1 0.036(4) 0.035(4) 0.035(4) -0.008(3) -0.011(3) 0.002(3) F11 0.090(4) 0.059(3) 0.045(2) -0.019(2) -0.009(2) 0.042(3) F12 0.053(3) 0.084(3) 0.042(2) -0.015(2) -0.0134(19) -0.029(2) F13 0.056(3) 0.091(4) 0.052(3) 0.001(2) -0.014(2) -0.037(3) F14 0.080(3) 0.045(2) 0.047(2) -0.0056(19) -0.003(2) 0.028(2) B2 0.051(5) 0.052(5) 0.034(4) -0.006(4) 0.010(4) 0.007(4) F21 0.195(11) 0.221(12) 0.205(12) -0.119(10) 0.014(9) 0.001(9) F22 0.323(16) 0.183(10) 0.071(5) -0.013(6) 0.004(7) -0.097(10) F23 0.251(12) 0.158(8) 0.092(6) -0.036(6) -0.043(7) 0.078(8) F24 0.227(13) 0.199(11) 0.145(9) 0.006(8) 0.016(9) -0.029(10) B3 0.054(7) 0.087(10) 0.018(5) 0.001(5) -0.009(5) 0.001(7) F31 0.074(4) 0.053(3) 0.031(3) 0.005(2) 0.001(3) -0.018(3) F32 0.148(9) 0.056(5) 0.201(12) 0.023(6) -0.109(9) -0.040(5) F33 0.243(14) 0.217(12) 0.044(5) 0.050(6) 0.043(6) 0.172(12) F34 0.123(7) 0.119(7) 0.047(4) 0.027(4) -0.047(4) -0.019(5) B3' 0.027(14) 0.08(2) 0.026(14) 0.004(14) -0.003(11) -0.009(14) F35 0.040(7) 0.046(8) 0.026(6) 0.021(6) -0.018(6) -0.027(6) F36 0.035(7) 0.072(9) 0.007(5) 0.002(6) -0.004(5) -0.031(7) F37 0.048(8) 0.036(7) 0.062(10) -0.006(7) -0.044(8) 0.003(6) F38 0.068(12) 0.044(10) 0.121(18) -0.009(10) -0.011(12) 0.011(9) B4 0.119(10) 0.046(5) 0.046(6) 0.007(4) 0.021(6) 0.010(6) F41 0.138(5) 0.047(3) 0.028(2) -0.0033(19) -0.016(3) 0.011(3) F42 0.145(9) 0.060(5) 0.024(3) 0.002(3) 0.003(4) 0.030(5) F43 0.114(9) 0.164(13) 0.141(13) 0.046(10) -0.019(9) -0.015(9) F44 0.172(10) 0.084(6) 0.039(4) -0.002(4) -0.010(5) 0.018(6) F45 0.172(10) 0.084(6) 0.039(4) -0.002(4) -0.010(5) 0.018(6) F46 0.145(9) 0.060(5) 0.024(3) 0.002(3) 0.003(4) 0.030(5) F47 0.114(9) 0.164(13) 0.141(13) 0.046(10) -0.019(9) -0.015(9) B5 0.070(7) 0.133(12) 0.046(6) -0.027(7) -0.008(5) -0.007(7) F51 0.078(4) 0.115(5) 0.060(3) 0.000(3) -0.021(3) -0.001(3) F52 0.166(14) 0.148(12) 0.120(13) -0.027(10) -0.062(11) -0.019(10) F53 0.066(6) 0.29(2) 0.050(6) -0.061(10) -0.019(4) 0.010(9) F54 0.104(8) 0.157(12) 0.184(16) 0.077(11) -0.005(9) 0.016(8) F55 0.104(8) 0.157(12) 0.184(16) 0.077(11) -0.005(9) 0.016(8) F56 0.166(14) 0.148(12) 0.120(13) -0.027(10) -0.062(11) -0.019(10) F57 0.066(6) 0.29(2) 0.050(6) -0.061(10) -0.019(4) 0.010(9) B6 0.063(6) 0.083(8) 0.051(6) 0.004(5) 0.011(5) 0.018(6) F61 0.050(3) 0.098(4) 0.031(2) 0.003(2) 0.0005(18) 0.011(2) F62 0.083(6) 0.088(6) 0.073(6) 0.002(5) 0.010(5) 0.012(5) F63 0.069(5) 0.288(18) 0.020(3) 0.024(7) -0.004(3) 0.029(8) F64 0.075(5) 0.088(6) 0.093(6) 0.006(5) 0.008(5) -0.005(4) F65 0.075(5) 0.088(6) 0.093(6) 0.006(5) 0.008(5) -0.005(4) F66 0.083(6) 0.088(6) 0.073(6) 0.002(5) 0.010(5) 0.012(5) F67 0.069(5) 0.288(18) 0.020(3) 0.024(7) -0.004(3) 0.029(8) N600 0.110(7) 0.079(6) 0.057(5) 0.003(4) -0.005(5) -0.023(5) C600 0.067(5) 0.051(5) 0.060(6) 0.005(4) -0.003(4) -0.015(4) C601 0.087(7) 0.090(8) 0.071(7) -0.005(6) 0.019(6) -0.007(6) N610 0.051(5) 0.104(9) 0.176(12) -0.083(10) -0.020(8) 0.022(5) C610 0.049(6) 0.081(9) 0.159(14) -0.072(11) -0.004(9) 0.018(6) C611 0.058(7) 0.091(9) 0.223(19) -0.088(12) -0.009(10) 0.016(6) N620 0.049(4) 0.059(5) 0.124(8) -0.021(5) -0.029(5) 0.001(4) C620 0.054(5) 0.042(5) 0.127(10) -0.001(6) -0.039(6) -0.015(4) C621 0.125(11) 0.092(9) 0.142(13) 0.028(8) -0.060(10) -0.055(8) O70 0.125(14) 0.054(8) 0.146(16) 0.020(9) -0.042(12) 0.032(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 Cu1 N2 1.914(5) . y Cu1 O4 1.958(4) . y Cu1 N3 2.004(5) . y Cu1 N1 2.032(5) . y Cu1 N10 2.316(5) . y Cu2 N8 1.915(5) . y Cu2 O6 1.974(4) . y Cu2 N9 2.027(5) . y Cu2 N7 2.052(5) . y Cu2 N16 2.247(5) . y Cu3 N14 1.931(5) . y Cu3 O8 1.997(4) . y Cu3 N15 2.007(5) . y Cu3 N13 2.039(5) . y Cu3 N22 2.275(5) . y Cu4 N20 1.924(5) . y Cu4 O2 1.993(4) . y Cu4 N21 2.012(5) . y Cu4 N19 2.027(5) . y Cu4 N4 2.313(5) . y N1 C1 1.327(7) . ? N1 C4 1.355(8) . ? N2 C5 1.315(8) . ? N2 C6 1.473(7) . ? N3 C12 1.347(8) . ? N3 C8 1.354(8) . ? N4 C2 1.327(8) . ? N4 C3 1.364(7) . ? N5 C13 1.313(7) . ? N5 C14 1.468(8) . ? N6 C16 1.356(8) . ? N6 C20 1.364(10) . ? O1 C5 1.249(7) . ? O2 C13 1.269(7) . ? C1 C2 1.383(9) . ? C3 C4 1.403(8) . ? C3 C13 1.517(8) . ? C4 C5 1.539(7) . ? C6 C7 1.515(9) . ? C7 C8 1.510(9) . ? C8 C9 1.394(9) . ? C9 C10 1.367(10) . ? C10 C11 1.381(10) . ? C11 C12 1.389(9) . ? C14 C15 1.522(8) . ? C15 C16 1.516(9) . ? C16 C17 1.369(10) . ? C17 C18 1.388(11) . ? C18 C19 1.386(11) . ? C19 C20 1.357(12) . ? N7 C21 1.326(8) . ? N7 C24 1.353(7) . ? N8 C25 1.320(8) . ? N8 C26 1.462(8) . ? N9 C32 1.350(9) . ? N9 C28 1.351(9) . ? N10 C22 1.314(8) . ? N10 C23 1.350(7) . ? N11 C33 1.303(8) . ? N11 C34 1.469(8) . ? N12 C36 1.333(9) . ? N12 C40 1.338(9) . ? O3 C25 1.249(7) . ? O4 C33 1.260(7) . ? C21 C22 1.389(9) . ? C23 C24 1.410(8) . ? C23 C33 1.526(8) . ? C24 C25 1.524(8) . ? C26 C27 1.525(9) . ? C27 C28 1.510(10) . ? C28 C29 1.391(10) . ? C29 C30 1.385(13) . ? C30 C31 1.359(15) . ? C31 C32 1.381(11) . ? C34 C35 1.516(9) . ? C35 C36 1.513(9) . ? C36 C37 1.393(10) . ? C37 C38 1.381(10) . ? C38 C39 1.368(11) . ? C39 C40 1.389(11) . ? N13 C41 1.317(7) . ? N13 C44 1.360(7) . ? N14 C45 1.309(8) . ? N14 C46 1.453(7) . ? N15 C48 1.349(8) . ? N15 C52 1.352(8) . ? N16 C42 1.329(7) . ? N16 C43 1.347(7) . ? N17 C53 1.306(8) . ? N17 C54 1.487(8) . ? N18 C60 1.325(12) . ? N18 C56 1.341(11) . ? O5 C45 1.262(7) . ? O6 C53 1.253(7) . ? C41 C42 1.384(8) . ? C43 C44 1.414(8) . ? C43 C53 1.524(8) . ? C44 C45 1.515(8) . ? C46 C47 1.517(9) . ? C47 C48 1.496(9) . ? C48 C49 1.387(9) . ? C49 C50 1.392(10) . ? C50 C51 1.370(11) . ? C51 C52 1.362(9) . ? C54 C55 1.494(11) . ? C55 C56 1.478(13) . ? C56 C57 1.439(12) . ? C57 C58 1.341(16) . ? C58 C59 1.359(15) . ? C59 C60 1.327(13) . ? N19 C61 1.322(7) . ? N19 C64 1.361(7) . ? N20 C65 1.307(7) . ? N20 C66 1.482(7) . ? N21 C72 1.357(8) . ? N21 C68 1.358(8) . ? N22 C62 1.336(7) . ? N22 C63 1.342(7) . ? N23 C73 1.310(7) . ? N23 C74 1.477(7) . ? N24 C80 1.346(9) . ? N24 C76 1.351(8) . ? O7 C65 1.264(7) . ? O8 C73 1.254(7) . ? C61 C62 1.383(8) . ? C63 C64 1.407(8) . ? C63 C73 1.530(7) . ? C64 C65 1.527(7) . ? C66 C67 1.530(8) . ? C67 C68 1.505(8) . ? C68 C69 1.388(9) . ? C69 C70 1.384(10) . ? C70 C71 1.400(10) . ? C71 C72 1.376(9) . ? C74 C75 1.522(8) . ? C75 C76 1.506(9) . ? C76 C77 1.386(9) . ? C77 C78 1.387(11) . ? C78 C79 1.379(11) . ? C79 C80 1.377(11) . ? B1 F13 1.324(7) . ? B1 F11 1.364(7) . ? B1 F14 1.405(7) . ? B1 F12 1.412(6) . ? B2 F23 1.275(8) . ? B2 F21 1.376(8) . ? B2 F22 1.388(8) . ? B2 F24 1.406(8) . ? B3 F33 1.340(15) . ? B3 F32 1.346(16) . ? B3 F34 1.350(13) . ? B3 F31 1.398(16) . ? B3' F37 1.284(9) . ? B3' F35 1.348(9) . ? B3' F38 1.415(10) . ? B3' F36 1.438(9) . ? B4 F46 1.249(8) . ? B4 F43 1.266(8) . ? B4 F41 1.341(7) . ? B4 F47 1.402(9) . ? B4 F42 1.405(8) . ? B4 F44 1.496(9) . ? B4 F45 1.506(9) . ? B5 F53 1.266(8) . ? B5 F56 1.271(9) . ? B5 F51 1.346(8) . ? B5 F57 1.403(9) . ? B5 F52 1.441(9) . ? B5 F54 1.447(9) . ? B5 F55 1.464(9) . ? B6 F63 1.240(8) . ? B6 F66 1.303(8) . ? B6 F61 1.343(7) . ? B6 F67 1.360(9) . ? B6 F62 1.452(8) . ? B6 F64 1.481(9) . ? B6 F65 1.483(9) . ? N600 C600 1.119(12) . ? C600 C601 1.433(13) . ? N610 C610 1.12(2) . ? C610 C611 1.41(2) . ? N620 C620 1.117(14) . ? C620 C621 1.432(18) . ? 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 N2 Cu1 O4 173.98(19) . . y N2 Cu1 N3 94.2(2) . . y O4 Cu1 N3 91.79(19) . . y N2 Cu1 N1 80.64(19) . . y O4 Cu1 N1 93.50(18) . . y N3 Cu1 N1 160.2(2) . . y N2 Cu1 N10 105.16(19) . . y O4 Cu1 N10 74.33(16) . . y N3 Cu1 N10 100.29(18) . . y N1 Cu1 N10 99.56(18) . . y N8 Cu2 O6 171.63(19) . . y N8 Cu2 N9 94.9(2) . . y O6 Cu2 N9 92.9(2) . . y N8 Cu2 N7 80.75(19) . . y O6 Cu2 N7 90.91(18) . . y N9 Cu2 N7 163.0(2) . . y N8 Cu2 N16 106.77(19) . . y O6 Cu2 N16 74.99(16) . . y N9 Cu2 N16 98.43(19) . . y N7 Cu2 N16 98.54(18) . . y N14 Cu3 O8 174.87(18) . . y N14 Cu3 N15 93.7(2) . . y O8 Cu3 N15 91.36(18) . . y N14 Cu3 N13 80.14(19) . . y O8 Cu3 N13 95.44(17) . . y N15 Cu3 N13 159.33(19) . . y N14 Cu3 N22 103.69(18) . . y O8 Cu3 N22 74.04(16) . . y N15 Cu3 N22 104.69(18) . . y N13 Cu3 N22 95.95(17) . . y N20 Cu4 O2 173.31(18) . . y N20 Cu4 N21 94.0(2) . . y O2 Cu4 N21 92.67(18) . . y N20 Cu4 N19 80.35(18) . . y O2 Cu4 N19 93.20(17) . . y N21 Cu4 N19 163.66(19) . . y N20 Cu4 N4 105.66(18) . . y O2 Cu4 N4 73.20(16) . . y N21 Cu4 N4 99.37(18) . . y N19 Cu4 N4 96.92(18) . . y C1 N1 C4 121.3(5) . . ? C1 N1 Cu1 124.1(4) . . ? C4 N1 Cu1 114.2(4) . . ? C5 N2 C6 117.7(5) . . ? C5 N2 Cu1 120.1(4) . . ? C6 N2 Cu1 122.1(4) . . ? C12 N3 C8 119.1(5) . . ? C12 N3 Cu1 120.1(4) . . ? C8 N3 Cu1 120.5(4) . . ? C2 N4 C3 119.3(5) . . ? C2 N4 Cu4 126.0(4) . . ? C3 N4 Cu4 114.5(4) . . ? C13 N5 C14 120.4(5) . . ? C16 N6 C20 119.2(6) . . ? C13 O2 Cu4 124.3(4) . . ? N1 C1 C2 119.5(5) . . ? N4 C2 C1 121.5(5) . . ? N4 C3 C4 119.8(5) . . ? N4 C3 C13 109.3(5) . . ? C4 C3 C13 130.9(5) . . ? N1 C4 C3 118.6(5) . . ? N1 C4 C5 112.3(5) . . ? C3 C4 C5 129.1(5) . . ? O1 C5 N2 125.9(5) . . ? O1 C5 C4 121.9(5) . . ? N2 C5 C4 112.1(5) . . ? N2 C6 C7 110.4(5) . . ? C8 C7 C6 114.3(5) . . ? N3 C8 C9 120.3(6) . . ? N3 C8 C7 118.3(5) . . ? C9 C8 C7 121.4(6) . . ? C10 C9 C8 120.3(6) . . ? C9 C10 C11 119.5(6) . . ? C10 C11 C12 118.3(7) . . ? N3 C12 C11 122.4(6) . . ? O2 C13 N5 120.5(5) . . ? O2 C13 C3 118.5(5) . . ? N5 C13 C3 121.0(5) . . ? N5 C14 C15 111.8(5) . . ? C16 C15 C14 116.7(6) . . ? N6 C16 C17 120.2(6) . . ? N6 C16 C15 114.3(6) . . ? C17 C16 C15 125.3(6) . . ? C16 C17 C18 120.0(7) . . ? C19 C18 C17 120.0(7) . . ? C20 C19 C18 117.6(7) . . ? C19 C20 N6 123.0(7) . . ? C21 N7 C24 120.0(5) . . ? C21 N7 Cu2 126.0(4) . . ? C24 N7 Cu2 113.7(4) . . ? C25 N8 C26 116.8(5) . . ? C25 N8 Cu2 118.2(4) . . ? C26 N8 Cu2 123.0(4) . . ? C32 N9 C28 118.6(6) . . ? C32 N9 Cu2 119.2(5) . . ? C28 N9 Cu2 122.2(4) . . ? C22 N10 C23 119.2(5) . . ? C22 N10 Cu1 127.9(4) . . ? C23 N10 Cu1 112.6(4) . . ? C33 N11 C34 121.9(5) . . ? C36 N12 C40 118.4(6) . . ? C33 O4 Cu1 123.3(4) . . ? N7 C21 C22 120.4(5) . . ? N10 C22 C21 121.3(5) . . ? N10 C23 C24 120.4(5) . . ? N10 C23 C33 110.0(5) . . ? C24 C23 C33 129.5(5) . . ? N7 C24 C23 118.6(5) . . ? N7 C24 C25 111.9(5) . . ? C23 C24 C25 129.5(5) . . ? O3 C25 N8 125.2(6) . . ? O3 C25 C24 121.5(5) . . ? N8 C25 C24 113.3(5) . . ? N8 C26 C27 110.8(5) . . ? C28 C27 C26 114.2(6) . . ? N9 C28 C29 121.0(7) . . ? N9 C28 C27 118.1(5) . . ? C29 C28 C27 120.9(7) . . ? C30 C29 C28 119.9(9) . . ? C31 C30 C29 118.4(8) . . ? C30 C31 C32 120.3(8) . . ? N9 C32 C31 121.8(9) . . ? O4 C33 N11 122.3(5) . . ? O4 C33 C23 118.2(5) . . ? N11 C33 C23 119.4(5) . . ? N11 C34 C35 110.1(5) . . ? C36 C35 C34 111.9(5) . . ? N12 C36 C37 121.8(6) . . ? N12 C36 C35 116.6(6) . . ? C37 C36 C35 121.6(6) . . ? C38 C37 C36 119.5(7) . . ? C39 C38 C37 118.5(7) . . ? C38 C39 C40 119.2(7) . . ? N12 C40 C39 122.5(7) . . ? C41 N13 C44 120.5(5) . . ? C41 N13 Cu3 124.9(4) . . ? C44 N13 Cu3 114.5(4) . . ? C45 N14 C46 116.9(5) . . ? C45 N14 Cu3 119.1(4) . . ? C46 N14 Cu3 123.7(4) . . ? C48 N15 C52 118.9(5) . . ? C48 N15 Cu3 121.4(4) . . ? C52 N15 Cu3 119.5(4) . . ? C42 N16 C43 119.5(5) . . ? C42 N16 Cu2 125.9(4) . . ? C43 N16 Cu2 114.4(4) . . ? C53 N17 C54 120.6(6) . . ? C60 N18 C56 123.9(7) . . ? C53 O6 Cu2 122.5(4) . . ? N13 C41 C42 120.9(5) . . ? N16 C42 C41 120.6(5) . . ? N16 C43 C44 120.4(5) . . ? N16 C43 C53 109.5(5) . . ? C44 C43 C53 130.0(5) . . ? N13 C44 C43 118.1(5) . . ? N13 C44 C45 111.9(5) . . ? C43 C44 C45 129.9(5) . . ? O5 C45 N14 124.5(5) . . ? O5 C45 C44 121.8(5) . . ? N14 C45 C44 113.8(5) . . ? N14 C46 C47 111.4(5) . . ? C48 C47 C46 113.0(5) . . ? N15 C48 C49 120.7(6) . . ? N15 C48 C47 118.6(5) . . ? C49 C48 C47 120.7(6) . . ? C48 C49 C50 119.1(7) . . ? C51 C50 C49 119.7(6) . . ? C52 C51 C50 118.5(6) . . ? N15 C52 C51 123.0(6) . . ? O6 C53 N17 121.3(5) . . ? O6 C53 C43 118.5(5) . . ? N17 C53 C43 120.2(5) . . ? N17 C54 C55 111.4(6) . . ? C56 C55 C54 116.6(8) . . ? N18 C56 C57 115.0(9) . . ? N18 C56 C55 122.5(7) . . ? C57 C56 C55 122.4(9) . . ? C58 C57 C56 119.8(10) . . ? C57 C58 C59 120.7(9) . . ? C60 C59 C58 119.6(11) . . ? N18 C60 C59 120.8(10) . . ? C61 N19 C64 120.4(5) . . ? C61 N19 Cu4 124.6(4) . . ? C64 N19 Cu4 114.8(4) . . ? C65 N20 C66 117.2(5) . . ? C65 N20 Cu4 119.3(4) . . ? C66 N20 Cu4 122.9(4) . . ? C72 N21 C68 119.1(5) . . ? C72 N21 Cu4 119.1(4) . . ? C68 N21 Cu4 121.6(4) . . ? C62 N22 C63 119.9(5) . . ? C62 N22 Cu3 124.8(4) . . ? C63 N22 Cu3 115.0(4) . . ? C73 N23 C74 120.3(5) . . ? C80 N24 C76 122.7(6) . . ? C73 O8 Cu3 122.7(3) . . ? N19 C61 C62 120.8(5) . . ? N22 C62 C61 120.1(5) . . ? N22 C63 C64 120.4(5) . . ? N22 C63 C73 109.2(5) . . ? C64 C63 C73 130.4(5) . . ? N19 C64 C63 118.3(5) . . ? N19 C64 C65 111.6(5) . . ? C63 C64 C65 130.1(5) . . ? O7 C65 N20 125.5(5) . . ? O7 C65 C64 121.3(5) . . ? N20 C65 C64 113.2(5) . . ? N20 C66 C67 110.2(5) . . ? C68 C67 C66 114.3(5) . . ? N21 C68 C69 120.6(6) . . ? N21 C68 C67 118.7(5) . . ? C69 C68 C67 120.7(5) . . ? C70 C69 C68 120.2(6) . . ? C69 C70 C71 118.9(6) . . ? C72 C71 C70 118.5(6) . . ? N21 C72 C71 122.5(6) . . ? O8 C73 N23 121.9(5) . . ? O8 C73 C63 118.6(5) . . ? N23 C73 C63 119.5(5) . . ? N23 C74 C75 110.3(5) . . ? C76 C75 C74 116.7(5) . . ? N24 C76 C77 118.3(6) . . ? N24 C76 C75 114.8(5) . . ? C77 C76 C75 126.7(6) . . ? C76 C77 C78 119.8(6) . . ? C79 C78 C77 120.3(7) . . ? C80 C79 C78 118.6(7) . . ? N24 C80 C79 120.3(7) . . ? F13 B1 F11 113.9(5) . . ? F13 B1 F14 111.2(5) . . ? F11 B1 F14 106.6(5) . . ? F13 B1 F12 108.4(5) . . ? F11 B1 F12 109.1(5) . . ? F14 B1 F12 107.4(5) . . ? F23 B2 F21 112.7(8) . . ? F23 B2 F22 122.5(8) . . ? F21 B2 F22 103.5(8) . . ? F23 B2 F24 102.0(8) . . ? F21 B2 F24 108.4(8) . . ? F22 B2 F24 107.1(8) . . ? F33 B3 F32 112.5(14) . . ? F33 B3 F34 110.4(11) . . ? F32 B3 F34 106.6(10) . . ? F33 B3 F31 108.1(10) . . ? F32 B3 F31 110.0(10) . . ? F34 B3 F31 109.2(11) . . ? F37 B3' F35 116.1(10) . . ? F37 B3' F38 109.5(11) . . ? F35 B3' F38 107.2(10) . . ? F37 B3' F36 110.8(10) . . ? F35 B3' F36 108.6(9) . . ? F38 B3' F36 103.9(10) . . ? F46 B4 F43 37.0(8) . . ? F46 B4 F41 123.5(8) . . ? F43 B4 F41 118.9(8) . . ? F46 B4 F47 115.4(10) . . ? F43 B4 F47 127.3(12) . . ? F41 B4 F47 112.9(10) . . ? F46 B4 F42 125.6(9) . . ? F43 B4 F42 120.9(10) . . ? F41 B4 F42 110.2(6) . . ? F47 B4 F42 22.4(11) . . ? F46 B4 F44 67.4(9) . . ? F43 B4 F44 104.4(9) . . ? F41 B4 F44 101.4(6) . . ? F47 B4 F44 73.3(10) . . ? F42 B4 F44 95.6(7) . . ? F46 B4 F45 103.9(9) . . ? F43 B4 F45 68.2(10) . . ? F41 B4 F45 98.9(7) . . ? F47 B4 F45 95.5(10) . . ? F42 B4 F45 73.8(8) . . ? F44 B4 F45 159.3(8) . . ? F53 B5 F56 49.5(10) . . ? F53 B5 F51 120.4(8) . . ? F56 B5 F51 114.7(10) . . ? F53 B5 F57 123.3(10) . . ? F56 B5 F57 111.2(11) . . ? F51 B5 F57 115.8(8) . . ? F53 B5 F52 114.7(10) . . ? F56 B5 F52 135.3(12) . . ? F51 B5 F52 108.6(8) . . ? F57 B5 F52 35.0(10) . . ? F53 B5 F54 105.8(10) . . ? F56 B5 F54 59.9(11) . . ? F51 B5 F54 105.7(8) . . ? F57 B5 F54 63.9(10) . . ? F52 B5 F54 98.9(9) . . ? F53 B5 F55 63.1(11) . . ? F56 B5 F55 112.4(11) . . ? F51 B5 F55 101.6(8) . . ? F57 B5 F55 99.7(10) . . ? F52 B5 F55 67.3(10) . . ? F54 B5 F55 152.3(10) . . ? F63 B6 F66 40.9(8) . . ? F63 B6 F61 125.7(8) . . ? F66 B6 F61 110.6(7) . . ? F63 B6 F67 114.8(9) . . ? F66 B6 F67 115.0(10) . . ? F61 B6 F67 119.4(7) . . ? F63 B6 F62 116.6(9) . . ? F66 B6 F62 145.8(9) . . ? F61 B6 F62 103.6(6) . . ? F67 B6 F62 41.5(9) . . ? F63 B6 F64 106.5(9) . . ? F66 B6 F64 75.9(9) . . ? F61 B6 F64 105.0(6) . . ? F67 B6 F64 53.8(9) . . ? F62 B6 F64 94.2(7) . . ? F63 B6 F65 63.0(9) . . ? F66 B6 F65 103.1(8) . . ? F61 B6 F65 103.1(7) . . ? F67 B6 F65 103.2(9) . . ? F62 B6 F65 69.7(7) . . ? F64 B6 F65 150.3(8) . . ? N600 C600 C601 178.3(12) . . ? N610 C610 C611 178.3(15) . . ? N620 C620 C621 179.1(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C1 -178.1(5) . . . . ? O4 Cu1 N1 C1 0.6(5) . . . . ? N3 Cu1 N1 C1 105.7(7) . . . . ? N10 Cu1 N1 C1 -74.1(5) . . . . ? N2 Cu1 N1 C4 -5.7(4) . . . . ? O4 Cu1 N1 C4 172.9(4) . . . . ? N3 Cu1 N1 C4 -81.9(7) . . . . ? N10 Cu1 N1 C4 98.2(4) . . . . ? O4 Cu1 N2 C5 -12(2) . . . . ? N3 Cu1 N2 C5 161.5(5) . . . . ? N1 Cu1 N2 C5 0.8(5) . . . . ? N10 Cu1 N2 C5 -96.6(5) . . . . ? O4 Cu1 N2 C6 170.9(16) . . . . ? N3 Cu1 N2 C6 -15.3(5) . . . . ? N1 Cu1 N2 C6 -176.0(5) . . . . ? N10 Cu1 N2 C6 86.6(5) . . . . ? N2 Cu1 N3 C12 -148.5(5) . . . . ? O4 Cu1 N3 C12 30.9(5) . . . . ? N1 Cu1 N3 C12 -74.6(8) . . . . ? N10 Cu1 N3 C12 105.3(5) . . . . ? N2 Cu1 N3 C8 38.2(5) . . . . ? O4 Cu1 N3 C8 -142.5(5) . . . . ? N1 Cu1 N3 C8 112.0(6) . . . . ? N10 Cu1 N3 C8 -68.1(5) . . . . ? N20 Cu4 N4 C2 2.3(5) . . . . ? O2 Cu4 N4 C2 175.4(5) . . . . ? N21 Cu4 N4 C2 -94.6(5) . . . . ? N19 Cu4 N4 C2 84.1(5) . . . . ? N20 Cu4 N4 C3 -173.9(4) . . . . ? O2 Cu4 N4 C3 -0.7(4) . . . . ? N21 Cu4 N4 C3 89.2(4) . . . . ? N19 Cu4 N4 C3 -92.0(4) . . . . ? N20 Cu4 O2 C13 84.6(16) . . . . ? N21 Cu4 O2 C13 -95.6(4) . . . . ? N19 Cu4 O2 C13 99.7(4) . . . . ? N4 Cu4 O2 C13 3.4(4) . . . . ? C4 N1 C1 C2 -0.8(9) . . . . ? Cu1 N1 C1 C2 171.1(4) . . . . ? C3 N4 C2 C1 1.1(9) . . . . ? Cu4 N4 C2 C1 -174.9(4) . . . . ? N1 C1 C2 N4 -0.7(9) . . . . ? C2 N4 C3 C4 0.0(8) . . . . ? Cu4 N4 C3 C4 176.4(4) . . . . ? C2 N4 C3 C13 -177.7(5) . . . . ? Cu4 N4 C3 C13 -1.3(6) . . . . ? C1 N1 C4 C3 1.7(8) . . . . ? Cu1 N1 C4 C3 -170.9(4) . . . . ? C1 N1 C4 C5 -178.6(5) . . . . ? Cu1 N1 C4 C5 8.8(6) . . . . ? N4 C3 C4 N1 -1.3(8) . . . . ? C13 C3 C4 N1 175.8(5) . . . . ? N4 C3 C4 C5 179.1(5) . . . . ? C13 C3 C4 C5 -3.8(10) . . . . ? C6 N2 C5 O1 1.3(9) . . . . ? Cu1 N2 C5 O1 -175.7(5) . . . . ? C6 N2 C5 C4 -179.5(5) . . . . ? Cu1 N2 C5 C4 3.5(7) . . . . ? N1 C4 C5 O1 171.2(5) . . . . ? C3 C4 C5 O1 -9.2(9) . . . . ? N1 C4 C5 N2 -8.1(7) . . . . ? C3 C4 C5 N2 171.5(6) . . . . ? C5 N2 C6 C7 153.0(5) . . . . ? Cu1 N2 C6 C7 -30.1(7) . . . . ? N2 C6 C7 C8 69.8(7) . . . . ? C12 N3 C8 C9 -3.9(9) . . . . ? Cu1 N3 C8 C9 169.5(5) . . . . ? C12 N3 C8 C7 175.3(5) . . . . ? Cu1 N3 C8 C7 -11.3(7) . . . . ? C6 C7 C8 N3 -47.9(8) . . . . ? C6 C7 C8 C9 131.3(6) . . . . ? N3 C8 C9 C10 2.1(10) . . . . ? C7 C8 C9 C10 -177.1(6) . . . . ? C8 C9 C10 C11 1.1(11) . . . . ? C9 C10 C11 C12 -2.4(10) . . . . ? C8 N3 C12 C11 2.6(9) . . . . ? Cu1 N3 C12 C11 -170.8(5) . . . . ? C10 C11 C12 N3 0.5(10) . . . . ? Cu4 O2 C13 N5 174.6(4) . . . . ? Cu4 O2 C13 C3 -5.4(7) . . . . ? C14 N5 C13 O2 -1.5(9) . . . . ? C14 N5 C13 C3 178.5(6) . . . . ? N4 C3 C13 O2 4.1(7) . . . . ? C4 C3 C13 O2 -173.3(6) . . . . ? N4 C3 C13 N5 -176.0(5) . . . . ? C4 C3 C13 N5 6.7(9) . . . . ? C13 N5 C14 C15 -170.3(6) . . . . ? N5 C14 C15 C16 -73.1(8) . . . . ? C20 N6 C16 C17 0.0(11) . . . . ? C20 N6 C16 C15 175.1(7) . . . . ? C14 C15 C16 N6 155.4(6) . . . . ? C14 C15 C16 C17 -29.7(10) . . . . ? N6 C16 C17 C18 0.0(11) . . . . ? C15 C16 C17 C18 -174.7(7) . . . . ? C16 C17 C18 C19 1.0(11) . . . . ? C17 C18 C19 C20 -1.8(12) . . . . ? C18 C19 C20 N6 1.7(13) . . . . ? C16 N6 C20 C19 -0.9(13) . . . . ? N8 Cu2 N7 C21 174.2(5) . . . . ? O6 Cu2 N7 C21 -6.5(5) . . . . ? N9 Cu2 N7 C21 -109.6(8) . . . . ? N16 Cu2 N7 C21 68.5(5) . . . . ? N8 Cu2 N7 C24 0.2(4) . . . . ? O6 Cu2 N7 C24 179.5(4) . . . . ? N9 Cu2 N7 C24 76.4(8) . . . . ? N16 Cu2 N7 C24 -105.6(4) . . . . ? O6 Cu2 N8 C25 4.7(16) . . . . ? N9 Cu2 N8 C25 -154.0(5) . . . . ? N7 Cu2 N8 C25 9.4(4) . . . . ? N16 Cu2 N8 C25 105.6(4) . . . . ? O6 Cu2 N8 C26 168.1(11) . . . . ? N9 Cu2 N8 C26 9.4(5) . . . . ? N7 Cu2 N8 C26 172.8(5) . . . . ? N16 Cu2 N8 C26 -91.0(5) . . . . ? N8 Cu2 N9 C32 152.9(5) . . . . ? O6 Cu2 N9 C32 -24.1(5) . . . . ? N7 Cu2 N9 C32 78.7(9) . . . . ? N16 Cu2 N9 C32 -99.4(5) . . . . ? N8 Cu2 N9 C28 -28.3(5) . . . . ? O6 Cu2 N9 C28 154.8(5) . . . . ? N7 Cu2 N9 C28 -102.4(8) . . . . ? N16 Cu2 N9 C28 79.5(5) . . . . ? N2 Cu1 N10 C22 3.1(5) . . . . ? O4 Cu1 N10 C22 -170.6(5) . . . . ? N3 Cu1 N10 C22 100.4(5) . . . . ? N1 Cu1 N10 C22 -79.7(5) . . . . ? N2 Cu1 N10 C23 176.6(4) . . . . ? O4 Cu1 N10 C23 2.9(4) . . . . ? N3 Cu1 N10 C23 -86.1(4) . . . . ? N1 Cu1 N10 C23 93.8(4) . . . . ? N2 Cu1 O4 C33 -96.1(19) . . . . ? N3 Cu1 O4 C33 90.1(4) . . . . ? N1 Cu1 O4 C33 -109.1(4) . . . . ? N10 Cu1 O4 C33 -10.1(4) . . . . ? C24 N7 C21 C22 1.3(8) . . . . ? Cu2 N7 C21 C22 -172.3(4) . . . . ? C23 N10 C22 C21 -2.6(9) . . . . ? Cu1 N10 C22 C21 170.5(4) . . . . ? N7 C21 C22 N10 1.8(9) . . . . ? C22 N10 C23 C24 0.4(8) . . . . ? Cu1 N10 C23 C24 -173.7(4) . . . . ? C22 N10 C23 C33 177.0(5) . . . . ? Cu1 N10 C23 C33 2.9(5) . . . . ? C21 N7 C24 C23 -3.4(8) . . . . ? Cu2 N7 C24 C23 171.0(4) . . . . ? C21 N7 C24 C25 177.6(5) . . . . ? Cu2 N7 C24 C25 -8.0(6) . . . . ? N10 C23 C24 N7 2.6(8) . . . . ? C33 C23 C24 N7 -173.2(5) . . . . ? N10 C23 C24 C25 -178.6(5) . . . . ? C33 C23 C24 C25 5.6(9) . . . . ? C26 N8 C25 O3 -1.7(9) . . . . ? Cu2 N8 C25 O3 162.7(5) . . . . ? C26 N8 C25 C24 179.4(5) . . . . ? Cu2 N8 C25 C24 -16.2(7) . . . . ? N7 C24 C25 O3 -163.5(5) . . . . ? C23 C24 C25 O3 17.6(9) . . . . ? N7 C24 C25 N8 15.4(7) . . . . ? C23 C24 C25 N8 -163.4(5) . . . . ? C25 N8 C26 C27 -163.8(6) . . . . ? Cu2 N8 C26 C27 32.6(8) . . . . ? N8 C26 C27 C28 -70.3(7) . . . . ? C32 N9 C28 C29 1.8(10) . . . . ? Cu2 N9 C28 C29 -177.1(5) . . . . ? C32 N9 C28 C27 -179.9(6) . . . . ? Cu2 N9 C28 C27 1.2(8) . . . . ? C26 C27 C28 N9 52.5(8) . . . . ? C26 C27 C28 C29 -129.2(7) . . . . ? N9 C28 C29 C30 -0.4(12) . . . . ? C27 C28 C29 C30 -178.7(8) . . . . ? C28 C29 C30 C31 -1.7(14) . . . . ? C29 C30 C31 C32 2.4(15) . . . . ? C28 N9 C32 C31 -1.1(11) . . . . ? Cu2 N9 C32 C31 177.8(6) . . . . ? C30 C31 C32 N9 -1.1(14) . . . . ? Cu1 O4 C33 N11 -163.0(4) . . . . ? Cu1 O4 C33 C23 15.5(7) . . . . ? C34 N11 C33 O4 0.5(9) . . . . ? C34 N11 C33 C23 -178.0(5) . . . . ? N10 C23 C33 O4 -11.0(7) . . . . ? C24 C23 C33 O4 165.1(5) . . . . ? N10 C23 C33 N11 167.5(5) . . . . ? C24 C23 C33 N11 -16.3(9) . . . . ? C33 N11 C34 C35 -113.9(6) . . . . ? N11 C34 C35 C36 -54.6(7) . . . . ? C40 N12 C36 C37 -1.6(10) . . . . ? C40 N12 C36 C35 -179.8(6) . . . . ? C34 C35 C36 N12 120.8(6) . . . . ? C34 C35 C36 C37 -57.4(8) . . . . ? N12 C36 C37 C38 0.4(10) . . . . ? C35 C36 C37 C38 178.5(6) . . . . ? C36 C37 C38 C39 1.2(10) . . . . ? C37 C38 C39 C40 -1.5(11) . . . . ? C36 N12 C40 C39 1.3(11) . . . . ? C38 C39 C40 N12 0.2(12) . . . . ? N14 Cu3 N13 C41 -175.5(5) . . . . ? O8 Cu3 N13 C41 1.9(5) . . . . ? N15 Cu3 N13 C41 110.6(6) . . . . ? N22 Cu3 N13 C41 -72.6(5) . . . . ? N14 Cu3 N13 C44 -0.1(4) . . . . ? O8 Cu3 N13 C44 177.3(4) . . . . ? N15 Cu3 N13 C44 -74.0(7) . . . . ? N22 Cu3 N13 C44 102.8(4) . . . . ? O8 Cu3 N14 C45 -36(2) . . . . ? N15 Cu3 N14 C45 155.2(4) . . . . ? N13 Cu3 N14 C45 -4.9(4) . . . . ? N22 Cu3 N14 C45 -98.7(4) . . . . ? O8 Cu3 N14 C46 150.4(19) . . . . ? N15 Cu3 N14 C46 -18.8(5) . . . . ? N13 Cu3 N14 C46 -178.9(5) . . . . ? N22 Cu3 N14 C46 87.3(5) . . . . ? N14 Cu3 N15 C48 29.1(5) . . . . ? O8 Cu3 N15 C48 -149.9(4) . . . . ? N13 Cu3 N15 C48 100.7(7) . . . . ? N22 Cu3 N15 C48 -76.1(5) . . . . ? N14 Cu3 N15 C52 -146.5(4) . . . . ? O8 Cu3 N15 C52 34.5(4) . . . . ? N13 Cu3 N15 C52 -74.9(7) . . . . ? N22 Cu3 N15 C52 108.3(4) . . . . ? N8 Cu2 N16 C42 2.6(5) . . . . ? O6 Cu2 N16 C42 174.1(5) . . . . ? N9 Cu2 N16 C42 -95.1(5) . . . . ? N7 Cu2 N16 C42 85.4(5) . . . . ? N8 Cu2 N16 C43 -172.6(4) . . . . ? O6 Cu2 N16 C43 -1.1(4) . . . . ? N9 Cu2 N16 C43 89.7(4) . . . . ? N7 Cu2 N16 C43 -89.8(4) . . . . ? N8 Cu2 O6 C53 106.7(13) . . . . ? N9 Cu2 O6 C53 -94.5(5) . . . . ? N7 Cu2 O6 C53 102.1(5) . . . . ? N16 Cu2 O6 C53 3.5(4) . . . . ? C44 N13 C41 C42 -0.2(8) . . . . ? Cu3 N13 C41 C42 175.0(4) . . . . ? C43 N16 C42 C41 0.4(8) . . . . ? Cu2 N16 C42 C41 -174.6(4) . . . . ? N13 C41 C42 N16 -0.7(9) . . . . ? C42 N16 C43 C44 0.7(8) . . . . ? Cu2 N16 C43 C44 176.3(4) . . . . ? C42 N16 C43 C53 -176.3(5) . . . . ? Cu2 N16 C43 C53 -0.8(6) . . . . ? C41 N13 C44 C43 1.3(8) . . . . ? Cu3 N13 C44 C43 -174.4(4) . . . . ? C41 N13 C44 C45 179.7(5) . . . . ? Cu3 N13 C44 C45 4.1(6) . . . . ? N16 C43 C44 N13 -1.5(8) . . . . ? C53 C43 C44 N13 174.8(5) . . . . ? N16 C43 C44 C45 -179.7(5) . . . . ? C53 C43 C44 C45 -3.3(10) . . . . ? C46 N14 C45 O5 2.1(9) . . . . ? Cu3 N14 C45 O5 -172.4(5) . . . . ? C46 N14 C45 C44 -177.2(5) . . . . ? Cu3 N14 C45 C44 8.4(6) . . . . ? N13 C44 C45 O5 172.8(5) . . . . ? C43 C44 C45 O5 -9.0(9) . . . . ? N13 C44 C45 N14 -7.9(7) . . . . ? C43 C44 C45 N14 170.3(5) . . . . ? C45 N14 C46 C47 163.7(5) . . . . ? Cu3 N14 C46 C47 -22.2(7) . . . . ? N14 C46 C47 C48 67.0(7) . . . . ? C52 N15 C48 C49 0.3(9) . . . . ? Cu3 N15 C48 C49 -175.4(5) . . . . ? C52 N15 C48 C47 180.0(5) . . . . ? Cu3 N15 C48 C47 4.3(7) . . . . ? C46 C47 C48 N15 -58.7(7) . . . . ? C46 C47 C48 C49 121.0(6) . . . . ? N15 C48 C49 C50 -1.8(10) . . . . ? C47 C48 C49 C50 178.5(6) . . . . ? C48 C49 C50 C51 2.1(11) . . . . ? C49 C50 C51 C52 -0.8(10) . . . . ? C48 N15 C52 C51 1.1(9) . . . . ? Cu3 N15 C52 C51 176.8(5) . . . . ? C50 C51 C52 N15 -0.9(10) . . . . ? Cu2 O6 C53 N17 177.4(5) . . . . ? Cu2 O6 C53 C43 -5.2(7) . . . . ? C54 N17 C53 O6 0.7(10) . . . . ? C54 N17 C53 C43 -176.6(6) . . . . ? N16 C43 C53 O6 3.6(7) . . . . ? C44 C43 C53 O6 -173.0(6) . . . . ? N16 C43 C53 N17 -179.0(6) . . . . ? C44 C43 C53 N17 4.4(9) . . . . ? C53 N17 C54 C55 -161.8(7) . . . . ? N17 C54 C55 C56 -55.8(10) . . . . ? C60 N18 C56 C57 3.2(10) . . . . ? C60 N18 C56 C55 -175.8(7) . . . . ? C54 C55 C56 N18 -30.4(10) . . . . ? C54 C55 C56 C57 150.7(8) . . . . ? N18 C56 C57 C58 -4.5(12) . . . . ? C55 C56 C57 C58 174.5(8) . . . . ? C56 C57 C58 C59 3.1(15) . . . . ? C57 C58 C59 C60 -0.1(16) . . . . ? C56 N18 C60 C59 -0.4(12) . . . . ? C58 C59 C60 N18 -1.3(15) . . . . ? N20 Cu4 N19 C61 175.3(5) . . . . ? O2 Cu4 N19 C61 -2.9(5) . . . . ? N21 Cu4 N19 C61 -113.8(7) . . . . ? N4 Cu4 N19 C61 70.5(5) . . . . ? N20 Cu4 N19 C64 -0.8(4) . . . . ? O2 Cu4 N19 C64 -179.1(4) . . . . ? N21 Cu4 N19 C64 70.1(8) . . . . ? N4 Cu4 N19 C64 -105.6(4) . . . . ? O2 Cu4 N20 C65 21.2(18) . . . . ? N21 Cu4 N20 C65 -158.6(4) . . . . ? N19 Cu4 N20 C65 5.9(4) . . . . ? N4 Cu4 N20 C65 100.5(4) . . . . ? O2 Cu4 N20 C66 -167.1(14) . . . . ? N21 Cu4 N20 C66 13.1(4) . . . . ? N19 Cu4 N20 C66 177.6(5) . . . . ? N4 Cu4 N20 C66 -87.8(4) . . . . ? N20 Cu4 N21 C72 151.4(4) . . . . ? O2 Cu4 N21 C72 -28.6(4) . . . . ? N19 Cu4 N21 C72 82.3(8) . . . . ? N4 Cu4 N21 C72 -102.0(4) . . . . ? N20 Cu4 N21 C68 -34.6(5) . . . . ? O2 Cu4 N21 C68 145.4(4) . . . . ? N19 Cu4 N21 C68 -103.7(7) . . . . ? N4 Cu4 N21 C68 72.0(4) . . . . ? N14 Cu3 N22 C62 1.6(5) . . . . ? O8 Cu3 N22 C62 -173.6(5) . . . . ? N15 Cu3 N22 C62 99.2(5) . . . . ? N13 Cu3 N22 C62 -79.6(5) . . . . ? N14 Cu3 N22 C63 175.3(4) . . . . ? O8 Cu3 N22 C63 0.1(4) . . . . ? N15 Cu3 N22 C63 -87.1(4) . . . . ? N13 Cu3 N22 C63 94.0(4) . . . . ? N14 Cu3 O8 C73 -69(2) . . . . ? N15 Cu3 O8 C73 100.0(4) . . . . ? N13 Cu3 O8 C73 -99.5(4) . . . . ? N22 Cu3 O8 C73 -4.9(4) . . . . ? C64 N19 C61 C62 0.0(9) . . . . ? Cu4 N19 C61 C62 -176.0(4) . . . . ? C63 N22 C62 C61 0.2(9) . . . . ? Cu3 N22 C62 C61 173.5(4) . . . . ? N19 C61 C62 N22 0.3(9) . . . . ? C62 N22 C63 C64 -1.0(8) . . . . ? Cu3 N22 C63 C64 -175.0(4) . . . . ? C62 N22 C63 C73 177.5(5) . . . . ? Cu3 N22 C63 C73 3.5(5) . . . . ? C61 N19 C64 C63 -0.8(8) . . . . ? Cu4 N19 C64 C63 175.6(4) . . . . ? C61 N19 C64 C65 -179.7(5) . . . . ? Cu4 N19 C64 C65 -3.4(6) . . . . ? N22 C63 C64 N19 1.3(8) . . . . ? C73 C63 C64 N19 -176.8(5) . . . . ? N22 C63 C64 C65 180.0(5) . . . . ? C73 C63 C64 C65 1.9(10) . . . . ? C66 N20 C65 O7 -1.7(8) . . . . ? Cu4 N20 C65 O7 170.4(4) . . . . ? C66 N20 C65 C64 178.6(5) . . . . ? Cu4 N20 C65 C64 -9.3(6) . . . . ? N19 C64 C65 O7 -171.7(5) . . . . ? C63 C64 C65 O7 9.5(9) . . . . ? N19 C64 C65 N20 7.9(7) . . . . ? C63 C64 C65 N20 -170.8(5) . . . . ? C65 N20 C66 C67 -157.5(5) . . . . ? Cu4 N20 C66 C67 30.6(6) . . . . ? N20 C66 C67 C68 -69.2(6) . . . . ? C72 N21 C68 C69 3.8(8) . . . . ? Cu4 N21 C68 C69 -170.2(4) . . . . ? C72 N21 C68 C67 -178.1(5) . . . . ? Cu4 N21 C68 C67 7.9(7) . . . . ? C66 C67 C68 N21 49.3(7) . . . . ? C66 C67 C68 C69 -132.6(6) . . . . ? N21 C68 C69 C70 -1.3(9) . . . . ? C67 C68 C69 C70 -179.3(6) . . . . ? C68 C69 C70 C71 -2.5(10) . . . . ? C69 C70 C71 C72 3.7(10) . . . . ? C68 N21 C72 C71 -2.6(9) . . . . ? Cu4 N21 C72 C71 171.5(5) . . . . ? C70 C71 C72 N21 -1.1(10) . . . . ? Cu3 O8 C73 N23 -169.2(4) . . . . ? Cu3 O8 C73 C63 8.7(6) . . . . ? C74 N23 C73 O8 6.0(8) . . . . ? C74 N23 C73 C63 -171.8(5) . . . . ? N22 C63 C73 O8 -7.6(7) . . . . ? C64 C63 C73 O8 170.6(5) . . . . ? N22 C63 C73 N23 170.3(5) . . . . ? C64 C63 C73 N23 -11.5(9) . . . . ? C73 N23 C74 C75 177.2(5) . . . . ? N23 C74 C75 C76 82.9(7) . . . . ? C80 N24 C76 C77 1.1(9) . . . . ? C80 N24 C76 C75 -174.3(6) . . . . ? C74 C75 C76 N24 -176.9(5) . . . . ? C74 C75 C76 C77 8.1(9) . . . . ? N24 C76 C77 C78 -1.0(9) . . . . ? C75 C76 C77 C78 173.9(6) . . . . ? C76 C77 C78 C79 -0.6(11) . . . . ? C77 C78 C79 C80 2.1(11) . . . . ? C76 N24 C80 C79 0.4(10) . . . . ? C78 C79 C80 N24 -2.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.101 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.142 # Attachment 'H2L6DfinalNov06.cif' data_h2l6d _database_code_depnum_ccdc_archive 'CCDC 296870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 N6 O2' _chemical_formula_weight 376.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.0400(2) _cell_length_b 20.6432(6) _cell_length_c 17.8496(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.204(2) _cell_angle_gamma 90.00 _cell_volume 1854.20(9) _cell_formula_units_Z 4 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used 3019 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25.7 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10187 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.69 _reflns_number_total 3494 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 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. All non-H ANIS. No solvent. No disorder. H's calc and ride except for amide N-H's where the H's were found and x,y,z,U freely refined. Both amide N-H's are involved in H-bonds to, different, adjacent ligands. ; _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^)+(0.0416P)^2^+0.6889P] 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 3494 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.4473(4) 0.46978(9) -0.29083(10) 0.0242(5) Uani 1 1 d . . . O2 O -0.3928(4) 0.37436(9) -0.17534(10) 0.0234(5) Uani 1 1 d . . . N1 N -0.3392(5) 0.33748(11) -0.41068(12) 0.0217(6) Uani 1 1 d . . . N2 N -0.6993(4) 0.43577(12) -0.39220(13) 0.0188(6) Uani 1 1 d . . . H2B H -0.721(6) 0.4094(14) -0.4293(16) 0.024(8) Uiso 1 1 d . . . N3 N -1.0876(4) 0.62607(11) -0.45371(13) 0.0226(6) Uani 1 1 d . . . N4 N 0.0209(5) 0.30153(11) -0.29250(13) 0.0228(6) Uani 1 1 d . . . N5 N 0.0532(5) 0.39330(12) -0.17060(13) 0.0222(6) Uani 1 1 d . . . H5A H 0.210(8) 0.3867(17) -0.1896(19) 0.061(12) Uiso 1 1 d . . . N6 N 0.0004(5) 0.35596(13) 0.08455(13) 0.0322(7) Uani 1 1 d . . . C1 C -0.1689(6) 0.28825(13) -0.41688(16) 0.0231(7) Uani 1 1 d . . . H1 H -0.1749 0.2637 -0.4620 0.028 Uiso 1 1 calc R . . C2 C 0.0148(6) 0.27212(14) -0.35988(16) 0.0244(7) Uani 1 1 d . . . H2 H 0.1412 0.2392 -0.3684 0.029 Uiso 1 1 calc R . . C3 C -0.1592(5) 0.34885(13) -0.28415(15) 0.0182(6) Uani 1 1 d . . . C4 C -0.3313(5) 0.36885(13) -0.34454(15) 0.0170(6) Uani 1 1 d . . . C5 C -0.4984(5) 0.42887(13) -0.33999(15) 0.0187(6) Uani 1 1 d . . . C6 C -0.8623(5) 0.49435(13) -0.39225(16) 0.0207(7) Uani 1 1 d . . . H6A H -0.9129 0.5033 -0.3405 0.025 Uiso 1 1 calc R . . H6B H -1.0275 0.4870 -0.4238 0.025 Uiso 1 1 calc R . . C7 C -0.7171(6) 0.55313(13) -0.42193(16) 0.0223(7) Uani 1 1 d . . . H7A H -0.5377 0.5560 -0.3966 0.027 Uiso 1 1 calc R . . H7B H -0.6957 0.5478 -0.4764 0.027 Uiso 1 1 calc R . . C8 C -0.8681(5) 0.61497(13) -0.40862(15) 0.0190(6) Uani 1 1 d . . . C9 C -0.7857(6) 0.65726(14) -0.35111(15) 0.0237(7) Uani 1 1 d . . . H9 H -0.6322 0.6476 -0.3198 0.028 Uiso 1 1 calc R . . C10 C -0.9280(6) 0.71323(14) -0.33980(15) 0.0254(7) Uani 1 1 d . . . H10 H -0.8716 0.7430 -0.3016 0.031 Uiso 1 1 calc R . . C11 C -1.1538(6) 0.72509(14) -0.38516(16) 0.0259(7) Uani 1 1 d . . . H11 H -1.2573 0.7629 -0.3785 0.031 Uiso 1 1 calc R . . C12 C -1.2255(6) 0.68040(14) -0.44052(16) 0.0259(7) Uani 1 1 d . . . H12 H -1.3821 0.6886 -0.4712 0.031 Uiso 1 1 calc R . . C13 C -0.1760(6) 0.37466(13) -0.20507(15) 0.0191(6) Uani 1 1 d . . . C14 C 0.0698(6) 0.41378(14) -0.09184(14) 0.0225(7) Uani 1 1 d . . . H14A H -0.1097 0.4260 -0.0769 0.027 Uiso 1 1 calc R . . H14B H 0.1848 0.4526 -0.0865 0.027 Uiso 1 1 calc R . . C15 C 0.1814(6) 0.36067(14) -0.03907(15) 0.0262(7) Uani 1 1 d . . . H15A H 0.0712 0.3212 -0.0458 0.031 Uiso 1 1 calc R . . H15B H 0.3644 0.3498 -0.0523 0.031 Uiso 1 1 calc R . . C16 C 0.1853(6) 0.38177(14) 0.04194(15) 0.0217(7) Uani 1 1 d . . . C17 C 0.3713(6) 0.42659(15) 0.07050(16) 0.0297(7) Uani 1 1 d . . . H17 H 0.5018 0.4433 0.0393 0.036 Uiso 1 1 calc R . . C18 C 0.3656(6) 0.44662(15) 0.14427(16) 0.0329(8) Uani 1 1 d . . . H18 H 0.4889 0.4778 0.1641 0.039 Uiso 1 1 calc R . . C19 C 0.1773(6) 0.42036(15) 0.18841(16) 0.0281(7) Uani 1 1 d . . . H19 H 0.1686 0.4326 0.2395 0.034 Uiso 1 1 calc R . . C20 C 0.0020(7) 0.37584(16) 0.15627(17) 0.0360(8) Uani 1 1 d . . . H20 H -0.1271 0.3579 0.1870 0.043 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 O1 0.0274(12) 0.0238(11) 0.0208(11) -0.0037(9) -0.0044(9) 0.0033(9) O2 0.0153(11) 0.0304(12) 0.0248(11) 0.0043(9) 0.0031(9) 0.0005(9) N1 0.0222(13) 0.0210(14) 0.0215(13) -0.0003(11) -0.0013(11) 0.0012(11) N2 0.0152(13) 0.0201(14) 0.0209(14) -0.0020(11) -0.0016(11) 0.0032(10) N3 0.0177(13) 0.0229(14) 0.0272(14) -0.0001(11) 0.0005(11) -0.0004(11) N4 0.0192(13) 0.0245(14) 0.0247(14) 0.0039(11) 0.0004(11) 0.0033(11) N5 0.0143(14) 0.0329(16) 0.0190(13) -0.0021(11) -0.0022(11) 0.0002(11) N6 0.0335(16) 0.0411(18) 0.0221(14) -0.0052(12) 0.0022(12) -0.0078(13) C1 0.0258(17) 0.0216(16) 0.0216(16) -0.0064(13) -0.0003(13) 0.0012(13) C2 0.0254(17) 0.0202(16) 0.0276(17) 0.0007(13) 0.0009(14) 0.0055(13) C3 0.0149(15) 0.0180(15) 0.0215(15) 0.0013(12) -0.0004(12) -0.0019(12) C4 0.0148(15) 0.0171(15) 0.0188(15) 0.0012(12) -0.0014(12) -0.0012(11) C5 0.0192(15) 0.0205(16) 0.0163(15) 0.0031(13) 0.0007(12) -0.0001(12) C6 0.0173(15) 0.0197(16) 0.0249(16) 0.0013(12) -0.0014(13) 0.0018(12) C7 0.0203(16) 0.0214(16) 0.0250(16) 0.0005(13) 0.0002(13) 0.0052(13) C8 0.0180(15) 0.0184(16) 0.0209(15) 0.0049(12) 0.0043(12) -0.0016(12) C9 0.0214(16) 0.0265(17) 0.0227(16) 0.0025(13) -0.0033(13) 0.0001(14) C10 0.0265(17) 0.0270(18) 0.0223(16) -0.0064(13) -0.0030(14) -0.0013(14) C11 0.0245(17) 0.0215(17) 0.0311(18) -0.0059(13) -0.0024(14) 0.0057(13) C12 0.0211(17) 0.0257(17) 0.0303(17) -0.0017(14) -0.0034(13) 0.0052(13) C13 0.0195(16) 0.0169(15) 0.0208(15) 0.0050(12) -0.0006(13) 0.0029(12) C14 0.0209(16) 0.0294(18) 0.0170(15) -0.0045(13) 0.0001(12) -0.0010(13) C15 0.0307(18) 0.0252(18) 0.0225(16) -0.0022(13) -0.0001(14) -0.0008(14) C16 0.0230(16) 0.0230(16) 0.0190(15) 0.0003(13) 0.0014(13) 0.0042(13) C17 0.0294(18) 0.0351(19) 0.0252(17) -0.0037(14) 0.0051(14) -0.0101(15) C18 0.037(2) 0.0344(19) 0.0271(18) -0.0037(15) -0.0020(15) -0.0074(16) C19 0.0338(19) 0.0326(19) 0.0178(16) -0.0071(14) 0.0019(14) -0.0019(15) C20 0.041(2) 0.043(2) 0.0245(18) -0.0028(15) 0.0078(15) -0.0103(17) _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 O1 C5 1.235(3) . ? O2 C13 1.241(3) . ? N1 C1 1.339(3) . ? N1 C4 1.345(3) . ? N2 C5 1.345(3) . ? N2 C6 1.462(3) . ? N3 C12 1.347(3) . ? N3 C8 1.351(3) . ? N4 C2 1.346(3) . ? N4 C3 1.348(3) . ? N5 C13 1.335(3) . ? N5 C14 1.466(3) . ? N6 C20 1.344(4) . ? N6 C16 1.345(4) . ? C1 C2 1.378(4) . ? C3 C4 1.407(3) . ? C3 C13 1.515(4) . ? C4 C5 1.503(4) . ? C6 C7 1.527(4) . ? C7 C8 1.512(4) . ? C8 C9 1.393(4) . ? C9 C10 1.381(4) . ? C10 C11 1.381(4) . ? C11 C12 1.385(4) . ? C14 C15 1.532(4) . ? C15 C16 1.509(4) . ? C16 C17 1.393(4) . ? C17 C18 1.382(4) . ? C18 C19 1.378(4) . ? C19 C20 1.377(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 116.8(2) . . ? C5 N2 C6 119.3(2) . . ? C12 N3 C8 116.8(2) . . ? C2 N4 C3 116.3(2) . . ? C13 N5 C14 121.8(3) . . ? C20 N6 C16 116.8(3) . . ? N1 C1 C2 122.0(3) . . ? N4 C2 C1 122.1(3) . . ? N4 C3 C4 121.2(2) . . ? N4 C3 C13 115.5(2) . . ? C4 C3 C13 123.1(2) . . ? N1 C4 C3 121.2(2) . . ? N1 C4 C5 117.1(2) . . ? C3 C4 C5 121.6(2) . . ? O1 C5 N2 122.6(3) . . ? O1 C5 C4 120.5(2) . . ? N2 C5 C4 116.9(2) . . ? N2 C6 C7 112.2(2) . . ? C8 C7 C6 111.2(2) . . ? N3 C8 C9 122.2(3) . . ? N3 C8 C7 116.9(2) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 119.8(3) . . ? C9 C10 C11 118.7(3) . . ? C10 C11 C12 118.3(3) . . ? N3 C12 C11 124.2(3) . . ? O2 C13 N5 124.3(3) . . ? O2 C13 C3 119.5(2) . . ? N5 C13 C3 116.0(2) . . ? N5 C14 C15 112.5(2) . . ? C16 C15 C14 111.6(2) . . ? N6 C16 C17 122.0(3) . . ? N6 C16 C15 117.1(3) . . ? C17 C16 C15 121.0(3) . . ? C18 C17 C16 119.8(3) . . ? C19 C18 C17 118.6(3) . . ? C20 C19 C18 118.1(3) . . ? N6 C20 C19 124.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -3.0(4) . . . . ? C3 N4 C2 C1 -1.4(4) . . . . ? N1 C1 C2 N4 5.2(4) . . . . ? C2 N4 C3 C4 -4.1(4) . . . . ? C2 N4 C3 C13 171.5(2) . . . . ? C1 N1 C4 C3 -2.5(4) . . . . ? C1 N1 C4 C5 173.0(2) . . . . ? N4 C3 C4 N1 6.3(4) . . . . ? C13 C3 C4 N1 -169.0(3) . . . . ? N4 C3 C4 C5 -169.0(3) . . . . ? C13 C3 C4 C5 15.7(4) . . . . ? C6 N2 C5 O1 1.2(4) . . . . ? C6 N2 C5 C4 -177.7(2) . . . . ? N1 C4 C5 O1 -159.1(2) . . . . ? C3 C4 C5 O1 16.4(4) . . . . ? N1 C4 C5 N2 19.8(4) . . . . ? C3 C4 C5 N2 -164.7(2) . . . . ? C5 N2 C6 C7 74.4(3) . . . . ? N2 C6 C7 C8 -169.8(2) . . . . ? C12 N3 C8 C9 -0.1(4) . . . . ? C12 N3 C8 C7 178.4(2) . . . . ? C6 C7 C8 N3 -75.1(3) . . . . ? C6 C7 C8 C9 103.4(3) . . . . ? N3 C8 C9 C10 -1.2(4) . . . . ? C7 C8 C9 C10 -179.6(3) . . . . ? C8 C9 C10 C11 1.5(4) . . . . ? C9 C10 C11 C12 -0.6(4) . . . . ? C8 N3 C12 C11 1.0(4) . . . . ? C10 C11 C12 N3 -0.7(4) . . . . ? C14 N5 C13 O2 1.9(4) . . . . ? C14 N5 C13 C3 -174.5(2) . . . . ? N4 C3 C13 O2 -124.6(3) . . . . ? C4 C3 C13 O2 50.9(4) . . . . ? N4 C3 C13 N5 51.9(3) . . . . ? C4 C3 C13 N5 -132.6(3) . . . . ? C13 N5 C14 C15 101.3(3) . . . . ? N5 C14 C15 C16 -177.5(2) . . . . ? C20 N6 C16 C17 0.5(4) . . . . ? C20 N6 C16 C15 -178.8(3) . . . . ? C14 C15 C16 N6 105.5(3) . . . . ? C14 C15 C16 C17 -73.8(4) . . . . ? N6 C16 C17 C18 -1.2(5) . . . . ? C15 C16 C17 C18 178.0(3) . . . . ? C16 C17 C18 C19 1.3(5) . . . . ? C17 C18 C19 C20 -0.7(5) . . . . ? C16 N6 C20 C19 0.2(5) . . . . ? C18 C19 C20 N6 -0.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B N3 0.86(3) 2.37(3) 3.165(3) 155(3) 3_364 N5 H5A O2 0.89(4) 2.02(4) 2.825(3) 150(3) 1_655 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.256 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.063 # Attachment 'lgnio_noDisorder_edited_23Nov06.cif' data_lgnio_nodisorder _database_code_depnum_ccdc_archive 'CCDC 296871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H78 B2 F8 N24 Ni4 O8' _chemical_formula_weight 2494.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 21.7134(3) _cell_length_b 21.8434(3) _cell_length_c 26.24680(10) _cell_angle_alpha 108.8230(10) _cell_angle_beta 103.0400(10) _cell_angle_gamma 90.7210(10) _cell_volume 11429.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6588 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 24.71 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ? _exptl_special_details ; Calculations of molar mass, density, F_000 and absorption cooefficient are based upon our best estimate of stoichiometry from a model that included the well-defined components of the structure (the two cations and 4 BF4- groups) and the highly disordered components that were later SQUEEZEd (four BF4- anions and approximately 10 acetonitrile solvate molecules). These acetonitrile solvent molecules and four BF4- anions were marginally visible in electron density maps. Because of this disorder and the large amounts of missing electron density, the structure was subjected to the SQUEEZE procedure from the PLATON suite (Spek, A.L. (1990), Acta Cryst. A46, C34). Further details are provided under the descriptor _refine_special_details. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 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 38305 _diffrn_reflns_av_R_equivalents 0.0996 _diffrn_reflns_av_sigmaI/netI 0.1778 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 24.71 _reflns_number_total 38305 _reflns_number_gt 13885 _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 'XP in SHELXTL' _computing_publication_material 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. Refinements with four ordered BF4s and four disordered BF4s distributed over 6 sites and 10 disordered CH3CN moieties converged at R1 (I>2sig(I)) ~0.13. There was much residual uninterpretable electron density away from the grid complexes. Therefore, the two crystallographically independent Ni4 grid complexes and the four ordered BF4 groups were retained and the structure subjected to SQUEEZE from the PLATON suite (AL Spek, Acta Cryst A46, C34 (1990)). A total solvent-accessible void volume of 4264 A^3 containing 1349 electrons per unit cell was calculated. Final refinement converged at R1 = 0.0629 (0.072 with inclusion of contribution from contents of the void volume). Somewhat to our surprise 4 of the 8 hydrogens turned up -- none were exactly symmetrical with the shorter O-H separations in the range 1.12-1.16 A and the longer separations in the range 1.29-1.21 A. On reflection this is not so surprising as the crystal environment is full of charges and dipoles. These hydrogens, curiously are all on opposite sides of the square and all four observed O..H..O pointed "North-South". Four of the pyridyl rings on one of the two crystallographically independent molecules have anomalously high apparent thermal motion, due to apparent libration about CH2-CH2 bonds. A disorder model was imposed, including bond distance and planarity restraints; atoms were restricted to isotropic displacement factors with tight similarity restraints imposed on sites closer than 1 A apart, but this did not lead to an improved model. Significant residual electron density remained in the vicinity of these putatively disordered pyridyl rings. Although the ellipsoids are rather eccentric, their sizes and relative orientations seem more consistent with free librational motion than with two discrete non-resolved conformations. No significant residual electron density was present in these regions, and R1 and wR2 were slightly lower. ; _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^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 38305 _refine_ls_number_parameters 2270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 0.746 _refine_ls_restrained_S_all 0.746 _refine_ls_shift/su_max 0.430 _refine_ls_shift/su_mean 0.014 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 0.63859(4) 0.14781(4) 0.17910(3) 0.0633(2) Uani 1 1 d . . . Ni2 Ni 0.95872(4) 0.14270(3) 0.18129(3) 0.0555(2) Uani 1 1 d . . . Ni3 Ni 0.61446(3) 0.41642(3) 0.08778(3) 0.0496(2) Uani 1 1 d . . . Ni4 Ni 0.93812(3) 0.41316(3) 0.09154(3) 0.04698(19) Uani 1 1 d . . . O1 O 0.7827(2) 0.2488(2) 0.31683(15) 0.0842(14) Uani 1 1 d . . . H1A H 0.8371 0.2437 0.3147 0.101 Uiso 1 1 calc R . . O2 O 0.89266(19) 0.24348(18) 0.31798(14) 0.0710(12) Uani 1 1 d . . . O3 O 0.75808(19) 0.5306(3) 0.21841(18) 0.140(2) Uani 1 1 d . . . H3A H 0.8135 0.5268 0.2197 0.168 Uiso 1 1 calc R . . O4 O 0.86867(17) 0.5233(2) 0.22303(17) 0.0954(16) Uani 1 1 d . . . O5 O 0.60280(16) 0.13417(16) 0.01431(13) 0.0519(9) Uani 1 1 d . . . H5A H 0.5964 0.1794 -0.0023 0.062 Uiso 1 1 calc R . . O6 O 0.59041(17) 0.22580(15) -0.01649(12) 0.0510(10) Uani 1 1 d . . . O7 O 0.90238(16) 0.13182(15) 0.01731(13) 0.0529(10) Uani 1 1 d . . . H7C H 0.9011 0.1781 0.0020 0.063 Uiso 1 1 calc R . . O8 O 0.89949(16) 0.22402(16) -0.01361(13) 0.0492(9) Uani 1 1 d . . . N1 N 0.7340(2) 0.1464(2) 0.17393(17) 0.0551(13) Uani 1 1 d . . . N2 N 0.6864(3) 0.1958(3) 0.25828(19) 0.0728(15) Uani 1 1 d . . . N3 N 0.5507(3) 0.1625(2) 0.1985(2) 0.0760(15) Uani 1 1 d . . . N4 N 0.8604(2) 0.1418(2) 0.17537(19) 0.0567(12) Uani 1 1 d . . . N5 N 0.9548(3) 0.1883(2) 0.26094(17) 0.0640(14) Uani 1 1 d . . . N6 N 1.0588(2) 0.1594(2) 0.2035(2) 0.0673(14) Uani 1 1 d . . . N7 N 0.71134(19) 0.4113(2) 0.08291(17) 0.0483(11) Uani 1 1 d . . . N8 N 0.6633(2) 0.4864(2) 0.15838(18) 0.0629(13) Uani 1 1 d . . . N9 N 0.52877(19) 0.4261(2) 0.11395(17) 0.0489(11) Uani 1 1 d . . . N10 N 0.83850(19) 0.40928(19) 0.08481(17) 0.0417(10) Uani 1 1 d . . . N11 N 0.9301(2) 0.48122(19) 0.16342(16) 0.0504(12) Uani 1 1 d . . . N12 N 1.0381(2) 0.4230(2) 0.11583(18) 0.0535(12) Uani 1 1 d . . . N13 N 0.6371(2) 0.2341(2) 0.15784(17) 0.0527(12) Uani 1 1 d . . . N14 N 0.6056(2) 0.1135(2) 0.09458(17) 0.0571(12) Uani 1 1 d . . . N15 N 0.6455(3) 0.0527(3) 0.1832(2) 0.0720(15) Uani 1 1 d . . . N16 N 0.62892(18) 0.3398(2) 0.12165(16) 0.0472(11) Uani 1 1 d . . . N17 N 0.58298(18) 0.33496(19) 0.02020(14) 0.0392(10) Uani 1 1 d . . . N18 N 0.6046(2) 0.4757(2) 0.0350(2) 0.0575(13) Uani 1 1 d . . . N19 N 0.9504(2) 0.2297(2) 0.16024(17) 0.0522(12) Uani 1 1 d . . . N20 N 0.9451(2) 0.1107(2) 0.09708(16) 0.0499(11) Uani 1 1 d . . . N21 N 0.9548(2) 0.0462(2) 0.18192(19) 0.0612(13) Uani 1 1 d . . . N22 N 0.93935(18) 0.33550(19) 0.12489(17) 0.0423(11) Uani 1 1 d . . . N23 N 0.93054(18) 0.3324(2) 0.02409(15) 0.0415(10) Uani 1 1 d . . . N24 N 0.9205(2) 0.4744(2) 0.0403(2) 0.0575(13) Uani 1 1 d . . . C1 C 0.7534(3) 0.1144(3) 0.1289(2) 0.0589(16) Uani 1 1 d . . . H1 H 0.7227 0.0931 0.0953 0.071 Uiso 1 1 d R . . C2 C 0.8166(3) 0.1122(3) 0.1295(2) 0.0526(15) Uani 1 1 d . . . H2 H 0.8288 0.0889 0.0965 0.063 Uiso 1 1 d R . . C3 C 0.8425(3) 0.1759(3) 0.2226(2) 0.0535(15) Uani 1 1 d . . . C4 C 0.7775(3) 0.1776(3) 0.2209(2) 0.0558(16) Uani 1 1 d . . . C5 C 0.7453(4) 0.2108(3) 0.2698(2) 0.0609(17) Uani 1 1 d . . . C6 C 0.6552(3) 0.2218(4) 0.3045(2) 0.093(2) Uani 1 1 d . . . H6A H 0.6410 0.2650 0.3057 0.112 Uiso 1 1 d R . . H6B H 0.6858 0.2267 0.3401 0.112 Uiso 1 1 d R . . C7 C 0.5990(4) 0.1741(4) 0.2967(3) 0.099(2) Uani 1 1 d . . . H7A H 0.6129 0.1297 0.2891 0.119 Uiso 1 1 d R . . H7B H 0.5855 0.1858 0.3319 0.119 Uiso 1 1 d R . . C8 C 0.5421(4) 0.1722(4) 0.2510(3) 0.095(2) Uani 1 1 d . . . C9 C 0.4829(5) 0.1817(4) 0.2615(3) 0.098(2) Uani 1 1 d . . . H9 H 0.4754 0.1865 0.2968 0.118 Uiso 1 1 d R . . C10 C 0.4319(4) 0.1833(4) 0.2208(4) 0.113(3) Uani 1 1 d . . . H10 H 0.3908 0.1907 0.2272 0.136 Uiso 1 1 d R . . C11 C 0.4392(4) 0.1754(3) 0.1672(3) 0.092(2) Uani 1 1 d . . . H11 H 0.4053 0.1750 0.1370 0.111 Uiso 1 1 d R . . C12 C 0.4994(4) 0.1655(3) 0.1606(3) 0.081(2) Uani 1 1 d . . . H12 H 0.5051 0.1610 0.1248 0.097 Uiso 1 1 d R . . C15 C 0.9018(4) 0.2052(3) 0.2713(2) 0.0621(18) Uani 1 1 d . . . C16 C 1.0100(3) 0.2114(3) 0.3085(2) 0.0721(18) Uani 1 1 d . . . H16A H 0.9978 0.2125 0.3429 0.086 Uiso 1 1 d R . . H16B H 1.0260 0.2561 0.3133 0.086 Uiso 1 1 d R . . C17 C 1.0608(3) 0.1650(3) 0.2990(2) 0.085(2) Uani 1 1 d . . . H17A H 1.0431 0.1198 0.2901 0.102 Uiso 1 1 d R . . H17B H 1.0933 0.1765 0.3345 0.102 Uiso 1 1 d R . . C18 C 1.0939(4) 0.1687(3) 0.2548(3) 0.0731(19) Uani 1 1 d . . . C19 C 1.1598(4) 0.1845(3) 0.2679(3) 0.099(3) Uani 1 1 d . . . H19 H 1.1852 0.1904 0.3040 0.119 Uiso 1 1 d R . . C20 C 1.1878(4) 0.1866(4) 0.2260(4) 0.117(3) Uani 1 1 d . . . H20 H 1.2322 0.1979 0.2343 0.140 Uiso 1 1 d R . . C21 C 1.1522(4) 0.1781(3) 0.1745(3) 0.098(2) Uani 1 1 d . . . H21 H 1.1699 0.1784 0.1446 0.118 Uiso 1 1 d R . . C22 C 1.0870(3) 0.1648(3) 0.1648(3) 0.076(2) Uani 1 1 d . . . H22 H 1.0609 0.1608 0.1294 0.092 Uiso 1 1 d R . . C31 C 0.7313(3) 0.3743(2) 0.0392(2) 0.0471(14) Uani 1 1 d . . . H31 H 0.7010 0.3477 0.0072 0.056 Uiso 1 1 d R . . C32 C 0.7951(3) 0.3735(2) 0.0404(2) 0.0416(13) Uani 1 1 d . . . H32 H 0.8078 0.3469 0.0086 0.050 Uiso 1 1 d R . . C33 C 0.8201(3) 0.4477(3) 0.1298(2) 0.0499(14) Uani 1 1 d . . . C34 C 0.7556(3) 0.4499(2) 0.1290(2) 0.0490(14) Uani 1 1 d . . . C35 C 0.7252(3) 0.4913(3) 0.1728(3) 0.080(2) Uani 1 1 d . . . C36 C 0.6333(3) 0.5349(3) 0.1976(3) 0.100(3) Uani 1 1 d . . . H36A H 0.6565 0.5783 0.2087 0.120 Uiso 1 1 d R . . H36B H 0.6372 0.5226 0.2312 0.120 Uiso 1 1 d R . . C37 C 0.5654(3) 0.5394(3) 0.1700(3) 0.086(2) Uani 1 1 d . . . H37A H 0.5491 0.5751 0.1964 0.103 Uiso 1 1 d R . . H37B H 0.5629 0.5511 0.1362 0.103 Uiso 1 1 d R . . C38 C 0.5207(3) 0.4790(3) 0.1562(2) 0.0630(17) Uani 1 1 d . . . C39 C 0.4751(3) 0.4782(3) 0.1856(2) 0.0680(17) Uani 1 1 d . . . H39 H 0.4711 0.5163 0.2146 0.082 Uiso 1 1 d R . . C40 C 0.4349(3) 0.4227(3) 0.1707(2) 0.0755(19) Uani 1 1 d . . . H40 H 0.4049 0.4215 0.1917 0.091 Uiso 1 1 d R . . C41 C 0.4408(3) 0.3671(3) 0.1265(2) 0.0721(18) Uani 1 1 d . . . H41 H 0.4125 0.3290 0.1149 0.087 Uiso 1 1 d R . . C42 C 0.4882(3) 0.3723(3) 0.0998(2) 0.0577(15) Uani 1 1 d . . . H42 H 0.4929 0.3353 0.0701 0.069 Uiso 1 1 d R . . C45 C 0.8756(3) 0.4868(3) 0.1756(3) 0.0616(16) Uani 1 1 d . . . C46 C 0.9854(3) 0.5232(3) 0.2049(2) 0.0741(19) Uani 1 1 d . . . H46A H 1.0026 0.5020 0.2325 0.089 Uiso 1 1 d R . . H46B H 0.9717 0.5657 0.2244 0.089 Uiso 1 1 d R . . C47 C 1.0368(3) 0.5334(3) 0.1757(2) 0.0714(18) Uani 1 1 d . . . H47A H 1.0162 0.5456 0.1431 0.086 Uiso 1 1 d R . . H47B H 1.0678 0.5701 0.2012 0.086 Uiso 1 1 d R . . C48 C 1.0718(3) 0.4754(3) 0.1563(2) 0.0529(15) Uani 1 1 d . . . C49 C 1.1371(3) 0.4763(3) 0.1808(2) 0.0617(16) Uani 1 1 d . . . H49 H 1.1597 0.5135 0.2097 0.074 Uiso 1 1 d R . . C50 C 1.1672(3) 0.4201(3) 0.1606(2) 0.0708(18) Uani 1 1 d . . . H50 H 1.2111 0.4190 0.1758 0.085 Uiso 1 1 d R . . C51 C 1.1335(3) 0.3660(3) 0.1201(2) 0.0635(17) Uani 1 1 d . . . H51 H 1.1527 0.3271 0.1066 0.076 Uiso 1 1 d R . . C52 C 1.0697(3) 0.3695(3) 0.0986(2) 0.0591(16) Uani 1 1 d . . . H52 H 1.0461 0.3331 0.0693 0.071 Uiso 1 1 d R . . C61 C 0.6485(3) 0.2937(3) 0.1931(2) 0.0661(18) Uani 1 1 d . . . H61 H 0.6607 0.3006 0.2318 0.079 Uiso 1 1 d R . . C62 C 0.6455(3) 0.3471(3) 0.1758(2) 0.0632(17) Uani 1 1 d . . . H62 H 0.6538 0.3895 0.2025 0.076 Uiso 1 1 d R . . C63 C 0.6180(2) 0.2783(3) 0.08392(19) 0.0396(13) Uani 1 1 d . . . C64 C 0.6219(2) 0.2236(3) 0.1018(2) 0.0474(14) Uani 1 1 d . . . C65 C 0.6098(2) 0.1544(3) 0.0673(2) 0.0525(15) Uani 1 1 d . . . C66 C 0.5873(3) 0.0460(3) 0.0607(2) 0.0673(17) Uani 1 1 d . . . H66A H 0.6239 0.0256 0.0477 0.081 Uiso 1 1 d R . . H66B H 0.5527 0.0426 0.0278 0.081 Uiso 1 1 d R . . C67 C 0.5632(3) 0.0102(3) 0.0958(2) 0.0777(19) Uani 1 1 d . . . H67A H 0.5307 0.0352 0.1124 0.093 Uiso 1 1 d R . . H67B H 0.5421 -0.0329 0.0710 0.093 Uiso 1 1 d R . . C68 C 0.6135(3) 0.0016(4) 0.1423(3) 0.0717(19) Uani 1 1 d . . . C69 C 0.6259(3) -0.0619(3) 0.1395(3) 0.084(2) Uani 1 1 d . . . H69 H 0.6037 -0.0987 0.1098 0.101 Uiso 1 1 d R . . C70 C 0.6742(4) -0.0717(4) 0.1815(3) 0.091(2) Uani 1 1 d . . . H70 H 0.6847 -0.1138 0.1816 0.110 Uiso 1 1 d R . . C71 C 0.7057(4) -0.0162(4) 0.2242(3) 0.090(2) Uani 1 1 d . . . H71 H 0.7380 -0.0208 0.2536 0.108 Uiso 1 1 d R . . C72 C 0.6899(3) 0.0423(3) 0.2234(3) 0.081(2) Uani 1 1 d . . . H72 H 0.7111 0.0789 0.2538 0.097 Uiso 1 1 d R . . C75 C 0.5958(2) 0.2787(3) 0.02507(19) 0.0425(13) Uani 1 1 d . . . C76 C 0.5505(2) 0.3324(3) -0.03613(18) 0.0501(14) Uani 1 1 d . . . H76A H 0.5819 0.3260 -0.0591 0.060 Uiso 1 1 d R . . H76B H 0.5170 0.2956 -0.0535 0.060 Uiso 1 1 d R . . C77 C 0.5224(3) 0.3960(3) -0.0338(2) 0.0560(15) Uani 1 1 d . . . H77A H 0.4969 0.4054 -0.0057 0.067 Uiso 1 1 d R . . H77B H 0.4932 0.3912 -0.0701 0.067 Uiso 1 1 d R . . C78 C 0.5722(3) 0.4521(3) -0.0185(3) 0.0589(16) Uani 1 1 d . . . C79 C 0.5849(3) 0.4765(3) -0.0584(3) 0.081(2) Uani 1 1 d . . . H79 H 0.5629 0.4571 -0.0962 0.097 Uiso 1 1 d R . . C80 C 0.6313(4) 0.5257(4) -0.0449(4) 0.101(3) Uani 1 1 d . . . H80 H 0.6412 0.5432 -0.0711 0.121 Uiso 1 1 d R . . C81 C 0.6632(3) 0.5511(3) 0.0091(4) 0.093(2) Uani 1 1 d . . . H81 H 0.6956 0.5859 0.0210 0.111 Uiso 1 1 d R . . C82 C 0.6487(3) 0.5266(3) 0.0494(3) 0.0751(19) Uani 1 1 d . . . H82 H 0.6694 0.5465 0.0875 0.090 Uiso 1 1 d R . . C91 C 0.9585(3) 0.2901(3) 0.1972(2) 0.0561(15) Uani 1 1 d . . . H91 H 0.9676 0.2966 0.2358 0.067 Uiso 1 1 d R . . C92 C 0.9518(2) 0.3423(3) 0.1785(2) 0.0509(15) Uani 1 1 d . . . H92 H 0.9571 0.3850 0.2048 0.061 Uiso 1 1 d R . . C93 C 0.9289(2) 0.2753(3) 0.0873(2) 0.0401(13) Uani 1 1 d . . . C94 C 0.9339(2) 0.2207(2) 0.1045(2) 0.0409(13) Uani 1 1 d . . . C95 C 0.9268(2) 0.1504(3) 0.0706(2) 0.0466(14) Uani 1 1 d . . . C96 C 0.9443(3) 0.0423(2) 0.0624(2) 0.0548(15) Uani 1 1 d . . . H96A H 0.9575 0.0392 0.0280 0.066 Uiso 1 1 d R . . H96B H 0.9004 0.0215 0.0520 0.066 Uiso 1 1 d R . . C97 C 0.9880(3) 0.0065(3) 0.0950(2) 0.0637(17) Uani 1 1 d . . . H97A H 0.9948 -0.0359 0.0694 0.076 Uiso 1 1 d R . . H97B H 1.0296 0.0327 0.1113 0.076 Uiso 1 1 d R . . C98 C 0.9633(3) -0.0053(3) 0.1404(2) 0.0594(16) Uani 1 1 d . . . C99 C 0.9524(3) -0.0696(3) 0.1398(3) 0.0734(18) Uani 1 1 d . . . H99 H 0.9584 -0.1056 0.1099 0.088 Uiso 1 1 d R . . C100 C 0.9303(3) -0.0801(3) 0.1818(3) 0.080(2) Uani 1 1 d . . . H100 H 0.9222 -0.1230 0.1817 0.096 Uiso 1 1 d R . . C101 C 0.9190(3) -0.0277(4) 0.2234(3) 0.083(2) Uani 1 1 d . . . H101 H 0.9052 -0.0337 0.2535 0.100 Uiso 1 1 d R . . C102 C 0.9315(3) 0.0355(3) 0.2232(2) 0.0694(18) Uani 1 1 d . . . H102 H 0.9239 0.0718 0.2521 0.083 Uiso 1 1 d R . . C105 C 0.9176(2) 0.2765(3) 0.0284(2) 0.0402(13) Uani 1 1 d . . . C106 C 0.9304(3) 0.3312(2) -0.0323(2) 0.0554(15) Uani 1 1 d . . . H10A H 0.8861 0.3236 -0.0549 0.066 Uiso 1 1 d R . . H10B H 0.9542 0.2952 -0.0498 0.066 Uiso 1 1 d R . . C107 C 0.9604(3) 0.3943(3) -0.0309(2) 0.0530(15) Uani 1 1 d . . . H10C H 1.0029 0.4038 -0.0049 0.064 Uiso 1 1 d R . . H10D H 0.9660 0.3911 -0.0680 0.064 Uiso 1 1 d R . . C108 C 0.9221(3) 0.4497(3) -0.0135(3) 0.0627(16) Uani 1 1 d . . . C109 C 0.8855(3) 0.4734(3) -0.0534(3) 0.0773(19) Uani 1 1 d . . . H109 H 0.8864 0.4553 -0.0914 0.093 Uiso 1 1 d R . . C110 C 0.8477(3) 0.5242(4) -0.0361(4) 0.103(3) Uani 1 1 d . . . H110 H 0.8229 0.5434 -0.0605 0.124 Uiso 1 1 d R . . C111 C 0.8488(3) 0.5497(3) 0.0187(4) 0.088(2) Uani 1 1 d . . . H111 H 0.8254 0.5851 0.0327 0.106 Uiso 1 1 d R . . C112 C 0.8856(3) 0.5242(3) 0.0554(3) 0.0645(17) Uani 1 1 d . . . H112 H 0.8853 0.5424 0.0935 0.077 Uiso 1 1 d R . . Ni5 Ni 0.21110(4) 0.68565(4) 0.44469(3) 0.0697(3) Uani 1 1 d . . . Ni6 Ni 0.53728(4) 0.69506(3) 0.45790(3) 0.0702(3) Uani 1 1 d . . . Ni7 Ni 0.16733(3) 0.88503(3) 0.27965(3) 0.0524(2) Uani 1 1 d . . . Ni8 Ni 0.49103(3) 0.88869(3) 0.28691(3) 0.0520(2) Uani 1 1 d . . . O9 O 0.3473(2) 0.81616(19) 0.57135(15) 0.0890(14) Uani 1 1 d . . . H9A H 0.4031 0.8130 0.5749 0.107 Uiso 1 1 calc R . . O10 O 0.4577(2) 0.81224(18) 0.57965(15) 0.0827(14) Uani 1 1 d . . . O11 O 0.30206(19) 1.02778(17) 0.39276(14) 0.0655(11) Uani 1 1 d . . . H11A H 0.3578 1.0261 0.3949 0.079 Uiso 1 1 calc R . . O12 O 0.41431(18) 1.02589(17) 0.39847(14) 0.0660(11) Uani 1 1 d . . . O13 O 0.17572(17) 0.61665(16) 0.27373(15) 0.0624(11) Uani 1 1 d . . . H13E H 0.1644 0.6510 0.2458 0.075 Uiso 1 1 calc R . . O14 O 0.15299(17) 0.68401(17) 0.21695(13) 0.0565(10) Uani 1 1 d . . . O15 O 0.4972(2) 0.62220(17) 0.28721(15) 0.0759(13) Uani 1 1 d . . . H15E H 0.4876 0.6567 0.2593 0.091 Uiso 1 1 calc R . . O16 O 0.47878(18) 0.68717(17) 0.22812(13) 0.0654(11) Uani 1 1 d . . . N25 N 0.3098(2) 0.6798(2) 0.44618(19) 0.0621(14) Uani 1 1 d . . . N26 N 0.2552(3) 0.7530(3) 0.5176(2) 0.0737(16) Uani 1 1 d . . . N28 N 0.4386(2) 0.6817(2) 0.45091(17) 0.0561(13) Uani 1 1 d . . . N29 N 0.5259(3) 0.7603(2) 0.52956(19) 0.0713(16) Uani 1 1 d . . . N31 N 0.2647(2) 0.8813(2) 0.27635(16) 0.0478(11) Uani 1 1 d . . . N32 N 0.2099(3) 0.9708(2) 0.33714(17) 0.0579(13) Uani 1 1 d . . . N33 N 0.0810(2) 0.9017(3) 0.30321(18) 0.0609(13) Uani 1 1 d . . . N34 N 0.3921(2) 0.8808(2) 0.28070(16) 0.0505(12) Uani 1 1 d . . . N35 N 0.4785(3) 0.9727(2) 0.34384(17) 0.0587(13) Uani 1 1 d . . . N36 N 0.5913(2) 0.9123(2) 0.31002(16) 0.0575(13) Uani 1 1 d . . . N37 N 0.2092(2) 0.7522(2) 0.39949(18) 0.0532(12) Uani 1 1 d . . . N38 N 0.1819(2) 0.6271(2) 0.36415(18) 0.0628(13) Uani 1 1 d . . . N40 N 0.1900(2) 0.8285(2) 0.33501(17) 0.0514(12) Uani 1 1 d . . . N41 N 0.1418(2) 0.7909(2) 0.22909(16) 0.0523(12) Uani 1 1 d . . . N42 N 0.1485(2) 0.9190(2) 0.21098(16) 0.0516(12) Uani 1 1 d . . . N43 N 0.5161(2) 0.7581(2) 0.41003(18) 0.0574(13) Uani 1 1 d . . . N44 N 0.5315(2) 0.6359(2) 0.37956(18) 0.0686(15) Uani 1 1 d . . . N46 N 0.4994(2) 0.8347(2) 0.34342(17) 0.0512(12) Uani 1 1 d . . . N47 N 0.4909(2) 0.7944(2) 0.23801(16) 0.0498(12) Uani 1 1 d . . . N48 N 0.4714(2) 0.9209(2) 0.21725(16) 0.0507(12) Uani 1 1 d . . . C121 C 0.3315(4) 0.6360(3) 0.4060(2) 0.0685(18) Uani 1 1 d . . . H121 H 0.3038 0.6035 0.3759 0.082 Uiso 1 1 d R . . C122 C 0.3955(4) 0.6383(3) 0.4094(2) 0.0609(18) Uani 1 1 d . . . H122 H 0.4106 0.6084 0.3806 0.073 Uiso 1 1 d R . . C123 C 0.4166(4) 0.7252(3) 0.4917(2) 0.0586(16) Uani 1 1 d . . . C124 C 0.3521(4) 0.7246(3) 0.4894(2) 0.0634(18) Uani 1 1 d . . . C125 C 0.3150(4) 0.7663(3) 0.5285(2) 0.069(2) Uani 1 1 d . . . C126 C 0.2222(3) 0.7926(3) 0.5570(2) 0.082(2) Uani 1 1 d . . . H12A H 0.2087 0.8309 0.5466 0.099 Uiso 1 1 d R . . H12B H 0.2510 0.8087 0.5946 0.099 Uiso 1 1 d R . . C127 C 0.1641(4) 0.7539(4) 0.5581(3) 0.101(3) Uani 1 1 d . . . H12C H 0.1757 0.7114 0.5615 0.122 Uiso 1 1 d R . . H12D H 0.1498 0.7785 0.5916 0.122 Uiso 1 1 d R . . N27 N 0.1207(3) 0.7120(3) 0.4567(3) 0.0903(18) Uani 1 1 d . . . C128 C 0.1087(5) 0.7420(4) 0.5071(4) 0.111(3) Uani 1 1 d . . . C129 C 0.0492(6) 0.7619(6) 0.5125(5) 0.178(5) Uani 1 1 d . . . H129 H 0.0416 0.7811 0.5483 0.214 Uiso 1 1 d R . . C130 C 0.0012(5) 0.7534(6) 0.4656(5) 0.197(6) Uani 1 1 d . . . H130 H -0.0390 0.7686 0.4690 0.236 Uiso 1 1 d R . . C131 C 0.0119(5) 0.7235(5) 0.4140(5) 0.161(4) Uani 1 1 d . . . H131 H -0.0205 0.7163 0.3811 0.193 Uiso 1 1 d R . . C132 C 0.0715(5) 0.7045(4) 0.4124(3) 0.103(2) Uani 1 1 d . . . H132 H 0.0790 0.6839 0.3767 0.124 Uiso 1 1 d R . . C135 C 0.4698(4) 0.7691(3) 0.5366(2) 0.0632(18) Uani 1 1 d . . . C136 C 0.5780(4) 0.8012(3) 0.5736(2) 0.096(2) Uani 1 1 d . . . H13A H 0.5665 0.8083 0.6094 0.115 Uiso 1 1 d R . . H13B H 0.5837 0.8442 0.5695 0.115 Uiso 1 1 d R . . C137 C 0.6409(5) 0.7695(5) 0.5744(4) 0.172(5) Uani 1 1 d . . . H13C H 0.6346 0.7250 0.5756 0.207 Uiso 1 1 d R . . H13D H 0.6714 0.7954 0.6093 0.207 Uiso 1 1 d R . . N30 N 0.6341(4) 0.7306(3) 0.4766(4) 0.117(3) Uani 1 1 d . . . C138 C 0.6671(6) 0.7659(5) 0.5278(5) 0.134(4) Uani 1 1 d . . . C139 C 0.7266(8) 0.8004(8) 0.5362(8) 0.253(10) Uani 1 1 d . . . H139 H 0.7495 0.8239 0.5730 0.304 Uiso 1 1 d R . . C140 C 0.7533(8) 0.8008(11) 0.4912(9) 0.299(12) Uani 1 1 d . . . H140 H 0.7934 0.8231 0.4969 0.359 Uiso 1 1 d R . . C141 C 0.7158(8) 0.7662(8) 0.4381(6) 0.243(7) Uani 1 1 d . . . H141 H 0.7289 0.7656 0.4057 0.291 Uiso 1 1 d R . . C142 C 0.6590(6) 0.7330(5) 0.4339(6) 0.160(4) Uani 1 1 d . . . H142 H 0.6350 0.7093 0.3975 0.193 Uiso 1 1 d R . . C151 C 0.2869(3) 0.8343(2) 0.24082(19) 0.0509(15) Uani 1 1 d . . . H151 H 0.2579 0.8010 0.2127 0.061 Uiso 1 1 d R . . C152 C 0.3510(3) 0.8338(3) 0.2426(2) 0.0551(15) Uani 1 1 d . . . H152 H 0.3658 0.7994 0.2169 0.034(12) Uiso 1 1 d R . . C153 C 0.3710(3) 0.9292(3) 0.3180(2) 0.0497(15) Uani 1 1 d . . . C154 C 0.3061(3) 0.9293(2) 0.31601(19) 0.0480(15) Uani 1 1 d . . . C155 C 0.2710(3) 0.9795(3) 0.3518(2) 0.0516(15) Uani 1 1 d . . . C156 C 0.1754(3) 1.0235(3) 0.3665(2) 0.0670(17) Uani 1 1 d . . . H15A H 0.1986 1.0662 0.3748 0.080 Uiso 1 1 d R . . H15B H 0.1732 1.0186 0.4023 0.080 Uiso 1 1 d R . . C157 C 0.1088(3) 1.0205(3) 0.3332(2) 0.0741(19) Uani 1 1 d . . . H15C H 0.0903 1.0609 0.3504 0.089 Uiso 1 1 d R . . H15D H 0.1103 1.0185 0.2953 0.089 Uiso 1 1 d R . . C158 C 0.0674(3) 0.9627(4) 0.3290(2) 0.075(2) Uani 1 1 d . . . C159 C 0.0129(4) 0.9707(5) 0.3510(3) 0.102(3) Uani 1 1 d . . . H159 H 0.0033 1.0135 0.3686 0.123 Uiso 1 1 d R . . C160 C -0.0252(4) 0.9183(6) 0.3472(3) 0.122(3) Uani 1 1 d . . . H160 H -0.0613 0.9248 0.3625 0.147 Uiso 1 1 d R . . C161 C -0.0104(4) 0.8569(4) 0.3219(3) 0.093(2) Uani 1 1 d . . . H161 H -0.0368 0.8206 0.3197 0.111 Uiso 1 1 d R . . C162 C 0.0424(4) 0.8514(4) 0.3006(2) 0.078(2) Uani 1 1 d . . . H162 H 0.0521 0.8086 0.2830 0.094 Uiso 1 1 d R . . C165 C 0.4241(3) 0.9796(2) 0.3565(2) 0.0555(16) Uani 1 1 d . . . C166 C 0.5289(3) 1.0252(3) 0.3749(2) 0.0713(18) Uani 1 1 d . . . H16C H 0.5518 1.0168 0.4087 0.086 Uiso 1 1 d R . . H16D H 0.5107 1.0674 0.3866 0.086 Uiso 1 1 d R . . C167 C 0.5757(3) 1.0279(3) 0.3405(2) 0.0715(18) Uani 1 1 d . . . H16E H 0.5517 1.0262 0.3031 0.086 Uiso 1 1 d R . . H16F H 0.6021 1.0700 0.3581 0.086 Uiso 1 1 d R . . C168 C 0.6172(3) 0.9743(3) 0.3346(2) 0.0628(17) Uani 1 1 d . . . C169 C 0.6836(4) 0.9860(4) 0.3534(2) 0.084(2) Uani 1 1 d . . . H169 H 0.7020 1.0296 0.3700 0.100 Uiso 1 1 d R . . C170 C 0.7232(4) 0.9366(5) 0.3483(3) 0.096(2) Uani 1 1 d . . . H170 H 0.7681 0.9446 0.3603 0.115 Uiso 1 1 d R . . C171 C 0.6946(3) 0.8734(4) 0.3227(2) 0.079(2) Uani 1 1 d . . . H171 H 0.7190 0.8371 0.3189 0.094 Uiso 1 1 d R . . C172 C 0.6295(3) 0.8638(3) 0.3049(2) 0.0658(17) Uani 1 1 d . . . H172 H 0.6110 0.8202 0.2875 0.079 Uiso 1 1 d R . . C181 C 0.2191(3) 0.8153(3) 0.4225(2) 0.0554(15) Uani 1 1 d . . . H181 H 0.2336 0.8345 0.4616 0.067 Uiso 1 1 d R . . C182 C 0.2080(3) 0.8552(3) 0.3893(2) 0.0581(16) Uani 1 1 d . . . H182 H 0.2140 0.9011 0.4063 0.070 Uiso 1 1 d R . . C183 C 0.1821(2) 0.7637(2) 0.3098(2) 0.0433(13) Uani 1 1 d . . . C184 C 0.1910(2) 0.7237(3) 0.3431(2) 0.0499(14) Uani 1 1 d . . . C185 C 0.1836(3) 0.6508(3) 0.3247(2) 0.0549(15) Uani 1 1 d . . . C186 C 0.1642(3) 0.5572(3) 0.3479(2) 0.085(2) Uani 1 1 d . . . H18A H 0.2024 0.5331 0.3463 0.102 Uiso 1 1 d R . . H18B H 0.1345 0.5414 0.3107 0.102 Uiso 1 1 d R . . C187 C 0.1308(4) 0.5430(3) 0.3902(3) 0.102(2) Uani 1 1 d . . . H18C H 0.0935 0.5686 0.3889 0.123 Uiso 1 1 d R . . H18D H 0.1132 0.4970 0.3729 0.123 Uiso 1 1 d R . . N39 N 0.2100(3) 0.6058(3) 0.4739(2) 0.096(2) Uani 1 1 d . . . C188 C 0.1729(5) 0.5513(4) 0.4444(3) 0.115(3) Uani 1 1 d . . . C189 C 0.1736(6) 0.4981(4) 0.4654(4) 0.191(6) Uani 1 1 d . . . H189 H 0.1483 0.4583 0.4448 0.230 Uiso 1 1 d R . . C190 C 0.2130(6) 0.5083(5) 0.5175(5) 0.185(5) Uani 1 1 d . . . H190 H 0.2124 0.4749 0.5333 0.222 Uiso 1 1 d R . . C191 C 0.2530(6) 0.5641(5) 0.5478(4) 0.158(4) Uani 1 1 d . . . H191 H 0.2817 0.5696 0.5825 0.190 Uiso 1 1 d R . . C192 C 0.2477(4) 0.6106(4) 0.5229(3) 0.122(3) Uani 1 1 d . . . H192 H 0.2734 0.6504 0.5426 0.147 Uiso 1 1 d R . . C195 C 0.1583(2) 0.7451(3) 0.2483(2) 0.0443(13) Uani 1 1 d . . . C196 C 0.1106(2) 0.7711(2) 0.16922(18) 0.0522(15) Uani 1 1 d . . . H19A H 0.0834 0.7298 0.1570 0.063 Uiso 1 1 d R . . H19B H 0.1437 0.7644 0.1480 0.063 Uiso 1 1 d R . . C197 C 0.0707(3) 0.8247(3) 0.1582(2) 0.0560(15) Uani 1 1 d . . . H19C H 0.0416 0.8069 0.1208 0.067 Uiso 1 1 d R . . H19D H 0.0443 0.8371 0.1855 0.067 Uiso 1 1 d R . . C198 C 0.1076(3) 0.8846(3) 0.1619(2) 0.0507(14) Uani 1 1 d . . . C199 C 0.1035(3) 0.9034(3) 0.1153(2) 0.0511(15) Uani 1 1 d . . . H199 H 0.0761 0.8782 0.0808 0.061 Uiso 1 1 d R . . C200 C 0.1395(3) 0.9580(3) 0.1191(2) 0.0623(17) Uani 1 1 d . . . H200 H 0.1361 0.9707 0.0872 0.075 Uiso 1 1 d R . . C201 C 0.1797(3) 0.9939(3) 0.1692(2) 0.0619(17) Uani 1 1 d . . . H201 H 0.2051 1.0313 0.1724 0.074 Uiso 1 1 d R . . C202 C 0.1827(3) 0.9723(3) 0.2134(2) 0.0645(17) Uani 1 1 d . . . H202 H 0.2091 0.9978 0.2482 0.077 Uiso 1 1 d R . . C211 C 0.5151(3) 0.8222(3) 0.4314(2) 0.0599(16) Uani 1 1 d . . . H211 H 0.5200 0.8419 0.4702 0.072 Uiso 1 1 d R . . C212 C 0.5071(3) 0.8611(3) 0.3970(2) 0.0561(15) Uani 1 1 d . . . H212 H 0.5077 0.9068 0.4133 0.067 Uiso 1 1 d R . . C213 C 0.4974(3) 0.7699(3) 0.3206(2) 0.0522(15) Uani 1 1 d . . . C214 C 0.5068(3) 0.7294(3) 0.3545(2) 0.0527(15) Uani 1 1 d . . . C215 C 0.5117(3) 0.6575(3) 0.3392(3) 0.0604(16) Uani 1 1 d . . . C216 C 0.5455(3) 0.5678(3) 0.3643(2) 0.081(2) Uani 1 1 d . . . H21A H 0.5065 0.5403 0.3594 0.097 Uiso 1 1 d R . . H21B H 0.5590 0.5540 0.3291 0.097 Uiso 1 1 d R . . C217 C 0.6022(4) 0.5623(3) 0.4110(3) 0.120(3) Uani 1 1 d . . . H21C H 0.6364 0.5976 0.4215 0.144 Uiso 1 1 d R . . H21D H 0.6205 0.5206 0.3970 0.144 Uiso 1 1 d R . . N45 N 0.5557(3) 0.6175(3) 0.4893(2) 0.100(2) Uani 1 1 d . . . C218 C 0.5807(5) 0.5648(4) 0.4647(3) 0.143(4) Uani 1 1 d . . . C219 C 0.5978(6) 0.5166(4) 0.4867(4) 0.182(5) Uani 1 1 d . . . H219 H 0.6138 0.4789 0.4657 0.218 Uiso 1 1 d R . . C220 C 0.5916(6) 0.5229(4) 0.5366(4) 0.198(6) Uani 1 1 d . . . H220 H 0.6066 0.4921 0.5540 0.238 Uiso 1 1 d R . . C221 C 0.5627(6) 0.5759(4) 0.5635(3) 0.213(6) Uani 1 1 d . . . H221 H 0.5527 0.5801 0.5978 0.255 Uiso 1 1 d R . . C222 C 0.5489(5) 0.6221(3) 0.5384(3) 0.150(4) Uani 1 1 d . . . H222 H 0.5332 0.6606 0.5585 0.180 Uiso 1 1 d R . . C225 C 0.4880(3) 0.7483(3) 0.2576(2) 0.0548(15) Uani 1 1 d . . . C226 C 0.4885(3) 0.7747(2) 0.17786(19) 0.0563(15) Uani 1 1 d . . . H22A H 0.4438 0.7664 0.1559 0.068 Uiso 1 1 d R . . H22B H 0.5092 0.7340 0.1667 0.068 Uiso 1 1 d R . . C227 C 0.5213(3) 0.8286(3) 0.16499(19) 0.0552(15) Uani 1 1 d . . . H22C H 0.5623 0.8443 0.1928 0.066 Uiso 1 1 d R . . H22D H 0.5302 0.8108 0.1278 0.066 Uiso 1 1 d R . . C228 C 0.4835(3) 0.8865(3) 0.1682(2) 0.0513(14) Uani 1 1 d . . . C229 C 0.4602(3) 0.9044(3) 0.1214(2) 0.0545(15) Uani 1 1 d . . . H229 H 0.4681 0.8792 0.0869 0.065 Uiso 1 1 d R . . C230 C 0.4274(3) 0.9566(3) 0.1244(2) 0.0669(18) Uani 1 1 d . . . H230 H 0.4114 0.9683 0.0924 0.080 Uiso 1 1 d R . . C231 C 0.4142(3) 0.9919(3) 0.1743(2) 0.0633(17) Uani 1 1 d . . . H231 H 0.3913 1.0293 0.1778 0.076 Uiso 1 1 d R . . C232 C 0.4382(3) 0.9724(3) 0.2197(2) 0.0591(16) Uani 1 1 d . . . H232 H 0.4305 0.9971 0.2544 0.071 Uiso 1 1 d R . . B1 B 0.0778(5) 0.1813(5) 0.0235(4) 0.090(3) Uani 1 1 d . . . F11 F 0.0489(2) 0.21722(18) 0.06161(16) 0.1097(13) Uani 1 1 d . . . F12 F 0.0728(2) 0.1169(2) 0.02312(19) 0.1404(17) Uani 1 1 d . . . F13 F 0.0506(3) 0.1860(3) -0.0267(2) 0.161(2) Uani 1 1 d . . . F14 F 0.1420(2) 0.2038(2) 0.0402(2) 0.1540(19) Uani 1 1 d . . . B2 B 0.2807(5) 0.6869(4) 0.1097(3) 0.074(2) Uani 1 1 d . . . F21 F 0.2282(2) 0.7145(3) 0.0928(2) 0.1550(19) Uani 1 1 d . . . F22 F 0.2750(2) 0.6238(2) 0.08016(15) 0.1375(17) Uani 1 1 d . . . F23 F 0.2942(3) 0.6984(2) 0.16417(17) 0.162(2) Uani 1 1 d . . . F24 F 0.3278(2) 0.7188(3) 0.0983(2) 0.166(2) Uani 1 1 d . . . B3 B 0.4305(6) 0.1838(6) 0.0206(5) 0.111(4) Uani 1 1 d . . . F31 F 0.4821(2) 0.2185(2) 0.05711(18) 0.1141(13) Uani 1 1 d . . . F32 F 0.4352(3) 0.1190(3) 0.0182(2) 0.163(2) Uani 1 1 d . . . F33 F 0.3789(3) 0.2025(3) 0.0371(3) 0.195(3) Uani 1 1 d . . . F34 F 0.4319(3) 0.1867(3) -0.0308(2) 0.174(2) Uani 1 1 d . . . B4 B 0.8583(6) 0.0708(5) 0.3465(4) 0.100(3) Uani 1 1 d . . . F41 F 0.85333(19) 0.0040(2) 0.32635(18) 0.1164(14) Uani 1 1 d . . . F42 F 0.9184(3) 0.0963(3) 0.3604(2) 0.166(2) Uani 1 1 d . . . F43 F 0.8387(4) 0.0859(3) 0.3944(3) 0.277(5) Uani 1 1 d . . . F44 F 0.8247(3) 0.0980(3) 0.3134(3) 0.225(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0730(6) 0.0880(6) 0.0471(4) 0.0401(4) 0.0243(4) 0.0133(5) Ni2 0.0659(5) 0.0569(5) 0.0475(4) 0.0267(4) 0.0073(4) 0.0099(4) Ni3 0.0415(5) 0.0521(5) 0.0499(4) 0.0103(3) 0.0107(3) 0.0054(4) Ni4 0.0408(4) 0.0453(4) 0.0557(4) 0.0198(3) 0.0090(3) 0.0021(4) O1 0.108(4) 0.103(3) 0.042(2) 0.022(2) 0.022(2) 0.007(3) O2 0.096(3) 0.073(3) 0.037(2) 0.015(2) 0.010(2) 0.004(2) O3 0.040(3) 0.182(5) 0.097(3) -0.081(3) 0.003(2) -0.004(3) O4 0.035(3) 0.113(4) 0.082(3) -0.035(3) 0.003(2) -0.003(2) O5 0.066(3) 0.054(2) 0.040(2) 0.0234(17) 0.0109(18) 0.000(2) O6 0.083(3) 0.036(2) 0.033(2) 0.0095(16) 0.0173(18) 0.0027(19) O7 0.069(3) 0.045(2) 0.042(2) 0.0160(17) 0.0056(19) 0.0039(19) O8 0.063(3) 0.041(2) 0.041(2) 0.0155(17) 0.0059(18) 0.0018(19) N1 0.075(4) 0.065(3) 0.031(3) 0.024(2) 0.013(3) 0.009(3) N2 0.081(4) 0.107(4) 0.054(3) 0.047(3) 0.033(3) 0.019(4) N3 0.079(4) 0.093(4) 0.081(4) 0.050(3) 0.040(3) 0.018(3) N4 0.069(4) 0.054(3) 0.053(3) 0.028(3) 0.011(3) 0.004(3) N5 0.082(4) 0.070(4) 0.042(3) 0.028(2) 0.006(3) 0.019(3) N6 0.070(4) 0.081(4) 0.062(3) 0.041(3) 0.013(3) 0.016(3) N7 0.043(3) 0.050(3) 0.049(3) 0.014(2) 0.010(2) 0.010(2) N8 0.034(3) 0.066(3) 0.069(3) -0.005(2) 0.014(3) 0.006(3) N9 0.033(3) 0.059(3) 0.050(3) 0.013(2) 0.009(2) 0.010(3) N10 0.039(3) 0.042(3) 0.045(3) 0.017(2) 0.008(2) 0.003(2) N11 0.035(3) 0.042(3) 0.057(3) 0.004(2) -0.004(2) -0.002(2) N12 0.041(3) 0.049(3) 0.068(3) 0.019(3) 0.010(2) -0.002(3) N13 0.061(3) 0.066(3) 0.036(3) 0.022(2) 0.017(2) 0.008(3) N14 0.066(3) 0.064(3) 0.053(3) 0.032(3) 0.020(2) -0.003(3) N15 0.089(4) 0.075(4) 0.074(4) 0.047(3) 0.029(3) -0.004(3) N16 0.036(3) 0.063(3) 0.036(3) 0.011(2) 0.005(2) -0.003(2) N17 0.040(3) 0.040(3) 0.034(2) 0.012(2) 0.0033(19) 0.001(2) N18 0.047(3) 0.048(3) 0.077(4) 0.020(3) 0.015(3) 0.000(3) N19 0.057(3) 0.059(3) 0.046(3) 0.024(2) 0.012(2) 0.018(3) N20 0.057(3) 0.043(3) 0.053(3) 0.020(2) 0.014(2) 0.010(2) N21 0.071(4) 0.060(3) 0.058(3) 0.030(3) 0.010(3) 0.012(3) N22 0.034(3) 0.043(3) 0.047(3) 0.013(2) 0.008(2) 0.007(2) N23 0.037(3) 0.050(3) 0.042(3) 0.020(2) 0.011(2) 0.007(2) N24 0.046(3) 0.056(3) 0.086(4) 0.043(3) 0.021(3) 0.012(3) C1 0.081(5) 0.065(4) 0.031(3) 0.021(3) 0.006(3) 0.004(4) C2 0.054(4) 0.069(4) 0.035(3) 0.017(3) 0.012(3) -0.001(3) C3 0.070(5) 0.052(4) 0.053(4) 0.033(3) 0.021(4) 0.016(3) C4 0.077(5) 0.059(4) 0.042(4) 0.029(3) 0.019(3) 0.013(4) C5 0.080(5) 0.075(5) 0.048(4) 0.038(3) 0.028(4) 0.024(4) C6 0.119(6) 0.135(7) 0.044(4) 0.040(4) 0.040(4) 0.021(5) C7 0.142(8) 0.119(6) 0.075(5) 0.061(5) 0.058(5) 0.021(6) C8 0.114(7) 0.117(6) 0.091(6) 0.060(5) 0.063(6) 0.025(5) C9 0.109(7) 0.106(6) 0.103(6) 0.042(5) 0.060(6) 0.013(6) C10 0.069(6) 0.136(7) 0.149(8) 0.040(7) 0.066(6) 0.001(5) C11 0.078(6) 0.110(6) 0.093(6) 0.028(4) 0.036(5) 0.010(5) C12 0.068(5) 0.109(6) 0.095(5) 0.061(5) 0.035(5) 0.008(5) C15 0.101(6) 0.054(4) 0.028(3) 0.018(3) 0.003(4) 0.010(4) C16 0.075(5) 0.086(5) 0.054(4) 0.033(3) -0.001(4) 0.001(4) C17 0.116(6) 0.073(5) 0.056(4) 0.033(3) -0.018(4) 0.011(4) C18 0.070(5) 0.070(5) 0.066(5) 0.025(4) -0.012(4) 0.014(4) C19 0.092(7) 0.081(5) 0.099(6) 0.026(5) -0.022(5) 0.009(5) C20 0.059(6) 0.123(7) 0.143(9) 0.033(7) -0.008(6) 0.028(5) C21 0.056(5) 0.109(6) 0.112(7) 0.024(5) 0.003(5) 0.018(5) C22 0.076(6) 0.061(4) 0.084(5) 0.029(4) -0.004(4) 0.026(4) C31 0.058(4) 0.051(4) 0.035(3) 0.020(3) 0.010(3) 0.006(3) C32 0.043(4) 0.044(3) 0.041(3) 0.022(3) 0.007(3) 0.007(3) C33 0.040(4) 0.055(4) 0.050(4) 0.014(3) 0.007(3) 0.001(3) C34 0.048(4) 0.052(4) 0.038(3) 0.006(3) 0.008(3) 0.000(3) C35 0.042(4) 0.087(5) 0.076(5) -0.020(4) 0.013(4) 0.001(4) C36 0.056(5) 0.097(5) 0.100(5) -0.026(4) 0.015(4) 0.012(4) C37 0.067(5) 0.069(5) 0.102(5) -0.005(4) 0.028(4) 0.020(4) C38 0.045(4) 0.069(5) 0.063(4) 0.008(3) 0.012(3) 0.005(4) C39 0.064(5) 0.070(5) 0.058(4) 0.003(3) 0.018(3) 0.005(4) C40 0.084(5) 0.077(5) 0.071(4) 0.018(4) 0.040(4) 0.002(4) C41 0.065(5) 0.068(4) 0.088(5) 0.018(4) 0.040(4) 0.001(4) C42 0.045(4) 0.059(4) 0.061(4) 0.011(3) 0.009(3) 0.001(3) C45 0.036(4) 0.061(4) 0.073(4) 0.006(3) 0.009(3) 0.009(3) C46 0.052(4) 0.064(4) 0.087(5) 0.001(3) 0.013(4) 0.007(3) C47 0.051(4) 0.049(4) 0.093(5) 0.002(3) 0.008(4) -0.007(3) C48 0.060(4) 0.036(3) 0.059(4) 0.014(3) 0.011(3) -0.003(3) C49 0.053(4) 0.047(4) 0.073(4) 0.017(3) -0.003(3) -0.003(3) C50 0.043(4) 0.070(5) 0.077(4) 0.006(4) 0.000(3) 0.000(4) C51 0.040(4) 0.046(4) 0.099(5) 0.018(3) 0.015(4) 0.014(3) C52 0.055(4) 0.056(4) 0.065(4) 0.021(3) 0.011(3) 0.002(3) C61 0.075(5) 0.094(5) 0.029(3) 0.019(4) 0.017(3) 0.005(4) C62 0.075(5) 0.079(5) 0.036(3) 0.015(3) 0.018(3) 0.022(4) C63 0.034(3) 0.049(4) 0.040(3) 0.015(3) 0.015(2) 0.004(3) C64 0.047(4) 0.061(4) 0.033(3) 0.014(3) 0.010(3) -0.001(3) C65 0.047(4) 0.075(4) 0.040(3) 0.027(3) 0.007(3) -0.013(3) C66 0.074(5) 0.056(4) 0.074(4) 0.032(3) 0.008(3) -0.009(3) C67 0.086(5) 0.083(5) 0.088(5) 0.057(4) 0.027(4) 0.003(4) C68 0.082(5) 0.083(5) 0.087(5) 0.061(4) 0.045(4) 0.014(5) C69 0.090(6) 0.079(5) 0.097(5) 0.042(4) 0.033(4) 0.002(4) C70 0.107(7) 0.079(6) 0.103(6) 0.052(5) 0.024(5) 0.013(5) C71 0.114(7) 0.103(6) 0.086(5) 0.067(5) 0.036(5) 0.039(5) C72 0.098(6) 0.097(6) 0.077(5) 0.068(4) 0.022(4) 0.022(5) C75 0.038(3) 0.064(4) 0.029(3) 0.015(3) 0.015(2) -0.001(3) C76 0.054(4) 0.061(4) 0.037(3) 0.017(3) 0.014(3) 0.016(3) C77 0.051(4) 0.072(4) 0.050(3) 0.026(3) 0.012(3) 0.008(3) C78 0.048(4) 0.063(4) 0.072(4) 0.028(4) 0.019(4) 0.013(3) C79 0.072(5) 0.079(5) 0.107(6) 0.055(4) 0.018(4) 0.014(4) C80 0.084(6) 0.118(7) 0.120(7) 0.072(6) 0.015(5) 0.013(5) C81 0.052(5) 0.084(5) 0.178(8) 0.078(6) 0.049(5) 0.005(4) C82 0.049(4) 0.075(5) 0.110(5) 0.038(4) 0.025(4) 0.013(4) C91 0.068(4) 0.055(4) 0.049(3) 0.026(3) 0.008(3) 0.017(3) C92 0.053(4) 0.049(4) 0.043(3) 0.011(3) 0.004(3) 0.007(3) C93 0.025(3) 0.047(4) 0.049(3) 0.017(3) 0.008(2) 0.008(3) C94 0.045(3) 0.037(3) 0.046(3) 0.020(3) 0.014(3) 0.012(3) C95 0.045(4) 0.060(4) 0.045(3) 0.030(3) 0.012(3) 0.009(3) C96 0.064(4) 0.048(4) 0.056(4) 0.022(3) 0.016(3) 0.008(3) C97 0.086(5) 0.051(4) 0.069(4) 0.029(3) 0.033(4) 0.016(3) C98 0.060(4) 0.057(4) 0.060(4) 0.022(3) 0.008(3) 0.016(3) C99 0.085(5) 0.055(4) 0.087(5) 0.034(4) 0.020(4) 0.006(4) C100 0.088(5) 0.060(5) 0.115(6) 0.050(4) 0.038(5) 0.015(4) C101 0.095(6) 0.097(6) 0.079(5) 0.053(4) 0.030(4) 0.022(5) C102 0.088(5) 0.060(4) 0.073(4) 0.043(3) 0.015(4) 0.015(4) C105 0.037(3) 0.041(3) 0.046(3) 0.016(3) 0.016(3) 0.009(3) C106 0.066(4) 0.053(4) 0.053(4) 0.027(3) 0.011(3) 0.002(3) C107 0.054(4) 0.056(4) 0.052(3) 0.024(3) 0.011(3) -0.005(3) C108 0.057(4) 0.061(4) 0.076(5) 0.033(4) 0.012(4) -0.007(3) C109 0.074(5) 0.090(5) 0.091(5) 0.064(4) 0.016(4) 0.001(4) C110 0.070(6) 0.113(7) 0.150(8) 0.095(6) -0.003(6) 0.014(5) C111 0.072(5) 0.085(5) 0.132(7) 0.072(5) 0.020(5) 0.023(4) C112 0.048(4) 0.065(4) 0.098(5) 0.042(4) 0.028(4) 0.017(3) Ni5 0.1015(7) 0.0608(5) 0.0515(5) 0.0274(4) 0.0152(4) 0.0023(5) Ni6 0.0953(7) 0.0480(5) 0.0515(5) 0.0112(4) -0.0058(4) 0.0116(5) Ni7 0.0663(5) 0.0544(5) 0.0404(4) 0.0190(3) 0.0150(4) 0.0170(4) Ni8 0.0663(5) 0.0449(4) 0.0425(4) 0.0105(3) 0.0150(4) -0.0039(4) O9 0.125(4) 0.069(3) 0.051(3) -0.007(2) 0.019(3) 0.006(3) O10 0.130(4) 0.051(3) 0.045(2) -0.003(2) 0.006(2) -0.001(3) O11 0.091(3) 0.052(2) 0.047(2) 0.005(2) 0.021(2) 0.012(2) O12 0.085(3) 0.056(2) 0.046(2) 0.0006(19) 0.018(2) -0.005(2) O13 0.082(3) 0.050(2) 0.047(2) 0.0101(19) 0.008(2) 0.004(2) O14 0.071(3) 0.052(2) 0.045(2) 0.0173(19) 0.0082(19) 0.013(2) O15 0.128(4) 0.041(2) 0.053(3) 0.006(2) 0.024(2) 0.002(2) O16 0.100(3) 0.042(2) 0.050(2) 0.0101(19) 0.017(2) -0.004(2) N25 0.093(4) 0.050(3) 0.050(3) 0.027(3) 0.013(3) 0.023(3) N26 0.105(5) 0.074(4) 0.049(3) 0.028(3) 0.023(4) 0.031(4) N28 0.086(4) 0.040(3) 0.039(3) 0.018(2) 0.001(3) 0.009(3) N29 0.089(4) 0.051(3) 0.050(3) 0.006(2) -0.013(3) -0.004(3) N31 0.063(3) 0.041(3) 0.042(3) 0.017(2) 0.013(2) 0.013(3) N32 0.073(4) 0.047(3) 0.051(3) 0.017(2) 0.007(3) 0.025(3) N33 0.071(4) 0.069(4) 0.055(3) 0.032(3) 0.020(3) 0.027(3) N34 0.076(4) 0.036(3) 0.034(2) 0.002(2) 0.018(2) -0.001(3) N35 0.091(4) 0.039(3) 0.044(3) 0.007(2) 0.025(3) -0.014(3) N36 0.069(4) 0.052(3) 0.041(3) 0.005(2) 0.009(2) -0.017(3) N37 0.051(3) 0.046(3) 0.061(3) 0.017(2) 0.013(2) 0.002(2) N38 0.081(4) 0.046(3) 0.061(3) 0.020(3) 0.015(3) -0.011(3) N40 0.065(3) 0.054(3) 0.038(3) 0.018(2) 0.016(2) 0.013(3) N41 0.058(3) 0.055(3) 0.045(3) 0.021(2) 0.007(2) 0.009(3) N42 0.066(3) 0.054(3) 0.038(3) 0.019(2) 0.011(2) 0.014(3) N43 0.076(4) 0.029(3) 0.055(3) 0.005(2) 0.007(3) -0.003(2) N44 0.089(4) 0.055(3) 0.057(3) 0.020(3) 0.006(3) 0.027(3) N46 0.064(3) 0.037(3) 0.040(3) -0.002(2) 0.011(2) -0.011(2) N47 0.058(3) 0.044(3) 0.041(3) 0.006(2) 0.012(2) -0.006(2) N48 0.064(3) 0.044(3) 0.046(3) 0.012(2) 0.021(2) 0.009(3) C121 0.087(6) 0.062(4) 0.050(4) 0.020(3) 0.003(4) 0.007(4) C122 0.107(6) 0.038(4) 0.027(3) 0.006(3) 0.003(3) -0.001(4) C123 0.085(5) 0.046(4) 0.047(4) 0.021(3) 0.012(4) 0.007(4) C124 0.118(6) 0.030(3) 0.030(3) 0.004(3) 0.004(4) -0.001(4) C125 0.117(6) 0.051(4) 0.041(4) 0.019(3) 0.020(4) 0.021(5) C126 0.113(6) 0.087(5) 0.052(4) 0.033(4) 0.016(4) 0.017(5) C127 0.155(8) 0.103(6) 0.063(5) 0.042(4) 0.038(5) 0.020(6) N27 0.110(5) 0.104(5) 0.074(4) 0.046(4) 0.033(4) 0.001(4) C128 0.131(9) 0.124(7) 0.091(7) 0.038(5) 0.052(7) -0.003(6) C129 0.124(10) 0.269(14) 0.141(10) 0.041(10) 0.069(9) 0.015(10) C130 0.103(9) 0.302(16) 0.139(10) -0.003(10) 0.051(8) 0.024(10) C131 0.102(8) 0.213(11) 0.158(10) 0.023(8) 0.068(7) 0.017(8) C132 0.103(7) 0.122(7) 0.100(7) 0.044(5) 0.045(6) 0.008(6) C135 0.110(6) 0.032(4) 0.047(4) 0.020(3) 0.008(4) 0.002(4) C136 0.123(7) 0.057(4) 0.069(5) 0.002(3) -0.027(4) 0.004(5) C137 0.134(10) 0.150(9) 0.130(9) -0.023(7) -0.069(7) 0.026(8) N30 0.103(6) 0.110(6) 0.096(6) 0.002(5) -0.010(5) 0.006(4) C138 0.114(10) 0.131(9) 0.126(10) 0.021(8) 0.001(8) 0.018(7) C139 0.115(14) 0.216(15) 0.28(2) -0.064(14) -0.023(12) -0.026(11) C140 0.119(14) 0.36(2) 0.30(3) -0.02(2) 0.028(15) -0.049(14) C141 0.160(14) 0.288(18) 0.183(14) -0.014(12) -0.010(11) -0.046(12) C142 0.115(10) 0.152(10) 0.175(13) 0.042(9) -0.022(9) -0.018(8) C151 0.068(4) 0.043(3) 0.037(3) 0.001(3) 0.020(3) 0.013(3) C152 0.079(5) 0.044(4) 0.041(3) 0.006(3) 0.026(3) 0.008(4) C153 0.076(5) 0.043(4) 0.035(3) 0.015(3) 0.020(3) 0.004(4) C154 0.077(5) 0.041(3) 0.023(3) 0.013(2) 0.004(3) 0.006(3) C155 0.085(5) 0.038(4) 0.033(3) 0.015(3) 0.013(3) 0.012(4) C156 0.097(5) 0.045(4) 0.059(4) 0.016(3) 0.022(4) 0.022(4) C157 0.095(6) 0.078(5) 0.064(4) 0.039(4) 0.023(4) 0.045(4) C158 0.070(5) 0.107(6) 0.060(4) 0.034(4) 0.031(4) 0.049(5) C159 0.111(8) 0.122(8) 0.084(5) 0.041(5) 0.032(5) 0.069(6) C160 0.111(8) 0.179(10) 0.118(7) 0.076(8) 0.068(6) 0.095(8) C161 0.090(6) 0.117(7) 0.112(6) 0.066(5) 0.062(5) 0.049(5) C162 0.093(6) 0.083(5) 0.077(5) 0.041(4) 0.035(4) 0.044(5) C165 0.103(6) 0.030(3) 0.041(3) 0.013(3) 0.032(4) 0.006(4) C166 0.090(5) 0.049(4) 0.068(4) 0.002(3) 0.032(4) -0.020(4) C167 0.103(6) 0.046(4) 0.063(4) 0.010(3) 0.028(4) -0.014(4) C168 0.082(5) 0.070(5) 0.032(3) 0.016(3) 0.008(3) -0.018(4) C169 0.084(6) 0.096(6) 0.066(4) 0.034(4) 0.000(4) -0.035(5) C170 0.084(6) 0.121(7) 0.084(5) 0.053(5) -0.004(4) -0.017(6) C171 0.067(5) 0.091(6) 0.076(5) 0.037(4) -0.001(4) 0.003(4) C172 0.071(5) 0.064(5) 0.058(4) 0.016(3) 0.015(4) -0.003(4) C181 0.067(4) 0.048(4) 0.044(3) 0.010(3) 0.008(3) 0.006(3) C182 0.066(4) 0.062(4) 0.047(4) 0.023(3) 0.008(3) 0.016(3) C183 0.050(4) 0.032(3) 0.050(3) 0.020(3) 0.007(3) 0.008(3) C184 0.053(4) 0.055(4) 0.034(3) 0.009(3) 0.003(3) -0.002(3) C185 0.052(4) 0.054(4) 0.061(4) 0.029(3) 0.003(3) 0.004(3) C186 0.116(6) 0.061(5) 0.065(4) 0.018(3) 0.002(4) -0.018(4) C187 0.131(7) 0.084(5) 0.080(5) 0.026(4) 0.007(5) -0.041(5) N39 0.158(6) 0.059(4) 0.072(4) 0.029(3) 0.016(4) 0.003(4) C188 0.203(10) 0.077(6) 0.072(5) 0.035(5) 0.032(6) -0.022(6) C189 0.381(17) 0.088(7) 0.094(7) 0.051(6) 0.011(9) -0.047(8) C190 0.338(17) 0.101(8) 0.124(9) 0.074(7) 0.019(9) -0.013(9) C191 0.270(14) 0.092(7) 0.108(7) 0.052(6) 0.006(8) 0.041(8) C192 0.211(10) 0.086(6) 0.072(5) 0.037(5) 0.020(6) 0.032(6) C195 0.048(4) 0.047(4) 0.039(3) 0.011(3) 0.016(3) 0.012(3) C196 0.056(4) 0.060(4) 0.034(3) 0.016(3) -0.001(3) 0.004(3) C197 0.055(4) 0.061(4) 0.053(3) 0.022(3) 0.010(3) 0.011(3) C198 0.053(4) 0.059(4) 0.043(3) 0.016(3) 0.015(3) 0.014(3) C199 0.053(4) 0.056(4) 0.037(3) 0.007(3) 0.008(3) 0.011(3) C200 0.076(5) 0.067(4) 0.047(4) 0.019(3) 0.020(3) 0.019(4) C201 0.083(5) 0.062(4) 0.042(3) 0.026(3) 0.006(3) -0.002(3) C202 0.091(5) 0.049(4) 0.051(4) 0.016(3) 0.013(3) 0.005(4) C211 0.060(4) 0.063(4) 0.049(4) 0.011(3) 0.011(3) -0.005(3) C212 0.076(4) 0.033(3) 0.058(4) 0.014(3) 0.016(3) -0.002(3) C213 0.065(4) 0.047(4) 0.035(3) 0.001(3) 0.014(3) -0.012(3) C214 0.065(4) 0.051(4) 0.037(3) 0.013(3) 0.006(3) 0.002(3) C215 0.065(4) 0.040(4) 0.065(4) 0.001(3) 0.018(3) 0.008(3) C216 0.103(6) 0.058(4) 0.064(4) 0.011(3) -0.001(4) 0.034(4) C217 0.126(7) 0.076(5) 0.122(7) 0.012(5) -0.012(6) 0.039(5) N45 0.167(6) 0.054(4) 0.053(4) 0.011(3) -0.015(4) 0.033(4) C218 0.244(12) 0.090(7) 0.063(5) 0.021(5) -0.020(6) 0.055(7) C219 0.349(16) 0.106(7) 0.084(6) 0.045(6) 0.014(8) 0.122(8) C220 0.396(18) 0.091(7) 0.097(7) 0.042(6) 0.018(9) 0.102(9) C221 0.46(2) 0.104(7) 0.070(6) 0.051(5) 0.027(8) 0.115(10) C222 0.301(13) 0.071(5) 0.053(5) 0.020(4) -0.008(6) 0.058(7) C225 0.067(4) 0.040(4) 0.048(4) 0.004(3) 0.011(3) -0.008(3) C226 0.075(4) 0.046(3) 0.046(3) 0.012(3) 0.015(3) 0.002(3) C227 0.061(4) 0.067(4) 0.031(3) 0.006(3) 0.015(3) -0.001(3) C228 0.054(4) 0.056(4) 0.042(3) 0.011(3) 0.017(3) -0.010(3) C229 0.070(4) 0.050(4) 0.036(3) 0.004(3) 0.016(3) -0.008(3) C230 0.089(5) 0.069(4) 0.044(4) 0.022(3) 0.017(3) 0.002(4) C231 0.079(5) 0.057(4) 0.058(4) 0.022(3) 0.021(3) -0.004(3) C232 0.091(5) 0.051(4) 0.041(3) 0.017(3) 0.025(3) -0.002(4) B1 0.093(8) 0.091(8) 0.095(7) 0.016(6) 0.063(6) 0.007(6) F11 0.127(4) 0.092(3) 0.121(3) 0.039(2) 0.047(3) 0.023(3) F12 0.159(5) 0.080(3) 0.155(4) 0.002(3) 0.040(3) 0.014(3) F13 0.177(5) 0.209(6) 0.091(3) 0.046(3) 0.027(3) 0.030(4) F14 0.094(4) 0.150(4) 0.213(5) 0.045(4) 0.050(4) 0.007(3) B2 0.095(7) 0.061(6) 0.058(5) 0.009(4) 0.018(5) 0.009(5) F21 0.086(4) 0.163(5) 0.207(5) 0.063(4) 0.014(3) 0.028(3) F22 0.224(5) 0.088(3) 0.074(3) 0.003(2) 0.019(3) 0.010(3) F23 0.306(7) 0.091(3) 0.075(3) 0.024(2) 0.027(4) 0.024(4) F24 0.118(4) 0.166(5) 0.243(6) 0.077(4) 0.088(4) 0.011(4) B3 0.100(9) 0.099(9) 0.108(9) 0.031(7) -0.020(7) -0.027(8) F31 0.122(4) 0.103(3) 0.121(3) 0.046(3) 0.024(3) 0.002(3) F32 0.189(6) 0.100(4) 0.176(5) 0.020(3) 0.037(4) -0.013(4) F33 0.081(4) 0.241(7) 0.266(7) 0.087(5) 0.046(4) 0.031(4) F34 0.208(6) 0.203(6) 0.110(4) 0.062(4) 0.024(4) -0.031(4) B4 0.123(10) 0.071(7) 0.101(8) 0.019(6) 0.036(7) 0.001(7) F41 0.110(3) 0.111(4) 0.157(4) 0.059(3) 0.067(3) 0.035(3) F42 0.133(5) 0.125(4) 0.216(6) 0.056(4) -0.003(4) -0.003(4) F43 0.446(12) 0.142(5) 0.348(9) 0.061(5) 0.328(10) 0.088(6) F44 0.232(7) 0.139(5) 0.247(7) 0.089(5) -0.091(6) 0.022(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 Ni1 N2 2.022(5) . ? Ni1 N14 2.048(4) . ? Ni1 N3 2.088(5) . ? Ni1 N1 2.107(5) . ? Ni1 N15 2.120(5) . ? Ni1 N13 2.130(4) . ? Ni2 N5 2.027(5) . ? Ni2 N20 2.040(4) . ? Ni2 N4 2.105(5) . ? Ni2 N6 2.113(5) . ? Ni2 N21 2.114(4) . ? Ni2 N19 2.143(4) . ? Ni3 N8 2.034(4) . ? Ni3 N17 2.041(4) . ? Ni3 N9 2.115(4) . ? Ni3 N16 2.130(4) . ? Ni3 N7 2.138(4) . ? Ni3 N18 2.162(5) . ? Ni4 N23 2.030(4) . ? Ni4 N11 2.036(4) . ? Ni4 N12 2.107(4) . ? Ni4 N10 2.129(4) . ? Ni4 N22 2.143(4) . ? Ni4 N24 2.165(4) . ? O1 C5 1.320(7) . ? O2 C15 1.300(6) . ? O3 C35 1.271(6) . ? O4 C45 1.287(6) . ? O5 C65 1.289(5) . ? O6 C75 1.290(5) . ? O7 C95 1.303(5) . ? O8 C105 1.290(5) . ? N1 C1 1.327(6) . ? N1 C4 1.339(6) . ? N2 C5 1.259(7) . ? N2 C6 1.478(7) . ? N3 C12 1.334(7) . ? N3 C8 1.379(7) . ? N4 C2 1.319(6) . ? N4 C3 1.368(6) . ? N5 C15 1.274(7) . ? N5 C16 1.468(6) . ? N6 C22 1.332(7) . ? N6 C18 1.340(7) . ? N7 C31 1.338(5) . ? N7 C34 1.376(6) . ? N8 C35 1.304(6) . ? N8 C36 1.491(6) . ? N9 C42 1.356(6) . ? N9 C38 1.364(6) . ? N10 C32 1.325(5) . ? N10 C33 1.357(6) . ? N11 C45 1.291(6) . ? N11 C46 1.486(6) . ? N12 C48 1.348(6) . ? N12 C52 1.365(6) . ? N13 C61 1.313(6) . ? N13 C64 1.372(6) . ? N14 C65 1.325(6) . ? N14 C66 1.451(6) . ? N15 C68 1.323(7) . ? N15 C72 1.341(7) . ? N16 C62 1.340(6) . ? N16 C63 1.367(6) . ? N17 C75 1.303(6) . ? N17 C76 1.470(5) . ? N18 C78 1.345(6) . ? N18 C82 1.355(7) . ? N19 C91 1.343(6) . ? N19 C94 1.371(5) . ? N20 C95 1.289(6) . ? N20 C96 1.475(6) . ? N21 C98 1.338(6) . ? N21 C102 1.376(6) . ? N22 C92 1.330(5) . ? N22 C93 1.345(5) . ? N23 C105 1.293(5) . ? N23 C106 1.472(5) . ? N24 C112 1.340(6) . ? N24 C108 1.349(6) . ? C1 C2 1.370(7) . ? C3 C4 1.404(7) . ? C3 C15 1.552(8) . ? C4 C5 1.574(7) . ? C6 C7 1.528(8) . ? C7 C8 1.505(9) . ? C8 C9 1.379(9) . ? C9 C10 1.363(9) . ? C10 C11 1.409(9) . ? C11 C12 1.367(8) . ? C16 C17 1.516(7) . ? C17 C18 1.516(8) . ? C18 C19 1.404(9) . ? C19 C20 1.384(10) . ? C20 C21 1.351(9) . ? C21 C22 1.391(8) . ? C31 C32 1.379(6) . ? C33 C34 1.398(7) . ? C33 C45 1.511(7) . ? C34 C35 1.505(7) . ? C36 C37 1.509(7) . ? C37 C38 1.521(8) . ? C38 C39 1.389(7) . ? C39 C40 1.377(7) . ? C40 C41 1.414(7) . ? C41 C42 1.391(7) . ? C46 C47 1.540(7) . ? C47 C48 1.492(7) . ? C48 C49 1.414(7) . ? C49 C50 1.405(7) . ? C50 C51 1.369(7) . ? C51 C52 1.385(7) . ? C61 C62 1.379(7) . ? C63 C64 1.417(7) . ? C63 C75 1.513(6) . ? C64 C65 1.474(7) . ? C66 C67 1.551(7) . ? C67 C68 1.506(8) . ? C68 C69 1.398(8) . ? C69 C70 1.414(8) . ? C70 C71 1.396(8) . ? C71 C72 1.332(8) . ? C76 C77 1.514(6) . ? C77 C78 1.512(7) . ? C78 C79 1.396(8) . ? C79 C80 1.364(9) . ? C80 C81 1.355(9) . ? C81 C82 1.418(8) . ? C91 C92 1.377(6) . ? C93 C94 1.402(6) . ? C93 C105 1.519(6) . ? C94 C95 1.492(7) . ? C96 C97 1.525(6) . ? C97 C98 1.503(7) . ? C98 C99 1.417(7) . ? C99 C100 1.377(7) . ? C100 C101 1.374(8) . ? C101 C102 1.405(8) . ? C106 C107 1.504(6) . ? C107 C108 1.484(7) . ? C108 C109 1.407(8) . ? C109 C110 1.407(9) . ? C110 C111 1.359(9) . ? C111 C112 1.372(8) . ? Ni5 N26 2.016(5) . ? Ni5 N38 2.034(4) . ? Ni5 N27 2.116(6) . ? Ni5 N39 2.122(5) . ? Ni5 N25 2.141(5) . ? Ni5 N37 2.148(4) . ? Ni6 N44 2.019(4) . ? Ni6 N29 2.029(5) . ? Ni6 N45 2.117(5) . ? Ni6 N28 2.118(5) . ? Ni6 N30 2.123(8) . ? Ni6 N43 2.135(4) . ? Ni7 N32 2.035(5) . ? Ni7 N41 2.043(4) . ? Ni7 N33 2.104(5) . ? Ni7 N42 2.123(4) . ? Ni7 N31 2.136(4) . ? Ni7 N40 2.174(4) . ? Ni8 N35 2.026(4) . ? Ni8 N47 2.045(4) . ? Ni8 N34 2.118(4) . ? Ni8 N48 2.123(4) . ? Ni8 N36 2.132(5) . ? Ni8 N46 2.153(4) . ? O9 C125 1.333(7) . ? O10 C135 1.300(6) . ? O11 C155 1.284(6) . ? O12 C165 1.294(5) . ? O13 C185 1.276(6) . ? O14 C195 1.310(5) . ? O15 C215 1.294(6) . ? O16 C225 1.296(6) . ? N25 C121 1.354(7) . ? N25 C124 1.370(7) . ? N26 C125 1.274(7) . ? N26 C126 1.450(7) . ? N28 C122 1.346(6) . ? N28 C123 1.364(6) . ? N29 C135 1.280(7) . ? N29 C136 1.460(7) . ? N31 C151 1.325(6) . ? N31 C154 1.358(6) . ? N32 C155 1.290(7) . ? N32 C156 1.479(6) . ? N33 C162 1.348(7) . ? N33 C158 1.356(7) . ? N34 C152 1.328(6) . ? N34 C153 1.353(6) . ? N35 C165 1.296(7) . ? N35 C166 1.461(6) . ? N36 C172 1.345(7) . ? N36 C168 1.350(7) . ? N37 C181 1.306(6) . ? N37 C184 1.367(6) . ? N38 C185 1.304(6) . ? N38 C186 1.467(6) . ? N40 C182 1.315(6) . ? N40 C183 1.346(6) . ? N41 C195 1.280(6) . ? N41 C196 1.480(5) . ? N42 C202 1.350(6) . ? N42 C198 1.361(6) . ? N43 C211 1.332(6) . ? N43 C214 1.353(6) . ? N44 C215 1.285(7) . ? N44 C216 1.466(6) . ? N46 C212 1.306(6) . ? N46 C213 1.343(6) . ? N47 C225 1.277(6) . ? N47 C226 1.484(5) . ? N48 C232 1.335(6) . ? N48 C228 1.351(6) . ? C121 C122 1.372(8) . ? C123 C124 1.390(8) . ? C123 C135 1.507(8) . ? C124 C125 1.522(8) . ? C126 C127 1.521(8) . ? C127 C128 1.533(10) . ? N27 C132 1.355(8) . ? N27 C128 1.359(8) . ? C128 C129 1.391(11) . ? C129 C130 1.378(12) . ? C130 C131 1.375(11) . ? C131 C132 1.369(10) . ? C136 C137 1.537(10) . ? C137 C138 1.443(13) . ? N30 C138 1.339(11) . ? N30 C142 1.366(12) . ? C138 C139 1.423(16) . ? C139 C140 1.43(2) . ? C140 C141 1.404(18) . ? C141 C142 1.386(15) . ? C151 C152 1.381(7) . ? C153 C154 1.398(7) . ? C153 C165 1.511(7) . ? C154 C155 1.531(7) . ? C156 C157 1.500(7) . ? C157 C158 1.499(8) . ? C158 C159 1.418(9) . ? C159 C160 1.367(10) . ? C160 C161 1.370(10) . ? C161 C162 1.375(8) . ? C166 C167 1.515(7) . ? C167 C168 1.477(8) . ? C168 C169 1.406(8) . ? C169 C170 1.380(9) . ? C170 C171 1.390(8) . ? C171 C172 1.377(8) . ? C181 C182 1.408(7) . ? C183 C184 1.410(6) . ? C183 C195 1.493(6) . ? C184 C185 1.503(7) . ? C186 C187 1.560(8) . ? C187 C188 1.460(9) . ? N39 C188 1.330(8) . ? N39 C192 1.331(8) . ? C188 C189 1.435(9) . ? C189 C190 1.387(12) . ? C190 C191 1.381(12) . ? C191 C192 1.368(10) . ? C196 C197 1.529(6) . ? C197 C198 1.490(7) . ? C198 C199 1.396(7) . ? C199 C200 1.383(7) . ? C200 C201 1.380(7) . ? C201 C202 1.374(7) . ? C211 C212 1.413(7) . ? C213 C214 1.429(7) . ? C213 C225 1.530(6) . ? C214 C215 1.503(7) . ? C216 C217 1.566(8) . ? C217 C218 1.567(11) . ? N45 C222 1.301(8) . ? N45 C218 1.315(9) . ? C218 C219 1.372(10) . ? C219 C220 1.312(11) . ? C220 C221 1.385(11) . ? C221 C222 1.375(9) . ? C226 C227 1.533(7) . ? C227 C228 1.508(7) . ? C228 C229 1.395(7) . ? C229 C230 1.343(7) . ? C230 C231 1.383(7) . ? C231 C232 1.389(7) . ? B1 F11 1.341(8) . ? B1 F13 1.354(10) . ? B1 F14 1.393(10) . ? B1 F12 1.406(10) . ? B2 F23 1.330(8) . ? B2 F22 1.335(8) . ? B2 F21 1.349(9) . ? B2 F24 1.368(9) . ? B3 F33 1.316(13) . ? B3 F31 1.331(10) . ? B3 F34 1.378(12) . ? B3 F32 1.401(11) . ? B4 F44 1.303(11) . ? B4 F42 1.334(11) . ? B4 F43 1.361(10) . ? B4 F41 1.377(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N14 165.7(2) . . ? N2 Ni1 N3 92.4(2) . . ? N14 Ni1 N3 97.2(2) . . ? N2 Ni1 N1 77.3(2) . . ? N14 Ni1 N1 92.41(17) . . ? N3 Ni1 N1 169.3(2) . . ? N2 Ni1 N15 96.9(2) . . ? N14 Ni1 N15 92.3(2) . . ? N3 Ni1 N15 97.7(2) . . ? N1 Ni1 N15 86.40(18) . . ? N2 Ni1 N13 92.26(19) . . ? N14 Ni1 N13 77.10(17) . . ? N3 Ni1 N13 90.77(18) . . ? N1 Ni1 N13 86.96(16) . . ? N15 Ni1 N13 167.24(18) . . ? N5 Ni2 N20 165.78(19) . . ? N5 Ni2 N4 77.4(2) . . ? N20 Ni2 N4 92.05(17) . . ? N5 Ni2 N6 91.0(2) . . ? N20 Ni2 N6 98.71(19) . . ? N4 Ni2 N6 167.78(19) . . ? N5 Ni2 N21 98.09(19) . . ? N20 Ni2 N21 91.17(17) . . ? N4 Ni2 N21 89.19(17) . . ? N6 Ni2 N21 96.32(18) . . ? N5 Ni2 N19 93.56(17) . . ? N20 Ni2 N19 76.04(16) . . ? N4 Ni2 N19 86.10(16) . . ? N6 Ni2 N19 90.87(17) . . ? N21 Ni2 N19 166.17(17) . . ? N8 Ni3 N17 167.00(17) . . ? N8 Ni3 N9 92.62(17) . . ? N17 Ni3 N9 96.46(16) . . ? N8 Ni3 N16 94.55(18) . . ? N17 Ni3 N16 76.77(16) . . ? N9 Ni3 N16 86.58(16) . . ? N8 Ni3 N7 75.83(17) . . ? N17 Ni3 N7 93.69(16) . . ? N9 Ni3 N7 165.63(16) . . ? N16 Ni3 N7 85.87(15) . . ? N8 Ni3 N18 96.49(19) . . ? N17 Ni3 N18 90.62(17) . . ? N9 Ni3 N18 102.51(16) . . ? N16 Ni3 N18 165.32(16) . . ? N7 Ni3 N18 87.49(16) . . ? N23 Ni4 N11 166.12(17) . . ? N23 Ni4 N12 95.92(17) . . ? N11 Ni4 N12 93.07(18) . . ? N23 Ni4 N10 93.31(16) . . ? N11 Ni4 N10 76.56(17) . . ? N12 Ni4 N10 168.23(16) . . ? N23 Ni4 N22 76.58(16) . . ? N11 Ni4 N22 93.20(16) . . ? N12 Ni4 N22 88.07(16) . . ? N10 Ni4 N22 86.98(14) . . ? N23 Ni4 N24 91.65(18) . . ? N11 Ni4 N24 96.93(18) . . ? N12 Ni4 N24 101.44(16) . . ? N10 Ni4 N24 85.55(15) . . ? N22 Ni4 N24 165.67(17) . . ? C1 N1 C4 118.9(5) . . ? C1 N1 Ni1 124.8(4) . . ? C4 N1 Ni1 116.2(4) . . ? C5 N2 C6 115.7(6) . . ? C5 N2 Ni1 120.3(4) . . ? C6 N2 Ni1 123.7(5) . . ? C12 N3 C8 115.9(6) . . ? C12 N3 Ni1 121.1(4) . . ? C8 N3 Ni1 123.0(5) . . ? C2 N4 C3 119.6(5) . . ? C2 N4 Ni2 124.2(4) . . ? C3 N4 Ni2 116.2(4) . . ? C15 N5 C16 115.1(5) . . ? C15 N5 Ni2 119.3(4) . . ? C16 N5 Ni2 125.2(4) . . ? C22 N6 C18 119.3(6) . . ? C22 N6 Ni2 117.3(4) . . ? C18 N6 Ni2 123.2(5) . . ? C31 N7 C34 118.8(5) . . ? C31 N7 Ni3 125.3(4) . . ? C34 N7 Ni3 115.9(3) . . ? C35 N8 C36 114.6(5) . . ? C35 N8 Ni3 120.8(4) . . ? C36 N8 Ni3 124.6(4) . . ? C42 N9 C38 117.0(5) . . ? C42 N9 Ni3 118.7(4) . . ? C38 N9 Ni3 121.8(4) . . ? C32 N10 C33 119.8(4) . . ? C32 N10 Ni4 124.7(3) . . ? C33 N10 Ni4 115.6(3) . . ? C45 N11 C46 117.4(4) . . ? C45 N11 Ni4 119.6(4) . . ? C46 N11 Ni4 122.9(4) . . ? C48 N12 C52 117.0(5) . . ? C48 N12 Ni4 123.0(4) . . ? C52 N12 Ni4 118.6(4) . . ? C61 N13 C64 119.9(5) . . ? C61 N13 Ni1 125.8(4) . . ? C64 N13 Ni1 114.3(4) . . ? C65 N14 C66 116.0(4) . . ? C65 N14 Ni1 117.6(4) . . ? C66 N14 Ni1 125.7(3) . . ? C68 N15 C72 118.2(6) . . ? C68 N15 Ni1 121.3(4) . . ? C72 N15 Ni1 119.8(5) . . ? C62 N16 C63 118.6(5) . . ? C62 N16 Ni3 125.7(4) . . ? C63 N16 Ni3 115.7(3) . . ? C75 N17 C76 114.6(4) . . ? C75 N17 Ni3 118.4(3) . . ? C76 N17 Ni3 126.8(3) . . ? C78 N18 C82 117.2(5) . . ? C78 N18 Ni3 121.2(4) . . ? C82 N18 Ni3 117.6(4) . . ? C91 N19 C94 119.8(4) . . ? C91 N19 Ni2 124.7(3) . . ? C94 N19 Ni2 115.4(3) . . ? C95 N20 C96 115.8(4) . . ? C95 N20 Ni2 118.7(4) . . ? C96 N20 Ni2 124.7(3) . . ? C98 N21 C102 118.4(5) . . ? C98 N21 Ni2 124.1(4) . . ? C102 N21 Ni2 116.6(4) . . ? C92 N22 C93 118.9(4) . . ? C92 N22 Ni4 125.6(3) . . ? C93 N22 Ni4 115.5(3) . . ? C105 N23 C106 115.2(4) . . ? C105 N23 Ni4 118.4(3) . . ? C106 N23 Ni4 125.9(3) . . ? C112 N24 C108 118.4(5) . . ? C112 N24 Ni4 117.4(4) . . ? C108 N24 Ni4 119.3(4) . . ? N1 C1 C2 121.7(5) . . ? N4 C2 C1 120.6(5) . . ? N4 C3 C4 118.7(5) . . ? N4 C3 C15 110.5(5) . . ? C4 C3 C15 130.8(5) . . ? N1 C4 C3 120.5(5) . . ? N1 C4 C5 111.2(6) . . ? C3 C4 C5 128.3(6) . . ? N2 C5 O1 129.0(6) . . ? N2 C5 C4 114.1(6) . . ? O1 C5 C4 117.0(6) . . ? N2 C6 C7 109.0(6) . . ? C8 C7 C6 115.4(6) . . ? N3 C8 C9 120.5(7) . . ? N3 C8 C7 118.6(7) . . ? C9 C8 C7 120.9(7) . . ? C10 C9 C8 121.0(8) . . ? C9 C10 C11 120.1(7) . . ? C12 C11 C10 114.7(7) . . ? N3 C12 C11 127.8(6) . . ? N5 C15 O2 126.9(6) . . ? N5 C15 C3 115.4(5) . . ? O2 C15 C3 117.7(6) . . ? N5 C16 C17 108.6(5) . . ? C16 C17 C18 114.8(5) . . ? N6 C18 C19 120.4(7) . . ? N6 C18 C17 118.7(6) . . ? C19 C18 C17 120.8(7) . . ? C20 C19 C18 118.6(7) . . ? C21 C20 C19 120.8(8) . . ? C20 C21 C22 117.5(8) . . ? N6 C22 C21 123.3(6) . . ? N7 C31 C32 121.0(5) . . ? N10 C32 C31 121.0(5) . . ? N10 C33 C34 119.9(5) . . ? N10 C33 C45 112.5(5) . . ? C34 C33 C45 127.5(5) . . ? N7 C34 C33 119.4(4) . . ? N7 C34 C35 112.1(5) . . ? C33 C34 C35 128.5(5) . . ? O3 C35 N8 123.7(5) . . ? O3 C35 C34 121.7(5) . . ? N8 C35 C34 114.5(5) . . ? N8 C36 C37 110.5(5) . . ? C36 C37 C38 114.8(6) . . ? N9 C38 C39 122.6(6) . . ? N9 C38 C37 116.0(5) . . ? C39 C38 C37 121.4(5) . . ? C40 C39 C38 119.1(6) . . ? C39 C40 C41 120.2(6) . . ? C42 C41 C40 116.6(6) . . ? N9 C42 C41 124.5(5) . . ? O4 C45 N11 122.7(5) . . ? O4 C45 C33 122.1(5) . . ? N11 C45 C33 115.2(5) . . ? N11 C46 C47 109.8(5) . . ? C48 C47 C46 114.6(5) . . ? N12 C48 C49 122.8(5) . . ? N12 C48 C47 116.9(5) . . ? C49 C48 C47 120.3(5) . . ? C50 C49 C48 117.4(5) . . ? C51 C50 C49 120.6(5) . . ? C50 C51 C52 118.0(5) . . ? N12 C52 C51 124.1(5) . . ? N13 C61 C62 122.1(5) . . ? N16 C62 C61 120.6(5) . . ? N16 C63 C64 120.5(4) . . ? N16 C63 C75 111.8(4) . . ? C64 C63 C75 127.4(5) . . ? N13 C64 C63 118.2(5) . . ? N13 C64 C65 113.9(5) . . ? C63 C64 C65 127.9(5) . . ? O5 C65 N14 121.5(5) . . ? O5 C65 C64 123.3(5) . . ? N14 C65 C64 115.2(5) . . ? N14 C66 C67 108.6(5) . . ? C68 C67 C66 115.0(5) . . ? N15 C68 C69 121.9(6) . . ? N15 C68 C67 120.6(6) . . ? C69 C68 C67 117.5(7) . . ? C68 C69 C70 118.9(7) . . ? C71 C70 C69 116.8(7) . . ? C72 C71 C70 119.7(7) . . ? C71 C72 N15 124.5(7) . . ? O6 C75 N17 123.9(4) . . ? O6 C75 C63 120.6(5) . . ? N17 C75 C63 115.6(4) . . ? N17 C76 C77 109.6(4) . . ? C78 C77 C76 113.0(4) . . ? N18 C78 C79 122.0(6) . . ? N18 C78 C77 116.7(5) . . ? C79 C78 C77 121.3(6) . . ? C80 C79 C78 121.2(7) . . ? C81 C80 C79 117.4(7) . . ? C80 C81 C82 120.7(7) . . ? N18 C82 C81 121.5(6) . . ? N19 C91 C92 119.3(5) . . ? N22 C92 C91 122.4(5) . . ? N22 C93 C94 120.5(4) . . ? N22 C93 C105 111.8(4) . . ? C94 C93 C105 127.5(5) . . ? N19 C94 C93 118.9(4) . . ? N19 C94 C95 111.4(4) . . ? C93 C94 C95 129.6(5) . . ? N20 C95 O7 123.5(5) . . ? N20 C95 C94 116.5(5) . . ? O7 C95 C94 120.0(4) . . ? N20 C96 C97 110.1(4) . . ? C98 C97 C96 114.0(5) . . ? N21 C98 C99 121.7(6) . . ? N21 C98 C97 118.3(5) . . ? C99 C98 C97 119.9(5) . . ? C100 C99 C98 119.6(6) . . ? C101 C100 C99 119.1(6) . . ? C100 C101 C102 119.7(6) . . ? N21 C102 C101 121.4(6) . . ? O8 C105 N23 123.6(4) . . ? O8 C105 C93 120.9(5) . . ? N23 C105 C93 115.5(4) . . ? N23 C106 C107 110.8(4) . . ? C108 C107 C106 113.0(5) . . ? N24 C108 C109 120.9(6) . . ? N24 C108 C107 119.0(5) . . ? C109 C108 C107 120.0(6) . . ? C110 C109 C108 118.7(6) . . ? C111 C110 C109 119.0(6) . . ? C110 C111 C112 119.2(7) . . ? N24 C112 C111 123.6(6) . . ? N26 Ni5 N38 166.3(2) . . ? N26 Ni5 N27 91.7(3) . . ? N38 Ni5 N27 97.4(2) . . ? N26 Ni5 N39 97.2(2) . . ? N38 Ni5 N39 92.2(2) . . ? N27 Ni5 N39 94.9(2) . . ? N26 Ni5 N25 76.2(2) . . ? N38 Ni5 N25 93.76(19) . . ? N27 Ni5 N25 167.2(2) . . ? N39 Ni5 N25 90.9(2) . . ? N26 Ni5 N37 93.33(19) . . ? N38 Ni5 N37 76.80(18) . . ? N27 Ni5 N37 88.39(18) . . ? N39 Ni5 N37 168.8(2) . . ? N25 Ni5 N37 88.13(16) . . ? N44 Ni6 N29 168.2(2) . . ? N44 Ni6 N45 91.7(2) . . ? N29 Ni6 N45 96.0(2) . . ? N44 Ni6 N28 93.78(19) . . ? N29 Ni6 N28 77.0(2) . . ? N45 Ni6 N28 92.1(2) . . ? N44 Ni6 N30 97.2(3) . . ? N29 Ni6 N30 91.1(3) . . ? N45 Ni6 N30 95.1(3) . . ? N28 Ni6 N30 166.7(2) . . ? N44 Ni6 N43 76.61(18) . . ? N29 Ni6 N43 95.42(18) . . ? N45 Ni6 N43 168.2(2) . . ? N28 Ni6 N43 87.63(16) . . ? N30 Ni6 N43 87.5(3) . . ? N32 Ni7 N41 167.55(18) . . ? N32 Ni7 N33 91.6(2) . . ? N41 Ni7 N33 96.6(2) . . ? N32 Ni7 N42 96.15(18) . . ? N41 Ni7 N42 91.82(17) . . ? N33 Ni7 N42 99.00(17) . . ? N32 Ni7 N31 76.57(19) . . ? N41 Ni7 N31 94.00(17) . . ? N33 Ni7 N31 166.11(17) . . ? N42 Ni7 N31 89.55(16) . . ? N32 Ni7 N40 95.31(17) . . ? N41 Ni7 N40 75.61(16) . . ? N33 Ni7 N40 88.56(17) . . ? N42 Ni7 N40 166.07(16) . . ? N31 Ni7 N40 85.45(15) . . ? N35 Ni8 N47 166.66(18) . . ? N35 Ni8 N34 76.96(19) . . ? N47 Ni8 N34 93.86(16) . . ? N35 Ni8 N48 97.16(17) . . ? N47 Ni8 N48 92.13(17) . . ? N34 Ni8 N48 88.15(16) . . ? N35 Ni8 N36 91.2(2) . . ? N47 Ni8 N36 97.12(18) . . ? N34 Ni8 N36 167.58(16) . . ? N48 Ni8 N36 97.21(17) . . ? N35 Ni8 N46 93.76(16) . . ? N47 Ni8 N46 75.81(16) . . ? N34 Ni8 N46 86.42(16) . . ? N48 Ni8 N46 166.39(16) . . ? N36 Ni8 N46 90.63(17) . . ? C121 N25 C124 119.5(6) . . ? C121 N25 Ni5 123.3(5) . . ? C124 N25 Ni5 117.2(4) . . ? C125 N26 C126 116.7(6) . . ? C125 N26 Ni5 119.2(5) . . ? C126 N26 Ni5 123.8(5) . . ? C122 N28 C123 117.4(6) . . ? C122 N28 Ni6 127.3(4) . . ? C123 N28 Ni6 115.1(4) . . ? C135 N29 C136 116.5(6) . . ? C135 N29 Ni6 119.3(4) . . ? C136 N29 Ni6 124.1(5) . . ? C151 N31 C154 118.9(5) . . ? C151 N31 Ni7 124.8(4) . . ? C154 N31 Ni7 116.2(4) . . ? C155 N32 C156 116.5(5) . . ? C155 N32 Ni7 119.0(4) . . ? C156 N32 Ni7 124.4(4) . . ? C162 N33 C158 118.0(6) . . ? C162 N33 Ni7 120.1(4) . . ? C158 N33 Ni7 121.1(5) . . ? C152 N34 C153 119.7(5) . . ? C152 N34 Ni8 124.7(4) . . ? C153 N34 Ni8 115.6(4) . . ? C165 N35 C166 117.1(5) . . ? C165 N35 Ni8 118.9(4) . . ? C166 N35 Ni8 123.9(4) . . ? C172 N36 C168 119.2(6) . . ? C172 N36 Ni8 118.9(4) . . ? C168 N36 Ni8 121.6(5) . . ? C181 N37 C184 121.2(5) . . ? C181 N37 Ni5 124.3(4) . . ? C184 N37 Ni5 114.3(3) . . ? C185 N38 C186 117.5(5) . . ? C185 N38 Ni5 119.4(4) . . ? C186 N38 Ni5 122.8(4) . . ? C182 N40 C183 122.0(4) . . ? C182 N40 Ni7 122.9(4) . . ? C183 N40 Ni7 115.0(3) . . ? C195 N41 C196 116.4(4) . . ? C195 N41 Ni7 119.0(3) . . ? C196 N41 Ni7 124.3(3) . . ? C202 N42 C198 118.2(4) . . ? C202 N42 Ni7 119.6(4) . . ? C198 N42 Ni7 121.8(4) . . ? C211 N43 C214 119.8(5) . . ? C211 N43 Ni6 124.5(4) . . ? C214 N43 Ni6 115.6(3) . . ? C215 N44 C216 116.2(5) . . ? C215 N44 Ni6 119.1(4) . . ? C216 N44 Ni6 124.7(4) . . ? C212 N46 C213 119.7(4) . . ? C212 N46 Ni8 124.3(3) . . ? C213 N46 Ni8 116.0(3) . . ? C225 N47 C226 116.2(4) . . ? C225 N47 Ni8 120.3(4) . . ? C226 N47 Ni8 123.3(3) . . ? C232 N48 C228 118.3(4) . . ? C232 N48 Ni8 118.5(3) . . ? C228 N48 Ni8 122.5(4) . . ? N25 C121 C122 118.7(6) . . ? N28 C122 C121 123.6(6) . . ? N28 C123 C124 120.5(5) . . ? N28 C123 C135 112.0(6) . . ? C124 C123 C135 127.5(6) . . ? N25 C124 C123 120.1(5) . . ? N25 C124 C125 108.2(6) . . ? C123 C124 C125 131.6(6) . . ? N26 C125 O9 123.8(6) . . ? N26 C125 C124 118.6(6) . . ? O9 C125 C124 117.5(7) . . ? N26 C126 C127 110.7(6) . . ? C126 C127 C128 113.9(6) . . ? C132 N27 C128 115.5(7) . . ? C132 N27 Ni5 120.0(5) . . ? C128 N27 Ni5 124.2(6) . . ? N27 C128 C129 121.9(9) . . ? N27 C128 C127 116.9(9) . . ? C129 C128 C127 121.2(9) . . ? C130 C129 C128 119.7(10) . . ? C131 C130 C129 119.9(11) . . ? C132 C131 C130 116.8(10) . . ? N27 C132 C131 126.2(8) . . ? N29 C135 O10 123.7(6) . . ? N29 C135 C123 116.0(6) . . ? O10 C135 C123 120.3(7) . . ? N29 C136 C137 111.8(6) . . ? C138 C137 C136 114.2(9) . . ? C138 N30 C142 116.2(10) . . ? C138 N30 Ni6 123.4(8) . . ? C142 N30 Ni6 118.1(8) . . ? N30 C138 C139 120.8(12) . . ? N30 C138 C137 119.0(12) . . ? C139 C138 C137 120.3(14) . . ? C138 C139 C140 122.4(17) . . ? C141 C140 C139 115.2(18) . . ? C142 C141 C140 118.3(17) . . ? N30 C142 C141 126.9(13) . . ? N31 C151 C152 121.5(5) . . ? N34 C152 C151 120.3(5) . . ? N34 C153 C154 119.7(5) . . ? N34 C153 C165 112.2(5) . . ? C154 C153 C165 128.0(5) . . ? N31 C154 C153 119.8(5) . . ? N31 C154 C155 110.8(5) . . ? C153 C154 C155 129.3(5) . . ? O11 C155 N32 123.4(5) . . ? O11 C155 C154 120.4(6) . . ? N32 C155 C154 116.1(5) . . ? N32 C156 C157 111.0(5) . . ? C158 C157 C156 113.2(5) . . ? N33 C158 C159 118.8(7) . . ? N33 C158 C157 120.3(6) . . ? C159 C158 C157 121.0(7) . . ? C160 C159 C158 121.3(8) . . ? C159 C160 C161 119.5(8) . . ? C160 C161 C162 117.3(8) . . ? N33 C162 C161 125.1(6) . . ? O12 C165 N35 123.7(6) . . ? O12 C165 C153 121.2(6) . . ? N35 C165 C153 115.1(5) . . ? N35 C166 C167 110.7(4) . . ? C168 C167 C166 113.2(5) . . ? N36 C168 C169 118.6(6) . . ? N36 C168 C167 119.6(6) . . ? C169 C168 C167 121.8(6) . . ? C170 C169 C168 122.6(7) . . ? C169 C170 C171 117.0(7) . . ? C172 C171 C170 118.8(7) . . ? N36 C172 C171 123.8(6) . . ? N37 C181 C182 119.9(5) . . ? N40 C182 C181 119.6(5) . . ? N40 C183 C184 118.4(4) . . ? N40 C183 C195 112.2(4) . . ? C184 C183 C195 129.2(5) . . ? N37 C184 C183 118.8(5) . . ? N37 C184 C185 113.1(5) . . ? C183 C184 C185 128.1(5) . . ? O13 C185 N38 124.5(5) . . ? O13 C185 C184 120.9(5) . . ? N38 C185 C184 114.6(5) . . ? N38 C186 C187 110.3(5) . . ? C188 C187 C186 114.6(6) . . ? C188 N39 C192 119.5(7) . . ? C188 N39 Ni5 121.6(5) . . ? C192 N39 Ni5 118.9(5) . . ? N39 C188 C189 120.0(8) . . ? N39 C188 C187 121.9(7) . . ? C189 C188 C187 118.0(8) . . ? C190 C189 C188 116.4(9) . . ? C191 C190 C189 123.9(9) . . ? C192 C191 C190 113.6(9) . . ? N39 C192 C191 126.5(8) . . ? N41 C195 O14 123.1(5) . . ? N41 C195 C183 116.9(4) . . ? O14 C195 C183 120.0(5) . . ? N41 C196 C197 109.1(4) . . ? C198 C197 C196 115.2(5) . . ? N42 C198 C199 120.1(5) . . ? N42 C198 C197 118.9(5) . . ? C199 C198 C197 120.9(5) . . ? C200 C199 C198 120.2(5) . . ? C201 C200 C199 119.6(5) . . ? C202 C201 C200 117.6(6) . . ? N42 C202 C201 124.3(5) . . ? N43 C211 C212 120.8(5) . . ? N46 C212 C211 120.6(5) . . ? N46 C213 C214 120.9(4) . . ? N46 C213 C225 112.0(5) . . ? C214 C213 C225 127.0(5) . . ? N43 C214 C213 118.2(5) . . ? N43 C214 C215 111.4(5) . . ? C213 C214 C215 130.4(5) . . ? N44 C215 O15 124.9(5) . . ? N44 C215 C214 116.4(5) . . ? O15 C215 C214 118.7(5) . . ? N44 C216 C217 107.4(5) . . ? C216 C217 C218 111.9(7) . . ? C222 N45 C218 114.6(6) . . ? C222 N45 Ni6 120.9(5) . . ? C218 N45 Ni6 124.1(6) . . ? N45 C218 C219 124.9(9) . . ? N45 C218 C217 117.2(7) . . ? C219 C218 C217 117.2(9) . . ? C220 C219 C218 119.5(9) . . ? C219 C220 C221 118.1(8) . . ? C222 C221 C220 117.3(9) . . ? N45 C222 C221 125.2(8) . . ? N47 C225 O16 124.5(5) . . ? N47 C225 C213 115.0(5) . . ? O16 C225 C213 120.5(5) . . ? N47 C226 C227 110.5(4) . . ? C228 C227 C226 113.0(4) . . ? N48 C228 C229 119.9(5) . . ? N48 C228 C227 118.8(5) . . ? C229 C228 C227 121.2(5) . . ? C230 C229 C228 121.2(5) . . ? C229 C230 C231 119.5(5) . . ? C230 C231 C232 117.3(6) . . ? N48 C232 C231 123.7(5) . . ? F11 B1 F13 109.6(9) . . ? F11 B1 F14 108.2(8) . . ? F13 B1 F14 111.2(7) . . ? F11 B1 F12 107.8(7) . . ? F13 B1 F12 111.8(8) . . ? F14 B1 F12 108.1(8) . . ? F23 B2 F22 113.0(7) . . ? F23 B2 F21 111.6(7) . . ? F22 B2 F21 110.3(7) . . ? F23 B2 F24 108.1(7) . . ? F22 B2 F24 110.0(7) . . ? F21 B2 F24 103.4(7) . . ? F33 B3 F31 110.8(10) . . ? F33 B3 F34 115.1(10) . . ? F31 B3 F34 108.1(10) . . ? F33 B3 F32 107.7(10) . . ? F31 B3 F32 107.2(9) . . ? F34 B3 F32 107.6(10) . . ? F44 B4 F42 108.1(9) . . ? F44 B4 F43 109.9(10) . . ? F42 B4 F43 106.6(9) . . ? F44 B4 F41 115.0(9) . . ? F42 B4 F41 112.1(9) . . ? F43 B4 F41 104.9(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 173.8(4) . . . . ? N14 Ni1 N1 C1 -16.3(4) . . . . ? N3 Ni1 N1 C1 -171.1(9) . . . . ? N15 Ni1 N1 C1 75.9(4) . . . . ? N13 Ni1 N1 C1 -93.2(4) . . . . ? N2 Ni1 N1 C4 -2.5(4) . . . . ? N14 Ni1 N1 C4 167.5(4) . . . . ? N3 Ni1 N1 C4 12.6(12) . . . . ? N15 Ni1 N1 C4 -100.4(4) . . . . ? N13 Ni1 N1 C4 90.5(4) . . . . ? N14 Ni1 N2 C5 -36.9(11) . . . . ? N3 Ni1 N2 C5 -169.2(5) . . . . ? N1 Ni1 N2 C5 8.0(5) . . . . ? N15 Ni1 N2 C5 92.7(5) . . . . ? N13 Ni1 N2 C5 -78.4(5) . . . . ? N14 Ni1 N2 C6 136.1(8) . . . . ? N3 Ni1 N2 C6 3.8(5) . . . . ? N1 Ni1 N2 C6 -179.0(5) . . . . ? N15 Ni1 N2 C6 -94.3(5) . . . . ? N13 Ni1 N2 C6 94.6(5) . . . . ? N2 Ni1 N3 C12 151.9(5) . . . . ? N14 Ni1 N3 C12 -17.5(5) . . . . ? N1 Ni1 N3 C12 137.2(9) . . . . ? N15 Ni1 N3 C12 -110.8(5) . . . . ? N13 Ni1 N3 C12 59.6(5) . . . . ? N2 Ni1 N3 C8 -25.5(5) . . . . ? N14 Ni1 N3 C8 165.1(5) . . . . ? N1 Ni1 N3 C8 -40.2(12) . . . . ? N15 Ni1 N3 C8 71.8(5) . . . . ? N13 Ni1 N3 C8 -117.8(5) . . . . ? N5 Ni2 N4 C2 -174.9(4) . . . . ? N20 Ni2 N4 C2 14.7(4) . . . . ? N6 Ni2 N4 C2 166.6(7) . . . . ? N21 Ni2 N4 C2 -76.4(4) . . . . ? N19 Ni2 N4 C2 90.6(4) . . . . ? N5 Ni2 N4 C3 6.6(3) . . . . ? N20 Ni2 N4 C3 -163.7(4) . . . . ? N6 Ni2 N4 C3 -11.9(10) . . . . ? N21 Ni2 N4 C3 105.1(4) . . . . ? N19 Ni2 N4 C3 -87.9(4) . . . . ? N20 Ni2 N5 C15 32.1(11) . . . . ? N4 Ni2 N5 C15 -10.7(5) . . . . ? N6 Ni2 N5 C15 165.4(5) . . . . ? N21 Ni2 N5 C15 -98.1(5) . . . . ? N19 Ni2 N5 C15 74.5(5) . . . . ? N20 Ni2 N5 C16 -140.0(7) . . . . ? N4 Ni2 N5 C16 177.2(5) . . . . ? N6 Ni2 N5 C16 -6.6(5) . . . . ? N21 Ni2 N5 C16 89.9(5) . . . . ? N19 Ni2 N5 C16 -97.6(4) . . . . ? N5 Ni2 N6 C22 -151.3(4) . . . . ? N20 Ni2 N6 C22 18.3(4) . . . . ? N4 Ni2 N6 C22 -133.2(8) . . . . ? N21 Ni2 N6 C22 110.4(4) . . . . ? N19 Ni2 N6 C22 -57.7(4) . . . . ? N5 Ni2 N6 C18 24.5(5) . . . . ? N20 Ni2 N6 C18 -165.9(5) . . . . ? N4 Ni2 N6 C18 42.7(11) . . . . ? N21 Ni2 N6 C18 -73.7(5) . . . . ? N19 Ni2 N6 C18 118.1(5) . . . . ? N8 Ni3 N7 C31 -173.6(4) . . . . ? N17 Ni3 N7 C31 14.2(4) . . . . ? N9 Ni3 N7 C31 149.1(6) . . . . ? N16 Ni3 N7 C31 90.7(4) . . . . ? N18 Ni3 N7 C31 -76.2(4) . . . . ? N8 Ni3 N7 C34 6.3(4) . . . . ? N17 Ni3 N7 C34 -165.9(4) . . . . ? N9 Ni3 N7 C34 -31.0(9) . . . . ? N16 Ni3 N7 C34 -89.5(4) . . . . ? N18 Ni3 N7 C34 103.6(4) . . . . ? N17 Ni3 N8 C35 28.0(11) . . . . ? N9 Ni3 N8 C35 162.3(5) . . . . ? N16 Ni3 N8 C35 75.5(5) . . . . ? N7 Ni3 N8 C35 -9.1(5) . . . . ? N18 Ni3 N8 C35 -94.8(5) . . . . ? N17 Ni3 N8 C36 -151.5(7) . . . . ? N9 Ni3 N8 C36 -17.2(5) . . . . ? N16 Ni3 N8 C36 -103.9(5) . . . . ? N7 Ni3 N8 C36 171.5(5) . . . . ? N18 Ni3 N8 C36 85.7(5) . . . . ? N8 Ni3 N9 C42 -145.0(4) . . . . ? N17 Ni3 N9 C42 25.6(4) . . . . ? N16 Ni3 N9 C42 -50.6(4) . . . . ? N7 Ni3 N9 C42 -109.0(7) . . . . ? N18 Ni3 N9 C42 117.7(4) . . . . ? N8 Ni3 N9 C38 16.5(4) . . . . ? N17 Ni3 N9 C38 -172.8(4) . . . . ? N16 Ni3 N9 C38 110.9(4) . . . . ? N7 Ni3 N9 C38 52.5(9) . . . . ? N18 Ni3 N9 C38 -80.8(4) . . . . ? N23 Ni4 N10 C32 -14.9(4) . . . . ? N11 Ni4 N10 C32 174.7(4) . . . . ? N12 Ni4 N10 C32 -156.5(7) . . . . ? N22 Ni4 N10 C32 -91.3(4) . . . . ? N24 Ni4 N10 C32 76.5(4) . . . . ? N23 Ni4 N10 C33 166.3(3) . . . . ? N11 Ni4 N10 C33 -4.1(3) . . . . ? N12 Ni4 N10 C33 24.6(10) . . . . ? N22 Ni4 N10 C33 89.9(4) . . . . ? N24 Ni4 N10 C33 -102.4(4) . . . . ? N23 Ni4 N11 C45 -36.8(9) . . . . ? N12 Ni4 N11 C45 -167.1(4) . . . . ? N10 Ni4 N11 C45 7.3(4) . . . . ? N22 Ni4 N11 C45 -78.8(5) . . . . ? N24 Ni4 N11 C45 91.0(5) . . . . ? N23 Ni4 N11 C46 139.8(6) . . . . ? N12 Ni4 N11 C46 9.4(4) . . . . ? N10 Ni4 N11 C46 -176.2(4) . . . . ? N22 Ni4 N11 C46 97.7(4) . . . . ? N24 Ni4 N11 C46 -92.5(4) . . . . ? N23 Ni4 N12 C48 171.3(4) . . . . ? N11 Ni4 N12 C48 -19.3(4) . . . . ? N10 Ni4 N12 C48 -47.3(10) . . . . ? N22 Ni4 N12 C48 -112.4(4) . . . . ? N24 Ni4 N12 C48 78.4(4) . . . . ? N23 Ni4 N12 C52 -22.8(4) . . . . ? N11 Ni4 N12 C52 146.6(4) . . . . ? N10 Ni4 N12 C52 118.7(8) . . . . ? N22 Ni4 N12 C52 53.5(4) . . . . ? N24 Ni4 N12 C52 -115.7(4) . . . . ? N2 Ni1 N13 C61 -16.2(5) . . . . ? N14 Ni1 N13 C61 173.4(5) . . . . ? N3 Ni1 N13 C61 76.2(5) . . . . ? N1 Ni1 N13 C61 -93.4(5) . . . . ? N15 Ni1 N13 C61 -152.2(9) . . . . ? N2 Ni1 N13 C64 164.6(4) . . . . ? N14 Ni1 N13 C64 -5.7(3) . . . . ? N3 Ni1 N13 C64 -103.0(4) . . . . ? N1 Ni1 N13 C64 87.4(4) . . . . ? N15 Ni1 N13 C64 28.7(11) . . . . ? N2 Ni1 N14 C65 -30.9(10) . . . . ? N3 Ni1 N14 C65 100.9(4) . . . . ? N1 Ni1 N14 C65 -74.5(4) . . . . ? N15 Ni1 N14 C65 -161.0(4) . . . . ? N13 Ni1 N14 C65 11.8(4) . . . . ? N2 Ni1 N14 C66 138.5(8) . . . . ? N3 Ni1 N14 C66 -89.6(5) . . . . ? N1 Ni1 N14 C66 94.9(4) . . . . ? N15 Ni1 N14 C66 8.5(5) . . . . ? N13 Ni1 N14 C66 -178.7(5) . . . . ? N2 Ni1 N15 C68 171.0(5) . . . . ? N14 Ni1 N15 C68 -20.0(5) . . . . ? N3 Ni1 N15 C68 77.6(5) . . . . ? N1 Ni1 N15 C68 -112.3(5) . . . . ? N13 Ni1 N15 C68 -53.5(12) . . . . ? N2 Ni1 N15 C72 -19.3(5) . . . . ? N14 Ni1 N15 C72 149.7(5) . . . . ? N3 Ni1 N15 C72 -112.6(5) . . . . ? N1 Ni1 N15 C72 57.5(5) . . . . ? N13 Ni1 N15 C72 116.3(9) . . . . ? N8 Ni3 N16 C62 18.9(4) . . . . ? N17 Ni3 N16 C62 -170.9(4) . . . . ? N9 Ni3 N16 C62 -73.5(4) . . . . ? N7 Ni3 N16 C62 94.3(4) . . . . ? N18 Ni3 N16 C62 157.6(6) . . . . ? N8 Ni3 N16 C63 -163.4(3) . . . . ? N17 Ni3 N16 C63 6.8(3) . . . . ? N9 Ni3 N16 C63 104.2(3) . . . . ? N7 Ni3 N16 C63 -88.0(3) . . . . ? N18 Ni3 N16 C63 -24.7(8) . . . . ? N8 Ni3 N17 C75 36.9(10) . . . . ? N9 Ni3 N17 C75 -97.1(4) . . . . ? N16 Ni3 N17 C75 -12.2(3) . . . . ? N7 Ni3 N17 C75 72.7(4) . . . . ? N18 Ni3 N17 C75 160.2(4) . . . . ? N8 Ni3 N17 C76 -138.3(7) . . . . ? N9 Ni3 N17 C76 87.7(4) . . . . ? N16 Ni3 N17 C76 172.7(4) . . . . ? N7 Ni3 N17 C76 -102.5(4) . . . . ? N18 Ni3 N17 C76 -14.9(4) . . . . ? N8 Ni3 N18 C78 -177.5(4) . . . . ? N17 Ni3 N18 C78 13.4(4) . . . . ? N9 Ni3 N18 C78 -83.3(4) . . . . ? N16 Ni3 N18 C78 44.0(9) . . . . ? N7 Ni3 N18 C78 107.1(4) . . . . ? N8 Ni3 N18 C82 25.9(4) . . . . ? N17 Ni3 N18 C82 -143.2(4) . . . . ? N9 Ni3 N18 C82 120.0(4) . . . . ? N16 Ni3 N18 C82 -112.7(7) . . . . ? N7 Ni3 N18 C82 -49.6(4) . . . . ? N5 Ni2 N19 C91 14.8(5) . . . . ? N20 Ni2 N19 C91 -175.0(5) . . . . ? N4 Ni2 N19 C91 91.9(4) . . . . ? N6 Ni2 N19 C91 -76.2(4) . . . . ? N21 Ni2 N19 C91 162.3(7) . . . . ? N5 Ni2 N19 C94 -163.4(4) . . . . ? N20 Ni2 N19 C94 6.8(3) . . . . ? N4 Ni2 N19 C94 -86.3(4) . . . . ? N6 Ni2 N19 C94 105.6(4) . . . . ? N21 Ni2 N19 C94 -15.9(9) . . . . ? N5 Ni2 N20 C95 31.3(10) . . . . ? N4 Ni2 N20 C95 72.9(4) . . . . ? N6 Ni2 N20 C95 -101.3(4) . . . . ? N21 Ni2 N20 C95 162.1(4) . . . . ? N19 Ni2 N20 C95 -12.6(4) . . . . ? N5 Ni2 N20 C96 -138.1(7) . . . . ? N4 Ni2 N20 C96 -96.6(4) . . . . ? N6 Ni2 N20 C96 89.2(4) . . . . ? N21 Ni2 N20 C96 -7.3(4) . . . . ? N19 Ni2 N20 C96 178.0(4) . . . . ? N5 Ni2 N21 C98 -171.8(5) . . . . ? N20 Ni2 N21 C98 19.0(5) . . . . ? N4 Ni2 N21 C98 111.1(5) . . . . ? N6 Ni2 N21 C98 -79.9(5) . . . . ? N19 Ni2 N21 C98 41.1(10) . . . . ? N5 Ni2 N21 C102 19.5(4) . . . . ? N20 Ni2 N21 C102 -149.6(4) . . . . ? N4 Ni2 N21 C102 -57.6(4) . . . . ? N6 Ni2 N21 C102 111.5(4) . . . . ? N19 Ni2 N21 C102 -127.6(7) . . . . ? N23 Ni4 N22 C92 171.3(4) . . . . ? N11 Ni4 N22 C92 -18.2(4) . . . . ? N12 Ni4 N22 C92 74.8(4) . . . . ? N10 Ni4 N22 C92 -94.5(4) . . . . ? N24 Ni4 N22 C92 -153.2(6) . . . . ? N23 Ni4 N22 C93 -6.0(3) . . . . ? N11 Ni4 N22 C93 164.5(3) . . . . ? N12 Ni4 N22 C93 -102.5(3) . . . . ? N10 Ni4 N22 C93 88.1(3) . . . . ? N24 Ni4 N22 C93 29.5(8) . . . . ? N11 Ni4 N23 C105 -30.3(9) . . . . ? N12 Ni4 N23 C105 99.7(4) . . . . ? N10 Ni4 N23 C105 -73.0(4) . . . . ? N22 Ni4 N23 C105 13.1(4) . . . . ? N24 Ni4 N23 C105 -158.6(4) . . . . ? N11 Ni4 N23 C106 141.5(6) . . . . ? N12 Ni4 N23 C106 -88.5(4) . . . . ? N10 Ni4 N23 C106 98.9(4) . . . . ? N22 Ni4 N23 C106 -175.1(4) . . . . ? N24 Ni4 N23 C106 13.2(4) . . . . ? N23 Ni4 N24 C112 142.7(4) . . . . ? N11 Ni4 N24 C112 -26.4(4) . . . . ? N12 Ni4 N24 C112 -121.0(4) . . . . ? N10 Ni4 N24 C112 49.5(4) . . . . ? N22 Ni4 N24 C112 108.3(7) . . . . ? N23 Ni4 N24 C108 -12.2(4) . . . . ? N11 Ni4 N24 C108 178.7(4) . . . . ? N12 Ni4 N24 C108 84.1(4) . . . . ? N10 Ni4 N24 C108 -105.4(4) . . . . ? N22 Ni4 N24 C108 -46.6(9) . . . . ? C4 N1 C1 C2 0.4(8) . . . . ? Ni1 N1 C1 C2 -175.7(4) . . . . ? C3 N4 C2 C1 -1.0(8) . . . . ? Ni2 N4 C2 C1 -179.4(4) . . . . ? N1 C1 C2 N4 0.3(8) . . . . ? C2 N4 C3 C4 0.8(7) . . . . ? Ni2 N4 C3 C4 179.3(4) . . . . ? C2 N4 C3 C15 178.8(4) . . . . ? Ni2 N4 C3 C15 -2.6(5) . . . . ? C1 N1 C4 C3 -0.6(7) . . . . ? Ni1 N1 C4 C3 175.9(4) . . . . ? C1 N1 C4 C5 -178.4(4) . . . . ? Ni1 N1 C4 C5 -1.9(5) . . . . ? N4 C3 C4 N1 0.0(8) . . . . ? C15 C3 C4 N1 -177.6(5) . . . . ? N4 C3 C4 C5 177.4(5) . . . . ? C15 C3 C4 C5 -0.2(9) . . . . ? C6 N2 C5 O1 -3.3(10) . . . . ? Ni1 N2 C5 O1 170.3(4) . . . . ? C6 N2 C5 C4 175.3(5) . . . . ? Ni1 N2 C5 C4 -11.2(7) . . . . ? N1 C4 C5 N2 8.2(7) . . . . ? C3 C4 C5 N2 -169.4(6) . . . . ? N1 C4 C5 O1 -173.0(5) . . . . ? C3 C4 C5 O1 9.4(8) . . . . ? C5 N2 C6 C7 -148.9(6) . . . . ? Ni1 N2 C6 C7 37.7(7) . . . . ? N2 C6 C7 C8 -73.1(8) . . . . ? C12 N3 C8 C9 2.5(10) . . . . ? Ni1 N3 C8 C9 -180.0(5) . . . . ? C12 N3 C8 C7 -175.8(6) . . . . ? Ni1 N3 C8 C7 1.7(9) . . . . ? C6 C7 C8 N3 53.0(9) . . . . ? C6 C7 C8 C9 -125.3(7) . . . . ? N3 C8 C9 C10 -1.6(12) . . . . ? C7 C8 C9 C10 176.6(8) . . . . ? C8 C9 C10 C11 -0.1(13) . . . . ? C9 C10 C11 C12 0.9(11) . . . . ? C8 N3 C12 C11 -1.8(11) . . . . ? Ni1 N3 C12 C11 -179.4(6) . . . . ? C10 C11 C12 N3 0.1(11) . . . . ? C16 N5 C15 O2 4.7(9) . . . . ? Ni2 N5 C15 O2 -168.1(4) . . . . ? C16 N5 C15 C3 -174.7(4) . . . . ? Ni2 N5 C15 C3 12.5(7) . . . . ? N4 C3 C15 N5 -6.1(7) . . . . ? C4 C3 C15 N5 171.7(6) . . . . ? N4 C3 C15 O2 174.5(4) . . . . ? C4 C3 C15 O2 -7.8(8) . . . . ? C15 N5 C16 C17 153.6(5) . . . . ? Ni2 N5 C16 C17 -34.1(7) . . . . ? N5 C16 C17 C18 72.3(7) . . . . ? C22 N6 C18 C19 0.6(9) . . . . ? Ni2 N6 C18 C19 -175.1(5) . . . . ? C22 N6 C18 C17 177.7(5) . . . . ? Ni2 N6 C18 C17 2.0(8) . . . . ? C16 C17 C18 N6 -57.0(8) . . . . ? C16 C17 C18 C19 120.1(7) . . . . ? N6 C18 C19 C20 -3.6(10) . . . . ? C17 C18 C19 C20 179.3(7) . . . . ? C18 C19 C20 C21 4.6(12) . . . . ? C19 C20 C21 C22 -2.5(12) . . . . ? C18 N6 C22 C21 1.6(9) . . . . ? Ni2 N6 C22 C21 177.6(5) . . . . ? C20 C21 C22 N6 -0.7(10) . . . . ? C34 N7 C31 C32 1.1(7) . . . . ? Ni3 N7 C31 C32 -179.0(3) . . . . ? C33 N10 C32 C31 -0.6(7) . . . . ? Ni4 N10 C32 C31 -179.4(3) . . . . ? N7 C31 C32 N10 0.3(7) . . . . ? C32 N10 C33 C34 -0.5(7) . . . . ? Ni4 N10 C33 C34 178.4(4) . . . . ? C32 N10 C33 C45 -177.8(4) . . . . ? Ni4 N10 C33 C45 1.1(6) . . . . ? C31 N7 C34 C33 -2.2(7) . . . . ? Ni3 N7 C34 C33 177.9(4) . . . . ? C31 N7 C34 C35 176.5(5) . . . . ? Ni3 N7 C34 C35 -3.4(6) . . . . ? N10 C33 C34 N7 2.0(8) . . . . ? C45 C33 C34 N7 178.8(5) . . . . ? N10 C33 C34 C35 -176.6(5) . . . . ? C45 C33 C34 C35 0.3(10) . . . . ? C36 N8 C35 O3 5.3(11) . . . . ? Ni3 N8 C35 O3 -174.2(6) . . . . ? C36 N8 C35 C34 -170.5(5) . . . . ? Ni3 N8 C35 C34 10.0(8) . . . . ? N7 C34 C35 O3 -179.7(6) . . . . ? C33 C34 C35 O3 -1.1(11) . . . . ? N7 C34 C35 N8 -3.8(8) . . . . ? C33 C34 C35 N8 174.8(6) . . . . ? C35 N8 C36 C37 162.6(6) . . . . ? Ni3 N8 C36 C37 -17.9(8) . . . . ? N8 C36 C37 C38 67.4(8) . . . . ? C42 N9 C38 C39 2.6(8) . . . . ? Ni3 N9 C38 C39 -159.2(4) . . . . ? C42 N9 C38 C37 -178.1(5) . . . . ? Ni3 N9 C38 C37 20.1(7) . . . . ? C36 C37 C38 N9 -71.1(7) . . . . ? C36 C37 C38 C39 108.3(7) . . . . ? N9 C38 C39 C40 -2.1(9) . . . . ? C37 C38 C39 C40 178.6(6) . . . . ? C38 C39 C40 C41 0.9(9) . . . . ? C39 C40 C41 C42 -0.4(9) . . . . ? C38 N9 C42 C41 -2.1(8) . . . . ? Ni3 N9 C42 C41 160.3(5) . . . . ? C40 C41 C42 N9 1.0(9) . . . . ? C46 N11 C45 O4 -5.0(9) . . . . ? Ni4 N11 C45 O4 171.7(4) . . . . ? C46 N11 C45 C33 174.4(5) . . . . ? Ni4 N11 C45 C33 -8.9(7) . . . . ? N10 C33 C45 O4 -175.8(5) . . . . ? C34 C33 C45 O4 7.2(9) . . . . ? N10 C33 C45 N11 4.8(7) . . . . ? C34 C33 C45 N11 -172.3(5) . . . . ? C45 N11 C46 C47 -154.9(5) . . . . ? Ni4 N11 C46 C47 28.5(6) . . . . ? N11 C46 C47 C48 -72.8(6) . . . . ? C52 N12 C48 C49 -0.2(8) . . . . ? Ni4 N12 C48 C49 165.9(4) . . . . ? C52 N12 C48 C47 -178.8(5) . . . . ? Ni4 N12 C48 C47 -12.7(7) . . . . ? C46 C47 C48 N12 65.5(7) . . . . ? C46 C47 C48 C49 -113.1(6) . . . . ? N12 C48 C49 C50 1.4(8) . . . . ? C47 C48 C49 C50 179.9(5) . . . . ? C48 C49 C50 C51 -2.4(9) . . . . ? C49 C50 C51 C52 2.2(9) . . . . ? C48 N12 C52 C51 0.0(8) . . . . ? Ni4 N12 C52 C51 -166.7(4) . . . . ? C50 C51 C52 N12 -1.0(9) . . . . ? C64 N13 C61 C62 0.2(9) . . . . ? Ni1 N13 C61 C62 -178.9(4) . . . . ? C63 N16 C62 C61 -3.0(8) . . . . ? Ni3 N16 C62 C61 174.6(4) . . . . ? N13 C61 C62 N16 1.9(9) . . . . ? C62 N16 C63 C64 2.2(7) . . . . ? Ni3 N16 C63 C64 -175.7(4) . . . . ? C62 N16 C63 C75 176.4(4) . . . . ? Ni3 N16 C63 C75 -1.5(5) . . . . ? C61 N13 C64 C63 -1.0(7) . . . . ? Ni1 N13 C64 C63 178.2(4) . . . . ? C61 N13 C64 C65 -179.4(5) . . . . ? Ni1 N13 C64 C65 -0.2(6) . . . . ? N16 C63 C64 N13 -0.2(7) . . . . ? C75 C63 C64 N13 -173.4(4) . . . . ? N16 C63 C64 C65 178.0(5) . . . . ? C75 C63 C64 C65 4.7(9) . . . . ? C66 N14 C65 O5 -5.1(8) . . . . ? Ni1 N14 C65 O5 165.4(4) . . . . ? C66 N14 C65 C64 173.9(5) . . . . ? Ni1 N14 C65 C64 -15.6(6) . . . . ? N13 C64 C65 O5 -170.9(4) . . . . ? C63 C64 C65 O5 10.8(9) . . . . ? N13 C64 C65 N14 10.0(7) . . . . ? C63 C64 C65 N14 -168.2(5) . . . . ? C65 N14 C66 C67 -161.4(5) . . . . ? Ni1 N14 C66 C67 29.0(6) . . . . ? N14 C66 C67 C68 -69.4(7) . . . . ? C72 N15 C68 C69 -1.6(9) . . . . ? Ni1 N15 C68 C69 168.3(4) . . . . ? C72 N15 C68 C67 -179.8(5) . . . . ? Ni1 N15 C68 C67 -10.0(8) . . . . ? C66 C67 C68 N15 62.0(8) . . . . ? C66 C67 C68 C69 -116.4(6) . . . . ? N15 C68 C69 C70 -0.2(9) . . . . ? C67 C68 C69 C70 178.1(6) . . . . ? C68 C69 C70 C71 1.4(10) . . . . ? C69 C70 C71 C72 -0.7(10) . . . . ? C70 C71 C72 N15 -1.2(11) . . . . ? C68 N15 C72 C71 2.4(10) . . . . ? Ni1 N15 C72 C71 -167.6(5) . . . . ? C76 N17 C75 O6 10.7(7) . . . . ? Ni3 N17 C75 O6 -165.1(4) . . . . ? C76 N17 C75 C63 -169.1(4) . . . . ? Ni3 N17 C75 C63 15.2(6) . . . . ? N16 C63 C75 O6 171.7(4) . . . . ? C64 C63 C75 O6 -14.6(8) . . . . ? N16 C63 C75 N17 -8.5(6) . . . . ? C64 C63 C75 N17 165.2(5) . . . . ? C75 N17 C76 C77 164.6(4) . . . . ? Ni3 N17 C76 C77 -20.0(6) . . . . ? N17 C76 C77 C78 69.0(6) . . . . ? C82 N18 C78 C79 2.9(8) . . . . ? Ni3 N18 C78 C79 -153.8(4) . . . . ? C82 N18 C78 C77 -179.1(5) . . . . ? Ni3 N18 C78 C77 24.2(6) . . . . ? C76 C77 C78 N18 -74.4(6) . . . . ? C76 C77 C78 C79 103.6(6) . . . . ? N18 C78 C79 C80 0.1(10) . . . . ? C77 C78 C79 C80 -177.8(6) . . . . ? C78 C79 C80 C81 -1.8(11) . . . . ? C79 C80 C81 C82 0.5(11) . . . . ? C78 N18 C82 C81 -4.2(8) . . . . ? Ni3 N18 C82 C81 153.4(5) . . . . ? C80 C81 C82 N18 2.6(10) . . . . ? C94 N19 C91 C92 -1.8(8) . . . . ? Ni2 N19 C91 C92 -179.9(4) . . . . ? C93 N22 C92 C91 4.4(8) . . . . ? Ni4 N22 C92 C91 -172.8(4) . . . . ? N19 C91 C92 N22 -2.0(8) . . . . ? C92 N22 C93 C94 -3.0(7) . . . . ? Ni4 N22 C93 C94 174.6(4) . . . . ? C92 N22 C93 C105 -178.2(4) . . . . ? Ni4 N22 C93 C105 -0.6(5) . . . . ? C91 N19 C94 C93 3.1(7) . . . . ? Ni2 N19 C94 C93 -178.6(3) . . . . ? C91 N19 C94 C95 -179.5(4) . . . . ? Ni2 N19 C94 C95 -1.2(5) . . . . ? N22 C93 C94 N19 -0.7(7) . . . . ? C105 C93 C94 N19 173.6(4) . . . . ? N22 C93 C94 C95 -177.5(5) . . . . ? C105 C93 C94 C95 -3.2(9) . . . . ? C96 N20 C95 O7 7.4(7) . . . . ? Ni2 N20 C95 O7 -163.0(4) . . . . ? C96 N20 C95 C94 -173.6(4) . . . . ? Ni2 N20 C95 C94 16.0(6) . . . . ? N19 C94 C95 N20 -9.2(7) . . . . ? C93 C94 C95 N20 167.8(5) . . . . ? N19 C94 C95 O7 169.9(4) . . . . ? C93 C94 C95 O7 -13.1(8) . . . . ? C95 N20 C96 C97 159.4(5) . . . . ? Ni2 N20 C96 C97 -30.8(6) . . . . ? N20 C96 C97 C98 71.1(6) . . . . ? C102 N21 C98 C99 -3.5(8) . . . . ? Ni2 N21 C98 C99 -172.0(4) . . . . ? C102 N21 C98 C97 179.3(5) . . . . ? Ni2 N21 C98 C97 10.8(7) . . . . ? C96 C97 C98 N21 -62.2(7) . . . . ? C96 C97 C98 C99 120.5(6) . . . . ? N21 C98 C99 C100 2.3(9) . . . . ? C97 C98 C99 C100 179.4(6) . . . . ? C98 C99 C100 C101 0.3(10) . . . . ? C99 C100 C101 C102 -1.6(10) . . . . ? C98 N21 C102 C101 2.2(8) . . . . ? Ni2 N21 C102 C101 171.5(5) . . . . ? C100 C101 C102 N21 0.4(10) . . . . ? C106 N23 C105 O8 -6.9(7) . . . . ? Ni4 N23 C105 O8 165.8(3) . . . . ? C106 N23 C105 C93 169.7(4) . . . . ? Ni4 N23 C105 C93 -17.6(6) . . . . ? N22 C93 C105 O8 -171.9(4) . . . . ? C94 C93 C105 O8 13.4(8) . . . . ? N22 C93 C105 N23 11.5(6) . . . . ? C94 C93 C105 N23 -163.3(5) . . . . ? C105 N23 C106 C107 -166.7(4) . . . . ? Ni4 N23 C106 C107 21.3(6) . . . . ? N23 C106 C107 C108 -68.1(6) . . . . ? C112 N24 C108 C109 -3.3(8) . . . . ? Ni4 N24 C108 C109 151.4(4) . . . . ? C112 N24 C108 C107 -179.8(5) . . . . ? Ni4 N24 C108 C107 -25.1(7) . . . . ? C106 C107 C108 N24 73.7(6) . . . . ? C106 C107 C108 C109 -102.8(6) . . . . ? N24 C108 C109 C110 0.9(9) . . . . ? C107 C108 C109 C110 177.3(6) . . . . ? C108 C109 C110 C111 1.6(10) . . . . ? C109 C110 C111 C112 -1.6(11) . . . . ? C108 N24 C112 C111 3.4(8) . . . . ? Ni4 N24 C112 C111 -151.7(5) . . . . ? C110 C111 C112 N24 -0.9(10) . . . . ? N26 Ni5 N25 C121 176.7(4) . . . . ? N38 Ni5 N25 C121 -12.8(4) . . . . ? N27 Ni5 N25 C121 -163.8(8) . . . . ? N39 Ni5 N25 C121 79.5(4) . . . . ? N37 Ni5 N25 C121 -89.4(4) . . . . ? N26 Ni5 N25 C124 -5.5(4) . . . . ? N38 Ni5 N25 C124 165.0(4) . . . . ? N27 Ni5 N25 C124 14.0(10) . . . . ? N39 Ni5 N25 C124 -102.8(4) . . . . ? N37 Ni5 N25 C124 88.4(4) . . . . ? N38 Ni5 N26 C125 -36.7(12) . . . . ? N27 Ni5 N26 C125 -168.5(5) . . . . ? N39 Ni5 N26 C125 96.4(5) . . . . ? N25 Ni5 N26 C125 7.2(5) . . . . ? N37 Ni5 N26 C125 -80.0(5) . . . . ? N38 Ni5 N26 C126 136.9(8) . . . . ? N27 Ni5 N26 C126 5.0(5) . . . . ? N39 Ni5 N26 C126 -90.1(5) . . . . ? N25 Ni5 N26 C126 -179.2(5) . . . . ? N37 Ni5 N26 C126 93.5(5) . . . . ? N44 Ni6 N28 C122 9.7(4) . . . . ? N29 Ni6 N28 C122 -177.8(4) . . . . ? N45 Ni6 N28 C122 -82.1(4) . . . . ? N30 Ni6 N28 C122 154.8(12) . . . . ? N43 Ni6 N28 C122 86.1(4) . . . . ? N44 Ni6 N28 C123 -165.8(4) . . . . ? N29 Ni6 N28 C123 6.7(3) . . . . ? N45 Ni6 N28 C123 102.4(4) . . . . ? N30 Ni6 N28 C123 -20.6(14) . . . . ? N43 Ni6 N28 C123 -89.4(4) . . . . ? N44 Ni6 N29 C135 33.0(13) . . . . ? N45 Ni6 N29 C135 -97.1(5) . . . . ? N28 Ni6 N29 C135 -6.4(5) . . . . ? N30 Ni6 N29 C135 167.6(5) . . . . ? N43 Ni6 N29 C135 79.9(5) . . . . ? N44 Ni6 N29 C136 -143.7(10) . . . . ? N45 Ni6 N29 C136 86.1(5) . . . . ? N28 Ni6 N29 C136 176.9(5) . . . . ? N30 Ni6 N29 C136 -9.1(5) . . . . ? N43 Ni6 N29 C136 -96.8(5) . . . . ? N32 Ni7 N31 C151 -175.6(4) . . . . ? N41 Ni7 N31 C151 12.6(4) . . . . ? N33 Ni7 N31 C151 152.6(7) . . . . ? N42 Ni7 N31 C151 -79.2(4) . . . . ? N40 Ni7 N31 C151 87.8(4) . . . . ? N32 Ni7 N31 C154 8.3(3) . . . . ? N41 Ni7 N31 C154 -163.5(3) . . . . ? N33 Ni7 N31 C154 -23.6(9) . . . . ? N42 Ni7 N31 C154 104.7(3) . . . . ? N40 Ni7 N31 C154 -88.3(3) . . . . ? N41 Ni7 N32 C155 30.6(11) . . . . ? N33 Ni7 N32 C155 161.8(4) . . . . ? N42 Ni7 N32 C155 -99.0(4) . . . . ? N31 Ni7 N32 C155 -10.9(4) . . . . ? N40 Ni7 N32 C155 73.1(4) . . . . ? N41 Ni7 N32 C156 -145.4(7) . . . . ? N33 Ni7 N32 C156 -14.2(4) . . . . ? N42 Ni7 N32 C156 85.0(4) . . . . ? N31 Ni7 N32 C156 173.1(4) . . . . ? N40 Ni7 N32 C156 -102.9(4) . . . . ? N32 Ni7 N33 C162 -146.9(4) . . . . ? N41 Ni7 N33 C162 23.7(4) . . . . ? N42 Ni7 N33 C162 116.6(4) . . . . ? N31 Ni7 N33 C162 -116.0(8) . . . . ? N40 Ni7 N33 C162 -51.7(4) . . . . ? N32 Ni7 N33 C158 22.8(4) . . . . ? N41 Ni7 N33 C158 -166.5(4) . . . . ? N42 Ni7 N33 C158 -73.6(4) . . . . ? N31 Ni7 N33 C158 53.7(9) . . . . ? N40 Ni7 N33 C158 118.1(4) . . . . ? N35 Ni8 N34 C152 173.0(4) . . . . ? N47 Ni8 N34 C152 -16.8(4) . . . . ? N48 Ni8 N34 C152 75.2(4) . . . . ? N36 Ni8 N34 C152 -168.8(7) . . . . ? N46 Ni8 N34 C152 -92.3(4) . . . . ? N35 Ni8 N34 C153 -5.0(3) . . . . ? N47 Ni8 N34 C153 165.2(4) . . . . ? N48 Ni8 N34 C153 -102.8(4) . . . . ? N36 Ni8 N34 C153 13.2(10) . . . . ? N46 Ni8 N34 C153 89.7(3) . . . . ? N47 Ni8 N35 C165 -37.5(11) . . . . ? N34 Ni8 N35 C165 9.9(4) . . . . ? N48 Ni8 N35 C165 96.3(4) . . . . ? N36 Ni8 N35 C165 -166.3(4) . . . . ? N46 Ni8 N35 C165 -75.6(4) . . . . ? N47 Ni8 N35 C166 138.0(8) . . . . ? N34 Ni8 N35 C166 -174.6(4) . . . . ? N48 Ni8 N35 C166 -88.2(4) . . . . ? N36 Ni8 N35 C166 9.3(4) . . . . ? N46 Ni8 N35 C166 100.0(4) . . . . ? N35 Ni8 N36 C172 150.0(4) . . . . ? N47 Ni8 N36 C172 -19.6(4) . . . . ? N34 Ni8 N36 C172 132.3(8) . . . . ? N48 Ni8 N36 C172 -112.7(4) . . . . ? N46 Ni8 N36 C172 56.2(4) . . . . ? N35 Ni8 N36 C168 -23.5(4) . . . . ? N47 Ni8 N36 C168 166.9(4) . . . . ? N34 Ni8 N36 C168 -41.2(10) . . . . ? N48 Ni8 N36 C168 73.8(4) . . . . ? N46 Ni8 N36 C168 -117.3(4) . . . . ? N26 Ni5 N37 C181 -15.6(5) . . . . ? N38 Ni5 N37 C181 174.0(5) . . . . ? N27 Ni5 N37 C181 75.9(5) . . . . ? N39 Ni5 N37 C181 -176.7(10) . . . . ? N25 Ni5 N37 C181 -91.7(4) . . . . ? N26 Ni5 N37 C184 170.1(4) . . . . ? N38 Ni5 N37 C184 -0.3(4) . . . . ? N27 Ni5 N37 C184 -98.4(4) . . . . ? N39 Ni5 N37 C184 9.0(13) . . . . ? N25 Ni5 N37 C184 94.0(4) . . . . ? N26 Ni5 N38 C185 -35.7(11) . . . . ? N27 Ni5 N38 C185 95.6(5) . . . . ? N39 Ni5 N38 C185 -169.2(5) . . . . ? N25 Ni5 N38 C185 -78.2(4) . . . . ? N37 Ni5 N38 C185 9.0(4) . . . . ? N26 Ni5 N38 C186 138.7(8) . . . . ? N27 Ni5 N38 C186 -90.0(5) . . . . ? N39 Ni5 N38 C186 5.2(5) . . . . ? N25 Ni5 N38 C186 96.2(5) . . . . ? N37 Ni5 N38 C186 -176.6(5) . . . . ? N32 Ni7 N40 C182 16.4(4) . . . . ? N41 Ni7 N40 C182 -172.3(4) . . . . ? N33 Ni7 N40 C182 -75.1(4) . . . . ? N42 Ni7 N40 C182 161.7(7) . . . . ? N31 Ni7 N40 C182 92.4(4) . . . . ? N32 Ni7 N40 C183 -165.9(4) . . . . ? N41 Ni7 N40 C183 5.5(4) . . . . ? N33 Ni7 N40 C183 102.7(4) . . . . ? N42 Ni7 N40 C183 -20.6(9) . . . . ? N31 Ni7 N40 C183 -89.9(4) . . . . ? N32 Ni7 N41 C195 33.6(11) . . . . ? N33 Ni7 N41 C195 -97.2(4) . . . . ? N42 Ni7 N41 C195 163.5(4) . . . . ? N31 Ni7 N41 C195 73.9(4) . . . . ? N40 Ni7 N41 C195 -10.4(4) . . . . ? N32 Ni7 N41 C196 -140.0(8) . . . . ? N33 Ni7 N41 C196 89.1(4) . . . . ? N42 Ni7 N41 C196 -10.1(4) . . . . ? N31 Ni7 N41 C196 -99.8(4) . . . . ? N40 Ni7 N41 C196 175.9(4) . . . . ? N32 Ni7 N42 C202 21.7(4) . . . . ? N41 Ni7 N42 C202 -148.7(4) . . . . ? N33 Ni7 N42 C202 114.3(4) . . . . ? N31 Ni7 N42 C202 -54.7(4) . . . . ? N40 Ni7 N42 C202 -123.5(7) . . . . ? N32 Ni7 N42 C198 -165.8(4) . . . . ? N41 Ni7 N42 C198 23.8(4) . . . . ? N33 Ni7 N42 C198 -73.2(4) . . . . ? N31 Ni7 N42 C198 117.8(4) . . . . ? N40 Ni7 N42 C198 49.0(9) . . . . ? N44 Ni6 N43 C211 -173.3(5) . . . . ? N29 Ni6 N43 C211 15.5(5) . . . . ? N45 Ni6 N43 C211 -179(60) . . . . ? N28 Ni6 N43 C211 92.2(5) . . . . ? N30 Ni6 N43 C211 -75.4(5) . . . . ? N44 Ni6 N43 C214 2.8(4) . . . . ? N29 Ni6 N43 C214 -168.4(4) . . . . ? N45 Ni6 N43 C214 -2.7(13) . . . . ? N28 Ni6 N43 C214 -91.7(4) . . . . ? N30 Ni6 N43 C214 100.7(4) . . . . ? N29 Ni6 N44 C215 40.2(13) . . . . ? N45 Ni6 N44 C215 170.7(5) . . . . ? N28 Ni6 N44 C215 78.4(5) . . . . ? N30 Ni6 N44 C215 -93.9(5) . . . . ? N43 Ni6 N44 C215 -8.2(5) . . . . ? N29 Ni6 N44 C216 -136.6(10) . . . . ? N45 Ni6 N44 C216 -6.1(5) . . . . ? N28 Ni6 N44 C216 -98.4(5) . . . . ? N30 Ni6 N44 C216 89.2(5) . . . . ? N43 Ni6 N44 C216 175.0(5) . . . . ? N35 Ni8 N46 C212 -12.6(5) . . . . ? N47 Ni8 N46 C212 175.8(5) . . . . ? N34 Ni8 N46 C212 -89.3(4) . . . . ? N48 Ni8 N46 C212 -156.0(6) . . . . ? N36 Ni8 N46 C212 78.6(4) . . . . ? N35 Ni8 N46 C213 168.6(4) . . . . ? N47 Ni8 N46 C213 -3.0(4) . . . . ? N34 Ni8 N46 C213 91.9(4) . . . . ? N48 Ni8 N46 C213 25.2(9) . . . . ? N36 Ni8 N46 C213 -100.2(4) . . . . ? N35 Ni8 N47 C225 -31.4(11) . . . . ? N34 Ni8 N47 C225 -77.3(5) . . . . ? N48 Ni8 N47 C225 -165.6(4) . . . . ? N36 Ni8 N47 C225 96.8(4) . . . . ? N46 Ni8 N47 C225 8.0(4) . . . . ? N35 Ni8 N47 C226 143.1(8) . . . . ? N34 Ni8 N47 C226 97.2(4) . . . . ? N48 Ni8 N47 C226 8.9(4) . . . . ? N36 Ni8 N47 C226 -88.7(4) . . . . ? N46 Ni8 N47 C226 -177.5(4) . . . . ? N35 Ni8 N48 C232 -20.8(4) . . . . ? N47 Ni8 N48 C232 149.6(4) . . . . ? N34 Ni8 N48 C232 55.8(4) . . . . ? N36 Ni8 N48 C232 -113.0(4) . . . . ? N46 Ni8 N48 C232 122.3(7) . . . . ? N35 Ni8 N48 C228 168.4(4) . . . . ? N47 Ni8 N48 C228 -21.2(4) . . . . ? N34 Ni8 N48 C228 -115.0(4) . . . . ? N36 Ni8 N48 C228 76.3(4) . . . . ? N46 Ni8 N48 C228 -48.5(9) . . . . ? C124 N25 C121 C122 -0.9(8) . . . . ? Ni5 N25 C121 C122 176.8(4) . . . . ? C123 N28 C122 C121 0.4(8) . . . . ? Ni6 N28 C122 C121 -174.9(4) . . . . ? N25 C121 C122 N28 0.5(9) . . . . ? C122 N28 C123 C124 -0.9(7) . . . . ? Ni6 N28 C123 C124 175.1(4) . . . . ? C122 N28 C123 C135 177.8(4) . . . . ? Ni6 N28 C123 C135 -6.2(5) . . . . ? C121 N25 C124 C123 0.5(8) . . . . ? Ni5 N25 C124 C123 -177.4(4) . . . . ? C121 N25 C124 C125 -178.9(5) . . . . ? Ni5 N25 C124 C125 3.2(5) . . . . ? N28 C123 C124 N25 0.5(8) . . . . ? C135 C123 C124 N25 -178.0(5) . . . . ? N28 C123 C124 C125 179.7(5) . . . . ? C135 C123 C124 C125 1.2(10) . . . . ? C126 N26 C125 O9 -4.2(9) . . . . ? Ni5 N26 C125 O9 169.8(4) . . . . ? C126 N26 C125 C124 178.0(5) . . . . ? Ni5 N26 C125 C124 -8.0(8) . . . . ? N25 C124 C125 N26 2.8(8) . . . . ? C123 C124 C125 N26 -176.5(6) . . . . ? N25 C124 C125 O9 -175.1(5) . . . . ? C123 C124 C125 O9 5.6(9) . . . . ? C125 N26 C126 C127 -150.0(6) . . . . ? Ni5 N26 C126 C127 36.4(7) . . . . ? N26 C126 C127 C128 -73.9(8) . . . . ? N26 Ni5 N27 C132 150.9(6) . . . . ? N38 Ni5 N27 C132 -18.9(6) . . . . ? N39 Ni5 N27 C132 -111.7(6) . . . . ? N25 Ni5 N27 C132 131.9(9) . . . . ? N37 Ni5 N27 C132 57.6(5) . . . . ? N26 Ni5 N27 C128 -23.2(6) . . . . ? N38 Ni5 N27 C128 167.1(6) . . . . ? N39 Ni5 N27 C128 74.3(6) . . . . ? N25 Ni5 N27 C128 -42.1(12) . . . . ? N37 Ni5 N27 C128 -116.4(6) . . . . ? C132 N27 C128 C129 1.7(12) . . . . ? Ni5 N27 C128 C129 175.9(8) . . . . ? C132 N27 C128 C127 -177.6(6) . . . . ? Ni5 N27 C128 C127 -3.3(9) . . . . ? C126 C127 C128 N27 56.3(9) . . . . ? C126 C127 C128 C129 -122.9(9) . . . . ? N27 C128 C129 C130 -2.4(18) . . . . ? C127 C128 C129 C130 176.7(11) . . . . ? C128 C129 C130 C131 2(2) . . . . ? C129 C130 C131 C132 -1.1(19) . . . . ? C128 N27 C132 C131 -0.6(12) . . . . ? Ni5 N27 C132 C131 -175.2(7) . . . . ? C130 C131 C132 N27 0.4(16) . . . . ? C136 N29 C135 O10 0.8(9) . . . . ? Ni6 N29 C135 O10 -176.1(4) . . . . ? C136 N29 C135 C123 -178.1(5) . . . . ? Ni6 N29 C135 C123 4.9(7) . . . . ? N28 C123 C135 N29 1.2(7) . . . . ? C124 C123 C135 N29 179.7(6) . . . . ? N28 C123 C135 O10 -177.9(5) . . . . ? C124 C123 C135 O10 0.7(9) . . . . ? C135 N29 C136 C137 155.8(8) . . . . ? Ni6 N29 C136 C137 -27.5(9) . . . . ? N29 C136 C137 C138 69.6(11) . . . . ? N44 Ni6 N30 C138 -169.8(7) . . . . ? N29 Ni6 N30 C138 18.6(8) . . . . ? N45 Ni6 N30 C138 -77.5(8) . . . . ? N28 Ni6 N30 C138 45.3(17) . . . . ? N43 Ni6 N30 C138 114.0(8) . . . . ? N44 Ni6 N30 C142 28.2(8) . . . . ? N29 Ni6 N30 C142 -143.4(8) . . . . ? N45 Ni6 N30 C142 120.5(8) . . . . ? N28 Ni6 N30 C142 -116.7(12) . . . . ? N43 Ni6 N30 C142 -48.0(8) . . . . ? C142 N30 C138 C139 -3.7(16) . . . . ? Ni6 N30 C138 C139 -166.0(10) . . . . ? C142 N30 C138 C137 175.3(10) . . . . ? Ni6 N30 C138 C137 13.0(13) . . . . ? C136 C137 C138 N30 -62.7(13) . . . . ? C136 C137 C138 C139 116.3(12) . . . . ? N30 C138 C139 C140 2(3) . . . . ? C137 C138 C139 C140 -177.2(18) . . . . ? C138 C139 C140 C141 2(3) . . . . ? C139 C140 C141 C142 -3(3) . . . . ? C138 N30 C142 C141 2.4(18) . . . . ? Ni6 N30 C142 C141 165.7(11) . . . . ? C140 C141 C142 N30 1(2) . . . . ? C154 N31 C151 C152 -1.2(7) . . . . ? Ni7 N31 C151 C152 -177.3(4) . . . . ? C153 N34 C152 C151 0.3(7) . . . . ? Ni8 N34 C152 C151 -177.6(4) . . . . ? N31 C151 C152 N34 0.4(8) . . . . ? C152 N34 C153 C154 -0.1(7) . . . . ? Ni8 N34 C153 C154 178.0(4) . . . . ? C152 N34 C153 C165 -177.7(4) . . . . ? Ni8 N34 C153 C165 0.4(5) . . . . ? C151 N31 C154 C153 1.4(7) . . . . ? Ni7 N31 C154 C153 177.8(3) . . . . ? C151 N31 C154 C155 178.7(4) . . . . ? Ni7 N31 C154 C155 -4.9(5) . . . . ? N34 C153 C154 N31 -0.7(7) . . . . ? C165 C153 C154 N31 176.4(4) . . . . ? N34 C153 C154 C155 -177.4(4) . . . . ? C165 C153 C154 C155 -0.2(9) . . . . ? C156 N32 C155 O11 6.1(8) . . . . ? Ni7 N32 C155 O11 -170.2(4) . . . . ? C156 N32 C155 C154 -172.0(4) . . . . ? Ni7 N32 C155 C154 11.7(6) . . . . ? N31 C154 C155 O11 177.9(4) . . . . ? C153 C154 C155 O11 -5.2(8) . . . . ? N31 C154 C155 N32 -4.0(6) . . . . ? C153 C154 C155 N32 172.9(5) . . . . ? C155 N32 C156 C157 158.7(5) . . . . ? Ni7 N32 C156 C157 -25.2(6) . . . . ? N32 C156 C157 C158 69.0(6) . . . . ? C162 N33 C158 C159 -1.1(8) . . . . ? Ni7 N33 C158 C159 -171.1(4) . . . . ? C162 N33 C158 C157 179.8(5) . . . . ? Ni7 N33 C158 C157 9.8(7) . . . . ? C156 C157 C158 N33 -63.2(7) . . . . ? C156 C157 C158 C159 117.8(6) . . . . ? N33 C158 C159 C160 0.7(11) . . . . ? C157 C158 C159 C160 179.8(7) . . . . ? C158 C159 C160 C161 0.4(13) . . . . ? C159 C160 C161 C162 -1.2(12) . . . . ? C158 N33 C162 C161 0.4(9) . . . . ? Ni7 N33 C162 C161 170.5(5) . . . . ? C160 C161 C162 N33 0.8(10) . . . . ? C166 N35 C165 O12 -8.1(8) . . . . ? Ni8 N35 C165 O12 167.7(4) . . . . ? C166 N35 C165 C153 171.5(4) . . . . ? Ni8 N35 C165 C153 -12.6(6) . . . . ? N34 C153 C165 O12 -172.7(4) . . . . ? C154 C153 C165 O12 9.9(8) . . . . ? N34 C153 C165 N35 7.6(7) . . . . ? C154 C153 C165 N35 -169.7(5) . . . . ? C165 N35 C166 C167 -152.9(5) . . . . ? Ni8 N35 C166 C167 31.5(7) . . . . ? N35 C166 C167 C168 -73.0(7) . . . . ? C172 N36 C168 C169 0.7(7) . . . . ? Ni8 N36 C168 C169 174.2(4) . . . . ? C172 N36 C168 C167 -179.9(5) . . . . ? Ni8 N36 C168 C167 -6.5(6) . . . . ? C166 C167 C168 N36 60.6(7) . . . . ? C166 C167 C168 C169 -120.1(6) . . . . ? N36 C168 C169 C170 -0.8(9) . . . . ? C167 C168 C169 C170 179.8(6) . . . . ? C168 C169 C170 C171 0.9(10) . . . . ? C169 C170 C171 C172 -0.8(9) . . . . ? C168 N36 C172 C171 -0.7(8) . . . . ? Ni8 N36 C172 C171 -174.4(4) . . . . ? C170 C171 C172 N36 0.8(9) . . . . ? C184 N37 C181 C182 3.0(8) . . . . ? Ni5 N37 C181 C182 -171.0(4) . . . . ? C183 N40 C182 C181 -0.5(8) . . . . ? Ni7 N40 C182 C181 177.1(4) . . . . ? N37 C181 C182 N40 -2.4(8) . . . . ? C182 N40 C183 C184 2.7(8) . . . . ? Ni7 N40 C183 C184 -175.1(4) . . . . ? C182 N40 C183 C195 177.0(4) . . . . ? Ni7 N40 C183 C195 -0.8(5) . . . . ? C181 N37 C184 C183 -0.7(8) . . . . ? Ni5 N37 C184 C183 173.8(4) . . . . ? C181 N37 C184 C185 178.7(5) . . . . ? Ni5 N37 C184 C185 -6.8(6) . . . . ? N40 C183 C184 N37 -2.1(8) . . . . ? C195 C183 C184 N37 -175.3(5) . . . . ? N40 C183 C184 C185 178.6(5) . . . . ? C195 C183 C184 C185 5.4(9) . . . . ? C186 N38 C185 O13 -5.9(9) . . . . ? Ni5 N38 C185 O13 168.9(4) . . . . ? C186 N38 C185 C184 170.0(5) . . . . ? Ni5 N38 C185 C184 -15.3(7) . . . . ? N37 C184 C185 O13 -169.9(5) . . . . ? C183 C184 C185 O13 9.5(9) . . . . ? N37 C184 C185 N38 14.2(7) . . . . ? C183 C184 C185 N38 -166.5(5) . . . . ? C185 N38 C186 C187 -150.3(6) . . . . ? Ni5 N38 C186 C187 35.2(7) . . . . ? N38 C186 C187 C188 -71.3(8) . . . . ? N26 Ni5 N39 C188 164.4(6) . . . . ? N38 Ni5 N39 C188 -25.6(6) . . . . ? N27 Ni5 N39 C188 72.1(7) . . . . ? N25 Ni5 N39 C188 -119.4(6) . . . . ? N37 Ni5 N39 C188 -34.7(15) . . . . ? N26 Ni5 N39 C192 -15.8(6) . . . . ? N38 Ni5 N39 C192 154.2(6) . . . . ? N27 Ni5 N39 C192 -108.1(6) . . . . ? N25 Ni5 N39 C192 60.4(6) . . . . ? N37 Ni5 N39 C192 145.1(10) . . . . ? C192 N39 C188 C189 -0.1(13) . . . . ? Ni5 N39 C188 C189 179.7(7) . . . . ? C192 N39 C188 C187 -179.7(8) . . . . ? Ni5 N39 C188 C187 0.1(11) . . . . ? C186 C187 C188 N39 53.2(11) . . . . ? C186 C187 C188 C189 -126.4(8) . . . . ? N39 C188 C189 C190 1.9(16) . . . . ? C187 C188 C189 C190 -178.5(10) . . . . ? C188 C189 C190 C191 -3.8(19) . . . . ? C189 C190 C191 C192 3.6(18) . . . . ? C188 N39 C192 C191 0.0(14) . . . . ? Ni5 N39 C192 C191 -179.8(8) . . . . ? C190 C191 C192 N39 -1.6(16) . . . . ? C196 N41 C195 O14 5.3(8) . . . . ? Ni7 N41 C195 O14 -168.8(4) . . . . ? C196 N41 C195 C183 -172.3(4) . . . . ? Ni7 N41 C195 C183 13.5(6) . . . . ? N40 C183 C195 N41 -7.9(7) . . . . ? C184 C183 C195 N41 165.6(5) . . . . ? N40 C183 C195 O14 174.3(4) . . . . ? C184 C183 C195 O14 -12.1(8) . . . . ? C195 N41 C196 C197 156.7(5) . . . . ? Ni7 N41 C196 C197 -29.4(6) . . . . ? N41 C196 C197 C198 72.1(5) . . . . ? C202 N42 C198 C199 2.1(7) . . . . ? Ni7 N42 C198 C199 -170.5(4) . . . . ? C202 N42 C198 C197 178.5(5) . . . . ? Ni7 N42 C198 C197 5.9(6) . . . . ? C196 C197 C198 N42 -61.0(6) . . . . ? C196 C197 C198 C199 115.3(5) . . . . ? N42 C198 C199 C200 -1.7(8) . . . . ? C197 C198 C199 C200 -178.0(5) . . . . ? C198 C199 C200 C201 0.0(8) . . . . ? C199 C200 C201 C202 1.2(8) . . . . ? C198 N42 C202 C201 -0.9(8) . . . . ? Ni7 N42 C202 C201 171.9(4) . . . . ? C200 C201 C202 N42 -0.8(9) . . . . ? C214 N43 C211 C212 -2.5(8) . . . . ? Ni6 N43 C211 C212 173.4(4) . . . . ? C213 N46 C212 C211 1.8(8) . . . . ? Ni8 N46 C212 C211 -177.0(4) . . . . ? N43 C211 C212 N46 1.1(8) . . . . ? C212 N46 C213 C214 -3.1(8) . . . . ? Ni8 N46 C213 C214 175.7(4) . . . . ? C212 N46 C213 C225 179.9(5) . . . . ? Ni8 N46 C213 C225 -1.2(6) . . . . ? C211 N43 C214 C213 1.2(8) . . . . ? Ni6 N43 C214 C213 -175.2(4) . . . . ? C211 N43 C214 C215 178.3(5) . . . . ? Ni6 N43 C214 C215 2.0(6) . . . . ? N46 C213 C214 N43 1.7(8) . . . . ? C225 C213 C214 N43 178.2(5) . . . . ? N46 C213 C214 C215 -174.8(5) . . . . ? C225 C213 C214 C215 1.7(10) . . . . ? C216 N44 C215 O15 7.6(9) . . . . ? Ni6 N44 C215 O15 -169.5(4) . . . . ? C216 N44 C215 C214 -171.0(5) . . . . ? Ni6 N44 C215 C214 11.9(7) . . . . ? N43 C214 C215 N44 -8.8(8) . . . . ? C213 C214 C215 N44 167.9(6) . . . . ? N43 C214 C215 O15 172.6(5) . . . . ? C213 C214 C215 O15 -10.7(9) . . . . ? C215 N44 C216 C217 146.8(6) . . . . ? Ni6 N44 C216 C217 -36.3(8) . . . . ? N44 C216 C217 C218 75.6(7) . . . . ? N44 Ni6 N45 C222 -162.8(7) . . . . ? N29 Ni6 N45 C222 8.2(7) . . . . ? N28 Ni6 N45 C222 -69.0(7) . . . . ? N30 Ni6 N45 C222 99.8(7) . . . . ? N43 Ni6 N45 C222 -157.5(9) . . . . ? N44 Ni6 N45 C218 24.7(7) . . . . ? N29 Ni6 N45 C218 -164.3(7) . . . . ? N28 Ni6 N45 C218 118.5(7) . . . . ? N30 Ni6 N45 C218 -72.7(7) . . . . ? N43 Ni6 N45 C218 30.0(16) . . . . ? C222 N45 C218 C219 1.4(15) . . . . ? Ni6 N45 C218 C219 174.3(8) . . . . ? C222 N45 C218 C217 -168.6(8) . . . . ? Ni6 N45 C218 C217 4.4(11) . . . . ? C216 C217 C218 N45 -60.2(10) . . . . ? C216 C217 C218 C219 129.0(9) . . . . ? N45 C218 C219 C220 -2.7(19) . . . . ? C217 C218 C219 C220 167.3(11) . . . . ? C218 C219 C220 C221 6(2) . . . . ? C219 C220 C221 C222 -7.2(19) . . . . ? C218 N45 C222 C221 -3.4(15) . . . . ? Ni6 N45 C222 C221 -176.6(9) . . . . ? C220 C221 C222 N45 6.4(18) . . . . ? C226 N47 C225 O16 -5.0(8) . . . . ? Ni8 N47 C225 O16 169.8(4) . . . . ? C226 N47 C225 C213 174.1(4) . . . . ? Ni8 N47 C225 C213 -11.1(7) . . . . ? N46 C213 C225 N47 7.7(7) . . . . ? C214 C213 C225 N47 -169.1(6) . . . . ? N46 C213 C225 O16 -173.2(5) . . . . ? C214 C213 C225 O16 10.1(9) . . . . ? C225 N47 C226 C227 -154.4(5) . . . . ? Ni8 N47 C226 C227 30.9(6) . . . . ? N47 C226 C227 C228 -72.6(5) . . . . ? C232 N48 C228 C229 -1.3(7) . . . . ? Ni8 N48 C228 C229 169.5(4) . . . . ? C232 N48 C228 C227 179.5(5) . . . . ? Ni8 N48 C228 C227 -9.7(6) . . . . ? C226 C227 C228 N48 62.7(6) . . . . ? C226 C227 C228 C229 -116.5(5) . . . . ? N48 C228 C229 C230 1.9(8) . . . . ? C227 C228 C229 C230 -178.9(5) . . . . ? C228 C229 C230 C231 -2.6(9) . . . . ? C229 C230 C231 C232 2.5(9) . . . . ? C228 N48 C232 C231 1.4(8) . . . . ? Ni8 N48 C232 C231 -169.8(4) . . . . ? C230 C231 C232 N48 -2.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.485 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.065