# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'D Dolphin' _publ_contact_author_email DAVID.DOLPHIN@UBC.CA _publ_section_title ; Self-Assembly of Oligomeric Linear Dipyrromethene Metal Complexes ; loop_ _publ_author_name 'D Dolphin' 'Qing Miao.' 'Brian O Patrick' 'Ji-Young Shin.' # Attachment 'CIFs.txt' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 684023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 B F2 N4' _chemical_formula_weight 438.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 6.2217(8) _cell_length_b 30.104(4) _cell_length_c 11.954(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.072(9) _cell_angle_gamma 90.00 _cell_volume 2226.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2082 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 23.89 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11838 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.23 _reflns_number_total 2611 _reflns_number_gt 1568 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.1923P] 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 2611 _refine_ls_number_parameters 175 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9175(2) 0.28954(5) 0.39302(14) 0.0553(4) Uani 1 1 d . . . H1A H 0.8042 0.3082 0.3585 0.083 Uiso 0.50 1 calc PR . . H1B H 1.0508 0.2968 0.3635 0.083 Uiso 0.50 1 calc PR . . H1C H 0.9330 0.2942 0.4729 0.083 Uiso 0.50 1 calc PR . . H1D H 1.0545 0.2912 0.4381 0.083 Uiso 0.50 1 calc PR . . H1E H 0.8079 0.3027 0.4332 0.083 Uiso 0.50 1 calc PR . . H1F H 0.9256 0.3052 0.3237 0.083 Uiso 0.50 1 calc PR . . C2 C 0.8629(2) 0.24248(5) 0.36860(12) 0.0430(4) Uani 1 1 d . . . C3 C 0.9824(2) 0.20469(5) 0.40300(13) 0.0527(4) Uani 1 1 d . . . H3 H 1.1171 0.2045 0.4449 0.063 Uiso 1 1 calc R . . C4 C 0.8675(2) 0.16817(5) 0.36471(13) 0.0507(4) Uani 1 1 d . . . H4 H 0.9096 0.1387 0.3755 0.061 Uiso 1 1 calc R . . C5 C 0.6739(2) 0.18329(5) 0.30596(12) 0.0395(3) Uani 1 1 d . . . C6 C 0.5000 0.16055(6) 0.2500 0.0392(5) Uani 1 2 d S . . C7 C 0.5000 0.11134(7) 0.2500 0.0465(5) Uani 1 2 d S . . C8 C 0.5328(14) 0.08805(12) 0.1542(4) 0.0600(13) Uani 0.794(19) 1 d PD A 1 H8 H 0.5549 0.1033 0.0888 0.072 Uiso 0.794(19) 1 calc PR A 1 C9 C 0.5334(14) 0.04219(13) 0.1543(4) 0.0641(14) Uani 0.794(19) 1 d PD A 1 H9 H 0.5567 0.0270 0.0889 0.077 Uiso 0.794(19) 1 calc PR A 1 C8B C 0.628(4) 0.0870(5) 0.184(2) 0.065(5) Uani 0.206(19) 1 d PD A 2 H8B H 0.7173 0.1018 0.1390 0.079 Uiso 0.206(19) 1 calc PR A 2 C9B C 0.625(4) 0.0409(5) 0.184(3) 0.066(5) Uani 0.206(19) 1 d PD A 2 H9B H 0.7093 0.0254 0.1373 0.079 Uiso 0.206(19) 1 calc PR A 2 C10 C 0.5000 0.01849(7) 0.2500 0.0540(6) Uani 1 2 d S . . C11 C 0.5000 -0.03095(7) 0.2500 0.0592(6) Uani 1 2 d S . . C12 C 0.3291(3) -0.05241(6) 0.18627(16) 0.0669(5) Uani 1 1 d . . . C13 C 0.1448(3) -0.03442(6) 0.12479(16) 0.0745(6) Uani 1 1 d . A . H13 H 0.1137 -0.0044 0.1146 0.089 Uiso 1 1 calc R . . C14 C 0.0195(4) -0.06904(7) 0.0827(2) 0.0900(7) Uani 1 1 d . . . H14 H -0.1124 -0.0672 0.0384 0.108 Uiso 1 1 calc R A . C15 C 0.1282(4) -0.10776(7) 0.11939(19) 0.0975(8) Uani 1 1 d . A . H15 H 0.0777 -0.1364 0.1032 0.117 Uiso 1 1 calc R . . B1 B 0.5000 0.25967(7) 0.2500 0.0392(5) Uani 1 2 d S . . N1 N 0.67647(16) 0.22950(4) 0.30933(9) 0.0367(3) Uani 1 1 d . . . N2 N 0.3116(4) -0.09848(5) 0.17986(16) 0.0844(6) Uani 1 1 d . A . F1 F 0.41287(14) 0.28610(3) 0.32799(8) 0.0664(3) Uani 1 1 d . . . H2 H 0.388(6) -0.1176(12) 0.226(3) 0.082(13) 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 C1 0.0447(8) 0.0679(11) 0.0534(10) -0.0151(8) 0.0056(7) -0.0173(7) C2 0.0347(7) 0.0583(9) 0.0359(8) -0.0032(6) 0.0031(6) -0.0040(6) C3 0.0375(7) 0.0751(12) 0.0432(9) 0.0004(8) -0.0068(7) 0.0052(7) C4 0.0495(9) 0.0571(10) 0.0443(9) 0.0077(7) -0.0014(7) 0.0149(7) C5 0.0420(7) 0.0380(8) 0.0381(8) 0.0045(6) 0.0026(6) 0.0044(6) C6 0.0456(11) 0.0355(11) 0.0367(11) 0.000 0.0056(9) 0.000 C7 0.0544(12) 0.0392(12) 0.0456(13) 0.000 0.0040(10) 0.000 C8 0.098(4) 0.0394(14) 0.0440(18) 0.0001(11) 0.014(2) -0.0067(18) C9 0.105(4) 0.0428(16) 0.0461(19) -0.0073(12) 0.013(2) -0.0011(19) C8B 0.062(9) 0.049(6) 0.088(13) -0.011(7) 0.023(9) -0.008(6) C9B 0.070(10) 0.046(6) 0.086(14) -0.004(7) 0.024(9) 0.005(6) C10 0.0721(15) 0.0356(12) 0.0536(15) 0.000 0.0038(12) 0.000 C11 0.0842(17) 0.0370(12) 0.0558(15) 0.000 0.0043(13) 0.000 C12 0.0976(14) 0.0366(9) 0.0645(12) 0.0015(8) -0.0008(11) -0.0042(9) C13 0.0953(15) 0.0491(11) 0.0757(14) 0.0038(9) -0.0072(12) -0.0042(10) C14 0.1103(17) 0.0666(14) 0.0868(16) 0.0032(11) -0.0187(13) -0.0145(12) C15 0.146(2) 0.0544(13) 0.0860(17) -0.0027(11) -0.0151(16) -0.0259(14) B1 0.0376(12) 0.0364(12) 0.0434(14) 0.000 0.0030(10) 0.000 N1 0.0335(6) 0.0392(7) 0.0365(7) -0.0008(5) -0.0008(5) -0.0027(5) N2 0.1280(16) 0.0403(9) 0.0797(13) -0.0022(8) -0.0134(12) -0.0128(9) F1 0.0542(5) 0.0641(6) 0.0785(7) -0.0330(5) -0.0047(5) 0.0127(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 C1 C2 1.479(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C1 H1F 0.9600 . ? C2 N1 1.3515(17) . ? C2 C3 1.396(2) . ? C3 C4 1.364(2) . ? C3 H3 0.9300 . ? C4 C5 1.405(2) . ? C4 H4 0.9300 . ? C5 C6 1.3905(17) . ? C5 N1 1.3918(17) . ? C6 C5 1.3905(17) 2_655 ? C6 C7 1.481(3) . ? C7 C8 1.376(4) . ? C7 C8 1.376(4) 2_655 ? C7 C8B 1.387(17) 2_655 ? C7 C8B 1.387(17) . ? C8 C9 1.381(3) . ? C8 H8 0.9300 . ? C9 C10 1.382(5) . ? C9 H9 0.9300 . ? C8B C9B 1.385(9) . ? C8B H8B 0.9300 . ? C9B C10 1.35(2) . ? C9B H9B 0.9300 . ? C10 C9B 1.35(2) 2_655 ? C10 C9 1.382(5) 2_655 ? C10 C11 1.488(3) . ? C11 C12 1.399(2) . ? C11 C12 1.399(2) 2_655 ? C12 N2 1.392(2) . ? C12 C13 1.404(3) . ? C13 C14 1.365(3) . ? C13 H13 0.9300 . ? C14 C15 1.395(3) . ? C14 H14 0.9300 . ? C15 N2 1.315(3) . ? C15 H15 0.9300 . ? B1 F1 1.3796(15) . ? B1 F1 1.3796(15) 2_655 ? B1 N1 1.5390(17) 2_655 ? B1 N1 1.5390(17) . ? N2 H2 0.90(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1A C1 H1D 141.1 . . ? H1B C1 H1D 56.3 . . ? H1C C1 H1D 56.3 . . ? C2 C1 H1E 109.5 . . ? H1A C1 H1E 56.3 . . ? H1B C1 H1E 141.1 . . ? H1C C1 H1E 56.3 . . ? H1D C1 H1E 109.5 . . ? C2 C1 H1F 109.5 . . ? H1A C1 H1F 56.3 . . ? H1B C1 H1F 56.3 . . ? H1C C1 H1F 141.1 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? N1 C2 C3 108.63(13) . . ? N1 C2 C1 123.15(13) . . ? C3 C2 C1 128.19(14) . . ? C4 C3 C2 108.32(14) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? C3 C4 C5 107.32(14) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? C6 C5 N1 120.81(13) . . ? C6 C5 C4 131.56(14) . . ? N1 C5 C4 107.62(13) . . ? C5 C6 C5 121.00(18) . 2_655 ? C5 C6 C7 119.50(9) . . ? C5 C6 C7 119.50(9) 2_655 . ? C8 C7 C8 118.7(4) . 2_655 ? C8 C7 C8B 110.4(8) . 2_655 ? C8 C7 C8B 27.5(10) 2_655 2_655 ? C8 C7 C8B 27.5(10) . . ? C8 C7 C8B 110.4(8) 2_655 . ? C8B C7 C8B 116.1(14) 2_655 . ? C8 C7 C6 120.63(18) . . ? C8 C7 C6 120.63(18) 2_655 . ? C8B C7 C6 121.9(7) 2_655 . ? C8B C7 C6 121.9(7) . . ? C7 C8 C9 120.6(4) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 121.1(4) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9B C8B C7 121.5(15) . . ? C9B C8B H8B 119.2 . . ? C7 C8B H8B 119.2 . . ? C10 C9B C8B 120.5(16) . . ? C10 C9B H9B 119.7 . . ? C8B C9B H9B 119.7 . . ? C9B C10 C9B 119.8(14) . 2_655 ? C9B C10 C9 26.9(11) . . ? C9B C10 C9 112.0(8) 2_655 . ? C9B C10 C9 112.0(8) . 2_655 ? C9B C10 C9 26.9(11) 2_655 2_655 ? C9 C10 C9 117.8(4) . 2_655 ? C9B C10 C11 120.1(7) . . ? C9B C10 C11 120.1(7) 2_655 . ? C9 C10 C11 121.08(19) . . ? C9 C10 C11 121.08(19) 2_655 . ? C12 C11 C12 125.0(2) . 2_655 ? C12 C11 C10 117.51(11) . . ? C12 C11 C10 117.51(11) 2_655 . ? N2 C12 C11 122.71(19) . . ? N2 C12 C13 107.51(17) . . ? C11 C12 C13 129.69(17) . . ? C14 C13 C12 107.54(18) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? C13 C14 C15 106.4(2) . . ? C13 C14 H14 126.8 . . ? C15 C14 H14 126.8 . . ? N2 C15 C14 111.05(19) . . ? N2 C15 H15 124.5 . . ? C14 C15 H15 124.5 . . ? F1 B1 F1 109.55(18) . 2_655 ? F1 B1 N1 109.85(5) . 2_655 ? F1 B1 N1 109.94(6) 2_655 2_655 ? F1 B1 N1 109.94(6) . . ? F1 B1 N1 109.85(5) 2_655 . ? N1 B1 N1 107.67(16) 2_655 . ? C2 N1 C5 108.10(11) . . ? C2 N1 B1 127.02(12) . . ? C5 N1 B1 124.82(12) . . ? C15 N2 C12 107.47(19) . . ? C15 N2 H2 125(2) . . ? C12 N2 H2 125(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -0.20(16) . . . . ? C1 C2 C3 C4 177.83(13) . . . . ? C2 C3 C4 C5 -0.15(16) . . . . ? C3 C4 C5 C6 179.73(13) . . . . ? C3 C4 C5 N1 0.43(16) . . . . ? N1 C5 C6 C5 1.29(8) . . . 2_655 ? C4 C5 C6 C5 -177.93(17) . . . 2_655 ? N1 C5 C6 C7 -178.71(8) . . . . ? C4 C5 C6 C7 2.07(17) . . . . ? C5 C6 C7 C8 -107.4(4) . . . . ? C5 C6 C7 C8 72.6(4) 2_655 . . . ? C5 C6 C7 C8 72.6(4) . . . 2_655 ? C5 C6 C7 C8 -107.4(4) 2_655 . . 2_655 ? C5 C6 C7 C8B 104.9(16) . . . 2_655 ? C5 C6 C7 C8B -75.1(16) 2_655 . . 2_655 ? C5 C6 C7 C8B -75.1(16) . . . . ? C5 C6 C7 C8B 104.9(16) 2_655 . . . ? C8 C7 C8 C9 -0.2(2) 2_655 . . . ? C8B C7 C8 C9 -29.1(10) 2_655 . . . ? C8B C7 C8 C9 78.6(18) . . . . ? C6 C7 C8 C9 179.8(2) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C8 C7 C8B C9B -83.4(17) . . . . ? C8 C7 C8B C9B 30.1(16) 2_655 . . . ? C8B C7 C8B C9B 0.7(9) 2_655 . . . ? C6 C7 C8B C9B -179.3(9) . . . . ? C7 C8B C9B C10 -1.5(19) . . . . ? C8B C9B C10 C9B 0.7(9) . . . 2_655 ? C8B C9B C10 C9 80.6(18) . . . . ? C8B C9B C10 C9 -28.0(16) . . . 2_655 ? C8B C9B C10 C11 -179.3(9) . . . . ? C8 C9 C10 C9B -84.1(19) . . . . ? C8 C9 C10 C9B 28.8(11) . . . 2_655 ? C8 C9 C10 C9 -0.2(2) . . . 2_655 ? C8 C9 C10 C11 179.8(2) . . . . ? C9B C10 C11 C12 -99.8(16) . . . . ? C9B C10 C11 C12 80.2(16) 2_655 . . . ? C9 C10 C11 C12 -68.5(4) . . . . ? C9 C10 C11 C12 111.5(4) 2_655 . . . ? C9B C10 C11 C12 80.2(16) . . . 2_655 ? C9B C10 C11 C12 -99.8(16) 2_655 . . 2_655 ? C9 C10 C11 C12 111.5(4) . . . 2_655 ? C9 C10 C11 C12 -68.5(4) 2_655 . . 2_655 ? C12 C11 C12 N2 0.05(13) 2_655 . . . ? C10 C11 C12 N2 -179.95(13) . . . . ? C12 C11 C12 C13 176.1(2) 2_655 . . . ? C10 C11 C12 C13 -3.9(2) . . . . ? N2 C12 C13 C14 0.1(2) . . . . ? C11 C12 C13 C14 -176.35(18) . . . . ? C12 C13 C14 C15 0.2(3) . . . . ? C13 C14 C15 N2 -0.6(3) . . . . ? C3 C2 N1 C5 0.47(15) . . . . ? C1 C2 N1 C5 -177.68(12) . . . . ? C3 C2 N1 B1 -176.75(10) . . . . ? C1 C2 N1 B1 5.10(18) . . . . ? C6 C5 N1 C2 -179.94(10) . . . . ? C4 C5 N1 C2 -0.56(14) . . . . ? C6 C5 N1 B1 -2.65(16) . . . . ? C4 C5 N1 B1 176.73(9) . . . . ? F1 B1 N1 C2 -62.25(15) . . . . ? F1 B1 N1 C2 58.38(15) 2_655 . . . ? N1 B1 N1 C2 178.09(13) 2_655 . . . ? F1 B1 N1 C5 120.97(14) . . . . ? F1 B1 N1 C5 -118.40(14) 2_655 . . . ? N1 B1 N1 C5 1.31(8) 2_655 . . . ? C14 C15 N2 C12 0.7(3) . . . . ? C11 C12 N2 C15 176.29(18) . . . . ? C13 C12 N2 C15 -0.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.125 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.038 data_compound10 _database_code_depnum_ccdc_archive 'CCDC 684024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 B2 Cl4 Cu F4 N8' _chemical_formula_weight 1107.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 22.128(5) _cell_length_b 8.5689(18) _cell_length_c 27.299(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5176(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1468 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.12 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.219 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3365 _diffrn_reflns_av_R_equivalents 0.1215 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.51 _reflns_number_total 3365 _reflns_number_gt 1664 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3365 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.845 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7050(3) 0.7313(7) 0.84913(17) 0.064(2) Uani 1 1 d . . . H1A H 0.6708 0.6672 0.8384 0.095 Uiso 1 1 calc R . . H1B H 0.7339 0.7424 0.8221 0.095 Uiso 1 1 calc R . . H1C H 0.6904 0.8346 0.8590 0.095 Uiso 1 1 calc R . . C2 C 0.7354(3) 0.6549(6) 0.89147(17) 0.0411(16) Uani 1 1 d . . . C3 C 0.7964(3) 0.6594(7) 0.90378(19) 0.0487(17) Uani 1 1 d . . . H3 H 0.8276 0.7061 0.8848 0.058 Uiso 1 1 calc R . . C4 C 0.8041(3) 0.5856(6) 0.94769(17) 0.0367(15) Uani 1 1 d . . . H4 H 0.8410 0.5741 0.9652 0.044 Uiso 1 1 calc R . . C5 C 0.7468(3) 0.5294(6) 0.96219(16) 0.0294(14) Uani 1 1 d . . . C6 C 0.7276(2) 0.4534(6) 1.00457(16) 0.0274(14) Uani 1 1 d . . . C7 C 0.6674(3) 0.4073(6) 1.00934(17) 0.0305(14) Uani 1 1 d . . . C8 C 0.6379(3) 0.3172(6) 1.04489(18) 0.0409(15) Uani 1 1 d . . . H8 H 0.6553 0.2786 1.0743 0.049 Uiso 1 1 calc R . . C9 C 0.5796(3) 0.2946(7) 1.0296(2) 0.0471(16) Uani 1 1 d . . . H9 H 0.5493 0.2380 1.0467 0.057 Uiso 1 1 calc R . . C10 C 0.5726(3) 0.3688(6) 0.9849(2) 0.0398(15) Uani 1 1 d . . . C11 C 0.5179(2) 0.3772(7) 0.9531(2) 0.0605(19) Uani 1 1 d . . . H11A H 0.5127 0.4842 0.9412 0.091 Uiso 1 1 calc R . . H11B H 0.4823 0.3461 0.9720 0.091 Uiso 1 1 calc R . . H11C H 0.5229 0.3066 0.9251 0.091 Uiso 1 1 calc R . . C12 C 0.7702(2) 0.4191(6) 1.04396(15) 0.0295(14) Uani 1 1 d . . . C13 C 0.7601(2) 0.4711(6) 1.09088(16) 0.0336(15) Uani 1 1 d . . . H13 H 0.7242 0.5278 1.0978 0.040 Uiso 1 1 calc R . . C14 C 0.8008(2) 0.4429(6) 1.12825(16) 0.0337(15) Uani 1 1 d . . . H14 H 0.7930 0.4824 1.1602 0.040 Uiso 1 1 calc R . . C15 C 0.8532(2) 0.3569(6) 1.11941(16) 0.0316(14) Uani 1 1 d . . . C16 C 0.8629(2) 0.3002(6) 1.07281(15) 0.0280(13) Uani 1 1 d . . . H16 H 0.8976 0.2385 1.0664 0.034 Uiso 1 1 calc R . . C17 C 0.8226(2) 0.3317(6) 1.03506(16) 0.0302(13) Uani 1 1 d . . . H17 H 0.8307 0.2939 1.0030 0.036 Uiso 1 1 calc R . . C18 C 1.0514(3) 0.4394(7) 1.16330(18) 0.0443(16) Uani 1 1 d . . . H18 H 1.0905 0.4441 1.1777 0.053 Uiso 1 1 calc R . . C19 C 1.0360(3) 0.5122(6) 1.11798(18) 0.0432(16) Uani 1 1 d . . . H19 H 1.0616 0.5727 1.0975 0.052 Uiso 1 1 calc R . . C20 C 0.9772(3) 0.4768(7) 1.11024(19) 0.0410(16) Uani 1 1 d . . . H20 H 0.9537 0.5075 1.0828 0.049 Uiso 1 1 calc R . . C21 C 0.9567(3) 0.3857(6) 1.15035(17) 0.0319(14) Uani 1 1 d . . . C22 C 0.8986(2) 0.3291(6) 1.15929(16) 0.0320(14) Uani 1 1 d . . . C23 C 0.8789(2) 0.2576(6) 1.20189(16) 0.0287(14) Uani 1 1 d . . . C24 C 0.8226(2) 0.1843(7) 1.21062(17) 0.0388(15) Uani 1 1 d . . . H24 H 0.7891 0.1815 1.1889 0.047 Uiso 1 1 calc R . . C25 C 0.8253(2) 0.1183(6) 1.25601(18) 0.0413(15) Uani 1 1 d . . . H25 H 0.7945 0.0601 1.2719 0.050 Uiso 1 1 calc R . . C26 C 0.8828(3) 0.1539(6) 1.27435(18) 0.0387(15) Uani 1 1 d . . . H26 H 0.8965 0.1233 1.3059 0.046 Uiso 1 1 calc R . . N1 N 0.7056(2) 0.5740(5) 0.92614(13) 0.0313(11) Uani 1 1 d . . . N2 N 0.6254(2) 0.4398(5) 0.97231(13) 0.0276(11) Uani 1 1 d . . . N3 N 1.0044(2) 0.3634(5) 1.18309(13) 0.0311(11) Uani 1 1 d . . . N4 N 0.91612(17) 0.2351(5) 1.24277(13) 0.0319(11) Uani 1 1 d . . . F1 F 0.61698(14) 0.4738(3) 0.88548(9) 0.0524(10) Uani 1 1 d . . . F2 F 0.60622(13) 0.6858(4) 0.93438(10) 0.0502(9) Uani 1 1 d . . . Cu1 Cu 1.0000 0.29158(11) 1.2500 0.0342(3) Uani 1 2 d S . . B1 B 0.6363(3) 0.5426(8) 0.9285(2) 0.0339(17) 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 C1 0.112(6) 0.052(4) 0.027(3) 0.005(3) 0.002(3) 0.012(4) C2 0.071(5) 0.032(4) 0.021(3) -0.007(3) -0.003(3) 0.000(4) C3 0.074(5) 0.040(4) 0.032(3) 0.000(3) 0.019(3) -0.013(4) C4 0.031(4) 0.045(4) 0.034(3) -0.008(3) 0.008(3) -0.009(3) C5 0.038(4) 0.025(3) 0.025(3) -0.008(3) -0.007(3) 0.005(3) C6 0.031(4) 0.030(4) 0.021(3) -0.003(3) -0.005(3) 0.004(3) C7 0.032(4) 0.030(4) 0.029(3) 0.000(3) 0.001(3) 0.000(3) C8 0.046(4) 0.037(4) 0.039(3) 0.013(3) 0.002(3) 0.012(3) C9 0.026(4) 0.047(4) 0.068(4) 0.017(4) 0.002(3) -0.010(3) C10 0.031(4) 0.035(4) 0.053(4) -0.005(3) -0.005(3) 0.001(3) C11 0.041(5) 0.064(5) 0.077(4) -0.017(4) -0.023(4) -0.003(3) C12 0.033(4) 0.035(4) 0.021(3) -0.003(3) 0.001(3) 0.002(3) C13 0.026(4) 0.046(4) 0.029(3) -0.004(3) -0.004(3) 0.014(3) C14 0.039(4) 0.047(4) 0.015(2) -0.002(3) 0.001(3) 0.012(3) C15 0.034(4) 0.041(4) 0.020(3) -0.002(3) 0.000(3) 0.008(3) C16 0.022(3) 0.033(3) 0.030(3) 0.004(3) -0.005(2) 0.002(3) C17 0.032(4) 0.035(3) 0.023(3) -0.008(3) 0.004(3) 0.000(3) C18 0.035(4) 0.050(4) 0.048(4) 0.000(3) -0.009(3) -0.003(3) C19 0.050(5) 0.043(4) 0.037(3) 0.018(3) -0.008(3) -0.014(4) C20 0.041(4) 0.047(4) 0.036(3) 0.006(3) -0.011(3) -0.003(3) C21 0.041(4) 0.032(4) 0.023(3) 0.003(3) 0.000(3) -0.009(3) C22 0.036(4) 0.036(4) 0.024(3) -0.005(3) -0.002(3) 0.003(3) C23 0.034(4) 0.028(4) 0.024(3) -0.001(2) -0.001(3) -0.003(3) C24 0.031(4) 0.057(4) 0.029(3) 0.003(3) -0.005(3) -0.009(3) C25 0.035(4) 0.053(4) 0.037(3) 0.006(3) 0.002(3) -0.012(3) C26 0.034(4) 0.049(4) 0.033(3) 0.004(3) -0.006(3) -0.004(3) N1 0.048(3) 0.031(3) 0.015(2) -0.001(2) -0.002(2) 0.001(2) N2 0.030(3) 0.025(3) 0.027(2) -0.001(2) -0.009(2) 0.004(2) N3 0.030(3) 0.034(3) 0.030(2) 0.0025(19) -0.005(3) -0.008(3) N4 0.026(3) 0.046(3) 0.024(2) 0.005(2) -0.005(2) -0.009(2) F1 0.068(3) 0.052(2) 0.0369(17) -0.0135(16) -0.0259(17) 0.0044(18) F2 0.062(2) 0.041(2) 0.0471(17) 0.0026(16) -0.0141(17) 0.0183(18) Cu1 0.0329(6) 0.0464(6) 0.0232(4) 0.000 -0.0075(5) 0.000 B1 0.035(5) 0.036(5) 0.032(3) -0.003(3) -0.012(3) 0.008(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 C1 C2 1.489(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.346(6) . ? C2 C3 1.392(7) . ? C3 C4 1.366(7) . ? C3 H3 0.9500 . ? C4 C5 1.413(7) . ? C4 H4 0.9500 . ? C5 N1 1.395(6) . ? C5 C6 1.394(6) . ? C6 C7 1.394(6) . ? C6 C12 1.460(6) . ? C7 N2 1.402(6) . ? C7 C8 1.402(7) . ? C8 C9 1.369(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(7) . ? C9 H9 0.9500 . ? C10 N2 1.361(6) . ? C10 C11 1.492(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.374(6) . ? C12 C17 1.403(6) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.396(6) . ? C14 H14 0.9500 . ? C15 C16 1.378(6) . ? C15 C22 1.500(6) . ? C16 C17 1.388(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 N3 1.341(6) . ? C18 C19 1.427(7) . ? C18 H18 0.9500 . ? C19 C20 1.353(7) . ? C19 H19 0.9500 . ? C20 C21 1.419(7) . ? C20 H20 0.9500 . ? C21 C22 1.396(7) . ? C21 N3 1.397(6) . ? C22 C23 1.384(6) . ? C23 N4 1.400(5) . ? C23 C24 1.416(6) . ? C24 C25 1.363(6) . ? C24 H24 0.9500 . ? C25 C26 1.400(6) . ? C25 H25 0.9500 . ? C26 N4 1.331(6) . ? C26 H26 0.9500 . ? N1 B1 1.558(7) . ? N2 B1 1.505(7) . ? N3 Cu1 1.930(4) . ? N4 Cu1 1.928(4) . ? F1 B1 1.382(6) . ? F2 B1 1.406(7) . ? Cu1 N4 1.928(4) 4_757 ? Cu1 N3 1.930(4) 4_757 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.7(5) . . ? N1 C2 C1 123.4(6) . . ? C3 C2 C1 127.8(6) . . ? C4 C3 C2 108.6(5) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? C3 C4 C5 107.0(5) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N1 C5 C6 121.0(5) . . ? N1 C5 C4 107.2(4) . . ? C6 C5 C4 131.7(5) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 C12 120.6(5) . . ? C7 C6 C12 119.4(4) . . ? C6 C7 N2 120.7(4) . . ? C6 C7 C8 131.7(5) . . ? N2 C7 C8 107.4(5) . . ? C9 C8 C7 107.8(5) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C8 C9 C10 108.0(5) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? N2 C10 C9 109.4(5) . . ? N2 C10 C11 121.8(5) . . ? C9 C10 C11 128.8(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.0(5) . . ? C13 C12 C6 121.1(5) . . ? C17 C12 C6 120.9(4) . . ? C12 C13 C14 121.7(5) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.3(4) . . ? C16 C15 C22 120.7(5) . . ? C14 C15 C22 121.0(4) . . ? C15 C16 C17 121.2(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 120.4(4) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? N3 C18 C19 112.1(5) . . ? N3 C18 H18 124.0 . . ? C19 C18 H18 124.0 . . ? C20 C19 C18 105.5(5) . . ? C20 C19 H19 127.2 . . ? C18 C19 H19 127.2 . . ? C19 C20 C21 108.1(5) . . ? C19 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? C22 C21 N3 122.5(4) . . ? C22 C21 C20 128.3(5) . . ? N3 C21 C20 109.1(5) . . ? C23 C22 C21 126.1(5) . . ? C23 C22 C15 118.0(5) . . ? C21 C22 C15 115.8(4) . . ? C22 C23 N4 123.1(5) . . ? C22 C23 C24 127.9(5) . . ? N4 C23 C24 108.8(4) . . ? C25 C24 C23 107.3(5) . . ? C25 C24 H24 126.3 . . ? C23 C24 H24 126.3 . . ? C24 C25 C26 106.0(5) . . ? C24 C25 H25 127.0 . . ? C26 C25 H25 127.0 . . ? N4 C26 C25 112.7(4) . . ? N4 C26 H26 123.7 . . ? C25 C26 H26 123.7 . . ? C2 N1 C5 108.5(5) . . ? C2 N1 B1 126.9(5) . . ? C5 N1 B1 124.5(4) . . ? C10 N2 C7 107.4(4) . . ? C10 N2 B1 126.9(4) . . ? C7 N2 B1 125.6(5) . . ? C18 N3 C21 105.2(4) . . ? C18 N3 Cu1 125.2(4) . . ? C21 N3 Cu1 127.6(4) . . ? C26 N4 C23 105.2(4) . . ? C26 N4 Cu1 126.7(3) . . ? C23 N4 Cu1 127.8(3) . . ? N4 Cu1 N4 150.9(2) . 4_757 ? N4 Cu1 N3 97.34(18) . 4_757 ? N4 Cu1 N3 91.85(18) 4_757 4_757 ? N4 Cu1 N3 91.85(18) . . ? N4 Cu1 N3 97.34(18) 4_757 . ? N3 Cu1 N3 142.8(2) 4_757 . ? F1 B1 F2 108.8(4) . . ? F1 B1 N2 112.1(5) . . ? F2 B1 N2 110.1(4) . . ? F1 B1 N1 110.1(5) . . ? F2 B1 N1 108.7(5) . . ? N2 B1 N1 107.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -2.4(6) . . . . ? C1 C2 C3 C4 174.5(5) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C3 C4 C5 N1 -0.8(5) . . . . ? C3 C4 C5 C6 -176.2(5) . . . . ? N1 C5 C6 C7 6.2(7) . . . . ? C4 C5 C6 C7 -178.9(5) . . . . ? N1 C5 C6 C12 -174.7(4) . . . . ? C4 C5 C6 C12 0.2(8) . . . . ? C5 C6 C7 N2 -1.4(7) . . . . ? C12 C6 C7 N2 179.4(4) . . . . ? C5 C6 C7 C8 172.7(5) . . . . ? C12 C6 C7 C8 -6.5(8) . . . . ? C6 C7 C8 C9 -174.3(5) . . . . ? N2 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C8 C9 C10 N2 -1.0(7) . . . . ? C8 C9 C10 C11 179.3(5) . . . . ? C5 C6 C12 C13 123.7(5) . . . . ? C7 C6 C12 C13 -57.2(7) . . . . ? C5 C6 C12 C17 -56.5(7) . . . . ? C7 C6 C12 C17 122.6(5) . . . . ? C17 C12 C13 C14 1.9(8) . . . . ? C6 C12 C13 C14 -178.3(5) . . . . ? C12 C13 C14 C15 -1.5(8) . . . . ? C13 C14 C15 C16 -0.5(8) . . . . ? C13 C14 C15 C22 178.3(5) . . . . ? C14 C15 C16 C17 2.1(8) . . . . ? C22 C15 C16 C17 -176.8(5) . . . . ? C15 C16 C17 C12 -1.7(7) . . . . ? C13 C12 C17 C16 -0.3(7) . . . . ? C6 C12 C17 C16 179.9(5) . . . . ? N3 C18 C19 C20 -0.5(7) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C19 C20 C21 C22 176.7(5) . . . . ? C19 C20 C21 N3 -0.7(6) . . . . ? N3 C21 C22 C23 5.9(8) . . . . ? C20 C21 C22 C23 -171.2(5) . . . . ? N3 C21 C22 C15 -177.4(4) . . . . ? C20 C21 C22 C15 5.5(8) . . . . ? C16 C15 C22 C23 -124.4(5) . . . . ? C14 C15 C22 C23 56.8(7) . . . . ? C16 C15 C22 C21 58.6(7) . . . . ? C14 C15 C22 C21 -120.2(6) . . . . ? C21 C22 C23 N4 1.1(8) . . . . ? C15 C22 C23 N4 -175.6(4) . . . . ? C21 C22 C23 C24 -172.8(5) . . . . ? C15 C22 C23 C24 10.5(8) . . . . ? C22 C23 C24 C25 174.6(5) . . . . ? N4 C23 C24 C25 0.1(6) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C24 C25 C26 N4 -1.2(6) . . . . ? C3 C2 N1 C5 1.9(6) . . . . ? C1 C2 N1 C5 -175.2(5) . . . . ? C3 C2 N1 B1 178.3(5) . . . . ? C1 C2 N1 B1 1.1(8) . . . . ? C6 C5 N1 C2 175.3(4) . . . . ? C4 C5 N1 C2 -0.7(5) . . . . ? C6 C5 N1 B1 -1.1(7) . . . . ? C4 C5 N1 B1 -177.2(4) . . . . ? C9 C10 N2 C7 1.3(6) . . . . ? C11 C10 N2 C7 -179.0(4) . . . . ? C9 C10 N2 B1 -175.3(5) . . . . ? C11 C10 N2 B1 4.4(8) . . . . ? C6 C7 N2 C10 174.4(5) . . . . ? C8 C7 N2 C10 -1.0(5) . . . . ? C6 C7 N2 B1 -9.0(7) . . . . ? C8 C7 N2 B1 175.6(5) . . . . ? C19 C18 N3 C21 0.1(6) . . . . ? C19 C18 N3 Cu1 -164.8(4) . . . . ? C22 C21 N3 C18 -177.2(5) . . . . ? C20 C21 N3 C18 0.4(6) . . . . ? C22 C21 N3 Cu1 -12.8(7) . . . . ? C20 C21 N3 Cu1 164.8(4) . . . . ? C25 C26 N4 C23 1.2(6) . . . . ? C25 C26 N4 Cu1 -173.6(3) . . . . ? C22 C23 N4 C26 -175.6(5) . . . . ? C24 C23 N4 C26 -0.8(5) . . . . ? C22 C23 N4 Cu1 -0.9(7) . . . . ? C24 C23 N4 Cu1 174.0(3) . . . . ? C26 N4 Cu1 N4 61.3(4) . . . 4_757 ? C23 N4 Cu1 N4 -112.4(4) . . . 4_757 ? C26 N4 Cu1 N3 -46.1(5) . . . 4_757 ? C23 N4 Cu1 N3 140.2(4) . . . 4_757 ? C26 N4 Cu1 N3 170.0(4) . . . . ? C23 N4 Cu1 N3 -3.7(4) . . . . ? C18 N3 Cu1 N4 171.8(4) . . . . ? C21 N3 Cu1 N4 10.3(4) . . . . ? C18 N3 Cu1 N4 -35.8(5) . . . 4_757 ? C21 N3 Cu1 N4 162.6(4) . . . 4_757 ? C18 N3 Cu1 N3 67.1(4) . . . 4_757 ? C21 N3 Cu1 N3 -94.4(4) . . . 4_757 ? C10 N2 B1 F1 -50.9(7) . . . . ? C7 N2 B1 F1 133.1(5) . . . . ? C10 N2 B1 F2 70.4(7) . . . . ? C7 N2 B1 F2 -105.6(5) . . . . ? C10 N2 B1 N1 -171.7(4) . . . . ? C7 N2 B1 N1 12.3(7) . . . . ? C2 N1 B1 F1 54.8(7) . . . . ? C5 N1 B1 F1 -129.3(5) . . . . ? C2 N1 B1 F2 -64.3(6) . . . . ? C5 N1 B1 F2 111.6(5) . . . . ? C2 N1 B1 N2 176.9(4) . . . . ? C5 N1 B1 N2 -7.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.459 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.072 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 26 4 ' ' 2 1.000 -0.215 0.250 284 84 ' ' 3 0.500 0.285 0.250 284 84 ' ' 4 0.500 0.000 0.500 26 4 ' ' 5 1.000 0.215 0.750 284 84 ' ' 6 0.500 -0.285 0.750 284 84 ' ' 7 0.000 0.500 0.500 26 4 ' ' 8 1.000 0.500 1.000 26 4 ' ' _platon_squeeze_details ; ; #===End data_compound11 _database_code_depnum_ccdc_archive 'CCDC 684025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H52 B2 Cl4 Cu F4 N8' _chemical_formula_weight 1164.04 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.142(2) _cell_length_b 20.146(3) _cell_length_c 15.483(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.191(7) _cell_angle_gamma 90.00 _cell_volume 5658.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3213 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.80 _exptl_crystal_description tablet _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.293 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31031 _diffrn_reflns_av_R_equivalents 0.1295 _diffrn_reflns_av_sigmaI/netI 0.1349 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 22.53 _reflns_number_total 7184 _reflns_number_gt 4123 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+2.2872P] 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 7184 _refine_ls_number_parameters 702 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2093 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1402(4) 0.0192(4) 0.9071(5) 0.047(2) Uani 1 1 d . . . H1A H -0.1488 0.0594 0.9411 0.070 Uiso 1 1 calc R . . H1B H -0.1300 -0.0181 0.9460 0.070 Uiso 1 1 calc R . . H1C H -0.1840 0.0092 0.8723 0.070 Uiso 1 1 calc R . . C2 C -0.0750(4) 0.0299(3) 0.8482(5) 0.0350(19) Uani 1 1 d . . . C3 C 0.0004(4) 0.0221(4) 0.8674(5) 0.039(2) Uani 1 1 d . . . H3 H 0.0204 0.0075 0.9209 0.047 Uiso 1 1 calc R . . C4 C 0.0400(4) 0.0394(3) 0.7957(5) 0.0357(19) Uani 1 1 d . . . H4 H 0.0922 0.0391 0.7903 0.043 Uiso 1 1 calc R . . C5 C -0.0114(4) 0.0577(3) 0.7311(4) 0.0293(18) Uani 1 1 d . . . C6 C -0.0005(3) 0.0815(3) 0.6468(4) 0.0266(17) Uani 1 1 d . . . C7 C -0.0611(3) 0.0951(3) 0.5922(4) 0.0280(17) Uani 1 1 d . . . C8 C -0.0657(4) 0.1225(4) 0.5090(5) 0.0372(19) Uani 1 1 d . . . H8 H -0.0255 0.1382 0.4754 0.045 Uiso 1 1 calc R . . C9 C -0.1395(4) 0.1227(4) 0.4844(5) 0.043(2) Uani 1 1 d . . . H9 H -0.1589 0.1375 0.4306 0.051 Uiso 1 1 calc R . . C10 C -0.1797(4) 0.0972(4) 0.5531(5) 0.039(2) Uani 1 1 d . . . C11 C -0.2618(3) 0.0873(4) 0.5590(5) 0.051(2) Uani 1 1 d . . . H11A H -0.2721 0.0433 0.5833 0.076 Uiso 1 1 calc R . . H11B H -0.2836 0.0905 0.5011 0.076 Uiso 1 1 calc R . . H11C H -0.2831 0.1215 0.5962 0.076 Uiso 1 1 calc R . . C12 C 0.0764(3) 0.0931(3) 0.6122(4) 0.0256(17) Uani 1 1 d . . . C13 C 0.0989(3) 0.0661(3) 0.5341(5) 0.0307(18) Uani 1 1 d . . . H13 H 0.0661 0.0382 0.5027 0.037 Uiso 1 1 calc R . . C14 C 0.1684(3) 0.0789(3) 0.5013(5) 0.0305(18) Uani 1 1 d . . . H14 H 0.1821 0.0603 0.4473 0.037 Uiso 1 1 calc R . . C15 C 0.2187(3) 0.1186(3) 0.5459(4) 0.0213(16) Uani 1 1 d . . . C16 C 0.1964(4) 0.1448(3) 0.6249(5) 0.0339(19) Uani 1 1 d . . . H16 H 0.2298 0.1716 0.6569 0.041 Uiso 1 1 calc R . . C17 C 0.1264(3) 0.1327(3) 0.6584(5) 0.0327(19) Uani 1 1 d . . . H17 H 0.1127 0.1512 0.7124 0.039 Uiso 1 1 calc R . . C18 C 0.3902(4) 0.2668(4) 0.2659(5) 0.051(2) Uani 1 1 d . . . H18A H 0.4408 0.2595 0.2863 0.077 Uiso 1 1 calc R . . H18B H 0.3814 0.3145 0.2593 0.077 Uiso 1 1 calc R . . H18C H 0.3833 0.2447 0.2101 0.077 Uiso 1 1 calc R . . C19 C 0.3372(4) 0.2389(4) 0.3299(5) 0.0351(19) Uani 1 1 d . . . C20 C 0.2613(4) 0.2551(4) 0.3400(4) 0.0349(19) Uani 1 1 d . . . H20 H 0.2347 0.2870 0.3072 0.042 Uiso 1 1 calc R . . C21 C 0.2330(4) 0.2163(3) 0.4055(4) 0.0308(18) Uani 1 1 d . . . H21 H 0.1836 0.2157 0.4256 0.037 Uiso 1 1 calc R . . C22 C 0.2934(3) 0.1773(3) 0.4372(4) 0.0254(17) Uani 1 1 d . . . C23 C 0.2924(3) 0.1333(3) 0.5082(4) 0.0219(16) Uani 1 1 d . . . C24 C 0.3536(3) 0.1032(3) 0.5478(4) 0.0251(17) Uani 1 1 d . . . C25 C 0.3532(4) 0.0603(4) 0.6211(5) 0.0360(19) Uani 1 1 d . . . H25 H 0.3111 0.0466 0.6529 0.043 Uiso 1 1 calc R . . C26 C 0.4255(4) 0.0422(4) 0.6369(5) 0.040(2) Uani 1 1 d . . . H26 H 0.4423 0.0143 0.6823 0.049 Uiso 1 1 calc R . . C27 C 0.4697(4) 0.0724(3) 0.5737(5) 0.0307(18) Uani 1 1 d . . . C28 C 0.5519(3) 0.0659(4) 0.5634(5) 0.042(2) Uani 1 1 d . . . H28A H 0.5645 0.0680 0.5019 0.063 Uiso 1 1 calc R . . H28B H 0.5681 0.0232 0.5872 0.063 Uiso 1 1 calc R . . H28C H 0.5765 0.1021 0.5943 0.063 Uiso 1 1 calc R . . C29 C 1.1764(4) 0.1463(4) 0.1794(6) 0.059(3) Uani 1 1 d . . . H29A H 1.1906 0.1091 0.1423 0.088 Uiso 1 1 calc R . . H29B H 1.2055 0.1450 0.2328 0.088 Uiso 1 1 calc R . . H29C H 1.1856 0.1882 0.1492 0.088 Uiso 1 1 calc R . . C30 C 1.0952(4) 0.1411(4) 0.2010(5) 0.039(2) Uani 1 1 d . . . C31 C 1.0623(4) 0.1229(4) 0.2790(5) 0.043(2) Uani 1 1 d . . . H31 H 1.0872 0.1086 0.3298 0.051 Uiso 1 1 calc R . . C32 C 0.9864(4) 0.1295(4) 0.2689(5) 0.0361(19) Uani 1 1 d . . . H32 H 0.9502 0.1212 0.3118 0.043 Uiso 1 1 calc R . . C33 C 0.9728(3) 0.1506(3) 0.1834(4) 0.0276(17) Uani 1 1 d . . . C34 C 0.9068(3) 0.1655(3) 0.1392(4) 0.0266(17) Uani 1 1 d . . . C35 C 0.9077(3) 0.1832(3) 0.0515(4) 0.0263(17) Uani 1 1 d . . . C36 C 0.8489(4) 0.1933(3) -0.0070(5) 0.0367(19) Uani 1 1 d . . . H36 H 0.7977 0.1927 0.0060 0.044 Uiso 1 1 calc R . . C37 C 0.8807(4) 0.2044(3) -0.0880(5) 0.037(2) Uani 1 1 d . . . H37 H 0.8550 0.2126 -0.1405 0.045 Uiso 1 1 calc R . . C38 C 0.9575(4) 0.2010(3) -0.0773(5) 0.039(2) Uani 1 1 d . . . C39 C 1.0155(4) 0.2093(4) -0.1458(5) 0.053(2) Uani 1 1 d . . . H39A H 1.0456 0.2484 -0.1326 0.079 Uiso 1 1 calc R . . H39B H 0.9916 0.2152 -0.2022 0.079 Uiso 1 1 calc R . . H39C H 1.0469 0.1697 -0.1472 0.079 Uiso 1 1 calc R . . C40 C 0.8350(3) 0.1639(3) 0.1870(4) 0.0238(17) Uani 1 1 d . . . C41 C 0.7918(4) 0.2222(4) 0.1921(4) 0.0298(18) Uani 1 1 d . . . H41 H 0.8089 0.2624 0.1670 0.036 Uiso 1 1 calc R . . C42 C 0.7247(3) 0.2206(3) 0.2338(4) 0.0247(17) Uani 1 1 d . . . H42 H 0.6967 0.2603 0.2379 0.030 Uiso 1 1 calc R . . C43 C 0.6964(3) 0.1626(3) 0.2701(4) 0.0241(17) Uani 1 1 d . . . C44 C 0.7401(4) 0.1053(4) 0.2651(5) 0.038(2) Uani 1 1 d . . . H44 H 0.7229 0.0651 0.2902 0.046 Uiso 1 1 calc R . . C45 C 0.8078(4) 0.1062(4) 0.2242(5) 0.0351(19) Uani 1 1 d . . . H45 H 0.8362 0.0667 0.2216 0.042 Uiso 1 1 calc R . . C46 C 0.5097(4) 0.2502(4) 0.5804(5) 0.050(2) Uani 1 1 d . . . H46A H 0.4607 0.2520 0.5536 0.074 Uiso 1 1 calc R . . H46B H 0.5208 0.2931 0.6072 0.074 Uiso 1 1 calc R . . H46C H 0.5105 0.2153 0.6245 0.074 Uiso 1 1 calc R . . C47 C 0.5656(4) 0.2353(3) 0.5135(4) 0.0293(18) Uani 1 1 d . . . C48 C 0.6401(4) 0.2549(4) 0.5133(5) 0.0365(19) Uani 1 1 d . . . H48 H 0.6644 0.2806 0.5563 0.044 Uiso 1 1 calc R . . C49 C 0.6714(4) 0.2295(4) 0.4387(5) 0.0346(19) Uani 1 1 d . . . H49 H 0.7213 0.2345 0.4212 0.041 Uiso 1 1 calc R . . C50 C 0.6153(3) 0.1947(3) 0.3931(4) 0.0248(17) Uani 1 1 d . . . C51 C 0.6219(3) 0.1617(3) 0.3131(4) 0.0251(17) Uani 1 1 d . . . C52 C 0.5651(3) 0.1289(3) 0.2686(4) 0.0255(17) Uani 1 1 d . . . C53 C 0.5696(4) 0.0938(3) 0.1883(4) 0.0313(18) Uani 1 1 d . . . H53 H 0.6125 0.0889 0.1538 0.038 Uiso 1 1 calc R . . C54 C 0.5006(4) 0.0685(3) 0.1700(5) 0.0342(19) Uani 1 1 d . . . H54 H 0.4871 0.0430 0.1208 0.041 Uiso 1 1 calc R . . C55 C 0.4538(3) 0.0877(3) 0.2386(5) 0.0288(18) Uani 1 1 d . . . C56 C 0.3733(4) 0.0713(4) 0.2476(5) 0.050(2) Uani 1 1 d . . . H56A H 0.3628 0.0598 0.3079 0.075 Uiso 1 1 calc R . . H56B H 0.3612 0.0334 0.2104 0.075 Uiso 1 1 calc R . . H56C H 0.3436 0.1097 0.2306 0.075 Uiso 1 1 calc R . . B1 B -0.1554(4) 0.0602(4) 0.7140(6) 0.034(2) Uani 1 1 d . . . B2 B 1.0530(5) 0.1792(5) 0.0463(6) 0.039(2) Uani 1 1 d . . . N1 N -0.1336(3) 0.0809(3) 0.6205(4) 0.0298(15) Uani 1 1 d . . . N2 N -0.0828(3) 0.0511(3) 0.7651(4) 0.0284(14) Uani 1 1 d . . . N3 N 0.3578(3) 0.1917(3) 0.3888(3) 0.0260(14) Uani 1 1 d . . . N4 N 0.4273(3) 0.1098(3) 0.5195(4) 0.0277(14) Uani 1 1 d . . . N5 N 1.0415(3) 0.1566(3) 0.1409(4) 0.0294(14) Uani 1 1 d . . . N6 N 0.9740(3) 0.1873(3) 0.0055(4) 0.0291(14) Uani 1 1 d . . . N7 N 0.5500(3) 0.1991(3) 0.4416(4) 0.0284(14) Uani 1 1 d . . . N8 N 0.4912(3) 0.1236(3) 0.2996(3) 0.0243(14) Uani 1 1 d . . . F1 F -0.1982(2) 0.1107(2) 0.7498(3) 0.0519(12) Uani 1 1 d . . . F2 F -0.1956(2) 0.0012(2) 0.7117(3) 0.0486(12) Uani 1 1 d . . . F3 F 1.0920(2) 0.1302(2) 0.0009(3) 0.0549(13) Uani 1 1 d . . . F4 F 1.0910(2) 0.2394(2) 0.0417(3) 0.0616(14) Uani 1 1 d . . . Cu1 Cu 0.45600(4) 0.15652(4) 0.41180(5) 0.0280(3) Uani 1 1 d . . . C57 C 0.3512(7) 0.6075(6) 0.6530(11) 0.151(7) Uani 1 1 d . . . H57A H 0.3259 0.6502 0.6415 0.181 Uiso 1 1 calc R . . H57B H 0.3190 0.5805 0.6907 0.181 Uiso 1 1 calc R . . Cl1 Cl 0.4293(2) 0.6219(2) 0.7027(3) 0.1675(19) Uani 1 1 d . . . Cl2 Cl 0.3661(3) 0.56328(18) 0.5499(2) 0.1506(16) Uani 1 1 d . . . C58 C 0.2793(7) 0.4039(6) 0.4605(8) 0.110(4) Uani 1 1 d . . . H58A H 0.2610 0.4332 0.5070 0.132 Uiso 1 1 calc R . . H58B H 0.2456 0.3653 0.4571 0.132 Uiso 1 1 calc R . . Cl3 Cl 0.2737(3) 0.4459(2) 0.3659(4) 0.206(2) Uani 1 1 d . . . Cl4 Cl 0.3634(3) 0.3761(3) 0.4894(5) 0.280(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 C1 0.049(5) 0.053(5) 0.037(5) 0.000(4) 0.022(4) -0.009(4) C2 0.048(5) 0.030(4) 0.027(5) -0.004(4) 0.007(4) 0.000(4) C3 0.039(5) 0.049(5) 0.030(5) 0.004(4) -0.007(4) 0.002(4) C4 0.026(4) 0.045(5) 0.035(5) 0.009(4) -0.004(4) 0.002(4) C5 0.026(4) 0.039(5) 0.022(4) 0.001(3) 0.001(4) 0.000(3) C6 0.015(4) 0.031(4) 0.034(5) -0.005(4) 0.003(3) -0.005(3) C7 0.021(4) 0.032(4) 0.032(5) 0.001(4) 0.004(3) -0.001(3) C8 0.032(5) 0.044(5) 0.035(5) 0.007(4) 0.008(4) -0.004(4) C9 0.024(5) 0.070(6) 0.034(5) 0.023(4) -0.005(4) -0.002(4) C10 0.026(4) 0.040(5) 0.049(5) 0.001(4) -0.012(4) -0.001(4) C11 0.017(4) 0.064(6) 0.071(6) 0.013(5) -0.011(4) -0.002(4) C12 0.023(4) 0.034(4) 0.020(4) 0.006(3) 0.000(3) 0.001(3) C13 0.018(4) 0.041(5) 0.033(5) -0.001(4) -0.004(3) -0.003(3) C14 0.021(4) 0.043(5) 0.028(4) -0.010(4) 0.007(3) -0.001(3) C15 0.012(4) 0.035(4) 0.016(4) -0.002(3) 0.003(3) 0.004(3) C16 0.018(4) 0.050(5) 0.034(5) -0.008(4) 0.004(4) -0.007(3) C17 0.017(4) 0.049(5) 0.032(5) -0.011(4) 0.002(3) -0.001(3) C18 0.039(5) 0.068(6) 0.047(5) 0.030(5) 0.019(4) 0.010(4) C19 0.033(5) 0.044(5) 0.029(5) 0.003(4) 0.001(4) -0.001(4) C20 0.027(4) 0.049(5) 0.028(4) 0.012(4) 0.002(3) 0.011(4) C21 0.016(4) 0.045(5) 0.031(5) 0.000(4) 0.004(3) 0.002(3) C22 0.019(4) 0.030(4) 0.028(4) -0.004(3) -0.002(3) -0.002(3) C23 0.017(4) 0.030(4) 0.019(4) -0.003(3) 0.007(3) -0.002(3) C24 0.019(4) 0.038(4) 0.018(4) 0.008(3) 0.002(3) -0.013(3) C25 0.026(4) 0.047(5) 0.035(5) 0.010(4) 0.000(4) -0.002(4) C26 0.038(5) 0.043(5) 0.040(5) 0.021(4) -0.004(4) 0.003(4) C27 0.022(4) 0.036(5) 0.033(5) 0.005(4) -0.006(4) 0.007(3) C28 0.021(4) 0.047(5) 0.057(6) 0.007(4) -0.004(4) 0.009(4) C29 0.019(4) 0.069(6) 0.088(7) -0.026(5) -0.006(4) -0.003(4) C30 0.025(4) 0.044(5) 0.047(6) -0.013(4) -0.002(4) 0.000(4) C31 0.033(5) 0.051(5) 0.045(6) -0.009(4) -0.012(4) 0.012(4) C32 0.034(5) 0.050(5) 0.024(5) -0.010(4) 0.006(4) 0.000(4) C33 0.015(4) 0.038(5) 0.030(5) -0.011(4) 0.003(3) 0.005(3) C34 0.023(4) 0.030(4) 0.027(4) -0.003(3) 0.005(3) -0.003(3) C35 0.023(4) 0.027(4) 0.029(5) -0.001(3) 0.007(4) 0.005(3) C36 0.026(4) 0.044(5) 0.041(5) -0.002(4) -0.010(4) 0.011(4) C37 0.043(5) 0.044(5) 0.025(5) 0.004(4) -0.007(4) 0.011(4) C38 0.052(6) 0.031(5) 0.034(5) -0.001(4) 0.009(4) 0.008(4) C39 0.065(6) 0.051(6) 0.042(5) 0.012(4) 0.031(5) 0.010(4) C40 0.015(4) 0.040(5) 0.017(4) 0.001(3) 0.001(3) 0.000(3) C41 0.027(4) 0.036(5) 0.026(4) 0.006(3) 0.007(3) 0.002(4) C42 0.018(4) 0.028(4) 0.027(4) 0.002(3) 0.004(3) 0.006(3) C43 0.016(4) 0.037(5) 0.019(4) -0.007(3) 0.006(3) -0.009(3) C44 0.037(5) 0.032(5) 0.046(5) 0.011(4) 0.013(4) 0.000(4) C45 0.025(4) 0.031(5) 0.049(5) 0.007(4) 0.010(4) 0.003(3) C46 0.044(5) 0.057(6) 0.048(5) -0.018(4) 0.012(4) -0.009(4) C47 0.029(4) 0.039(5) 0.020(4) -0.006(4) 0.007(3) -0.007(3) C48 0.028(5) 0.049(5) 0.032(5) -0.010(4) 0.001(4) -0.008(4) C49 0.020(4) 0.053(5) 0.031(5) 0.000(4) 0.001(4) -0.005(4) C50 0.017(4) 0.037(4) 0.021(4) 0.003(3) 0.002(3) -0.003(3) C51 0.017(4) 0.032(4) 0.025(4) 0.002(4) 0.000(3) 0.004(3) C52 0.021(4) 0.028(4) 0.027(4) 0.003(3) 0.003(3) 0.003(3) C53 0.030(4) 0.039(5) 0.025(4) 0.007(4) 0.003(3) 0.004(4) C54 0.037(5) 0.038(5) 0.027(5) -0.008(4) -0.010(4) 0.001(4) C55 0.021(4) 0.034(4) 0.032(5) 0.003(4) -0.009(4) 0.002(3) C56 0.023(5) 0.062(6) 0.065(6) -0.013(5) -0.005(4) -0.011(4) B1 0.015(5) 0.041(6) 0.045(6) -0.003(5) 0.004(4) 0.003(4) B2 0.031(5) 0.044(6) 0.042(6) -0.014(5) 0.017(5) -0.003(5) N1 0.012(3) 0.045(4) 0.033(4) 0.004(3) 0.004(3) -0.003(3) N2 0.025(3) 0.038(4) 0.023(4) 0.003(3) 0.009(3) -0.002(3) N3 0.020(3) 0.038(4) 0.020(3) 0.004(3) 0.010(3) -0.003(3) N4 0.018(3) 0.027(3) 0.038(4) 0.009(3) -0.001(3) -0.006(3) N5 0.020(3) 0.035(4) 0.034(4) -0.007(3) 0.002(3) -0.001(3) N6 0.032(4) 0.029(3) 0.027(4) -0.002(3) 0.007(3) 0.002(3) N7 0.019(3) 0.038(4) 0.029(4) -0.001(3) 0.005(3) -0.004(3) N8 0.010(3) 0.036(4) 0.028(3) 0.000(3) 0.005(3) 0.000(3) F1 0.033(3) 0.070(3) 0.052(3) 0.000(2) 0.011(2) 0.012(2) F2 0.034(2) 0.054(3) 0.058(3) 0.011(2) 0.000(2) -0.021(2) F3 0.031(3) 0.081(3) 0.053(3) -0.014(3) 0.012(2) 0.017(2) F4 0.049(3) 0.068(3) 0.067(3) -0.002(3) 0.010(2) -0.036(3) Cu1 0.0155(5) 0.0416(6) 0.0269(5) -0.0008(4) 0.0040(4) -0.0015(4) C57 0.123(12) 0.077(9) 0.25(2) 0.017(11) 0.076(13) 0.033(8) Cl1 0.144(4) 0.128(3) 0.231(5) -0.003(3) -0.074(3) -0.018(3) Cl2 0.254(5) 0.095(3) 0.103(3) 0.003(2) -0.004(3) 0.024(3) C58 0.135(11) 0.092(9) 0.104(10) -0.005(8) 0.047(8) 0.005(8) Cl3 0.271(6) 0.161(4) 0.186(5) 0.083(4) -0.035(4) -0.053(4) Cl4 0.214(5) 0.259(6) 0.365(9) -0.185(6) -0.191(6) 0.127(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.510(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N2 1.363(8) . ? C2 C3 1.408(9) . ? C3 C4 1.370(9) . ? C3 H3 0.9500 . ? C4 C5 1.415(9) . ? C4 H4 0.9500 . ? C5 C6 1.404(9) . ? C5 N2 1.408(8) . ? C6 C7 1.411(9) . ? C6 C12 1.515(9) . ? C7 C8 1.404(9) . ? C7 N1 1.416(8) . ? C8 C9 1.391(9) . ? C8 H8 0.9500 . ? C9 C10 1.391(10) . ? C9 H9 0.9500 . ? C10 N1 1.375(8) . ? C10 C11 1.506(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.389(9) . ? C12 C17 1.402(9) . ? C13 C14 1.386(9) . ? C13 H13 0.9500 . ? C14 C15 1.394(9) . ? C14 H14 0.9500 . ? C15 C16 1.393(9) . ? C15 C23 1.491(8) . ? C16 C17 1.394(9) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.493(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.369(8) . ? C19 C20 1.425(9) . ? C20 C21 1.380(9) . ? C20 H20 0.9500 . ? C21 C22 1.433(9) . ? C21 H21 0.9500 . ? C22 C23 1.413(9) . ? C22 N3 1.420(8) . ? C23 C24 1.403(9) . ? C24 N4 1.414(8) . ? C24 C25 1.428(9) . ? C25 C26 1.382(9) . ? C25 H25 0.9500 . ? C26 C27 1.406(9) . ? C26 H26 0.9500 . ? C27 N4 1.364(8) . ? C27 C28 1.505(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.515(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.381(9) . ? C30 C31 1.398(10) . ? C31 C32 1.391(9) . ? C31 H31 0.9500 . ? C32 C33 1.410(10) . ? C32 H32 0.9500 . ? C33 C34 1.410(9) . ? C33 N5 1.416(8) . ? C34 C35 1.404(9) . ? C34 C40 1.501(9) . ? C35 N6 1.403(8) . ? C35 C36 1.412(9) . ? C36 C37 1.400(9) . ? C36 H36 0.9500 . ? C37 C38 1.405(9) . ? C37 H37 0.9500 . ? C38 N6 1.344(9) . ? C38 C39 1.505(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.388(9) . ? C40 C41 1.415(9) . ? C41 C42 1.381(8) . ? C41 H41 0.9500 . ? C42 C43 1.396(9) . ? C42 H42 0.9500 . ? C43 C44 1.403(9) . ? C43 C51 1.508(8) . ? C44 C45 1.385(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.482(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N7 1.362(8) . ? C47 C48 1.408(9) . ? C48 C49 1.387(9) . ? C48 H48 0.9500 . ? C49 C50 1.422(9) . ? C49 H49 0.9500 . ? C50 N7 1.408(8) . ? C50 C51 1.410(9) . ? C51 C52 1.404(9) . ? C52 N8 1.429(8) . ? C52 C53 1.432(9) . ? C53 C54 1.381(9) . ? C53 H53 0.9500 . ? C54 C55 1.417(9) . ? C54 H54 0.9500 . ? C55 N8 1.368(8) . ? C55 C56 1.503(9) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? B1 F2 1.395(9) . ? B1 F1 1.396(9) . ? B1 N2 1.545(9) . ? B1 N1 1.558(10) . ? B2 F4 1.396(9) . ? B2 F3 1.406(9) . ? B2 N5 1.549(11) . ? B2 N6 1.572(10) . ? N3 Cu1 1.949(5) . ? N4 Cu1 1.985(5) . ? N7 Cu1 1.962(5) . ? N8 Cu1 1.968(5) . ? C57 Cl1 1.635(15) . ? C57 Cl2 1.849(15) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl4 1.683(12) . ? C58 Cl3 1.694(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 109.4(6) . . ? N2 C2 C1 122.3(7) . . ? C3 C2 C1 128.3(7) . . ? C4 C3 C2 108.2(6) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? C3 C4 C5 107.0(6) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? C6 C5 N2 120.8(6) . . ? C6 C5 C4 130.7(6) . . ? N2 C5 C4 108.4(6) . . ? C5 C6 C7 120.8(6) . . ? C5 C6 C12 120.9(6) . . ? C7 C6 C12 118.3(6) . . ? C8 C7 C6 132.1(6) . . ? C8 C7 N1 108.2(6) . . ? C6 C7 N1 119.8(6) . . ? C9 C8 C7 107.8(6) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C8 C9 C10 107.2(6) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? N1 C10 C9 110.5(6) . . ? N1 C10 C11 121.5(7) . . ? C9 C10 C11 128.0(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.3(6) . . ? C13 C12 C6 121.4(6) . . ? C17 C12 C6 120.2(6) . . ? C14 C13 C12 121.1(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 117.5(6) . . ? C16 C15 C23 122.1(6) . . ? C14 C15 C23 120.4(6) . . ? C15 C16 C17 121.8(6) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C12 119.9(7) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 110.3(6) . . ? N3 C19 C18 122.0(6) . . ? C20 C19 C18 127.7(7) . . ? C21 C20 C19 108.2(6) . . ? C21 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? C20 C21 C22 106.1(6) . . ? C20 C21 H21 127.0 . . ? C22 C21 H21 127.0 . . ? C23 C22 N3 123.4(6) . . ? C23 C22 C21 126.8(6) . . ? N3 C22 C21 109.7(6) . . ? C24 C23 C22 126.8(6) . . ? C24 C23 C15 117.0(6) . . ? C22 C23 C15 116.2(6) . . ? C23 C24 N4 124.9(6) . . ? C23 C24 C25 127.0(6) . . ? N4 C24 C25 108.1(6) . . ? C26 C25 C24 107.0(6) . . ? C26 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? C25 C26 C27 107.9(6) . . ? C25 C26 H26 126.1 . . ? C27 C26 H26 126.1 . . ? N4 C27 C26 110.2(6) . . ? N4 C27 C28 122.7(6) . . ? C26 C27 C28 127.1(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C31 109.8(6) . . ? N5 C30 C29 121.3(7) . . ? C31 C30 C29 128.9(7) . . ? C32 C31 C30 107.7(7) . . ? C32 C31 H31 126.2 . . ? C30 C31 H31 126.2 . . ? C31 C32 C33 107.7(6) . . ? C31 C32 H32 126.1 . . ? C33 C32 H32 126.1 . . ? C34 C33 C32 131.7(6) . . ? C34 C33 N5 120.2(6) . . ? C32 C33 N5 108.1(6) . . ? C35 C34 C33 120.8(6) . . ? C35 C34 C40 119.6(6) . . ? C33 C34 C40 119.5(6) . . ? N6 C35 C34 121.2(6) . . ? N6 C35 C36 108.3(6) . . ? C34 C35 C36 130.3(6) . . ? C37 C36 C35 106.5(6) . . ? C37 C36 H36 126.7 . . ? C35 C36 H36 126.7 . . ? C36 C37 C38 107.4(6) . . ? C36 C37 H37 126.3 . . ? C38 C37 H37 126.3 . . ? N6 C38 C37 109.9(6) . . ? N6 C38 C39 122.7(7) . . ? C37 C38 C39 127.4(7) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 118.3(6) . . ? C45 C40 C34 122.2(6) . . ? C41 C40 C34 119.4(6) . . ? C42 C41 C40 119.7(6) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 122.3(6) . . ? C41 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C42 C43 C44 117.3(6) . . ? C42 C43 C51 121.2(6) . . ? C44 C43 C51 121.5(6) . . ? C45 C44 C43 121.1(7) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C40 121.2(6) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C48 110.2(6) . . ? N7 C47 C46 122.6(6) . . ? C48 C47 C46 127.2(6) . . ? C49 C48 C47 107.2(6) . . ? C49 C48 H48 126.4 . . ? C47 C48 H48 126.4 . . ? C48 C49 C50 107.5(6) . . ? C48 C49 H49 126.3 . . ? C50 C49 H49 126.3 . . ? N7 C50 C51 124.9(6) . . ? N7 C50 C49 107.9(6) . . ? C51 C50 C49 127.2(6) . . ? C52 C51 C50 126.0(6) . . ? C52 C51 C43 116.5(6) . . ? C50 C51 C43 117.5(6) . . ? C51 C52 N8 123.9(6) . . ? C51 C52 C53 127.9(6) . . ? N8 C52 C53 108.1(6) . . ? C54 C53 C52 107.9(6) . . ? C54 C53 H53 126.1 . . ? C52 C53 H53 126.1 . . ? C53 C54 C55 106.9(6) . . ? C53 C54 H54 126.6 . . ? C55 C54 H54 126.6 . . ? N8 C55 C54 111.4(6) . . ? N8 C55 C56 122.2(6) . . ? C54 C55 C56 126.4(6) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? F2 B1 F1 109.9(6) . . ? F2 B1 N2 110.9(6) . . ? F1 B1 N2 110.9(6) . . ? F2 B1 N1 109.8(6) . . ? F1 B1 N1 108.5(6) . . ? N2 B1 N1 106.8(5) . . ? F4 B2 F3 109.5(6) . . ? F4 B2 N5 111.8(7) . . ? F3 B2 N5 109.6(7) . . ? F4 B2 N6 109.8(7) . . ? F3 B2 N6 109.4(6) . . ? N5 B2 N6 106.6(6) . . ? C10 N1 C7 106.2(6) . . ? C10 N1 B1 127.8(6) . . ? C7 N1 B1 125.5(5) . . ? C2 N2 C5 106.9(5) . . ? C2 N2 B1 127.4(6) . . ? C5 N2 B1 125.5(6) . . ? C19 N3 C22 105.7(5) . . ? C19 N3 Cu1 128.4(4) . . ? C22 N3 Cu1 125.7(4) . . ? C27 N4 C24 106.8(5) . . ? C27 N4 Cu1 129.0(5) . . ? C24 N4 Cu1 123.7(4) . . ? C30 N5 C33 106.7(6) . . ? C30 N5 B2 127.4(6) . . ? C33 N5 B2 125.9(6) . . ? C38 N6 C35 107.9(6) . . ? C38 N6 B2 127.2(6) . . ? C35 N6 B2 124.9(6) . . ? C47 N7 C50 107.3(5) . . ? C47 N7 Cu1 127.2(4) . . ? C50 N7 Cu1 125.4(4) . . ? C55 N8 C52 105.8(5) . . ? C55 N8 Cu1 128.7(4) . . ? C52 N8 Cu1 125.4(4) . . ? N3 Cu1 N7 132.6(2) . . ? N3 Cu1 N8 105.1(2) . . ? N7 Cu1 N8 94.0(2) . . ? N3 Cu1 N4 94.8(2) . . ? N7 Cu1 N4 103.9(2) . . ? N8 Cu1 N4 131.9(2) . . ? Cl1 C57 Cl2 111.3(7) . . ? Cl1 C57 H57A 109.4 . . ? Cl2 C57 H57A 109.4 . . ? Cl1 C57 H57B 109.4 . . ? Cl2 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? Cl4 C58 Cl3 116.6(7) . . ? Cl4 C58 H58A 108.1 . . ? Cl3 C58 H58A 108.1 . . ? Cl4 C58 H58B 108.1 . . ? Cl3 C58 H58B 108.1 . . ? H58A C58 H58B 107.3 . . ? 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 N2 C2 C3 C4 0.6(8) . . . . ? C1 C2 C3 C4 -177.9(7) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C3 C4 C5 C6 177.6(7) . . . . ? C3 C4 C5 N2 -0.1(8) . . . . ? N2 C5 C6 C7 -4.3(10) . . . . ? C4 C5 C6 C7 178.3(7) . . . . ? N2 C5 C6 C12 175.7(6) . . . . ? C4 C5 C6 C12 -1.8(11) . . . . ? C5 C6 C7 C8 175.4(7) . . . . ? C12 C6 C7 C8 -4.6(11) . . . . ? C5 C6 C7 N1 -3.9(10) . . . . ? C12 C6 C7 N1 176.2(6) . . . . ? C6 C7 C8 C9 178.1(7) . . . . ? N1 C7 C8 C9 -2.6(8) . . . . ? C7 C8 C9 C10 1.6(9) . . . . ? C8 C9 C10 N1 0.0(9) . . . . ? C8 C9 C10 C11 179.9(7) . . . . ? C5 C6 C12 C13 127.9(7) . . . . ? C7 C6 C12 C13 -52.2(9) . . . . ? C5 C6 C12 C17 -53.0(9) . . . . ? C7 C6 C12 C17 127.0(7) . . . . ? C17 C12 C13 C14 -1.5(10) . . . . ? C6 C12 C13 C14 177.6(6) . . . . ? C12 C13 C14 C15 1.0(11) . . . . ? C13 C14 C15 C16 0.2(10) . . . . ? C13 C14 C15 C23 -178.3(6) . . . . ? C14 C15 C16 C17 -0.7(10) . . . . ? C23 C15 C16 C17 177.8(6) . . . . ? C15 C16 C17 C12 0.1(11) . . . . ? C13 C12 C17 C16 1.0(10) . . . . ? C6 C12 C17 C16 -178.2(6) . . . . ? N3 C19 C20 C21 -1.1(8) . . . . ? C18 C19 C20 C21 178.5(7) . . . . ? C19 C20 C21 C22 1.4(8) . . . . ? C20 C21 C22 C23 175.5(6) . . . . ? C20 C21 C22 N3 -1.3(7) . . . . ? N3 C22 C23 C24 7.4(11) . . . . ? C21 C22 C23 C24 -169.0(7) . . . . ? N3 C22 C23 C15 -174.0(6) . . . . ? C21 C22 C23 C15 9.6(10) . . . . ? C16 C15 C23 C24 72.3(8) . . . . ? C14 C15 C23 C24 -109.3(7) . . . . ? C16 C15 C23 C22 -106.5(7) . . . . ? C14 C15 C23 C22 72.0(8) . . . . ? C22 C23 C24 N4 -3.3(11) . . . . ? C15 C23 C24 N4 178.0(6) . . . . ? C22 C23 C24 C25 178.1(7) . . . . ? C15 C23 C24 C25 -0.5(10) . . . . ? C23 C24 C25 C26 179.5(7) . . . . ? N4 C24 C25 C26 0.7(8) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C25 C26 C27 N4 1.0(8) . . . . ? C25 C26 C27 C28 -178.4(7) . . . . ? N5 C30 C31 C32 -2.2(8) . . . . ? C29 C30 C31 C32 176.3(7) . . . . ? C30 C31 C32 C33 1.1(8) . . . . ? C31 C32 C33 C34 -179.2(7) . . . . ? C31 C32 C33 N5 0.3(8) . . . . ? C32 C33 C34 C35 -177.2(7) . . . . ? N5 C33 C34 C35 3.3(10) . . . . ? C32 C33 C34 C40 4.1(11) . . . . ? N5 C33 C34 C40 -175.4(6) . . . . ? C33 C34 C35 N6 -0.7(10) . . . . ? C40 C34 C35 N6 178.0(6) . . . . ? C33 C34 C35 C36 172.7(7) . . . . ? C40 C34 C35 C36 -8.6(11) . . . . ? N6 C35 C36 C37 -0.8(8) . . . . ? C34 C35 C36 C37 -174.9(7) . . . . ? C35 C36 C37 C38 -0.2(8) . . . . ? C36 C37 C38 N6 1.1(8) . . . . ? C36 C37 C38 C39 179.7(7) . . . . ? C35 C34 C40 C45 118.9(7) . . . . ? C33 C34 C40 C45 -62.4(9) . . . . ? C35 C34 C40 C41 -58.9(9) . . . . ? C33 C34 C40 C41 119.9(7) . . . . ? C45 C40 C41 C42 0.3(10) . . . . ? C34 C40 C41 C42 178.1(6) . . . . ? C40 C41 C42 C43 -1.4(10) . . . . ? C41 C42 C43 C44 1.8(10) . . . . ? C41 C42 C43 C51 -178.3(6) . . . . ? C42 C43 C44 C45 -1.2(10) . . . . ? C51 C43 C44 C45 178.9(6) . . . . ? C43 C44 C45 C40 0.2(11) . . . . ? C41 C40 C45 C44 0.3(10) . . . . ? C34 C40 C45 C44 -177.5(6) . . . . ? N7 C47 C48 C49 -0.2(8) . . . . ? C46 C47 C48 C49 179.6(7) . . . . ? C47 C48 C49 C50 0.3(8) . . . . ? C48 C49 C50 N7 -0.4(8) . . . . ? C48 C49 C50 C51 179.0(7) . . . . ? N7 C50 C51 C52 0.8(11) . . . . ? C49 C50 C51 C52 -178.5(7) . . . . ? N7 C50 C51 C43 179.6(6) . . . . ? C49 C50 C51 C43 0.3(10) . . . . ? C42 C43 C51 C52 108.0(7) . . . . ? C44 C43 C51 C52 -72.2(8) . . . . ? C42 C43 C51 C50 -71.0(8) . . . . ? C44 C43 C51 C50 108.9(8) . . . . ? C50 C51 C52 N8 -0.9(11) . . . . ? C43 C51 C52 N8 -179.7(6) . . . . ? C50 C51 C52 C53 -178.7(7) . . . . ? C43 C51 C52 C53 2.4(10) . . . . ? C51 C52 C53 C54 178.8(7) . . . . ? N8 C52 C53 C54 0.7(8) . . . . ? C52 C53 C54 C55 0.0(8) . . . . ? C53 C54 C55 N8 -0.7(8) . . . . ? C53 C54 C55 C56 -179.5(7) . . . . ? C9 C10 N1 C7 -1.6(8) . . . . ? C11 C10 N1 C7 178.6(6) . . . . ? C9 C10 N1 B1 170.8(7) . . . . ? C11 C10 N1 B1 -9.1(11) . . . . ? C8 C7 N1 C10 2.5(7) . . . . ? C6 C7 N1 C10 -178.0(6) . . . . ? C8 C7 N1 B1 -170.1(6) . . . . ? C6 C7 N1 B1 9.4(10) . . . . ? F2 B1 N1 C10 62.8(9) . . . . ? F1 B1 N1 C10 -57.3(9) . . . . ? N2 B1 N1 C10 -176.9(6) . . . . ? F2 B1 N1 C7 -126.2(7) . . . . ? F1 B1 N1 C7 113.7(7) . . . . ? N2 B1 N1 C7 -5.9(9) . . . . ? C3 C2 N2 C5 -0.6(8) . . . . ? C1 C2 N2 C5 178.0(6) . . . . ? C3 C2 N2 B1 174.1(6) . . . . ? C1 C2 N2 B1 -7.3(11) . . . . ? C6 C5 N2 C2 -177.5(6) . . . . ? C4 C5 N2 C2 0.5(7) . . . . ? C6 C5 N2 B1 7.6(10) . . . . ? C4 C5 N2 B1 -174.4(6) . . . . ? F2 B1 N2 C2 -56.7(9) . . . . ? F1 B1 N2 C2 65.6(9) . . . . ? N1 B1 N2 C2 -176.4(6) . . . . ? F2 B1 N2 C5 117.1(7) . . . . ? F1 B1 N2 C5 -120.6(7) . . . . ? N1 B1 N2 C5 -2.6(9) . . . . ? C20 C19 N3 C22 0.2(8) . . . . ? C18 C19 N3 C22 -179.4(7) . . . . ? C20 C19 N3 Cu1 -174.1(5) . . . . ? C18 C19 N3 Cu1 6.2(10) . . . . ? C23 C22 N3 C19 -176.3(6) . . . . ? C21 C22 N3 C19 0.7(7) . . . . ? C23 C22 N3 Cu1 -1.7(9) . . . . ? C21 C22 N3 Cu1 175.2(4) . . . . ? C26 C27 N4 C24 -0.5(8) . . . . ? C28 C27 N4 C24 179.0(6) . . . . ? C26 C27 N4 Cu1 -173.2(5) . . . . ? C28 C27 N4 Cu1 6.3(10) . . . . ? C23 C24 N4 C27 -178.9(6) . . . . ? C25 C24 N4 C27 -0.1(7) . . . . ? C23 C24 N4 Cu1 -5.8(9) . . . . ? C25 C24 N4 Cu1 173.0(4) . . . . ? C31 C30 N5 C33 2.3(8) . . . . ? C29 C30 N5 C33 -176.3(6) . . . . ? C31 C30 N5 B2 -180.0(7) . . . . ? C29 C30 N5 B2 1.4(11) . . . . ? C34 C33 N5 C30 178.0(6) . . . . ? C32 C33 N5 C30 -1.6(7) . . . . ? C34 C33 N5 B2 0.2(10) . . . . ? C32 C33 N5 B2 -179.3(6) . . . . ? F4 B2 N5 C30 -62.4(9) . . . . ? F3 B2 N5 C30 59.3(9) . . . . ? N6 B2 N5 C30 177.6(6) . . . . ? F4 B2 N5 C33 114.9(7) . . . . ? F3 B2 N5 C33 -123.5(7) . . . . ? N6 B2 N5 C33 -5.2(9) . . . . ? C37 C38 N6 C35 -1.6(8) . . . . ? C39 C38 N6 C35 179.7(6) . . . . ? C37 C38 N6 B2 -179.8(6) . . . . ? C39 C38 N6 B2 1.4(11) . . . . ? C34 C35 N6 C38 176.2(6) . . . . ? C36 C35 N6 C38 1.4(7) . . . . ? C34 C35 N6 B2 -5.5(10) . . . . ? C36 C35 N6 B2 179.8(6) . . . . ? F4 B2 N6 C38 64.4(9) . . . . ? F3 B2 N6 C38 -55.8(10) . . . . ? N5 B2 N6 C38 -174.2(6) . . . . ? F4 B2 N6 C35 -113.6(7) . . . . ? F3 B2 N6 C35 126.2(7) . . . . ? N5 B2 N6 C35 7.8(9) . . . . ? C48 C47 N7 C50 -0.1(8) . . . . ? C46 C47 N7 C50 -179.8(7) . . . . ? C48 C47 N7 Cu1 177.2(5) . . . . ? C46 C47 N7 Cu1 -2.5(10) . . . . ? C51 C50 N7 C47 -179.2(6) . . . . ? C49 C50 N7 C47 0.3(7) . . . . ? C51 C50 N7 Cu1 3.5(9) . . . . ? C49 C50 N7 Cu1 -177.1(4) . . . . ? C54 C55 N8 C52 1.1(7) . . . . ? C56 C55 N8 C52 180.0(6) . . . . ? C54 C55 N8 Cu1 -174.7(4) . . . . ? C56 C55 N8 Cu1 4.2(9) . . . . ? C51 C52 N8 C55 -179.3(6) . . . . ? C53 C52 N8 C55 -1.1(7) . . . . ? C51 C52 N8 Cu1 -3.3(9) . . . . ? C53 C52 N8 Cu1 174.9(4) . . . . ? C19 N3 Cu1 N7 54.7(7) . . . . ? C22 N3 Cu1 N7 -118.6(5) . . . . ? C19 N3 Cu1 N8 -55.7(6) . . . . ? C22 N3 Cu1 N8 131.0(5) . . . . ? C19 N3 Cu1 N4 168.5(6) . . . . ? C22 N3 Cu1 N4 -4.8(5) . . . . ? C47 N7 Cu1 N3 62.8(7) . . . . ? C50 N7 Cu1 N3 -120.4(5) . . . . ? C47 N7 Cu1 N8 177.6(6) . . . . ? C50 N7 Cu1 N8 -5.6(5) . . . . ? C47 N7 Cu1 N4 -47.4(6) . . . . ? C50 N7 Cu1 N4 129.4(5) . . . . ? C55 N8 Cu1 N3 -43.2(6) . . . . ? C52 N8 Cu1 N3 141.8(5) . . . . ? C55 N8 Cu1 N7 -179.5(6) . . . . ? C52 N8 Cu1 N7 5.5(5) . . . . ? C55 N8 Cu1 N4 67.8(6) . . . . ? C52 N8 Cu1 N4 -107.2(5) . . . . ? C27 N4 Cu1 N3 179.8(6) . . . . ? C24 N4 Cu1 N3 8.3(5) . . . . ? C27 N4 Cu1 N7 -44.0(6) . . . . ? C24 N4 Cu1 N7 144.4(5) . . . . ? C27 N4 Cu1 N8 64.6(6) . . . . ? C24 N4 Cu1 N8 -107.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 22.53 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.101 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.083 #===End data_compound12 _database_code_depnum_ccdc_archive 'CCDC 684026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 B2 Cl4 F4 N8 Ni' _chemical_formula_weight 1103.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 22.249(2) _cell_length_b 8.5705(7) _cell_length_c 27.197(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5186.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1987 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 21.06 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14428 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 22.43 _reflns_number_total 3328 _reflns_number_gt 2133 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+12.7278P] 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 3328 _refine_ls_number_parameters 372 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1295 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4816(3) 0.1255(8) 0.4532(3) 0.059(2) Uani 1 1 d . . . H1A H 0.4882 0.0180 0.4421 0.089 Uiso 1 1 calc R . . H1B H 0.5167 0.1610 0.4719 0.089 Uiso 1 1 calc R . . H1C H 0.4757 0.1934 0.4247 0.089 Uiso 1 1 calc R . . C2 C 0.4273(3) 0.1315(7) 0.4853(2) 0.0377(17) Uani 1 1 d . . . C3 C 0.4195(3) 0.2052(7) 0.5305(2) 0.0447(18) Uani 1 1 d . . . H3 H 0.4494 0.2620 0.5479 0.054 Uiso 1 1 calc R . . C4 C 0.3615(3) 0.1815(7) 0.5456(2) 0.0339(16) Uani 1 1 d . . . H4 H 0.3438 0.2189 0.5751 0.041 Uiso 1 1 calc R . . C5 C 0.3331(3) 0.0919(6) 0.50922(19) 0.0235(14) Uani 1 1 d . . . C6 C 0.2732(2) 0.0464(6) 0.50375(19) 0.0214(14) Uani 1 1 d . . . C7 C 0.2546(3) -0.0302(6) 0.46146(18) 0.0205(14) Uani 1 1 d . . . C8 C 0.1975(3) -0.0856(6) 0.4470(2) 0.0299(16) Uani 1 1 d . . . H8 H 0.1608 -0.0733 0.4644 0.036 Uiso 1 1 calc R . . C9 C 0.2052(3) -0.1606(7) 0.4029(2) 0.0414(18) Uani 1 1 d . . . H9 H 0.1744 -0.2081 0.3840 0.050 Uiso 1 1 calc R . . C10 C 0.2657(3) -0.1554(7) 0.3907(2) 0.0361(17) Uani 1 1 d . . . C11 C 0.2963(3) -0.2302(7) 0.3479(2) 0.054(2) Uani 1 1 d . . . H11A H 0.3341 -0.1757 0.3411 0.081 Uiso 1 1 calc R . . H11B H 0.2702 -0.2242 0.3190 0.081 Uiso 1 1 calc R . . H11C H 0.3047 -0.3398 0.3555 0.081 Uiso 1 1 calc R . . C12 C 0.2302(3) 0.0812(6) 0.54400(19) 0.0227(15) Uani 1 1 d . . . C13 C 0.2408(3) 0.0285(6) 0.59186(19) 0.0291(16) Uani 1 1 d . . . H13 H 0.2767 -0.0276 0.5989 0.035 Uiso 1 1 calc R . . C14 C 0.2002(3) 0.0565(7) 0.62904(19) 0.0299(16) Uani 1 1 d . . . H14 H 0.2082 0.0193 0.6613 0.036 Uiso 1 1 calc R . . C15 C 0.1474(3) 0.1390(6) 0.6198(2) 0.0248(15) Uani 1 1 d . . . C16 C 0.1375(2) 0.1949(6) 0.57250(18) 0.0231(14) Uani 1 1 d . . . H16 H 0.1024 0.2544 0.5658 0.028 Uiso 1 1 calc R . . C17 C 0.1776(2) 0.1657(6) 0.53527(19) 0.0238(14) Uani 1 1 d . . . H17 H 0.1695 0.2035 0.5031 0.029 Uiso 1 1 calc R . . C18 C -0.0516(3) 0.0559(7) 0.6633(2) 0.0368(17) Uani 1 1 d . . . H18 H -0.0900 0.0474 0.6783 0.044 Uiso 1 1 calc R . . C19 C -0.0366(3) -0.0110(7) 0.6181(2) 0.0448(19) Uani 1 1 d . . . H19 H -0.0624 -0.0691 0.5971 0.054 Uiso 1 1 calc R . . C20 C 0.0221(3) 0.0234(7) 0.6099(2) 0.0337(17) Uani 1 1 d . . . H20 H 0.0450 -0.0073 0.5821 0.040 Uiso 1 1 calc R . . C21 C 0.0433(3) 0.1131(6) 0.6502(2) 0.0227(15) Uani 1 1 d . . . C22 C 0.1016(3) 0.1624(6) 0.65929(18) 0.0214(14) Uani 1 1 d . . . C23 C 0.1203(3) 0.2267(6) 0.70365(19) 0.0230(14) Uani 1 1 d . . . C24 C 0.1743(3) 0.3057(7) 0.7148(2) 0.0331(15) Uani 1 1 d . . . H24 H 0.2082 0.3146 0.6938 0.040 Uiso 1 1 calc R . . C25 C 0.1695(3) 0.3669(7) 0.7609(2) 0.0384(17) Uani 1 1 d . . . H25 H 0.1990 0.4259 0.7780 0.046 Uiso 1 1 calc R . . C26 C 0.1126(3) 0.3257(7) 0.7780(2) 0.0351(16) Uani 1 1 d . . . H26 H 0.0970 0.3548 0.8092 0.042 Uiso 1 1 calc R . . B1 B 0.3643(3) -0.0460(8) 0.4280(2) 0.0321(19) Uani 1 1 d . . . N1 N 0.3753(2) 0.0616(5) 0.47245(15) 0.0227(12) Uani 1 1 d . . . N2 N 0.2956(2) -0.0747(5) 0.42545(15) 0.0245(12) Uani 1 1 d . . . N3 N -0.0051(2) 0.1335(5) 0.68297(15) 0.0285(12) Uani 1 1 d . . . N4 N 0.08268(19) 0.2402(5) 0.74503(17) 0.0266(12) Uani 1 1 d . . . F1 F 0.38363(15) 0.0266(4) 0.38499(11) 0.0469(10) Uani 1 1 d . . . F2 F 0.39452(15) -0.1854(4) 0.43431(11) 0.0426(9) Uani 1 1 d . . . Ni1 Ni 0.0000 0.18946(12) 0.7500 0.0265(3) Uani 1 2 d S . . C27A C 0.5813(10) 0.881(3) 0.3009(13) 0.132(9) Uiso 0.359(13) 1 d PD A 1 H27A H 0.5870 0.9696 0.2781 0.158 Uiso 0.359(13) 1 calc PR A 1 H27B H 0.6143 0.8838 0.3254 0.158 Uiso 0.359(13) 1 calc PR A 1 Cl1A Cl 0.5137(5) 0.9011(13) 0.3307(3) 0.073(4) Uani 0.359(13) 1 d PD A 1 Cl2A Cl 0.5853(7) 0.7119(17) 0.2690(6) 0.122(6) Uani 0.359(13) 1 d PD A 1 C27B C 0.5671(6) 0.782(3) 0.2916(10) 0.132(9) Uiso 0.483(15) 1 d PD B 2 H27C H 0.5585 0.8121 0.2572 0.158 Uiso 0.483(15) 1 calc PR B 2 H27D H 0.5449 0.6844 0.2988 0.158 Uiso 0.483(15) 1 calc PR B 2 Cl1B Cl 0.6422(4) 0.7500(11) 0.2982(5) 0.167(7) Uani 0.483(15) 1 d PD B 2 Cl2B Cl 0.5429(6) 0.9247(15) 0.3299(6) 0.199(9) Uani 0.483(15) 1 d PD B 2 C27C C 0.610(3) 0.772(12) 0.3234(15) 0.132(9) Uiso 0.159(16) 1 d PD C 3 H27E H 0.6190 0.6937 0.3492 0.158 Uiso 0.159(16) 1 calc PR C 3 H27F H 0.6356 0.8646 0.3296 0.158 Uiso 0.159(16) 1 calc PR C 3 Cl1C Cl 0.627(3) 0.696(4) 0.2674(9) 0.16(2) Uani 0.159(16) 1 d PD C 3 Cl2C Cl 0.537(3) 0.825(4) 0.3274(14) 0.30(3) Uani 0.159(16) 1 d PD C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(5) 0.060(5) 0.094(6) 0.014(4) 0.021(4) 0.000(4) C2 0.019(4) 0.024(4) 0.071(5) 0.004(3) 0.009(4) -0.002(3) C3 0.025(5) 0.036(4) 0.073(5) -0.015(4) -0.004(4) -0.003(4) C4 0.019(4) 0.035(4) 0.048(4) -0.014(3) -0.002(3) 0.007(3) C5 0.023(4) 0.021(3) 0.026(3) -0.005(3) 0.004(3) 0.002(3) C6 0.023(4) 0.016(3) 0.025(3) 0.002(3) 0.007(3) 0.000(3) C7 0.028(4) 0.017(3) 0.017(3) 0.001(3) 0.000(3) -0.005(3) C8 0.033(5) 0.029(4) 0.028(4) 0.015(3) -0.004(3) -0.006(3) C9 0.059(6) 0.037(4) 0.028(4) 0.004(3) -0.018(4) -0.016(4) C10 0.058(5) 0.022(4) 0.028(4) 0.002(3) 0.000(4) -0.004(4) C11 0.090(6) 0.042(4) 0.031(4) -0.008(3) 0.004(4) 0.005(4) C12 0.019(4) 0.025(3) 0.024(3) 0.002(3) 0.004(3) 0.004(3) C13 0.023(4) 0.037(4) 0.028(3) 0.001(3) 0.002(3) 0.014(3) C14 0.028(4) 0.043(4) 0.019(3) 0.002(3) 0.003(3) 0.012(3) C15 0.019(4) 0.026(4) 0.030(4) -0.002(3) 0.009(3) -0.002(3) C16 0.013(4) 0.028(3) 0.028(3) 0.004(3) 0.003(3) -0.001(3) C17 0.022(4) 0.030(4) 0.020(3) 0.008(3) 0.001(3) 0.000(3) C18 0.031(5) 0.034(4) 0.045(4) -0.005(3) 0.012(4) -0.016(4) C19 0.042(5) 0.048(4) 0.045(4) -0.021(4) 0.006(4) -0.023(4) C20 0.033(5) 0.032(4) 0.036(4) -0.013(3) 0.010(3) -0.008(3) C21 0.022(4) 0.015(3) 0.031(4) -0.001(3) 0.005(3) 0.001(3) C22 0.023(4) 0.017(3) 0.024(3) -0.001(3) 0.005(3) 0.006(3) C23 0.013(4) 0.028(4) 0.027(3) -0.002(3) 0.006(3) 0.001(3) C24 0.025(4) 0.039(4) 0.035(4) -0.001(3) 0.009(3) 0.002(4) C25 0.026(4) 0.054(4) 0.035(4) -0.009(3) -0.002(3) -0.009(3) C26 0.042(5) 0.036(4) 0.028(3) -0.015(3) -0.003(3) -0.003(4) B1 0.042(6) 0.030(5) 0.025(4) 0.002(3) 0.017(4) -0.001(4) N1 0.022(3) 0.012(3) 0.034(3) 0.000(2) 0.011(3) 0.003(2) N2 0.037(4) 0.018(3) 0.019(3) -0.004(2) 0.005(3) -0.003(3) N3 0.023(3) 0.028(3) 0.034(3) -0.003(2) 0.009(3) -0.002(3) N4 0.023(3) 0.031(3) 0.026(3) -0.003(2) 0.010(3) -0.003(2) F1 0.055(3) 0.049(2) 0.037(2) 0.0099(18) 0.0262(19) 0.003(2) F2 0.052(2) 0.0253(19) 0.051(2) -0.0006(17) 0.0171(19) 0.019(2) Ni1 0.0230(7) 0.0300(6) 0.0264(6) 0.000 0.0081(6) 0.000 Cl1A 0.091(8) 0.045(8) 0.083(6) -0.002(5) -0.014(5) 0.026(6) Cl2A 0.148(12) 0.069(6) 0.149(11) -0.020(5) 0.040(9) -0.003(8) Cl1B 0.123(8) 0.102(7) 0.277(19) 0.103(9) -0.002(8) 0.029(6) Cl2B 0.29(2) 0.071(7) 0.242(12) -0.007(7) 0.115(11) -0.065(9) Cl1C 0.33(7) 0.086(19) 0.050(14) 0.009(12) 0.01(2) -0.07(3) Cl2C 0.61(9) 0.037(19) 0.24(3) 0.03(2) 0.12(5) 0.08(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.491(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.348(7) . ? C2 C3 1.393(8) . ? C3 C4 1.369(8) . ? C3 H3 0.9500 . ? C4 C5 1.402(7) . ? C4 H4 0.9500 . ? C5 C6 1.395(7) . ? C5 N1 1.396(6) . ? C6 C7 1.388(7) . ? C6 C12 1.484(7) . ? C7 N2 1.392(6) . ? C7 C8 1.411(8) . ? C8 C9 1.370(8) . ? C8 H8 0.9500 . ? C9 C10 1.388(8) . ? C9 H9 0.9500 . ? C10 N2 1.347(7) . ? C10 C11 1.493(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.397(7) . ? C12 C13 1.398(7) . ? C13 C14 1.378(7) . ? C13 H13 0.9500 . ? C14 C15 1.394(7) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C15 C22 1.494(7) . ? C16 C17 1.373(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 N3 1.342(7) . ? C18 C19 1.397(7) . ? C18 H18 0.9500 . ? C19 C20 1.356(7) . ? C19 H19 0.9500 . ? C20 C21 1.419(7) . ? C20 H20 0.9500 . ? C21 C22 1.386(7) . ? C21 N3 1.409(7) . ? C22 C23 1.390(7) . ? C23 N4 1.407(6) . ? C23 C24 1.412(7) . ? C24 C25 1.363(7) . ? C24 H24 0.9500 . ? C25 C26 1.394(8) . ? C25 H25 0.9500 . ? C26 N4 1.335(6) . ? C26 H26 0.9500 . ? B1 F2 1.381(7) . ? B1 F1 1.393(7) . ? B1 N1 1.540(8) . ? B1 N2 1.551(8) . ? N3 Ni1 1.888(4) . ? N4 Ni1 1.895(4) . ? Ni1 N3 1.888(4) 4_556 ? Ni1 N4 1.895(4) 4_556 ? C27A Cl2A 1.691(12) . ? C27A Cl1A 1.719(9) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C27B Cl2B 1.693(11) . ? C27B Cl1B 1.702(11) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C27C Cl2C 1.698(12) . ? C27C Cl1C 1.700(12) . ? C27C H27E 0.9900 . ? C27C H27F 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.9(6) . . ? N1 C2 C1 121.9(6) . . ? C3 C2 C1 129.2(6) . . ? C4 C3 C2 108.3(6) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? C3 C4 C5 107.2(5) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? C6 C5 N1 120.9(5) . . ? C6 C5 C4 131.1(5) . . ? N1 C5 C4 107.7(5) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 C12 120.8(5) . . ? C5 C6 C12 118.7(5) . . ? C6 C7 N2 121.1(5) . . ? C6 C7 C8 131.3(5) . . ? N2 C7 C8 107.6(5) . . ? C9 C8 C7 106.8(6) . . ? C9 C8 H8 126.6 . . ? C7 C8 H8 126.6 . . ? C8 C9 C10 108.5(6) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? N2 C10 C9 109.0(5) . . ? N2 C10 C11 122.9(6) . . ? C9 C10 C11 128.0(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 117.9(5) . . ? C17 C12 C6 121.3(5) . . ? C13 C12 C6 120.8(5) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 118.4(5) . . ? C16 C15 C22 120.7(5) . . ? C14 C15 C22 120.8(5) . . ? C17 C16 C15 121.1(5) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C12 120.9(5) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? N3 C18 C19 111.7(6) . . ? N3 C18 H18 124.1 . . ? C19 C18 H18 124.1 . . ? C20 C19 C18 106.5(6) . . ? C20 C19 H19 126.7 . . ? C18 C19 H19 126.7 . . ? C19 C20 C21 108.2(6) . . ? C19 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? C22 C21 N3 124.4(5) . . ? C22 C21 C20 127.9(5) . . ? N3 C21 C20 107.5(5) . . ? C21 C22 C23 123.7(5) . . ? C21 C22 C15 117.9(5) . . ? C23 C22 C15 118.3(5) . . ? C22 C23 N4 123.3(5) . . ? C22 C23 C24 129.1(5) . . ? N4 C23 C24 107.2(5) . . ? C25 C24 C23 108.3(5) . . ? C25 C24 H24 125.8 . . ? C23 C24 H24 125.8 . . ? C24 C25 C26 106.3(6) . . ? C24 C25 H25 126.9 . . ? C26 C25 H25 126.9 . . ? N4 C26 C25 111.6(5) . . ? N4 C26 H26 124.2 . . ? C25 C26 H26 124.2 . . ? F2 B1 F1 109.9(5) . . ? F2 B1 N1 110.1(5) . . ? F1 B1 N1 110.0(5) . . ? F2 B1 N2 110.4(5) . . ? F1 B1 N2 109.7(5) . . ? N1 B1 N2 106.6(5) . . ? C2 N1 C5 108.0(5) . . ? C2 N1 B1 127.3(5) . . ? C5 N1 B1 124.5(5) . . ? C10 N2 C7 108.1(5) . . ? C10 N2 B1 126.8(5) . . ? C7 N2 B1 124.9(5) . . ? C18 N3 C21 106.0(4) . . ? C18 N3 Ni1 123.8(4) . . ? C21 N3 Ni1 126.6(4) . . ? C26 N4 C23 106.6(4) . . ? C26 N4 Ni1 124.2(4) . . ? C23 N4 Ni1 128.0(4) . . ? N3 Ni1 N3 150.6(3) 4_556 . ? N3 Ni1 N4 94.0(2) 4_556 . ? N3 Ni1 N4 92.7(2) . . ? N3 Ni1 N4 92.7(2) 4_556 4_556 ? N3 Ni1 N4 94.0(2) . 4_556 ? N4 Ni1 N4 153.5(2) . 4_556 ? Cl2A C27A Cl1A 112.0(10) . . ? Cl2A C27A H27A 109.2 . . ? Cl1A C27A H27A 109.2 . . ? Cl2A C27A H27B 109.2 . . ? Cl1A C27A H27B 109.2 . . ? H27A C27A H27B 107.9 . . ? Cl2B C27B Cl1B 111.4(11) . . ? Cl2B C27B H27C 109.3 . . ? Cl1B C27B H27C 109.4 . . ? Cl2B C27B H27D 109.4 . . ? Cl1B C27B H27D 109.4 . . ? H27C C27B H27D 108.0 . . ? Cl2C C27C Cl1C 111.7(12) . . ? Cl2C C27C H27E 109.3 . . ? Cl1C C27C H27E 109.3 . . ? Cl2C C27C H27F 109.3 . . ? Cl1C C27C H27F 109.3 . . ? H27E C27C H27F 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -0.7(7) . . . . ? C1 C2 C3 C4 178.7(6) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 -173.6(6) . . . . ? C3 C4 C5 N1 0.4(6) . . . . ? N1 C5 C6 C7 0.1(8) . . . . ? C4 C5 C6 C7 173.4(6) . . . . ? N1 C5 C6 C12 179.9(4) . . . . ? C4 C5 C6 C12 -6.8(9) . . . . ? C5 C6 C7 N2 5.2(8) . . . . ? C12 C6 C7 N2 -174.6(4) . . . . ? C5 C6 C7 C8 -179.1(5) . . . . ? C12 C6 C7 C8 1.1(9) . . . . ? C6 C7 C8 C9 -176.4(6) . . . . ? N2 C7 C8 C9 -0.4(6) . . . . ? C7 C8 C9 C10 1.3(6) . . . . ? C8 C9 C10 N2 -1.8(7) . . . . ? C8 C9 C10 C11 175.6(6) . . . . ? C7 C6 C12 C17 -55.8(7) . . . . ? C5 C6 C12 C17 124.4(6) . . . . ? C7 C6 C12 C13 123.4(6) . . . . ? C5 C6 C12 C13 -56.4(7) . . . . ? C17 C12 C13 C14 1.2(8) . . . . ? C6 C12 C13 C14 -178.1(5) . . . . ? C12 C13 C14 C15 -0.2(9) . . . . ? C13 C14 C15 C16 -1.4(8) . . . . ? C13 C14 C15 C22 176.7(5) . . . . ? C14 C15 C16 C17 2.1(8) . . . . ? C22 C15 C16 C17 -176.0(5) . . . . ? C15 C16 C17 C12 -1.2(8) . . . . ? C13 C12 C17 C16 -0.5(8) . . . . ? C6 C12 C17 C16 178.8(5) . . . . ? N3 C18 C19 C20 1.5(8) . . . . ? C18 C19 C20 C21 -0.5(7) . . . . ? C19 C20 C21 C22 174.1(6) . . . . ? C19 C20 C21 N3 -0.7(7) . . . . ? N3 C21 C22 C23 5.5(8) . . . . ? C20 C21 C22 C23 -168.5(5) . . . . ? N3 C21 C22 C15 -177.1(5) . . . . ? C20 C21 C22 C15 9.0(8) . . . . ? C16 C15 C22 C21 53.9(7) . . . . ? C14 C15 C22 C21 -124.2(6) . . . . ? C16 C15 C22 C23 -128.5(6) . . . . ? C14 C15 C22 C23 53.5(7) . . . . ? C21 C22 C23 N4 3.9(8) . . . . ? C15 C22 C23 N4 -173.6(5) . . . . ? C21 C22 C23 C24 -167.6(6) . . . . ? C15 C22 C23 C24 14.9(9) . . . . ? C22 C23 C24 C25 171.7(6) . . . . ? N4 C23 C24 C25 -0.9(6) . . . . ? C23 C24 C25 C26 0.0(7) . . . . ? C24 C25 C26 N4 1.0(7) . . . . ? C3 C2 N1 C5 0.9(6) . . . . ? C1 C2 N1 C5 -178.5(5) . . . . ? C3 C2 N1 B1 -173.8(5) . . . . ? C1 C2 N1 B1 6.7(9) . . . . ? C6 C5 N1 C2 173.9(5) . . . . ? C4 C5 N1 C2 -0.8(6) . . . . ? C6 C5 N1 B1 -11.2(8) . . . . ? C4 C5 N1 B1 174.1(5) . . . . ? F2 B1 N1 C2 68.6(7) . . . . ? F1 B1 N1 C2 -52.7(8) . . . . ? N2 B1 N1 C2 -171.6(5) . . . . ? F2 B1 N1 C5 -105.3(6) . . . . ? F1 B1 N1 C5 133.4(5) . . . . ? N2 B1 N1 C5 14.5(7) . . . . ? C9 C10 N2 C7 1.6(6) . . . . ? C11 C10 N2 C7 -176.0(5) . . . . ? C9 C10 N2 B1 177.0(5) . . . . ? C11 C10 N2 B1 -0.5(9) . . . . ? C6 C7 N2 C10 175.8(5) . . . . ? C8 C7 N2 C10 -0.8(6) . . . . ? C6 C7 N2 B1 0.2(8) . . . . ? C8 C7 N2 B1 -176.3(5) . . . . ? F2 B1 N2 C10 -64.2(7) . . . . ? F1 B1 N2 C10 57.0(7) . . . . ? N1 B1 N2 C10 176.2(5) . . . . ? F2 B1 N2 C7 110.5(5) . . . . ? F1 B1 N2 C7 -128.2(5) . . . . ? N1 B1 N2 C7 -9.1(7) . . . . ? C19 C18 N3 C21 -1.9(7) . . . . ? C19 C18 N3 Ni1 -161.9(4) . . . . ? C22 C21 N3 C18 -173.5(5) . . . . ? C20 C21 N3 C18 1.6(6) . . . . ? C22 C21 N3 Ni1 -14.2(7) . . . . ? C20 C21 N3 Ni1 160.8(4) . . . . ? C25 C26 N4 C23 -1.6(7) . . . . ? C25 C26 N4 Ni1 -169.6(4) . . . . ? C22 C23 N4 C26 -171.6(5) . . . . ? C24 C23 N4 C26 1.5(6) . . . . ? C22 C23 N4 Ni1 -4.1(7) . . . . ? C24 C23 N4 Ni1 168.9(4) . . . . ? C18 N3 Ni1 N3 63.8(4) . . . 4_556 ? C21 N3 Ni1 N3 -92.0(4) . . . 4_556 ? C18 N3 Ni1 N4 166.8(5) . . . . ? C21 N3 Ni1 N4 11.0(4) . . . . ? C18 N3 Ni1 N4 -38.9(5) . . . 4_556 ? C21 N3 Ni1 N4 165.3(4) . . . 4_556 ? C26 N4 Ni1 N3 -45.6(5) . . . 4_556 ? C23 N4 Ni1 N3 148.9(4) . . . 4_556 ? C26 N4 Ni1 N3 163.0(4) . . . . ? C23 N4 Ni1 N3 -2.4(4) . . . . ? C26 N4 Ni1 N4 58.5(4) . . . 4_556 ? C23 N4 Ni1 N4 -106.9(4) . . . 4_556 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 22.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.502 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.066 #===End data_compound13 _database_code_depnum_ccdc_archive 'CCDC 684027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 B2 Cl6 F4 N8 Ni' _chemical_formula_weight 1228.09 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8400(10) _cell_length_b 14.501(2) _cell_length_c 19.830(2) _cell_angle_alpha 109.761(6) _cell_angle_beta 104.839(6) _cell_angle_gamma 93.027(6) _cell_volume 2802.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6405 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 24.34 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9772 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.1081 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.23 _reflns_number_total 9772 _reflns_number_gt 5802 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1325P)^2^+0.4578P] 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 9772 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2302 _refine_ls_wR_factor_gt 0.2040 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2605(7) 0.4812(4) -0.1183(3) 0.0419(16) Uani 1 1 d . . . H1A H 0.3167 0.4636 -0.1509 0.063 Uiso 1 1 calc R . . H1B H 0.2570 0.5525 -0.1029 0.063 Uiso 1 1 calc R . . H1C H 0.1734 0.4442 -0.1456 0.063 Uiso 1 1 calc R . . C2 C 0.3136(6) 0.4553(4) -0.0498(3) 0.0326(14) Uani 1 1 d . . . C3 C 0.3354(6) 0.5148(4) 0.0242(3) 0.0347(15) Uani 1 1 d . . . H3 H 0.3187 0.5810 0.0425 0.042 Uiso 1 1 calc R . . C4 C 0.3859(6) 0.4602(4) 0.0663(3) 0.0313(14) Uani 1 1 d . . . H4 H 0.4115 0.4821 0.1195 0.038 Uiso 1 1 calc R . . C5 C 0.3928(6) 0.3655(4) 0.0167(3) 0.0238(12) Uani 1 1 d . . . C6 C 0.4395(5) 0.2839(4) 0.0303(3) 0.0235(12) Uani 1 1 d . . . C7 C 0.4436(6) 0.1995(4) -0.0286(3) 0.0267(13) Uani 1 1 d . . . C8 C 0.4833(6) 0.1077(4) -0.0295(3) 0.0331(15) Uani 1 1 d . . . H8 H 0.5192 0.0911 0.0131 0.040 Uiso 1 1 calc R . . C9 C 0.4602(6) 0.0466(4) -0.1037(3) 0.0328(14) Uani 1 1 d . . . H9 H 0.4784 -0.0193 -0.1211 0.039 Uiso 1 1 calc R . . C10 C 0.4052(6) 0.0994(4) -0.1485(3) 0.0287(13) Uani 1 1 d . . . C11 C 0.3586(7) 0.0641(4) -0.2313(3) 0.0391(16) Uani 1 1 d . . . H11A H 0.2647 0.0618 -0.2474 0.059 Uiso 1 1 calc R . . H11B H 0.3799 -0.0025 -0.2525 0.059 Uiso 1 1 calc R . . H11C H 0.4002 0.1095 -0.2488 0.059 Uiso 1 1 calc R . . C12 C 0.4778(5) 0.2845(4) 0.1079(3) 0.0236(12) Uani 1 1 d . . . C13 C 0.3901(6) 0.2978(4) 0.1487(3) 0.0276(13) Uani 1 1 d . . . H13 H 0.3062 0.3098 0.1277 0.033 Uiso 1 1 calc R . . C14 C 0.4232(6) 0.2938(4) 0.2204(3) 0.0274(13) Uani 1 1 d . . . H14 H 0.3618 0.3027 0.2478 0.033 Uiso 1 1 calc R . . C15 C 0.5453(5) 0.2770(4) 0.2515(3) 0.0225(12) Uani 1 1 d . . . C16 C 0.6348(6) 0.2657(4) 0.2116(3) 0.0273(13) Uani 1 1 d . . . H16 H 0.7198 0.2564 0.2333 0.033 Uiso 1 1 calc R . . C17 C 0.6005(6) 0.2682(4) 0.1400(3) 0.0281(13) Uani 1 1 d . . . H17 H 0.6617 0.2585 0.1125 0.034 Uiso 1 1 calc R . . C18 C 0.8672(7) 0.4511(4) 0.5803(3) 0.0392(16) Uani 1 1 d . . . H18A H 0.8075 0.4809 0.6081 0.059 Uiso 1 1 calc R . . H18B H 0.9462 0.4986 0.5964 0.059 Uiso 1 1 calc R . . H18C H 0.8887 0.3911 0.5901 0.059 Uiso 1 1 calc R . . C19 C 0.8053(6) 0.4248(4) 0.4990(3) 0.0266(13) Uani 1 1 d . . . C20 C 0.8268(6) 0.4769(4) 0.4535(3) 0.0288(13) Uani 1 1 d . . . H20 H 0.8855 0.5361 0.4688 0.035 Uiso 1 1 calc R . . C21 C 0.7464(5) 0.4252(4) 0.3830(3) 0.0243(12) Uani 1 1 d . . . H21 H 0.7390 0.4423 0.3401 0.029 Uiso 1 1 calc R . . C22 C 0.6764(5) 0.3421(4) 0.3855(3) 0.0219(12) Uani 1 1 d . . . C23 C 0.5785(5) 0.2705(3) 0.3278(3) 0.0217(12) Uani 1 1 d . . . C24 C 0.5058(6) 0.1930(4) 0.3351(3) 0.0235(12) Uani 1 1 d . . . C25 C 0.4144(6) 0.1145(4) 0.2778(3) 0.0336(14) Uani 1 1 d . . . H25 H 0.3888 0.1039 0.2259 0.040 Uiso 1 1 calc R . . C26 C 0.3700(6) 0.0569(4) 0.3111(4) 0.0381(16) Uani 1 1 d . . . H26 H 0.3064 -0.0008 0.2869 0.046 Uiso 1 1 calc R . . C27 C 0.4355(6) 0.0986(4) 0.3874(4) 0.0375(16) Uani 1 1 d . . . C28 C 0.4167(8) 0.0675(6) 0.4498(4) 0.069(3) Uani 1 1 d . . . H28A H 0.4875 0.1025 0.4956 0.104 Uiso 1 1 calc R . . H28B H 0.4161 -0.0042 0.4358 0.104 Uiso 1 1 calc R . . H28C H 0.3343 0.0840 0.4587 0.104 Uiso 1 1 calc R . . C29 C 1.0996(7) 0.4293(4) 1.2310(3) 0.0427(17) Uani 1 1 d . . . H29A H 1.0243 0.4173 1.2473 0.064 Uiso 1 1 calc R . . H29B H 1.1349 0.5001 1.2538 0.064 Uiso 1 1 calc R . . H29C H 1.1655 0.3909 1.2464 0.064 Uiso 1 1 calc R . . C30 C 1.0604(6) 0.3988(4) 1.1487(3) 0.0312(14) Uani 1 1 d . . . C31 C 1.0717(7) 0.4565(4) 1.1059(3) 0.0366(15) Uani 1 1 d . . . H31 H 1.1108 0.5239 1.1249 0.044 Uiso 1 1 calc R . . C32 C 1.0167(6) 0.3991(4) 1.0322(3) 0.0339(15) Uani 1 1 d . . . H32 H 1.0087 0.4198 0.9909 0.041 Uiso 1 1 calc R . . C33 C 0.9739(6) 0.3035(4) 1.0285(3) 0.0265(13) Uani 1 1 d . . . C34 C 0.9065(6) 0.2185(4) 0.9677(3) 0.0254(13) Uani 1 1 d . . . C35 C 0.8713(6) 0.1315(4) 0.9784(3) 0.0267(13) Uani 1 1 d . . . C36 C 0.8097(6) 0.0363(4) 0.9267(3) 0.0346(14) Uani 1 1 d . . . H36 H 0.7786 0.0173 0.8738 0.041 Uiso 1 1 calc R . . C37 C 0.8033(6) -0.0233(4) 0.9668(4) 0.0400(16) Uani 1 1 d . . . H37 H 0.7672 -0.0915 0.9466 0.048 Uiso 1 1 calc R . . C38 C 0.8591(6) 0.0336(4) 1.0424(3) 0.0337(15) Uani 1 1 d . . . C39 C 0.8776(7) 0.0024(5) 1.1086(4) 0.0474(18) Uani 1 1 d . . . H39A H 0.9693 0.0171 1.1369 0.071 Uiso 1 1 calc R . . H39B H 0.8479 -0.0690 1.0913 0.071 Uiso 1 1 calc R . . H39C H 0.8276 0.0387 1.1409 0.071 Uiso 1 1 calc R . . C40 C 0.8668(6) 0.2237(4) 0.8915(3) 0.0254(12) Uani 1 1 d . . . C41 C 0.7355(6) 0.2066(4) 0.8521(3) 0.0288(13) Uani 1 1 d . . . H41 H 0.6722 0.1894 0.8730 0.035 Uiso 1 1 calc R . . C42 C 0.6987(6) 0.2150(4) 0.7830(3) 0.0292(13) Uani 1 1 d . . . H42 H 0.6095 0.2047 0.7568 0.035 Uiso 1 1 calc R . . C43 C 0.7907(6) 0.2385(3) 0.7506(3) 0.0220(12) Uani 1 1 d . . . C44 C 0.9191(6) 0.2544(4) 0.7897(3) 0.0270(13) Uani 1 1 d . . . H44 H 0.9823 0.2705 0.7683 0.032 Uiso 1 1 calc R . . C45 C 0.9587(6) 0.2473(4) 0.8603(3) 0.0268(13) Uani 1 1 d . . . H45 H 1.0479 0.2586 0.8868 0.032 Uiso 1 1 calc R . . C46 C 0.4657(8) 0.4243(5) 0.5472(4) 0.059(2) Uani 1 1 d . . . H46A H 0.4941 0.3929 0.5027 0.088 Uiso 1 1 calc R . . H46B H 0.4829 0.4965 0.5623 0.088 Uiso 1 1 calc R . . H46C H 0.3729 0.4030 0.5354 0.088 Uiso 1 1 calc R . . C47 C 0.5377(6) 0.3945(4) 0.6097(4) 0.0366(15) Uani 1 1 d . . . C48 C 0.5413(7) 0.4324(4) 0.6848(3) 0.0398(16) Uani 1 1 d . . . H48 H 0.4980 0.4843 0.7074 0.048 Uiso 1 1 calc R . . C49 C 0.6180(6) 0.3814(4) 0.7193(3) 0.0348(15) Uani 1 1 d . . . H49 H 0.6387 0.3907 0.7709 0.042 Uiso 1 1 calc R . . C50 C 0.6623(5) 0.3115(3) 0.6644(3) 0.0231(12) Uani 1 1 d . . . C51 C 0.7477(5) 0.2448(3) 0.6748(3) 0.0204(12) Uani 1 1 d . . . C52 C 0.7925(5) 0.1807(4) 0.6181(3) 0.0221(12) Uani 1 1 d . . . C53 C 0.8713(6) 0.1067(4) 0.6233(3) 0.0270(13) Uani 1 1 d . . . H53 H 0.9091 0.0936 0.6673 0.032 Uiso 1 1 calc R . . C54 C 0.8829(6) 0.0581(4) 0.5537(3) 0.0281(13) Uani 1 1 d . . . H54 H 0.9294 0.0044 0.5400 0.034 Uiso 1 1 calc R . . C55 C 0.8130(6) 0.1022(4) 0.5064(3) 0.0253(12) Uani 1 1 d . . . C56 C 0.7947(7) 0.0755(4) 0.4251(3) 0.0372(15) Uani 1 1 d . . . H56A H 0.7065 0.0411 0.3972 0.056 Uiso 1 1 calc R . . H56B H 0.8565 0.0318 0.4099 0.056 Uiso 1 1 calc R . . H56C H 0.8089 0.1358 0.4145 0.056 Uiso 1 1 calc R . . C57 C 1.0698(7) 0.2133(4) 0.3216(4) 0.0431(17) Uani 1 1 d . . . H57 H 1.0542 0.2079 0.2683 0.052 Uiso 1 1 calc R . . C58 C 1.1575(10) 0.2475(6) 0.6182(5) 0.082(3) Uani 1 1 d . . . H58 H 1.0950 0.1997 0.6241 0.098 Uiso 1 1 calc R . . B1 B 0.3474(7) 0.2774(5) -0.1284(4) 0.0275(15) Uani 1 1 d . . . B2 B 0.9744(7) 0.2157(5) 1.1235(3) 0.0249(14) Uani 1 1 d . . . N1 N 0.3489(5) 0.3649(3) -0.0555(2) 0.0252(11) Uani 1 1 d . . . N2 N 0.3978(5) 0.1925(3) -0.1024(2) 0.0238(10) Uani 1 1 d . . . N3 N 0.7155(4) 0.3447(3) 0.4593(2) 0.0227(10) Uani 1 1 d . . . N4 N 0.5183(5) 0.1805(3) 0.4031(2) 0.0258(11) Uani 1 1 d . . . N5 N 1.0024(5) 0.3053(3) 1.1014(2) 0.0253(11) Uani 1 1 d . . . N6 N 0.9019(5) 0.1279(3) 1.0504(3) 0.0279(11) Uani 1 1 d . . . N7 N 0.6112(5) 0.3216(3) 0.5962(2) 0.0260(11) Uani 1 1 d . . . N8 N 0.7596(4) 0.1760(3) 0.5439(2) 0.0224(10) Uani 1 1 d . . . F1 F 0.2256(3) 0.2466(2) -0.17666(17) 0.0364(8) Uani 1 1 d . . . F2 F 0.4322(3) 0.3079(2) -0.16174(17) 0.0357(8) Uani 1 1 d . . . F3 F 0.8991(3) 0.2368(2) 1.17156(17) 0.0348(8) Uani 1 1 d . . . F4 F 1.0897(3) 0.1914(2) 1.15866(17) 0.0316(8) Uani 1 1 d . . . Ni1 Ni 0.64574(8) 0.25468(5) 0.50040(4) 0.0272(2) Uani 1 1 d . . . Cl1 Cl 0.95466(18) 0.27819(13) 0.35658(10) 0.0498(5) Uani 1 1 d . . . Cl2 Cl 1.0527(2) 0.09234(13) 0.32293(12) 0.0642(6) Uani 1 1 d . . . Cl3 Cl 1.22479(19) 0.27761(13) 0.37219(11) 0.0564(5) Uani 1 1 d . . . Cl4 Cl 1.1045(3) 0.24787(17) 0.52638(12) 0.0912(9) Uani 1 1 d . . . Cl5 Cl 1.3134(3) 0.2056(2) 0.62976(17) 0.1111(10) Uani 1 1 d . . . Cl6 Cl 1.1660(3) 0.36260(18) 0.68240(13) 0.1023(10) 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 C1 0.048(5) 0.042(4) 0.036(4) 0.020(3) 0.005(3) 0.013(3) C2 0.032(4) 0.028(3) 0.036(4) 0.015(3) 0.004(3) 0.003(2) C3 0.035(4) 0.029(3) 0.039(4) 0.009(3) 0.011(3) 0.010(3) C4 0.035(4) 0.033(3) 0.023(3) 0.005(3) 0.008(3) 0.008(3) C5 0.026(3) 0.030(3) 0.010(3) 0.004(2) -0.001(3) 0.003(2) C6 0.020(3) 0.031(3) 0.011(3) 0.003(2) -0.003(2) 0.001(2) C7 0.031(4) 0.031(3) 0.019(3) 0.011(2) 0.006(3) 0.007(2) C8 0.042(4) 0.033(3) 0.025(3) 0.013(3) 0.007(3) 0.009(3) C9 0.042(4) 0.029(3) 0.021(3) 0.003(2) 0.007(3) 0.012(3) C10 0.037(4) 0.031(3) 0.012(3) 0.000(2) 0.010(3) 0.005(2) C11 0.046(4) 0.044(4) 0.017(3) 0.002(3) 0.005(3) 0.010(3) C12 0.028(3) 0.026(3) 0.015(3) 0.007(2) 0.006(3) 0.004(2) C13 0.025(3) 0.033(3) 0.019(3) 0.008(2) -0.001(3) 0.009(2) C14 0.032(4) 0.036(3) 0.016(3) 0.008(2) 0.010(3) 0.012(2) C15 0.025(3) 0.026(3) 0.012(3) 0.003(2) 0.002(3) 0.005(2) C16 0.023(3) 0.044(3) 0.012(3) 0.008(2) 0.003(3) 0.008(2) C17 0.033(4) 0.032(3) 0.018(3) 0.008(2) 0.009(3) 0.006(2) C18 0.042(4) 0.046(4) 0.019(3) 0.006(3) 0.003(3) -0.008(3) C19 0.028(3) 0.028(3) 0.015(3) 0.001(2) 0.002(3) 0.003(2) C20 0.029(4) 0.025(3) 0.028(4) 0.006(2) 0.007(3) -0.003(2) C21 0.028(3) 0.027(3) 0.020(3) 0.010(2) 0.009(3) 0.007(2) C22 0.027(3) 0.023(3) 0.017(3) 0.007(2) 0.007(3) 0.007(2) C23 0.025(3) 0.023(3) 0.019(3) 0.006(2) 0.010(3) 0.010(2) C24 0.025(3) 0.023(3) 0.016(3) 0.001(2) 0.003(3) 0.006(2) C25 0.040(4) 0.026(3) 0.028(4) 0.001(3) 0.011(3) 0.006(3) C26 0.036(4) 0.019(3) 0.047(4) 0.002(3) 0.006(3) -0.001(2) C27 0.035(4) 0.030(3) 0.048(4) 0.021(3) 0.004(3) -0.002(3) C28 0.063(6) 0.077(5) 0.068(6) 0.054(5) -0.011(5) -0.025(4) C29 0.059(5) 0.039(3) 0.016(3) 0.002(3) 0.001(3) -0.004(3) C30 0.043(4) 0.026(3) 0.010(3) -0.004(2) -0.001(3) 0.001(2) C31 0.054(5) 0.023(3) 0.028(4) 0.006(3) 0.010(3) 0.002(3) C32 0.050(4) 0.030(3) 0.019(3) 0.011(3) 0.002(3) 0.001(3) C33 0.031(4) 0.029(3) 0.017(3) 0.005(2) 0.008(3) -0.001(2) C34 0.028(4) 0.036(3) 0.015(3) 0.008(2) 0.011(3) 0.005(2) C35 0.027(4) 0.031(3) 0.020(3) 0.007(2) 0.006(3) 0.003(2) C36 0.039(4) 0.031(3) 0.022(3) 0.001(3) 0.003(3) -0.006(3) C37 0.040(4) 0.031(3) 0.042(4) 0.009(3) 0.008(3) -0.006(3) C38 0.034(4) 0.032(3) 0.039(4) 0.018(3) 0.012(3) -0.003(3) C39 0.048(5) 0.049(4) 0.054(5) 0.033(4) 0.012(4) 0.002(3) C40 0.031(4) 0.030(3) 0.009(3) 0.002(2) 0.002(3) 0.000(2) C41 0.032(4) 0.033(3) 0.020(3) 0.006(2) 0.012(3) 0.002(2) C42 0.028(4) 0.034(3) 0.017(3) 0.004(2) 0.000(3) -0.001(2) C43 0.032(3) 0.017(2) 0.013(3) 0.001(2) 0.007(3) 0.002(2) C44 0.032(4) 0.032(3) 0.017(3) 0.011(2) 0.005(3) 0.001(2) C45 0.028(3) 0.028(3) 0.017(3) 0.004(2) 0.001(3) 0.000(2) C46 0.080(6) 0.067(5) 0.054(5) 0.040(4) 0.028(5) 0.052(4) C47 0.036(4) 0.037(3) 0.045(4) 0.022(3) 0.015(3) 0.014(3) C48 0.048(5) 0.033(3) 0.034(4) 0.003(3) 0.016(3) 0.014(3) C49 0.044(4) 0.029(3) 0.023(3) 0.001(3) 0.005(3) 0.010(3) C50 0.026(3) 0.019(3) 0.022(3) 0.004(2) 0.009(3) 0.004(2) C51 0.027(3) 0.019(3) 0.010(3) 0.003(2) 0.001(2) -0.002(2) C52 0.026(3) 0.023(3) 0.018(3) 0.010(2) 0.004(3) 0.002(2) C53 0.032(4) 0.031(3) 0.021(3) 0.014(2) 0.008(3) 0.009(2) C54 0.037(4) 0.029(3) 0.023(3) 0.011(2) 0.014(3) 0.012(2) C55 0.028(3) 0.029(3) 0.018(3) 0.007(2) 0.007(3) 0.001(2) C56 0.048(4) 0.041(3) 0.016(3) 0.004(3) 0.006(3) 0.013(3) C57 0.058(5) 0.042(4) 0.040(4) 0.026(3) 0.015(4) 0.016(3) C58 0.103(8) 0.063(5) 0.059(6) 0.025(4) -0.007(6) -0.021(5) B1 0.024(4) 0.037(4) 0.025(4) 0.016(3) 0.005(3) 0.007(3) B2 0.026(4) 0.036(3) 0.013(3) 0.008(3) 0.007(3) 0.006(3) N1 0.024(3) 0.028(2) 0.022(3) 0.009(2) 0.003(2) 0.0038(19) N2 0.026(3) 0.031(2) 0.011(2) 0.0049(19) 0.004(2) 0.0046(19) N3 0.026(3) 0.021(2) 0.015(2) 0.0039(18) 0.001(2) 0.0042(18) N4 0.025(3) 0.026(2) 0.025(3) 0.014(2) 0.001(2) 0.0003(19) N5 0.032(3) 0.026(2) 0.013(3) 0.0050(19) 0.002(2) 0.0013(19) N6 0.031(3) 0.030(3) 0.024(3) 0.013(2) 0.009(2) 0.003(2) N7 0.031(3) 0.027(2) 0.025(3) 0.015(2) 0.008(2) 0.009(2) N8 0.030(3) 0.023(2) 0.012(2) 0.0047(18) 0.004(2) 0.0018(19) F1 0.031(2) 0.0449(19) 0.0197(19) 0.0061(15) -0.0071(16) 0.0052(15) F2 0.045(2) 0.0420(19) 0.0270(19) 0.0159(15) 0.0171(18) 0.0049(16) F3 0.036(2) 0.050(2) 0.0238(19) 0.0146(15) 0.0150(17) 0.0091(15) F4 0.031(2) 0.0390(18) 0.0235(19) 0.0131(15) 0.0026(16) 0.0084(14) Ni1 0.0378(5) 0.0286(4) 0.0164(4) 0.0120(3) 0.0043(3) 0.0056(3) Cl1 0.0489(12) 0.0609(10) 0.0455(11) 0.0214(8) 0.0171(9) 0.0262(8) Cl2 0.0800(16) 0.0483(10) 0.0843(15) 0.0372(10) 0.0376(13) 0.0199(10) Cl3 0.0488(12) 0.0587(11) 0.0615(13) 0.0206(9) 0.0161(10) 0.0136(8) Cl4 0.136(3) 0.0815(15) 0.0419(13) 0.0255(11) 0.0038(14) -0.0175(14) Cl5 0.129(3) 0.0876(18) 0.099(2) 0.0419(16) -0.004(2) 0.0035(16) Cl6 0.161(3) 0.0836(16) 0.0491(15) 0.0187(12) 0.0180(17) 0.0071(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.511(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.361(6) . ? C2 C3 1.378(8) . ? C3 C4 1.373(8) . ? C3 H3 0.9500 . ? C4 C5 1.413(7) . ? C4 H4 0.9500 . ? C5 N1 1.385(6) . ? C5 C6 1.392(7) . ? C6 C7 1.390(7) . ? C6 C12 1.483(7) . ? C7 N2 1.386(6) . ? C7 C8 1.416(7) . ? C8 C9 1.386(8) . ? C8 H8 0.9500 . ? C9 C10 1.404(8) . ? C9 H9 0.9500 . ? C10 N2 1.372(7) . ? C10 C11 1.480(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.379(8) . ? C12 C17 1.390(8) . ? C13 C14 1.396(7) . ? C13 H13 0.9500 . ? C14 C15 1.381(8) . ? C14 H14 0.9500 . ? C15 C16 1.385(8) . ? C15 C23 1.498(7) . ? C16 C17 1.385(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.483(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.336(7) . ? C19 C20 1.410(7) . ? C20 C21 1.369(8) . ? C20 H20 0.9500 . ? C21 C22 1.411(7) . ? C21 H21 0.9500 . ? C22 C23 1.404(8) . ? C22 N3 1.404(6) . ? C23 C24 1.409(8) . ? C24 N4 1.394(6) . ? C24 C25 1.414(8) . ? C25 C26 1.363(8) . ? C25 H25 0.9500 . ? C26 C27 1.396(9) . ? C26 H26 0.9500 . ? C27 N4 1.344(7) . ? C27 C28 1.507(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.474(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.364(7) . ? C30 C31 1.399(8) . ? C31 C32 1.365(8) . ? C31 H31 0.9500 . ? C32 C33 1.411(7) . ? C32 H32 0.9500 . ? C33 N5 1.388(6) . ? C33 C34 1.399(8) . ? C34 C35 1.398(7) . ? C34 C40 1.490(7) . ? C35 N6 1.401(7) . ? C35 C36 1.413(8) . ? C36 C37 1.368(8) . ? C36 H36 0.9500 . ? C37 C38 1.393(9) . ? C37 H37 0.9500 . ? C38 N6 1.363(7) . ? C38 C39 1.498(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.384(8) . ? C40 C41 1.400(8) . ? C41 C42 1.374(7) . ? C41 H41 0.9500 . ? C42 C43 1.401(8) . ? C42 H42 0.9500 . ? C43 C44 1.373(8) . ? C43 C51 1.492(7) . ? C44 C45 1.397(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.495(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N7 1.353(7) . ? C47 C48 1.391(8) . ? C48 C49 1.350(8) . ? C48 H48 0.9500 . ? C49 C50 1.420(7) . ? C49 H49 0.9500 . ? C50 N7 1.384(6) . ? C50 C51 1.402(7) . ? C51 C52 1.409(7) . ? C52 N8 1.398(6) . ? C52 C53 1.421(7) . ? C53 C54 1.363(7) . ? C53 H53 0.9500 . ? C54 C55 1.399(7) . ? C54 H54 0.9500 . ? C55 N8 1.335(7) . ? C55 C56 1.480(7) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 Cl3 1.743(7) . ? C57 Cl1 1.747(7) . ? C57 Cl2 1.764(6) . ? C57 H57 1.0000 . ? C58 Cl6 1.704(9) . ? C58 Cl4 1.764(8) . ? C58 Cl5 1.811(11) . ? C58 H58 1.0000 . ? B1 F1 1.364(8) . ? B1 F2 1.393(7) . ? B1 N2 1.561(7) . ? B1 N1 1.563(8) . ? B2 F3 1.377(7) . ? B2 F4 1.393(7) . ? B2 N5 1.544(7) . ? B2 N6 1.549(8) . ? N3 Ni1 1.967(4) . ? N4 Ni1 1.965(5) . ? N7 Ni1 1.961(4) . ? N8 Ni1 1.959(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.7(5) . . ? N1 C2 C1 121.6(5) . . ? C3 C2 C1 127.8(5) . . ? C4 C3 C2 106.9(5) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? C3 C4 C5 107.9(5) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? N1 C5 C6 121.3(4) . . ? N1 C5 C4 107.6(4) . . ? C6 C5 C4 131.0(5) . . ? C5 C6 C7 120.5(5) . . ? C5 C6 C12 119.9(4) . . ? C7 C6 C12 119.5(4) . . ? N2 C7 C6 121.3(4) . . ? N2 C7 C8 107.4(4) . . ? C6 C7 C8 131.2(5) . . ? C9 C8 C7 107.6(5) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 C10 107.8(5) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? N2 C10 C9 108.3(5) . . ? N2 C10 C11 123.7(5) . . ? C9 C10 C11 128.0(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.5(5) . . ? C13 C12 C6 120.3(5) . . ? C17 C12 C6 121.1(5) . . ? C12 C13 C14 120.8(5) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 C23 119.5(5) . . ? C16 C15 C23 121.0(5) . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C12 C17 C16 121.0(5) . . ? C12 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 110.9(5) . . ? N3 C19 C18 121.4(5) . . ? C20 C19 C18 127.6(5) . . ? C21 C20 C19 106.4(5) . . ? C21 C20 H20 126.8 . . ? C19 C20 H20 126.8 . . ? C20 C21 C22 107.9(5) . . ? C20 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? C23 C22 N3 123.5(5) . . ? C23 C22 C21 128.5(5) . . ? N3 C22 C21 107.9(5) . . ? C22 C23 C24 125.7(5) . . ? C22 C23 C15 118.1(5) . . ? C24 C23 C15 116.2(5) . . ? N4 C24 C23 123.5(5) . . ? N4 C24 C25 108.7(5) . . ? C23 C24 C25 127.8(5) . . ? C26 C25 C24 107.0(5) . . ? C26 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? C25 C26 C27 107.1(5) . . ? C25 C26 H26 126.5 . . ? C27 C26 H26 126.5 . . ? N4 C27 C26 111.2(5) . . ? N4 C27 C28 120.1(6) . . ? C26 C27 C28 128.6(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C31 108.6(5) . . ? N5 C30 C29 123.2(5) . . ? C31 C30 C29 128.2(5) . . ? C32 C31 C30 108.1(5) . . ? C32 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? C31 C32 C33 107.6(5) . . ? C31 C32 H32 126.2 . . ? C33 C32 H32 126.2 . . ? N5 C33 C34 121.1(5) . . ? N5 C33 C32 107.6(5) . . ? C34 C33 C32 131.2(5) . . ? C33 C34 C35 120.8(5) . . ? C33 C34 C40 118.8(5) . . ? C35 C34 C40 120.3(5) . . ? C34 C35 N6 120.6(5) . . ? C34 C35 C36 131.3(5) . . ? N6 C35 C36 108.0(5) . . ? C37 C36 C35 107.4(5) . . ? C37 C36 H36 126.3 . . ? C35 C36 H36 126.3 . . ? C36 C37 C38 108.0(5) . . ? C36 C37 H37 126.0 . . ? C38 C37 H37 126.0 . . ? N6 C38 C37 109.8(5) . . ? N6 C38 C39 121.5(5) . . ? C37 C38 C39 128.7(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 119.9(5) . . ? C45 C40 C34 120.4(5) . . ? C41 C40 C34 119.7(5) . . ? C42 C41 C40 119.7(5) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 121.1(6) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 118.7(5) . . ? C44 C43 C51 121.6(5) . . ? C42 C43 C51 119.8(5) . . ? C43 C44 C45 121.2(5) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C40 C45 C44 119.4(5) . . ? C40 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C48 111.5(5) . . ? N7 C47 C46 120.1(6) . . ? C48 C47 C46 128.5(6) . . ? C49 C48 C47 106.8(5) . . ? C49 C48 H48 126.6 . . ? C47 C48 H48 126.6 . . ? C48 C49 C50 107.6(5) . . ? C48 C49 H49 126.2 . . ? C50 C49 H49 126.2 . . ? N7 C50 C51 123.5(4) . . ? N7 C50 C49 108.6(4) . . ? C51 C50 C49 127.9(5) . . ? C50 C51 C52 124.7(4) . . ? C50 C51 C43 117.7(4) . . ? C52 C51 C43 117.5(4) . . ? N8 C52 C51 124.6(4) . . ? N8 C52 C53 107.6(4) . . ? C51 C52 C53 127.7(5) . . ? C54 C53 C52 107.5(5) . . ? C54 C53 H53 126.3 . . ? C52 C53 H53 126.3 . . ? C53 C54 C55 106.9(5) . . ? C53 C54 H54 126.6 . . ? C55 C54 H54 126.6 . . ? N8 C55 C54 111.1(5) . . ? N8 C55 C56 121.1(5) . . ? C54 C55 C56 127.9(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Cl3 C57 Cl1 110.4(4) . . ? Cl3 C57 Cl2 111.6(3) . . ? Cl1 C57 Cl2 110.1(4) . . ? Cl3 C57 H57 108.2 . . ? Cl1 C57 H57 108.2 . . ? Cl2 C57 H57 108.2 . . ? Cl6 C58 Cl4 110.6(5) . . ? Cl6 C58 Cl5 111.6(5) . . ? Cl4 C58 Cl5 107.5(6) . . ? Cl6 C58 H58 109.0 . . ? Cl4 C58 H58 109.0 . . ? Cl5 C58 H58 109.0 . . ? F1 B1 F2 111.0(5) . . ? F1 B1 N2 110.6(5) . . ? F2 B1 N2 109.2(5) . . ? F1 B1 N1 110.9(5) . . ? F2 B1 N1 109.1(5) . . ? N2 B1 N1 105.8(4) . . ? F3 B2 F4 108.8(4) . . ? F3 B2 N5 110.8(5) . . ? F4 B2 N5 110.0(5) . . ? F3 B2 N6 109.8(5) . . ? F4 B2 N6 110.1(4) . . ? N5 B2 N6 107.3(4) . . ? C2 N1 C5 107.0(4) . . ? C2 N1 B1 127.5(4) . . ? C5 N1 B1 125.4(4) . . ? C10 N2 C7 108.9(4) . . ? C10 N2 B1 125.7(5) . . ? C7 N2 B1 125.4(4) . . ? C19 N3 C22 106.9(4) . . ? C19 N3 Ni1 125.4(4) . . ? C22 N3 Ni1 127.6(3) . . ? C27 N4 C24 106.0(5) . . ? C27 N4 Ni1 125.6(4) . . ? C24 N4 Ni1 127.9(4) . . ? C30 N5 C33 108.0(4) . . ? C30 N5 B2 126.8(5) . . ? C33 N5 B2 125.2(4) . . ? C38 N6 C35 106.8(5) . . ? C38 N6 B2 128.2(4) . . ? C35 N6 B2 124.9(4) . . ? C47 N7 C50 105.6(4) . . ? C47 N7 Ni1 125.5(4) . . ? C50 N7 Ni1 128.7(3) . . ? C55 N8 C52 106.9(4) . . ? C55 N8 Ni1 125.8(3) . . ? C52 N8 Ni1 127.1(3) . . ? N8 Ni1 N7 91.24(17) . . ? N8 Ni1 N3 119.58(19) . . ? N7 Ni1 N3 114.40(17) . . ? N8 Ni1 N4 115.73(17) . . ? N7 Ni1 N4 127.2(2) . . ? N3 Ni1 N4 91.47(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C4 -179.1(6) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C3 C4 C5 N1 1.4(7) . . . . ? C3 C4 C5 C6 178.0(6) . . . . ? N1 C5 C6 C7 0.3(9) . . . . ? C4 C5 C6 C7 -175.9(6) . . . . ? N1 C5 C6 C12 -176.0(5) . . . . ? C4 C5 C6 C12 7.8(10) . . . . ? C5 C6 C7 N2 -2.2(9) . . . . ? C12 C6 C7 N2 174.1(5) . . . . ? C5 C6 C7 C8 -178.4(6) . . . . ? C12 C6 C7 C8 -2.1(10) . . . . ? N2 C7 C8 C9 -0.3(7) . . . . ? C6 C7 C8 C9 176.3(6) . . . . ? C7 C8 C9 C10 -0.7(7) . . . . ? C8 C9 C10 N2 1.5(7) . . . . ? C8 C9 C10 C11 -177.1(6) . . . . ? C5 C6 C12 C13 57.6(7) . . . . ? C7 C6 C12 C13 -118.7(6) . . . . ? C5 C6 C12 C17 -124.8(6) . . . . ? C7 C6 C12 C17 58.9(7) . . . . ? C17 C12 C13 C14 -0.7(8) . . . . ? C6 C12 C13 C14 177.0(5) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C13 C14 C15 C16 1.1(8) . . . . ? C13 C14 C15 C23 -178.5(5) . . . . ? C14 C15 C16 C17 -2.1(8) . . . . ? C23 C15 C16 C17 177.5(5) . . . . ? C13 C12 C17 C16 -0.4(8) . . . . ? C6 C12 C17 C16 -178.0(5) . . . . ? C15 C16 C17 C12 1.8(8) . . . . ? N3 C19 C20 C21 -0.3(7) . . . . ? C18 C19 C20 C21 -179.0(6) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C20 C21 C22 C23 176.7(5) . . . . ? C20 C21 C22 N3 0.4(6) . . . . ? N3 C22 C23 C24 0.6(9) . . . . ? C21 C22 C23 C24 -175.2(5) . . . . ? N3 C22 C23 C15 179.3(5) . . . . ? C21 C22 C23 C15 3.5(8) . . . . ? C14 C15 C23 C22 -116.7(6) . . . . ? C16 C15 C23 C22 63.7(7) . . . . ? C14 C15 C23 C24 62.1(6) . . . . ? C16 C15 C23 C24 -117.5(6) . . . . ? C22 C23 C24 N4 3.2(9) . . . . ? C15 C23 C24 N4 -175.5(5) . . . . ? C22 C23 C24 C25 -174.1(5) . . . . ? C15 C23 C24 C25 7.1(8) . . . . ? N4 C24 C25 C26 1.5(6) . . . . ? C23 C24 C25 C26 179.2(5) . . . . ? C24 C25 C26 C27 -1.2(7) . . . . ? C25 C26 C27 N4 0.5(7) . . . . ? C25 C26 C27 C28 175.8(7) . . . . ? N5 C30 C31 C32 2.0(8) . . . . ? C29 C30 C31 C32 -176.8(7) . . . . ? C30 C31 C32 C33 -1.8(8) . . . . ? C31 C32 C33 N5 0.9(7) . . . . ? C31 C32 C33 C34 176.7(7) . . . . ? N5 C33 C34 C35 -3.1(9) . . . . ? C32 C33 C34 C35 -178.4(6) . . . . ? N5 C33 C34 C40 173.9(5) . . . . ? C32 C33 C34 C40 -1.4(10) . . . . ? C33 C34 C35 N6 0.6(9) . . . . ? C40 C34 C35 N6 -176.3(5) . . . . ? C33 C34 C35 C36 -176.5(6) . . . . ? C40 C34 C35 C36 6.6(10) . . . . ? C34 C35 C36 C37 177.4(6) . . . . ? N6 C35 C36 C37 0.0(7) . . . . ? C35 C36 C37 C38 0.4(8) . . . . ? C36 C37 C38 N6 -0.7(8) . . . . ? C36 C37 C38 C39 -178.9(7) . . . . ? C33 C34 C40 C45 60.3(7) . . . . ? C35 C34 C40 C45 -122.7(6) . . . . ? C33 C34 C40 C41 -118.2(6) . . . . ? C35 C34 C40 C41 58.7(7) . . . . ? C45 C40 C41 C42 -1.0(8) . . . . ? C34 C40 C41 C42 177.6(5) . . . . ? C40 C41 C42 C43 1.2(8) . . . . ? C41 C42 C43 C44 -0.8(7) . . . . ? C41 C42 C43 C51 178.6(5) . . . . ? C42 C43 C44 C45 0.1(7) . . . . ? C51 C43 C44 C45 -179.3(4) . . . . ? C41 C40 C45 C44 0.3(8) . . . . ? C34 C40 C45 C44 -178.2(5) . . . . ? C43 C44 C45 C40 0.1(8) . . . . ? N7 C47 C48 C49 -0.6(8) . . . . ? C46 C47 C48 C49 179.4(7) . . . . ? C47 C48 C49 C50 0.2(8) . . . . ? C48 C49 C50 N7 0.2(7) . . . . ? C48 C49 C50 C51 177.6(6) . . . . ? N7 C50 C51 C52 0.4(9) . . . . ? C49 C50 C51 C52 -176.7(6) . . . . ? N7 C50 C51 C43 -177.3(5) . . . . ? C49 C50 C51 C43 5.7(9) . . . . ? C44 C43 C51 C50 -123.3(6) . . . . ? C42 C43 C51 C50 57.3(6) . . . . ? C44 C43 C51 C52 58.8(7) . . . . ? C42 C43 C51 C52 -120.5(6) . . . . ? C50 C51 C52 N8 1.1(9) . . . . ? C43 C51 C52 N8 178.8(5) . . . . ? C50 C51 C52 C53 -175.1(6) . . . . ? C43 C51 C52 C53 2.6(8) . . . . ? N8 C52 C53 C54 -1.1(6) . . . . ? C51 C52 C53 C54 175.7(5) . . . . ? C52 C53 C54 C55 0.5(7) . . . . ? C53 C54 C55 N8 0.3(7) . . . . ? C53 C54 C55 C56 -179.3(6) . . . . ? C3 C2 N1 C5 0.9(7) . . . . ? C1 C2 N1 C5 -180.0(6) . . . . ? C3 C2 N1 B1 -176.4(5) . . . . ? C1 C2 N1 B1 2.7(9) . . . . ? C6 C5 N1 C2 -178.3(5) . . . . ? C4 C5 N1 C2 -1.4(6) . . . . ? C6 C5 N1 B1 -1.0(8) . . . . ? C4 C5 N1 B1 176.0(5) . . . . ? F1 B1 N1 C2 -60.3(7) . . . . ? F2 B1 N1 C2 62.3(7) . . . . ? N2 B1 N1 C2 179.7(5) . . . . ? F1 B1 N1 C5 122.9(5) . . . . ? F2 B1 N1 C5 -114.6(6) . . . . ? N2 B1 N1 C5 2.9(7) . . . . ? C9 C10 N2 C7 -1.7(7) . . . . ? C11 C10 N2 C7 177.0(6) . . . . ? C9 C10 N2 B1 177.6(5) . . . . ? C11 C10 N2 B1 -3.6(9) . . . . ? C6 C7 N2 C10 -175.7(5) . . . . ? C8 C7 N2 C10 1.3(7) . . . . ? C6 C7 N2 B1 4.9(9) . . . . ? C8 C7 N2 B1 -178.1(5) . . . . ? F1 B1 N2 C10 55.7(7) . . . . ? F2 B1 N2 C10 -66.8(7) . . . . ? N1 B1 N2 C10 175.9(5) . . . . ? F1 B1 N2 C7 -125.0(6) . . . . ? F2 B1 N2 C7 112.5(6) . . . . ? N1 B1 N2 C7 -4.8(7) . . . . ? C20 C19 N3 C22 0.5(6) . . . . ? C18 C19 N3 C22 179.3(5) . . . . ? C20 C19 N3 Ni1 -175.7(4) . . . . ? C18 C19 N3 Ni1 3.0(8) . . . . ? C23 C22 N3 C19 -177.1(5) . . . . ? C21 C22 N3 C19 -0.6(6) . . . . ? C23 C22 N3 Ni1 -1.0(7) . . . . ? C21 C22 N3 Ni1 175.6(4) . . . . ? C26 C27 N4 C24 0.5(7) . . . . ? C28 C27 N4 C24 -175.3(6) . . . . ? C26 C27 N4 Ni1 -172.2(4) . . . . ? C28 C27 N4 Ni1 12.0(9) . . . . ? C23 C24 N4 C27 -179.0(5) . . . . ? C25 C24 N4 C27 -1.2(6) . . . . ? C23 C24 N4 Ni1 -6.5(8) . . . . ? C25 C24 N4 Ni1 171.3(4) . . . . ? C31 C30 N5 C33 -1.4(7) . . . . ? C29 C30 N5 C33 177.5(6) . . . . ? C31 C30 N5 B2 177.8(5) . . . . ? C29 C30 N5 B2 -3.3(10) . . . . ? C34 C33 N5 C30 -176.0(6) . . . . ? C32 C33 N5 C30 0.3(7) . . . . ? C34 C33 N5 B2 4.8(9) . . . . ? C32 C33 N5 B2 -178.9(5) . . . . ? F3 B2 N5 C30 57.5(8) . . . . ? F4 B2 N5 C30 -62.8(7) . . . . ? N6 B2 N5 C30 177.4(5) . . . . ? F3 B2 N5 C33 -123.5(6) . . . . ? F4 B2 N5 C33 116.2(6) . . . . ? N6 B2 N5 C33 -3.6(8) . . . . ? C37 C38 N6 C35 0.7(7) . . . . ? C39 C38 N6 C35 179.1(6) . . . . ? C37 C38 N6 B2 -177.6(6) . . . . ? C39 C38 N6 B2 0.7(10) . . . . ? C34 C35 N6 C38 -178.2(6) . . . . ? C36 C35 N6 C38 -0.5(7) . . . . ? C34 C35 N6 B2 0.2(9) . . . . ? C36 C35 N6 B2 178.0(5) . . . . ? F3 B2 N6 C38 -60.3(7) . . . . ? F4 B2 N6 C38 59.4(8) . . . . ? N5 B2 N6 C38 179.1(5) . . . . ? F3 B2 N6 C35 121.6(5) . . . . ? F4 B2 N6 C35 -118.6(5) . . . . ? N5 B2 N6 C35 1.1(7) . . . . ? C48 C47 N7 C50 0.7(7) . . . . ? C46 C47 N7 C50 -179.2(6) . . . . ? C48 C47 N7 Ni1 -174.8(4) . . . . ? C46 C47 N7 Ni1 5.3(9) . . . . ? C51 C50 N7 C47 -178.1(5) . . . . ? C49 C50 N7 C47 -0.6(6) . . . . ? C51 C50 N7 Ni1 -2.8(8) . . . . ? C49 C50 N7 Ni1 174.7(4) . . . . ? C54 C55 N8 C52 -1.0(6) . . . . ? C56 C55 N8 C52 178.7(5) . . . . ? C54 C55 N8 Ni1 -176.5(4) . . . . ? C56 C55 N8 Ni1 3.1(8) . . . . ? C51 C52 N8 C55 -175.6(5) . . . . ? C53 C52 N8 C55 1.3(6) . . . . ? C51 C52 N8 Ni1 -0.2(8) . . . . ? C53 C52 N8 Ni1 176.7(4) . . . . ? C55 N8 Ni1 N7 173.2(5) . . . . ? C52 N8 Ni1 N7 -1.4(4) . . . . ? C55 N8 Ni1 N3 -67.6(5) . . . . ? C52 N8 Ni1 N3 117.7(4) . . . . ? C55 N8 Ni1 N4 40.2(5) . . . . ? C52 N8 Ni1 N4 -134.4(4) . . . . ? C47 N7 Ni1 N8 177.3(5) . . . . ? C50 N7 Ni1 N8 2.9(5) . . . . ? C47 N7 Ni1 N3 53.8(5) . . . . ? C50 N7 Ni1 N3 -120.6(4) . . . . ? C47 N7 Ni1 N4 -58.5(5) . . . . ? C50 N7 Ni1 N4 127.1(4) . . . . ? C19 N3 Ni1 N8 -64.9(5) . . . . ? C22 N3 Ni1 N8 119.6(4) . . . . ? C19 N3 Ni1 N7 41.7(5) . . . . ? C22 N3 Ni1 N7 -133.8(4) . . . . ? C19 N3 Ni1 N4 174.2(4) . . . . ? C22 N3 Ni1 N4 -1.3(4) . . . . ? C27 N4 Ni1 N8 51.9(6) . . . . ? C24 N4 Ni1 N8 -119.2(4) . . . . ? C27 N4 Ni1 N7 -61.4(5) . . . . ? C24 N4 Ni1 N7 127.5(4) . . . . ? C27 N4 Ni1 N3 176.0(5) . . . . ? C24 N4 Ni1 N3 4.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.033 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.129 #===End data_compound14 _database_code_depnum_ccdc_archive 'CCDC 684028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H52 B2 Cl4 Co F4 N8' _chemical_formula_weight 1159.43 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 10.6690(10) _cell_length_b 14.432(2) _cell_length_c 19.145(2) _cell_angle_alpha 70.375(4) _cell_angle_beta 78.215(4) _cell_angle_gamma 86.892(4) _cell_volume 2717.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7008 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 21.59 _exptl_crystal_description irrregular _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10121 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 22.55 _reflns_number_total 10121 _reflns_number_gt 6424 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^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 10121 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3669(6) 0.0770(4) 0.7399(3) 0.0402(17) Uani 1 1 d . . . H1A H 0.4054 0.1217 0.7587 0.060 Uiso 1 1 calc R . . H1B H 0.3916 0.0093 0.7647 0.060 Uiso 1 1 calc R . . H1C H 0.2735 0.0818 0.7512 0.060 Uiso 1 1 calc R . . C2 C 0.4125(5) 0.1041(4) 0.6573(3) 0.0308(15) Uani 1 1 d . . . C3 C 0.4649(6) 0.0427(4) 0.6164(3) 0.0343(15) Uani 1 1 d . . . H3 H 0.4819 -0.0253 0.6371 0.041 Uiso 1 1 calc R . . C4 C 0.4874(5) 0.0979(4) 0.5411(3) 0.0288(14) Uani 1 1 d . . . H4 H 0.5237 0.0752 0.5002 0.035 Uiso 1 1 calc R . . C5 C 0.4471(5) 0.1941(4) 0.5351(3) 0.0201(13) Uani 1 1 d . . . C6 C 0.4421(5) 0.2770(4) 0.4721(3) 0.0206(13) Uani 1 1 d . . . C7 C 0.3976(5) 0.3640(4) 0.4815(3) 0.0235(14) Uani 1 1 d . . . C8 C 0.3888(5) 0.4581(4) 0.4279(3) 0.0301(15) Uani 1 1 d . . . H8 H 0.4115 0.4747 0.3745 0.036 Uiso 1 1 calc R . . C9 C 0.3420(5) 0.5212(4) 0.4663(3) 0.0342(15) Uani 1 1 d . . . H9 H 0.3266 0.5893 0.4445 0.041 Uiso 1 1 calc R . . C10 C 0.3212(5) 0.4674(5) 0.5432(3) 0.0316(15) Uani 1 1 d . . . C11 C 0.2720(6) 0.5021(5) 0.6086(3) 0.0419(17) Uani 1 1 d . . . H11A H 0.1924 0.4665 0.6380 0.063 Uiso 1 1 calc R . . H11B H 0.2554 0.5728 0.5900 0.063 Uiso 1 1 calc R . . H11C H 0.3359 0.4899 0.6408 0.063 Uiso 1 1 calc R . . C12 C 0.4786(5) 0.2690(4) 0.3949(3) 0.0211(13) Uani 1 1 d . . . C13 C 0.3886(5) 0.2897(4) 0.3485(3) 0.0232(14) Uani 1 1 d . . . H13 H 0.3053 0.3097 0.3661 0.028 Uiso 1 1 calc R . . C14 C 0.4192(5) 0.2814(4) 0.2779(3) 0.0280(14) Uani 1 1 d . . . H14 H 0.3564 0.2955 0.2472 0.034 Uiso 1 1 calc R . . C15 C 0.5414(5) 0.2525(4) 0.2500(3) 0.0202(13) Uani 1 1 d . . . C16 C 0.6287(5) 0.2312(4) 0.2967(3) 0.0203(13) Uani 1 1 d . . . H16 H 0.7118 0.2107 0.2792 0.024 Uiso 1 1 calc R . . C17 C 0.5995(5) 0.2388(4) 0.3683(3) 0.0210(13) Uani 1 1 d . . . H17 H 0.6620 0.2233 0.3993 0.025 Uiso 1 1 calc R . . C18 C 0.8873(6) 0.4002(5) -0.0605(3) 0.0470(18) Uani 1 1 d . . . H18A H 0.8507 0.3610 -0.0847 0.071 Uiso 1 1 calc R . . H18B H 0.9782 0.3850 -0.0616 0.071 Uiso 1 1 calc R . . H18C H 0.8785 0.4703 -0.0878 0.071 Uiso 1 1 calc R . . C19 C 0.8185(5) 0.3766(4) 0.0191(3) 0.0264(14) Uani 1 1 d . . . C20 C 0.8414(5) 0.4149(4) 0.0746(3) 0.0266(14) Uani 1 1 d . . . H20 H 0.9051 0.4623 0.0680 0.032 Uiso 1 1 calc R . . C21 C 0.7552(5) 0.3711(4) 0.1389(3) 0.0251(14) Uani 1 1 d . . . H21 H 0.7482 0.3813 0.1860 0.030 Uiso 1 1 calc R . . C22 C 0.6776(5) 0.3074(4) 0.1230(3) 0.0190(13) Uani 1 1 d . . . C23 C 0.5731(5) 0.2491(4) 0.1713(3) 0.0166(12) Uani 1 1 d . . . C24 C 0.4943(5) 0.1902(4) 0.1522(2) 0.0145(12) Uani 1 1 d . . . C25 C 0.3963(5) 0.1241(4) 0.2008(3) 0.0286(15) Uani 1 1 d . . . H25 H 0.3690 0.1113 0.2536 0.034 Uiso 1 1 calc R . . C26 C 0.3481(5) 0.0817(4) 0.1579(3) 0.0328(15) Uani 1 1 d . . . H26 H 0.2810 0.0339 0.1753 0.039 Uiso 1 1 calc R . . C27 C 0.4161(5) 0.1221(4) 0.0834(3) 0.0269(14) Uani 1 1 d . . . C28 C 0.3963(6) 0.1034(5) 0.0142(3) 0.0395(16) Uani 1 1 d . . . H28A H 0.3210 0.1391 -0.0024 0.059 Uiso 1 1 calc R . . H28B H 0.3830 0.0328 0.0257 0.059 Uiso 1 1 calc R . . H28C H 0.4719 0.1262 -0.0262 0.059 Uiso 1 1 calc R . . C29 C 1.1084(5) 0.4347(4) -0.7393(3) 0.0374(16) Uani 1 1 d . . . H29A H 1.1529 0.3820 -0.7556 0.056 Uiso 1 1 calc R . . H29B H 1.1666 0.4913 -0.7545 0.056 Uiso 1 1 calc R . . H29C H 1.0335 0.4543 -0.7629 0.056 Uiso 1 1 calc R . . C30 C 1.0664(5) 0.3988(4) -0.6556(3) 0.0272(14) Uani 1 1 d . . . C31 C 1.0688(5) 0.4500(4) -0.6060(3) 0.0318(15) Uani 1 1 d . . . H31 H 1.1015 0.5149 -0.6194 0.038 Uiso 1 1 calc R . . C32 C 1.0156(5) 0.3904(4) -0.5339(3) 0.0302(15) Uani 1 1 d . . . H32 H 1.0044 0.4066 -0.4889 0.036 Uiso 1 1 calc R . . C33 C 0.9817(5) 0.3020(4) -0.5397(3) 0.0216(13) Uani 1 1 d . . . C34 C 0.9166(5) 0.2182(4) -0.4858(3) 0.0198(13) Uani 1 1 d . . . C35 C 0.8876(5) 0.1393(4) -0.5061(3) 0.0237(14) Uani 1 1 d . . . C36 C 0.8303(5) 0.0468(4) -0.4619(3) 0.0298(15) Uani 1 1 d . . . H36 H 0.7989 0.0247 -0.4087 0.036 Uiso 1 1 calc R . . C37 C 0.8284(6) -0.0050(4) -0.5096(3) 0.0351(15) Uani 1 1 d . . . H37 H 0.7940 -0.0695 -0.4959 0.042 Uiso 1 1 calc R . . C38 C 0.8869(5) 0.0547(5) -0.5833(3) 0.0323(15) Uani 1 1 d . . . C39 C 0.9089(6) 0.0287(5) -0.6540(3) 0.0430(17) Uani 1 1 d . . . H39A H 0.8859 0.0844 -0.6952 0.064 Uiso 1 1 calc R . . H39B H 0.8559 -0.0288 -0.6458 0.064 Uiso 1 1 calc R . . H39C H 0.9994 0.0134 -0.6674 0.064 Uiso 1 1 calc R . . C40 C 0.8759(5) 0.2162(4) -0.4059(3) 0.0206(13) Uani 1 1 d . . . C41 C 0.7485(5) 0.1986(4) -0.3702(3) 0.0224(14) Uani 1 1 d . . . H41 H 0.6890 0.1840 -0.3959 0.027 Uiso 1 1 calc R . . C42 C 0.7068(5) 0.2019(4) -0.2983(3) 0.0236(14) Uani 1 1 d . . . H42 H 0.6188 0.1906 -0.2751 0.028 Uiso 1 1 calc R . . C43 C 0.7936(5) 0.2220(4) -0.2590(3) 0.0176(13) Uani 1 1 d . . . C44 C 0.9207(5) 0.2378(4) -0.2941(3) 0.0230(13) Uani 1 1 d . . . H44 H 0.9810 0.2506 -0.2681 0.028 Uiso 1 1 calc R . . C45 C 0.9611(5) 0.2351(4) -0.3664(3) 0.0188(13) Uani 1 1 d . . . H45 H 1.0490 0.2465 -0.3897 0.023 Uiso 1 1 calc R . . C46 C 0.7802(5) 0.0427(4) 0.0790(3) 0.0329(15) Uani 1 1 d . . . H46A H 0.7768 0.1010 0.0947 0.049 Uiso 1 1 calc R . . H46B H 0.8477 -0.0008 0.0989 0.049 Uiso 1 1 calc R . . H46C H 0.6976 0.0076 0.0988 0.049 Uiso 1 1 calc R . . C47 C 0.8084(5) 0.0737(4) -0.0054(3) 0.0195(13) Uani 1 1 d . . . C48 C 0.8831(5) 0.0262(4) -0.0522(3) 0.0208(13) Uani 1 1 d . . . H48 H 0.9316 -0.0316 -0.0364 0.025 Uiso 1 1 calc R . . C49 C 0.8730(5) 0.0783(4) -0.1243(3) 0.0205(13) Uani 1 1 d . . . H49 H 0.9136 0.0638 -0.1684 0.025 Uiso 1 1 calc R . . C50 C 0.7911(5) 0.1580(4) -0.1221(3) 0.0159(12) Uani 1 1 d . . . C51 C 0.7473(5) 0.2289(4) -0.1814(3) 0.0172(12) Uani 1 1 d . . . C52 C 0.6643(5) 0.3052(4) -0.1765(3) 0.0183(13) Uani 1 1 d . . . C53 C 0.6221(5) 0.3801(4) -0.2367(3) 0.0251(14) Uani 1 1 d . . . H53 H 0.6412 0.3848 -0.2885 0.030 Uiso 1 1 calc R . . C54 C 0.5497(5) 0.4438(4) -0.2073(3) 0.0287(14) Uani 1 1 d . . . H54 H 0.5090 0.5010 -0.2343 0.034 Uiso 1 1 calc R . . C55 C 0.5472(5) 0.4080(4) -0.1289(3) 0.0240(13) Uani 1 1 d . . . C56 C 0.4842(6) 0.4525(4) -0.0709(3) 0.0423(17) Uani 1 1 d . . . H56A H 0.3935 0.4629 -0.0734 0.063 Uiso 1 1 calc R . . H56B H 0.5259 0.5157 -0.0808 0.063 Uiso 1 1 calc R . . H56C H 0.4919 0.4081 -0.0205 0.063 Uiso 1 1 calc R . . C57 C 0.2555(6) 0.3063(5) -0.1602(4) 0.0514(19) Uani 1 1 d . . . H57A H 0.3033 0.2991 -0.1195 0.062 Uiso 1 1 calc R . . H57B H 0.3160 0.2953 -0.2032 0.062 Uiso 1 1 calc R . . C58 C 0.0966(6) 0.2586(5) 0.1395(3) 0.0476(18) Uani 1 1 d . . . H58A H 0.0338 0.2980 0.1629 0.057 Uiso 1 1 calc R . . H58B H 0.1469 0.2211 0.1778 0.057 Uiso 1 1 calc R . . B1 B 0.3519(6) 0.2880(5) 0.6286(3) 0.0240(16) Uani 1 1 d . . . B2 B 0.9957(6) 0.2262(5) -0.6478(3) 0.0276(17) Uani 1 1 d . . . N1 N 0.4038(4) 0.1962(3) 0.6082(2) 0.0219(11) Uani 1 1 d . . . N2 N 0.3548(4) 0.3722(3) 0.5532(2) 0.0223(11) Uani 1 1 d . . . N3 N 0.7204(4) 0.3129(3) 0.0475(2) 0.0190(10) Uani 1 1 d . . . N4 N 0.5043(4) 0.1863(3) 0.0791(2) 0.0188(10) Uani 1 1 d . . . N5 N 1.0140(4) 0.3086(3) -0.6160(2) 0.0234(11) Uani 1 1 d . . . N6 N 0.9212(4) 0.1410(3) -0.5808(2) 0.0234(11) Uani 1 1 d . . . N7 N 0.7532(4) 0.1533(3) -0.0462(2) 0.0180(10) Uani 1 1 d . . . N8 N 0.6132(4) 0.3250(3) -0.1098(2) 0.0218(11) Uani 1 1 d . . . F1 F 0.4308(3) 0.3113(2) 0.66994(15) 0.0302(8) Uani 1 1 d . . . F2 F 0.2288(3) 0.2710(2) 0.67044(16) 0.0354(8) Uani 1 1 d . . . F3 F 1.1113(3) 0.1943(2) -0.67713(16) 0.0380(9) Uani 1 1 d . . . F4 F 0.9230(3) 0.2613(2) -0.70356(16) 0.0364(8) Uani 1 1 d . . . Co1 Co 0.64340(7) 0.24643(5) -0.00803(4) 0.0191(2) Uani 1 1 d . . . Cl1 Cl 0.13340(19) 0.21760(13) -0.12722(10) 0.0617(5) Uani 1 1 d . . . Cl2 Cl 0.1972(2) 0.42439(13) -0.18893(11) 0.0714(6) Uani 1 1 d . . . Cl3 Cl 0.0148(3) 0.17650(19) 0.11675(18) 0.1298(12) Uani 1 1 d . . . Cl4 Cl 0.1974(3) 0.33652(19) 0.06461(16) 0.1431(14) 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 C1 0.050(4) 0.043(4) 0.017(3) 0.000(3) 0.000(3) -0.002(3) C2 0.032(4) 0.031(4) 0.025(3) -0.002(3) -0.007(3) -0.005(3) C3 0.047(4) 0.025(4) 0.024(3) -0.002(3) -0.003(3) -0.002(3) C4 0.032(4) 0.031(4) 0.025(3) -0.014(3) -0.004(3) 0.001(3) C5 0.021(3) 0.019(3) 0.020(3) -0.005(3) -0.006(2) -0.001(3) C6 0.012(3) 0.029(4) 0.019(3) -0.005(3) -0.003(2) 0.003(3) C7 0.023(3) 0.031(4) 0.017(3) -0.008(3) -0.007(2) 0.006(3) C8 0.039(4) 0.036(4) 0.013(3) -0.005(3) -0.007(3) 0.005(3) C9 0.038(4) 0.028(4) 0.038(4) -0.009(3) -0.016(3) 0.009(3) C10 0.029(4) 0.039(4) 0.032(4) -0.015(3) -0.014(3) 0.008(3) C11 0.043(4) 0.049(4) 0.045(4) -0.031(3) -0.011(3) 0.015(3) C12 0.025(4) 0.025(3) 0.015(3) -0.009(3) -0.005(3) 0.002(3) C13 0.017(3) 0.037(4) 0.017(3) -0.012(3) -0.006(2) 0.010(3) C14 0.024(4) 0.037(4) 0.026(3) -0.012(3) -0.010(3) 0.009(3) C15 0.015(3) 0.026(3) 0.017(3) -0.003(3) -0.005(2) -0.002(3) C16 0.018(3) 0.026(3) 0.017(3) -0.008(3) -0.003(2) -0.004(3) C17 0.024(4) 0.020(3) 0.021(3) -0.007(3) -0.009(3) 0.001(3) C18 0.042(4) 0.067(5) 0.031(4) -0.024(3) 0.013(3) -0.028(4) C19 0.024(4) 0.030(4) 0.023(3) -0.007(3) -0.001(3) -0.006(3) C20 0.025(3) 0.032(4) 0.027(3) -0.016(3) 0.000(3) -0.009(3) C21 0.029(4) 0.028(4) 0.019(3) -0.011(3) -0.001(3) -0.006(3) C22 0.022(3) 0.022(3) 0.012(3) -0.004(2) -0.003(2) -0.005(3) C23 0.014(3) 0.018(3) 0.017(3) -0.003(2) -0.007(2) 0.008(3) C24 0.011(3) 0.021(3) 0.009(3) -0.004(2) 0.002(2) -0.003(3) C25 0.026(4) 0.038(4) 0.018(3) -0.008(3) 0.000(3) -0.002(3) C26 0.031(4) 0.035(4) 0.032(3) -0.010(3) -0.004(3) -0.016(3) C27 0.025(4) 0.032(4) 0.023(3) -0.011(3) -0.003(3) -0.002(3) C28 0.034(4) 0.055(4) 0.040(4) -0.028(3) -0.006(3) -0.014(3) C29 0.033(4) 0.047(4) 0.027(3) -0.006(3) -0.004(3) -0.002(3) C30 0.021(3) 0.038(4) 0.022(3) -0.011(3) -0.004(3) 0.005(3) C31 0.034(4) 0.031(4) 0.030(4) -0.009(3) -0.006(3) -0.002(3) C32 0.033(4) 0.036(4) 0.022(3) -0.011(3) -0.004(3) 0.000(3) C33 0.019(3) 0.029(4) 0.018(3) -0.009(3) -0.001(2) -0.005(3) C34 0.010(3) 0.036(4) 0.015(3) -0.011(3) -0.006(2) 0.006(3) C35 0.024(3) 0.030(4) 0.020(3) -0.013(3) -0.003(3) 0.006(3) C36 0.028(4) 0.034(4) 0.027(3) -0.009(3) -0.009(3) 0.007(3) C37 0.041(4) 0.030(4) 0.041(4) -0.018(3) -0.012(3) 0.000(3) C38 0.032(4) 0.040(4) 0.036(4) -0.024(3) -0.014(3) 0.010(3) C39 0.052(5) 0.048(4) 0.041(4) -0.030(3) -0.012(3) 0.010(4) C40 0.020(3) 0.024(3) 0.018(3) -0.008(3) -0.001(3) 0.003(3) C41 0.028(4) 0.030(4) 0.015(3) -0.012(3) -0.009(3) 0.002(3) C42 0.023(3) 0.032(4) 0.017(3) -0.009(3) -0.003(2) 0.000(3) C43 0.023(4) 0.017(3) 0.014(3) -0.008(2) -0.004(3) 0.003(3) C44 0.022(4) 0.030(4) 0.020(3) -0.010(3) -0.006(3) -0.001(3) C45 0.014(3) 0.028(3) 0.016(3) -0.011(3) 0.001(2) -0.001(3) C46 0.041(4) 0.030(4) 0.025(3) -0.005(3) -0.011(3) 0.006(3) C47 0.021(3) 0.023(3) 0.015(3) -0.005(3) -0.006(2) -0.001(3) C48 0.017(3) 0.026(3) 0.022(3) -0.010(3) -0.009(2) 0.008(3) C49 0.015(3) 0.027(3) 0.024(3) -0.016(3) -0.001(2) 0.003(3) C50 0.012(3) 0.024(3) 0.014(3) -0.011(3) 0.000(2) -0.005(3) C51 0.011(3) 0.024(3) 0.017(3) -0.008(3) 0.000(2) -0.003(3) C52 0.021(3) 0.023(3) 0.012(3) -0.007(3) -0.003(2) -0.003(3) C53 0.032(4) 0.027(4) 0.014(3) -0.005(3) -0.005(3) 0.003(3) C54 0.033(4) 0.028(4) 0.024(3) -0.007(3) -0.008(3) 0.011(3) C55 0.023(3) 0.026(4) 0.025(3) -0.012(3) -0.002(3) 0.005(3) C56 0.055(5) 0.041(4) 0.031(4) -0.015(3) -0.008(3) 0.022(4) C57 0.047(5) 0.049(5) 0.059(5) -0.021(4) -0.006(4) -0.002(4) C58 0.060(5) 0.046(4) 0.038(4) -0.016(3) -0.008(3) 0.003(4) B1 0.017(4) 0.040(5) 0.019(3) -0.013(3) -0.008(3) 0.005(3) B2 0.026(4) 0.043(5) 0.018(3) -0.016(3) -0.003(3) -0.003(4) N1 0.024(3) 0.029(3) 0.011(2) -0.005(2) -0.0024(19) 0.001(2) N2 0.019(3) 0.029(3) 0.022(3) -0.011(2) -0.007(2) 0.007(2) N3 0.015(3) 0.028(3) 0.016(2) -0.011(2) 0.001(2) 0.003(2) N4 0.015(3) 0.024(3) 0.020(2) -0.011(2) -0.0020(19) -0.002(2) N5 0.019(3) 0.036(3) 0.015(2) -0.010(2) -0.003(2) 0.004(2) N6 0.021(3) 0.032(3) 0.023(3) -0.017(2) -0.004(2) 0.005(2) N7 0.016(3) 0.023(3) 0.016(2) -0.008(2) -0.0026(19) 0.001(2) N8 0.025(3) 0.022(3) 0.019(2) -0.007(2) -0.005(2) 0.007(2) F1 0.0295(19) 0.041(2) 0.0268(17) -0.0160(15) -0.0140(14) 0.0042(16) F2 0.020(2) 0.056(2) 0.0260(17) -0.0138(16) 0.0030(15) 0.0026(16) F3 0.024(2) 0.058(2) 0.0374(19) -0.0294(18) 0.0045(15) 0.0038(17) F4 0.033(2) 0.055(2) 0.0247(17) -0.0131(16) -0.0135(15) -0.0010(17) Co1 0.0201(4) 0.0255(5) 0.0127(4) -0.0085(3) -0.0019(3) 0.0012(4) Cl1 0.0761(14) 0.0409(11) 0.0626(12) -0.0148(9) -0.0025(10) -0.0132(10) Cl2 0.0848(15) 0.0397(12) 0.0733(13) -0.0237(10) 0.0315(11) -0.0089(10) Cl3 0.162(3) 0.096(2) 0.206(3) -0.106(2) -0.118(2) 0.0525(18) Cl4 0.106(2) 0.0900(19) 0.140(2) 0.0273(17) 0.0662(18) 0.0246(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 C1 C2 1.478(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.356(6) . ? C2 C3 1.395(7) . ? C3 C4 1.372(7) . ? C3 H3 0.9500 . ? C4 C5 1.405(7) . ? C4 H4 0.9500 . ? C5 N1 1.391(6) . ? C5 C6 1.393(7) . ? C6 C7 1.374(7) . ? C6 C12 1.493(7) . ? C7 N2 1.397(6) . ? C7 C8 1.413(7) . ? C8 C9 1.366(7) . ? C8 H8 0.9500 . ? C9 C10 1.391(7) . ? C9 H9 0.9500 . ? C10 N2 1.361(7) . ? C10 C11 1.490(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.391(7) . ? C12 C17 1.391(7) . ? C13 C14 1.369(7) . ? C13 H13 0.9500 . ? C14 C15 1.402(7) . ? C14 H14 0.9500 . ? C15 C16 1.372(6) . ? C15 C23 1.493(6) . ? C16 C17 1.382(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.483(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.332(6) . ? C19 C20 1.417(7) . ? C20 C21 1.356(7) . ? C20 H20 0.9500 . ? C21 C22 1.412(7) . ? C21 H21 0.9500 . ? C22 N3 1.400(6) . ? C22 C23 1.402(7) . ? C23 C24 1.404(7) . ? C24 N4 1.402(6) . ? C24 C25 1.408(7) . ? C25 C26 1.361(7) . ? C25 H25 0.9500 . ? C26 C27 1.402(7) . ? C26 H26 0.9500 . ? C27 N4 1.327(6) . ? C27 C28 1.495(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.486(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.351(7) . ? C30 C31 1.391(7) . ? C31 C32 1.379(7) . ? C31 H31 0.9500 . ? C32 C33 1.391(7) . ? C32 H32 0.9500 . ? C33 N5 1.401(6) . ? C33 C34 1.404(7) . ? C34 C35 1.389(7) . ? C34 C40 1.493(7) . ? C35 N6 1.394(6) . ? C35 C36 1.411(8) . ? C36 C37 1.365(7) . ? C36 H36 0.9500 . ? C37 C38 1.416(8) . ? C37 H37 0.9500 . ? C38 N6 1.336(7) . ? C38 C39 1.492(7) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.385(7) . ? C40 C41 1.386(7) . ? C41 C42 1.374(6) . ? C41 H41 0.9500 . ? C42 C43 1.403(7) . ? C42 H42 0.9500 . ? C43 C44 1.378(7) . ? C43 C51 1.501(6) . ? C44 C45 1.376(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.494(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N7 1.337(6) . ? C47 C48 1.404(7) . ? C48 C49 1.355(6) . ? C48 H48 0.9500 . ? C49 C50 1.413(7) . ? C49 H49 0.9500 . ? C50 C51 1.393(7) . ? C50 N7 1.406(6) . ? C51 C52 1.391(7) . ? C52 N8 1.399(6) . ? C52 C53 1.421(7) . ? C53 C54 1.361(7) . ? C53 H53 0.9500 . ? C54 C55 1.408(7) . ? C54 H54 0.9500 . ? C55 N8 1.336(6) . ? C55 C56 1.491(7) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 Cl2 1.729(7) . ? C57 Cl1 1.743(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl4 1.702(6) . ? C58 Cl3 1.724(7) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? B1 F2 1.378(7) . ? B1 F1 1.389(6) . ? B1 N2 1.540(7) . ? B1 N1 1.547(7) . ? B2 F3 1.370(7) . ? B2 F4 1.388(7) . ? B2 N5 1.544(8) . ? B2 N6 1.555(8) . ? N3 Co1 1.962(4) . ? N4 Co1 1.974(4) . ? N7 Co1 1.962(4) . ? N8 Co1 1.979(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.9(5) . . ? N1 C2 C1 123.4(5) . . ? C3 C2 C1 127.7(5) . . ? C4 C3 C2 107.8(5) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? C3 C4 C5 107.7(5) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? N1 C5 C6 121.4(5) . . ? N1 C5 C4 107.4(4) . . ? C6 C5 C4 131.2(5) . . ? C7 C6 C5 119.9(5) . . ? C7 C6 C12 120.5(5) . . ? C5 C6 C12 119.5(5) . . ? C6 C7 N2 121.9(5) . . ? C6 C7 C8 130.8(5) . . ? N2 C7 C8 107.2(5) . . ? C9 C8 C7 108.1(5) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? C8 C9 C10 107.5(5) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? N2 C10 C9 109.7(5) . . ? N2 C10 C11 121.6(5) . . ? C9 C10 C11 128.6(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.7(4) . . ? C13 C12 C6 119.5(5) . . ? C17 C12 C6 121.8(4) . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 121.3(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 117.5(5) . . ? C16 C15 C23 122.7(5) . . ? C14 C15 C23 119.7(4) . . ? C15 C16 C17 122.0(5) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C12 119.9(5) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 110.4(4) . . ? N3 C19 C18 121.3(5) . . ? C20 C19 C18 128.3(5) . . ? C21 C20 C19 107.0(5) . . ? C21 C20 H20 126.5 . . ? C19 C20 H20 126.5 . . ? C20 C21 C22 107.5(5) . . ? C20 C21 H21 126.2 . . ? C22 C21 H21 126.2 . . ? N3 C22 C23 123.7(5) . . ? N3 C22 C21 108.2(4) . . ? C23 C22 C21 128.1(5) . . ? C22 C23 C24 126.4(4) . . ? C22 C23 C15 116.2(5) . . ? C24 C23 C15 117.4(4) . . ? N4 C24 C23 124.2(4) . . ? N4 C24 C25 108.0(4) . . ? C23 C24 C25 127.8(4) . . ? C26 C25 C24 107.3(5) . . ? C26 C25 H25 126.3 . . ? C24 C25 H25 126.3 . . ? C25 C26 C27 107.1(5) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? N4 C27 C26 110.7(4) . . ? N4 C27 C28 121.0(5) . . ? C26 C27 C28 128.3(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C31 108.9(5) . . ? N5 C30 C29 123.4(5) . . ? C31 C30 C29 127.6(6) . . ? C32 C31 C30 108.3(5) . . ? C32 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? C31 C32 C33 106.9(5) . . ? C31 C32 H32 126.5 . . ? C33 C32 H32 126.5 . . ? C32 C33 N5 108.3(5) . . ? C32 C33 C34 131.5(5) . . ? N5 C33 C34 120.0(5) . . ? C35 C34 C33 121.0(5) . . ? C35 C34 C40 120.2(5) . . ? C33 C34 C40 118.7(5) . . ? C34 C35 N6 121.1(5) . . ? C34 C35 C36 131.0(5) . . ? N6 C35 C36 107.8(5) . . ? C37 C36 C35 107.2(5) . . ? C37 C36 H36 126.4 . . ? C35 C36 H36 126.4 . . ? C36 C37 C38 107.6(5) . . ? C36 C37 H37 126.2 . . ? C38 C37 H37 126.2 . . ? N6 C38 C37 109.1(5) . . ? N6 C38 C39 123.8(5) . . ? C37 C38 C39 127.2(6) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 118.2(5) . . ? C45 C40 C34 122.0(5) . . ? C41 C40 C34 119.8(4) . . ? C42 C41 C40 121.2(5) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C43 120.2(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 118.5(4) . . ? C44 C43 C51 121.3(4) . . ? C42 C43 C51 120.2(5) . . ? C45 C44 C43 120.8(5) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C40 121.2(5) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C48 110.9(4) . . ? N7 C47 C46 120.3(4) . . ? C48 C47 C46 128.6(5) . . ? C49 C48 C47 107.1(4) . . ? C49 C48 H48 126.5 . . ? C47 C48 H48 126.5 . . ? C48 C49 C50 107.7(4) . . ? C48 C49 H49 126.2 . . ? C50 C49 H49 126.2 . . ? C51 C50 N7 123.1(4) . . ? C51 C50 C49 128.9(4) . . ? N7 C50 C49 108.0(4) . . ? C52 C51 C50 127.0(4) . . ? C52 C51 C43 116.4(4) . . ? C50 C51 C43 116.6(4) . . ? C51 C52 N8 124.8(4) . . ? C51 C52 C53 127.7(4) . . ? N8 C52 C53 107.3(4) . . ? C54 C53 C52 108.2(4) . . ? C54 C53 H53 125.9 . . ? C52 C53 H53 125.9 . . ? C53 C54 C55 106.2(5) . . ? C53 C54 H54 126.9 . . ? C55 C54 H54 126.9 . . ? N8 C55 C54 111.2(4) . . ? N8 C55 C56 121.0(5) . . ? C54 C55 C56 127.9(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Cl2 C57 Cl1 112.0(4) . . ? Cl2 C57 H57A 109.2 . . ? Cl1 C57 H57A 109.2 . . ? Cl2 C57 H57B 109.2 . . ? Cl1 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? Cl4 C58 Cl3 114.2(4) . . ? Cl4 C58 H58A 108.7 . . ? Cl3 C58 H58A 108.7 . . ? Cl4 C58 H58B 108.7 . . ? Cl3 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? F2 B1 F1 109.5(4) . . ? F2 B1 N2 110.5(4) . . ? F1 B1 N2 110.1(5) . . ? F2 B1 N1 110.8(5) . . ? F1 B1 N1 109.3(4) . . ? N2 B1 N1 106.5(4) . . ? F3 B2 F4 109.9(4) . . ? F3 B2 N5 111.1(5) . . ? F4 B2 N5 109.2(5) . . ? F3 B2 N6 110.6(5) . . ? F4 B2 N6 109.4(5) . . ? N5 B2 N6 106.6(4) . . ? C2 N1 C5 108.2(4) . . ? C2 N1 B1 126.7(4) . . ? C5 N1 B1 125.1(4) . . ? C10 N2 C7 107.4(4) . . ? C10 N2 B1 127.5(4) . . ? C7 N2 B1 125.1(4) . . ? C19 N3 C22 106.9(4) . . ? C19 N3 Co1 126.3(3) . . ? C22 N3 Co1 126.6(3) . . ? C27 N4 C24 106.9(4) . . ? C27 N4 Co1 126.7(3) . . ? C24 N4 Co1 125.5(3) . . ? C30 N5 C33 107.6(4) . . ? C30 N5 B2 126.7(4) . . ? C33 N5 B2 125.8(5) . . ? C38 N6 C35 108.2(5) . . ? C38 N6 B2 126.5(4) . . ? C35 N6 B2 125.1(5) . . ? C47 N7 C50 106.3(4) . . ? C47 N7 Co1 126.9(3) . . ? C50 N7 Co1 126.8(3) . . ? C55 N8 C52 107.0(4) . . ? C55 N8 Co1 127.7(3) . . ? C52 N8 Co1 125.2(3) . . ? N3 Co1 N7 115.98(16) . . ? N3 Co1 N4 93.08(16) . . ? N7 Co1 N4 115.34(17) . . ? N3 Co1 N8 118.17(17) . . ? N7 Co1 N8 92.93(16) . . ? N4 Co1 N8 123.36(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -0.6(7) . . . . ? C1 C2 C3 C4 176.8(5) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 N1 1.8(6) . . . . ? C3 C4 C5 C6 -176.1(6) . . . . ? N1 C5 C6 C7 2.1(8) . . . . ? C4 C5 C6 C7 179.7(5) . . . . ? N1 C5 C6 C12 -174.5(4) . . . . ? C4 C5 C6 C12 3.1(9) . . . . ? C5 C6 C7 N2 -0.9(8) . . . . ? C12 C6 C7 N2 175.7(5) . . . . ? C5 C6 C7 C8 176.6(5) . . . . ? C12 C6 C7 C8 -6.8(9) . . . . ? C6 C7 C8 C9 -177.7(6) . . . . ? N2 C7 C8 C9 0.0(6) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 N2 0.3(6) . . . . ? C8 C9 C10 C11 179.4(6) . . . . ? C7 C6 C12 C13 -57.5(7) . . . . ? C5 C6 C12 C13 119.1(6) . . . . ? C7 C6 C12 C17 124.2(6) . . . . ? C5 C6 C12 C17 -59.2(7) . . . . ? C17 C12 C13 C14 -0.7(8) . . . . ? C6 C12 C13 C14 -179.0(5) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 1.1(8) . . . . ? C13 C14 C15 C23 -177.0(5) . . . . ? C14 C15 C16 C17 -0.8(8) . . . . ? C23 C15 C16 C17 177.2(5) . . . . ? C15 C16 C17 C12 -0.2(8) . . . . ? C13 C12 C17 C16 0.9(8) . . . . ? C6 C12 C17 C16 179.2(5) . . . . ? N3 C19 C20 C21 1.1(6) . . . . ? C18 C19 C20 C21 -179.6(6) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? C20 C21 C22 N3 0.8(6) . . . . ? C20 C21 C22 C23 -177.8(5) . . . . ? N3 C22 C23 C24 -1.7(8) . . . . ? C21 C22 C23 C24 176.7(5) . . . . ? N3 C22 C23 C15 180.0(4) . . . . ? C21 C22 C23 C15 -1.6(8) . . . . ? C16 C15 C23 C22 -56.0(7) . . . . ? C14 C15 C23 C22 122.0(5) . . . . ? C16 C15 C23 C24 125.6(5) . . . . ? C14 C15 C23 C24 -56.5(7) . . . . ? C22 C23 C24 N4 -4.4(8) . . . . ? C15 C23 C24 N4 173.9(4) . . . . ? C22 C23 C24 C25 173.7(5) . . . . ? C15 C23 C24 C25 -8.0(8) . . . . ? N4 C24 C25 C26 -0.3(6) . . . . ? C23 C24 C25 C26 -178.6(5) . . . . ? C24 C25 C26 C27 -0.2(6) . . . . ? C25 C26 C27 N4 0.6(7) . . . . ? C25 C26 C27 C28 -177.1(5) . . . . ? N5 C30 C31 C32 -0.5(6) . . . . ? C29 C30 C31 C32 177.3(5) . . . . ? C30 C31 C32 C33 0.5(6) . . . . ? C31 C32 C33 N5 -0.3(6) . . . . ? C31 C32 C33 C34 -175.0(5) . . . . ? C32 C33 C34 C35 176.7(6) . . . . ? N5 C33 C34 C35 2.5(7) . . . . ? C32 C33 C34 C40 -1.8(8) . . . . ? N5 C33 C34 C40 -176.0(4) . . . . ? C33 C34 C35 N6 -0.5(8) . . . . ? C40 C34 C35 N6 178.0(4) . . . . ? C33 C34 C35 C36 176.0(5) . . . . ? C40 C34 C35 C36 -5.5(9) . . . . ? C34 C35 C36 C37 -177.6(6) . . . . ? N6 C35 C36 C37 -0.8(6) . . . . ? C35 C36 C37 C38 1.2(6) . . . . ? C36 C37 C38 N6 -1.2(6) . . . . ? C36 C37 C38 C39 178.8(5) . . . . ? C35 C34 C40 C45 128.6(5) . . . . ? C33 C34 C40 C45 -52.9(7) . . . . ? C35 C34 C40 C41 -53.8(7) . . . . ? C33 C34 C40 C41 124.6(5) . . . . ? C45 C40 C41 C42 1.5(8) . . . . ? C34 C40 C41 C42 -176.2(5) . . . . ? C40 C41 C42 C43 -1.0(8) . . . . ? C41 C42 C43 C44 -0.2(8) . . . . ? C41 C42 C43 C51 178.0(5) . . . . ? C42 C43 C44 C45 0.8(8) . . . . ? C51 C43 C44 C45 -177.3(5) . . . . ? C43 C44 C45 C40 -0.3(8) . . . . ? C41 C40 C45 C44 -0.8(8) . . . . ? C34 C40 C45 C44 176.8(5) . . . . ? N7 C47 C48 C49 -0.2(6) . . . . ? C46 C47 C48 C49 175.7(5) . . . . ? C47 C48 C49 C50 -0.4(6) . . . . ? C48 C49 C50 C51 -176.7(5) . . . . ? C48 C49 C50 N7 0.8(6) . . . . ? N7 C50 C51 C52 1.4(8) . . . . ? C49 C50 C51 C52 178.5(5) . . . . ? N7 C50 C51 C43 -178.1(4) . . . . ? C49 C50 C51 C43 -1.0(8) . . . . ? C44 C43 C51 C52 113.9(5) . . . . ? C42 C43 C51 C52 -64.2(7) . . . . ? C44 C43 C51 C50 -66.6(7) . . . . ? C42 C43 C51 C50 115.3(5) . . . . ? C50 C51 C52 N8 2.0(8) . . . . ? C43 C51 C52 N8 -178.5(5) . . . . ? C50 C51 C52 C53 177.6(5) . . . . ? C43 C51 C52 C53 -2.9(8) . . . . ? C51 C52 C53 C54 -175.3(5) . . . . ? N8 C52 C53 C54 0.9(6) . . . . ? C52 C53 C54 C55 -0.1(6) . . . . ? C53 C54 C55 N8 -0.9(6) . . . . ? C53 C54 C55 C56 178.0(6) . . . . ? C3 C2 N1 C5 1.7(6) . . . . ? C1 C2 N1 C5 -175.9(5) . . . . ? C3 C2 N1 B1 -179.7(5) . . . . ? C1 C2 N1 B1 2.7(8) . . . . ? C6 C5 N1 C2 176.0(5) . . . . ? C4 C5 N1 C2 -2.1(6) . . . . ? C6 C5 N1 B1 -2.6(8) . . . . ? C4 C5 N1 B1 179.3(5) . . . . ? F2 B1 N1 C2 -56.5(7) . . . . ? F1 B1 N1 C2 64.3(7) . . . . ? N2 B1 N1 C2 -176.7(5) . . . . ? F2 B1 N1 C5 121.9(5) . . . . ? F1 B1 N1 C5 -117.3(5) . . . . ? N2 B1 N1 C5 1.6(7) . . . . ? C9 C10 N2 C7 -0.3(6) . . . . ? C11 C10 N2 C7 -179.5(5) . . . . ? C9 C10 N2 B1 177.8(5) . . . . ? C11 C10 N2 B1 -1.4(8) . . . . ? C6 C7 N2 C10 178.2(5) . . . . ? C8 C7 N2 C10 0.2(6) . . . . ? C6 C7 N2 B1 0.0(8) . . . . ? C8 C7 N2 B1 -177.9(5) . . . . ? F2 B1 N2 C10 61.5(7) . . . . ? F1 B1 N2 C10 -59.6(7) . . . . ? N1 B1 N2 C10 -178.1(5) . . . . ? F2 B1 N2 C7 -120.8(5) . . . . ? F1 B1 N2 C7 118.1(5) . . . . ? N1 B1 N2 C7 -0.3(7) . . . . ? C20 C19 N3 C22 -0.6(6) . . . . ? C18 C19 N3 C22 -179.9(5) . . . . ? C20 C19 N3 Co1 175.6(3) . . . . ? C18 C19 N3 Co1 -3.7(8) . . . . ? C23 C22 N3 C19 178.6(5) . . . . ? C21 C22 N3 C19 -0.1(6) . . . . ? C23 C22 N3 Co1 2.4(7) . . . . ? C21 C22 N3 Co1 -176.3(3) . . . . ? C26 C27 N4 C24 -0.8(6) . . . . ? C28 C27 N4 C24 177.1(5) . . . . ? C26 C27 N4 Co1 169.0(4) . . . . ? C28 C27 N4 Co1 -13.1(7) . . . . ? C23 C24 N4 C27 179.0(5) . . . . ? C25 C24 N4 C27 0.7(5) . . . . ? C23 C24 N4 Co1 9.1(7) . . . . ? C25 C24 N4 Co1 -169.3(3) . . . . ? C31 C30 N5 C33 0.3(6) . . . . ? C29 C30 N5 C33 -177.7(5) . . . . ? C31 C30 N5 B2 -178.2(5) . . . . ? C29 C30 N5 B2 3.8(8) . . . . ? C32 C33 N5 C30 0.0(6) . . . . ? C34 C33 N5 C30 175.4(5) . . . . ? C32 C33 N5 B2 178.6(5) . . . . ? C34 C33 N5 B2 -6.0(7) . . . . ? F3 B2 N5 C30 64.1(7) . . . . ? F4 B2 N5 C30 -57.3(7) . . . . ? N6 B2 N5 C30 -175.4(4) . . . . ? F3 B2 N5 C33 -114.1(5) . . . . ? F4 B2 N5 C33 124.5(5) . . . . ? N6 B2 N5 C33 6.4(7) . . . . ? C37 C38 N6 C35 0.7(6) . . . . ? C39 C38 N6 C35 -179.3(5) . . . . ? C37 C38 N6 B2 176.1(5) . . . . ? C39 C38 N6 B2 -3.9(8) . . . . ? C34 C35 N6 C38 177.3(5) . . . . ? C36 C35 N6 C38 0.1(6) . . . . ? C34 C35 N6 B2 1.8(8) . . . . ? C36 C35 N6 B2 -175.5(5) . . . . ? F3 B2 N6 C38 -58.1(7) . . . . ? F4 B2 N6 C38 63.1(7) . . . . ? N5 B2 N6 C38 -178.9(5) . . . . ? F3 B2 N6 C35 116.6(5) . . . . ? F4 B2 N6 C35 -122.2(5) . . . . ? N5 B2 N6 C35 -4.2(7) . . . . ? C48 C47 N7 C50 0.7(6) . . . . ? C46 C47 N7 C50 -175.6(5) . . . . ? C48 C47 N7 Co1 -178.3(3) . . . . ? C46 C47 N7 Co1 5.4(7) . . . . ? C51 C50 N7 C47 176.8(5) . . . . ? C49 C50 N7 C47 -0.9(5) . . . . ? C51 C50 N7 Co1 -4.2(7) . . . . ? C49 C50 N7 Co1 178.1(3) . . . . ? C54 C55 N8 C52 1.4(6) . . . . ? C56 C55 N8 C52 -177.5(5) . . . . ? C54 C55 N8 Co1 178.5(4) . . . . ? C56 C55 N8 Co1 -0.5(8) . . . . ? C51 C52 N8 C55 174.9(5) . . . . ? C53 C52 N8 C55 -1.4(6) . . . . ? C51 C52 N8 Co1 -2.2(7) . . . . ? C53 C52 N8 Co1 -178.6(3) . . . . ? C19 N3 Co1 N7 65.6(5) . . . . ? C22 N3 Co1 N7 -118.9(4) . . . . ? C19 N3 Co1 N4 -174.2(4) . . . . ? C22 N3 Co1 N4 1.3(4) . . . . ? C19 N3 Co1 N8 -43.4(5) . . . . ? C22 N3 Co1 N8 132.1(4) . . . . ? C47 N7 Co1 N3 58.6(5) . . . . ? C50 N7 Co1 N3 -120.2(4) . . . . ? C47 N7 Co1 N4 -48.7(5) . . . . ? C50 N7 Co1 N4 132.5(4) . . . . ? C47 N7 Co1 N8 -178.0(4) . . . . ? C50 N7 Co1 N8 3.2(4) . . . . ? C27 N4 Co1 N3 -174.6(4) . . . . ? C24 N4 Co1 N3 -6.7(4) . . . . ? C27 N4 Co1 N7 -53.9(5) . . . . ? C24 N4 Co1 N7 114.0(4) . . . . ? C27 N4 Co1 N8 58.4(5) . . . . ? C24 N4 Co1 N8 -133.7(4) . . . . ? C55 N8 Co1 N3 -55.0(5) . . . . ? C52 N8 Co1 N3 121.5(4) . . . . ? C55 N8 Co1 N7 -176.7(4) . . . . ? C52 N8 Co1 N7 -0.2(4) . . . . ? C55 N8 Co1 N4 60.2(5) . . . . ? C52 N8 Co1 N4 -123.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.228 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.080 #===End data_compound15 _database_code_depnum_ccdc_archive 'CCDC 684029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H52 B2 Cl4 F4 N8 Zn' _chemical_formula_weight 1165.87 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7063(11) _cell_length_b 14.4785(12) _cell_length_c 19.1263(18) _cell_angle_alpha 70.425(4) _cell_angle_beta 78.184(4) _cell_angle_gamma 86.994(4) _cell_volume 2733.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6794 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.61 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18068 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.19 _reflns_number_total 18068 _reflns_number_gt 10208 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^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 18068 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2276(4) -0.0027(3) -0.6085(2) 0.0435(12) Uani 1 1 d . . . H1A H 1.1651 0.0106 -0.6414 0.065 Uiso 1 1 calc R . . H1B H 1.2417 -0.0734 -0.5894 0.065 Uiso 1 1 calc R . . H1C H 1.3083 0.0313 -0.6373 0.065 Uiso 1 1 calc R . . C2 C 1.1785(4) 0.0329(3) -0.5434(2) 0.0337(11) Uani 1 1 d . . . C3 C 1.1576(4) -0.0206(3) -0.4663(2) 0.0363(11) Uani 1 1 d . . . H3 H 1.1733 -0.0884 -0.4446 0.044 Uiso 1 1 calc R . . C4 C 1.1109(4) 0.0413(3) -0.4280(2) 0.0328(11) Uani 1 1 d . . . H4 H 1.0873 0.0242 -0.3745 0.039 Uiso 1 1 calc R . . C5 C 1.1033(4) 0.1350(3) -0.4805(2) 0.0247(10) Uani 1 1 d . . . C6 C 1.0582(4) 0.2229(3) -0.4718(2) 0.0226(10) Uani 1 1 d . . . C7 C 1.0523(4) 0.3058(3) -0.5344(2) 0.0233(10) Uani 1 1 d . . . C8 C 1.0140(4) 0.4017(3) -0.5406(2) 0.0306(11) Uani 1 1 d . . . H8 H 0.9795 0.4245 -0.4996 0.037 Uiso 1 1 calc R . . C9 C 1.0346(4) 0.4570(3) -0.6159(2) 0.0355(11) Uani 1 1 d . . . H9 H 1.0164 0.5246 -0.6363 0.043 Uiso 1 1 calc R . . C10 C 1.0874(4) 0.3961(3) -0.6572(2) 0.0314(11) Uani 1 1 d . . . C11 C 1.1329(5) 0.4226(3) -0.7399(2) 0.0444(13) Uani 1 1 d . . . H11A H 1.2262 0.4197 -0.7512 0.067 Uiso 1 1 calc R . . H11B H 1.1062 0.4892 -0.7650 0.067 Uiso 1 1 calc R . . H11C H 1.0965 0.3765 -0.7582 0.067 Uiso 1 1 calc R . . C12 C 1.0208(4) 0.2311(3) -0.3947(2) 0.0234(10) Uani 1 1 d . . . C13 C 1.1102(4) 0.2095(3) -0.3481(2) 0.0270(10) Uani 1 1 d . . . H13 H 1.1927 0.1886 -0.3656 0.032 Uiso 1 1 calc R . . C14 C 1.0804(4) 0.2181(3) -0.2769(2) 0.0297(10) Uani 1 1 d . . . H14 H 1.1430 0.2039 -0.2462 0.036 Uiso 1 1 calc R . . C15 C 0.9593(4) 0.2474(3) -0.24938(19) 0.0194(9) Uani 1 1 d . . . C16 C 0.8714(4) 0.2692(3) -0.2965(2) 0.0222(9) Uani 1 1 d . . . H16 H 0.7888 0.2901 -0.2791 0.027 Uiso 1 1 calc R . . C17 C 0.9011(4) 0.2615(3) -0.3682(2) 0.0225(9) Uani 1 1 d . . . H17 H 0.8391 0.2771 -0.3994 0.027 Uiso 1 1 calc R . . C18 C 1.1038(5) 0.3978(3) -0.0142(2) 0.0455(13) Uani 1 1 d . . . H18A H 1.0291 0.3745 0.0267 0.068 Uiso 1 1 calc R . . H18B H 1.1159 0.4685 -0.0260 0.068 Uiso 1 1 calc R . . H18C H 1.1797 0.3634 0.0019 0.068 Uiso 1 1 calc R . . C19 C 1.0837(4) 0.3783(3) -0.0826(2) 0.0289(10) Uani 1 1 d . . . C20 C 1.1509(4) 0.4190(3) -0.1575(2) 0.0365(12) Uani 1 1 d . . . H20 H 1.2169 0.4676 -0.1750 0.044 Uiso 1 1 calc R . . C21 C 1.1041(4) 0.3759(3) -0.2009(2) 0.0311(11) Uani 1 1 d . . . H21 H 1.1325 0.3879 -0.2536 0.037 Uiso 1 1 calc R . . C22 C 1.0047(4) 0.3097(3) -0.1517(2) 0.0188(9) Uani 1 1 d . . . C23 C 0.9267(4) 0.2506(3) -0.17053(19) 0.0188(9) Uani 1 1 d . . . C24 C 0.8222(4) 0.1925(3) -0.1225(2) 0.0207(9) Uani 1 1 d . . . C25 C 0.7459(4) 0.1285(3) -0.1387(2) 0.0291(10) Uani 1 1 d . . . H25 H 0.7542 0.1173 -0.1856 0.035 Uiso 1 1 calc R . . C26 C 0.6581(4) 0.0858(3) -0.0744(2) 0.0334(11) Uani 1 1 d . . . H26 H 0.5934 0.0396 -0.0682 0.040 Uiso 1 1 calc R . . C27 C 0.6812(4) 0.1227(3) -0.0192(2) 0.0318(11) Uani 1 1 d . . . C28 C 0.6108(5) 0.0992(4) 0.0608(2) 0.0535(15) Uani 1 1 d . . . H28A H 0.6484 0.1368 0.0857 0.080 Uiso 1 1 calc R . . H28B H 0.6168 0.0289 0.0878 0.080 Uiso 1 1 calc R . . H28C H 0.5209 0.1164 0.0613 0.080 Uiso 1 1 calc R . . C29 C 0.3929(4) 0.0650(3) 0.7390(2) 0.0429(13) Uani 1 1 d . . . H29A H 0.4673 0.0418 0.7622 0.064 Uiso 1 1 calc R . . H29B H 0.3311 0.0109 0.7540 0.064 Uiso 1 1 calc R . . H29C H 0.3533 0.1183 0.7561 0.064 Uiso 1 1 calc R . . C30 C 0.4339(4) 0.1012(3) 0.6556(2) 0.0316(11) Uani 1 1 d . . . C31 C 0.4308(4) 0.0498(3) 0.6063(2) 0.0344(11) Uani 1 1 d . . . H31 H 0.3978 -0.0148 0.6197 0.041 Uiso 1 1 calc R . . C32 C 0.4843(4) 0.1099(3) 0.5343(2) 0.0319(11) Uani 1 1 d . . . H32 H 0.4957 0.0936 0.4893 0.038 Uiso 1 1 calc R . . C33 C 0.5186(4) 0.1982(3) 0.5395(2) 0.0229(10) Uani 1 1 d . . . C34 C 0.5835(4) 0.2822(3) 0.4851(2) 0.0234(10) Uani 1 1 d . . . C35 C 0.6120(4) 0.3615(3) 0.5053(2) 0.0257(10) Uani 1 1 d . . . C36 C 0.6704(4) 0.4535(3) 0.4617(2) 0.0332(11) Uani 1 1 d . . . H36 H 0.7030 0.4755 0.4086 0.040 Uiso 1 1 calc R . . C37 C 0.6717(4) 0.5050(3) 0.5094(3) 0.0371(12) Uani 1 1 d . . . H37 H 0.7056 0.5693 0.4957 0.044 Uiso 1 1 calc R . . C38 C 0.6142(4) 0.4461(3) 0.5823(2) 0.0342(11) Uani 1 1 d . . . C39 C 0.5924(5) 0.4720(3) 0.6536(2) 0.0496(14) Uani 1 1 d . . . H39A H 0.5005 0.4733 0.6733 0.074 Uiso 1 1 calc R . . H39B H 0.6305 0.5367 0.6426 0.074 Uiso 1 1 calc R . . H39C H 0.6321 0.4229 0.6916 0.074 Uiso 1 1 calc R . . C40 C 0.6242(4) 0.2838(3) 0.4058(2) 0.0215(9) Uani 1 1 d . . . C41 C 0.7523(4) 0.3018(3) 0.3697(2) 0.0258(10) Uani 1 1 d . . . H41 H 0.8118 0.3167 0.3952 0.031 Uiso 1 1 calc R . . C42 C 0.7927(4) 0.2981(3) 0.2980(2) 0.0226(9) Uani 1 1 d . . . H42 H 0.8804 0.3094 0.2747 0.027 Uiso 1 1 calc R . . C43 C 0.7068(4) 0.2778(3) 0.2582(2) 0.0184(9) Uani 1 1 d . . . C44 C 0.5790(4) 0.2619(3) 0.2941(2) 0.0256(10) Uani 1 1 d . . . H44 H 0.5186 0.2493 0.2682 0.031 Uiso 1 1 calc R . . C45 C 0.5386(4) 0.2642(3) 0.3665(2) 0.0259(10) Uani 1 1 d . . . H45 H 0.4511 0.2522 0.3901 0.031 Uiso 1 1 calc R . . C46 C 1.0167(5) 0.0472(3) 0.0707(2) 0.0474(14) Uani 1 1 d . . . H46A H 1.0042 0.0889 0.0205 0.071 Uiso 1 1 calc R . . H46B H 0.9786 -0.0178 0.0828 0.071 Uiso 1 1 calc R . . H46C H 1.1082 0.0408 0.0708 0.071 Uiso 1 1 calc R . . C47 C 0.9541(4) 0.0924(3) 0.1286(2) 0.0259(10) Uani 1 1 d . . . C48 C 0.9503(4) 0.0570(3) 0.2066(2) 0.0320(11) Uani 1 1 d . . . H48 H 0.9906 0.0001 0.2337 0.038 Uiso 1 1 calc R . . C49 C 0.8771(4) 0.1205(3) 0.2363(2) 0.0267(10) Uani 1 1 d . . . H49 H 0.8579 0.1160 0.2881 0.032 Uiso 1 1 calc R . . C50 C 0.8352(4) 0.1940(3) 0.1762(2) 0.0197(9) Uani 1 1 d . . . C51 C 0.7535(4) 0.2707(3) 0.1809(2) 0.0212(9) Uani 1 1 d . . . C52 C 0.7082(4) 0.3418(3) 0.12165(19) 0.0183(9) Uani 1 1 d . . . C53 C 0.6273(4) 0.4214(3) 0.1245(2) 0.0242(10) Uani 1 1 d . . . H53 H 0.5876 0.4356 0.1689 0.029 Uiso 1 1 calc R . . C54 C 0.6165(4) 0.4736(3) 0.0526(2) 0.0271(10) Uani 1 1 d . . . H54 H 0.5683 0.5312 0.0369 0.033 Uiso 1 1 calc R . . C55 C 0.6905(4) 0.4258(3) 0.0058(2) 0.0258(10) Uani 1 1 d . . . C56 C 0.7193(4) 0.4571(3) -0.0796(2) 0.0383(12) Uani 1 1 d . . . H56A H 0.7992 0.4955 -0.0994 0.057 Uiso 1 1 calc R . . H56B H 0.6496 0.4973 -0.0993 0.057 Uiso 1 1 calc R . . H56C H 0.7277 0.3990 -0.0954 0.057 Uiso 1 1 calc R . . C57 C 1.4028(5) 0.2410(4) -0.1385(3) 0.0568(15) Uani 1 1 d . . . H57A H 1.3536 0.2782 -0.1773 0.068 Uiso 1 1 calc R . . H57B H 1.4660 0.2018 -0.1615 0.068 Uiso 1 1 calc R . . C58 C 1.2455(5) 0.1940(4) 0.1595(3) 0.0618(16) Uani 1 1 d . . . H58A H 1.1844 0.2050 0.2023 0.074 Uiso 1 1 calc R . . H58B H 1.1990 0.2012 0.1183 0.074 Uiso 1 1 calc R . . B1 B 1.1480(5) 0.2115(4) -0.6286(2) 0.0262(12) Uani 1 1 d . . . B2 B 0.5052(5) 0.2736(4) 0.6473(3) 0.0327(13) Uani 1 1 d . . . N1 N 1.1459(3) 0.1272(2) -0.55298(17) 0.0250(8) Uani 1 1 d . . . N2 N 1.0969(3) 0.3041(2) -0.60825(17) 0.0250(8) Uani 1 1 d . . . N3 N 0.9959(3) 0.3144(2) -0.07876(16) 0.0204(7) Uani 1 1 d . . . N4 N 0.7785(3) 0.1867(2) -0.04728(16) 0.0240(8) Uani 1 1 d . . . N5 N 0.4861(3) 0.1922(2) 0.61579(17) 0.0276(8) Uani 1 1 d . . . N6 N 0.5790(3) 0.3593(2) 0.58074(17) 0.0278(8) Uani 1 1 d . . . N7 N 0.8872(3) 0.1747(2) 0.10920(16) 0.0222(8) Uani 1 1 d . . . N8 N 0.7454(3) 0.3473(2) 0.04598(16) 0.0217(8) Uani 1 1 d . . . F1 F 1.2714(2) 0.22970(17) -0.67051(12) 0.0393(6) Uani 1 1 d . . . F2 F 1.0698(2) 0.18877(16) -0.67006(12) 0.0333(6) Uani 1 1 d . . . F3 F 0.5775(2) 0.23933(18) 0.70318(12) 0.0430(7) Uani 1 1 d . . . F4 F 0.3895(2) 0.30653(18) 0.67691(13) 0.0441(7) Uani 1 1 d . . . Zn1 Zn 0.85662(5) 0.25335(3) 0.00804(2) 0.02388(15) Uani 1 1 d . . . Cl1 Cl 1.4841(3) 0.32373(15) -0.11607(15) 0.1516(10) Uani 1 1 d . . . Cl2 Cl 1.3021(2) 0.16377(15) -0.06583(13) 0.1644(12) Uani 1 1 d . . . Cl3 Cl 1.30250(16) 0.07579(10) 0.18883(9) 0.0794(5) Uani 1 1 d . . . Cl4 Cl 1.36682(15) 0.28197(10) 0.12758(8) 0.0681(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 C1 0.043(3) 0.051(3) 0.049(3) -0.032(3) -0.013(2) 0.017(2) C2 0.031(3) 0.039(3) 0.039(3) -0.020(2) -0.014(2) 0.009(2) C3 0.045(3) 0.027(3) 0.037(3) -0.008(2) -0.016(2) 0.011(2) C4 0.044(3) 0.033(3) 0.016(2) -0.001(2) -0.007(2) 0.006(2) C5 0.026(3) 0.031(3) 0.019(2) -0.010(2) -0.0061(18) 0.002(2) C6 0.020(2) 0.032(3) 0.016(2) -0.007(2) -0.0032(17) -0.0017(18) C7 0.030(3) 0.025(2) 0.014(2) -0.0059(19) -0.0011(18) -0.0036(19) C8 0.041(3) 0.025(3) 0.025(2) -0.009(2) -0.003(2) 0.001(2) C9 0.050(3) 0.020(3) 0.032(3) -0.002(2) -0.006(2) -0.004(2) C10 0.032(3) 0.032(3) 0.025(2) 0.000(2) -0.005(2) -0.010(2) C11 0.057(4) 0.045(3) 0.018(2) 0.003(2) 0.001(2) -0.007(2) C12 0.028(3) 0.025(2) 0.015(2) -0.0049(19) -0.0035(18) 0.0032(19) C13 0.022(3) 0.039(3) 0.021(2) -0.015(2) -0.0020(18) 0.007(2) C14 0.030(3) 0.041(3) 0.020(2) -0.011(2) -0.0103(19) 0.013(2) C15 0.022(2) 0.018(2) 0.014(2) -0.0021(17) -0.0021(17) 0.0007(17) C16 0.022(2) 0.020(2) 0.022(2) -0.0067(19) -0.0005(18) 0.0007(18) C17 0.027(3) 0.023(2) 0.018(2) -0.0050(19) -0.0099(18) 0.0041(18) C18 0.046(3) 0.058(3) 0.043(3) -0.030(3) -0.004(2) -0.016(3) C19 0.031(3) 0.032(3) 0.027(2) -0.014(2) -0.003(2) -0.003(2) C20 0.039(3) 0.031(3) 0.039(3) -0.010(2) -0.005(2) -0.016(2) C21 0.035(3) 0.035(3) 0.020(2) -0.006(2) -0.002(2) -0.004(2) C22 0.020(2) 0.018(2) 0.018(2) -0.0052(18) -0.0038(17) 0.0006(18) C23 0.025(2) 0.016(2) 0.014(2) -0.0049(17) -0.0048(17) 0.0096(18) C24 0.025(2) 0.023(2) 0.015(2) -0.0065(18) -0.0039(18) 0.0004(19) C25 0.039(3) 0.027(3) 0.020(2) -0.008(2) -0.002(2) -0.005(2) C26 0.036(3) 0.033(3) 0.031(3) -0.012(2) 0.000(2) -0.016(2) C27 0.033(3) 0.036(3) 0.025(2) -0.011(2) 0.000(2) -0.004(2) C28 0.059(4) 0.067(4) 0.031(3) -0.021(3) 0.014(2) -0.034(3) C29 0.045(3) 0.048(3) 0.023(3) 0.001(2) -0.001(2) -0.002(2) C30 0.025(3) 0.041(3) 0.024(2) -0.006(2) -0.0038(19) 0.005(2) C31 0.039(3) 0.028(3) 0.034(3) -0.012(2) -0.002(2) -0.001(2) C32 0.035(3) 0.036(3) 0.024(2) -0.012(2) -0.001(2) 0.000(2) C33 0.024(2) 0.030(3) 0.017(2) -0.010(2) -0.0025(18) 0.0014(19) C34 0.021(2) 0.032(3) 0.020(2) -0.011(2) -0.0053(18) 0.0076(19) C35 0.025(3) 0.033(3) 0.020(2) -0.012(2) -0.0015(18) 0.007(2) C36 0.036(3) 0.036(3) 0.030(3) -0.015(2) -0.004(2) 0.003(2) C37 0.041(3) 0.028(3) 0.050(3) -0.021(2) -0.011(2) 0.002(2) C38 0.032(3) 0.038(3) 0.043(3) -0.026(2) -0.011(2) 0.007(2) C39 0.059(4) 0.055(3) 0.049(3) -0.036(3) -0.014(3) 0.008(3) C40 0.027(3) 0.021(2) 0.016(2) -0.0068(18) -0.0011(18) 0.0016(18) C41 0.029(3) 0.031(3) 0.022(2) -0.014(2) -0.0074(19) 0.0035(19) C42 0.022(2) 0.025(2) 0.020(2) -0.0079(19) 0.0001(18) -0.0018(18) C43 0.024(2) 0.014(2) 0.016(2) -0.0060(17) 0.0002(17) 0.0015(17) C44 0.031(3) 0.030(2) 0.019(2) -0.0126(19) -0.0055(19) 0.0012(19) C45 0.026(3) 0.029(3) 0.022(2) -0.008(2) -0.0021(19) -0.0039(19) C46 0.065(4) 0.039(3) 0.034(3) -0.014(2) -0.005(2) 0.026(3) C47 0.032(3) 0.021(2) 0.024(2) -0.010(2) -0.0006(19) 0.0016(19) C48 0.041(3) 0.022(2) 0.026(2) 0.000(2) -0.007(2) 0.009(2) C49 0.033(3) 0.028(3) 0.018(2) -0.007(2) -0.0043(19) 0.001(2) C50 0.026(2) 0.019(2) 0.014(2) -0.0087(18) -0.0008(17) 0.0027(18) C51 0.023(2) 0.023(2) 0.019(2) -0.0106(19) 0.0004(18) -0.0053(18) C52 0.021(2) 0.021(2) 0.014(2) -0.0083(18) -0.0025(17) 0.0004(18) C53 0.024(2) 0.024(2) 0.024(2) -0.010(2) 0.0005(18) -0.0005(18) C54 0.031(3) 0.025(2) 0.023(2) -0.007(2) -0.0048(19) 0.0047(19) C55 0.027(3) 0.030(3) 0.019(2) -0.005(2) -0.0051(19) 0.001(2) C56 0.048(3) 0.037(3) 0.026(2) -0.006(2) -0.008(2) 0.008(2) C57 0.074(4) 0.056(3) 0.044(3) -0.022(3) -0.014(3) 0.011(3) C58 0.062(4) 0.057(4) 0.069(4) -0.027(3) -0.005(3) -0.009(3) B1 0.022(3) 0.040(3) 0.020(3) -0.015(2) -0.002(2) 0.003(2) B2 0.029(3) 0.054(4) 0.020(3) -0.019(3) -0.005(2) 0.004(3) N1 0.027(2) 0.029(2) 0.0207(19) -0.0097(16) -0.0062(15) 0.0062(16) N2 0.031(2) 0.027(2) 0.0141(18) -0.0028(16) -0.0025(15) -0.0021(16) N3 0.022(2) 0.0239(19) 0.0166(17) -0.0109(15) 0.0006(14) -0.0014(15) N4 0.025(2) 0.028(2) 0.0141(18) -0.0071(16) 0.0063(15) -0.0024(16) N5 0.026(2) 0.038(2) 0.0187(19) -0.0109(18) -0.0026(15) 0.0037(17) N6 0.031(2) 0.034(2) 0.026(2) -0.0175(17) -0.0091(16) 0.0066(17) N7 0.028(2) 0.0212(19) 0.0166(18) -0.0050(15) -0.0066(15) 0.0080(15) N8 0.026(2) 0.024(2) 0.0142(18) -0.0052(15) -0.0036(15) 0.0024(15) F1 0.0280(15) 0.0572(17) 0.0272(14) -0.0126(12) 0.0045(11) 0.0004(12) F2 0.0377(16) 0.0410(15) 0.0285(13) -0.0164(12) -0.0144(11) 0.0017(11) F3 0.0439(17) 0.0642(18) 0.0248(14) -0.0156(13) -0.0135(12) -0.0026(13) F4 0.0311(16) 0.0666(18) 0.0406(15) -0.0329(14) 0.0051(12) 0.0036(13) Zn1 0.0291(3) 0.0281(3) 0.0148(2) -0.0095(2) -0.0019(2) 0.0029(2) Cl1 0.198(3) 0.1100(16) 0.236(3) -0.1232(18) -0.145(2) 0.0659(15) Cl2 0.1219(19) 0.1040(15) 0.157(2) 0.0337(14) 0.0766(16) 0.0339(13) Cl3 0.0927(13) 0.0457(9) 0.0824(11) -0.0266(8) 0.0329(9) -0.0092(8) Cl4 0.0833(12) 0.0474(9) 0.0675(10) -0.0169(7) -0.0016(8) -0.0130(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.492(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.351(5) . ? C2 C3 1.392(5) . ? C3 C4 1.355(5) . ? C3 H3 0.9500 . ? C4 C5 1.401(5) . ? C4 H4 0.9500 . ? C5 C6 1.388(5) . ? C5 N1 1.407(5) . ? C6 C7 1.391(5) . ? C6 C12 1.490(5) . ? C7 C8 1.399(5) . ? C7 N2 1.405(4) . ? C8 C9 1.371(5) . ? C8 H8 0.9500 . ? C9 C10 1.398(6) . ? C9 H9 0.9500 . ? C10 N2 1.360(5) . ? C10 C11 1.477(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.385(5) . ? C12 C13 1.392(5) . ? C13 C14 1.380(5) . ? C13 H13 0.9500 . ? C14 C15 1.397(5) . ? C14 H14 0.9500 . ? C15 C16 1.386(5) . ? C15 C23 1.493(5) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.487(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.327(5) . ? C19 C20 1.405(5) . ? C20 C21 1.370(5) . ? C20 H20 0.9500 . ? C21 C22 1.424(5) . ? C21 H21 0.9500 . ? C22 C23 1.402(5) . ? C22 N3 1.403(4) . ? C23 C24 1.401(5) . ? C24 N4 1.394(4) . ? C24 C25 1.414(5) . ? C25 C26 1.362(5) . ? C25 H25 0.9500 . ? C26 C27 1.400(5) . ? C26 H26 0.9500 . ? C27 N4 1.331(5) . ? C27 C28 1.493(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.481(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.363(5) . ? C30 C31 1.388(5) . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 C33 1.389(5) . ? C32 H32 0.9500 . ? C33 N5 1.403(4) . ? C33 C34 1.410(5) . ? C34 C35 1.394(5) . ? C34 C40 1.483(5) . ? C35 N6 1.404(5) . ? C35 C36 1.411(6) . ? C36 C37 1.361(5) . ? C36 H36 0.9500 . ? C37 C38 1.399(6) . ? C37 H37 0.9500 . ? C38 N6 1.342(5) . ? C38 C39 1.503(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.391(5) . ? C40 C41 1.398(5) . ? C41 C42 1.370(5) . ? C41 H41 0.9500 . ? C42 C43 1.405(5) . ? C42 H42 0.9500 . ? C43 C44 1.393(5) . ? C43 C51 1.497(5) . ? C44 C45 1.375(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.498(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N7 1.339(5) . ? C47 C48 1.397(5) . ? C48 C49 1.368(5) . ? C48 H48 0.9500 . ? C49 C50 1.413(5) . ? C49 H49 0.9500 . ? C50 C51 1.393(5) . ? C50 N7 1.400(4) . ? C51 C52 1.404(5) . ? C52 N8 1.397(4) . ? C52 C53 1.414(5) . ? C53 C54 1.355(5) . ? C53 H53 0.9500 . ? C54 C55 1.407(5) . ? C54 H54 0.9500 . ? C55 N8 1.326(5) . ? C55 C56 1.508(5) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 Cl2 1.678(5) . ? C57 Cl1 1.726(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl3 1.733(5) . ? C58 Cl4 1.735(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? B1 F2 1.384(5) . ? B1 F1 1.385(5) . ? B1 N1 1.545(5) . ? B1 N2 1.559(5) . ? B2 F4 1.383(5) . ? B2 F3 1.389(5) . ? B2 N5 1.533(6) . ? B2 N6 1.555(6) . ? N3 Zn1 1.975(3) . ? N4 Zn1 1.970(3) . ? N7 Zn1 1.972(3) . ? N8 Zn1 1.982(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.5(4) . . ? N1 C2 C1 122.4(4) . . ? C3 C2 C1 128.1(4) . . ? C4 C3 C2 107.8(4) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? C3 C4 C5 108.4(4) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? C6 C5 C4 132.0(4) . . ? C6 C5 N1 121.0(3) . . ? C4 C5 N1 106.9(3) . . ? C5 C6 C7 121.1(3) . . ? C5 C6 C12 120.1(3) . . ? C7 C6 C12 118.7(4) . . ? C6 C7 C8 132.0(4) . . ? C6 C7 N2 120.8(4) . . ? C8 C7 N2 107.1(3) . . ? C9 C8 C7 108.4(4) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? C8 C9 C10 107.6(4) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? N2 C10 C9 108.9(3) . . ? N2 C10 C11 122.8(4) . . ? C9 C10 C11 128.2(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 118.7(3) . . ? C17 C12 C6 122.4(3) . . ? C13 C12 C6 118.9(4) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.8(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 117.8(3) . . ? C16 C15 C23 122.3(3) . . ? C14 C15 C23 119.9(3) . . ? C17 C16 C15 121.7(4) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C12 120.2(4) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 110.3(3) . . ? N3 C19 C18 121.8(4) . . ? C20 C19 C18 127.9(4) . . ? C21 C20 C19 107.6(4) . . ? C21 C20 H20 126.2 . . ? C19 C20 H20 126.2 . . ? C20 C21 C22 106.8(4) . . ? C20 C21 H21 126.6 . . ? C22 C21 H21 126.6 . . ? C23 C22 N3 124.8(3) . . ? C23 C22 C21 127.8(3) . . ? N3 C22 C21 107.5(3) . . ? C24 C23 C22 126.7(3) . . ? C24 C23 C15 116.3(3) . . ? C22 C23 C15 117.0(3) . . ? N4 C24 C23 124.0(3) . . ? N4 C24 C25 107.9(3) . . ? C23 C24 C25 128.0(3) . . ? C26 C25 C24 107.2(3) . . ? C26 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? C25 C26 C27 107.1(4) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? N4 C27 C26 110.6(4) . . ? N4 C27 C28 121.3(4) . . ? C26 C27 C28 128.1(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C31 109.6(4) . . ? N5 C30 C29 123.3(4) . . ? C31 C30 C29 127.1(4) . . ? C32 C31 C30 107.4(4) . . ? C32 C31 H31 126.3 . . ? C30 C31 H31 126.3 . . ? C31 C32 C33 107.9(4) . . ? C31 C32 H32 126.1 . . ? C33 C32 H32 126.1 . . ? C32 C33 N5 108.1(3) . . ? C32 C33 C34 131.9(4) . . ? N5 C33 C34 119.9(4) . . ? C35 C34 C33 121.1(3) . . ? C35 C34 C40 120.2(3) . . ? C33 C34 C40 118.7(4) . . ? C34 C35 N6 120.9(4) . . ? C34 C35 C36 131.6(4) . . ? N6 C35 C36 107.4(4) . . ? C37 C36 C35 107.6(4) . . ? C37 C36 H36 126.2 . . ? C35 C36 H36 126.2 . . ? C36 C37 C38 107.8(4) . . ? C36 C37 H37 126.1 . . ? C38 C37 H37 126.1 . . ? N6 C38 C37 109.8(4) . . ? N6 C38 C39 123.0(4) . . ? C37 C38 C39 127.2(4) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 118.4(3) . . ? C45 C40 C34 121.6(4) . . ? C41 C40 C34 119.9(4) . . ? C42 C41 C40 120.6(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 121.2(4) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 117.7(3) . . ? C44 C43 C51 121.9(3) . . ? C42 C43 C51 120.4(3) . . ? C45 C44 C43 121.1(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C40 120.9(4) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C48 111.2(3) . . ? N7 C47 C46 120.9(4) . . ? C48 C47 C46 127.8(4) . . ? C49 C48 C47 106.5(3) . . ? C49 C48 H48 126.7 . . ? C47 C48 H48 126.7 . . ? C48 C49 C50 107.8(3) . . ? C48 C49 H49 126.1 . . ? C50 C49 H49 126.1 . . ? C51 C50 N7 124.8(3) . . ? C51 C50 C49 127.5(3) . . ? N7 C50 C49 107.7(3) . . ? C50 C51 C52 127.6(3) . . ? C50 C51 C43 116.5(3) . . ? C52 C51 C43 115.9(3) . . ? N8 C52 C51 123.1(3) . . ? N8 C52 C53 108.0(3) . . ? C51 C52 C53 128.8(3) . . ? C54 C53 C52 107.6(3) . . ? C54 C53 H53 126.2 . . ? C52 C53 H53 126.2 . . ? C53 C54 C55 106.6(4) . . ? C53 C54 H54 126.7 . . ? C55 C54 H54 126.7 . . ? N8 C55 C54 111.2(3) . . ? N8 C55 C56 120.1(3) . . ? C54 C55 C56 128.5(4) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Cl2 C57 Cl1 115.6(3) . . ? Cl2 C57 H57A 108.4 . . ? Cl1 C57 H57A 108.4 . . ? Cl2 C57 H57B 108.4 . . ? Cl1 C57 H57B 108.4 . . ? H57A C57 H57B 107.4 . . ? Cl3 C58 Cl4 112.4(3) . . ? Cl3 C58 H58A 109.1 . . ? Cl4 C58 H58A 109.1 . . ? Cl3 C58 H58B 109.1 . . ? Cl4 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? F2 B1 F1 109.8(3) . . ? F2 B1 N1 110.6(4) . . ? F1 B1 N1 110.4(3) . . ? F2 B1 N2 109.5(3) . . ? F1 B1 N2 109.7(3) . . ? N1 B1 N2 107.0(3) . . ? F4 B2 F3 109.6(3) . . ? F4 B2 N5 111.3(4) . . ? F3 B2 N5 109.8(4) . . ? F4 B2 N6 109.6(4) . . ? F3 B2 N6 109.1(4) . . ? N5 B2 N6 107.4(3) . . ? C2 N1 C5 107.4(3) . . ? C2 N1 B1 127.5(3) . . ? C5 N1 B1 125.1(3) . . ? C10 N2 C7 107.9(3) . . ? C10 N2 B1 127.2(3) . . ? C7 N2 B1 124.9(3) . . ? C19 N3 C22 107.8(3) . . ? C19 N3 Zn1 127.1(3) . . ? C22 N3 Zn1 124.3(2) . . ? C27 N4 C24 107.1(3) . . ? C27 N4 Zn1 127.0(3) . . ? C24 N4 Zn1 125.7(3) . . ? C30 N5 C33 107.0(3) . . ? C30 N5 B2 127.1(3) . . ? C33 N5 B2 125.9(3) . . ? C38 N6 C35 107.4(3) . . ? C38 N6 B2 127.8(3) . . ? C35 N6 B2 124.6(3) . . ? C47 N7 C50 106.7(3) . . ? C47 N7 Zn1 128.4(3) . . ? C50 N7 Zn1 124.8(2) . . ? C55 N8 C52 106.6(3) . . ? C55 N8 Zn1 127.5(3) . . ? C52 N8 Zn1 125.9(2) . . ? N4 Zn1 N7 117.81(13) . . ? N4 Zn1 N3 94.02(12) . . ? N7 Zn1 N3 122.94(13) . . ? N4 Zn1 N8 115.26(13) . . ? N7 Zn1 N8 93.78(12) . . ? N3 Zn1 N8 114.78(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 0.3(5) . . . . ? C1 C2 C3 C4 -179.2(4) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? C3 C4 C5 C6 177.2(4) . . . . ? C3 C4 C5 N1 0.8(5) . . . . ? C4 C5 C6 C7 -175.2(4) . . . . ? N1 C5 C6 C7 0.8(6) . . . . ? C4 C5 C6 C12 7.6(7) . . . . ? N1 C5 C6 C12 -176.4(4) . . . . ? C5 C6 C7 C8 -178.5(4) . . . . ? C12 C6 C7 C8 -1.3(7) . . . . ? C5 C6 C7 N2 -2.8(6) . . . . ? C12 C6 C7 N2 174.4(3) . . . . ? C6 C7 C8 C9 176.1(4) . . . . ? N2 C7 C8 C9 -0.1(5) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? C8 C9 C10 N2 1.1(5) . . . . ? C8 C9 C10 C11 -176.3(4) . . . . ? C5 C6 C12 C17 -124.6(4) . . . . ? C7 C6 C12 C17 58.2(5) . . . . ? C5 C6 C12 C13 56.9(5) . . . . ? C7 C6 C12 C13 -120.4(4) . . . . ? C17 C12 C13 C14 0.1(6) . . . . ? C6 C12 C13 C14 178.6(4) . . . . ? C12 C13 C14 C15 0.9(6) . . . . ? C13 C14 C15 C16 -1.2(6) . . . . ? C13 C14 C15 C23 176.5(4) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C23 C15 C16 C17 -176.9(4) . . . . ? C15 C16 C17 C12 0.1(6) . . . . ? C13 C12 C17 C16 -0.5(6) . . . . ? C6 C12 C17 C16 -179.1(4) . . . . ? N3 C19 C20 C21 -1.7(5) . . . . ? C18 C19 C20 C21 176.9(4) . . . . ? C19 C20 C21 C22 1.4(5) . . . . ? C20 C21 C22 C23 178.4(4) . . . . ? C20 C21 C22 N3 -0.7(5) . . . . ? N3 C22 C23 C24 5.0(6) . . . . ? C21 C22 C23 C24 -174.0(4) . . . . ? N3 C22 C23 C15 -173.7(3) . . . . ? C21 C22 C23 C15 7.3(6) . . . . ? C16 C15 C23 C24 56.1(5) . . . . ? C14 C15 C23 C24 -121.5(4) . . . . ? C16 C15 C23 C22 -125.0(4) . . . . ? C14 C15 C23 C22 57.3(5) . . . . ? C22 C23 C24 N4 1.3(6) . . . . ? C15 C23 C24 N4 -180.0(3) . . . . ? C22 C23 C24 C25 -176.5(4) . . . . ? C15 C23 C24 C25 2.2(6) . . . . ? N4 C24 C25 C26 0.2(5) . . . . ? C23 C24 C25 C26 178.3(4) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C25 C26 C27 N4 0.6(5) . . . . ? C25 C26 C27 C28 179.7(5) . . . . ? N5 C30 C31 C32 1.0(5) . . . . ? C29 C30 C31 C32 -176.7(4) . . . . ? C30 C31 C32 C33 -0.8(5) . . . . ? C31 C32 C33 N5 0.3(5) . . . . ? C31 C32 C33 C34 175.3(4) . . . . ? C32 C33 C34 C35 -177.0(4) . . . . ? N5 C33 C34 C35 -2.5(6) . . . . ? C32 C33 C34 C40 1.5(7) . . . . ? N5 C33 C34 C40 176.0(3) . . . . ? C33 C34 C35 N6 1.3(6) . . . . ? C40 C34 C35 N6 -177.3(3) . . . . ? C33 C34 C35 C36 -177.1(4) . . . . ? C40 C34 C35 C36 4.4(7) . . . . ? C34 C35 C36 C37 178.2(4) . . . . ? N6 C35 C36 C37 -0.3(5) . . . . ? C35 C36 C37 C38 -0.3(5) . . . . ? C36 C37 C38 N6 0.8(5) . . . . ? C36 C37 C38 C39 -179.3(4) . . . . ? C35 C34 C40 C45 -128.5(4) . . . . ? C33 C34 C40 C45 52.9(5) . . . . ? C35 C34 C40 C41 54.0(5) . . . . ? C33 C34 C40 C41 -124.6(4) . . . . ? C45 C40 C41 C42 -1.3(6) . . . . ? C34 C40 C41 C42 176.3(4) . . . . ? C40 C41 C42 C43 1.0(6) . . . . ? C41 C42 C43 C44 0.2(6) . . . . ? C41 C42 C43 C51 -177.9(3) . . . . ? C42 C43 C44 C45 -1.2(6) . . . . ? C51 C43 C44 C45 176.9(4) . . . . ? C43 C44 C45 C40 0.9(6) . . . . ? C41 C40 C45 C44 0.4(6) . . . . ? C34 C40 C45 C44 -177.2(4) . . . . ? N7 C47 C48 C49 0.2(5) . . . . ? C46 C47 C48 C49 -177.0(4) . . . . ? C47 C48 C49 C50 0.7(5) . . . . ? C48 C49 C50 C51 176.6(4) . . . . ? C48 C49 C50 N7 -1.3(5) . . . . ? N7 C50 C51 C52 0.0(7) . . . . ? C49 C50 C51 C52 -177.6(4) . . . . ? N7 C50 C51 C43 179.1(3) . . . . ? C49 C50 C51 C43 1.5(6) . . . . ? C44 C43 C51 C50 -113.1(4) . . . . ? C42 C43 C51 C50 65.0(5) . . . . ? C44 C43 C51 C52 66.1(5) . . . . ? C42 C43 C51 C52 -115.8(4) . . . . ? C50 C51 C52 N8 -2.9(6) . . . . ? C43 C51 C52 N8 178.1(3) . . . . ? C50 C51 C52 C53 -178.8(4) . . . . ? C43 C51 C52 C53 2.2(6) . . . . ? N8 C52 C53 C54 -0.3(4) . . . . ? C51 C52 C53 C54 176.1(4) . . . . ? C52 C53 C54 C55 0.2(5) . . . . ? C53 C54 C55 N8 0.0(5) . . . . ? C53 C54 C55 C56 -175.2(4) . . . . ? C3 C2 N1 C5 0.2(5) . . . . ? C1 C2 N1 C5 179.7(4) . . . . ? C3 C2 N1 B1 -177.3(4) . . . . ? C1 C2 N1 B1 2.3(6) . . . . ? C6 C5 N1 C2 -177.5(4) . . . . ? C4 C5 N1 C2 -0.6(4) . . . . ? C6 C5 N1 B1 0.0(6) . . . . ? C4 C5 N1 B1 176.9(4) . . . . ? F2 B1 N1 C2 58.8(5) . . . . ? F1 B1 N1 C2 -62.9(5) . . . . ? N2 B1 N1 C2 177.9(4) . . . . ? F2 B1 N1 C5 -118.2(4) . . . . ? F1 B1 N1 C5 120.2(4) . . . . ? N2 B1 N1 C5 0.9(5) . . . . ? C9 C10 N2 C7 -1.2(5) . . . . ? C11 C10 N2 C7 176.4(4) . . . . ? C9 C10 N2 B1 178.9(4) . . . . ? C11 C10 N2 B1 -3.5(6) . . . . ? C6 C7 N2 C10 -175.9(4) . . . . ? C8 C7 N2 C10 0.8(4) . . . . ? C6 C7 N2 B1 4.0(6) . . . . ? C8 C7 N2 B1 -179.3(4) . . . . ? F2 B1 N2 C10 -63.2(5) . . . . ? F1 B1 N2 C10 57.3(5) . . . . ? N1 B1 N2 C10 177.0(4) . . . . ? F2 B1 N2 C7 116.9(4) . . . . ? F1 B1 N2 C7 -122.6(4) . . . . ? N1 B1 N2 C7 -2.9(5) . . . . ? C20 C19 N3 C22 1.2(5) . . . . ? C18 C19 N3 C22 -177.4(4) . . . . ? C20 C19 N3 Zn1 -168.8(3) . . . . ? C18 C19 N3 Zn1 12.6(6) . . . . ? C23 C22 N3 C19 -179.5(4) . . . . ? C21 C22 N3 C19 -0.3(4) . . . . ? C23 C22 N3 Zn1 -9.1(5) . . . . ? C21 C22 N3 Zn1 170.0(3) . . . . ? C26 C27 N4 C24 -0.4(5) . . . . ? C28 C27 N4 C24 -179.6(4) . . . . ? C26 C27 N4 Zn1 -175.8(3) . . . . ? C28 C27 N4 Zn1 5.0(6) . . . . ? C23 C24 N4 C27 -178.1(4) . . . . ? C25 C24 N4 C27 0.1(4) . . . . ? C23 C24 N4 Zn1 -2.6(5) . . . . ? C25 C24 N4 Zn1 175.6(3) . . . . ? C31 C30 N5 C33 -0.8(5) . . . . ? C29 C30 N5 C33 177.0(4) . . . . ? C31 C30 N5 B2 178.6(4) . . . . ? C29 C30 N5 B2 -3.6(6) . . . . ? C32 C33 N5 C30 0.3(4) . . . . ? C34 C33 N5 C30 -175.4(3) . . . . ? C32 C33 N5 B2 -179.1(4) . . . . ? C34 C33 N5 B2 5.2(6) . . . . ? F4 B2 N5 C30 -64.9(5) . . . . ? F3 B2 N5 C30 56.6(5) . . . . ? N6 B2 N5 C30 175.1(4) . . . . ? F4 B2 N5 C33 114.4(4) . . . . ? F3 B2 N5 C33 -124.1(4) . . . . ? N6 B2 N5 C33 -5.6(5) . . . . ? C37 C38 N6 C35 -1.0(5) . . . . ? C39 C38 N6 C35 179.1(4) . . . . ? C37 C38 N6 B2 -176.3(4) . . . . ? C39 C38 N6 B2 3.8(7) . . . . ? C34 C35 N6 C38 -177.9(4) . . . . ? C36 C35 N6 C38 0.8(4) . . . . ? C34 C35 N6 B2 -2.4(6) . . . . ? C36 C35 N6 B2 176.3(4) . . . . ? F4 B2 N6 C38 57.7(5) . . . . ? F3 B2 N6 C38 -62.3(5) . . . . ? N5 B2 N6 C38 178.7(4) . . . . ? F4 B2 N6 C35 -116.9(4) . . . . ? F3 B2 N6 C35 123.1(4) . . . . ? N5 B2 N6 C35 4.2(5) . . . . ? C48 C47 N7 C50 -1.0(5) . . . . ? C46 C47 N7 C50 176.4(4) . . . . ? C48 C47 N7 Zn1 -178.2(3) . . . . ? C46 C47 N7 Zn1 -0.8(6) . . . . ? C51 C50 N7 C47 -176.6(4) . . . . ? C49 C50 N7 C47 1.4(4) . . . . ? C51 C50 N7 Zn1 0.8(5) . . . . ? C49 C50 N7 Zn1 178.8(3) . . . . ? C54 C55 N8 C52 -0.2(4) . . . . ? C56 C55 N8 C52 175.5(4) . . . . ? C54 C55 N8 Zn1 178.9(3) . . . . ? C56 C55 N8 Zn1 -5.5(6) . . . . ? C51 C52 N8 C55 -176.4(4) . . . . ? C53 C52 N8 C55 0.3(4) . . . . ? C51 C52 N8 Zn1 4.6(5) . . . . ? C53 C52 N8 Zn1 -178.8(2) . . . . ? C27 N4 Zn1 N7 43.0(4) . . . . ? C24 N4 Zn1 N7 -131.6(3) . . . . ? C27 N4 Zn1 N3 173.8(4) . . . . ? C24 N4 Zn1 N3 -0.8(3) . . . . ? C27 N4 Zn1 N8 -66.4(4) . . . . ? C24 N4 Zn1 N8 119.0(3) . . . . ? C47 N7 Zn1 N4 56.1(4) . . . . ? C50 N7 Zn1 N4 -120.7(3) . . . . ? C47 N7 Zn1 N3 -59.8(4) . . . . ? C50 N7 Zn1 N3 123.5(3) . . . . ? C47 N7 Zn1 N8 177.3(3) . . . . ? C50 N7 Zn1 N8 0.5(3) . . . . ? C19 N3 Zn1 N4 174.7(3) . . . . ? C22 N3 Zn1 N4 6.3(3) . . . . ? C19 N3 Zn1 N7 -58.2(4) . . . . ? C22 N3 Zn1 N7 133.4(3) . . . . ? C19 N3 Zn1 N8 54.5(4) . . . . ? C22 N3 Zn1 N8 -114.0(3) . . . . ? C55 N8 Zn1 N4 -58.8(4) . . . . ? C52 N8 Zn1 N4 120.1(3) . . . . ? C55 N8 Zn1 N7 178.0(3) . . . . ? C52 N8 Zn1 N7 -3.1(3) . . . . ? C55 N8 Zn1 N3 48.9(4) . . . . ? C52 N8 Zn1 N3 -132.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.492 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.101 #===End data_compound16 _database_code_depnum_ccdc_archive 'CCDC 709603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H74 B2 Cl6 Co2 F4 N12' _chemical_formula_weight 1703.75 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4104(15) _cell_length_b 26.078(2) _cell_length_c 12.7437(14) _cell_angle_alpha 90.00 _cell_angle_beta 115.666(5) _cell_angle_gamma 90.00 _cell_volume 4017.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5141 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.35 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29741 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.11 _reflns_number_total 7078 _reflns_number_gt 4797 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+6.8338P] 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 7078 _refine_ls_number_parameters 518 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1926(4) 0.2631(2) 0.8696(4) 0.0500(15) Uani 1 1 d . . . H1A H 0.2441 0.2885 0.8644 0.075 Uiso 1 1 calc R . . H1B H 0.2337 0.2324 0.9096 0.075 Uiso 1 1 calc R . . H1C H 0.1545 0.2776 0.9133 0.075 Uiso 1 1 calc R . . C2 C 0.1098(4) 0.24908(19) 0.7503(4) 0.0360(12) Uani 1 1 d . . . C3 C 0.0754(4) 0.20063(19) 0.7054(4) 0.0425(13) Uani 1 1 d . . . H3 H 0.1003 0.1692 0.7461 0.051 Uiso 1 1 calc R . . C4 C -0.0004(4) 0.20581(18) 0.5928(4) 0.0393(12) Uani 1 1 d . . . H4 H -0.0373 0.1786 0.5407 0.047 Uiso 1 1 calc R . . C5 C -0.0145(3) 0.25839(17) 0.5668(3) 0.0264(10) Uani 1 1 d . . . C6 C -0.0875(3) 0.28453(17) 0.4696(3) 0.0260(10) Uani 1 1 d . A . C7 C -0.0940(3) 0.33795(17) 0.4699(3) 0.0261(10) Uani 1 1 d . . . C8 C -0.1620(4) 0.37259(18) 0.3854(4) 0.0356(11) Uani 1 1 d . . . H8 H -0.2169 0.3641 0.3099 0.043 Uiso 1 1 calc R . . C9 C -0.1356(4) 0.42044(19) 0.4307(4) 0.0408(12) Uani 1 1 d . . . H9 H -0.1685 0.4515 0.3926 0.049 Uiso 1 1 calc R . . C10 C -0.0514(4) 0.41580(18) 0.5435(4) 0.0342(11) Uani 1 1 d . . . C11 C 0.0068(5) 0.45696(18) 0.6303(4) 0.0454(13) Uani 1 1 d . . . H11A H -0.0115 0.4539 0.6966 0.068 Uiso 1 1 calc R . . H11B H -0.0167 0.4906 0.5936 0.068 Uiso 1 1 calc R . . H11C H 0.0869 0.4533 0.6574 0.068 Uiso 1 1 calc R . . C12 C -0.1630(3) 0.25579(16) 0.3634(3) 0.0237(9) Uiso 1 1 d D . . C13 C -0.1192(4) 0.22399(18) 0.3064(4) 0.0286(12) Uani 0.919(6) 1 d PD A 1 H13 H -0.0414 0.2193 0.3376 0.034 Uiso 0.919(6) 1 calc PR A 1 C14 C -0.1876(4) 0.19908(18) 0.2049(4) 0.0278(12) Uani 0.919(6) 1 d PD A 1 H14 H -0.1567 0.1782 0.1653 0.033 Uiso 0.919(6) 1 calc PR A 1 C15 C -0.3021(3) 0.20454(16) 0.1605(3) 0.0240(9) Uiso 1 1 d D . . C16 C -0.3454(4) 0.23340(18) 0.2212(4) 0.0259(12) Uani 0.919(6) 1 d P A 1 H16 H -0.4234 0.2354 0.1940 0.031 Uiso 0.919(6) 1 calc PR A 1 C17 C -0.2772(4) 0.25960(18) 0.3217(4) 0.0253(12) Uani 0.919(6) 1 d P A 1 H17 H -0.3084 0.2800 0.3617 0.030 Uiso 0.919(6) 1 calc PR A 1 C18 C -0.6744(4) 0.23389(18) -0.3263(4) 0.0350(11) Uani 1 1 d . . . H18A H -0.6427 0.2313 -0.3824 0.053 Uiso 1 1 calc R . . H18B H -0.7204 0.2648 -0.3427 0.053 Uiso 1 1 calc R . . H18C H -0.7200 0.2036 -0.3329 0.053 Uiso 1 1 calc R . . C19 C -0.5834(4) 0.23701(17) -0.2059(4) 0.0287(10) Uani 1 1 d . . . C20 C -0.5296(4) 0.28105(17) -0.1440(4) 0.0341(11) Uani 1 1 d . . . H20 H -0.5464 0.3154 -0.1704 0.041 Uiso 1 1 calc R . . C21 C -0.4491(4) 0.26575(17) -0.0396(4) 0.0311(11) Uani 1 1 d . A . H21 H -0.3997 0.2874 0.0204 0.037 Uiso 1 1 calc R . . C22 C -0.4528(3) 0.21154(16) -0.0371(3) 0.0228(9) Uani 1 1 d . . . C23 C -0.3790(3) 0.17885(17) 0.0496(3) 0.0225(9) Uani 1 1 d . A . C24 C -0.3692(3) 0.12587(16) 0.0409(3) 0.0246(9) Uani 1 1 d . . . C25 C -0.2916(4) 0.09230(19) 0.1224(4) 0.0367(12) Uani 1 1 d . A . H25 H -0.2370 0.1013 0.1977 0.044 Uiso 1 1 calc R . . C26 C -0.3091(4) 0.04472(19) 0.0738(4) 0.0417(13) Uani 1 1 d . . . H26 H -0.2687 0.0145 0.1080 0.050 Uiso 1 1 calc R A . C27 C -0.3990(4) 0.04909(17) -0.0370(4) 0.0332(11) Uani 1 1 d . A . C28 C -0.4504(5) 0.00790(19) -0.1249(5) 0.0503(15) Uani 1 1 d . . . H28A H -0.4809 -0.0186 -0.0925 0.075 Uiso 1 1 calc R A . H28B H -0.3943 -0.0073 -0.1453 0.075 Uiso 1 1 calc R . . H28C H -0.5100 0.0225 -0.1949 0.075 Uiso 1 1 calc R . . C29 C -0.6552(4) 0.13207(17) 0.0442(4) 0.0328(11) Uani 1 1 d . . . H29A H -0.5863 0.1123 0.0777 0.049 Uiso 1 1 calc R . . H29B H -0.6869 0.1340 0.1004 0.049 Uiso 1 1 calc R . . H29C H -0.6397 0.1668 0.0256 0.049 Uiso 1 1 calc R . . C30 C -0.7355(3) 0.10643(16) -0.0643(3) 0.0251(9) Uani 1 1 d . . . C31 C -0.8409(4) 0.08726(16) -0.0889(4) 0.0280(10) Uani 1 1 d . . . H31 H -0.8763 0.0878 -0.0386 0.034 Uiso 1 1 calc R . . C32 C -0.8834(3) 0.06755(16) -0.2002(4) 0.0257(10) Uani 1 1 d . . . H32 H -0.9538 0.0519 -0.2409 0.031 Uiso 1 1 calc R . . C33 C -0.8036(3) 0.07477(15) -0.2425(3) 0.0221(9) Uani 1 1 d . . . C34 C -0.8124(3) 0.06321(15) -0.3541(3) 0.0209(9) Uani 1 1 d . . . C35 C -0.7403(3) 0.07667(16) -0.4002(3) 0.0235(9) Uani 1 1 d . . . C36 C -0.7521(4) 0.06959(18) -0.5165(4) 0.0336(11) Uani 1 1 d . . . H36 H -0.8125 0.0534 -0.5784 0.040 Uiso 1 1 calc R . . C37 C -0.6622(4) 0.0900(2) -0.5225(4) 0.0364(12) Uani 1 1 d . . . H37 H -0.6488 0.0918 -0.5898 0.044 Uiso 1 1 calc R . . C38 C -0.5917(4) 0.10818(17) -0.4102(4) 0.0301(10) Uani 1 1 d . . . C39 C -0.4791(4) 0.1315(2) -0.3682(4) 0.0482(14) Uani 1 1 d . . . H39A H -0.4731 0.1607 -0.3173 0.072 Uiso 1 1 calc R . . H39B H -0.4674 0.1434 -0.4350 0.072 Uiso 1 1 calc R . . H39C H -0.4229 0.1059 -0.3247 0.072 Uiso 1 1 calc R . . C40 C -0.9113(3) 0.03171(15) -0.4297(3) 0.0209(9) Uani 1 1 d . . . C41 C -0.9921(3) 0.04937(16) -0.5357(3) 0.0236(9) Uani 1 1 d . . . H41 H -0.9877 0.0833 -0.5607 0.028 Uiso 1 1 calc R . . C42 C -0.9217(3) -0.01796(16) -0.3955(3) 0.0237(9) Uani 1 1 d . . . H42 H -0.8680 -0.0305 -0.3230 0.028 Uiso 1 1 calc R . . C43 C 0.7076(6) 0.0647(3) 0.4679(6) 0.0711(19) Uani 1 1 d . . . H43 H 0.7415 0.0393 0.4342 0.085 Uiso 1 1 calc R . . B1 B 0.0667(4) 0.3435(2) 0.6803(4) 0.0296(12) Uani 1 1 d . . . N1 N 0.0560(3) 0.28473(14) 0.6675(3) 0.0272(8) Uani 1 1 d . . . N2 N -0.0259(3) 0.36590(13) 0.5670(3) 0.0260(8) Uani 1 1 d . . . N3 N -0.5377(3) 0.19517(13) -0.1418(3) 0.0228(8) Uani 1 1 d . A . N4 N -0.4360(3) 0.09710(13) -0.0570(3) 0.0248(8) Uani 1 1 d . A . N5 N -0.7125(3) 0.09968(13) -0.1558(3) 0.0211(7) Uani 1 1 d . A . N6 N -0.6383(3) 0.10088(14) -0.3379(3) 0.0259(8) Uani 1 1 d . A . F1 F 0.1696(2) 0.35925(11) 0.6922(2) 0.0451(7) Uani 1 1 d . . . F2 F 0.0508(2) 0.35909(10) 0.7750(2) 0.0390(7) Uani 1 1 d . . . Co1 Co -0.58045(4) 0.12271(2) -0.17368(5) 0.02237(18) Uani 1 1 d . . . Cl1 Cl 0.7094(3) 0.12482(9) 0.4065(2) 0.1186(9) Uani 1 1 d . . . Cl2 Cl 0.57392(16) 0.04559(9) 0.4309(2) 0.1016(8) Uani 1 1 d . . . Cl3 Cl 0.78794(17) 0.06665(9) 0.61567(16) 0.0970(7) Uani 1 1 d . . . C13B C -0.163(3) 0.2694(12) 0.2570(8) 0.016(11) Uiso 0.081(6) 1 d PD A 2 H13B H -0.1142 0.2950 0.2543 0.019 Uiso 0.081(6) 1 calc PR A 2 C14B C -0.237(3) 0.2453(13) 0.1548(9) 0.028(13) Uiso 0.081(6) 1 d PD A 2 H14B H -0.2419 0.2564 0.0816 0.034 Uiso 0.081(6) 1 calc PR A 2 C16B C -0.311(4) 0.196(2) 0.2640(15) 0.06(2) Uiso 0.081(6) 1 d PD A 2 H16B H -0.3639 0.1717 0.2658 0.071 Uiso 0.081(6) 1 calc PR A 2 C17B C -0.243(4) 0.2221(18) 0.3649(14) 0.044(17) Uiso 0.081(6) 1 d PD A 2 H17B H -0.2513 0.2172 0.4346 0.053 Uiso 0.081(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(3) 0.069(4) 0.024(2) -0.002(3) 0.001(2) 0.012(3) C2 0.031(2) 0.041(3) 0.026(2) 0.000(2) 0.002(2) 0.009(2) C3 0.047(3) 0.028(3) 0.036(3) 0.006(2) 0.003(2) 0.012(2) C4 0.044(3) 0.025(3) 0.039(3) -0.007(2) 0.008(2) 0.002(2) C5 0.028(2) 0.027(2) 0.018(2) -0.0055(18) 0.0046(18) 0.0000(19) C6 0.022(2) 0.031(3) 0.022(2) -0.0044(19) 0.0069(18) -0.0020(19) C7 0.027(2) 0.029(3) 0.018(2) -0.0034(18) 0.0055(18) -0.0019(19) C8 0.036(3) 0.037(3) 0.026(2) 0.003(2) 0.006(2) 0.002(2) C9 0.048(3) 0.032(3) 0.040(3) 0.009(2) 0.016(2) 0.007(2) C10 0.043(3) 0.027(3) 0.036(3) -0.003(2) 0.019(2) -0.003(2) C11 0.067(4) 0.025(3) 0.049(3) -0.009(2) 0.030(3) -0.003(3) C13 0.018(2) 0.036(3) 0.024(2) -0.008(2) 0.0024(19) 0.003(2) C14 0.025(2) 0.033(3) 0.025(2) -0.012(2) 0.010(2) 0.000(2) C16 0.020(2) 0.033(3) 0.023(2) -0.005(2) 0.0078(19) -0.001(2) C17 0.028(2) 0.031(3) 0.017(2) -0.006(2) 0.0094(19) 0.002(2) C18 0.037(3) 0.029(3) 0.026(2) 0.007(2) 0.002(2) 0.002(2) C19 0.028(2) 0.028(3) 0.028(2) 0.0009(19) 0.0098(19) 0.001(2) C20 0.044(3) 0.019(2) 0.034(3) 0.002(2) 0.011(2) 0.002(2) C21 0.039(3) 0.022(2) 0.027(2) -0.0054(19) 0.009(2) -0.006(2) C22 0.022(2) 0.022(2) 0.022(2) -0.0055(18) 0.0079(17) -0.0050(18) C23 0.019(2) 0.030(2) 0.0153(19) -0.0035(17) 0.0049(16) -0.0063(18) C24 0.022(2) 0.025(2) 0.021(2) -0.0043(18) 0.0038(17) -0.0014(18) C25 0.033(2) 0.040(3) 0.022(2) -0.003(2) -0.002(2) 0.006(2) C26 0.042(3) 0.029(3) 0.036(3) 0.004(2) 0.001(2) 0.009(2) C27 0.035(2) 0.021(3) 0.035(3) -0.003(2) 0.007(2) 0.001(2) C28 0.055(3) 0.025(3) 0.050(3) -0.008(2) 0.004(3) 0.002(2) C29 0.041(3) 0.029(3) 0.026(2) -0.0095(19) 0.012(2) -0.006(2) C30 0.032(2) 0.019(2) 0.024(2) -0.0020(17) 0.0109(19) 0.0023(18) C31 0.034(2) 0.027(2) 0.027(2) -0.0006(19) 0.017(2) -0.005(2) C32 0.023(2) 0.023(2) 0.028(2) -0.0014(19) 0.0086(18) -0.0055(18) C33 0.023(2) 0.014(2) 0.019(2) 0.0009(17) -0.0011(17) -0.0024(17) C34 0.0159(19) 0.017(2) 0.020(2) 0.0005(17) -0.0010(16) -0.0002(16) C35 0.021(2) 0.021(2) 0.018(2) -0.0037(17) -0.0012(17) -0.0047(18) C36 0.031(2) 0.041(3) 0.022(2) -0.007(2) 0.0051(19) -0.010(2) C37 0.037(3) 0.052(3) 0.021(2) -0.002(2) 0.013(2) -0.006(2) C38 0.030(2) 0.032(3) 0.028(2) -0.002(2) 0.012(2) -0.010(2) C39 0.043(3) 0.064(4) 0.037(3) -0.013(3) 0.017(2) -0.026(3) C40 0.019(2) 0.018(2) 0.019(2) -0.0037(17) 0.0018(16) -0.0020(17) C41 0.024(2) 0.017(2) 0.023(2) 0.0012(17) 0.0032(18) -0.0034(17) C42 0.023(2) 0.022(2) 0.016(2) 0.0030(17) -0.0005(17) 0.0024(18) C43 0.070(4) 0.071(5) 0.078(4) -0.008(4) 0.038(4) 0.018(4) B1 0.027(3) 0.033(3) 0.023(3) -0.006(2) 0.006(2) -0.008(2) N1 0.0241(18) 0.031(2) 0.0169(17) -0.0052(16) 0.0001(15) 0.0000(16) N2 0.0314(19) 0.020(2) 0.0231(18) -0.0049(15) 0.0082(16) -0.0026(16) N3 0.0218(17) 0.023(2) 0.0167(17) -0.0003(15) 0.0020(14) -0.0035(15) N4 0.0241(18) 0.022(2) 0.0206(18) -0.0038(15) 0.0024(15) -0.0046(15) N5 0.0203(17) 0.0179(18) 0.0184(17) -0.0030(14) 0.0022(14) -0.0038(14) N6 0.0232(18) 0.027(2) 0.0209(18) -0.0044(15) 0.0037(15) -0.0102(16) F1 0.0312(14) 0.0514(18) 0.0440(16) -0.0050(14) 0.0080(12) -0.0118(13) F2 0.0530(17) 0.0366(15) 0.0228(13) -0.0104(11) 0.0119(12) -0.0013(13) Co1 0.0200(3) 0.0219(3) 0.0173(3) -0.0033(2) 0.0005(2) -0.0058(2) Cl1 0.164(2) 0.0912(16) 0.134(2) 0.0293(14) 0.0961(19) 0.0334(15) Cl2 0.0644(12) 0.1086(17) 0.1080(16) -0.0423(13) 0.0151(11) 0.0000(11) Cl3 0.0813(13) 0.1147(17) 0.0672(11) -0.0247(11) 0.0061(10) 0.0176(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.488(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.356(6) . ? C2 C3 1.381(7) . ? C3 C4 1.359(6) . ? C3 H3 0.9500 . ? C4 C5 1.404(6) . ? C4 H4 0.9500 . ? C5 C6 1.381(6) . ? C5 N1 1.401(5) . ? C6 C7 1.396(6) . ? C6 C12 1.494(6) . ? C7 N2 1.385(5) . ? C7 C8 1.399(6) . ? C8 C9 1.356(7) . ? C8 H8 0.9500 . ? C9 C10 1.396(7) . ? C9 H9 0.9500 . ? C10 N2 1.346(6) . ? C10 C11 1.496(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.389(5) . ? C12 C17 1.390(6) . ? C12 C17B 1.394(7) . ? C12 C13B 1.399(7) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(6) . ? C15 C16B 1.396(7) . ? C15 C14B 1.400(7) . ? C15 C23 1.499(5) . ? C16 C17 1.389(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.493(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.341(5) . ? C19 C20 1.403(6) . ? C20 C21 1.361(6) . ? C20 H20 0.9500 . ? C21 C22 1.415(6) . ? C21 H21 0.9500 . ? C22 N3 1.394(5) . ? C22 C23 1.407(6) . ? C23 C24 1.397(6) . ? C24 N4 1.397(5) . ? C24 C25 1.412(6) . ? C25 C26 1.361(7) . ? C25 H25 0.9500 . ? C26 C27 1.409(6) . ? C26 H26 0.9500 . ? C27 N4 1.330(5) . ? C27 C28 1.488(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.493(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.341(5) . ? C30 C31 1.401(6) . ? C31 C32 1.378(6) . ? C31 H31 0.9500 . ? C32 C33 1.404(6) . ? C32 H32 0.9500 . ? C33 N5 1.402(5) . ? C33 C34 1.408(6) . ? C34 C35 1.377(6) . ? C34 C40 1.502(5) . ? C35 N6 1.399(5) . ? C35 C36 1.433(6) . ? C36 C37 1.350(6) . ? C36 H36 0.9500 . ? C37 C38 1.413(6) . ? C37 H37 0.9500 . ? C38 N6 1.332(6) . ? C38 C39 1.496(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.392(6) . ? C40 C41 1.394(5) . ? C41 C42 1.378(6) 3_354 ? C41 H41 0.9500 . ? C42 C41 1.378(6) 3_354 ? C42 H42 0.9500 . ? C43 Cl3 1.718(7) . ? C43 Cl2 1.718(7) . ? C43 Cl1 1.757(7) . ? C43 H43 1.0000 . ? B1 F2 1.375(6) . ? B1 F1 1.383(6) . ? B1 N1 1.543(6) . ? B1 N2 1.554(6) . ? N3 Co1 1.965(3) . ? N4 Co1 1.979(3) . ? N5 Co1 1.974(3) . ? N6 Co1 1.975(3) . ? C13B C14B 1.395(8) . ? C13B H13B 0.9500 . ? C14B H14B 0.9500 . ? C16B C17B 1.395(8) . ? C16B H16B 0.9500 . ? C17B H17B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C1 122.4(5) . . ? C3 C2 C1 128.0(5) . . ? C4 C3 C2 108.0(4) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C3 C4 C5 108.0(4) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? C6 C5 N1 121.0(4) . . ? C6 C5 C4 131.6(4) . . ? N1 C5 C4 107.1(4) . . ? C5 C6 C7 120.8(4) . . ? C5 C6 C12 120.3(4) . . ? C7 C6 C12 119.0(4) . . ? N2 C7 C6 120.6(4) . . ? N2 C7 C8 107.8(4) . . ? C6 C7 C8 131.6(4) . . ? C9 C8 C7 107.7(4) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 C10 107.7(4) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? N2 C10 C9 109.1(4) . . ? N2 C10 C11 121.9(4) . . ? C9 C10 C11 129.0(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 119.2(4) . . ? C13 C12 C17B 98(2) . . ? C17 C12 C17B 47(3) . . ? C13 C12 C13B 58.0(17) . . ? C17 C12 C13B 93.9(14) . . ? C17B C12 C13B 119.5(6) . . ? C13 C12 C6 120.0(4) . . ? C17 C12 C6 120.8(4) . . ? C17B C12 C6 121.8(4) . . ? C13B C12 C6 117.9(4) . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.1(4) . . ? C16 C15 C16B 48(3) . . ? C14 C15 C16B 98(2) . . ? C16 C15 C14B 92.4(17) . . ? C14 C15 C14B 60(2) . . ? C16B C15 C14B 119.2(6) . . ? C16 C15 C23 119.3(4) . . ? C14 C15 C23 121.6(4) . . ? C16B C15 C23 120.7(5) . . ? C14B C15 C23 118.8(4) . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 119.7(4) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 109.6(4) . . ? N3 C19 C18 122.4(4) . . ? C20 C19 C18 127.9(4) . . ? C21 C20 C19 107.8(4) . . ? C21 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? C20 C21 C22 107.1(4) . . ? C20 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? N3 C22 C23 124.8(4) . . ? N3 C22 C21 107.8(3) . . ? C23 C22 C21 127.1(4) . . ? C24 C23 C22 126.5(4) . . ? C24 C23 C15 117.9(4) . . ? C22 C23 C15 115.6(4) . . ? C23 C24 N4 123.8(4) . . ? C23 C24 C25 128.3(4) . . ? N4 C24 C25 107.9(4) . . ? C26 C25 C24 107.7(4) . . ? C26 C25 H25 126.2 . . ? C24 C25 H25 126.2 . . ? C25 C26 C27 106.7(4) . . ? C25 C26 H26 126.7 . . ? C27 C26 H26 126.7 . . ? N4 C27 C26 110.7(4) . . ? N4 C27 C28 121.5(4) . . ? C26 C27 C28 127.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C31 110.4(4) . . ? N5 C30 C29 121.3(4) . . ? C31 C30 C29 128.3(4) . . ? C32 C31 C30 106.9(4) . . ? C32 C31 H31 126.6 . . ? C30 C31 H31 126.6 . . ? C31 C32 C33 107.5(4) . . ? C31 C32 H32 126.3 . . ? C33 C32 H32 126.3 . . ? N5 C33 C32 108.0(3) . . ? N5 C33 C34 123.9(4) . . ? C32 C33 C34 127.9(4) . . ? C35 C34 C33 127.5(4) . . ? C35 C34 C40 117.0(4) . . ? C33 C34 C40 115.4(4) . . ? C34 C35 N6 124.6(4) . . ? C34 C35 C36 128.7(4) . . ? N6 C35 C36 106.7(4) . . ? C37 C36 C35 107.9(4) . . ? C37 C36 H36 126.1 . . ? C35 C36 H36 126.1 . . ? C36 C37 C38 107.3(4) . . ? C36 C37 H37 126.4 . . ? C38 C37 H37 126.4 . . ? N6 C38 C37 110.1(4) . . ? N6 C38 C39 121.0(4) . . ? C37 C38 C39 128.9(4) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C41 118.0(4) . . ? C42 C40 C34 119.2(3) . . ? C41 C40 C34 122.7(4) . . ? C42 C41 C40 120.4(4) 3_354 . ? C42 C41 H41 119.8 3_354 . ? C40 C41 H41 119.8 . . ? C41 C42 C40 121.6(4) 3_354 . ? C41 C42 H42 119.2 3_354 . ? C40 C42 H42 119.2 . . ? Cl3 C43 Cl2 113.2(4) . . ? Cl3 C43 Cl1 109.8(4) . . ? Cl2 C43 Cl1 110.5(4) . . ? Cl3 C43 H43 107.7 . . ? Cl2 C43 H43 107.7 . . ? Cl1 C43 H43 107.7 . . ? F2 B1 F1 110.1(4) . . ? F2 B1 N1 110.0(4) . . ? F1 B1 N1 110.4(4) . . ? F2 B1 N2 109.9(4) . . ? F1 B1 N2 110.4(4) . . ? N1 B1 N2 105.9(3) . . ? C2 N1 C5 107.3(4) . . ? C2 N1 B1 127.3(4) . . ? C5 N1 B1 125.4(3) . . ? C10 N2 C7 107.7(4) . . ? C10 N2 B1 126.4(4) . . ? C7 N2 B1 125.8(3) . . ? C19 N3 C22 107.6(3) . . ? C19 N3 Co1 129.9(3) . . ? C22 N3 Co1 122.4(3) . . ? C27 N4 C24 107.0(3) . . ? C27 N4 Co1 128.6(3) . . ? C24 N4 Co1 122.0(3) . . ? C30 N5 C33 107.2(3) . . ? C30 N5 Co1 128.0(3) . . ? C33 N5 Co1 124.7(3) . . ? C38 N6 C35 108.0(3) . . ? C38 N6 Co1 127.2(3) . . ? C35 N6 Co1 124.7(3) . . ? N3 Co1 N5 117.67(14) . . ? N3 Co1 N6 116.21(14) . . ? N5 Co1 N6 94.26(13) . . ? N3 Co1 N4 93.80(14) . . ? N5 Co1 N4 116.50(14) . . ? N6 Co1 N4 120.42(15) . . ? C14B C13B C12 119.8(5) . . ? C14B C13B H13B 120.1 . . ? C12 C13B H13B 120.1 . . ? C13B C14B C15 119.8(6) . . ? C13B C14B H14B 120.1 . . ? C15 C14B H14B 120.1 . . ? C17B C16B C15 119.9(5) . . ? C17B C16B H16B 120.0 . . ? C15 C16B H16B 120.0 . . ? C12 C17B C16B 120.0(6) . . ? C12 C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 0.5(6) . . . . ? C1 C2 C3 C4 -179.4(5) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 C6 -173.6(5) . . . . ? C3 C4 C5 N1 0.4(6) . . . . ? N1 C5 C6 C7 -0.9(7) . . . . ? C4 C5 C6 C7 172.4(5) . . . . ? N1 C5 C6 C12 -179.4(4) . . . . ? C4 C5 C6 C12 -6.1(8) . . . . ? C5 C6 C7 N2 1.2(7) . . . . ? C12 C6 C7 N2 179.6(4) . . . . ? C5 C6 C7 C8 -177.9(5) . . . . ? C12 C6 C7 C8 0.6(7) . . . . ? N2 C7 C8 C9 -0.1(5) . . . . ? C6 C7 C8 C9 179.0(5) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 N2 0.4(6) . . . . ? C8 C9 C10 C11 179.9(5) . . . . ? C5 C6 C12 C13 -60.0(6) . . . . ? C7 C6 C12 C13 121.5(5) . . . . ? C5 C6 C12 C17 118.7(5) . . . . ? C7 C6 C12 C17 -59.8(6) . . . . ? C5 C6 C12 C17B 63(3) . . . . ? C7 C6 C12 C17B -116(3) . . . . ? C5 C6 C12 C13B -127(2) . . . . ? C7 C6 C12 C13B 54(2) . . . . ? C17 C12 C13 C14 4.4(7) . . . . ? C17B C12 C13 C14 49.4(18) . . . . ? C13B C12 C13 C14 -70.7(8) . . . . ? C6 C12 C13 C14 -176.8(4) . . . . ? C12 C13 C14 C15 -1.9(7) . . . . ? C13 C14 C15 C16 -2.3(7) . . . . ? C13 C14 C15 C16B -48(2) . . . . ? C13 C14 C15 C14B 71.9(10) . . . . ? C13 C14 C15 C23 179.0(4) . . . . ? C14 C15 C16 C17 4.0(7) . . . . ? C16B C15 C16 C17 76.4(13) . . . . ? C14B C15 C16 C17 -52.1(14) . . . . ? C23 C15 C16 C17 -177.3(4) . . . . ? C15 C16 C17 C12 -1.5(7) . . . . ? C13 C12 C17 C16 -2.7(7) . . . . ? C17B C12 C17 C16 -74.9(11) . . . . ? C13B C12 C17 C16 52.5(13) . . . . ? C6 C12 C17 C16 178.5(4) . . . . ? N3 C19 C20 C21 0.0(6) . . . . ? C18 C19 C20 C21 -177.5(5) . . . . ? C19 C20 C21 C22 0.3(5) . . . . ? C20 C21 C22 N3 -0.5(5) . . . . ? C20 C21 C22 C23 174.3(4) . . . . ? N3 C22 C23 C24 8.0(7) . . . . ? C21 C22 C23 C24 -165.9(4) . . . . ? N3 C22 C23 C15 -173.6(4) . . . . ? C21 C22 C23 C15 12.4(6) . . . . ? C16 C15 C23 C24 -124.3(5) . . . . ? C14 C15 C23 C24 54.4(6) . . . . ? C16B C15 C23 C24 -69(3) . . . . ? C14B C15 C23 C24 124(2) . . . . ? C16 C15 C23 C22 57.2(5) . . . . ? C14 C15 C23 C22 -124.1(5) . . . . ? C16B C15 C23 C22 113(3) . . . . ? C14B C15 C23 C22 -54(2) . . . . ? C22 C23 C24 N4 -2.1(7) . . . . ? C15 C23 C24 N4 179.6(4) . . . . ? C22 C23 C24 C25 175.3(5) . . . . ? C15 C23 C24 C25 -3.0(7) . . . . ? C23 C24 C25 C26 -176.2(5) . . . . ? N4 C24 C25 C26 1.5(5) . . . . ? C24 C25 C26 C27 -0.9(6) . . . . ? C25 C26 C27 N4 0.0(6) . . . . ? C25 C26 C27 C28 180.0(5) . . . . ? N5 C30 C31 C32 0.5(5) . . . . ? C29 C30 C31 C32 179.5(4) . . . . ? C30 C31 C32 C33 0.1(5) . . . . ? C31 C32 C33 N5 -0.7(5) . . . . ? C31 C32 C33 C34 -176.4(4) . . . . ? N5 C33 C34 C35 -4.7(7) . . . . ? C32 C33 C34 C35 170.3(4) . . . . ? N5 C33 C34 C40 174.1(4) . . . . ? C32 C33 C34 C40 -10.9(6) . . . . ? C33 C34 C35 N6 6.2(7) . . . . ? C40 C34 C35 N6 -172.6(4) . . . . ? C33 C34 C35 C36 -173.7(4) . . . . ? C40 C34 C35 C36 7.6(7) . . . . ? C34 C35 C36 C37 178.4(4) . . . . ? N6 C35 C36 C37 -1.5(5) . . . . ? C35 C36 C37 C38 2.2(6) . . . . ? C36 C37 C38 N6 -2.1(6) . . . . ? C36 C37 C38 C39 176.4(5) . . . . ? C35 C34 C40 C42 115.3(4) . . . . ? C33 C34 C40 C42 -63.6(5) . . . . ? C35 C34 C40 C41 -62.3(6) . . . . ? C33 C34 C40 C41 118.8(4) . . . . ? C42 C40 C41 C42 -0.9(7) . . . 3_354 ? C34 C40 C41 C42 176.8(4) . . . 3_354 ? C41 C40 C42 C41 0.9(7) . . . 3_354 ? C34 C40 C42 C41 -176.8(4) . . . 3_354 ? C3 C2 N1 C5 -0.2(5) . . . . ? C1 C2 N1 C5 179.7(5) . . . . ? C3 C2 N1 B1 178.5(4) . . . . ? C1 C2 N1 B1 -1.6(7) . . . . ? C6 C5 N1 C2 174.6(4) . . . . ? C4 C5 N1 C2 -0.2(5) . . . . ? C6 C5 N1 B1 -4.1(7) . . . . ? C4 C5 N1 B1 -178.8(4) . . . . ? F2 B1 N1 C2 -52.4(6) . . . . ? F1 B1 N1 C2 69.3(6) . . . . ? N2 B1 N1 C2 -171.1(4) . . . . ? F2 B1 N1 C5 126.0(4) . . . . ? F1 B1 N1 C5 -112.3(4) . . . . ? N2 B1 N1 C5 7.3(6) . . . . ? C9 C10 N2 C7 -0.5(5) . . . . ? C11 C10 N2 C7 180.0(4) . . . . ? C9 C10 N2 B1 177.0(4) . . . . ? C11 C10 N2 B1 -2.5(7) . . . . ? C6 C7 N2 C10 -178.9(4) . . . . ? C8 C7 N2 C10 0.4(5) . . . . ? C6 C7 N2 B1 3.6(7) . . . . ? C8 C7 N2 B1 -177.2(4) . . . . ? F2 B1 N2 C10 57.0(6) . . . . ? F1 B1 N2 C10 -64.6(6) . . . . ? N1 B1 N2 C10 175.8(4) . . . . ? F2 B1 N2 C7 -125.9(4) . . . . ? F1 B1 N2 C7 112.5(5) . . . . ? N1 B1 N2 C7 -7.1(6) . . . . ? C20 C19 N3 C22 -0.3(5) . . . . ? C18 C19 N3 C22 177.4(4) . . . . ? C20 C19 N3 Co1 175.7(3) . . . . ? C18 C19 N3 Co1 -6.7(6) . . . . ? C23 C22 N3 C19 -174.4(4) . . . . ? C21 C22 N3 C19 0.5(5) . . . . ? C23 C22 N3 Co1 9.2(6) . . . . ? C21 C22 N3 Co1 -175.8(3) . . . . ? C26 C27 N4 C24 0.9(5) . . . . ? C28 C27 N4 C24 -179.0(5) . . . . ? C26 C27 N4 Co1 -161.6(3) . . . . ? C28 C27 N4 Co1 18.5(7) . . . . ? C23 C24 N4 C27 176.4(4) . . . . ? C25 C24 N4 C27 -1.5(5) . . . . ? C23 C24 N4 Co1 -19.7(6) . . . . ? C25 C24 N4 Co1 162.4(3) . . . . ? C31 C30 N5 C33 -1.0(5) . . . . ? C29 C30 N5 C33 180.0(4) . . . . ? C31 C30 N5 Co1 176.1(3) . . . . ? C29 C30 N5 Co1 -2.9(6) . . . . ? C32 C33 N5 C30 1.0(4) . . . . ? C34 C33 N5 C30 176.9(4) . . . . ? C32 C33 N5 Co1 -176.2(3) . . . . ? C34 C33 N5 Co1 -0.3(5) . . . . ? C37 C38 N6 C35 1.1(5) . . . . ? C39 C38 N6 C35 -177.5(4) . . . . ? C37 C38 N6 Co1 -176.1(3) . . . . ? C39 C38 N6 Co1 5.2(7) . . . . ? C34 C35 N6 C38 -179.7(4) . . . . ? C36 C35 N6 C38 0.2(5) . . . . ? C34 C35 N6 Co1 -2.4(6) . . . . ? C36 C35 N6 Co1 177.5(3) . . . . ? C19 N3 Co1 N5 -75.0(4) . . . . ? C22 N3 Co1 N5 100.4(3) . . . . ? C19 N3 Co1 N6 35.6(4) . . . . ? C22 N3 Co1 N6 -149.0(3) . . . . ? C19 N3 Co1 N4 162.3(4) . . . . ? C22 N3 Co1 N4 -22.2(3) . . . . ? C30 N5 Co1 N3 -51.3(4) . . . . ? C33 N5 Co1 N3 125.3(3) . . . . ? C30 N5 Co1 N6 -173.9(4) . . . . ? C33 N5 Co1 N6 2.6(3) . . . . ? C30 N5 Co1 N4 58.9(4) . . . . ? C33 N5 Co1 N4 -124.5(3) . . . . ? C38 N6 Co1 N3 51.6(4) . . . . ? C35 N6 Co1 N3 -125.2(3) . . . . ? C38 N6 Co1 N5 175.4(4) . . . . ? C35 N6 Co1 N5 -1.4(4) . . . . ? C38 N6 Co1 N4 -60.4(4) . . . . ? C35 N6 Co1 N4 122.8(3) . . . . ? C27 N4 Co1 N3 -172.6(4) . . . . ? C24 N4 Co1 N3 27.3(3) . . . . ? C27 N4 Co1 N5 63.8(4) . . . . ? C24 N4 Co1 N5 -96.3(3) . . . . ? C27 N4 Co1 N6 -49.1(4) . . . . ? C24 N4 Co1 N6 150.8(3) . . . . ? C13 C12 C13B C14B 74(4) . . . . ? C17 C12 C13B C14B -49(4) . . . . ? C17B C12 C13B C14B -7(5) . . . . ? C6 C12 C13B C14B -177(3) . . . . ? C12 C13B C14B C15 -6(6) . . . . ? C16 C15 C14B C13B 55(4) . . . . ? C14 C15 C14B C13B -68(4) . . . . ? C16B C15 C14B C13B 14(6) . . . . ? C23 C15 C14B C13B -179(3) . . . . ? C16 C15 C16B C17B -73(5) . . . . ? C14 C15 C16B C17B 50(6) . . . . ? C14B C15 C16B C17B -10(7) . . . . ? C23 C15 C16B C17B -176(4) . . . . ? C13 C12 C17B C16B -47(6) . . . . ? C17 C12 C17B C16B 76(5) . . . . ? C13B C12 C17B C16B 11(7) . . . . ? C6 C12 C17B C16B -179(4) . . . . ? C15 C16B C17B C12 -3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.874 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.086 #===End