# Copyright The Royal Society of Chemistry, 1998 data_coke _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H20 N6' _chemical_formula_weight 392.46 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1) /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1831(10) _cell_length_b 24.930(3) _cell_length_c 8.1034(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.111(6) _cell_angle_gamma 90.00 _cell_volume 2011.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method ? _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11978 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4566 _reflns_number_observed 3753 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.9333P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4563 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_obs 0.0524 _refine_ls_wR_factor_all 0.1464 _refine_ls_wR_factor_obs 0.1302 _refine_ls_goodness_of_fit_all 1.112 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C11 C -0.1042(2) 0.27814(7) 0.7070(2) 0.0300(3) Uani 1 d . . C12 C -0.1066(2) 0.22243(7) 0.7208(2) 0.0366(4) Uani 1 d . . H12 H -0.0358(2) 0.20474(7) 0.7962(2) 0.044 Uiso 1 calc R . C13 C -0.2101(2) 0.19244(8) 0.6269(2) 0.0435(5) Uani 1 d . . H13 H -0.2091(2) 0.15445(8) 0.6362(2) 0.052 Uiso 1 calc R . C14 C -0.3154(2) 0.21798(8) 0.5190(2) 0.0436(5) Uani 1 d . . H14 H -0.3874(2) 0.19762(8) 0.4555(2) 0.052 Uiso 1 calc R . C15 C -0.3148(2) 0.27332(8) 0.5046(2) 0.0381(4) Uani 1 d . . H15 H -0.3873(2) 0.29073(8) 0.4313(2) 0.046 Uiso 1 calc R . C16 C -0.2093(2) 0.30402(7) 0.5961(2) 0.0314(4) Uani 1 d . . C21 C -0.2115(2) 0.36429(7) 0.5686(2) 0.0367(4) Uani 1 d . . H21A H -0.1181(2) 0.37725(7) 0.5801(2) 0.044 Uiso 1 calc R . H21B H -0.2603(2) 0.37218(7) 0.4521(2) 0.044 Uiso 1 calc R . N32 N -0.19988(14) 0.41605(6) 0.8281(2) 0.0324(3) Uani 1 d . . N31 N -0.27532(14) 0.39357(6) 0.6878(2) 0.0337(3) Uani 1 d . . C35 C -0.4081(2) 0.39699(8) 0.6838(3) 0.0416(4) Uani 1 d . . H35 H -0.4786(2) 0.38391(8) 0.5973(3) 0.050 Uiso 1 calc R . C34 C -0.4220(2) 0.42288(8) 0.8281(2) 0.0418(4) Uani 1 d . . H34 H -0.5032(2) 0.43131(8) 0.8626(2) 0.050 Uiso 1 calc R . C33 C -0.2901(2) 0.43430(7) 0.9141(2) 0.0328(4) Uani 1 d . . N41 N -0.3421(2) 0.46377(9) 1.1793(2) 0.0615(5) Uani 1 d . . C42 C -0.2486(2) 0.46191(7) 1.0778(2) 0.0351(4) Uani 1 d . . C43 C -0.1235(2) 0.48418(7) 1.1211(2) 0.0394(4) Uani 1 d . . H43 H -0.0611(2) 0.48129(7) 1.0493(2) 0.047 Uiso 1 calc R . C44 C -0.0918(3) 0.51054(10) 1.2705(3) 0.0676(7) Uani 1 d . . H44 H -0.0058(3) 0.52680(10) 1.3017(3) 0.081 Uiso 1 calc R . C45 C -0.1780(4) 0.51473(10) 1.3777(3) 0.0758(9) Uani 1 d . . H45 H -0.1530(4) 0.53333(10) 1.4819(3) 0.091 Uiso 1 calc R . C46 C -0.3027(3) 0.49112(12) 1.3301(3) 0.0732(9) Uani 1 d . . H46 H -0.3638(3) 0.49373(12) 1.4036(3) 0.088 Uiso 1 calc R . C51 C 0.0132(2) 0.30837(8) 0.8130(2) 0.0350(4) Uani 1 d . . H51A H -0.0163(2) 0.34499(8) 0.8356(2) 0.042 Uiso 1 calc R . H51B H 0.0423(2) 0.28990(8) 0.9227(2) 0.042 Uiso 1 calc R . N62 N 0.11336(14) 0.33970(6) 0.5828(2) 0.0311(3) Uani 1 d . . N61 N 0.12707(14) 0.31196(6) 0.7285(2) 0.0317(3) Uani 1 d . . C65 C 0.2482(2) 0.28792(7) 0.7722(2) 0.0353(4) Uani 1 d . . H65 H 0.2789(2) 0.26625(7) 0.8690(2) 0.042 Uiso 1 calc R . C64 C 0.3190(2) 0.30062(7) 0.6504(2) 0.0341(4) Uani 1 d . . H64 H 0.4076(2) 0.28989(7) 0.6454(2) 0.041 Uiso 1 calc R . C63 C 0.2310(2) 0.33303(6) 0.5350(2) 0.0281(3) Uani 1 d . . N71 N 0.36928(14) 0.34758(7) 0.3334(2) 0.0383(4) Uani 1 d . . C72 C 0.2490(2) 0.35617(6) 0.3739(2) 0.0288(3) Uani 1 d . . C73 C 0.1456(2) 0.38396(7) 0.2684(2) 0.0327(4) Uani 1 d . . H73 H 0.0629(2) 0.38988(7) 0.3021(2) 0.039 Uiso 1 calc R . C74 C 0.1641(2) 0.40288(8) 0.1144(2) 0.0397(4) Uani 1 d . . H74 H 0.0944(2) 0.42166(8) 0.0405(2) 0.048 Uiso 1 calc R . C75 C 0.2863(2) 0.39380(9) 0.0705(3) 0.0475(5) Uani 1 d . . H75 H 0.3021(2) 0.40597(9) -0.0347(3) 0.057 Uiso 1 calc R . C76 C 0.3853(2) 0.36662(9) 0.1829(3) 0.0480(5) Uani 1 d . . H76 H 0.4693(2) 0.36105(9) 0.1523(3) 0.058 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0341(8) 0.0360(9) 0.0231(7) -0.0011(6) 0.0131(6) 0.0005(7) C12 0.0430(10) 0.0380(9) 0.0321(8) 0.0030(7) 0.0155(7) 0.0065(8) C13 0.0616(12) 0.0338(9) 0.0403(10) -0.0043(8) 0.0228(9) -0.0050(9) C14 0.0485(11) 0.0495(11) 0.0351(9) -0.0111(8) 0.0139(8) -0.0146(9) C15 0.0374(9) 0.0480(11) 0.0293(8) -0.0030(7) 0.0081(7) -0.0013(8) C16 0.0354(9) 0.0355(9) 0.0260(7) -0.0002(6) 0.0129(6) 0.0012(7) C21 0.0451(10) 0.0371(9) 0.0302(8) 0.0038(7) 0.0134(7) 0.0040(8) N32 0.0314(7) 0.0313(7) 0.0349(7) 0.0002(6) 0.0076(6) 0.0007(6) N31 0.0328(7) 0.0343(7) 0.0342(7) -0.0016(6) 0.0077(6) 0.0011(6) C35 0.0321(9) 0.0456(10) 0.0452(10) -0.0027(8) 0.0038(8) 0.0006(8) C34 0.0306(9) 0.0466(11) 0.0489(11) -0.0022(9) 0.0101(8) 0.0038(8) C33 0.0323(8) 0.0292(8) 0.0377(9) 0.0046(7) 0.0096(7) 0.0038(6) N41 0.0698(13) 0.0667(13) 0.0544(11) 0.0025(9) 0.0280(10) 0.0205(10) C42 0.0411(9) 0.0275(8) 0.0370(9) 0.0025(7) 0.0092(7) 0.0082(7) C43 0.0408(10) 0.0352(9) 0.0383(9) 0.0060(7) -0.0003(8) -0.0042(7) C44 0.081(2) 0.0493(13) 0.0584(15) 0.0064(11) -0.0171(13) -0.0115(12) C45 0.123(3) 0.0500(14) 0.0420(13) -0.0092(11) -0.0114(15) 0.024(2) C46 0.103(2) 0.080(2) 0.0443(12) 0.0072(12) 0.0334(14) 0.048(2) C51 0.0349(9) 0.0478(10) 0.0239(7) -0.0011(7) 0.0099(6) -0.0016(7) N62 0.0308(7) 0.0366(8) 0.0264(7) 0.0024(6) 0.0071(5) 0.0003(6) N61 0.0318(7) 0.0399(8) 0.0238(6) 0.0018(6) 0.0063(5) -0.0011(6) C65 0.0345(9) 0.0407(9) 0.0286(8) 0.0040(7) 0.0017(7) 0.0009(7) C64 0.0296(8) 0.0392(9) 0.0324(8) 0.0007(7) 0.0040(7) 0.0023(7) C63 0.0274(8) 0.0293(8) 0.0272(7) -0.0029(6) 0.0051(6) -0.0027(6) N71 0.0299(7) 0.0492(9) 0.0371(8) 0.0033(7) 0.0098(6) -0.0022(6) C72 0.0283(8) 0.0292(8) 0.0291(8) -0.0028(6) 0.0065(6) -0.0049(6) C73 0.0313(8) 0.0330(8) 0.0348(8) 0.0014(7) 0.0090(7) 0.0001(7) C74 0.0418(10) 0.0402(10) 0.0371(9) 0.0080(8) 0.0083(8) -0.0007(8) C75 0.0483(11) 0.0576(12) 0.0403(10) 0.0124(9) 0.0175(9) -0.0041(9) C76 0.0365(10) 0.0660(14) 0.0463(11) 0.0084(10) 0.0197(8) -0.0015(9) _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 C11 C12 1.394(2) . ? C11 C16 1.402(2) . ? C11 C51 1.518(2) . ? C12 C13 1.383(3) . ? C13 C14 1.388(3) . ? C14 C15 1.385(3) . ? C15 C16 1.398(2) . ? C16 C21 1.519(2) . ? C21 N31 1.467(2) . ? N32 C33 1.344(2) . ? N32 N31 1.353(2) . ? N31 C35 1.348(2) . ? C35 C34 1.368(3) . ? C34 C33 1.407(3) . ? C33 C42 1.476(2) . ? N41 C46 1.383(3) . ? N41 C42 1.384(3) . ? C42 C43 1.366(3) . ? C43 C44 1.355(3) . ? C44 C45 1.363(4) . ? C45 C46 1.379(4) . ? C51 N61 1.468(2) . ? N62 C63 1.344(2) . ? N62 N61 1.351(2) . ? N61 C65 1.350(2) . ? C65 C64 1.375(2) . ? C64 C63 1.407(2) . ? C63 C72 1.473(2) . ? N71 C72 1.350(2) . ? N71 C76 1.350(2) . ? C72 C73 1.394(2) . ? C73 C74 1.383(2) . ? C74 C75 1.383(3) . ? C75 C76 1.385(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 C12 C11 C16 119.1(2) . . ? C12 C11 C51 118.3(2) . . ? C16 C11 C51 122.6(2) . . ? C13 C12 C11 121.2(2) . . ? C12 C13 C14 119.8(2) . . ? C15 C14 C13 119.6(2) . . ? C14 C15 C16 121.1(2) . . ? C15 C16 C11 119.1(2) . . ? C15 C16 C21 118.6(2) . . ? C11 C16 C21 122.3(2) . . ? N31 C21 C16 112.98(14) . . ? C33 N32 N31 104.28(14) . . ? C35 N31 N32 112.56(14) . . ? C35 N31 C21 126.6(2) . . ? N32 N31 C21 120.49(14) . . ? N31 C35 C34 107.0(2) . . ? C35 C34 C33 105.0(2) . . ? N32 C33 C34 111.1(2) . . ? N32 C33 C42 121.8(2) . . ? C34 C33 C42 127.1(2) . . ? C46 N41 C42 115.6(2) . . ? C43 C42 N41 123.7(2) . . ? C43 C42 C33 119.7(2) . . ? N41 C42 C33 116.5(2) . . ? C44 C43 C42 117.5(2) . . ? C43 C44 C45 122.8(3) . . ? C44 C45 C46 117.9(2) . . ? C45 C46 N41 122.5(2) . . ? N61 C51 C11 111.84(13) . . ? C63 N62 N61 104.70(13) . . ? N62 N61 C65 112.16(13) . . ? N62 N61 C51 119.48(13) . . ? C65 N61 C51 128.24(14) . . ? N61 C65 C64 107.33(15) . . ? C65 C64 C63 104.59(15) . . ? N62 C63 C64 111.20(14) . . ? N62 C63 C72 119.43(14) . . ? C64 C63 C72 129.27(15) . . ? C72 N71 C76 116.8(2) . . ? N71 C72 C73 122.47(15) . . ? N71 C72 C63 116.21(15) . . ? C73 C72 C63 121.29(14) . . ? C74 C73 C72 119.7(2) . . ? C73 C74 C75 118.4(2) . . ? C74 C75 C76 118.7(2) . . ? N71 C76 C75 123.9(2) . . ? _refine_diff_density_max 0.325 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.047 #=END data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24.50 H21 Cl Cu F6 N6 P' _chemical_formula_weight 643.43 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 tetragonal _symmetry_space_group_name_H-M 'P 4(3) 2(1) 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 16.3084(14) _cell_length_b 16.308(2) _cell_length_c 19.627(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5220.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method ? _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33732 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6003 _reflns_number_observed 4669 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+4.5299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 6003 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_obs 0.0535 _refine_ls_wR_factor_all 0.1576 _refine_ls_wR_factor_obs 0.1421 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.029 _refine_ls_restrained_S_obs 1.058 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.61657(3) 0.77534(4) 0.08849(3) 0.0410(2) Uani 1 d . . N11 N 0.5079(2) 0.7448(3) 0.0459(2) 0.0384(9) Uani 1 d . . C12 C 0.4911(3) 0.6635(3) 0.0477(2) 0.0396(10) Uani 1 d . . C13 C 0.4228(3) 0.6311(4) 0.0161(3) 0.0561(15) Uani 1 d . . H13 H 0.4112(3) 0.5741(4) 0.0191(3) 0.067 Uiso 1 calc R . C14 C 0.3716(3) 0.6831(5) -0.0201(3) 0.064(2) Uani 1 d . . H14 H 0.3247(3) 0.6617(5) -0.0427(3) 0.077 Uiso 1 calc R . C15 C 0.3882(3) 0.7644(5) -0.0232(3) 0.058(2) Uani 1 d . . H15 H 0.3533(3) 0.8003(5) -0.0478(3) 0.070 Uiso 1 calc R . C16 C 0.4573(3) 0.7945(4) 0.0104(3) 0.0525(13) Uani 1 d . . H16 H 0.4691(3) 0.8515(4) 0.0082(3) 0.063 Uiso 1 calc R . N21 N 0.6196(2) 0.6516(2) 0.1063(2) 0.0350(8) Uani 1 d . . N22 N 0.6601(2) 0.5961(2) 0.1453(2) 0.0386(9) Uani 1 d . . C23 C 0.6165(4) 0.5261(3) 0.1508(3) 0.0557(14) Uani 1 d . . H23 H 0.6321(4) 0.4787(3) 0.1757(3) 0.067 Uiso 1 calc R . C24 C 0.5459(4) 0.5357(3) 0.1142(3) 0.0563(15) Uani 1 d . . H24 H 0.5032(4) 0.4967(3) 0.1082(3) 0.068 Uiso 1 calc R . C25 C 0.5498(3) 0.6143(3) 0.0876(2) 0.0373(9) Uani 1 d . . C3 C 0.7353(3) 0.6191(3) 0.1811(2) 0.0441(11) Uani 1 d . . H3A H 0.7309(3) 0.6012(3) 0.2291(2) 0.053 Uiso 1 calc R . H3B H 0.7401(3) 0.6796(3) 0.1809(2) 0.053 Uiso 1 calc R . C41 C 0.8126(3) 0.5829(3) 0.1506(2) 0.0416(11) Uani 1 d . . C42 C 0.8586(3) 0.6230(3) 0.1008(2) 0.0345(9) Uani 1 d . . C43 C 0.9315(3) 0.5892(3) 0.0785(3) 0.0455(12) Uani 1 d . . H43A H 0.9634(3) 0.6173(3) 0.0454(3) 0.055 Uiso 1 calc R . C44 C 0.9590(4) 0.5134(4) 0.1042(3) 0.063(2) Uani 1 d . . H44A H 1.0088(4) 0.4901(4) 0.0880(3) 0.076 Uiso 1 calc R . C45 C 0.9140(4) 0.4738(4) 0.1522(4) 0.074(2) Uani 1 d . . H45 H 0.9323(4) 0.4225(4) 0.1694(4) 0.089 Uiso 1 calc R . C46 C 0.8402(4) 0.5080(4) 0.1767(3) 0.060(2) Uani 1 d . . H46 H 0.8093(4) 0.4803(4) 0.2107(3) 0.072 Uiso 1 calc R . N51 N 0.6511(2) 0.8380(3) 0.1744(2) 0.0396(9) Uani 1 d . . C52 C 0.6989(3) 0.9038(3) 0.1617(2) 0.0389(10) Uani 1 d . . C53 C 0.7184(3) 0.9595(3) 0.2135(3) 0.0478(12) Uani 1 d . . H53 H 0.7516(3) 1.0060(3) 0.2043(3) 0.057 Uiso 1 calc R . C54 C 0.6883(4) 0.9454(4) 0.2790(3) 0.056(2) Uani 1 d . . H54 H 0.6990(4) 0.9835(4) 0.3144(3) 0.067 Uiso 1 calc R . C55 C 0.6426(3) 0.8752(4) 0.2920(3) 0.0568(15) Uani 1 d . . H55 H 0.6239(3) 0.8625(4) 0.3366(3) 0.068 Uiso 1 calc R . C56 C 0.6260(3) 0.8261(4) 0.2388(3) 0.0566(14) Uani 1 d . . H56 H 0.5937(3) 0.7788(4) 0.2475(3) 0.068 Uiso 1 calc R . N61 N 0.6958(2) 0.8566(2) 0.0463(2) 0.0312(7) Uani 1 d . . N62 N 0.7326(2) 0.8722(2) -0.0138(2) 0.0339(7) Uani 1 d . . C63 C 0.7879(3) 0.9335(3) -0.0073(3) 0.0436(11) Uani 1 d . . H43 H 0.8216(3) 0.9547(3) -0.0426(3) 0.052 Uiso 1 calc R . C64 C 0.7868(3) 0.9596(3) 0.0594(3) 0.0416(11) Uani 1 d . . H44 H 0.8186(3) 1.0019(3) 0.0796(3) 0.050 Uiso 1 calc R . C65 C 0.7278(3) 0.9094(2) 0.0907(2) 0.0355(9) Uani 1 d . . C7 C 0.7054(3) 0.8298(3) -0.0745(2) 0.0362(10) Uani 1 d . . H7A H 0.7021(3) 0.7704(3) -0.0645(2) 0.043 Uiso 1 calc R . H7B H 0.7469(3) 0.8376(3) -0.1108(2) 0.043 Uiso 1 calc R . P1 P 0.82484(10) 1.10616(10) 0.37092(7) 0.0530(4) Uani 1 d . . F1 F 0.8039(4) 1.1929(3) 0.3991(3) 0.119(2) Uani 1 d . . F2 F 0.9014(3) 1.1399(4) 0.3330(2) 0.123(2) Uani 1 d . . F3 F 0.8477(2) 1.0190(3) 0.3413(2) 0.0875(14) Uani 1 d . . F4 F 0.7481(2) 1.0706(3) 0.4073(2) 0.0802(13) Uani 1 d . . F5 F 0.7678(3) 1.1209(2) 0.3057(2) 0.0799(12) Uani 1 d . . F6 F 0.8796(2) 1.0901(3) 0.4366(2) 0.0679(10) Uani 1 d . . C80 C 0.7136(6) 1.2864(6) 0.2500 0.114(5) Uani 1 d S . H80A H 0.7145(6) 1.2368(6) 0.2792 0.136 Uiso 0.50 calc PR . H80B H 0.7632(6) 1.2855(6) 0.2208 0.136 Uiso 0.50 calc PR . Cl81 Cl 0.62605(12) 1.28550(14) 0.19900(8) 0.0829(6) Uani 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 Cu1 0.0339(3) 0.0402(3) 0.0487(3) 0.0015(3) -0.0070(3) -0.0115(2) N11 0.026(2) 0.055(3) 0.035(2) -0.002(2) 0.0002(15) -0.005(2) C12 0.032(2) 0.053(3) 0.033(2) -0.014(2) 0.008(2) -0.009(2) C13 0.038(3) 0.077(4) 0.053(3) -0.022(3) 0.005(2) -0.015(3) C14 0.034(3) 0.109(5) 0.049(3) -0.015(3) -0.008(2) -0.011(3) C15 0.034(3) 0.104(5) 0.038(2) 0.004(3) 0.000(2) 0.007(3) C16 0.036(3) 0.077(4) 0.044(3) 0.007(3) 0.001(2) -0.002(2) N21 0.036(2) 0.041(2) 0.028(2) 0.0005(14) 0.0045(15) -0.004(2) N22 0.041(2) 0.039(2) 0.036(2) 0.004(2) 0.009(2) 0.001(2) C23 0.057(3) 0.036(3) 0.073(4) 0.010(2) 0.017(3) 0.001(2) C24 0.048(3) 0.037(3) 0.084(4) -0.003(3) 0.011(3) -0.011(2) C25 0.036(2) 0.036(2) 0.040(2) -0.011(2) 0.008(2) -0.006(2) C3 0.048(3) 0.056(3) 0.029(2) 0.010(2) 0.002(2) -0.002(2) C41 0.037(2) 0.056(3) 0.032(2) 0.009(2) -0.005(2) 0.007(2) C42 0.032(2) 0.041(2) 0.030(2) 0.002(2) -0.007(2) 0.006(2) C43 0.033(2) 0.059(3) 0.044(3) 0.005(2) -0.002(2) 0.009(2) C44 0.045(3) 0.069(4) 0.076(4) 0.014(3) -0.001(3) 0.025(3) C45 0.062(4) 0.068(4) 0.094(5) 0.033(4) -0.012(4) 0.021(3) C46 0.060(3) 0.056(3) 0.063(4) 0.025(3) 0.005(3) 0.012(3) N51 0.032(2) 0.051(2) 0.036(2) -0.004(2) -0.004(2) -0.001(2) C52 0.038(2) 0.041(2) 0.038(2) -0.004(2) -0.011(2) 0.007(2) C53 0.046(3) 0.048(3) 0.049(3) -0.012(2) -0.011(2) 0.001(2) C54 0.052(3) 0.078(4) 0.037(2) -0.023(3) -0.016(2) 0.026(3) C55 0.043(3) 0.086(4) 0.041(3) -0.003(3) -0.001(2) 0.006(3) C56 0.038(3) 0.090(4) 0.042(3) 0.003(3) -0.001(2) 0.001(3) N61 0.037(2) 0.029(2) 0.028(2) -0.0023(14) -0.0036(14) -0.0030(14) N62 0.039(2) 0.030(2) 0.033(2) 0.0074(14) -0.005(2) -0.0025(15) C63 0.044(3) 0.037(2) 0.050(3) 0.010(2) -0.005(2) -0.009(2) C64 0.043(3) 0.029(2) 0.053(3) 0.004(2) -0.011(2) -0.008(2) C65 0.037(2) 0.025(2) 0.044(2) -0.001(2) -0.011(2) -0.001(2) C7 0.046(3) 0.033(2) 0.029(2) -0.003(2) -0.003(2) 0.002(2) P1 0.0527(8) 0.0622(9) 0.0441(7) -0.0014(7) 0.0005(6) -0.0093(7) F1 0.179(6) 0.057(3) 0.121(4) -0.032(3) -0.032(4) 0.003(3) F2 0.113(4) 0.198(6) 0.059(2) 0.024(3) -0.007(2) -0.092(4) F3 0.054(2) 0.121(4) 0.087(3) -0.038(3) -0.008(2) 0.027(2) F4 0.041(2) 0.144(4) 0.056(2) -0.039(2) 0.001(2) -0.012(2) F5 0.094(3) 0.076(3) 0.070(2) 0.017(2) -0.023(2) -0.008(2) F6 0.045(2) 0.115(3) 0.043(2) 0.009(2) -0.0078(14) -0.018(2) C80 0.100(6) 0.100(6) 0.141(12) -0.025(7) -0.025(7) 0.021(8) Cl81 0.0858(13) 0.109(2) 0.0535(8) -0.0059(9) 0.0029(8) -0.0230(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.022(4) . ? Cu1 N61 2.028(4) . ? Cu1 N21 2.049(4) . ? Cu1 N51 2.050(4) . ? N11 C16 1.351(7) . ? N11 C12 1.353(7) . ? C12 C13 1.380(7) . ? C12 C25 1.474(7) . ? C13 C14 1.387(9) . ? C14 C15 1.354(10) . ? C15 C16 1.395(8) . ? N21 C25 1.341(6) . ? N21 N22 1.356(5) . ? N22 C23 1.349(6) . ? N22 C3 1.462(6) . ? C23 C24 1.366(9) . ? C24 C25 1.386(7) . ? C3 C41 1.516(7) . ? C41 C42 1.395(7) . ? C41 C46 1.398(7) . ? C42 C43 1.382(7) . ? C42 C7 1.514(6) 7 ? C43 C44 1.409(8) . ? C44 C45 1.358(9) . ? C45 C46 1.412(9) . ? N51 C56 1.343(7) . ? N51 C52 1.350(6) . ? C52 C53 1.400(7) . ? C52 C65 1.473(7) . ? C53 C54 1.394(8) . ? C54 C55 1.389(9) . ? C55 C56 1.344(8) . ? N61 C65 1.332(5) . ? N61 N62 1.348(5) . ? N62 C63 1.352(6) . ? N62 C7 1.446(6) . ? C63 C64 1.378(7) . ? C64 C65 1.404(7) . ? C7 C42 1.514(6) 7 ? P1 F2 1.554(4) . ? P1 F4 1.554(4) . ? P1 F1 1.557(5) . ? P1 F3 1.580(4) . ? P1 F6 1.589(3) . ? P1 F5 1.599(4) . ? C80 Cl81 1.744(8) 8_775 ? C80 Cl81 1.744(8) . ? 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 N11 Cu1 N61 123.4(2) . . ? N11 Cu1 N21 81.3(2) . . ? N61 Cu1 N21 134.27(15) . . ? N11 Cu1 N51 134.7(2) . . ? N61 Cu1 N51 80.48(15) . . ? N21 Cu1 N51 110.1(2) . . ? C16 N11 C12 118.6(4) . . ? C16 N11 Cu1 126.9(4) . . ? C12 N11 Cu1 114.1(3) . . ? N11 C12 C13 121.8(5) . . ? N11 C12 C25 114.6(4) . . ? C13 C12 C25 123.6(5) . . ? C12 C13 C14 118.8(6) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 119.1(6) . . ? N11 C16 C15 121.7(6) . . ? C25 N21 N22 105.4(4) . . ? C25 N21 Cu1 112.3(3) . . ? N22 N21 Cu1 139.9(3) . . ? C23 N22 N21 110.6(4) . . ? C23 N22 C3 128.3(5) . . ? N21 N22 C3 120.6(4) . . ? N22 C23 C24 107.8(5) . . ? C23 C24 C25 105.4(5) . . ? N21 C25 C24 110.7(5) . . ? N21 C25 C12 116.8(4) . . ? C24 C25 C12 132.4(4) . . ? N22 C3 C41 114.1(4) . . ? C42 C41 C46 119.6(5) . . ? C42 C41 C3 122.7(4) . . ? C46 C41 C3 117.6(4) . . ? C43 C42 C41 119.8(4) . . ? C43 C42 C7 120.8(4) . 7 ? C41 C42 C7 119.3(4) . 7 ? C42 C43 C44 120.7(5) . . ? C45 C44 C43 119.6(5) . . ? C44 C45 C46 120.6(6) . . ? C41 C46 C45 119.6(5) . . ? C56 N51 C52 117.7(5) . . ? C56 N51 Cu1 128.2(4) . . ? C52 N51 Cu1 113.8(3) . . ? N51 C52 C53 120.8(5) . . ? N51 C52 C65 114.1(4) . . ? C53 C52 C65 125.1(5) . . ? C54 C53 C52 118.9(5) . . ? C55 C54 C53 119.6(5) . . ? C56 C55 C54 117.1(5) . . ? N51 C56 C55 125.7(6) . . ? C65 N61 N62 106.0(4) . . ? C65 N61 Cu1 113.9(3) . . ? N62 N61 Cu1 139.9(3) . . ? N61 N62 C63 110.7(4) . . ? N61 N62 C7 119.6(4) . . ? C63 N62 C7 129.4(4) . . ? N62 C63 C64 108.0(4) . . ? C63 C64 C65 104.1(4) . . ? N61 C65 C64 111.1(4) . . ? N61 C65 C52 117.0(4) . . ? C64 C65 C52 131.9(4) . . ? N62 C7 C42 113.9(4) . 7 ? F2 P1 F4 178.5(3) . . ? F2 P1 F1 91.4(4) . . ? F4 P1 F1 89.9(3) . . ? F2 P1 F3 87.3(3) . . ? F4 P1 F3 91.3(3) . . ? F1 P1 F3 178.7(3) . . ? F2 P1 F6 89.7(2) . . ? F4 P1 F6 91.1(2) . . ? F1 P1 F6 89.1(3) . . ? F3 P1 F6 91.1(2) . . ? F2 P1 F5 91.8(2) . . ? F4 P1 F5 87.5(2) . . ? F1 P1 F5 91.2(3) . . ? F3 P1 F5 88.7(2) . . ? F6 P1 F5 178.5(2) . . ? Cl81 C80 Cl81 110.0(7) 8_775 . ? _refine_diff_density_max 0.684 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.081 #=END data_gem _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H20 B Cl Cu F4 N6' _chemical_formula_weight 578.26 _chemical_melting_point ? _chemical_compound_source ? 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 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.333(2) _cell_length_b 8.492(2) _cell_length_c 17.002(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.423(9) _cell_angle_gamma 90.00 _cell_volume 2358.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method ? _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23437 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5371 _reflns_number_observed 3973 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0708P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5371 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_obs 0.0362 _refine_ls_wR_factor_all 0.1078 _refine_ls_wR_factor_obs 0.0889 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.95373(2) 0.69189(4) -0.16768(2) 0.02311(11) Uani 1 d . . Cl Cl 0.94160(4) 0.92495(8) -0.10126(4) 0.0305(2) Uani 1 d . . C11 C 0.6933(2) 0.6919(3) -0.10254(15) 0.0243(5) Uani 1 d . . C12 C 0.6833(2) 0.6192(3) -0.17641(15) 0.0238(6) Uani 1 d . . C13 C 0.6102(2) 0.6437(4) -0.2177(2) 0.0308(6) Uani 1 d . . H13 H 0.6031(2) 0.5955(4) -0.2678(2) 0.037 Uiso 1 calc R . C14 C 0.5478(2) 0.7355(4) -0.1883(2) 0.0351(7) Uani 1 d . . H14 H 0.4992(2) 0.7516(4) -0.2182(2) 0.042 Uiso 1 calc R . C15 C 0.5566(2) 0.8042(3) -0.1148(2) 0.0347(7) Uani 1 d . . C16 C 0.6285(2) 0.7815(3) -0.0726(2) 0.0299(6) Uani 1 d . . H16 H 0.6341(2) 0.8279(3) -0.0220(2) 0.036 Uiso 1 calc R . H15 H 0.5136(2) 0.8661(3) -0.0935(2) 0.036 Uiso 1 d R . C2 C 0.7459(2) 0.5104(3) -0.21534(15) 0.0241(6) Uani 1 d . . H2A H 0.7840(2) 0.4700(3) -0.17453(15) 0.029 Uiso 1 calc R . H2B H 0.7167(2) 0.4190(3) -0.23840(15) 0.029 Uiso 1 calc R . C3 C 0.7707(2) 0.6994(3) -0.0525(2) 0.0291(6) Uani 1 d . . H3A H 0.8036(2) 0.7894(3) -0.0715(2) 0.035 Uiso 1 calc R . H3B H 0.7542(2) 0.7241(3) 0.0020(2) 0.035 Uiso 1 calc R . N41 N 0.86743(12) 0.6521(2) -0.26101(12) 0.0216(5) Uani 1 d . . N42 N 0.79352(13) 0.5883(2) -0.27735(12) 0.0224(5) Uani 1 d . . C43 C 0.7739(2) 0.6066(3) -0.35404(15) 0.0280(6) Uani 1 d . . H43 H 0.7250(2) 0.5718(3) -0.37899(15) 0.034 Uiso 1 calc R . C44 C 0.8374(2) 0.6847(3) -0.38973(15) 0.0266(6) Uani 1 d . . H44 H 0.8415(2) 0.7142(3) -0.44345(15) 0.032 Uiso 1 calc R . C45 C 0.8942(2) 0.7108(3) -0.33005(14) 0.0225(5) Uani 1 d . . N51 N 1.01103(13) 0.7973(3) -0.25802(12) 0.0251(5) Uani 1 d . . C52 C 0.9740(2) 0.7896(3) -0.32925(15) 0.0236(6) Uani 1 d . . C53 C 1.0090(2) 0.8575(4) -0.3954(2) 0.0326(6) Uani 1 d . . H53 H 0.9833(2) 0.8475(4) -0.4455(2) 0.039 Uiso 1 calc R . C54 C 1.0813(2) 0.9394(4) -0.3874(2) 0.0366(7) Uani 1 d . . H54 H 1.1058(2) 0.9874(4) -0.4318(2) 0.044 Uiso 1 calc R . C55 C 1.1180(2) 0.9510(4) -0.3140(2) 0.0368(7) Uani 1 d . . H55 H 1.1673(2) 1.0090(4) -0.3072(2) 0.044 Uiso 1 calc R . C56 C 1.0818(2) 0.8768(4) -0.2506(2) 0.0318(6) Uani 1 d . . H56 H 1.1077(2) 0.8823(4) -0.2005(2) 0.038 Uiso 1 calc R . N61 N 0.89651(12) 0.5599(3) -0.08798(12) 0.0220(5) Uani 1 d . . N62 N 0.82440(13) 0.5617(3) -0.04936(12) 0.0248(5) Uani 1 d . . C63 C 0.8152(2) 0.4274(3) -0.00738(15) 0.0293(6) Uani 1 d . . H63 H 0.7699(2) 0.4020(3) 0.02499(15) 0.035 Uiso 1 calc R . C64 C 0.8827(2) 0.3341(3) -0.01970(15) 0.0276(6) Uani 1 d . . H64 H 0.8935(2) 0.2328(3) 0.00178(15) 0.033 Uiso 1 calc R . C65 C 0.9321(2) 0.4207(3) -0.07074(14) 0.0212(5) Uani 1 d . . N71 N 1.03460(12) 0.5017(2) -0.15986(12) 0.0223(5) Uani 1 d . . C72 C 1.0111(2) 0.3899(3) -0.10747(14) 0.0211(5) Uani 1 d . . C73 C 1.0578(2) 0.2579(3) -0.09156(15) 0.0259(6) Uani 1 d . . H73 H 1.0403(2) 0.1829(3) -0.05376(15) 0.031 Uiso 1 calc R . C74 C 1.1305(2) 0.2367(3) -0.1317(2) 0.0313(6) Uani 1 d . . H74 H 1.1637(2) 0.1469(3) -0.1217(2) 0.038 Uiso 1 calc R . C75 C 1.1542(2) 0.3478(4) -0.1865(2) 0.0313(6) Uani 1 d . . H75 H 1.2033(2) 0.3342(4) -0.2154(2) 0.038 Uiso 1 calc R . C76 C 1.1052(2) 0.4796(3) -0.1989(2) 0.0277(6) Uani 1 d . . H76 H 1.1220(2) 0.5565(3) -0.2360(2) 0.033 Uiso 1 calc R . B1 B 0.7095(2) 0.0943(4) 0.1008(2) 0.0357(8) Uani 0.512(13) d P 1 F1 F 0.7497(11) 0.0391(24) 0.0377(12) 0.031(2) Uani 0.512(13) d P 1 F2 F 0.6485(5) 0.1868(15) 0.0801(5) 0.091(4) Uani 0.512(13) d P 1 F3 F 0.7586(4) 0.2065(14) 0.1468(4) 0.087(3) Uani 0.512(13) d P 1 F4 F 0.6934(9) -0.0244(7) 0.1426(7) 0.120(6) Uani 0.512(13) d P 1 B1' B 0.7095(2) 0.0943(4) 0.1008(2) 0.0357(8) Uani 0.488(13) d P 2 F1' F 0.7648(13) 0.0655(28) 0.0348(15) 0.034(3) Uani 0.488(13) d P 2 F2' F 0.6745(7) 0.2327(9) 0.0890(7) 0.094(4) Uani 0.488(13) d P 2 F3' F 0.7502(5) 0.0726(18) 0.1664(3) 0.094(5) Uani 0.488(13) d P 2 F4' F 0.6381(5) -0.0091(11) 0.1053(5) 0.086(3) Uani 0.488(13) d P 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 Cu1 0.0229(2) 0.0222(2) 0.0242(2) 0.00525(13) -0.00025(12) -0.00183(13) Cl 0.0416(4) 0.0219(3) 0.0281(3) 0.0004(3) -0.0010(3) -0.0040(3) C11 0.0208(12) 0.0225(13) 0.0297(13) 0.0010(11) -0.0004(10) -0.0031(11) C12 0.0232(13) 0.0183(13) 0.0301(14) 0.0022(11) 0.0015(11) -0.0043(11) C13 0.0306(15) 0.031(2) 0.0312(14) 0.0028(12) -0.0029(12) -0.0055(12) C14 0.0241(14) 0.033(2) 0.048(2) 0.0072(14) -0.0096(13) -0.0006(12) C15 0.0231(14) 0.028(2) 0.053(2) 0.0032(14) 0.0047(13) 0.0035(12) C16 0.0248(14) 0.029(2) 0.0354(15) -0.0015(12) 0.0028(12) -0.0018(12) C2 0.0265(13) 0.0197(13) 0.0262(13) -0.0017(10) -0.0008(11) -0.0067(11) C3 0.0232(13) 0.031(2) 0.0331(14) -0.0096(12) -0.0001(11) 0.0010(12) N41 0.0211(11) 0.0203(11) 0.0235(11) 0.0017(8) -0.0012(9) -0.0011(9) N42 0.0229(11) 0.0209(11) 0.0234(11) -0.0022(9) -0.0015(9) -0.0031(9) C43 0.0310(15) 0.029(2) 0.0237(13) -0.0064(11) -0.0067(11) -0.0016(12) C44 0.0343(15) 0.0242(14) 0.0211(12) -0.0013(11) -0.0021(11) -0.0003(12) C45 0.0252(13) 0.0189(13) 0.0234(12) -0.0001(10) 0.0028(10) 0.0020(10) N51 0.0235(11) 0.0227(11) 0.0291(11) 0.0049(9) -0.0004(9) -0.0012(9) C52 0.0257(13) 0.0188(13) 0.0263(13) 0.0025(10) 0.0044(11) 0.0044(11) C53 0.037(2) 0.034(2) 0.0272(14) 0.0044(12) 0.0052(12) 0.0016(13) C54 0.032(2) 0.039(2) 0.039(2) 0.0108(14) 0.0121(13) -0.0008(14) C55 0.028(2) 0.032(2) 0.050(2) 0.0047(14) 0.0070(14) -0.0033(13) C56 0.0243(14) 0.033(2) 0.038(2) 0.0057(13) -0.0004(12) -0.0019(12) N61 0.0191(11) 0.0249(12) 0.0221(10) 0.0010(9) 0.0000(9) -0.0005(9) N62 0.0198(11) 0.0308(13) 0.0238(11) -0.0007(9) 0.0003(9) -0.0016(10) C63 0.0286(15) 0.038(2) 0.0218(13) 0.0029(12) 0.0010(11) -0.0089(13) C64 0.0320(15) 0.027(2) 0.0237(13) 0.0068(11) -0.0010(11) -0.0055(12) C65 0.0235(13) 0.0220(13) 0.0182(11) 0.0009(10) -0.0045(10) -0.0002(11) N71 0.0202(11) 0.0250(12) 0.0217(11) 0.0013(9) -0.0022(9) 0.0002(9) C72 0.0230(13) 0.0217(13) 0.0187(12) -0.0001(10) -0.0047(10) -0.0014(10) C73 0.0308(14) 0.0227(13) 0.0242(13) -0.0003(10) -0.0056(11) -0.0013(12) C74 0.0294(15) 0.030(2) 0.0338(15) -0.0056(12) -0.0103(12) 0.0086(12) C75 0.0221(14) 0.040(2) 0.0319(15) -0.0066(12) 0.0004(11) 0.0043(12) C76 0.0241(14) 0.035(2) 0.0240(13) 0.0010(11) 0.0010(11) 0.0002(12) B1 0.035(2) 0.044(2) 0.028(2) 0.0015(15) 0.0019(15) 0.014(2) F1 0.032(7) 0.035(6) 0.026(3) 0.007(3) 0.012(4) 0.009(4) F2 0.056(4) 0.182(12) 0.036(3) -0.003(5) -0.006(3) 0.078(6) F3 0.069(4) 0.146(8) 0.048(3) -0.029(4) -0.002(3) -0.042(4) F4 0.183(12) 0.047(3) 0.133(9) 0.048(4) 0.133(9) 0.036(5) B1' 0.035(2) 0.044(2) 0.028(2) 0.0015(15) 0.0019(15) 0.014(2) F1' 0.026(5) 0.037(6) 0.040(4) 0.007(4) 0.017(3) -0.002(3) F2' 0.136(9) 0.027(3) 0.119(8) 0.022(3) 0.092(7) 0.037(4) F3' 0.059(4) 0.199(13) 0.025(3) -0.024(5) -0.017(3) 0.072(6) F4' 0.069(5) 0.079(6) 0.111(5) -0.033(4) 0.031(4) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N61 1.996(2) . ? Cu1 N51 2.014(2) . ? Cu1 N71 2.090(2) . ? Cu1 N41 2.141(2) . ? Cu1 Cl 2.2878(8) . ? C11 C16 1.402(4) . ? C11 C12 1.408(4) . ? C11 C3 1.519(4) . ? C12 C13 1.397(4) . ? C12 C2 1.532(4) . ? C13 C14 1.379(4) . ? C14 C15 1.385(4) . ? C15 C16 1.385(4) . ? C2 N42 1.472(3) . ? C3 N62 1.462(3) . ? N41 N42 1.350(3) . ? N41 C45 1.351(3) . ? N42 C43 1.349(3) . ? C43 C44 1.376(4) . ? C44 C45 1.388(4) . ? C45 C52 1.464(4) . ? N51 C56 1.343(3) . ? N51 C52 1.352(3) . ? C52 C53 1.391(4) . ? C53 C54 1.377(4) . ? C54 C55 1.383(4) . ? C55 C56 1.385(4) . ? N61 C65 1.349(3) . ? N61 N62 1.353(3) . ? N62 C63 1.355(3) . ? C63 C64 1.375(4) . ? C64 C65 1.398(3) . ? C65 C72 1.462(3) . ? N71 C76 1.347(3) . ? N71 C72 1.359(3) . ? C72 C73 1.381(4) . ? C73 C74 1.386(4) . ? C74 C75 1.383(4) . ? C75 C76 1.391(4) . ? B1 F4 1.262(6) . ? B1 F2 1.314(8) . ? B1 F1 1.35(2) . ? B1 F3 1.467(6) . ? B1' F3' 1.306(6) . ? B1' F2' 1.322(8) . ? B1' F4' 1.462(7) . ? B1' F1' 1.47(2) . ? 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 N61 Cu1 N51 171.74(9) . . ? N61 Cu1 N71 79.73(8) . . ? N51 Cu1 N71 95.45(8) . . ? N61 Cu1 N41 96.06(8) . . ? N51 Cu1 N41 79.17(8) . . ? N71 Cu1 N41 109.72(8) . . ? N61 Cu1 Cl 96.21(6) . . ? N51 Cu1 Cl 91.96(7) . . ? N71 Cu1 Cl 133.95(6) . . ? N41 Cu1 Cl 116.31(6) . . ? C16 C11 C12 118.6(2) . . ? C16 C11 C3 113.7(2) . . ? C12 C11 C3 127.5(2) . . ? C13 C12 C11 118.4(2) . . ? C13 C12 C2 116.3(2) . . ? C11 C12 C2 125.2(2) . . ? C14 C13 C12 122.2(3) . . ? C13 C14 C15 119.5(3) . . ? C16 C15 C14 119.4(3) . . ? C15 C16 C11 121.8(3) . . ? N42 C2 C12 113.3(2) . . ? N62 C3 C11 118.9(2) . . ? N42 N41 C45 105.3(2) . . ? N42 N41 Cu1 143.0(2) . . ? C45 N41 Cu1 111.7(2) . . ? C43 N42 N41 111.0(2) . . ? C43 N42 C2 128.4(2) . . ? N41 N42 C2 120.6(2) . . ? N42 C43 C44 107.9(2) . . ? C43 C44 C45 104.9(2) . . ? N41 C45 C44 110.9(2) . . ? N41 C45 C52 117.0(2) . . ? C44 C45 C52 132.1(2) . . ? C56 N51 C52 119.2(2) . . ? C56 N51 Cu1 123.8(2) . . ? C52 N51 Cu1 117.0(2) . . ? N51 C52 C53 121.4(3) . . ? N51 C52 C45 115.0(2) . . ? C53 C52 C45 123.6(2) . . ? C54 C53 C52 119.1(3) . . ? C53 C54 C55 119.4(3) . . ? C54 C55 C56 119.0(3) . . ? N51 C56 C55 121.9(3) . . ? C65 N61 N62 106.3(2) . . ? C65 N61 Cu1 115.9(2) . . ? N62 N61 Cu1 137.4(2) . . ? N61 N62 C63 110.3(2) . . ? N61 N62 C3 121.1(2) . . ? C63 N62 C3 128.6(2) . . ? N62 C63 C64 108.2(2) . . ? C63 C64 C65 105.0(2) . . ? N61 C65 C64 110.3(2) . . ? N61 C65 C72 116.4(2) . . ? C64 C65 C72 133.3(2) . . ? C76 N71 C72 118.2(2) . . ? C76 N71 Cu1 128.2(2) . . ? C72 N71 Cu1 113.6(2) . . ? N71 C72 C73 122.5(2) . . ? N71 C72 C65 114.2(2) . . ? C73 C72 C65 123.3(2) . . ? C72 C73 C74 118.8(3) . . ? C75 C74 C73 119.2(3) . . ? C74 C75 C76 119.2(2) . . ? N71 C76 C75 122.1(3) . . ? F4 B1 F2 117.9(6) . . ? F4 B1 F1 106.0(9) . . ? F2 B1 F1 111.6(10) . . ? F4 B1 F3 109.6(6) . . ? F2 B1 F3 99.5(5) . . ? F1 B1 F3 112.4(8) . . ? F3' B1' F2' 118.2(7) . . ? F3' B1' F4' 105.8(6) . . ? F2' B1' F4' 101.4(5) . . ? F3' B1' F1' 108.5(10) . . ? F2' B1' F1' 107.4(11) . . ? F4' B1' F1' 115.9(9) . . ? _refine_diff_density_max 0.429 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.114 #=END data_srip _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C49 H44 B2 Cu2 F14 N12 O Si' _chemical_formula_weight 1259.75 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1351(15) _cell_length_b 18.355(4) _cell_length_c 27.362(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.284(14) _cell_angle_gamma 90.00 _cell_volume 5023.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method ? _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50899 _diffrn_reflns_av_R_equivalents 0.1098 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11519 _reflns_number_observed 6677 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+8.9760P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11517 _refine_ls_number_parameters 749 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_obs 0.0628 _refine_ls_wR_factor_all 0.1247 _refine_ls_wR_factor_obs 0.1000 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_restrained_S_all 1.153 _refine_ls_restrained_S_obs 1.295 _refine_ls_shift/esd_max 0.369 _refine_ls_shift/esd_mean 0.010 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.75214(6) 0.84146(3) 0.18140(2) 0.02201(15) Uani 1 d . . Cu2 Cu 0.22617(6) 1.10303(3) 0.33362(2) 0.0239(2) Uani 1 d . . N111 N 0.7392(4) 0.7354(2) 0.15215(14) 0.0221(9) Uani 1 d . . C112 C 0.6516(5) 0.7303(3) 0.1097(2) 0.0217(11) Uani 1 d . . C113 C 0.6230(5) 0.6648(3) 0.0851(2) 0.0278(12) Uani 1 d . . H11A H 0.5586(5) 0.6625(3) 0.0558(2) 0.033 Uiso 1 calc R . C114 C 0.6901(5) 0.6027(3) 0.1041(2) 0.0308(12) Uani 1 d . . H11B H 0.6732(5) 0.5573(3) 0.0877(2) 0.037 Uiso 1 calc R . C115 C 0.7822(5) 0.6075(3) 0.1473(2) 0.0322(12) Uani 1 d . . H11C H 0.8298(5) 0.5657(3) 0.1609(2) 0.039 Uiso 1 calc R . C116 C 0.8028(5) 0.6743(2) 0.1699(2) 0.0261(11) Uani 1 d . . H11D H 0.8653(5) 0.6775(2) 0.1997(2) 0.031 Uiso 1 calc R . N121 N 0.6255(4) 0.8586(2) 0.12077(14) 0.0211(9) Uani 1 d . . C122 C 0.5917(5) 0.8002(3) 0.0917(2) 0.0233(11) Uani 1 d . . C123 C 0.5082(5) 0.8210(3) 0.0485(2) 0.0275(12) Uani 1 d . . H12A H 0.4699(5) 0.7907(3) 0.0218(2) 0.033 Uiso 1 calc R . C124 C 0.4936(5) 0.8950(3) 0.0529(2) 0.0271(11) Uani 1 d . . H12B H 0.4419(5) 0.9260(3) 0.0293(2) 0.033 Uiso 1 calc R . N125 N 0.5653(4) 0.9160(2) 0.09633(14) 0.0221(9) Uani 1 d . . C126 C 0.5757(5) 0.9884(2) 0.1195(2) 0.0252(11) Uani 1 d . . H12C H 0.6199(5) 0.9826(2) 0.1543(2) 0.030 Uiso 1 calc R . H12D H 0.4840(5) 1.0064(2) 0.1203(2) 0.030 Uiso 1 calc R . C131 C 0.6505(5) 1.0470(3) 0.0957(2) 0.0237(11) Uani 1 d . . C132 C 0.7773(5) 1.0394(3) 0.0822(2) 0.0241(11) Uani 1 d . . C133 C 0.8360(5) 1.0999(3) 0.0633(2) 0.0310(12) Uani 1 d . . H13A H 0.9200(5) 1.0944(3) 0.0526(2) 0.037 Uiso 1 calc R . C134 C 0.7749(6) 1.1675(3) 0.0598(2) 0.0342(13) Uani 1 d . . H13B H 0.8182(6) 1.2084(3) 0.0481(2) 0.041 Uiso 1 calc R . C135 C 0.6509(5) 1.1749(3) 0.0735(2) 0.0298(12) Uani 1 d . . H13C H 0.6084(5) 1.2212(3) 0.0712(2) 0.036 Uiso 1 calc R . C136 C 0.5873(5) 1.1153(3) 0.0905(2) 0.0272(12) Uani 1 d . . H13D H 0.5003(5) 1.1208(3) 0.0988(2) 0.033 Uiso 1 calc R . N141 N 0.9091(4) 0.9069(2) 0.16614(14) 0.0225(9) Uani 1 d . . C142 C 1.0155(5) 0.9029(2) 0.2021(2) 0.0221(10) Uani 1 d . . C143 C 1.1150(5) 0.9505(3) 0.1928(2) 0.0286(12) Uani 1 d . . H14A H 1.1997(5) 0.9585(3) 0.2126(2) 0.034 Uiso 1 calc R . C144 C 1.0646(5) 0.9836(3) 0.1487(2) 0.0289(12) Uani 1 d . . H14B H 1.1089(5) 1.0190(3) 0.1320(2) 0.035 Uiso 1 calc R . N145 N 0.9409(4) 0.9566(2) 0.13343(14) 0.0229(9) Uani 1 d . . C146 C 0.8549(5) 0.9686(3) 0.0854(2) 0.0250(11) Uani 1 d . . H14C H 0.7908(5) 0.9277(3) 0.0790(2) 0.030 Uiso 1 calc R . H14D H 0.9112(5) 0.9681(3) 0.0590(2) 0.030 Uiso 1 calc R . N151 N 0.8870(4) 0.8188(2) 0.24032(13) 0.0212(9) Uani 1 d . . C152 C 1.0071(5) 0.8516(2) 0.2423(2) 0.0212(10) Uani 1 d . . C153 C 1.1128(5) 0.8356(3) 0.2796(2) 0.0262(11) Uani 1 d . . H15A H 1.1980(5) 0.8572(3) 0.2797(2) 0.031 Uiso 1 calc R . C154 C 1.0925(5) 0.7877(3) 0.3166(2) 0.0288(12) Uani 1 d . . H15B H 1.1638(5) 0.7758(3) 0.3423(2) 0.035 Uiso 1 calc R . C155 C 0.9670(5) 0.7573(3) 0.3158(2) 0.0299(12) Uani 1 d . . H15C H 0.9502(5) 0.7256(3) 0.3415(2) 0.036 Uiso 1 calc R . C156 C 0.8670(5) 0.7739(3) 0.2770(2) 0.0270(12) Uani 1 d . . H15D H 0.7811(5) 0.7528(3) 0.2763(2) 0.032 Uiso 1 calc R . N211 N 0.2766(4) 1.2034(2) 0.36548(14) 0.0215(9) Uani 1 d . . C212 C 0.3770(5) 1.1994(2) 0.4048(2) 0.0209(10) Uani 1 d . . C213 C 0.4208(5) 1.2595(3) 0.4330(2) 0.0288(12) Uani 1 d . . H21A H 0.4929(5) 1.2555(3) 0.4597(2) 0.035 Uiso 1 calc R . C214 C 0.3580(5) 1.3257(3) 0.4217(2) 0.0316(13) Uani 1 d . . H21B H 0.3858(5) 1.3677(3) 0.4409(2) 0.038 Uiso 1 calc R . C215 C 0.2541(5) 1.3299(3) 0.3821(2) 0.0307(12) Uani 1 d . . H21C H 0.2104(5) 1.3750(3) 0.3736(2) 0.037 Uiso 1 calc R . C216 C 0.2153(5) 1.2682(2) 0.3555(2) 0.0260(11) Uani 1 d . . H21D H 0.1425(5) 1.2712(2) 0.3289(2) 0.031 Uiso 1 calc R . N221 N 0.3785(4) 1.0740(2) 0.38311(14) 0.0196(9) Uani 1 d . . C222 C 0.4314(4) 1.1263(2) 0.4146(2) 0.0201(10) Uani 1 d . . C223 C 0.5275(5) 1.0962(3) 0.4514(2) 0.0256(11) Uani 1 d . . H22A H 0.5802(5) 1.1208(3) 0.4783(2) 0.031 Uiso 1 calc R . C224 C 0.5290(5) 1.0234(3) 0.4403(2) 0.0238(11) Uani 1 d . . H22B H 0.5840(5) 0.9876(3) 0.4586(2) 0.029 Uiso 1 calc R . N225 N 0.4401(4) 1.0112(2) 0.39941(13) 0.0197(9) Uani 1 d . . C226 C 0.4075(5) 0.9424(2) 0.3722(2) 0.0223(11) Uani 1 d . . H22C H 0.4886(5) 0.9246(2) 0.3601(2) 0.027 Uiso 1 calc R . H22D H 0.3389(5) 0.9524(2) 0.3428(2) 0.027 Uiso 1 calc R . C231 C 0.3565(5) 0.8830(2) 0.4027(2) 0.0214(11) Uani 1 d . . C232 C 0.4215(5) 0.8158(2) 0.4048(2) 0.0271(12) Uani 1 d . . H23A H 0.4986(5) 0.8105(2) 0.3895(2) 0.032 Uiso 1 calc R . C233 C 0.3760(5) 0.7568(3) 0.4287(2) 0.0318(13) Uani 1 d . . H23B H 0.4214(5) 0.7114(3) 0.4297(2) 0.038 Uiso 1 calc R . C234 C 0.2642(5) 0.7643(3) 0.4513(2) 0.0307(13) Uani 1 d . . H23C H 0.2319(5) 0.7238(3) 0.4675(2) 0.037 Uiso 1 calc R . C235 C 0.1994(5) 0.8306(3) 0.4503(2) 0.0276(12) Uani 1 d . . H23D H 0.1237(5) 0.8356(3) 0.4665(2) 0.033 Uiso 1 calc R . C236 C 0.2436(5) 0.8904(2) 0.4259(2) 0.0212(10) Uani 1 d . . N241 N 0.0942(4) 1.0239(2) 0.34508(13) 0.0199(9) Uani 1 d . . C242 C -0.0144(4) 1.0216(2) 0.3096(2) 0.0210(10) Uani 1 d . . C243 C -0.1020(5) 0.9675(2) 0.3199(2) 0.0248(11) Uani 1 d . . H24A H -0.1848(5) 0.9541(2) 0.3005(2) 0.030 Uiso 1 calc R . C244 C -0.0434(5) 0.9378(2) 0.3638(2) 0.0237(11) Uani 1 d . . H24B H -0.0791(5) 0.8997(2) 0.3811(2) 0.028 Uiso 1 calc R . N245 N 0.0746(4) 0.9722(2) 0.37833(14) 0.0205(9) Uani 1 d . . C246 C 0.1656(5) 0.9609(2) 0.4254(2) 0.0214(11) Uani 1 d . . H24C H 0.1129(5) 0.9602(2) 0.4529(2) 0.026 Uiso 1 calc R . H24D H 0.2290(5) 1.0022(2) 0.4311(2) 0.026 Uiso 1 calc R . N251 N 0.0785(4) 1.1273(2) 0.27851(14) 0.0249(9) Uani 1 d . . C252 C -0.0218(5) 1.0770(3) 0.2714(2) 0.0223(11) Uani 1 d . . C253 C -0.1228(5) 1.0807(3) 0.2307(2) 0.0262(11) Uani 1 d . . H25A H -0.1920(5) 1.0452(3) 0.2262(2) 0.031 Uiso 1 calc R . C254 C -0.1219(5) 1.1366(3) 0.1967(2) 0.0305(13) Uani 1 d . . H25B H -0.1896(5) 1.1394(3) 0.1684(2) 0.037 Uiso 1 calc R . C255 C -0.0220(5) 1.1877(3) 0.2045(2) 0.0314(12) Uani 1 d . . H25C H -0.0206(5) 1.2269(3) 0.1819(2) 0.038 Uiso 1 calc R . C256 C 0.0765(5) 1.1816(3) 0.2456(2) 0.0296(12) Uani 1 d . . H25D H 0.1455(5) 1.2171(3) 0.2507(2) 0.035 Uiso 1 calc R . B1 B 0.2211(6) 0.0579(3) 0.0434(2) 0.0294(14) Uani 1 d D . F11 F 0.1591(4) -0.0087(2) 0.04477(14) 0.0732(12) Uani 1 d D . F12 F 0.3309(3) 0.0519(2) 0.02092(11) 0.0515(9) Uani 1 d D . F13 F 0.2551(3) 0.0858(2) 0.09154(10) 0.0418(8) Uani 1 d D . F14 F 0.1305(3) 0.1052(2) 0.01606(12) 0.0585(10) Uani 1 d D . B2 B -0.1901(6) 0.8832(3) 0.4835(2) 0.037(2) Uani 1 d D . F21 F -0.3185(5) 0.8632(3) 0.4679(3) 0.054(2) Uani 0.676(13) d PD 1 F22 F -0.1537(5) 0.9528(2) 0.47276(13) 0.0774(13) Uani 1 d D . F23 F -0.1709(6) 0.8790(3) 0.5377(2) 0.039(2) Uani 0.676(13) d PD 1 F24 F -0.1013(3) 0.8344(2) 0.47217(15) 0.0694(12) Uani 1 d D . F21' F -0.2694(23) 0.8899(9) 0.5116(9) 0.126(12) Uani 0.324(13) d PD 2 F23' F -0.2727(18) 0.8763(8) 0.4311(7) 0.112(8) Uani 0.324(13) d PD 2 Si Si 0.54255(13) 0.89280(7) 0.25090(5) 0.0229(3) Uani 1 d . . F31 F 0.5682(3) 0.81383(15) 0.22081(10) 0.0321(7) Uani 1 d . . F32 F 0.4115(3) 0.8581(2) 0.27246(11) 0.0392(8) Uani 1 d . . F33 F 0.4425(3) 0.9235(2) 0.20047(10) 0.0349(7) Uani 1 d . . F34 F 0.6778(3) 0.92678(15) 0.22664(10) 0.0292(7) Uani 1 d . . F35 F 0.5301(3) 0.97455(15) 0.27904(10) 0.0352(7) Uani 1 d . . F36 F 0.6437(3) 0.86427(14) 0.30058(9) 0.0304(7) Uani 1 d . . C1 C 0.3546(7) 1.1008(4) 0.2269(3) 0.066(2) Uani 1 d . . H1A H 0.4160(7) 1.0711(4) 0.2110(3) 0.099 Uiso 1 calc R . H1B H 0.3892(7) 1.1506(4) 0.2314(3) 0.099 Uiso 1 calc R . H1C H 0.2665(7) 1.1015(4) 0.2060(3) 0.099 Uiso 1 calc R . O1 O 0.3432(4) 1.0701(2) 0.27433(13) 0.0455(10) Uani 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 Cu1 0.0218(3) 0.0222(3) 0.0202(3) 0.0000(3) -0.0021(2) -0.0018(3) Cu2 0.0228(3) 0.0193(3) 0.0261(3) 0.0025(3) -0.0064(3) -0.0011(3) N111 0.023(2) 0.022(2) 0.021(2) -0.003(2) 0.005(2) 0.000(2) C112 0.021(3) 0.026(3) 0.020(2) -0.002(2) 0.006(2) -0.004(2) C113 0.030(3) 0.029(3) 0.024(3) -0.003(2) 0.002(2) -0.007(2) C114 0.039(3) 0.016(2) 0.041(3) -0.006(2) 0.016(3) -0.009(2) C115 0.035(3) 0.022(3) 0.043(3) 0.001(2) 0.016(3) 0.003(2) C116 0.026(3) 0.024(3) 0.029(3) 0.000(2) 0.006(2) 0.003(2) N121 0.021(2) 0.021(2) 0.021(2) 0.000(2) 0.001(2) -0.002(2) C122 0.024(3) 0.024(3) 0.022(3) -0.001(2) 0.006(2) -0.004(2) C123 0.034(3) 0.028(3) 0.019(3) -0.003(2) -0.001(2) -0.005(2) C124 0.027(3) 0.033(3) 0.020(2) 0.008(2) -0.002(2) -0.005(2) N125 0.024(2) 0.021(2) 0.020(2) 0.001(2) -0.001(2) -0.002(2) C126 0.027(3) 0.023(3) 0.025(3) -0.003(2) 0.001(2) 0.001(2) C131 0.029(3) 0.023(3) 0.018(2) -0.001(2) 0.001(2) 0.001(2) C132 0.031(3) 0.024(3) 0.017(2) 0.002(2) 0.001(2) 0.000(2) C133 0.033(3) 0.039(3) 0.023(3) 0.004(2) 0.008(2) -0.002(3) C134 0.044(4) 0.029(3) 0.028(3) 0.008(2) 0.001(3) -0.010(3) C135 0.041(3) 0.023(3) 0.022(3) 0.003(2) -0.005(2) -0.001(2) C136 0.028(3) 0.028(3) 0.024(3) 0.000(2) -0.002(2) -0.001(2) N141 0.023(2) 0.024(2) 0.020(2) 0.000(2) 0.002(2) -0.001(2) C142 0.020(3) 0.025(3) 0.021(2) -0.005(2) 0.004(2) 0.002(2) C143 0.018(3) 0.035(3) 0.033(3) -0.003(2) 0.004(2) -0.002(2) C144 0.024(3) 0.032(3) 0.032(3) 0.000(2) 0.011(2) -0.002(2) N145 0.021(2) 0.025(2) 0.022(2) 0.003(2) 0.003(2) 0.003(2) C146 0.027(3) 0.031(3) 0.017(2) 0.005(2) 0.003(2) -0.004(2) N151 0.021(2) 0.022(2) 0.019(2) -0.001(2) 0.001(2) -0.002(2) C152 0.021(3) 0.022(3) 0.021(2) -0.009(2) 0.004(2) 0.001(2) C153 0.018(3) 0.030(3) 0.028(3) -0.006(2) -0.001(2) 0.005(2) C154 0.028(3) 0.034(3) 0.023(3) -0.003(2) -0.002(2) 0.007(2) C155 0.037(3) 0.027(3) 0.026(3) 0.007(2) 0.007(2) 0.008(2) C156 0.028(3) 0.024(3) 0.029(3) 0.004(2) 0.004(2) -0.005(2) N211 0.019(2) 0.022(2) 0.023(2) 0.000(2) 0.002(2) -0.001(2) C212 0.019(3) 0.019(2) 0.024(3) 0.003(2) 0.003(2) -0.001(2) C213 0.028(3) 0.023(3) 0.032(3) -0.001(2) -0.004(2) 0.000(2) C214 0.041(3) 0.022(3) 0.031(3) -0.007(2) 0.004(3) -0.002(2) C215 0.038(3) 0.018(3) 0.037(3) 0.003(2) 0.011(3) 0.004(2) C216 0.030(3) 0.018(2) 0.028(3) 0.003(2) 0.001(2) 0.003(2) N221 0.018(2) 0.017(2) 0.024(2) 0.005(2) 0.003(2) 0.002(2) C222 0.019(3) 0.019(2) 0.022(2) 0.001(2) 0.001(2) -0.001(2) C223 0.021(3) 0.028(3) 0.024(3) 0.000(2) -0.006(2) -0.004(2) C224 0.020(3) 0.024(3) 0.025(3) 0.004(2) -0.005(2) 0.002(2) N225 0.022(2) 0.015(2) 0.021(2) -0.001(2) 0.002(2) 0.002(2) C226 0.027(3) 0.018(2) 0.023(3) -0.002(2) 0.004(2) -0.001(2) C231 0.026(3) 0.019(2) 0.018(2) -0.003(2) -0.001(2) -0.005(2) C232 0.026(3) 0.021(3) 0.032(3) -0.001(2) 0.000(2) 0.001(2) C233 0.036(3) 0.021(3) 0.035(3) 0.002(2) -0.005(3) -0.002(2) C234 0.034(3) 0.021(3) 0.035(3) 0.008(2) -0.002(3) -0.006(2) C235 0.028(3) 0.033(3) 0.020(3) 0.004(2) 0.001(2) -0.006(2) C236 0.025(3) 0.020(2) 0.016(2) -0.001(2) -0.003(2) -0.001(2) N241 0.023(2) 0.018(2) 0.018(2) 0.001(2) 0.001(2) 0.001(2) C242 0.018(3) 0.021(2) 0.021(2) -0.007(2) -0.004(2) 0.004(2) C243 0.014(2) 0.023(3) 0.036(3) -0.010(2) -0.001(2) 0.001(2) C244 0.020(3) 0.017(2) 0.034(3) -0.006(2) 0.005(2) -0.001(2) N245 0.022(2) 0.017(2) 0.022(2) -0.003(2) 0.004(2) 0.002(2) C246 0.021(3) 0.027(3) 0.016(2) -0.002(2) 0.000(2) -0.001(2) N251 0.027(2) 0.023(2) 0.022(2) -0.001(2) -0.003(2) 0.002(2) C252 0.020(3) 0.027(3) 0.019(2) -0.007(2) 0.000(2) 0.004(2) C253 0.023(3) 0.029(3) 0.025(3) -0.007(2) -0.003(2) 0.001(2) C254 0.030(3) 0.032(3) 0.024(3) -0.006(2) -0.012(2) 0.015(2) C255 0.042(3) 0.029(3) 0.022(3) 0.002(2) 0.002(2) 0.004(3) C256 0.032(3) 0.021(3) 0.033(3) 0.005(2) -0.001(2) 0.001(2) B1 0.039(4) 0.020(3) 0.030(3) -0.003(3) 0.009(3) 0.002(3) F11 0.121(4) 0.038(2) 0.072(3) -0.012(2) 0.051(3) -0.032(2) F12 0.033(2) 0.084(3) 0.041(2) -0.004(2) 0.015(2) -0.005(2) F13 0.045(2) 0.049(2) 0.032(2) -0.0008(15) 0.0081(15) -0.006(2) F14 0.058(2) 0.053(2) 0.058(2) -0.022(2) -0.010(2) 0.019(2) B2 0.026(3) 0.032(4) 0.052(4) -0.002(3) 0.007(3) 0.001(3) F21 0.025(3) 0.071(4) 0.064(5) -0.010(4) -0.001(3) 0.003(3) F22 0.150(4) 0.036(2) 0.050(2) 0.000(2) 0.026(3) -0.019(2) F23 0.038(4) 0.043(3) 0.037(3) 0.009(2) 0.007(2) 0.003(3) F24 0.048(2) 0.053(2) 0.106(3) -0.029(2) 0.006(2) 0.020(2) F21' 0.155(22) 0.099(13) 0.159(23) -0.076(14) 0.137(21) -0.072(14) F23' 0.106(14) 0.117(13) 0.091(14) 0.021(10) -0.049(12) -0.036(10) Si 0.0193(7) 0.0273(7) 0.0221(7) -0.0005(6) 0.0036(6) -0.0015(6) F31 0.034(2) 0.034(2) 0.030(2) -0.0067(13) 0.0086(13) -0.0028(13) F32 0.029(2) 0.045(2) 0.045(2) -0.0011(15) 0.0124(14) -0.0074(14) F33 0.026(2) 0.042(2) 0.035(2) 0.0005(14) -0.0015(13) 0.0012(13) F34 0.025(2) 0.036(2) 0.0260(15) 0.0043(13) 0.0029(12) -0.0060(13) F35 0.041(2) 0.030(2) 0.036(2) -0.0052(14) 0.0100(15) 0.0014(14) F36 0.033(2) 0.033(2) 0.0237(15) 0.0004(12) 0.0000(13) -0.0054(13) C1 0.064(5) 0.051(4) 0.090(6) 0.031(4) 0.032(4) 0.012(4) O1 0.048(3) 0.065(3) 0.026(2) 0.009(2) 0.011(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N121 1.952(4) . ? Cu1 N151 1.982(4) . ? Cu1 N141 2.089(4) . ? Cu1 N111 2.100(4) . ? Cu1 F34 2.203(3) . ? Cu1 F31 2.355(3) . ? Cu2 N221 1.957(4) . ? Cu2 N251 1.996(4) . ? Cu2 N241 2.033(4) . ? Cu2 N211 2.066(4) . ? Cu2 O1 2.242(4) . ? N111 C116 1.345(6) . ? N111 C112 1.346(6) . ? C112 C113 1.387(6) . ? C112 C122 1.469(6) . ? C113 C114 1.384(7) . ? C114 C115 1.385(7) . ? C115 C116 1.375(7) . ? N121 N125 1.341(5) . ? N121 C122 1.346(6) . ? C122 C123 1.392(6) . ? C123 C124 1.374(7) . ? C124 N125 1.346(6) . ? N125 C126 1.469(6) . ? C126 C131 1.521(6) . ? C131 C132 1.401(7) . ? C131 C136 1.405(6) . ? C132 C133 1.397(7) . ? C132 C146 1.514(6) . ? C133 C134 1.383(7) . ? C134 C135 1.375(7) . ? C135 C136 1.388(7) . ? N141 C142 1.340(6) . ? N141 N145 1.353(5) . ? C142 C143 1.388(6) . ? C142 C152 1.460(6) . ? C143 C144 1.373(7) . ? C144 N145 1.350(6) . ? N145 C146 1.472(6) . ? N151 C156 1.340(6) . ? N151 C152 1.352(6) . ? C152 C153 1.386(6) . ? C153 C154 1.380(7) . ? C154 C155 1.386(7) . ? C155 C156 1.377(6) . ? N211 C216 1.351(6) . ? N211 C212 1.358(6) . ? C212 C213 1.377(6) . ? C212 C222 1.460(6) . ? C213 C214 1.384(7) . ? C214 C215 1.387(7) . ? C215 C216 1.370(6) . ? N221 C222 1.342(6) . ? N221 N225 1.352(5) . ? C222 C223 1.397(6) . ? C223 C224 1.372(6) . ? C224 N225 1.338(5) . ? N225 C226 1.476(5) . ? C226 C231 1.515(6) . ? C231 C232 1.395(6) . ? C231 C236 1.400(6) . ? C232 C233 1.382(7) . ? C233 C234 1.382(7) . ? C234 C235 1.382(7) . ? C235 C236 1.397(6) . ? C236 C246 1.515(6) . ? N241 C242 1.345(5) . ? N241 N245 1.350(5) . ? C242 C243 1.390(6) . ? C242 C252 1.454(6) . ? C243 C244 1.363(6) . ? C244 N245 1.355(6) . ? N245 C246 1.473(5) . ? N251 C256 1.340(6) . ? N251 C252 1.364(6) . ? C252 C253 1.386(6) . ? C253 C254 1.386(7) . ? C254 C255 1.372(7) . ? C255 C256 1.383(7) . ? B1 F12 1.361(6) . ? B1 F11 1.377(6) . ? B1 F14 1.390(6) . ? B1 F13 1.404(6) . ? B2 F21' 1.207(11) . ? B2 F24 1.340(7) . ? B2 F21 1.353(7) . ? B2 F22 1.375(7) . ? B2 F23 1.468(8) . ? B2 F23' 1.544(13) . ? Si F36 1.650(3) . ? Si F32 1.665(3) . ? Si F33 1.673(3) . ? Si F35 1.701(3) . ? Si F31 1.707(3) . ? Si F34 1.733(3) . ? C1 O1 1.436(7) . ? 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 N121 Cu1 N151 175.9(2) . . ? N121 Cu1 N141 98.91(15) . . ? N151 Cu1 N141 80.55(15) . . ? N121 Cu1 N111 80.40(15) . . ? N151 Cu1 N111 96.22(15) . . ? N141 Cu1 N111 117.37(15) . . ? N121 Cu1 F34 97.20(13) . . ? N151 Cu1 F34 86.88(13) . . ? N141 Cu1 F34 92.52(12) . . ? N111 Cu1 F34 150.08(13) . . ? N121 Cu1 F31 87.89(13) . . ? N151 Cu1 F31 94.32(13) . . ? N141 Cu1 F31 154.20(12) . . ? N111 Cu1 F31 88.24(13) . . ? F34 Cu1 F31 61.84(9) . . ? N221 Cu2 N251 174.6(2) . . ? N221 Cu2 N241 99.44(15) . . ? N251 Cu2 N241 81.0(2) . . ? N221 Cu2 N211 80.63(15) . . ? N251 Cu2 N211 102.9(2) . . ? N241 Cu2 N211 134.08(15) . . ? N221 Cu2 O1 88.66(14) . . ? N251 Cu2 O1 86.17(15) . . ? N241 Cu2 O1 110.91(15) . . ? N211 Cu2 O1 115.0(2) . . ? C116 N111 C112 117.7(4) . . ? C116 N111 Cu1 129.7(3) . . ? C112 N111 Cu1 112.7(3) . . ? N111 C112 C113 122.4(4) . . ? N111 C112 C122 114.1(4) . . ? C113 C112 C122 123.5(4) . . ? C114 C113 C112 118.7(5) . . ? C113 C114 C115 119.4(5) . . ? C116 C115 C114 118.2(5) . . ? N111 C116 C115 123.5(5) . . ? N125 N121 C122 106.2(4) . . ? N125 N121 Cu1 137.2(3) . . ? C122 N121 Cu1 116.3(3) . . ? N121 C122 C123 110.2(4) . . ? N121 C122 C112 116.4(4) . . ? C123 C122 C112 133.3(4) . . ? C124 C123 C122 104.9(4) . . ? N125 C124 C123 108.0(4) . . ? N121 N125 C124 110.7(4) . . ? N121 N125 C126 120.0(4) . . ? C124 N125 C126 129.2(4) . . ? N125 C126 C131 117.4(4) . . ? C132 C131 C136 119.0(4) . . ? C132 C131 C126 125.8(4) . . ? C136 C131 C126 115.1(4) . . ? C133 C132 C131 118.9(4) . . ? C133 C132 C146 117.1(4) . . ? C131 C132 C146 124.0(4) . . ? C134 C133 C132 121.8(5) . . ? C135 C134 C133 119.2(5) . . ? C134 C135 C136 120.6(5) . . ? C135 C136 C131 120.6(5) . . ? C142 N141 N145 105.9(4) . . ? C142 N141 Cu1 111.7(3) . . ? N145 N141 Cu1 142.2(3) . . ? N141 C142 C143 110.7(4) . . ? N141 C142 C152 116.8(4) . . ? C143 C142 C152 132.5(4) . . ? C144 C143 C142 105.1(4) . . ? N145 C144 C143 107.8(4) . . ? C144 N145 N141 110.5(4) . . ? C144 N145 C146 127.5(4) . . ? N141 N145 C146 121.5(4) . . ? N145 C146 C132 114.0(4) . . ? C156 N151 C152 119.2(4) . . ? C156 N151 Cu1 124.8(3) . . ? C152 N151 Cu1 116.0(3) . . ? N151 C152 C153 121.2(4) . . ? N151 C152 C142 114.7(4) . . ? C153 C152 C142 124.0(4) . . ? C154 C153 C152 119.1(5) . . ? C153 C154 C155 119.3(5) . . ? C156 C155 C154 118.9(5) . . ? N151 C156 C155 122.1(5) . . ? C216 N211 C212 118.0(4) . . ? C216 N211 Cu2 128.7(3) . . ? C212 N211 Cu2 112.9(3) . . ? N211 C212 C213 122.2(4) . . ? N211 C212 C222 114.0(4) . . ? C213 C212 C222 123.7(4) . . ? C212 C213 C214 118.9(5) . . ? C213 C214 C215 119.1(5) . . ? C216 C215 C214 119.1(5) . . ? N211 C216 C215 122.5(5) . . ? C222 N221 N225 106.4(3) . . ? C222 N221 Cu2 116.0(3) . . ? N225 N221 Cu2 137.0(3) . . ? N221 C222 C223 109.9(4) . . ? N221 C222 C212 116.1(4) . . ? C223 C222 C212 134.0(4) . . ? C224 C223 C222 104.8(4) . . ? N225 C224 C223 108.6(4) . . ? C224 N225 N221 110.2(4) . . ? C224 N225 C226 129.2(4) . . ? N221 N225 C226 120.6(4) . . ? N225 C226 C231 113.9(4) . . ? C232 C231 C236 118.8(4) . . ? C232 C231 C226 117.3(4) . . ? C236 C231 C226 123.8(4) . . ? C233 C232 C231 121.4(5) . . ? C232 C233 C234 119.6(5) . . ? C233 C234 C235 120.0(5) . . ? C234 C235 C236 120.9(5) . . ? C235 C236 C231 119.3(4) . . ? C235 C236 C246 117.8(4) . . ? C231 C236 C246 122.9(4) . . ? C242 N241 N245 105.8(4) . . ? C242 N241 Cu2 113.2(3) . . ? N245 N241 Cu2 141.0(3) . . ? N241 C242 C243 110.6(4) . . ? N241 C242 C252 116.0(4) . . ? C243 C242 C252 133.2(4) . . ? C244 C243 C242 105.1(4) . . ? N245 C244 C243 108.2(4) . . ? N241 N245 C244 110.3(4) . . ? N241 N245 C246 123.3(4) . . ? C244 N245 C246 126.1(4) . . ? N245 C246 C236 112.3(4) . . ? C256 N251 C252 118.4(4) . . ? C256 N251 Cu2 127.0(3) . . ? C252 N251 Cu2 114.1(3) . . ? N251 C252 C253 121.2(4) . . ? N251 C252 C242 114.8(4) . . ? C253 C252 C242 123.9(4) . . ? C254 C253 C252 119.4(5) . . ? C255 C254 C253 119.1(4) . . ? C254 C255 C256 119.2(5) . . ? N251 C256 C255 122.5(5) . . ? F12 B1 F11 110.5(4) . . ? F12 B1 F14 108.9(4) . . ? F11 B1 F14 107.7(5) . . ? F12 B1 F13 111.0(5) . . ? F11 B1 F13 110.1(4) . . ? F14 B1 F13 108.5(4) . . ? F21' B2 F24 139.3(12) . . ? F24 B2 F21 113.2(5) . . ? F21' B2 F22 105.6(9) . . ? F24 B2 F22 111.0(5) . . ? F21 B2 F22 117.5(6) . . ? F24 B2 F23 102.4(5) . . ? F21 B2 F23 105.5(6) . . ? F22 B2 F23 105.5(5) . . ? F21' B2 F23' 106.5(14) . . ? F24 B2 F23' 90.8(8) . . ? F22 B2 F23' 90.1(7) . . ? F36 Si F32 90.7(2) . . ? F36 Si F33 178.6(2) . . ? F32 Si F33 90.5(2) . . ? F36 Si F35 89.34(15) . . ? F32 Si F35 93.2(2) . . ? F33 Si F35 89.8(2) . . ? F36 Si F31 90.30(15) . . ? F32 Si F31 92.2(2) . . ? F33 Si F31 90.41(15) . . ? F35 Si F31 174.6(2) . . ? F36 Si F34 90.29(14) . . ? F32 Si F34 177.9(2) . . ? F33 Si F34 88.54(14) . . ? F35 Si F34 88.67(15) . . ? F31 Si F34 85.97(14) . . ? Si F31 Cu1 103.37(13) . . ? Si F34 Cu1 108.83(14) . . ? C1 O1 Cu2 132.6(4) . . ? _refine_diff_density_max 0.755 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.101 #=END