# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1180 data_1.CH3CN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H41 B2 Cu2 F8 N7 O4' _chemical_formula_weight 900.43 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.059(2) _cell_length_b 21.760(4) _cell_length_c 21.431(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.50(1) _cell_angle_gamma 90.00 _cell_volume 3716.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 5 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 7596 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6524 _reflns_number_gt 3793 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. There is some disorder in one of the BF~4~^-^ counter ions, this was modeled as a rotation about the B1-F11 bond. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.3680P] 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 6524 _refine_ls_number_parameters 536 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.004 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.02742(9) 0.69753(3) 0.01097(3) 0.0271(2) Uani 1 1 d . . . Cu2 Cu 0.00451(9) 0.84646(3) 0.00696(3) 0.0265(2) Uani 1 1 d . . . O1 O -0.0879(5) 0.63963(19) -0.04775(17) 0.0283(10) Uani 1 1 d . . . C1 C -0.1517(7) 0.5865(3) -0.0362(3) 0.0281(15) Uani 1 1 d . . . C2 C -0.2439(7) 0.5524(3) -0.0867(3) 0.0279(14) Uani 1 1 d . . . C3 C -0.3117(8) 0.4955(3) -0.0753(3) 0.0328(15) Uani 1 1 d . . . H3 H -0.3712 0.4734 -0.1098 0.039 Uiso 1 1 calc R . . C4 C -0.2959(8) 0.4698(3) -0.0158(3) 0.0328(15) Uani 1 1 d . . . C5 C -0.3752(8) 0.4080(3) -0.0053(3) 0.0462(19) Uani 1 1 d . . . H5A H -0.4729 0.4141 0.0163 0.069 Uiso 1 1 calc R . . H5B H -0.2931 0.3819 0.0206 0.069 Uiso 1 1 calc R . . H5C H -0.4108 0.3881 -0.0461 0.069 Uiso 1 1 calc R . . C6 C -0.2102(8) 0.5033(3) 0.0333(3) 0.0337(16) Uani 1 1 d . . . H6 H -0.1987 0.4864 0.0745 0.040 Uiso 1 1 calc R . . C7 C -0.1391(8) 0.5610(3) 0.0255(3) 0.0281(15) Uani 1 1 d . . . C8 C -0.0581(8) 0.5921(3) 0.0803(3) 0.0339(16) Uani 1 1 d . . . H8 H -0.0531 0.5706 0.1191 0.041 Uiso 1 1 calc R . . N1 N 0.0090(7) 0.6458(3) 0.0833(2) 0.0384(14) Uani 1 1 d . . . C9 C 0.0723(13) 0.6703(4) 0.1470(3) 0.072(3) Uani 1 1 d . . . H9A H -0.0226 0.6885 0.1651 0.087 Uiso 1 1 calc R . . H9B H 0.1175 0.6358 0.1746 0.087 Uiso 1 1 calc R . . C10 C 0.2032(9) 0.7168(4) 0.1468(3) 0.047(2) Uani 1 1 d . . . H10A H 0.2887 0.7003 0.1226 0.056 Uiso 1 1 calc R . . H10B H 0.2585 0.7226 0.1908 0.056 Uiso 1 1 calc R . . C11 C 0.1506(12) 0.7774(4) 0.1209(3) 0.062(2) Uani 1 1 d . . . H11 H 0.2593 0.7989 0.1188 0.075 Uiso 1 1 calc R . . O2 O 0.0749(5) 0.7739(2) 0.05585(17) 0.0355(10) Uani 1 1 d . . . C12 C 0.0659(13) 0.8177(4) 0.1568(3) 0.078(3) Uani 1 1 d . . . H12A H 0.1204 0.8140 0.2012 0.094 Uiso 1 1 calc R . . H12B H -0.0498 0.8018 0.1551 0.094 Uiso 1 1 calc R . . C13 C 0.0519(10) 0.8841(3) 0.1422(3) 0.0440(19) Uani 1 1 d . . . H13A H 0.1660 0.9021 0.1491 0.053 Uiso 1 1 calc R . . H13B H -0.0130 0.9038 0.1725 0.053 Uiso 1 1 calc R . . N2 N -0.0287(6) 0.8999(2) 0.0771(2) 0.0297(12) Uani 1 1 d . . . C14 C -0.1097(8) 0.9508(3) 0.0710(3) 0.0332(16) Uani 1 1 d . . . H14 H -0.1120 0.9736 0.1087 0.040 Uiso 1 1 calc R . . C15 C -0.1975(7) 0.9779(3) 0.0142(3) 0.0284(15) Uani 1 1 d . . . C16 C -0.2809(8) 1.0338(3) 0.0194(3) 0.0347(16) Uani 1 1 d . . . H16 H -0.2726 1.0523 0.0599 0.042 Uiso 1 1 calc R . . C17 C -0.3744(8) 1.0635(3) -0.0309(3) 0.0373(17) Uani 1 1 d . . . C18 C -0.4623(9) 1.1239(3) -0.0224(4) 0.049(2) Uani 1 1 d . . . H18A H -0.3803 1.1575 -0.0188 0.073 Uiso 1 1 calc R . . H18B H -0.5148 1.1221 0.0160 0.073 Uiso 1 1 calc R . . H18C H -0.5486 1.1312 -0.0589 0.073 Uiso 1 1 calc R . . C19 C -0.3830(7) 1.0356(3) -0.0892(3) 0.0323(16) Uani 1 1 d . . . H19 H -0.4468 1.0548 -0.1247 0.039 Uiso 1 1 calc R . . C20 C -0.3009(7) 0.9798(3) -0.0979(3) 0.0291(15) Uani 1 1 d . . . C21 C -0.2047(7) 0.9497(3) -0.0456(3) 0.0256(14) Uani 1 1 d . . . O3 O -0.1307(5) 0.89748(19) -0.05497(17) 0.0277(10) Uani 1 1 d . . . C22 C -0.3200(8) 0.9554(3) -0.1606(3) 0.0316(15) Uani 1 1 d . . . H22 H -0.3807 0.9798 -0.1931 0.038 Uiso 1 1 calc R . . N3 N -0.2632(6) 0.9041(2) -0.1771(2) 0.0275(12) Uani 1 1 d . . . H3N H -0.2079 0.8808 -0.1474 0.033 Uiso 1 1 calc R . . C23 C -0.2842(8) 0.8815(3) -0.2421(3) 0.0347(17) Uani 1 1 d . . . H23A H -0.1720 0.8767 -0.2550 0.042 Uiso 1 1 calc R . . H23B H -0.3460 0.9128 -0.2699 0.042 Uiso 1 1 calc R . . C24 C -0.3767(8) 0.8211(3) -0.2519(3) 0.0331(16) Uani 1 1 d . . . H24A H -0.4172 0.8160 -0.2975 0.040 Uiso 1 1 calc R . . H24B H -0.4764 0.8228 -0.2299 0.040 Uiso 1 1 calc R . . C25 C -0.2734(8) 0.7654(3) -0.2287(3) 0.0334(15) Uani 1 1 d . . . H25 H -0.1667 0.7658 -0.2473 0.040 Uiso 1 1 calc R . . O4 O -0.2338(6) 0.7686(3) -0.1607(2) 0.0517(13) Uani 1 1 d . . . H4O H -0.1292 0.7687 -0.1502 0.062 Uiso 1 1 calc R . . C26 C -0.3643(9) 0.7059(3) -0.2456(3) 0.0378(17) Uani 1 1 d . . . H26A H -0.4131 0.7072 -0.2908 0.045 Uiso 1 1 calc R . . H26B H -0.4582 0.7024 -0.2208 0.045 Uiso 1 1 calc R . . C27 C -0.2541(9) 0.6486(3) -0.2339(3) 0.0365(16) Uani 1 1 d . . . H27A H -0.3078 0.6147 -0.2604 0.044 Uiso 1 1 calc R . . H27B H -0.1445 0.6571 -0.2477 0.044 Uiso 1 1 calc R . . N4 N -0.2246(6) 0.6280(2) -0.1684(2) 0.0254(12) Uani 1 1 d . . . H4N H -0.1717 0.6530 -0.1399 0.031 Uiso 1 1 calc R . . C28 C -0.2715(7) 0.5753(3) -0.1500(3) 0.0261(14) Uani 1 1 d . . . H28 H -0.3298 0.5492 -0.1814 0.031 Uiso 1 1 calc R . . N5 N 0.0924(6) 0.7407(2) -0.0610(2) 0.0250(12) Uani 1 1 d . . . N6 N 0.0851(6) 0.8032(2) -0.0630(2) 0.0284(12) Uani 1 1 d . . . C29 C 0.1338(7) 0.8219(3) -0.1169(3) 0.0308(15) Uani 1 1 d . . . H29 H 0.1384 0.8635 -0.1300 0.037 Uiso 1 1 calc R . . C30 C 0.1762(8) 0.7719(3) -0.1507(3) 0.0339(15) Uani 1 1 d . . . H30 H 0.2157 0.7720 -0.1904 0.041 Uiso 1 1 calc R . . C31 C 0.1486(7) 0.7215(3) -0.1141(3) 0.0316(15) Uani 1 1 d . . . H31 H 0.1665 0.6799 -0.1246 0.038 Uiso 1 1 calc R . . C32 C 0.4252(10) 0.2673(4) 0.0393(4) 0.060(2) Uani 1 1 d . . . H32A H 0.3489 0.2386 0.0560 0.089 Uiso 1 1 calc R . . H32B H 0.4126 0.3083 0.0570 0.089 Uiso 1 1 calc R . . H32C H 0.5411 0.2532 0.0511 0.089 Uiso 1 1 calc R . . C33 C 0.3849(10) 0.2699(4) -0.0290(5) 0.060(2) Uani 1 1 d . . . N7 N 0.3561(10) 0.2716(4) -0.0819(4) 0.084(2) Uani 1 1 d . . . B1 B 0.2309(11) 0.5439(4) 0.2793(4) 0.049(2) Uani 0.50 1 d PD A 1 F11 F 0.2921(5) 0.48777(17) 0.29965(18) 0.0540(12) Uani 0.50 1 d PD A 1 F12 F 0.3192(16) 0.5944(5) 0.2865(6) 0.073(4) Uani 0.50 1 d PD A 1 F13 F 0.0873(13) 0.5486(7) 0.3079(6) 0.044(3) Uani 0.50 1 d PD A 1 F14 F 0.1628(14) 0.5358(5) 0.2129(3) 0.066(3) Uani 0.50 1 d PD A 1 B1' B 0.2309(11) 0.5439(4) 0.2793(4) 0.049(2) Uani 0.50 1 d PD B 2 F11' F 0.2921(5) 0.48777(17) 0.29965(18) 0.0540(12) Uani 0.50 1 d PD B 2 F12' F 0.3415(13) 0.5829(5) 0.3247(5) 0.054(3) Uani 0.50 1 d PD B 2 F13' F 0.0782(15) 0.5618(9) 0.2825(7) 0.084(6) Uani 0.50 1 d PD B 2 F14' F 0.3019(16) 0.5567(5) 0.2255(4) 0.080(3) Uani 0.50 1 d PD B 2 B2 B 0.3001(9) 0.9231(4) 0.3019(4) 0.043(2) Uani 1 1 d D . . F21 F 0.1343(5) 0.9061(2) 0.2941(2) 0.0686(14) Uani 1 1 d D . . F22 F 0.3891(5) 0.8875(2) 0.34863(19) 0.0656(14) Uani 1 1 d D . . F23 F 0.3658(5) 0.9173(2) 0.24696(18) 0.0621(13) Uani 1 1 d D . . F24 F 0.3173(7) 0.9847(2) 0.3203(2) 0.0839(16) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0320(4) 0.0304(4) 0.0184(4) 0.0027(3) 0.0017(3) 0.0046(4) Cu2 0.0319(4) 0.0292(4) 0.0175(4) -0.0023(3) 0.0012(3) -0.0021(4) O1 0.037(2) 0.026(2) 0.021(2) 0.0049(18) 0.0029(18) -0.002(2) C1 0.024(3) 0.032(4) 0.031(3) 0.004(3) 0.011(3) 0.006(3) C2 0.029(3) 0.024(3) 0.031(3) 0.008(3) 0.002(3) 0.002(3) C3 0.033(4) 0.026(4) 0.040(4) 0.001(3) 0.006(3) 0.006(3) C4 0.029(4) 0.024(3) 0.047(4) 0.013(3) 0.011(3) 0.008(3) C5 0.042(4) 0.041(5) 0.056(5) 0.018(4) 0.010(4) 0.004(4) C6 0.036(4) 0.035(4) 0.033(4) 0.017(3) 0.014(3) 0.015(3) C7 0.034(4) 0.026(4) 0.024(3) 0.010(3) 0.006(3) 0.011(3) C8 0.047(4) 0.031(4) 0.025(3) 0.012(3) 0.009(3) 0.012(3) N1 0.057(4) 0.033(4) 0.024(3) 0.003(3) 0.001(3) 0.007(3) C9 0.127(8) 0.062(6) 0.023(4) 0.004(4) -0.003(5) -0.008(6) C10 0.044(4) 0.074(6) 0.018(3) 0.002(3) -0.010(3) 0.016(4) C11 0.105(7) 0.057(5) 0.017(3) 0.001(4) -0.015(4) 0.007(5) O2 0.054(3) 0.035(3) 0.0149(19) -0.003(2) -0.0024(19) 0.004(2) C12 0.124(8) 0.079(7) 0.026(4) -0.008(4) -0.011(5) 0.047(6) C13 0.072(5) 0.043(5) 0.015(3) -0.004(3) -0.002(3) -0.005(4) N2 0.037(3) 0.029(3) 0.023(3) -0.007(2) 0.006(2) -0.009(3) C14 0.036(4) 0.034(4) 0.031(4) -0.012(3) 0.009(3) -0.012(3) C15 0.027(3) 0.030(4) 0.028(3) -0.003(3) 0.006(3) -0.009(3) C16 0.033(4) 0.031(4) 0.041(4) -0.012(3) 0.011(3) -0.006(3) C17 0.024(3) 0.035(4) 0.053(4) -0.010(3) 0.006(3) -0.002(3) C18 0.042(4) 0.034(4) 0.070(5) -0.016(4) 0.009(4) -0.004(3) C19 0.020(3) 0.032(4) 0.043(4) 0.001(3) -0.002(3) 0.002(3) C20 0.022(3) 0.030(4) 0.034(4) -0.002(3) 0.001(3) -0.004(3) C21 0.022(3) 0.023(3) 0.032(3) -0.004(3) 0.003(3) -0.002(3) O3 0.032(2) 0.031(2) 0.019(2) -0.0038(19) -0.0002(18) 0.006(2) C22 0.029(3) 0.027(4) 0.036(4) 0.003(3) -0.004(3) 0.000(3) N3 0.031(3) 0.024(3) 0.027(3) 0.005(2) -0.001(2) 0.002(2) C23 0.048(4) 0.032(4) 0.020(3) -0.004(3) -0.007(3) 0.003(3) C24 0.041(4) 0.030(4) 0.025(3) -0.001(3) -0.011(3) 0.000(3) C25 0.038(4) 0.036(4) 0.024(3) 0.000(3) -0.001(3) 0.001(3) O4 0.055(3) 0.054(3) 0.041(3) -0.003(3) -0.010(2) 0.005(3) C26 0.050(4) 0.032(4) 0.027(3) 0.002(3) -0.008(3) 0.001(3) C27 0.056(4) 0.028(4) 0.024(3) 0.003(3) 0.000(3) -0.005(3) N4 0.027(3) 0.031(3) 0.019(2) 0.001(2) 0.002(2) 0.002(2) C28 0.028(3) 0.019(3) 0.031(4) -0.002(3) 0.004(3) 0.007(3) N5 0.028(3) 0.026(3) 0.021(2) 0.002(2) 0.003(2) 0.005(2) N6 0.031(3) 0.030(3) 0.023(3) -0.001(2) 0.000(2) 0.000(3) C29 0.035(4) 0.036(4) 0.022(3) 0.004(3) 0.006(3) -0.004(3) C30 0.041(4) 0.040(4) 0.022(3) -0.002(3) 0.010(3) 0.000(4) C31 0.031(3) 0.030(4) 0.034(3) -0.002(3) 0.007(3) 0.008(3) C32 0.068(5) 0.043(5) 0.068(5) 0.003(5) 0.011(4) 0.012(4) C33 0.046(5) 0.052(5) 0.081(6) -0.004(6) 0.009(5) 0.003(4) N7 0.083(6) 0.086(6) 0.077(6) 0.001(5) -0.008(5) 0.001(5) B1 0.071(7) 0.045(6) 0.035(5) 0.005(4) 0.021(5) 0.018(5) F11 0.070(3) 0.039(3) 0.051(2) 0.002(2) 0.000(2) 0.013(2) F12 0.077(8) 0.038(6) 0.114(11) 0.013(8) 0.047(9) -0.011(6) F13 0.042(7) 0.039(6) 0.049(8) 0.003(6) 0.002(6) 0.007(5) F14 0.112(9) 0.055(7) 0.029(5) 0.005(4) 0.000(5) 0.031(6) B1' 0.071(7) 0.045(6) 0.035(5) 0.005(4) 0.021(5) 0.018(5) F11' 0.070(3) 0.039(3) 0.051(2) 0.002(2) 0.000(2) 0.013(2) F12' 0.036(5) 0.050(7) 0.078(8) -0.011(6) 0.021(6) 0.005(5) F13' 0.043(7) 0.110(15) 0.084(13) -0.040(10) -0.040(7) 0.042(8) F14' 0.141(11) 0.055(7) 0.048(6) 0.006(5) 0.028(7) 0.011(7) B2 0.036(5) 0.051(6) 0.038(5) 0.010(4) 0.000(4) -0.006(4) F21 0.039(2) 0.103(4) 0.062(3) 0.019(3) -0.001(2) -0.013(3) F22 0.052(3) 0.086(4) 0.054(3) 0.031(3) -0.007(2) -0.021(3) F23 0.055(3) 0.094(4) 0.038(2) 0.014(2) 0.009(2) 0.000(3) F24 0.129(5) 0.057(4) 0.066(3) -0.001(3) 0.013(3) -0.024(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 Cu1 O1 1.921(4) . y Cu1 O2 1.930(4) . y Cu1 N1 1.939(5) . y Cu1 N5 1.943(5) . y Cu1 Cu2 3.2463(12) . y Cu2 O2 1.933(4) . y Cu2 O3 1.938(4) . y Cu2 N2 1.950(5) . y Cu2 N6 1.960(5) . y O1 C1 1.303(7) . ? C1 C7 1.425(8) . ? C1 C2 1.427(8) . ? C2 C3 1.390(8) . ? C2 C28 1.432(8) . ? C3 C4 1.381(9) . ? C4 C6 1.378(9) . ? C4 C5 1.520(9) . ? C6 C7 1.400(9) . ? C7 C8 1.427(8) . ? C8 N1 1.285(8) . ? N1 C9 1.484(8) . ? C9 C10 1.462(11) . ? C10 C11 1.469(10) . ? C11 C12 1.408(11) . ? C11 O2 1.438(7) . ? C12 C13 1.479(10) . ? C13 N2 1.489(7) . ? N2 C14 1.283(8) . ? C14 C15 1.440(8) . ? C15 C16 1.402(9) . ? C15 C21 1.415(8) . ? C16 C17 1.381(9) . ? C17 C19 1.381(9) . ? C17 C18 1.516(9) . ? C19 C20 1.409(8) . ? C20 C21 1.424(8) . ? C20 C22 1.432(8) . ? C21 O3 1.312(7) . ? C22 N3 1.278(8) . ? N3 C23 1.463(7) . ? C23 C24 1.511(8) . ? C24 C25 1.512(8) . ? C25 O4 1.446(7) . ? C25 C26 1.506(9) . ? C26 C27 1.530(9) . ? C27 N4 1.459(7) . ? N4 C28 1.287(7) . ? N5 C31 1.352(7) . ? N5 N6 1.361(6) . ? N6 C29 1.338(7) . ? C29 C30 1.378(8) . ? C30 C31 1.386(8) . ? C32 C33 1.453(11) . ? C33 N7 1.123(10) . ? B1 F12 1.306(12) . ? B1 F11 1.364(8) . ? B1 F13 1.391(12) . ? B1 F14 1.459(10) . ? B2 F23 1.367(8) . ? B2 F21 1.373(8) . ? B2 F22 1.379(8) . ? B2 F24 1.399(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 158.83(17) . . y O1 Cu1 N1 93.2(2) . . y O2 Cu1 N1 97.7(2) . . y O1 Cu1 N5 87.61(18) . . y O2 Cu1 N5 85.54(19) . . y N1 Cu1 N5 167.7(2) . . y O2 Cu2 O3 158.37(18) . . y O2 Cu2 N2 97.58(19) . . y O3 Cu2 N2 93.39(19) . . y O2 Cu2 N6 85.32(19) . . y O3 Cu2 N6 88.15(18) . . y N2 Cu2 N6 167.1(2) . . y C1 O1 Cu1 128.6(4) . . ? O1 C1 C7 123.1(6) . . ? O1 C1 C2 119.6(5) . . ? C7 C1 C2 117.3(6) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 C28 117.8(6) . . ? C1 C2 C28 121.8(6) . . ? C4 C3 C2 122.5(6) . . ? C6 C4 C3 117.2(6) . . ? C6 C4 C5 122.0(6) . . ? C3 C4 C5 120.7(6) . . ? C4 C6 C7 123.5(6) . . ? C6 C7 C1 119.1(6) . . ? C6 C7 C8 118.3(5) . . ? C1 C7 C8 122.7(6) . . ? N1 C8 C7 127.6(6) . . ? C8 N1 C9 117.2(6) . . ? C8 N1 Cu1 124.7(4) . . ? C9 N1 Cu1 118.1(5) . . ? C10 C9 N1 113.3(7) . . ? C9 C10 C11 117.0(7) . . ? C12 C11 O2 113.1(7) . . ? C12 C11 C10 119.2(7) . . ? O2 C11 C10 112.1(6) . . ? C11 O2 Cu1 123.6(4) . . ? C11 O2 Cu2 122.0(4) . . ? Cu1 O2 Cu2 114.36(18) . . ? C11 C12 C13 121.4(8) . . ? C12 C13 N2 115.6(6) . . ? C14 N2 C13 116.1(5) . . ? C14 N2 Cu2 124.2(4) . . ? C13 N2 Cu2 119.6(4) . . ? N2 C14 C15 128.2(6) . . ? C16 C15 C21 119.5(6) . . ? C16 C15 C14 118.0(6) . . ? C21 C15 C14 122.5(6) . . ? C17 C16 C15 123.9(6) . . ? C19 C17 C16 116.6(6) . . ? C19 C17 C18 121.9(6) . . ? C16 C17 C18 121.5(6) . . ? C17 C19 C20 122.5(6) . . ? C19 C20 C21 120.3(6) . . ? C19 C20 C22 117.2(5) . . ? C21 C20 C22 122.6(6) . . ? O3 C21 C15 123.7(5) . . ? O3 C21 C20 119.0(5) . . ? C15 C21 C20 117.2(6) . . ? C21 O3 Cu2 127.9(3) . . ? N3 C22 C20 126.1(6) . . ? C22 N3 C23 124.0(5) . . ? N3 C23 C24 114.2(5) . . ? C23 C24 C25 114.5(5) . . ? O4 C25 C26 108.1(5) . . ? O4 C25 C24 108.8(5) . . ? C26 C25 C24 112.7(5) . . ? C25 C26 C27 114.3(5) . . ? N4 C27 C26 114.6(5) . . ? C28 N4 C27 123.7(5) . . ? N4 C28 C2 126.1(6) . . ? C31 N5 N6 107.6(5) . . ? C31 N5 Cu1 133.0(4) . . ? N6 N5 Cu1 119.5(4) . . ? C29 N6 N5 108.3(5) . . ? C29 N6 Cu2 133.4(5) . . ? N5 N6 Cu2 118.3(4) . . ? N6 C29 C30 110.0(6) . . ? C29 C30 C31 104.7(5) . . ? N5 C31 C30 109.5(6) . . ? N7 C33 C32 179.0(10) . . ? F12 B1 F11 123.4(9) . . ? F12 B1 F13 111.1(10) . . ? F11 B1 F13 102.1(8) . . ? F12 B1 F14 109.7(9) . . ? F11 B1 F14 105.7(7) . . ? F13 B1 F14 102.8(9) . . ? F23 B2 F21 111.3(6) . . ? F23 B2 F22 110.3(6) . . ? F21 B2 F22 109.3(6) . . ? F23 B2 F24 107.3(6) . . ? F21 B2 F24 110.3(6) . . ? F22 B2 F24 108.3(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.845 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.095 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 B2 Cu4 F8 N8 O4' _chemical_formula_weight 1050.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4460(10) _cell_length_b 25.567(3) _cell_length_c 9.0340(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.23(1) _cell_angle_gamma 90.00 _cell_volume 1939.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 5 _cell_measurement_theta_max 11 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.253 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3444 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1313 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3233 _reflns_number_gt 1789 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Disorder in part of the saturated section of the macrocyclic ring was modelled as a 60:40 distribution between two conformations (C10', C11'). ; _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^)+(0.0400P)^2^+2.3192P] 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 3233 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.29820(12) 0.53715(4) 0.08590(12) 0.0285(3) Uani 1 1 d . . . Cu2 Cu 0.35983(12) 0.42141(4) -0.04650(12) 0.0301(3) Uani 1 1 d . . . C1 C 0.2443(10) 0.6547(4) 0.2045(9) 0.033(2) Uani 1 1 d . . . C2 C 0.1903(11) 0.7053(4) 0.2257(10) 0.040(3) Uani 1 1 d . . . H2 H 0.1025 0.7102 0.2817 0.048 Uiso 1 1 calc R . . C3 C 0.2604(12) 0.7488(4) 0.1679(11) 0.043(3) Uani 1 1 d . . . C4 C 0.1935(13) 0.8031(4) 0.1874(13) 0.068(4) Uani 1 1 d . . . H4A H 0.2080 0.8126 0.2931 0.103 Uiso 1 1 calc R . . H4B H 0.0797 0.8034 0.1517 0.103 Uiso 1 1 calc R . . H4C H 0.2495 0.8283 0.1301 0.103 Uiso 1 1 calc R . . C5 C 0.3931(11) 0.7416(4) 0.0933(11) 0.041(2) Uani 1 1 d . . . H5 H 0.4446 0.7712 0.0562 0.049 Uiso 1 1 calc R . . C6 C 0.4533(10) 0.6908(3) 0.0712(9) 0.027(2) Uani 1 1 d . . . C7 C 0.3791(10) 0.6471(3) 0.1276(9) 0.027(2) Uani 1 1 d . . . O1 O 0.4320(6) 0.5993(2) 0.1079(6) 0.0296(14) Uani 1 1 d . . . C8 C 0.1647(10) 0.6114(4) 0.2712(10) 0.035(2) Uani 1 1 d . . . H8 H 0.0968 0.6204 0.3445 0.042 Uiso 1 1 calc R A . N1 N 0.1761(8) 0.5625(3) 0.2419(8) 0.0319(19) Uani 1 1 d . A . C9 C 0.0853(12) 0.5249(4) 0.3218(11) 0.050(3) Uani 0.60 1 d P A 1 H9A H 0.1541 0.5125 0.4105 0.060 Uiso 0.60 1 calc PR A 1 H9B H -0.0063 0.5434 0.3576 0.060 Uiso 0.60 1 calc PR A 1 C10 C 0.0262(16) 0.4802(6) 0.2364(15) 0.027(4) Uani 0.60 1 d P A 1 H10A H -0.0321 0.4923 0.1416 0.032 Uiso 0.60 1 calc PR A 1 H10B H -0.0501 0.4611 0.2923 0.032 Uiso 0.60 1 calc PR A 1 C11 C 0.1614(18) 0.4419(7) 0.2009(18) 0.028(3) Uiso 0.60 1 d P A 1 H11 H 0.2399 0.4361 0.2905 0.033 Uiso 0.60 1 calc PR A 1 O2 O 0.2383(6) 0.4647(2) 0.0782(6) 0.0303(14) Uani 0.60 1 d P A 1 C9' C 0.0853(12) 0.5249(4) 0.3218(11) 0.050(3) Uani 0.40 1 d P A 2 H9A' H 0.1093 0.5317 0.4298 0.060 Uiso 0.40 1 calc PR A 2 H9B' H -0.0294 0.5322 0.2953 0.060 Uiso 0.40 1 calc PR A 2 C10' C 0.112(3) 0.4699(10) 0.296(3) 0.040(6) Uiso 0.40 1 d P A 2 H10C H 0.0287 0.4515 0.3455 0.048 Uiso 0.40 1 calc PR A 2 H10D H 0.2141 0.4617 0.3565 0.048 Uiso 0.40 1 calc PR A 2 C11' C 0.119(3) 0.4424(10) 0.157(3) 0.028(3) Uiso 0.40 1 d P A 2 H11' H 0.0218 0.4568 0.0977 0.033 Uiso 0.40 1 calc PR A 2 O2' O 0.2383(6) 0.4647(2) 0.0782(6) 0.0303(14) Uani 0.40 1 d P A 2 C12 C 0.0907(14) 0.3893(4) 0.1387(14) 0.072(4) Uani 1 1 d . . . H12A H 0.0013 0.3792 0.1951 0.086 Uiso 1 1 calc R A 1 H12B H 0.0473 0.3942 0.0334 0.086 Uiso 1 1 calc R A 1 C13 C 0.2087(13) 0.3465(4) 0.1478(15) 0.077(4) Uani 1 1 d . A . H13A H 0.1527 0.3131 0.1232 0.093 Uiso 1 1 calc R . . H13B H 0.2599 0.3440 0.2514 0.093 Uiso 1 1 calc R . . N2 N 0.3348(8) 0.3537(3) 0.0458(8) 0.035(2) Uani 1 1 d . . . C14 C 0.4121(10) 0.3138(4) 0.0174(10) 0.040(3) Uani 1 1 d . . . H14 H 0.3787 0.2821 0.0593 0.048 Uiso 1 1 calc R . . C15 C 0.3703(9) 0.5660(4) -0.2231(10) 0.034(2) Uani 1 1 d . . . H15 H 0.3657 0.6028 -0.2098 0.041 Uiso 1 1 calc R A . C16 C 0.3924(10) 0.5410(4) -0.3537(9) 0.038(2) Uani 1 1 d . A . H16 H 0.4048 0.5566 -0.4471 0.045 Uiso 1 1 calc R . . C17 C 0.3926(10) 0.4876(4) -0.3198(9) 0.034(2) Uani 1 1 d . . . H17 H 0.4070 0.4600 -0.3874 0.040 Uiso 1 1 calc R A . N3 N 0.3562(7) 0.5298(3) -0.1167(7) 0.0255(16) Uani 1 1 d . A . N4 N 0.3691(8) 0.4819(3) -0.1758(8) 0.0297(18) Uani 1 1 d . A . B1 B 0.2386(14) 0.3469(5) -0.3979(14) 0.044(3) Uani 1 1 d . A . F11 F 0.2173(11) 0.2959(3) -0.3706(12) 0.139(4) Uani 1 1 d . . . F12 F 0.1202(8) 0.3633(4) -0.5001(7) 0.107(3) Uani 1 1 d . . . F13 F 0.3838(7) 0.3547(3) -0.4475(7) 0.087(2) Uani 1 1 d . . . F14 F 0.2260(7) 0.3739(2) -0.2698(6) 0.0601(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 Cu1 0.0280(6) 0.0247(6) 0.0353(6) -0.0004(5) 0.0148(5) 0.0023(5) Cu2 0.0293(6) 0.0237(6) 0.0398(7) 0.0012(6) 0.0145(5) -0.0003(5) C1 0.029(5) 0.035(6) 0.032(5) -0.019(5) -0.007(4) -0.001(5) C2 0.039(6) 0.035(6) 0.048(6) -0.012(5) 0.004(5) 0.017(5) C3 0.049(6) 0.024(6) 0.054(7) -0.005(5) -0.009(5) 0.016(5) C4 0.055(7) 0.041(7) 0.107(10) -0.030(7) -0.004(7) 0.021(6) C5 0.034(6) 0.023(6) 0.063(7) 0.003(5) -0.005(5) 0.002(4) C6 0.039(5) 0.013(5) 0.026(5) -0.004(4) -0.008(4) 0.000(4) C7 0.026(5) 0.022(5) 0.032(5) -0.005(4) 0.000(4) 0.005(4) O1 0.030(3) 0.021(3) 0.040(4) -0.007(3) 0.015(3) -0.002(3) C8 0.023(5) 0.041(6) 0.042(6) -0.014(5) 0.005(4) 0.009(5) N1 0.028(4) 0.031(5) 0.040(5) -0.001(4) 0.016(3) 0.007(3) C9 0.053(6) 0.059(8) 0.045(6) -0.007(6) 0.035(5) -0.015(6) C10 0.012(7) 0.057(12) 0.011(7) 0.008(7) 0.001(6) -0.005(7) O2 0.031(3) 0.026(4) 0.038(3) -0.004(3) 0.021(3) -0.001(3) C9' 0.053(6) 0.059(8) 0.045(6) -0.007(6) 0.035(5) -0.015(6) O2' 0.031(3) 0.026(4) 0.038(3) -0.004(3) 0.021(3) -0.001(3) C12 0.091(9) 0.030(7) 0.108(10) -0.007(6) 0.070(8) -0.030(6) C13 0.062(8) 0.048(8) 0.134(12) 0.032(8) 0.063(8) 0.010(6) N2 0.035(5) 0.014(4) 0.061(6) 0.003(4) 0.024(4) 0.000(3) C14 0.037(6) 0.037(7) 0.048(6) 0.002(5) 0.009(5) -0.010(5) C15 0.029(5) 0.035(6) 0.039(6) 0.011(5) 0.004(4) -0.001(4) C16 0.036(5) 0.053(7) 0.025(5) 0.012(5) 0.002(4) -0.001(5) C17 0.034(5) 0.042(7) 0.027(5) -0.002(5) 0.012(4) -0.002(5) N3 0.022(4) 0.019(4) 0.036(4) -0.001(3) 0.007(3) -0.001(3) N4 0.025(4) 0.029(5) 0.035(4) -0.001(3) 0.004(3) 0.004(3) B1 0.034(7) 0.042(8) 0.056(8) -0.018(7) 0.002(6) -0.004(6) F11 0.153(8) 0.041(5) 0.236(11) -0.036(6) 0.080(8) -0.013(5) F12 0.056(4) 0.213(10) 0.052(4) -0.028(5) 0.004(4) 0.040(5) F13 0.044(4) 0.132(7) 0.087(5) -0.022(5) 0.018(4) 0.005(4) F14 0.060(4) 0.065(4) 0.055(4) -0.022(3) 0.006(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.918(6) . y Cu1 N1 1.945(7) . y Cu1 O1 1.949(5) . y Cu1 N3 1.954(6) . y Cu1 Cu2 3.1329(14) 3_665 y Cu1 Cu2 3.2545(16) . y Cu2 N2 1.942(7) . y Cu2 N4 1.945(7) . y Cu2 O2 1.950(5) . y Cu2 O1 1.973(5) 3_665 y Cu2 F14 2.515(6) . ? C1 C2 1.391(11) . ? C1 C7 1.410(11) . ? C1 C8 1.459(12) . ? C2 C3 1.389(13) . ? C3 C5 1.381(12) . ? C3 C4 1.515(12) . ? C5 C6 1.417(11) . ? C6 C7 1.404(11) . ? C6 C14 1.465(11) 3_665 ? C7 O1 1.319(9) . ? O1 Cu2 1.973(5) 3_665 ? C8 N1 1.285(11) . ? N1 C9 1.467(10) . ? C9 C10 1.439(16) . ? C10 C11 1.56(2) . ? C11 O2 1.466(16) . ? C11 C12 1.551(19) . ? C10' C11' 1.45(3) . ? C11' C12 1.39(3) . ? C12 C13 1.476(14) . ? C13 N2 1.494(11) . ? N2 C14 1.253(11) . ? C14 C6 1.465(11) 3_665 ? C15 N3 1.348(10) . ? C15 C16 1.372(11) . ? C16 C17 1.398(12) . ? C17 N4 1.346(10) . ? N3 N4 1.345(8) . ? B1 F11 1.341(14) . ? B1 F12 1.352(13) . ? B1 F14 1.363(12) . ? B1 F13 1.366(12) . ? 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 O2 Cu1 N1 100.9(3) . . y O2 Cu1 O1 159.9(2) . . y N1 Cu1 O1 90.1(3) . . y O2 Cu1 N3 88.0(2) . . y N1 Cu1 N3 156.4(3) . . y O1 Cu1 N3 88.4(3) . . y N2 Cu2 N4 168.4(3) . . y N2 Cu2 O2 99.8(3) . . y N4 Cu2 O2 87.3(3) . . y N2 Cu2 O1 91.3(3) . 3_665 y N4 Cu2 O1 87.1(3) . 3_665 y O2 Cu2 O1 148.9(2) . 3_665 y N2 Cu2 F14 81.6(3) . . ? N4 Cu2 F14 86.9(3) . . ? O2 Cu2 F14 121.3(2) . . ? O1 Cu2 F14 88.9(2) 3_665 . ? N2 Cu2 Cu1 128.5(2) . . ? N4 Cu2 Cu1 61.0(2) . . ? O2 Cu2 Cu1 32.41(16) . . ? O1 Cu2 Cu1 122.06(16) 3_665 . ? F14 Cu2 Cu1 131.13(15) . . ? C2 C1 C7 119.4(9) . . ? C2 C1 C8 118.4(8) . . ? C7 C1 C8 122.2(8) . . ? C3 C2 C1 122.2(9) . . ? C5 C3 C2 118.6(9) . . ? C5 C3 C4 120.7(10) . . ? C2 C3 C4 120.7(9) . . ? C3 C5 C6 120.8(9) . . ? C7 C6 C5 119.9(8) . . ? C7 C6 C14 122.6(8) . 3_665 ? C5 C6 C14 117.5(8) . 3_665 ? O1 C7 C6 121.1(7) . . ? O1 C7 C1 119.8(8) . . ? C6 C7 C1 119.0(8) . . ? C7 O1 Cu1 124.6(5) . . ? C7 O1 Cu2 127.8(5) . 3_665 ? Cu1 O1 Cu2 106.1(3) . 3_665 ? N1 C8 C1 127.2(8) . . ? C8 N1 C9 118.7(8) . . ? C8 N1 Cu1 122.1(6) . . ? C9 N1 Cu1 119.1(6) . . ? C10 C9 N1 115.2(8) . . ? C9 C10 C11 113.0(11) . . ? O2 C11 C12 104.9(11) . . ? O2 C11 C10 107.4(11) . . ? C12 C11 C10 110.9(12) . . ? C11 O2 Cu1 119.6(7) . . ? C11 O2 Cu2 121.0(7) . . ? Cu1 O2 Cu2 114.6(2) . . ? C12 C11' C10' 124(2) . . ? C11' C12 C13 127.8(14) . . ? C11' C12 C11 18.8(13) . . ? C13 C12 C11 113.0(12) . . ? C12 C13 N2 113.3(9) . . ? C14 N2 C13 116.5(8) . . ? C14 N2 Cu2 123.7(6) . . ? C13 N2 Cu2 119.5(6) . . ? N2 C14 C6 129.0(9) . 3_665 ? N3 C15 C16 108.9(8) . . ? C15 C16 C17 105.3(8) . . ? N4 C17 C16 108.7(8) . . ? N4 N3 C15 108.9(7) . . ? N4 N3 Cu1 119.9(5) . . ? C15 N3 Cu1 130.7(6) . . ? N3 N4 C17 108.2(7) . . ? N3 N4 Cu2 118.4(5) . . ? C17 N4 Cu2 133.4(6) . . ? F11 B1 F12 108.9(10) . . ? F11 B1 F14 108.2(11) . . ? F12 B1 F14 107.6(9) . . ? F11 B1 F13 110.2(10) . . ? F12 B1 F13 110.8(10) . . ? F14 B1 F13 111.1(9) . . ? B1 F14 Cu2 148.9(6) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.627 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.121