data_acl4p2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H58 Cu2 N6, 2(C32 H12 B F24)' _chemical_formula_sum 'C98 H82 B2 Cu2 F48 N6' _chemical_formula_weight 2404.40 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P 21/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 13.073(5) _cell_length_b 27.978(12) _cell_length_c 13.464(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.633(7) _cell_angle_gamma 90.00 _cell_volume 4891(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'platte' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69618 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.97 _reflns_number_total 11668 _reflns_number_gt 9205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. ; _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^)+(0.0374P)^2^+9.2015P] 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 11668 _refine_ls_number_parameters 749 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2021(3) 0.02070(12) -0.0059(3) 0.0206(8) Uani 0.821(4) 1 d P A 1 C2 C -0.1672(3) 0.02566(13) 0.0954(3) 0.0246(8) Uani 0.821(4) 1 d P A 1 H2A H -0.1687 0.0558 0.1275 0.030 Uiso 0.821(4) 1 calc PR A 1 C4 C -0.1243(3) -0.05774(13) 0.1048(3) 0.0210(8) Uani 0.821(4) 1 d P A 1 H4A H -0.0975 -0.0841 0.1440 0.025 Uiso 0.821(4) 1 calc PR A 1 C5 C -0.1572(3) -0.06341(12) 0.0037(3) 0.0205(8) Uani 0.821(4) 1 d P . 1 C6 C -0.1970(3) -0.02348(13) -0.0504(3) 0.0213(8) Uani 0.821(4) 1 d P A 1 H6A H -0.2211 -0.0269 -0.1194 0.026 Uiso 0.821(4) 1 calc PR A 1 C5' C -0.0083(11) 0.0426(5) 0.1776(10) 0.014(3) Uani 0.179(4) 1 d PU . 2 C4' C -0.1125(11) 0.0318(5) 0.1442(11) 0.012(3) Uani 0.179(4) 1 d PU A 2 H4'A H -0.1628 0.0552 0.1223 0.014 Uiso 0.179(4) 1 calc PR A 2 C6' C -0.0599(12) -0.0048(5) -0.1932(10) 0.015(3) Uani 0.179(4) 1 d PU . 2 H6'A H -0.1304 -0.0116 -0.2133 0.017 Uiso 0.179(4) 1 calc PR A 2 C1' C -0.0304(12) 0.0428(6) -0.1808(12) 0.021(4) Uani 0.179(4) 1 d PU . 2 C2' C -0.0729(13) -0.0515(5) 0.1502(12) 0.018(3) Uani 0.179(4) 1 d PU . 2 H2'A H -0.0990 -0.0825 0.1330 0.022 Uiso 0.179(4) 1 calc PR A 2 C3 C -0.1311(2) -0.01373(11) 0.1471(2) 0.0279(7) Uani 1 1 d . . . H3A H -0.1093 -0.0104 0.2165 0.033 Uiso 0.821(4) 1 calc PR A 1 H3B H -0.2021 -0.0210 0.1467 0.033 Uiso 0.179(4) 1 d PR A 2 Cu1 Cu -0.07187(3) 0.121120(12) 0.00635(3) 0.01780(9) Uani 1 1 d . . . N1 N -0.17324(19) 0.09633(9) -0.10510(19) 0.0229(5) Uani 1 1 d . A . N2 N -0.15957(19) 0.18010(8) 0.06223(18) 0.0208(5) Uani 1 1 d . A . N3 N 0.0607(2) 0.12362(9) 0.0965(2) 0.0255(5) Uani 1 1 d . A . C7 C -0.2487(2) 0.06226(11) -0.0670(3) 0.0313(7) Uani 1 1 d . . . H7D H -0.2937 0.0494 -0.1250 0.038 Uiso 0.821(4) 1 calc PR A 1 H7E H -0.2929 0.0805 -0.0256 0.038 Uiso 0.821(4) 1 calc PR A 1 H7A H -0.2970 0.0508 -0.1231 0.047 Uiso 0.179(4) 1 calc PR A 2 H7B H -0.2868 0.0787 -0.0186 0.047 Uiso 0.179(4) 1 calc PR A 2 H7C H -0.2114 0.0350 -0.0345 0.047 Uiso 0.179(4) 1 calc PR A 2 C8 C -0.1222(3) 0.07203(13) -0.1830(3) 0.0361(8) Uani 1 1 d . . . H8A H -0.1744 0.0605 -0.2356 0.054 Uiso 0.821(4) 1 calc PR A 1 H8B H -0.0822 0.0449 -0.1534 0.054 Uiso 0.821(4) 1 calc PR A 1 H8C H -0.0762 0.0945 -0.2117 0.054 Uiso 0.821(4) 1 calc PR A 1 H8D H -0.1771 0.0517 -0.2178 0.043 Uiso 0.179(4) 1 calc PR A 2 H8E H -0.1109 0.0979 -0.2307 0.043 Uiso 0.179(4) 1 calc PR A 2 C9 C -0.2337(2) 0.13669(11) -0.1567(2) 0.0238(6) Uani 1 1 d . . . H9A H -0.2852 0.1229 -0.2086 0.029 Uiso 1 1 calc R A . H9B H -0.1861 0.1564 -0.1915 0.029 Uiso 1 1 calc R . . C10 C -0.2895(2) 0.16921(11) -0.0912(2) 0.0265(6) Uani 1 1 d . A . H10A H -0.3287 0.1491 -0.0483 0.032 Uiso 1 1 calc R . . H10B H -0.3399 0.1885 -0.1347 0.032 Uiso 1 1 calc R . . C11 C -0.2216(2) 0.20286(11) -0.0246(2) 0.0272(7) Uani 1 1 d . . . H11A H -0.1740 0.2191 -0.0658 0.033 Uiso 1 1 calc R A . H11B H -0.2657 0.2278 0.0008 0.033 Uiso 1 1 calc R . . C12 C -0.2280(2) 0.16334(11) 0.1345(2) 0.0279(7) Uani 1 1 d . . . H12A H -0.2659 0.1906 0.1579 0.042 Uiso 1 1 calc R A . H12B H -0.1868 0.1483 0.1915 0.042 Uiso 1 1 calc R . . H12C H -0.2768 0.1400 0.1021 0.042 Uiso 1 1 calc R . . C13 C -0.0889(2) 0.21698(11) 0.1103(3) 0.0286(7) Uani 1 1 d . . . H13A H -0.1297 0.2399 0.1455 0.034 Uiso 1 1 calc R A . H13B H -0.0586 0.2348 0.0573 0.034 Uiso 1 1 calc R . . C14 C -0.0025(3) 0.19815(11) 0.1837(2) 0.0275(7) Uani 1 1 d . A . H14A H -0.0316 0.1755 0.2294 0.033 Uiso 1 1 calc R . . H14B H 0.0279 0.2252 0.2245 0.033 Uiso 1 1 calc R . . C15 C 0.0830(2) 0.17297(11) 0.1361(2) 0.0273(7) Uani 1 1 d . . . H15A H 0.1015 0.1931 0.0804 0.033 Uiso 1 1 calc R A . H15C H 0.1444 0.1713 0.1865 0.033 Uiso 1 1 calc R . . C17 C 0.1563(3) 0.11111(12) 0.0467(3) 0.0351(8) Uani 1 1 d . . . H17D H 0.1656 0.1361 -0.0036 0.042 Uiso 0.821(4) 1 calc PR A 1 H17E H 0.2168 0.1127 0.0982 0.042 Uiso 0.821(4) 1 calc PR A 1 H17A H 0.2174 0.1131 0.0961 0.053 Uiso 0.179(4) 1 calc PR A 2 H17B H 0.1632 0.1336 -0.0079 0.053 Uiso 0.179(4) 1 calc PR A 2 H17C H 0.1498 0.0785 0.0199 0.053 Uiso 0.179(4) 1 calc PR A 2 C16 C 0.0536(3) 0.09127(12) 0.1814(3) 0.0400(9) Uani 1 1 d . . . H16A H 0.1183 0.0922 0.2261 0.060 Uiso 0.821(4) 1 calc PR A 1 H16B H 0.0410 0.0586 0.1566 0.060 Uiso 0.821(4) 1 calc PR A 1 H16C H -0.0032 0.1014 0.2180 0.060 Uiso 0.821(4) 1 calc PR A 1 H16D H 0.0264 0.1108 0.2337 0.048 Uiso 0.179(4) 1 calc PR A 2 H16E H 0.1254 0.0831 0.2073 0.048 Uiso 0.179(4) 1 calc PR A 2 C1S C 0.2460(2) 0.11850(9) 0.6724(2) 0.0166(5) Uani 1 1 d . . . F1S F -0.03068(17) 0.11424(8) 0.42108(16) 0.0460(6) Uani 1 1 d . . . B1S B 0.3715(2) 0.11051(11) 0.6916(2) 0.0160(6) Uani 1 1 d . . . C2S C 0.1824(2) 0.09551(10) 0.5943(2) 0.0176(5) Uani 1 1 d . . . H2SA H 0.2117 0.0716 0.5562 0.021 Uiso 1 1 calc R . . F2S F -0.06048(17) 0.05643(9) 0.51634(18) 0.0534(6) Uani 1 1 d . . . C3S C 0.0792(2) 0.10660(10) 0.5717(2) 0.0210(6) Uani 1 1 d . . . F3S F 0.06893(16) 0.05363(9) 0.43355(18) 0.0526(6) Uani 1 1 d . . . F4S F -0.05340(13) 0.20840(7) 0.73791(14) 0.0297(4) Uani 1 1 d . . . C4S C 0.0319(2) 0.14090(10) 0.6252(2) 0.0223(6) Uani 1 1 d . . . H4SA H -0.0389 0.1486 0.6092 0.027 Uiso 1 1 calc R . . F5S F 0.05794(18) 0.19030(8) 0.86134(14) 0.0455(6) Uani 1 1 d . . . C5S C 0.0916(2) 0.16341(10) 0.7024(2) 0.0203(6) Uani 1 1 d . . . F6S F 0.09355(15) 0.24348(7) 0.75606(17) 0.0396(5) Uani 1 1 d . . . C6S C 0.1958(2) 0.15243(9) 0.7251(2) 0.0173(5) Uani 1 1 d . . . H6SA H 0.2343 0.1688 0.7788 0.021 Uiso 1 1 calc R . . F7S F 0.43074(17) 0.08687(7) 1.15005(13) 0.0384(5) Uani 1 1 d . . . C7S C 0.0149(2) 0.08265(12) 0.4863(2) 0.0286(7) Uani 1 1 d . . . F8S F 0.42690(19) 0.03028(7) 1.04209(15) 0.0449(5) Uani 1 1 d . . . C8S C 0.0474(2) 0.20108(11) 0.7630(2) 0.0252(6) Uani 1 1 d . . . C9S C 0.4115(2) 0.12680(10) 0.8063(2) 0.0165(5) Uani 1 1 d . . . F9S F 0.56889(16) 0.06463(8) 1.09136(16) 0.0448(5) Uani 1 1 d . . . F10S F 0.44275(17) 0.25341(7) 1.04659(14) 0.0400(5) Uani 1 1 d . . . C10S C 0.4263(2) 0.09411(10) 0.8850(2) 0.0171(5) Uani 1 1 d . . . H10C H 0.4211 0.0609 0.8706 0.021 Uiso 1 1 calc R . . F11S F 0.54742(15) 0.25939(7) 0.93486(18) 0.0413(5) Uani 1 1 d . . . C11S C 0.4485(2) 0.10880(11) 0.9840(2) 0.0207(6) Uani 1 1 d . . . F12S F 0.38621(15) 0.26883(6) 0.89464(14) 0.0311(4) Uani 1 1 d . . . C12S C 0.4570(2) 0.15717(11) 1.0082(2) 0.0210(6) Uani 1 1 d . . . H12D H 0.4715 0.1672 1.0758 0.025 Uiso 1 1 calc R . . F13S F 0.70133(13) 0.02959(6) 0.59983(16) 0.0332(4) Uani 1 1 d . . . C13S C 0.4439(2) 0.19012(10) 0.9317(2) 0.0193(6) Uani 1 1 d . . . F14S F 0.66402(13) -0.04277(7) 0.55775(13) 0.0293(4) Uani 1 1 d . . . C14S C 0.4229(2) 0.17501(10) 0.8328(2) 0.0190(6) Uani 1 1 d . . . H14C H 0.4161 0.1984 0.7813 0.023 Uiso 1 1 calc R . . F15S F 0.70838(14) -0.02519(7) 0.71061(13) 0.0324(4) Uani 1 1 d . . . C15S C 0.4673(2) 0.07293(11) 1.0661(2) 0.0258(6) Uani 1 1 d . . . F16S F 0.21617(15) -0.06362(7) 0.69023(17) 0.0392(5) Uani 1 1 d . . . C16S C 0.4548(2) 0.24256(11) 0.9529(2) 0.0249(6) Uani 1 1 d . . . F17S F 0.28476(16) -0.09186(7) 0.56676(14) 0.0372(5) Uani 1 1 d . . . C17S C 0.4065(2) 0.05488(9) 0.67451(19) 0.0145(5) Uani 1 1 d . . . C18S C 0.5086(2) 0.04515(10) 0.65682(19) 0.0169(5) Uani 1 1 d . . . H18A H 0.5556 0.0710 0.6557 0.020 Uiso 1 1 calc R . . F18S F 0.34802(17) -0.10971(7) 0.71417(17) 0.0451(6) Uani 1 1 d . . . F19S F 0.69765(13) 0.22180(6) 0.66920(14) 0.0297(4) Uani 1 1 d . . . C19S C 0.5428(2) -0.00068(10) 0.6410(2) 0.0172(5) Uani 1 1 d . . . F20S F 0.71207(15) 0.23118(8) 0.51431(16) 0.0447(6) Uani 1 1 d . . . C20S C 0.4768(2) -0.03950(10) 0.64028(19) 0.0177(5) Uani 1 1 d . . . H20A H 0.4997 -0.0708 0.6270 0.021 Uiso 1 1 calc R . . F21S F 0.75267(14) 0.16411(7) 0.58713(16) 0.0381(5) Uani 1 1 d . . . C21S C 0.3770(2) -0.03123(10) 0.6594(2) 0.0182(5) Uani 1 1 d . . . F22S F 0.32205(14) 0.13309(6) 0.30462(13) 0.0286(4) Uani 1 1 d . . . C22S C 0.3428(2) 0.01481(10) 0.6777(2) 0.0176(5) Uani 1 1 d . . . H22A H 0.2742 0.0191 0.6927 0.021 Uiso 1 1 calc R . . F23S F 0.30060(19) 0.20772(7) 0.32619(15) 0.0489(6) Uani 1 1 d . . . C23S C 0.6530(2) -0.00926(10) 0.6262(2) 0.0191(6) Uani 1 1 d . . . F24S F 0.43411(17) 0.18263(8) 0.26466(14) 0.0460(6) Uani 1 1 d . . . C24S C 0.3062(2) -0.07332(11) 0.6577(2) 0.0234(6) Uani 1 1 d . . . C25S C 0.4249(2) 0.14294(9) 0.6094(2) 0.0160(5) Uani 1 1 d . . . C26S C 0.5249(2) 0.16123(9) 0.6280(2) 0.0157(5) Uani 1 1 d . . . H26A H 0.5595 0.1590 0.6939 0.019 Uiso 1 1 calc R . . C27S C 0.5757(2) 0.18245(10) 0.5544(2) 0.0183(5) Uani 1 1 d . . . C28S C 0.5283(2) 0.18617(10) 0.4570(2) 0.0194(6) Uani 1 1 d . . . H28A H 0.5634 0.1997 0.4058 0.023 Uiso 1 1 calc R . . C29S C 0.4281(2) 0.16955(9) 0.4367(2) 0.0182(5) Uani 1 1 d . . . C30S C 0.3779(2) 0.14882(9) 0.5111(2) 0.0181(5) Uani 1 1 d . . . H30A H 0.3090 0.1382 0.4948 0.022 Uiso 1 1 calc R . . C31S C 0.6842(2) 0.19971(11) 0.5803(2) 0.0237(6) Uani 1 1 d . . . C32S C 0.3721(2) 0.17331(10) 0.3336(2) 0.0238(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0169(17) 0.0206(17) 0.0239(18) 0.0027(14) 0.0009(13) -0.0009(13) C2 0.0225(19) 0.0234(18) 0.028(2) -0.0015(15) 0.0040(16) 0.0008(14) C4 0.0173(18) 0.0202(17) 0.0263(19) 0.0058(15) 0.0054(16) 0.0024(13) C5 0.0140(16) 0.0213(17) 0.0261(18) -0.0006(14) 0.0022(13) 0.0001(12) C6 0.0200(17) 0.0237(18) 0.0195(17) 0.0035(14) -0.0005(13) 0.0017(13) C5' 0.022(6) 0.011(6) 0.009(6) 0.000(5) -0.004(5) 0.003(5) C4' 0.012(3) 0.012(3) 0.012(3) -0.0004(10) 0.0019(11) 0.0007(10) C6' 0.024(6) 0.015(6) 0.005(5) -0.003(5) 0.005(5) -0.007(5) C1' 0.020(6) 0.023(7) 0.019(6) 0.006(5) -0.003(5) -0.003(5) C2' 0.022(7) 0.015(6) 0.017(6) 0.003(5) -0.002(6) -0.007(5) C3 0.0261(16) 0.0305(17) 0.0287(16) 0.0049(13) 0.0099(13) -0.0009(12) Cu1 0.01800(17) 0.01749(17) 0.01734(17) 0.00098(13) -0.00043(13) -0.00106(13) N1 0.0234(13) 0.0196(12) 0.0245(13) 0.0012(10) -0.0018(10) 0.0015(10) N2 0.0228(12) 0.0186(12) 0.0214(12) -0.0005(10) 0.0037(10) 0.0005(9) N3 0.0247(13) 0.0215(13) 0.0282(14) -0.0030(10) -0.0062(11) 0.0017(10) C7 0.0269(16) 0.0202(15) 0.0432(19) 0.0069(14) -0.0122(14) -0.0060(12) C8 0.0279(17) 0.041(2) 0.0363(19) -0.0166(15) -0.0090(14) 0.0099(14) C9 0.0196(14) 0.0268(15) 0.0240(15) 0.0063(12) -0.0012(12) 0.0003(11) C10 0.0229(15) 0.0250(15) 0.0303(16) 0.0049(13) -0.0027(12) 0.0043(12) C11 0.0277(16) 0.0221(15) 0.0307(17) 0.0015(13) -0.0017(13) 0.0061(12) C12 0.0306(16) 0.0255(16) 0.0285(16) -0.0032(13) 0.0076(13) -0.0011(12) C13 0.0301(17) 0.0198(15) 0.0357(18) -0.0054(13) 0.0026(14) -0.0014(12) C14 0.0354(17) 0.0215(15) 0.0246(15) -0.0078(12) -0.0006(13) -0.0037(12) C15 0.0261(16) 0.0260(16) 0.0277(16) -0.0057(13) -0.0065(13) -0.0039(12) C17 0.0234(16) 0.0325(18) 0.046(2) -0.0097(15) -0.0117(14) 0.0021(13) C16 0.055(2) 0.0224(16) 0.0365(19) 0.0051(14) -0.0201(17) -0.0055(15) C1S 0.0200(13) 0.0155(13) 0.0143(12) 0.0039(10) 0.0027(10) -0.0011(10) F1S 0.0502(13) 0.0435(12) 0.0380(12) 0.0009(10) -0.0223(10) 0.0002(10) B1S 0.0156(14) 0.0162(14) 0.0154(14) -0.0025(11) -0.0019(11) 0.0010(11) C2S 0.0170(13) 0.0178(13) 0.0187(13) 0.0010(10) 0.0044(10) 0.0016(10) F2S 0.0406(13) 0.0614(15) 0.0560(15) -0.0014(12) -0.0041(11) -0.0290(11) C3S 0.0228(14) 0.0192(14) 0.0208(14) 0.0009(11) 0.0018(11) -0.0011(11) F3S 0.0370(12) 0.0627(15) 0.0533(14) -0.0361(12) -0.0152(10) 0.0095(11) F4S 0.0220(9) 0.0320(10) 0.0365(10) 0.0039(8) 0.0096(8) 0.0108(7) C4S 0.0171(14) 0.0237(15) 0.0254(15) 0.0070(12) -0.0001(11) 0.0016(11) F5S 0.0625(14) 0.0534(13) 0.0213(10) 0.0024(9) 0.0078(9) 0.0338(11) C5S 0.0197(14) 0.0202(14) 0.0222(14) 0.0066(11) 0.0070(11) 0.0031(11) F6S 0.0323(11) 0.0269(10) 0.0622(14) -0.0125(9) 0.0164(10) 0.0007(8) C6S 0.0214(14) 0.0160(13) 0.0143(12) 0.0013(10) 0.0016(10) 0.0000(10) F7S 0.0543(13) 0.0448(12) 0.0178(9) 0.0055(8) 0.0108(9) 0.0079(10) C7S 0.0207(15) 0.0301(17) 0.0335(17) -0.0028(14) -0.0035(13) 0.0000(12) F8S 0.0741(16) 0.0339(11) 0.0251(10) 0.0080(8) -0.0016(10) -0.0127(10) C8S 0.0256(15) 0.0277(16) 0.0230(15) 0.0042(12) 0.0056(12) 0.0074(12) C9S 0.0139(12) 0.0189(13) 0.0165(13) -0.0008(10) 0.0006(10) -0.0003(10) F9S 0.0371(12) 0.0599(14) 0.0362(11) 0.0183(10) -0.0006(9) 0.0146(10) F10S 0.0624(14) 0.0312(11) 0.0257(10) -0.0115(8) 0.0019(9) 0.0021(10) C10S 0.0177(13) 0.0191(13) 0.0148(12) -0.0007(10) 0.0029(10) -0.0004(10) F11S 0.0261(10) 0.0267(10) 0.0722(15) -0.0105(10) 0.0095(10) -0.0064(8) C11S 0.0172(13) 0.0285(15) 0.0164(13) 0.0032(11) 0.0021(11) 0.0019(11) F12S 0.0368(11) 0.0222(9) 0.0335(10) -0.0039(8) 0.0002(8) 0.0054(8) C12S 0.0189(14) 0.0268(15) 0.0172(13) -0.0039(11) 0.0007(11) -0.0001(11) F13S 0.0219(9) 0.0239(9) 0.0559(13) 0.0057(9) 0.0132(9) 0.0004(7) C13S 0.0174(13) 0.0220(14) 0.0193(14) -0.0057(11) 0.0048(11) -0.0007(10) F14S 0.0246(9) 0.0349(10) 0.0289(10) -0.0147(8) 0.0046(7) 0.0047(7) C14S 0.0174(13) 0.0222(14) 0.0170(13) 0.0025(11) 0.0002(10) 0.0003(10) F15S 0.0255(9) 0.0468(12) 0.0228(9) 0.0018(8) -0.0058(7) 0.0100(8) C15S 0.0300(16) 0.0268(16) 0.0204(15) -0.0003(12) 0.0021(12) -0.0010(12) F16S 0.0313(10) 0.0317(11) 0.0581(14) -0.0145(9) 0.0206(9) -0.0130(8) C16S 0.0274(16) 0.0263(16) 0.0214(15) -0.0088(12) 0.0041(12) 0.0003(12) F17S 0.0483(12) 0.0344(11) 0.0293(10) -0.0125(8) 0.0067(9) -0.0184(9) C17S 0.0169(13) 0.0167(12) 0.0096(11) 0.0007(10) -0.0002(9) -0.0003(10) C18S 0.0182(13) 0.0178(13) 0.0142(12) -0.0012(10) 0.0004(10) -0.0013(10) F18S 0.0426(12) 0.0318(11) 0.0574(14) 0.0214(10) -0.0092(10) -0.0122(9) F19S 0.0241(9) 0.0306(10) 0.0339(10) -0.0092(8) 0.0018(8) -0.0060(7) C19S 0.0178(13) 0.0203(14) 0.0128(12) 0.0018(10) -0.0015(10) 0.0026(10) F20S 0.0293(11) 0.0659(15) 0.0383(12) 0.0204(11) 0.0011(9) -0.0186(10) C20S 0.0243(14) 0.0146(13) 0.0136(12) -0.0011(10) -0.0004(10) 0.0025(10) F21S 0.0191(9) 0.0419(12) 0.0515(13) -0.0152(10) -0.0040(8) 0.0097(8) C21S 0.0210(14) 0.0187(13) 0.0140(12) 0.0013(10) -0.0020(10) -0.0028(10) F22S 0.0376(10) 0.0255(9) 0.0205(9) 0.0005(7) -0.0056(8) -0.0100(8) C22S 0.0182(13) 0.0209(14) 0.0138(12) 0.0013(10) 0.0021(10) -0.0003(10) F23S 0.0746(16) 0.0353(11) 0.0297(11) -0.0080(9) -0.0251(10) 0.0268(11) C23S 0.0192(14) 0.0192(13) 0.0182(13) -0.0004(11) -0.0004(11) 0.0037(10) F24S 0.0566(14) 0.0661(15) 0.0145(9) 0.0035(9) 0.0008(9) -0.0314(11) C24S 0.0259(15) 0.0206(14) 0.0238(15) -0.0002(12) 0.0034(12) -0.0019(11) C25S 0.0166(13) 0.0126(12) 0.0186(13) -0.0029(10) 0.0016(10) 0.0029(10) C26S 0.0173(13) 0.0148(12) 0.0144(12) 0.0010(10) -0.0008(10) 0.0034(10) C27S 0.0179(13) 0.0158(13) 0.0212(14) 0.0010(11) 0.0021(11) 0.0023(10) C28S 0.0216(14) 0.0182(13) 0.0191(14) 0.0012(11) 0.0048(11) 0.0002(10) C29S 0.0263(14) 0.0134(12) 0.0141(13) -0.0004(10) -0.0010(11) 0.0001(10) C30S 0.0190(13) 0.0140(12) 0.0203(14) -0.0005(10) -0.0023(11) -0.0002(10) C31S 0.0209(14) 0.0258(15) 0.0249(15) 0.0035(12) 0.0050(12) -0.0003(11) C32S 0.0348(17) 0.0193(14) 0.0163(14) 0.0018(11) -0.0016(12) -0.0041(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.378(5) . ? C1 C2 1.394(5) . ? C1 C7 1.511(4) . ? C2 C3 1.359(5) . ? C4 C3 1.363(5) . ? C4 C5 1.389(5) . ? C5 C6 1.401(5) . ? C5 C17 1.498(5) 3 ? C5' C6' 1.38(2) 3 ? C5' C4' 1.42(2) . ? C5' C16 1.581(15) . ? C4' C3 1.299(14) . ? C6' C5' 1.38(2) 3 ? C6' C1' 1.39(2) . ? C1' C2' 1.39(2) 3 ? C1' C8 1.451(17) . ? C2' C3 1.300(16) . ? C2' C1' 1.39(2) 3 ? Cu1 N3 1.999(3) . ? Cu1 N1 2.007(3) . ? Cu1 N2 2.192(2) . ? N1 C8 1.472(4) . ? N1 C9 1.502(4) . ? N1 C7 1.504(4) . ? N2 C12 1.472(4) . ? N2 C13 1.483(4) . ? N2 C11 1.487(4) . ? N3 C16 1.469(4) . ? N3 C15 1.497(4) . ? N3 C17 1.526(4) . ? C9 C10 1.512(4) . ? C10 C11 1.515(4) . ? C13 C14 1.507(5) . ? C14 C15 1.524(4) . ? C17 C5 1.498(5) 3 ? C1S C6S 1.393(4) . ? C1S C2S 1.417(4) . ? C1S B1S 1.646(4) . ? F1S C7S 1.336(4) . ? B1S C9S 1.637(4) . ? B1S C17S 1.646(4) . ? B1S C25S 1.647(4) . ? C2S C3S 1.383(4) . ? F2S C7S 1.329(4) . ? C3S C4S 1.387(4) . ? C3S C7S 1.502(4) . ? F3S C7S 1.333(4) . ? F4S C8S 1.338(4) . ? C4S C5S 1.378(4) . ? F5S C8S 1.350(4) . ? C5S C6S 1.396(4) . ? C5S C8S 1.489(4) . ? F6S C8S 1.339(4) . ? F7S C15S 1.335(4) . ? F8S C15S 1.330(4) . ? C9S C10S 1.396(4) . ? C9S C14S 1.399(4) . ? F9S C15S 1.352(4) . ? F10S C16S 1.324(3) . ? C10S C11S 1.393(4) . ? F11S C16S 1.347(4) . ? C11S C12S 1.394(4) . ? C11S C15S 1.493(4) . ? F12S C16S 1.341(4) . ? C12S C13S 1.378(4) . ? F13S C23S 1.326(3) . ? C13S C14S 1.395(4) . ? C13S C16S 1.498(4) . ? F14S C23S 1.334(3) . ? F15S C23S 1.351(3) . ? F16S C24S 1.330(3) . ? F17S C24S 1.330(3) . ? C17S C22S 1.400(4) . ? C17S C18S 1.410(4) . ? C18S C19S 1.382(4) . ? F18S C24S 1.348(4) . ? F19S C31S 1.340(4) . ? C19S C20S 1.387(4) . ? C19S C23S 1.496(4) . ? F20S C31S 1.331(4) . ? C20S C21S 1.379(4) . ? F21S C31S 1.335(3) . ? C21S C22S 1.394(4) . ? C21S C24S 1.496(4) . ? F22S C32S 1.337(3) . ? F23S C32S 1.338(4) . ? F24S C32S 1.327(4) . ? C25S C26S 1.399(4) . ? C25S C30S 1.404(4) . ? C26S C27S 1.389(4) . ? C27S C28S 1.389(4) . ? C27S C31S 1.500(4) . ? C28S C29S 1.387(4) . ? C29S C30S 1.386(4) . ? C29S C32S 1.497(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.2(3) . . ? C6 C1 C7 119.4(3) . . ? C2 C1 C7 121.4(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C4 C5 119.0(3) . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C17 121.9(3) . 3 ? C6 C5 C17 119.8(3) . 3 ? C1 C6 C5 121.5(3) . . ? C6' C5' C4' 117.6(13) 3 . ? C6' C5' C16 109.6(11) 3 . ? C4' C5' C16 131.5(11) . . ? C3 C4' C5' 112.1(12) . . ? C5' C6' C1' 123.3(14) 3 . ? C2' C1' C6' 116.8(15) 3 . ? C2' C1' C8 133.0(14) 3 . ? C6' C1' C8 108.6(12) . . ? C3 C2' C1' 114.4(13) . 3 ? C4' C3 C2' 133.4(10) . . ? C2' C3 C2 147.5(7) . . ? C4' C3 C4 148.5(7) . . ? C2 C3 C4 123.7(3) . . ? N3 Cu1 N1 156.52(10) . . ? N3 Cu1 N2 102.50(10) . . ? N1 Cu1 N2 100.98(10) . . ? C8 N1 C9 106.0(2) . . ? C8 N1 C7 108.6(3) . . ? C9 N1 C7 107.7(2) . . ? C8 N1 Cu1 112.19(19) . . ? C9 N1 Cu1 110.68(18) . . ? C7 N1 Cu1 111.49(19) . . ? C12 N2 C13 109.2(2) . . ? C12 N2 C11 109.8(2) . . ? C13 N2 C11 107.5(2) . . ? C12 N2 Cu1 111.65(18) . . ? C13 N2 Cu1 110.44(18) . . ? C11 N2 Cu1 108.17(18) . . ? C16 N3 C15 108.5(3) . . ? C16 N3 C17 109.2(3) . . ? C15 N3 C17 103.4(2) . . ? C16 N3 Cu1 108.8(2) . . ? C15 N3 Cu1 111.63(18) . . ? C17 N3 Cu1 114.97(19) . . ? N1 C7 C1 115.8(3) . . ? C1' C8 N1 133.5(7) . . ? N1 C9 C10 116.5(2) . . ? C9 C10 C11 115.5(3) . . ? N2 C11 C10 115.4(2) . . ? N2 C13 C14 115.1(3) . . ? C13 C14 C15 114.6(3) . . ? N3 C15 C14 117.0(3) . . ? C5 C17 N3 116.9(3) 3 . ? N3 C16 C5' 125.7(6) . . ? C6S C1S C2S 114.6(2) . . ? C6S C1S B1S 122.1(2) . . ? C2S C1S B1S 122.9(2) . . ? C9S B1S C1S 108.3(2) . . ? C9S B1S C17S 109.4(2) . . ? C1S B1S C17S 113.2(2) . . ? C9S B1S C25S 111.5(2) . . ? C1S B1S C25S 108.2(2) . . ? C17S B1S C25S 106.3(2) . . ? C3S C2S C1S 122.4(3) . . ? C2S C3S C4S 121.6(3) . . ? C2S C3S C7S 120.9(3) . . ? C4S C3S C7S 117.5(3) . . ? C5S C4S C3S 117.3(3) . . ? C4S C5S C6S 121.2(3) . . ? C4S C5S C8S 121.0(3) . . ? C6S C5S C8S 117.8(3) . . ? C1S C6S C5S 122.9(3) . . ? F2S C7S F3S 106.4(3) . . ? F2S C7S F1S 106.0(3) . . ? F3S C7S F1S 106.1(3) . . ? F2S C7S C3S 112.5(3) . . ? F3S C7S C3S 113.3(3) . . ? F1S C7S C3S 112.1(3) . . ? F4S C8S F6S 106.6(2) . . ? F4S C8S F5S 105.5(2) . . ? F6S C8S F5S 105.7(3) . . ? F4S C8S C5S 113.8(3) . . ? F6S C8S C5S 112.5(2) . . ? F5S C8S C5S 112.2(2) . . ? C10S C9S C14S 115.9(2) . . ? C10S C9S B1S 122.3(2) . . ? C14S C9S B1S 121.4(2) . . ? C11S C10S C9S 121.9(3) . . ? C10S C11S C12S 120.8(3) . . ? C10S C11S C15S 120.6(3) . . ? C12S C11S C15S 118.5(3) . . ? C13S C12S C11S 118.4(3) . . ? C12S C13S C14S 120.3(3) . . ? C12S C13S C16S 120.8(3) . . ? C14S C13S C16S 118.8(3) . . ? C13S C14S C9S 122.6(3) . . ? F8S C15S F7S 107.3(3) . . ? F8S C15S F9S 105.0(3) . . ? F7S C15S F9S 106.0(2) . . ? F8S C15S C11S 113.3(3) . . ? F7S C15S C11S 112.7(3) . . ? F9S C15S C11S 112.0(3) . . ? F10S C16S F12S 106.6(2) . . ? F10S C16S F11S 107.5(2) . . ? F12S C16S F11S 104.9(3) . . ? F10S C16S C13S 112.7(3) . . ? F12S C16S C13S 112.5(2) . . ? F11S C16S C13S 112.1(2) . . ? C22S C17S C18S 115.4(2) . . ? C22S C17S B1S 125.3(2) . . ? C18S C17S B1S 119.3(2) . . ? C19S C18S C17S 122.3(3) . . ? C18S C19S C20S 121.0(3) . . ? C18S C19S C23S 120.2(2) . . ? C20S C19S C23S 118.8(2) . . ? C21S C20S C19S 118.0(3) . . ? C20S C21S C22S 121.1(3) . . ? C20S C21S C24S 117.5(3) . . ? C22S C21S C24S 121.3(3) . . ? C21S C22S C17S 122.1(3) . . ? F13S C23S F14S 107.3(2) . . ? F13S C23S F15S 105.7(2) . . ? F14S C23S F15S 105.0(2) . . ? F13S C23S C19S 113.6(2) . . ? F14S C23S C19S 112.8(2) . . ? F15S C23S C19S 111.8(2) . . ? F17S C24S F16S 106.4(2) . . ? F17S C24S F18S 104.7(2) . . ? F16S C24S F18S 106.6(2) . . ? F17S C24S C21S 112.7(2) . . ? F16S C24S C21S 113.8(2) . . ? F18S C24S C21S 112.1(2) . . ? C26S C25S C30S 115.1(2) . . ? C26S C25S B1S 122.8(2) . . ? C30S C25S B1S 121.7(2) . . ? C27S C26S C25S 122.9(3) . . ? C26S C27S C28S 120.5(3) . . ? C26S C27S C31S 119.3(3) . . ? C28S C27S C31S 120.1(3) . . ? C29S C28S C27S 118.0(3) . . ? C30S C29S C28S 120.9(3) . . ? C30S C29S C32S 118.5(3) . . ? C28S C29S C32S 120.6(3) . . ? C29S C30S C25S 122.6(3) . . ? F20S C31S F21S 107.8(2) . . ? F20S C31S F19S 105.9(2) . . ? F21S C31S F19S 105.3(2) . . ? F20S C31S C27S 112.5(2) . . ? F21S C31S C27S 112.6(2) . . ? F19S C31S C27S 112.3(2) . . ? F24S C32S F22S 106.2(2) . . ? F24S C32S F23S 106.5(3) . . ? F22S C32S F23S 105.6(3) . . ? F24S C32S C29S 112.9(3) . . ? F22S C32S C29S 112.5(2) . . ? F23S C32S C29S 112.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.2(5) . . . . ? C7 C1 C2 C3 176.7(3) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C3 C4 C5 C17 -177.3(3) . . . 3 ? C2 C1 C6 C5 -0.3(5) . . . . ? C7 C1 C6 C5 -178.2(3) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? C17 C5 C6 C1 178.0(3) 3 . . . ? C6' C5' C4' C3 9.4(18) 3 . . . ? C16 C5' C4' C3 175.2(11) . . . . ? C5' C6' C1' C2' -1(2) 3 . . 3 ? C5' C6' C1' C8 -168.5(12) 3 . . . ? C5' C4' C3 C2' -19.6(19) . . . . ? C5' C4' C3 C2 -152.6(16) . . . . ? C5' C4' C3 C4 -77.8(18) . . . . ? C1' C2' C3 C4' 19(2) 3 . . . ? C1' C2' C3 C2 82(2) 3 . . . ? C1' C2' C3 C4 153(2) 3 . . . ? C1 C2 C3 C4' 144.6(10) . . . . ? C1 C2 C3 C2' 46.3(16) . . . . ? C1 C2 C3 C4 1.9(5) . . . . ? C5 C4 C3 C4' -50.4(15) . . . . ? C5 C4 C3 C2' -143.4(12) . . . . ? C5 C4 C3 C2 -1.0(5) . . . . ? N3 Cu1 N1 C8 -26.5(4) . . . . ? N2 Cu1 N1 C8 154.2(2) . . . . ? N3 Cu1 N1 C9 -144.6(3) . . . . ? N2 Cu1 N1 C9 36.0(2) . . . . ? N3 Cu1 N1 C7 95.5(3) . . . . ? N2 Cu1 N1 C7 -83.8(2) . . . . ? N3 Cu1 N2 C12 -95.1(2) . . . . ? N1 Cu1 N2 C12 84.6(2) . . . . ? N3 Cu1 N2 C13 26.6(2) . . . . ? N1 Cu1 N2 C13 -153.7(2) . . . . ? N3 Cu1 N2 C11 144.02(19) . . . . ? N1 Cu1 N2 C11 -36.3(2) . . . . ? N1 Cu1 N3 C16 -86.5(3) . . . . ? N2 Cu1 N3 C16 92.8(2) . . . . ? N1 Cu1 N3 C15 153.7(2) . . . . ? N2 Cu1 N3 C15 -27.0(2) . . . . ? N1 Cu1 N3 C17 36.3(4) . . . . ? N2 Cu1 N3 C17 -144.4(2) . . . . ? C8 N1 C7 C1 69.9(4) . . . . ? C9 N1 C7 C1 -175.8(3) . . . . ? Cu1 N1 C7 C1 -54.2(3) . . . . ? C6 C1 C7 N1 -100.3(4) . . . . ? C2 C1 C7 N1 81.8(4) . . . . ? C2' C1' C8 N1 -61(2) 3 . . . ? C6' C1' C8 N1 103.9(12) . . . . ? C9 N1 C8 C1' 155.4(9) . . . . ? C7 N1 C8 C1' -89.2(10) . . . . ? Cu1 N1 C8 C1' 34.5(10) . . . . ? C8 N1 C9 C10 -176.9(3) . . . . ? C7 N1 C9 C10 67.1(3) . . . . ? Cu1 N1 C9 C10 -55.0(3) . . . . ? N1 C9 C10 C11 72.7(3) . . . . ? C12 N2 C11 C10 -68.5(3) . . . . ? C13 N2 C11 C10 172.8(3) . . . . ? Cu1 N2 C11 C10 53.5(3) . . . . ? C9 C10 C11 N2 -73.0(4) . . . . ? C12 N2 C13 C14 75.2(3) . . . . ? C11 N2 C13 C14 -165.7(3) . . . . ? Cu1 N2 C13 C14 -47.9(3) . . . . ? N2 C13 C14 C15 73.7(4) . . . . ? C16 N3 C15 C14 -69.1(3) . . . . ? C17 N3 C15 C14 175.0(3) . . . . ? Cu1 N3 C15 C14 50.9(3) . . . . ? C13 C14 C15 N3 -75.6(4) . . . . ? C16 N3 C17 C5 66.1(4) . . . 3 ? C15 N3 C17 C5 -178.5(3) . . . 3 ? Cu1 N3 C17 C5 -56.5(4) . . . 3 ? C15 N3 C16 C5' 155.0(7) . . . . ? C17 N3 C16 C5' -92.9(8) . . . . ? Cu1 N3 C16 C5' 33.3(8) . . . . ? C6' C5' C16 N3 112.7(10) 3 . . . ? C4' C5' C16 N3 -53.9(17) . . . . ? C6S C1S B1S C9S 26.6(3) . . . . ? C2S C1S B1S C9S -160.6(2) . . . . ? C6S C1S B1S C17S 148.0(2) . . . . ? C2S C1S B1S C17S -39.1(3) . . . . ? C6S C1S B1S C25S -94.4(3) . . . . ? C2S C1S B1S C25S 78.5(3) . . . . ? C6S C1S C2S C3S 1.0(4) . . . . ? B1S C1S C2S C3S -172.4(3) . . . . ? C1S C2S C3S C4S -0.5(4) . . . . ? C1S C2S C3S C7S 178.0(3) . . . . ? C2S C3S C4S C5S -0.4(4) . . . . ? C7S C3S C4S C5S -178.9(3) . . . . ? C3S C4S C5S C6S 0.7(4) . . . . ? C3S C4S C5S C8S 179.3(3) . . . . ? C2S C1S C6S C5S -0.7(4) . . . . ? B1S C1S C6S C5S 172.7(2) . . . . ? C4S C5S C6S C1S -0.1(4) . . . . ? C8S C5S C6S C1S -178.8(3) . . . . ? C2S C3S C7S F2S 116.3(3) . . . . ? C4S C3S C7S F2S -65.2(4) . . . . ? C2S C3S C7S F3S -4.5(4) . . . . ? C4S C3S C7S F3S 174.0(3) . . . . ? C2S C3S C7S F1S -124.4(3) . . . . ? C4S C3S C7S F1S 54.1(4) . . . . ? C4S C5S C8S F4S 3.0(4) . . . . ? C6S C5S C8S F4S -178.4(2) . . . . ? C4S C5S C8S F6S -118.3(3) . . . . ? C6S C5S C8S F6S 60.3(3) . . . . ? C4S C5S C8S F5S 122.7(3) . . . . ? C6S C5S C8S F5S -58.7(4) . . . . ? C1S B1S C9S C10S 96.3(3) . . . . ? C17S B1S C9S C10S -27.5(3) . . . . ? C25S B1S C9S C10S -144.8(2) . . . . ? C1S B1S C9S C14S -77.1(3) . . . . ? C17S B1S C9S C14S 159.0(2) . . . . ? C25S B1S C9S C14S 41.8(3) . . . . ? C14S C9S C10S C11S 1.6(4) . . . . ? B1S C9S C10S C11S -172.2(2) . . . . ? C9S C10S C11S C12S -0.1(4) . . . . ? C9S C10S C11S C15S -178.0(3) . . . . ? C10S C11S C12S C13S -0.6(4) . . . . ? C15S C11S C12S C13S 177.3(3) . . . . ? C11S C12S C13S C14S -0.1(4) . . . . ? C11S C12S C13S C16S -178.4(3) . . . . ? C12S C13S C14S C9S 1.7(4) . . . . ? C16S C13S C14S C9S -180.0(3) . . . . ? C10S C9S C14S C13S -2.4(4) . . . . ? B1S C9S C14S C13S 171.5(2) . . . . ? C10S C11S C15S F8S -22.2(4) . . . . ? C12S C11S C15S F8S 160.0(3) . . . . ? C10S C11S C15S F7S -144.2(3) . . . . ? C12S C11S C15S F7S 37.9(4) . . . . ? C10S C11S C15S F9S 96.4(3) . . . . ? C12S C11S C15S F9S -81.5(3) . . . . ? C12S C13S C16S F10S -21.3(4) . . . . ? C14S C13S C16S F10S 160.4(3) . . . . ? C12S C13S C16S F12S -142.0(3) . . . . ? C14S C13S C16S F12S 39.7(4) . . . . ? C12S C13S C16S F11S 100.1(3) . . . . ? C14S C13S C16S F11S -78.2(3) . . . . ? C9S B1S C17S C22S 99.7(3) . . . . ? C1S B1S C17S C22S -21.2(4) . . . . ? C25S B1S C17S C22S -139.9(3) . . . . ? C9S B1S C17S C18S -79.1(3) . . . . ? C1S B1S C17S C18S 160.0(2) . . . . ? C25S B1S C17S C18S 41.3(3) . . . . ? C22S C17S C18S C19S 1.7(4) . . . . ? B1S C17S C18S C19S -179.4(2) . . . . ? C17S C18S C19S C20S 1.1(4) . . . . ? C17S C18S C19S C23S -177.8(2) . . . . ? C18S C19S C20S C21S -2.3(4) . . . . ? C23S C19S C20S C21S 176.6(2) . . . . ? C19S C20S C21S C22S 0.8(4) . . . . ? C19S C20S C21S C24S 179.6(2) . . . . ? C20S C21S C22S C17S 2.0(4) . . . . ? C24S C21S C22S C17S -176.7(2) . . . . ? C18S C17S C22S C21S -3.2(4) . . . . ? B1S C17S C22S C21S 178.0(2) . . . . ? C18S C19S C23S F13S -19.4(4) . . . . ? C20S C19S C23S F13S 161.8(2) . . . . ? C18S C19S C23S F14S -141.8(3) . . . . ? C20S C19S C23S F14S 39.4(3) . . . . ? C18S C19S C23S F15S 100.1(3) . . . . ? C20S C19S C23S F15S -78.8(3) . . . . ? C20S C21S C24S F17S -67.6(3) . . . . ? C22S C21S C24S F17S 111.2(3) . . . . ? C20S C21S C24S F16S 171.2(2) . . . . ? C22S C21S C24S F16S -10.0(4) . . . . ? C20S C21S C24S F18S 50.2(4) . . . . ? C22S C21S C24S F18S -131.1(3) . . . . ? C9S B1S C25S C26S 32.6(3) . . . . ? C1S B1S C25S C26S 151.6(2) . . . . ? C17S B1S C25S C26S -86.5(3) . . . . ? C9S B1S C25S C30S -155.8(2) . . . . ? C1S B1S C25S C30S -36.8(3) . . . . ? C17S B1S C25S C30S 85.1(3) . . . . ? C30S C25S C26S C27S -1.8(4) . . . . ? B1S C25S C26S C27S 170.2(2) . . . . ? C25S C26S C27S C28S -0.4(4) . . . . ? C25S C26S C27S C31S -178.1(3) . . . . ? C26S C27S C28S C29S 2.1(4) . . . . ? C31S C27S C28S C29S 179.8(3) . . . . ? C27S C28S C29S C30S -1.5(4) . . . . ? C27S C28S C29S C32S 178.9(3) . . . . ? C28S C29S C30S C25S -0.8(4) . . . . ? C32S C29S C30S C25S 178.8(3) . . . . ? C26S C25S C30S C29S 2.4(4) . . . . ? B1S C25S C30S C29S -169.8(2) . . . . ? C26S C27S C31S F20S -161.1(3) . . . . ? C28S C27S C31S F20S 21.2(4) . . . . ? C26S C27S C31S F21S 76.8(3) . . . . ? C28S C27S C31S F21S -100.9(3) . . . . ? C26S C27S C31S F19S -41.9(4) . . . . ? C28S C27S C31S F19S 140.4(3) . . . . ? C30S C29S C32S F24S -164.6(3) . . . . ? C28S C29S C32S F24S 15.0(4) . . . . ? C30S C29S C32S F22S -44.4(4) . . . . ? C28S C29S C32S F22S 135.2(3) . . . . ? C30S C29S C32S F23S 74.8(3) . . . . ? C28S C29S C32S F23S -105.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.801 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.105 #===END data_acl7p21g _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H56 Cu2 N6, 2(F6 Sb)' _chemical_formula_sum 'C28 H56 Cu2 F12 N6 Sb2' _chemical_formula_weight 1075.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 16.264(4) _cell_length_b 15.169(4) _cell_length_c 17.642(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.776(4) _cell_angle_gamma 90.00 _cell_volume 4227(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 2.337 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62969 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.34 _reflns_number_total 10415 _reflns_number_gt 8918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker Shelxtl' _computing_publication_material 'Bruker Shelxtl' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The SQUEEZE tool from PLATON (A.L.Spek (2005) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13) has been used to take the contribution of disordered solvents to the structure factors into account. ; _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^)+(0.0363P)^2^+4.3363P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10415 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.478165(11) 0.313766(13) 0.070991(10) 0.03348(6) Uani 1 1 d . . . Cu1 Cu 0.23771(2) 0.17092(2) 0.144721(19) 0.03085(8) Uani 1 1 d . A . F1 F 0.37558(15) 0.3051(2) 0.09966(17) 0.0898(9) Uani 1 1 d . . . N1 N 0.18076(16) 0.17357(18) 0.03164(15) 0.0432(6) Uani 1 1 d . . . C1 C 0.0995(12) 0.1187(18) 0.0087(15) 0.067(8) Uani 0.519(3) 1 d P A 1 H1A H 0.0756 0.1244 -0.0464 0.100 Uiso 0.519(3) 1 calc PR A 1 H1B H 0.0595 0.1395 0.0368 0.100 Uiso 0.519(3) 1 calc PR A 1 H1C H 0.1124 0.0579 0.0212 0.100 Uiso 0.519(3) 1 calc PR A 1 C1B C 0.0990(14) 0.1302(17) 0.0187(15) 0.049(4) Uani 0.481(3) 1 d P A 2 H1BA H 0.0678 0.1415 -0.0345 0.059 Uiso 0.481(3) 1 calc PR A 2 H1BB H 0.0674 0.1562 0.0533 0.059 Uiso 0.481(3) 1 calc PR A 2 Sb2 Sb 0.015722(11) 0.579851(14) 0.189484(10) 0.03678(6) Uani 1 1 d . . . Cu2 Cu 0.273193(19) -0.26660(2) 0.027033(17) 0.02949(8) Uani 1 1 d . A . F2 F 0.58040(15) 0.31567(18) 0.04072(17) 0.0796(8) Uani 1 1 d . . . N2 N 0.19889(16) 0.28768(17) 0.19229(17) 0.0424(6) Uani 1 1 d . . . C2 C 0.2377(2) 0.1325(3) -0.01406(19) 0.0609(10) Uani 1 1 d . A . H2A H 0.2103 0.1337 -0.0686 0.091 Uiso 1 1 calc R . . H2B H 0.2494 0.0726 0.0024 0.091 Uiso 1 1 calc R . . H2C H 0.2898 0.1650 -0.0052 0.091 Uiso 1 1 calc R . . N3 N 0.32287(13) 0.11649(15) 0.23171(13) 0.0303(4) Uani 1 1 d . . . F3 F 0.52574(14) 0.23195(16) 0.14828(12) 0.0649(6) Uani 1 1 d . . . C3 C 0.1648(2) 0.2661(3) 0.0044(2) 0.0609(11) Uani 1 1 d . A . H3A H 0.1300 0.2653 -0.0485 0.073 Uiso 1 1 calc R . . H3B H 0.2185 0.2929 0.0028 0.073 Uiso 1 1 calc R . . F4 F 0.44485(16) 0.21939(19) 0.00165(14) 0.0807(7) Uani 1 1 d . . . N4 N 0.34695(13) -0.27466(15) 0.13328(12) 0.0295(4) Uani 1 1 d . . . C4 C 0.1218(3) 0.3238(3) 0.0537(3) 0.0717(13) Uani 1 1 d . . . H4A H 0.0752 0.2909 0.0656 0.086 Uiso 1 1 calc R A . H4B H 0.0979 0.3747 0.0231 0.086 Uiso 1 1 calc R . . F5 F 0.5105(2) 0.40625(19) 0.13844(18) 0.0968(9) Uani 1 1 d . . . N5 N 0.23305(19) -0.3964(2) -0.00216(17) 0.0527(8) Uani 1 1 d . . . C5 C 0.1790(2) 0.3557(2) 0.1298(2) 0.0573(9) Uani 1 1 d . A . H5A H 0.2316 0.3766 0.1194 0.069 Uiso 1 1 calc R . . H5B H 0.1521 0.4054 0.1487 0.069 Uiso 1 1 calc R . . N6 N 0.2222(2) -0.1975(3) -0.06716(15) 0.0612(9) Uani 1 1 d . . . F6 F 0.4299(2) 0.3909(2) -0.00913(17) 0.0996(10) Uani 1 1 d . . . C6 C 0.1231(3) 0.2711(3) 0.2229(3) 0.0750(14) Uani 1 1 d . A . H6A H 0.1065 0.3248 0.2439 0.112 Uiso 1 1 calc R . . H6B H 0.1361 0.2273 0.2632 0.112 Uiso 1 1 calc R . . H6C H 0.0777 0.2506 0.1813 0.112 Uiso 1 1 calc R . . C7 C 0.2685(2) 0.3207(2) 0.2555(2) 0.0503(8) Uani 1 1 d . A . H7A H 0.2469 0.3677 0.2827 0.060 Uiso 1 1 calc R . . H7B H 0.3118 0.3458 0.2325 0.060 Uiso 1 1 calc R . . F7 F -0.10207(10) 0.59562(13) 0.16110(12) 0.0508(5) Uani 1 1 d . A . C8 C 0.3089(2) 0.2510(2) 0.31454(19) 0.0517(8) Uani 1 1 d . . . H8A H 0.3414 0.2803 0.3609 0.062 Uiso 1 1 calc R A . H8B H 0.2643 0.2178 0.3295 0.062 Uiso 1 1 calc R . . F8 F 0.13433(11) 0.56930(16) 0.21577(13) 0.0633(6) Uani 1 1 d . A . C9 C 0.36648(19) 0.1870(2) 0.28600(17) 0.0415(7) Uani 1 1 d . A . H9A H 0.4024 0.2203 0.2598 0.050 Uiso 1 1 calc R . . H9B H 0.4029 0.1589 0.3311 0.050 Uiso 1 1 calc R . . F9 F 0.0089(5) 0.4871(6) 0.1267(6) 0.108(4) Uani 0.519(3) 1 d P A 1 F10 F 0.0177(3) 0.5312(8) 0.2788(4) 0.141(4) Uani 0.519(3) 1 d P A 1 F11 F 0.0312(3) 0.6941(4) 0.2407(5) 0.097(2) Uani 0.519(3) 1 d P A 1 F12 F 0.0206(4) 0.6544(6) 0.0995(4) 0.097(3) Uani 0.519(3) 1 d P A 1 F9B F 0.0115(6) 0.5192(8) 0.0983(4) 0.080(4) Uani 0.481(3) 1 d P A 2 F10B F -0.0056(4) 0.4655(3) 0.2321(4) 0.0715(15) Uani 0.481(3) 1 d P A 2 F11B F 0.0135(3) 0.6314(5) 0.2842(3) 0.0686(17) Uani 0.481(3) 1 d P A 2 F12B F 0.0291(4) 0.6817(4) 0.1488(6) 0.090(2) Uani 0.481(3) 1 d P A 2 C10 C 0.3897(2) 0.0722(2) 0.2004(2) 0.0464(7) Uani 1 1 d . A . H10A H 0.4307 0.0459 0.2426 0.070 Uiso 1 1 calc R . . H10B H 0.4170 0.1148 0.1745 0.070 Uiso 1 1 calc R . . H10C H 0.3643 0.0273 0.1639 0.070 Uiso 1 1 calc R . . C11 C 0.2811(12) 0.0495(11) 0.2752(10) 0.057(5) Uani 0.519(3) 1 d P A 1 H11A H 0.3222 0.0311 0.3219 0.068 Uiso 0.519(3) 1 calc PR A 1 H11B H 0.2349 0.0782 0.2916 0.068 Uiso 0.519(3) 1 calc PR A 1 C11B C 0.2907(10) 0.0522(8) 0.2786(8) 0.024(3) Uani 0.481(3) 1 d P A 2 H11C H 0.3366 0.0300 0.3188 0.035 Uiso 0.481(3) 1 calc PR A 2 H11D H 0.2645 0.0044 0.2460 0.035 Uiso 0.481(3) 1 calc PR A 2 H11E H 0.2497 0.0798 0.3020 0.035 Uiso 0.481(3) 1 calc PR A 2 C12 C 0.2497(3) -0.0253(3) 0.2316(2) 0.0214(9) Uani 0.519(3) 1 d P A 1 C13 C 0.2933(3) -0.1048(3) 0.2327(2) 0.0221(9) Uani 0.519(3) 1 d P A 1 H13A H 0.3488 -0.1090 0.2621 0.027 Uiso 0.519(3) 1 calc PR A 1 C14 C 0.2554(3) -0.1781(3) 0.1905(2) 0.0204(9) Uani 0.519(3) 1 d P A 1 C15 C 0.1713(3) -0.1709(3) 0.1477(3) 0.0243(9) Uani 0.519(3) 1 d P A 1 H15A H 0.1459 -0.2219 0.1236 0.029 Uiso 0.519(3) 1 calc PR A 1 C17 C 0.1670(3) -0.0195(3) 0.1888(3) 0.0249(9) Uani 0.519(3) 1 d P A 1 H17A H 0.1385 0.0329 0.1925 0.030 Uiso 0.519(3) 1 calc PR A 1 C12B C 0.1038(4) 0.0337(5) 0.0317(4) 0.0418(15) Uani 0.481(3) 1 d P A 2 C13B C 0.1114(4) -0.0277(5) -0.0242(3) 0.0432(16) Uani 0.481(3) 1 d P A 2 H13B H 0.1110 -0.0085 -0.0744 0.052 Uiso 0.481(3) 1 calc PR A 2 C14B C 0.1198(3) -0.1176(5) -0.0074(3) 0.0403(14) Uani 0.481(3) 1 d P A 2 C15B C 0.1166(3) -0.1466(5) 0.0669(3) 0.0395(14) Uani 0.481(3) 1 d P A 2 H15B H 0.1124 -0.2071 0.0736 0.047 Uiso 0.481(3) 1 calc PR A 2 C17B C 0.1002(4) 0.0041(5) 0.1054(4) 0.0423(15) Uani 0.481(3) 1 d P A 2 H17B H 0.0849 0.0452 0.1387 0.051 Uiso 0.481(3) 1 calc PR A 2 C16 C 0.1190(2) -0.0897(2) 0.1371(2) 0.0560(9) Uani 1 1 d . . . H16A H 0.0655 -0.0835 0.1039 0.067 Uiso 0.519(3) 1 calc PR A 1 H16B H 0.1304 -0.1085 0.1905 0.067 Uiso 0.481(3) 1 d PR A 2 C18 C 0.2979(10) -0.2579(10) 0.1948(8) 0.048(5) Uani 0.519(3) 1 d P A 1 H18A H 0.2568 -0.3049 0.1918 0.058 Uiso 0.519(3) 1 calc PR A 1 H18B H 0.3370 -0.2617 0.2457 0.058 Uiso 0.519(3) 1 calc PR A 1 C18B C 0.3013(10) -0.2657(7) 0.1939(9) 0.027(3) Uani 0.481(3) 1 d P A 2 H18C H 0.3402 -0.2699 0.2441 0.040 Uiso 0.481(3) 1 calc PR A 2 H18D H 0.2599 -0.3118 0.1887 0.040 Uiso 0.481(3) 1 calc PR A 2 H18E H 0.2735 -0.2095 0.1892 0.040 Uiso 0.481(3) 1 calc PR A 2 C19 C 0.41429(19) -0.2070(2) 0.14252(18) 0.0428(7) Uani 1 1 d . A . H19A H 0.4505 -0.2108 0.1940 0.064 Uiso 1 1 calc R . . H19B H 0.3890 -0.1495 0.1349 0.064 Uiso 1 1 calc R . . H19C H 0.4470 -0.2168 0.1046 0.064 Uiso 1 1 calc R . . C20 C 0.38941(19) -0.3631(2) 0.1448(2) 0.0453(7) Uani 1 1 d . A . H20A H 0.4193 -0.3684 0.1991 0.054 Uiso 1 1 calc R . . H20B H 0.4314 -0.3650 0.1139 0.054 Uiso 1 1 calc R . . C21 C 0.3313(2) -0.4432(2) 0.1233(2) 0.0589(10) Uani 1 1 d . . . H21A H 0.3622 -0.4953 0.1459 0.071 Uiso 1 1 calc R A . H21B H 0.2836 -0.4362 0.1469 0.071 Uiso 1 1 calc R . . C22 C 0.2977(3) -0.4584(2) 0.0363(3) 0.0688(13) Uani 1 1 d . A . H22A H 0.3447 -0.4554 0.0114 0.083 Uiso 1 1 calc R . . H22B H 0.2745 -0.5175 0.0285 0.083 Uiso 1 1 calc R . . C23 C 0.1524(3) -0.4127(3) 0.0211(2) 0.0734(14) Uani 1 1 d . A . H23A H 0.1339 -0.4720 0.0078 0.110 Uiso 1 1 calc R . . H23B H 0.1101 -0.3721 -0.0058 0.110 Uiso 1 1 calc R . . H23C H 0.1611 -0.4044 0.0764 0.110 Uiso 1 1 calc R . . C24 C 0.2098(9) -0.3989(9) -0.0950(7) 0.043(3) Uani 0.519(3) 1 d P A 1 H24A H 0.2622 -0.4045 -0.1117 0.052 Uiso 0.519(3) 1 calc PR A 1 H24B H 0.1772 -0.4520 -0.1113 0.052 Uiso 0.519(3) 1 calc PR A 1 C25 C 0.1604(7) -0.3213(7) -0.1391(6) 0.047(3) Uani 0.519(3) 1 d P A 1 H25A H 0.1355 -0.3383 -0.1927 0.057 Uiso 0.519(3) 1 calc PR A 1 H25B H 0.1150 -0.3048 -0.1149 0.057 Uiso 0.519(3) 1 calc PR A 1 C24B C 0.2335(11) -0.4252(12) -0.0763(9) 0.069(5) Uani 0.481(3) 1 d P A 2 H24C H 0.2119 -0.4850 -0.0843 0.083 Uiso 0.481(3) 1 calc PR A 2 H24D H 0.2906 -0.4242 -0.0841 0.083 Uiso 0.481(3) 1 calc PR A 2 C25B C 0.1777(9) -0.3631(10) -0.1317(7) 0.061(4) Uani 0.481(3) 1 d P A 2 H25C H 0.1235 -0.3608 -0.1177 0.073 Uiso 0.481(3) 1 calc PR A 2 H25D H 0.1675 -0.3887 -0.1834 0.073 Uiso 0.481(3) 1 calc PR A 2 C26 C 0.2121(2) -0.2531(4) -0.13801(18) 0.0750(15) Uani 1 1 d . A . H26A H 0.1903 -0.2169 -0.1837 0.090 Uiso 0.519(3) 1 calc PR A 1 H26B H 0.2672 -0.2750 -0.1412 0.090 Uiso 0.519(3) 1 calc PR A 1 H26C H 0.2661 -0.2556 -0.1511 0.090 Uiso 0.481(3) 1 d PR A 2 H26D H 0.1737 -0.2234 -0.1800 0.090 Uiso 0.481(3) 1 d PR A 2 C27 C 0.1530(6) -0.1376(6) -0.0579(4) 0.055(2) Uani 0.519(3) 1 d P A 1 H27A H 0.1315 -0.1062 -0.1058 0.083 Uiso 0.519(3) 1 calc PR A 1 H27B H 0.1744 -0.0964 -0.0167 0.083 Uiso 0.519(3) 1 calc PR A 1 H27C H 0.1082 -0.1716 -0.0454 0.083 Uiso 0.519(3) 1 calc PR A 1 C27B C 0.1257(4) -0.1853(6) -0.0697(4) 0.0420(17) Uani 0.481(3) 1 d P A 2 H27D H 0.0955 -0.1646 -0.1208 0.050 Uiso 0.481(3) 1 calc PR A 2 H27E H 0.1011 -0.2408 -0.0592 0.050 Uiso 0.481(3) 1 calc PR A 2 C28 C 0.2785(4) -0.1248(3) -0.0765(3) 0.0839(15) Uani 1 1 d . A . H28A H 0.2530 -0.0916 -0.1224 0.126 Uiso 1 1 calc R . . H28B H 0.3318 -0.1482 -0.0815 0.126 Uiso 1 1 calc R . . H28C H 0.2875 -0.0870 -0.0316 0.126 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.02569(9) 0.04710(11) 0.02878(9) 0.00406(7) 0.00872(6) 0.00067(7) Cu1 0.02562(15) 0.03123(17) 0.03330(16) 0.00704(13) 0.00226(12) -0.00270(12) F1 0.0457(13) 0.142(3) 0.0939(19) -0.0004(17) 0.0415(13) 0.0033(14) N1 0.0347(13) 0.0495(15) 0.0389(13) 0.0125(11) -0.0043(10) -0.0122(11) C1 0.038(7) 0.095(16) 0.059(9) 0.009(8) -0.006(5) -0.041(8) C1B 0.048(8) 0.042(5) 0.041(6) 0.007(5) -0.021(4) -0.009(5) Sb2 0.02370(9) 0.05400(13) 0.03232(10) -0.01237(8) 0.00606(7) 0.00289(7) Cu2 0.02635(15) 0.03997(18) 0.02193(14) -0.00644(12) 0.00533(11) 0.00154(12) F2 0.0507(13) 0.0964(19) 0.106(2) 0.0205(15) 0.0477(13) -0.0004(12) N2 0.0343(13) 0.0365(13) 0.0630(17) 0.0111(12) 0.0245(12) 0.0048(10) C2 0.055(2) 0.091(3) 0.0342(16) -0.0033(17) 0.0051(14) -0.0150(19) N3 0.0241(10) 0.0354(12) 0.0320(11) 0.0056(9) 0.0076(8) 0.0000(8) F3 0.0648(13) 0.0763(15) 0.0455(11) 0.0235(10) -0.0032(9) 0.0002(11) C3 0.050(2) 0.065(2) 0.057(2) 0.0333(18) -0.0086(16) -0.0108(17) F4 0.0749(16) 0.0981(19) 0.0591(14) -0.0253(13) -0.0035(12) -0.0133(14) N4 0.0248(10) 0.0367(12) 0.0270(10) -0.0005(9) 0.0060(8) 0.0033(8) C4 0.050(2) 0.055(2) 0.102(3) 0.041(2) 0.001(2) 0.0098(17) F5 0.105(2) 0.0794(18) 0.095(2) -0.0388(16) 0.0029(17) -0.0120(16) N5 0.0567(17) 0.0602(18) 0.0530(16) -0.0277(14) 0.0365(14) -0.0306(14) C5 0.0504(19) 0.0370(17) 0.089(3) 0.0226(18) 0.0249(18) 0.0114(14) N6 0.0578(18) 0.101(3) 0.0241(12) 0.0096(14) 0.0087(11) 0.0384(17) F6 0.113(2) 0.101(2) 0.0787(18) 0.0448(16) 0.0100(16) 0.0397(18) C6 0.054(2) 0.062(2) 0.127(4) 0.028(3) 0.057(3) 0.0122(18) C7 0.064(2) 0.0395(17) 0.057(2) -0.0093(14) 0.0336(17) -0.0064(14) F7 0.0248(8) 0.0646(12) 0.0625(12) -0.0145(9) 0.0096(8) 0.0024(8) C8 0.070(2) 0.0507(19) 0.0374(16) -0.0089(14) 0.0185(15) -0.0124(16) F8 0.0266(9) 0.0902(16) 0.0657(13) -0.0325(12) -0.0038(8) 0.0107(9) C9 0.0346(15) 0.0514(18) 0.0347(14) 0.0020(12) 0.0005(11) -0.0105(12) F9 0.037(3) 0.086(5) 0.184(10) -0.101(7) -0.008(5) 0.008(3) F10 0.049(3) 0.288(12) 0.075(4) 0.097(6) -0.004(3) -0.064(5) F11 0.046(3) 0.094(4) 0.137(6) -0.069(4) -0.004(3) 0.007(3) F12 0.044(3) 0.162(7) 0.077(4) 0.054(4) 0.002(3) -0.001(3) F9B 0.040(3) 0.159(11) 0.046(3) -0.043(4) 0.015(2) 0.000(5) F10B 0.065(3) 0.055(3) 0.100(4) 0.034(3) 0.030(3) 0.009(2) F11B 0.059(3) 0.093(4) 0.046(2) -0.034(3) -0.003(2) 0.032(3) F12B 0.078(4) 0.053(3) 0.143(7) 0.036(4) 0.035(5) -0.019(3) C10 0.0412(17) 0.0510(19) 0.0504(18) 0.0115(15) 0.0179(13) 0.0152(14) C11 0.043(7) 0.066(8) 0.059(8) 0.040(6) 0.010(5) -0.011(5) C11B 0.023(4) 0.022(5) 0.026(5) -0.009(4) 0.007(3) 0.001(3) C12 0.023(2) 0.025(2) 0.0179(19) -0.0024(16) 0.0079(15) -0.0048(16) C13 0.018(2) 0.032(2) 0.0178(19) 0.0005(17) 0.0061(15) -0.0010(16) C14 0.023(2) 0.024(2) 0.0154(18) 0.0001(15) 0.0084(15) 0.0007(16) C15 0.023(2) 0.030(2) 0.021(2) -0.0048(17) 0.0071(16) -0.0063(17) C17 0.021(2) 0.029(2) 0.027(2) 0.0004(18) 0.0104(16) 0.0012(17) C12B 0.022(3) 0.060(4) 0.039(3) 0.013(3) 0.000(2) -0.009(2) C13B 0.028(3) 0.064(4) 0.032(3) 0.014(3) -0.003(2) -0.011(3) C14B 0.023(3) 0.064(4) 0.031(3) 0.003(3) 0.002(2) -0.008(2) C15B 0.026(3) 0.053(4) 0.037(3) 0.007(3) 0.004(2) -0.007(2) C17B 0.024(3) 0.060(4) 0.042(3) 0.002(3) 0.007(2) -0.006(3) C16 0.061(2) 0.0472(19) 0.076(2) -0.0107(17) 0.0481(19) -0.0140(16) C18 0.030(6) 0.104(11) 0.014(5) -0.011(5) 0.011(4) 0.014(6) C18B 0.032(7) 0.015(3) 0.031(7) 0.005(3) 0.000(4) -0.002(3) C19 0.0361(15) 0.0540(19) 0.0363(15) -0.0075(13) 0.0045(11) -0.0110(13) C20 0.0348(15) 0.0525(19) 0.0526(18) 0.0160(15) 0.0182(13) 0.0158(13) C21 0.068(2) 0.0315(16) 0.092(3) 0.0155(17) 0.050(2) 0.0101(15) C22 0.094(3) 0.0384(18) 0.100(3) -0.026(2) 0.074(3) -0.0255(19) C23 0.066(2) 0.104(3) 0.062(2) -0.028(2) 0.040(2) -0.051(2) C24 0.057(6) 0.055(8) 0.019(5) -0.017(4) 0.011(4) -0.013(5) C25 0.038(4) 0.078(7) 0.022(3) -0.014(5) 0.002(2) 0.007(5) C24B 0.092(12) 0.074(11) 0.051(9) -0.030(7) 0.036(8) -0.052(9) C25B 0.064(9) 0.088(11) 0.034(6) -0.033(7) 0.019(6) -0.033(7) C26 0.046(2) 0.160(5) 0.0203(14) -0.010(2) 0.0096(13) 0.012(2) C27 0.067(5) 0.073(5) 0.026(3) 0.002(3) 0.009(3) 0.044(4) C27B 0.026(3) 0.061(5) 0.033(3) -0.005(3) -0.004(2) -0.006(3) C28 0.135(5) 0.066(3) 0.058(2) 0.028(2) 0.039(3) 0.034(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 Sb1 F5 1.834(3) . ? Sb1 F6 1.858(2) . ? Sb1 F1 1.860(2) . ? Sb1 F2 1.864(2) . ? Sb1 F3 1.870(2) . ? Sb1 F4 1.877(2) . ? Cu1 N3 1.986(2) . ? Cu1 N1 1.990(3) . ? Cu1 N2 2.120(3) . ? N1 C1B 1.45(2) . ? N1 C3 1.486(4) . ? N1 C2 1.500(5) . ? N1 C1 1.53(2) . ? C1B C12B 1.48(2) . ? Sb2 F10 1.733(5) . ? Sb2 F12B 1.740(5) . ? Sb2 F9 1.778(7) . ? Sb2 F9B 1.840(8) . ? Sb2 F11B 1.854(4) . ? Sb2 F7 1.8764(17) . ? Sb2 F8 1.8803(18) . ? Sb2 F11 1.944(5) . ? Sb2 F10B 1.954(5) . ? Sb2 F12 1.967(6) . ? Cu2 N6 1.973(3) . ? Cu2 N4 1.974(2) . ? Cu2 N5 2.100(3) . ? N2 C7 1.475(5) . ? N2 C6 1.479(4) . ? N2 C5 1.488(4) . ? N3 C11B 1.454(15) . ? N3 C10 1.491(4) . ? N3 C9 1.496(4) . ? N3 C11 1.526(16) . ? C3 C4 1.517(6) . ? N4 C18B 1.447(15) . ? N4 C19 1.482(4) . ? N4 C20 1.501(4) . ? N4 C18 1.514(13) . ? C4 C5 1.519(6) . ? N5 C24B 1.381(17) . ? N5 C22 1.453(6) . ? N5 C23 1.486(4) . ? N5 C24 1.591(12) . ? N6 C28 1.467(6) . ? N6 C26 1.484(5) . ? N6 C27 1.486(7) . ? N6 C27B 1.571(7) . ? C7 C8 1.520(5) . ? C8 C9 1.516(5) . ? C11 C12 1.398(17) . ? C12 C17 1.379(6) . ? C12 C13 1.396(6) . ? C13 C14 1.397(6) . ? C14 C18 1.386(16) . ? C14 C15 1.400(6) . ? C15 C16 1.484(6) . ? C17 C16 1.497(6) . ? C12B C13B 1.384(10) . ? C12B C17B 1.389(9) . ? C13B C14B 1.395(10) . ? C14B C15B 1.396(8) . ? C14B C27B 1.523(10) . ? C15B C16 1.501(7) . ? C17B C16 1.533(8) . ? C20 C21 1.529(5) . ? C21 C22 1.519(6) . ? C24 C25 1.530(12) . ? C25 C26 1.330(13) . ? C24B C25B 1.498(18) . ? C25B C26 1.771(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F5 Sb1 F6 90.92(16) . . ? F5 Sb1 F1 90.85(15) . . ? F6 Sb1 F1 90.43(14) . . ? F5 Sb1 F2 92.10(14) . . ? F6 Sb1 F2 90.95(13) . . ? F1 Sb1 F2 176.73(14) . . ? F5 Sb1 F3 91.70(13) . . ? F6 Sb1 F3 177.37(13) . . ? F1 Sb1 F3 89.82(12) . . ? F2 Sb1 F3 88.67(11) . . ? F5 Sb1 F4 179.78(15) . . ? F6 Sb1 F4 88.87(14) . . ? F1 Sb1 F4 89.13(13) . . ? F2 Sb1 F4 87.93(13) . . ? F3 Sb1 F4 88.51(12) . . ? N3 Cu1 N1 148.84(11) . . ? N3 Cu1 N2 105.08(10) . . ? N1 Cu1 N2 105.59(11) . . ? C1B N1 C3 107.1(9) . . ? C1B N1 C2 112.8(13) . . ? C3 N1 C2 107.5(3) . . ? C1B N1 C1 9(2) . . ? C3 N1 C1 110.7(9) . . ? C2 N1 C1 103.7(12) . . ? C1B N1 Cu1 109.8(10) . . ? C3 N1 Cu1 110.3(2) . . ? C2 N1 Cu1 109.33(19) . . ? C1 N1 Cu1 114.8(9) . . ? N1 C1B C12B 114.3(14) . . ? F10 Sb2 F12B 141.0(5) . . ? F10 Sb2 F9 102.4(6) . . ? F12B Sb2 F9 116.2(5) . . ? F10 Sb2 F9B 124.8(5) . . ? F12B Sb2 F9B 93.8(4) . . ? F9 Sb2 F9B 22.4(5) . . ? F10 Sb2 F11B 50.2(4) . . ? F12B Sb2 F11B 91.6(4) . . ? F9 Sb2 F11B 152.2(4) . . ? F9B Sb2 F11B 174.0(4) . . ? F10 Sb2 F7 95.4(2) . . ? F12B Sb2 F7 89.8(2) . . ? F9 Sb2 F7 91.5(3) . . ? F9B Sb2 F7 90.4(3) . . ? F11B Sb2 F7 87.08(16) . . ? F10 Sb2 F8 86.8(2) . . ? F12B Sb2 F8 87.5(3) . . ? F9 Sb2 F8 89.7(3) . . ? F9B Sb2 F8 89.7(3) . . ? F11B Sb2 F8 93.01(16) . . ? F7 Sb2 F8 177.27(10) . . ? F10 Sb2 F11 89.2(5) . . ? F12B Sb2 F11 52.0(4) . . ? F9 Sb2 F11 167.9(4) . . ? F9B Sb2 F11 145.7(4) . . ? F11B Sb2 F11 39.9(3) . . ? F7 Sb2 F11 91.24(15) . . ? F8 Sb2 F11 87.09(16) . . ? F10 Sb2 F10B 40.4(4) . . ? F12B Sb2 F10B 177.0(3) . . ? F9 Sb2 F10B 63.1(4) . . ? F9B Sb2 F10B 85.4(4) . . ? F11B Sb2 F10B 89.1(3) . . ? F7 Sb2 F10B 87.29(18) . . ? F8 Sb2 F10B 95.44(18) . . ? F11 Sb2 F10B 128.9(3) . . ? F10 Sb2 F12 169.6(5) . . ? F12B Sb2 F12 28.6(3) . . ? F9 Sb2 F12 87.7(4) . . ? F9B Sb2 F12 65.3(4) . . ? F11B Sb2 F12 119.9(4) . . ? F7 Sb2 F12 86.92(18) . . ? F8 Sb2 F12 90.67(19) . . ? F11 Sb2 F12 80.6(4) . . ? F10B Sb2 F12 150.1(3) . . ? N6 Cu2 N4 150.62(13) . . ? N6 Cu2 N5 104.34(15) . . ? N4 Cu2 N5 104.95(12) . . ? C7 N2 C6 109.8(3) . . ? C7 N2 C5 108.5(3) . . ? C6 N2 C5 109.5(3) . . ? C7 N2 Cu1 109.62(19) . . ? C6 N2 Cu1 110.8(2) . . ? C5 N2 Cu1 108.6(2) . . ? C11B N3 C10 107.5(5) . . ? C11B N3 C9 107.1(5) . . ? C10 N3 C9 106.4(2) . . ? C11B N3 C11 5.4(13) . . ? C10 N3 C11 109.7(7) . . ? C9 N3 C11 110.7(6) . . ? C11B N3 Cu1 116.1(6) . . ? C10 N3 Cu1 109.69(17) . . ? C9 N3 Cu1 109.55(18) . . ? C11 N3 Cu1 110.7(7) . . ? N1 C3 C4 115.4(3) . . ? C18B N4 C19 110.5(5) . . ? C18B N4 C20 106.6(5) . . ? C19 N4 C20 107.5(2) . . ? C18B N4 C18 4.5(9) . . ? C19 N4 C18 107.9(6) . . ? C20 N4 C18 111.0(6) . . ? C18B N4 Cu2 113.2(6) . . ? C19 N4 Cu2 109.12(17) . . ? C20 N4 Cu2 109.85(18) . . ? C18 N4 Cu2 111.4(6) . . ? C3 C4 C5 114.9(3) . . ? C24B N5 C22 94.1(8) . . ? C24B N5 C23 114.4(8) . . ? C22 N5 C23 110.6(3) . . ? C24B N5 C24 21.7(9) . . ? C22 N5 C24 115.7(5) . . ? C23 N5 C24 105.7(6) . . ? C24B N5 Cu2 117.2(7) . . ? C22 N5 Cu2 110.1(2) . . ? C23 N5 Cu2 109.3(2) . . ? C24 N5 Cu2 105.0(6) . . ? N2 C5 C4 114.4(3) . . ? C28 N6 C26 106.3(3) . . ? C28 N6 C27 93.6(5) . . ? C26 N6 C27 120.3(4) . . ? C28 N6 C27B 123.6(4) . . ? C26 N6 C27B 97.7(4) . . ? C27 N6 C27B 32.0(4) . . ? C28 N6 Cu2 110.2(3) . . ? C26 N6 Cu2 110.3(3) . . ? C27 N6 Cu2 114.2(3) . . ? C27B N6 Cu2 107.7(3) . . ? N2 C7 C8 114.2(3) . . ? C9 C8 C7 114.7(3) . . ? N3 C9 C8 115.7(2) . . ? C12 C11 N3 114.3(11) . . ? C17 C12 C13 119.2(4) . . ? C17 C12 C11 115.5(8) . . ? C13 C12 C11 125.2(9) . . ? C12 C13 C14 121.5(4) . . ? C18 C14 C13 121.0(7) . . ? C18 C14 C15 120.4(7) . . ? C13 C14 C15 118.4(4) . . ? C14 C15 C16 126.1(4) . . ? C12 C17 C16 126.0(4) . . ? C13B C12B C17B 118.7(6) . . ? C13B C12B C1B 124.4(12) . . ? C17B C12B C1B 116.9(12) . . ? C12B C13B C14B 121.9(6) . . ? C13B C14B C15B 118.9(6) . . ? C13B C14B C27B 121.7(6) . . ? C15B C14B C27B 119.2(6) . . ? C14B C15B C16 126.4(6) . . ? C12B C17B C16 126.3(6) . . ? C15 C16 C17 108.3(4) . . ? C15 C16 C15B 61.9(3) . . ? C17 C16 C15B 145.1(3) . . ? C15 C16 C17B 151.1(4) . . ? C17 C16 C17B 65.9(3) . . ? C15B C16 C17B 105.6(4) . . ? C14 C18 N4 116.7(10) . . ? N4 C20 C21 116.1(3) . . ? C22 C21 C20 115.1(3) . . ? N5 C22 C21 114.8(3) . . ? C25 C24 N5 118.2(9) . . ? C26 C25 C24 109.7(9) . . ? N5 C24B C25B 106.2(14) . . ? C24B C25B C26 118.8(10) . . ? C25 C26 N6 113.4(5) . . ? C25 C26 C25B 20.1(6) . . ? N6 C26 C25B 117.1(5) . . ? C14B C27B N6 107.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C1B 100.4(12) . . . . ? N2 Cu1 N1 C1B -90.1(12) . . . . ? N3 Cu1 N1 C3 -141.9(2) . . . . ? N2 Cu1 N1 C3 27.7(2) . . . . ? N3 Cu1 N1 C2 -23.8(3) . . . . ? N2 Cu1 N1 C2 145.7(2) . . . . ? N3 Cu1 N1 C1 92.2(12) . . . . ? N2 Cu1 N1 C1 -98.3(12) . . . . ? C3 N1 C1B C12B 171.4(14) . . . . ? C2 N1 C1B C12B 53(2) . . . . ? C1 N1 C1B C12B 57(9) . . . . ? Cu1 N1 C1B C12B -69(2) . . . . ? N3 Cu1 N2 C7 28.5(2) . . . . ? N1 Cu1 N2 C7 -145.88(19) . . . . ? N3 Cu1 N2 C6 -92.8(3) . . . . ? N1 Cu1 N2 C6 92.8(3) . . . . ? N3 Cu1 N2 C5 146.9(2) . . . . ? N1 Cu1 N2 C5 -27.5(2) . . . . ? N1 Cu1 N3 C11B -97.8(4) . . . . ? N2 Cu1 N3 C11B 92.6(4) . . . . ? N1 Cu1 N3 C10 24.2(3) . . . . ? N2 Cu1 N3 C10 -145.34(19) . . . . ? N1 Cu1 N3 C9 140.7(2) . . . . ? N2 Cu1 N3 C9 -28.85(19) . . . . ? N1 Cu1 N3 C11 -97.0(7) . . . . ? N2 Cu1 N3 C11 93.5(6) . . . . ? C1B N1 C3 C4 69.3(13) . . . . ? C2 N1 C3 C4 -169.2(3) . . . . ? C1 N1 C3 C4 78.1(12) . . . . ? Cu1 N1 C3 C4 -50.1(3) . . . . ? N6 Cu2 N4 C18B 95.5(5) . . . . ? N5 Cu2 N4 C18B -88.9(4) . . . . ? N6 Cu2 N4 C19 -27.9(3) . . . . ? N5 Cu2 N4 C19 147.63(18) . . . . ? N6 Cu2 N4 C20 -145.5(2) . . . . ? N5 Cu2 N4 C20 30.01(19) . . . . ? N6 Cu2 N4 C18 91.1(7) . . . . ? N5 Cu2 N4 C18 -93.4(6) . . . . ? N1 C3 C4 C5 76.7(4) . . . . ? N6 Cu2 N5 C24B 41.3(9) . . . . ? N4 Cu2 N5 C24B -136.5(9) . . . . ? N6 Cu2 N5 C22 147.2(2) . . . . ? N4 Cu2 N5 C22 -30.6(2) . . . . ? N6 Cu2 N5 C23 -91.1(3) . . . . ? N4 Cu2 N5 C23 91.2(3) . . . . ? N6 Cu2 N5 C24 22.0(6) . . . . ? N4 Cu2 N5 C24 -155.8(5) . . . . ? C7 N2 C5 C4 167.7(3) . . . . ? C6 N2 C5 C4 -72.5(4) . . . . ? Cu1 N2 C5 C4 48.7(3) . . . . ? C3 C4 C5 N2 -76.2(4) . . . . ? N4 Cu2 N6 C28 29.1(4) . . . . ? N5 Cu2 N6 C28 -146.4(3) . . . . ? N4 Cu2 N6 C26 146.2(2) . . . . ? N5 Cu2 N6 C26 -29.4(3) . . . . ? N4 Cu2 N6 C27 -74.7(6) . . . . ? N5 Cu2 N6 C27 109.8(5) . . . . ? N4 Cu2 N6 C27B -108.3(4) . . . . ? N5 Cu2 N6 C27B 76.1(4) . . . . ? C6 N2 C7 C8 73.4(3) . . . . ? C5 N2 C7 C8 -166.9(3) . . . . ? Cu1 N2 C7 C8 -48.5(3) . . . . ? N2 C7 C8 C9 74.8(4) . . . . ? C11B N3 C9 C8 -75.1(6) . . . . ? C10 N3 C9 C8 170.1(3) . . . . ? C11 N3 C9 C8 -70.7(8) . . . . ? Cu1 N3 C9 C8 51.6(3) . . . . ? C7 C8 C9 N3 -76.9(4) . . . . ? C11B N3 C11 C12 -121(10) . . . . ? C10 N3 C11 C12 -53.9(14) . . . . ? C9 N3 C11 C12 -171.1(9) . . . . ? Cu1 N3 C11 C12 67.3(13) . . . . ? N3 C11 C12 C17 -89.9(13) . . . . ? N3 C11 C12 C13 94.6(12) . . . . ? C17 C12 C13 C14 0.9(6) . . . . ? C11 C12 C13 C14 176.3(9) . . . . ? C12 C13 C14 C18 -177.1(7) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C18 C14 C15 C16 -178.9(7) . . . . ? C13 C14 C15 C16 5.1(6) . . . . ? C13 C12 C17 C16 -4.7(6) . . . . ? C11 C12 C17 C16 179.4(8) . . . . ? N1 C1B C12B C13B -86.2(19) . . . . ? N1 C1B C12B C17B 94(2) . . . . ? C17B C12B C13B C14B -3.2(8) . . . . ? C1B C12B C13B C14B 176.8(11) . . . . ? C12B C13B C14B C15B 2.9(8) . . . . ? C12B C13B C14B C27B 178.2(5) . . . . ? C13B C14B C15B C16 -10.8(8) . . . . ? C27B C14B C15B C16 173.8(5) . . . . ? C13B C12B C17B C16 11.2(8) . . . . ? C1B C12B C17B C16 -168.7(10) . . . . ? C14 C15 C16 C17 -7.7(5) . . . . ? C14 C15 C16 C15B 135.6(5) . . . . ? C14 C15 C16 C17B 65.4(10) . . . . ? C12 C17 C16 C15 7.5(6) . . . . ? C12 C17 C16 C15B -59.3(9) . . . . ? C12 C17 C16 C17B -142.1(5) . . . . ? C14B C15B C16 C15 -136.1(6) . . . . ? C14B C15B C16 C17 -54.3(10) . . . . ? C14B C15B C16 C17B 15.8(7) . . . . ? C12B C17B C16 C15 43.4(12) . . . . ? C12B C17B C16 C17 127.8(6) . . . . ? C12B C17B C16 C15B -16.1(7) . . . . ? C13 C14 C18 N4 -93.2(11) . . . . ? C15 C14 C18 N4 90.9(11) . . . . ? C18B N4 C18 C14 -171(16) . . . . ? C19 N4 C18 C14 62.6(12) . . . . ? C20 N4 C18 C14 -179.9(9) . . . . ? Cu2 N4 C18 C14 -57.1(12) . . . . ? C18B N4 C20 C21 72.2(7) . . . . ? C19 N4 C20 C21 -169.3(3) . . . . ? C18 N4 C20 C21 72.9(7) . . . . ? Cu2 N4 C20 C21 -50.7(3) . . . . ? N4 C20 C21 C22 73.6(4) . . . . ? C24B N5 C22 C21 170.7(8) . . . . ? C23 N5 C22 C21 -71.3(4) . . . . ? C24 N5 C22 C21 168.5(7) . . . . ? Cu2 N5 C22 C21 49.7(3) . . . . ? C20 C21 C22 N5 -73.0(4) . . . . ? C24B N5 C24 C25 -170(4) . . . . ? C22 N5 C24 C25 -164.5(9) . . . . ? C23 N5 C24 C25 72.8(12) . . . . ? Cu2 N5 C24 C25 -42.8(12) . . . . ? N5 C24 C25 C26 76.9(12) . . . . ? C22 N5 C24B C25B -173.1(10) . . . . ? C23 N5 C24B C25B 72.1(12) . . . . ? C24 N5 C24B C25B 2(2) . . . . ? Cu2 N5 C24B C25B -58.0(13) . . . . ? N5 C24B C25B C26 69.2(15) . . . . ? C24 C25 C26 N6 -85.7(8) . . . . ? C24 C25 C26 C25B 19.4(18) . . . . ? C28 N6 C26 C25 -178.3(5) . . . . ? C27 N6 C26 C25 -74.1(8) . . . . ? C27B N6 C26 C25 -49.9(6) . . . . ? Cu2 N6 C26 C25 62.2(6) . . . . ? C28 N6 C26 C25B 159.8(6) . . . . ? C27 N6 C26 C25B -96.0(8) . . . . ? C27B N6 C26 C25B -71.8(7) . . . . ? Cu2 N6 C26 C25B 40.4(7) . . . . ? C24B C25B C26 C25 -149(3) . . . . ? C24B C25B C26 N6 -64.2(13) . . . . ? C13B C14B C27B N6 91.0(6) . . . . ? C15B C14B C27B N6 -93.7(6) . . . . ? C28 N6 C27B C14B -56.5(6) . . . . ? C26 N6 C27B C14B -171.9(5) . . . . ? C27 N6 C27B C14B -33.7(6) . . . . ? Cu2 N6 C27B C14B 73.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.403 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.083