Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'William Tolman' _publ_contact_author_address ; Department of Chemistry 139 Smith Hall University of Minnesota 207 Pleasant St. SE Minneapolis MN 55455 UNITED STATES OF AMERICA ; _publ_contact_author_email TOLMAN@CHEM.UMN.EDU _publ_section_title ; Electronic Tuning of ?-Diketiminate Ligands with Fluorinated Substituents: Effects on the O2-Reactivity of Mononuclear Cu(I) Complexes ; loop_ _publ_author_name 'William Tolman' 'Nermeen W.Aboelella' C.J.Cramer 'Benjamin Gherman' ; Lyndal M.R.Hill ; # Attachment 'CIF_revised.txt' data_05269m _database_code_depnum_ccdc_archive 'CCDC 614585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(L1)Cu(CH3CN)] ; _chemical_name_common ((L1)Cu(CH3CN)) _chemical_melting_point ? _chemical_formula_moiety 'C31 H41 Cu F3 N3' _chemical_formula_sum 'C31 H41 Cu F3 N3' _chemical_formula_weight 576.21 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.9031(7) _cell_length_b 14.2839(8) _cell_length_c 18.0089(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.469(2) _cell_angle_gamma 90.00 _cell_volume 3148.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3847 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.39 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6672 _exptl_absorpt_correction_T_max 0.8671 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18407 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7107 _reflns_number_gt 6454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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. One molecule of the Cu(I) complex occupies the asymmetric unit. Rotational disorder for an iso-propyl group on one phenyl ring of the ligand was modeled, with a 73:27 ratio for the two forms (C27, C28, C29, H27A versus C27, C28', C29', H27B, with the methine carbon, C27, occupying a single site). For C5, the ligand backbone methyl, its thermal ellipsoid is elongated in a similar manner to those of C29 and C29' (two rotationally related sites that belong to the nearby disordered iso-propyl methyl group). For the C29' position, one of its hydrogen atoms (H29D) is within Van der Waal's contact of H5B (2.017 Angstroms, as calculated in SHELXTL; though this is potentially an over-estimate of the distance given the default settings used for assigning C-H distances for riding H-atoms is much smaller than that used in neutron-scattering measurements, for example). This indicates that the elongation of the C5 thermal ellipsoid is coupled to the rotational disorder of the iso-propyl group at C27, particularly as the atoms in the six-membered chelate ring including the Cu center (Cu1-N1-C2-C3-C4-N2) have thermal ellipsoids that are not perturbed in this way. However, modeling this style of disorder at C5 is not possible. Alerts produced by the checkCIF program (http://checkcif.iucr.org/) do not warrant explanation or adjustment of the structure solution. ; _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^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(8) _refine_ls_number_reflns 7107 _refine_ls_number_parameters 350 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.026 _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 Cu1 Cu 0.160534(16) 0.646837(13) 0.509511(14) 0.03344(6) Uani 1 1 d . . . F1 F 0.26631(13) 0.84785(11) 0.33410(10) 0.0658(4) Uani 1 1 d . . . F2 F 0.13599(14) 0.77051(10) 0.25803(8) 0.0656(4) Uani 1 1 d . . . F3 F 0.10685(18) 0.90550(12) 0.29498(11) 0.0860(6) Uani 1 1 d . . . N1 N 0.18683(12) 0.70345(10) 0.41901(9) 0.0300(3) Uani 1 1 d . . . N2 N 0.06006(15) 0.73811(12) 0.52659(10) 0.0418(4) Uani 1 1 d . . . N3 N 0.21146(14) 0.53424(11) 0.56055(10) 0.0393(4) Uani 1 1 d . . . C1 C 0.1607(2) 0.82671(17) 0.31922(14) 0.0434(5) Uani 1 1 d . . . C2 C 0.13884(17) 0.78359(13) 0.39046(12) 0.0367(4) Uani 1 1 d . . . C3 C 0.0690(2) 0.83372(16) 0.41956(15) 0.0546(6) Uani 1 1 d . . . H3A H 0.0435 0.8911 0.3935 0.065 Uiso 1 1 calc R . . C4 C 0.0299(2) 0.81257(17) 0.48200(15) 0.0583(7) Uani 1 1 d . . . C5 C -0.0503(4) 0.8814(2) 0.4978(2) 0.1054(15) Uani 1 1 d . . . H5A H -0.0726 0.8590 0.5419 0.158 Uiso 1 1 calc R . . H5B H -0.1147 0.8868 0.4512 0.158 Uiso 1 1 calc R . . H5C H -0.0153 0.9428 0.5107 0.158 Uiso 1 1 calc R . . C6 C 0.25450(16) 0.65276(12) 0.38399(11) 0.0323(4) Uani 1 1 d . . . C7 C 0.20641(19) 0.58505(13) 0.32732(12) 0.0418(5) Uani 1 1 d . . . C8 C 0.2744(3) 0.53096(17) 0.29835(14) 0.0582(7) Uani 1 1 d . . . H8A H 0.2432 0.4840 0.2605 0.070 Uiso 1 1 calc R . . C9 C 0.3839(3) 0.5434(2) 0.32268(15) 0.0671(8) Uani 1 1 d . . . H9A H 0.4283 0.5068 0.3007 0.081 Uiso 1 1 calc R . . C10 C 0.4313(2) 0.6092(2) 0.37951(17) 0.0596(8) Uani 1 1 d . . . H10A H 0.5083 0.6170 0.3966 0.071 Uiso 1 1 calc R . . C11 C 0.36772(19) 0.66467(17) 0.41243(14) 0.0422(5) Uani 1 1 d D . . C12 C 0.0841(2) 0.56937(18) 0.30028(14) 0.0569(6) Uani 1 1 d . . . H12A H 0.0496 0.6270 0.3134 0.068 Uiso 1 1 calc R . . C13 C 0.0544(3) 0.4883(3) 0.34429(16) 0.0895(11) Uani 1 1 d . . . H13A H 0.0849 0.4994 0.4008 0.134 Uiso 1 1 calc R . . H13B H 0.0844 0.4301 0.3308 0.134 Uiso 1 1 calc R . . H13C H -0.0253 0.4832 0.3297 0.134 Uiso 1 1 calc R . . C14 C 0.0352(3) 0.5537(2) 0.21191(15) 0.0715(8) Uani 1 1 d . . . H14A H 0.0542 0.6064 0.1840 0.107 Uiso 1 1 calc R . . H14B H -0.0445 0.5489 0.1978 0.107 Uiso 1 1 calc R . . H14C H 0.0645 0.4956 0.1975 0.107 Uiso 1 1 calc R . . C15 C 0.4196(2) 0.73173(19) 0.47804(15) 0.0587(6) Uani 1 1 d . . . H15A H 0.3607 0.7723 0.4857 0.070 Uiso 1 1 calc R . . C16 C 0.5041(3) 0.7948(3) 0.4611(2) 0.0891(10) Uani 1 1 d . . . H16A H 0.4699 0.8305 0.4131 0.134 Uiso 1 1 calc R . . H16B H 0.5636 0.7566 0.4544 0.134 Uiso 1 1 calc R . . H16C H 0.5335 0.8382 0.5050 0.134 Uiso 1 1 calc R . . C17 C 0.4707(3) 0.6756(3) 0.55411(19) 0.0909(11) Uani 1 1 d . . . H17A H 0.4144 0.6368 0.5648 0.136 Uiso 1 1 calc R . . H17B H 0.5011 0.7190 0.5978 0.136 Uiso 1 1 calc R . . H17C H 0.5290 0.6354 0.5481 0.136 Uiso 1 1 calc R . . C18 C 0.0165(2) 0.72303(14) 0.58941(12) 0.0455(5) Uani 1 1 d . A . C19 C 0.0705(2) 0.76253(16) 0.66298(14) 0.0556(6) Uani 1 1 d . . . C20 C 0.0263(3) 0.7478(2) 0.72292(15) 0.0644(8) Uani 1 1 d . . . H20A H 0.0610 0.7746 0.7729 0.077 Uiso 1 1 calc R . . C21 C -0.0660(3) 0.6956(2) 0.71139(15) 0.0659(8) Uani 1 1 d . . . H21A H -0.0958 0.6877 0.7530 0.079 Uiso 1 1 calc R . . C22 C -0.1164(3) 0.65444(18) 0.63990(18) 0.0577(8) Uani 1 1 d . A . H22A H -0.1794 0.6168 0.6331 0.069 Uiso 1 1 calc R . . C23 C -0.0757(2) 0.66730(17) 0.57707(15) 0.0482(6) Uani 1 1 d . . . C24 C 0.1770(3) 0.8152(2) 0.67789(19) 0.0717(9) Uani 1 1 d . . . H24A H 0.1871 0.8272 0.6259 0.086 Uiso 1 1 calc R . . C25 C 0.2706(3) 0.7574(3) 0.7243(3) 0.1115(14) Uani 1 1 d . . . H25A H 0.2706 0.6977 0.6974 0.167 Uiso 1 1 calc R . . H25B H 0.2641 0.7455 0.7762 0.167 Uiso 1 1 calc R . . H25C H 0.3390 0.7908 0.7298 0.167 Uiso 1 1 calc R . . C26 C 0.1753(5) 0.9119(3) 0.7174(3) 0.131(2) Uani 1 1 d . . . H26A H 0.1133 0.9487 0.6852 0.197 Uiso 1 1 calc R . . H26B H 0.2435 0.9454 0.7224 0.197 Uiso 1 1 calc R . . H26C H 0.1682 0.9024 0.7694 0.197 Uiso 1 1 calc R . . C27 C -0.1283(2) 0.6177(2) 0.49948(16) 0.0598(6) Uani 0.731(6) 1 d PD A 1 H27A H -0.0936 0.6441 0.4617 0.072 Uiso 0.731(6) 1 calc PR A 1 C28 C -0.1055(5) 0.5141(3) 0.5039(3) 0.0948(17) Uani 0.731(6) 1 d P A 1 H28A H -0.0294 0.5030 0.5358 0.142 Uiso 0.731(6) 1 calc PR A 1 H28B H -0.1177 0.4894 0.4510 0.142 Uiso 0.731(6) 1 calc PR A 1 H28C H -0.1544 0.4825 0.5278 0.142 Uiso 0.731(6) 1 calc PR A 1 C29 C -0.2524(5) 0.6372(6) 0.4646(4) 0.125(3) Uani 0.731(6) 1 d P A 1 H29A H -0.2681 0.7005 0.4792 0.187 Uiso 0.731(6) 1 calc PR A 1 H29B H -0.2929 0.5915 0.4852 0.187 Uiso 0.731(6) 1 calc PR A 1 H29C H -0.2746 0.6321 0.4074 0.187 Uiso 0.731(6) 1 calc PR A 1 C27' C -0.1283(2) 0.6177(2) 0.49948(16) 0.0598(6) Uani 0.269(6) 1 d PD A 2 H27B H -0.0669 0.6018 0.4790 0.072 Uiso 0.269(6) 1 calc PR A 2 C28' C -0.1737(14) 0.5297(10) 0.5118(9) 0.0948(17) Uani 0.269(6) 1 d P A 2 H28D H -0.1215 0.4970 0.5556 0.142 Uiso 0.269(6) 1 calc PR A 2 H28E H -0.1889 0.4915 0.4643 0.142 Uiso 0.269(6) 1 calc PR A 2 H28F H -0.2417 0.5406 0.5237 0.142 Uiso 0.269(6) 1 calc PR A 2 C29' C -0.1929(14) 0.6915(19) 0.4461(11) 0.125(3) Uani 0.269(6) 1 d P A 2 H29D H -0.1503 0.7496 0.4539 0.187 Uiso 0.269(6) 1 calc PR A 2 H29E H -0.2612 0.7026 0.4575 0.187 Uiso 0.269(6) 1 calc PR A 2 H29F H -0.2094 0.6710 0.3916 0.187 Uiso 0.269(6) 1 calc PR A 2 C30 C 0.23802(17) 0.46311(14) 0.58838(12) 0.0395(4) Uani 1 1 d . . . C31 C 0.2715(2) 0.37227(15) 0.62314(14) 0.0512(6) Uani 1 1 d . . . H31A H 0.2569 0.3248 0.5818 0.077 Uiso 1 1 calc R . . H31B H 0.2304 0.3571 0.6589 0.077 Uiso 1 1 calc R . . H31C H 0.3498 0.3733 0.6522 0.077 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 Cu1 0.04473(12) 0.02781(10) 0.03089(10) 0.00469(11) 0.01636(8) 0.00818(12) F1 0.0710(10) 0.0706(10) 0.0665(10) 0.0169(7) 0.0370(8) -0.0100(7) F2 0.1043(12) 0.0589(8) 0.0361(7) 0.0095(6) 0.0260(7) -0.0043(8) F3 0.1292(15) 0.0673(11) 0.0968(13) 0.0557(10) 0.0859(12) 0.0548(11) N1 0.0367(8) 0.0260(7) 0.0298(7) 0.0023(6) 0.0141(6) 0.0017(6) N2 0.0609(11) 0.0356(9) 0.0366(9) 0.0094(7) 0.0266(8) 0.0181(8) N3 0.0504(10) 0.0365(9) 0.0352(8) 0.0057(7) 0.0196(7) 0.0131(8) C1 0.0578(14) 0.0363(11) 0.0461(13) 0.0133(10) 0.0306(11) 0.0089(9) C2 0.0496(11) 0.0304(9) 0.0357(10) 0.0059(8) 0.0214(9) 0.0041(8) C3 0.0822(17) 0.0389(12) 0.0585(15) 0.0230(10) 0.0448(13) 0.0273(11) C4 0.0878(18) 0.0475(13) 0.0568(15) 0.0197(11) 0.0471(14) 0.0326(13) C5 0.175(4) 0.0763(18) 0.113(3) 0.0601(19) 0.113(3) 0.085(2) C6 0.0440(10) 0.0267(9) 0.0311(9) 0.0052(7) 0.0188(8) 0.0042(7) C7 0.0677(14) 0.0301(9) 0.0335(10) 0.0023(8) 0.0244(9) -0.0001(9) C8 0.104(2) 0.0394(12) 0.0408(12) 0.0017(10) 0.0358(13) 0.0174(12) C9 0.095(2) 0.0682(17) 0.0504(14) 0.0197(13) 0.0403(15) 0.0473(16) C10 0.0505(15) 0.0762(19) 0.0602(17) 0.0326(16) 0.0292(13) 0.0282(14) C11 0.0427(12) 0.0476(13) 0.0395(12) 0.0119(10) 0.0175(10) 0.0066(10) C12 0.0758(16) 0.0530(13) 0.0456(12) -0.0160(11) 0.0244(11) -0.0294(12) C13 0.127(3) 0.099(2) 0.0437(14) -0.0159(15) 0.0292(16) -0.071(2) C14 0.089(2) 0.0742(18) 0.0480(14) -0.0098(13) 0.0174(14) -0.0326(16) C15 0.0451(13) 0.0699(16) 0.0571(15) -0.0017(13) 0.0104(11) -0.0114(12) C16 0.0627(18) 0.091(2) 0.110(3) 0.004(2) 0.0234(18) -0.0246(17) C17 0.085(2) 0.115(3) 0.0539(18) 0.0118(19) -0.0047(16) -0.032(2) C18 0.0716(15) 0.0349(10) 0.0408(11) 0.0138(9) 0.0331(11) 0.0280(10) C19 0.0842(18) 0.0433(12) 0.0488(13) 0.0061(10) 0.0348(13) 0.0243(12) C20 0.104(2) 0.0584(15) 0.0418(14) 0.0124(11) 0.0385(14) 0.0359(16) C21 0.102(2) 0.0638(17) 0.0517(15) 0.0289(13) 0.0524(15) 0.0480(16) C22 0.0704(17) 0.0547(16) 0.0634(17) 0.0266(13) 0.0432(14) 0.0341(13) C23 0.0598(15) 0.0480(12) 0.0456(14) 0.0175(11) 0.0291(12) 0.0264(12) C24 0.110(3) 0.0514(16) 0.0626(18) -0.0165(14) 0.0399(17) -0.0065(17) C25 0.089(3) 0.094(3) 0.137(4) -0.014(3) 0.016(2) -0.010(2) C26 0.214(6) 0.057(2) 0.137(4) -0.033(2) 0.075(4) -0.009(3) C27 0.0503(14) 0.0763(17) 0.0557(15) 0.0110(13) 0.0208(12) 0.0144(13) C28 0.089(4) 0.074(3) 0.099(3) -0.020(2) -0.003(3) 0.012(3) C29 0.062(3) 0.203(8) 0.091(4) -0.014(4) -0.002(3) 0.058(4) C27' 0.0503(14) 0.0763(17) 0.0557(15) 0.0110(13) 0.0208(12) 0.0144(13) C28' 0.089(4) 0.074(3) 0.099(3) -0.020(2) -0.003(3) 0.012(3) C29' 0.062(3) 0.203(8) 0.091(4) -0.014(4) -0.002(3) 0.058(4) C30 0.0486(11) 0.0397(11) 0.0322(10) 0.0003(8) 0.0156(8) 0.0091(9) C31 0.0720(15) 0.0387(11) 0.0435(12) 0.0104(9) 0.0194(11) 0.0224(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.8656(16) . ? Cu1 N2 1.9307(16) . ? Cu1 N1 1.9431(14) . ? F1 C1 1.338(3) . ? F2 C1 1.318(3) . ? F3 C1 1.322(3) . ? N1 C2 1.325(2) . ? N1 C6 1.426(2) . ? N2 C4 1.315(3) . ? N2 C18 1.430(3) . ? N3 C30 1.137(2) . ? C1 C2 1.528(3) . ? C2 C3 1.378(3) . ? C3 C4 1.403(3) . ? C3 H3A 0.9500 . ? C4 C5 1.518(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.397(3) . ? C6 C7 1.400(3) . ? C7 C8 1.389(3) . ? C7 C12 1.514(4) . ? C8 C9 1.351(4) . ? C8 H8A 0.9500 . ? C9 C10 1.382(4) . ? C9 H9A 0.9500 . ? C10 C11 1.400(4) . ? C10 H10A 0.9500 . ? C11 C15 1.504(3) . ? C12 C13 1.519(4) . ? C12 C14 1.531(3) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.518(4) . ? C15 C17 1.543(4) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.389(4) . ? C18 C19 1.405(3) . ? C19 C20 1.387(3) . ? C19 C24 1.515(4) . ? C20 C21 1.364(5) . ? C20 H20A 0.9500 . ? C21 C22 1.377(5) . ? C21 H21A 0.9500 . ? C22 C23 1.402(4) . ? C22 H22A 0.9500 . ? C23 C27 1.521(4) . ? C24 C25 1.482(5) . ? C24 C26 1.557(5) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.506(6) . ? C27 C29 1.548(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C30 C31 1.446(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 130.78(7) . . ? N3 Cu1 N1 130.10(7) . . ? N2 Cu1 N1 99.04(6) . . ? C2 N1 C6 122.91(15) . . ? C2 N1 Cu1 120.04(12) . . ? C6 N1 Cu1 116.98(11) . . ? C4 N2 C18 119.34(16) . . ? C4 N2 Cu1 122.19(14) . . ? C18 N2 Cu1 118.46(12) . . ? C30 N3 Cu1 176.12(18) . . ? F2 C1 F3 106.3(2) . . ? F2 C1 F1 105.43(19) . . ? F3 C1 F1 105.6(2) . . ? F2 C1 C2 113.36(19) . . ? F3 C1 C2 113.76(18) . . ? F1 C1 C2 111.73(19) . . ? N1 C2 C3 125.64(18) . . ? N1 C2 C1 119.09(17) . . ? C3 C2 C1 115.27(18) . . ? C2 C3 C4 129.6(2) . . ? C2 C3 H3A 115.2 . . ? C4 C3 H3A 115.2 . . ? N2 C4 C3 123.4(2) . . ? N2 C4 C5 119.8(2) . . ? C3 C4 C5 116.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.46(19) . . ? C11 C6 N1 119.46(17) . . ? C7 C6 N1 118.75(18) . . ? C8 C7 C6 118.1(2) . . ? C8 C7 C12 121.0(2) . . ? C6 C7 C12 120.86(19) . . ? C9 C8 C7 121.7(2) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 120.1(2) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C6 C11 C10 117.4(2) . . ? C6 C11 C15 121.3(2) . . ? C10 C11 C15 121.2(2) . . ? C7 C12 C13 110.8(2) . . ? C7 C12 C14 113.6(2) . . ? C13 C12 C14 109.98(19) . . ? C7 C12 H12A 107.4 . . ? C13 C12 H12A 107.4 . . ? C14 C12 H12A 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 113.0(2) . . ? C11 C15 C17 109.0(2) . . ? C16 C15 C17 110.8(2) . . ? C11 C15 H15A 108.0 . . ? C16 C15 H15A 108.0 . . ? C17 C15 H15A 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.6(2) . . ? C23 C18 N2 119.4(2) . . ? C19 C18 N2 118.9(2) . . ? C20 C19 C18 118.0(3) . . ? C20 C19 C24 120.7(3) . . ? C18 C19 C24 121.2(2) . . ? C21 C20 C19 121.3(3) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C21 C22 C23 120.8(3) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C18 C23 C22 117.8(3) . . ? C18 C23 C27 121.6(2) . . ? C22 C23 C27 120.5(3) . . ? C25 C24 C19 110.8(3) . . ? C25 C24 C26 111.3(4) . . ? C19 C24 C26 112.2(3) . . ? C25 C24 H24A 107.4 . . ? C19 C24 H24A 107.4 . . ? C26 C24 H24A 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 112.7(3) . . ? C28 C27 C29 111.0(4) . . ? C23 C27 C29 113.1(3) . . ? C28 C27 H27A 106.5 . . ? C23 C27 H27A 106.5 . . ? C29 C27 H27A 106.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H28D C28' H28E 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? H29D C29' H29E 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? N3 C30 C31 179.5(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 C2 177.71(14) . . . . ? N2 Cu1 N1 C2 0.81(16) . . . . ? N3 Cu1 N1 C6 0.63(18) . . . . ? N2 Cu1 N1 C6 -176.28(14) . . . . ? N3 Cu1 N2 C4 -177.1(2) . . . . ? N1 Cu1 N2 C4 -0.2(2) . . . . ? N3 Cu1 N2 C18 2.2(2) . . . . ? N1 Cu1 N2 C18 179.05(17) . . . . ? N2 Cu1 N3 C30 96(2) . . . . ? N1 Cu1 N3 C30 -80(2) . . . . ? C6 N1 C2 C3 177.0(2) . . . . ? Cu1 N1 C2 C3 0.1(3) . . . . ? C6 N1 C2 C1 -3.0(3) . . . . ? Cu1 N1 C2 C1 -179.95(16) . . . . ? F2 C1 C2 N1 57.2(3) . . . . ? F3 C1 C2 N1 178.7(2) . . . . ? F1 C1 C2 N1 -61.8(3) . . . . ? F2 C1 C2 C3 -122.9(2) . . . . ? F3 C1 C2 C3 -1.4(3) . . . . ? F1 C1 C2 C3 118.1(2) . . . . ? N1 C2 C3 C4 -2.2(5) . . . . ? C1 C2 C3 C4 177.9(3) . . . . ? C18 N2 C4 C3 179.4(3) . . . . ? Cu1 N2 C4 C3 -1.4(4) . . . . ? C18 N2 C4 C5 0.1(5) . . . . ? Cu1 N2 C4 C5 179.4(3) . . . . ? C2 C3 C4 N2 2.9(5) . . . . ? C2 C3 C4 C5 -177.9(4) . . . . ? C2 N1 C6 C11 95.9(2) . . . . ? Cu1 N1 C6 C11 -87.07(19) . . . . ? C2 N1 C6 C7 -90.6(2) . . . . ? Cu1 N1 C6 C7 86.39(18) . . . . ? C11 C6 C7 C8 -1.5(3) . . . . ? N1 C6 C7 C8 -174.86(17) . . . . ? C11 C6 C7 C12 176.7(2) . . . . ? N1 C6 C7 C12 3.3(3) . . . . ? C6 C7 C8 C9 -1.0(3) . . . . ? C12 C7 C8 C9 -179.2(2) . . . . ? C7 C8 C9 C10 2.0(4) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? C7 C6 C11 C10 2.9(3) . . . . ? N1 C6 C11 C10 176.14(19) . . . . ? C7 C6 C11 C15 -174.8(2) . . . . ? N1 C6 C11 C15 -1.5(3) . . . . ? C9 C10 C11 C6 -1.8(4) . . . . ? C9 C10 C11 C15 175.8(2) . . . . ? C8 C7 C12 C13 81.6(3) . . . . ? C6 C7 C12 C13 -96.5(2) . . . . ? C8 C7 C12 C14 -42.7(3) . . . . ? C6 C7 C12 C14 139.1(2) . . . . ? C6 C11 C15 C16 -132.4(3) . . . . ? C10 C11 C15 C16 50.1(3) . . . . ? C6 C11 C15 C17 104.0(3) . . . . ? C10 C11 C15 C17 -73.5(3) . . . . ? C4 N2 C18 C23 93.9(3) . . . . ? Cu1 N2 C18 C23 -85.3(2) . . . . ? C4 N2 C18 C19 -88.2(3) . . . . ? Cu1 N2 C18 C19 92.5(2) . . . . ? C23 C18 C19 C20 -2.8(3) . . . . ? N2 C18 C19 C20 179.41(18) . . . . ? C23 C18 C19 C24 173.9(2) . . . . ? N2 C18 C19 C24 -3.9(3) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C24 C19 C20 C21 -175.9(2) . . . . ? C19 C20 C21 C22 1.4(4) . . . . ? C20 C21 C22 C23 -1.7(4) . . . . ? C19 C18 C23 C22 2.5(3) . . . . ? N2 C18 C23 C22 -179.73(18) . . . . ? C19 C18 C23 C27 -174.6(2) . . . . ? N2 C18 C23 C27 3.2(3) . . . . ? C21 C22 C23 C18 -0.2(3) . . . . ? C21 C22 C23 C27 176.9(2) . . . . ? C20 C19 C24 C25 72.5(4) . . . . ? C18 C19 C24 C25 -104.2(3) . . . . ? C20 C19 C24 C26 -52.6(4) . . . . ? C18 C19 C24 C26 130.7(3) . . . . ? C18 C23 C27 C28 105.4(4) . . . . ? C22 C23 C27 C28 -71.6(4) . . . . ? C18 C23 C27 C29 -127.7(4) . . . . ? C22 C23 C27 C29 55.3(5) . . . . ? Cu1 N3 C30 C31 29(32) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.199 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.036 #====END data_03118 _database_code_depnum_ccdc_archive 'CCDC 614586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(L2)Cu(CH3CN)] ; _chemical_name_common ((L2)Cu(CH3CN)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 Cu F6 N3' _chemical_formula_weight 630.18 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8130(14) _cell_length_b 15.860(3) _cell_length_c 11.4149(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.702(3) _cell_angle_gamma 90.00 _cell_volume 1592.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1018 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7651 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details 'SADABS, R.Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18629 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7178 _reflns_number_gt 6507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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. Alerts produced by the checkCIF program (http://checkcif.iucr.org/) do not warrant explanation or adjustment of the structure solution. ; _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^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(7) _refine_ls_number_reflns 7178 _refine_ls_number_parameters 379 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Cu1 Cu 0.89903(2) 0.310352(14) 0.717099(16) 0.02764(6) Uani 1 1 d . . . F1 F 0.54199(13) 0.09097(7) 0.63067(9) 0.0412(3) Uani 1 1 d . . . F2 F 0.72428(14) 0.02511(7) 0.72428(11) 0.0422(3) Uani 1 1 d . . . F3 F 0.52997(14) 0.06375(7) 0.81364(10) 0.0409(3) Uani 1 1 d . . . F4 F 0.60033(16) 0.24341(8) 1.08847(10) 0.0464(3) Uani 1 1 d . . . F5 F 0.81958(13) 0.29902(11) 1.12138(9) 0.0521(3) Uani 1 1 d . . . F6 F 0.63039(16) 0.37456(8) 1.05901(11) 0.0466(3) Uani 1 1 d . . . N1 N 0.79410(16) 0.20436(9) 0.68627(12) 0.0243(3) Uani 1 1 d . . . N2 N 0.83030(15) 0.33351(8) 0.87147(12) 0.0243(3) Uani 1 1 d . . . N3 N 1.04019(19) 0.36491(11) 0.62792(14) 0.0377(4) Uani 1 1 d U . . C1 C 0.6244(2) 0.08830(12) 0.73303(16) 0.0298(4) Uani 1 1 d . . . C2 C 0.70471(18) 0.17248(10) 0.76253(14) 0.0229(3) Uani 1 1 d . . . C3 C 0.67571(19) 0.20735(11) 0.87171(14) 0.0247(3) Uani 1 1 d . . . H3 H 0.6067 0.1774 0.9170 0.030 Uiso 1 1 calc R . . C4 C 0.73755(19) 0.28152(11) 0.92119(14) 0.0239(3) Uani 1 1 d . . . C5 C 0.6968(2) 0.29956(13) 1.04793(15) 0.0318(4) Uani 1 1 d . . . C6 C 0.8310(2) 0.16365(11) 0.57877(15) 0.0294(4) Uani 1 1 d . . . C7 C 0.7505(2) 0.18608(12) 0.47335(16) 0.0348(4) Uani 1 1 d . . . C8 C 0.8018(3) 0.15335(15) 0.36934(18) 0.0488(6) Uani 1 1 d . . . H8 H 0.7478 0.1664 0.2969 0.059 Uiso 1 1 calc R . . C9 C 0.9287(3) 0.10269(16) 0.3692(2) 0.0573(7) Uani 1 1 d . . . H9 H 0.9622 0.0819 0.2973 0.069 Uiso 1 1 calc R . . C10 C 1.0066(3) 0.08228(14) 0.4732(2) 0.0497(6) Uani 1 1 d . . . H10 H 1.0936 0.0470 0.4722 0.060 Uiso 1 1 calc R . . C11 C 0.9611(2) 0.11205(12) 0.58082(17) 0.0365(4) Uani 1 1 d . . . C12 C 0.6179(2) 0.24727(12) 0.47006(16) 0.0342(4) Uani 1 1 d . . . H12 H 0.5886 0.2553 0.5525 0.041 Uiso 1 1 calc R . . C13 C 0.4786(3) 0.21530(16) 0.3979(2) 0.0542(6) Uani 1 1 d . . . H13A H 0.3941 0.2548 0.4049 0.081 Uiso 1 1 calc R . . H13B H 0.4499 0.1597 0.4269 0.081 Uiso 1 1 calc R . . H13C H 0.5018 0.2108 0.3153 0.081 Uiso 1 1 calc R . . C14 C 0.6696(3) 0.33306(13) 0.4248(2) 0.0464(5) Uani 1 1 d . . . H14A H 0.7513 0.3554 0.4783 0.070 Uiso 1 1 calc R . . H14B H 0.5836 0.3723 0.4208 0.070 Uiso 1 1 calc R . . H14C H 0.7070 0.3262 0.3463 0.070 Uiso 1 1 calc R . . C15 C 1.0536(2) 0.09281(14) 0.6941(2) 0.0428(5) Uani 1 1 d . . . H15 H 0.9856 0.1022 0.7598 0.051 Uiso 1 1 calc R . . C16 C 1.1872(3) 0.15309(19) 0.7133(3) 0.0748(9) Uani 1 1 d . . . H16A H 1.1495 0.2112 0.7151 0.112 Uiso 1 1 calc R . . H16B H 1.2551 0.1469 0.6492 0.112 Uiso 1 1 calc R . . H16C H 1.2431 0.1400 0.7881 0.112 Uiso 1 1 calc R . . C17 C 1.1097(4) 0.00195(17) 0.7036(3) 0.0676(8) Uani 1 1 d . . . H17A H 1.0244 -0.0365 0.6855 0.101 Uiso 1 1 calc R . . H17B H 1.1526 -0.0088 0.7835 0.101 Uiso 1 1 calc R . . H17C H 1.1880 -0.0072 0.6478 0.101 Uiso 1 1 calc R . . C18 C 0.8876(2) 0.41145(11) 0.92250(14) 0.0275(4) Uani 1 1 d . . . C19 C 0.8027(2) 0.48544(11) 0.90105(15) 0.0313(4) Uani 1 1 d . . . C20 C 0.8681(3) 0.56182(13) 0.93658(18) 0.0416(5) Uani 1 1 d . . . H20 H 0.8118 0.6125 0.9244 0.050 Uiso 1 1 calc R . . C21 C 1.0138(3) 0.56518(17) 0.9893(2) 0.0488(6) Uani 1 1 d . . . H21 H 1.0574 0.6180 1.0120 0.059 Uiso 1 1 calc R . . C22 C 1.0947(3) 0.49270(14) 1.00863(19) 0.0456(5) Uani 1 1 d . . . H22 H 1.1949 0.4959 1.0445 0.055 Uiso 1 1 calc R . . C23 C 1.0343(2) 0.41393(13) 0.97721(17) 0.0359(4) Uani 1 1 d . . . C24 C 0.6485(2) 0.48327(12) 0.83383(17) 0.0340(4) Uani 1 1 d . . . H24 H 0.6064 0.4251 0.8408 0.041 Uiso 1 1 calc R . . C25 C 0.5339(3) 0.54490(16) 0.8806(2) 0.0516(6) Uani 1 1 d . . . H25A H 0.4344 0.5364 0.8389 0.077 Uiso 1 1 calc R . . H25B H 0.5681 0.6028 0.8682 0.077 Uiso 1 1 calc R . . H25C H 0.5257 0.5351 0.9647 0.077 Uiso 1 1 calc R . . C26 C 0.6692(3) 0.50007(16) 0.70366(18) 0.0464(5) Uani 1 1 d . . . H26A H 0.7359 0.4569 0.6733 0.070 Uiso 1 1 calc R . . H26B H 0.7149 0.5558 0.6947 0.070 Uiso 1 1 calc R . . H26C H 0.5700 0.4982 0.6597 0.070 Uiso 1 1 calc R . . C27 C 1.1315(2) 0.33523(14) 0.99701(19) 0.0451(5) Uani 1 1 d . . . H27 H 1.0670 0.2853 0.9741 0.054 Uiso 1 1 calc R . . C28 C 1.1880(3) 0.32429(18) 1.1264(2) 0.0618(7) Uani 1 1 d . . . H28A H 1.2411 0.2702 1.1364 0.093 Uiso 1 1 calc R . . H28B H 1.1011 0.3254 1.1757 0.093 Uiso 1 1 calc R . . H28C H 1.2579 0.3703 1.1494 0.093 Uiso 1 1 calc R . . C29 C 1.2664(3) 0.3362(2) 0.9192(2) 0.0675(8) Uani 1 1 d . . . H29A H 1.3259 0.2844 0.9320 0.101 Uiso 1 1 calc R . . H29B H 1.3308 0.3851 0.9391 0.101 Uiso 1 1 calc R . . H29C H 1.2290 0.3395 0.8366 0.101 Uiso 1 1 calc R . . C30 C 1.1379(3) 0.39170(14) 0.5805(2) 0.0453(5) Uani 1 1 d U . . C31 C 1.2667(3) 0.4253(2) 0.5214(3) 0.0747(9) Uani 1 1 d U . . H31A H 1.2787 0.4854 0.5398 0.112 Uiso 1 1 calc R . . H31B H 1.2485 0.4182 0.4364 0.112 Uiso 1 1 calc R . . H31C H 1.3594 0.3950 0.5484 0.112 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 Cu1 0.03097(10) 0.02625(10) 0.02647(10) -0.00003(10) 0.00788(7) -0.00286(11) F1 0.0485(7) 0.0409(6) 0.0333(6) -0.0002(5) -0.0049(5) -0.0135(5) F2 0.0527(7) 0.0227(5) 0.0518(7) -0.0027(5) 0.0085(6) 0.0027(5) F3 0.0513(7) 0.0366(6) 0.0365(6) -0.0021(5) 0.0160(5) -0.0154(5) F4 0.0687(8) 0.0430(7) 0.0297(6) -0.0033(5) 0.0211(6) -0.0176(6) F5 0.0528(6) 0.0794(10) 0.0232(5) 0.0009(6) -0.0044(4) -0.0020(8) F6 0.0701(9) 0.0359(7) 0.0364(6) -0.0053(5) 0.0235(6) 0.0077(6) N1 0.0275(7) 0.0211(7) 0.0247(7) -0.0018(6) 0.0044(6) 0.0008(6) N2 0.0263(7) 0.0252(8) 0.0215(7) -0.0011(5) 0.0017(5) 0.0009(5) N3 0.0414(9) 0.0350(9) 0.0379(9) 0.0036(7) 0.0119(7) -0.0062(7) C1 0.0347(10) 0.0274(9) 0.0277(9) -0.0009(8) 0.0054(8) -0.0044(8) C2 0.0248(8) 0.0205(8) 0.0233(8) 0.0016(7) 0.0010(6) 0.0015(6) C3 0.0260(9) 0.0256(8) 0.0231(8) 0.0041(7) 0.0048(7) 0.0014(7) C4 0.0266(8) 0.0260(8) 0.0191(8) 0.0013(6) 0.0015(6) 0.0047(6) C5 0.0396(9) 0.0319(11) 0.0245(8) -0.0009(8) 0.0067(7) -0.0032(8) C6 0.0377(10) 0.0248(9) 0.0269(9) -0.0037(7) 0.0121(7) -0.0030(7) C7 0.0511(12) 0.0273(9) 0.0269(9) 0.0001(7) 0.0096(8) -0.0022(8) C8 0.0807(17) 0.0428(12) 0.0238(10) -0.0026(9) 0.0114(10) 0.0011(11) C9 0.089(2) 0.0491(14) 0.0370(13) -0.0059(11) 0.0310(13) 0.0097(13) C10 0.0603(14) 0.0407(13) 0.0512(14) -0.0044(10) 0.0279(12) 0.0094(11) C11 0.0421(11) 0.0289(10) 0.0403(11) -0.0001(8) 0.0160(9) 0.0026(8) C12 0.0478(12) 0.0305(10) 0.0240(9) 0.0009(8) 0.0008(8) -0.0006(9) C13 0.0628(15) 0.0496(13) 0.0479(13) 0.0000(11) -0.0134(11) -0.0090(12) C14 0.0571(13) 0.0362(13) 0.0460(12) 0.0079(9) 0.0046(10) -0.0006(9) C15 0.0380(11) 0.0418(11) 0.0497(12) -0.0008(10) 0.0100(9) 0.0124(9) C16 0.0494(15) 0.0591(17) 0.113(3) 0.0062(16) -0.0164(16) 0.0103(13) C17 0.083(2) 0.0476(15) 0.0729(18) 0.0057(13) 0.0072(15) 0.0230(14) C18 0.0344(9) 0.0264(9) 0.0222(8) -0.0018(7) 0.0040(7) -0.0039(7) C19 0.0414(10) 0.0276(9) 0.0254(9) -0.0006(7) 0.0055(7) -0.0011(8) C20 0.0604(14) 0.0263(10) 0.0382(11) -0.0004(8) 0.0028(10) -0.0030(9) C21 0.0685(15) 0.0346(11) 0.0425(12) -0.0068(9) -0.0023(11) -0.0177(10) C22 0.0456(12) 0.0496(13) 0.0401(11) -0.0066(10) -0.0079(9) -0.0152(10) C23 0.0396(11) 0.0369(10) 0.0305(10) -0.0026(8) -0.0023(8) -0.0046(9) C24 0.0375(10) 0.0297(10) 0.0352(10) 0.0014(8) 0.0050(8) 0.0045(8) C25 0.0541(14) 0.0480(14) 0.0542(14) -0.0006(11) 0.0136(11) 0.0175(11) C26 0.0467(13) 0.0564(14) 0.0357(11) 0.0025(10) -0.0002(9) 0.0107(11) C27 0.0362(11) 0.0450(13) 0.0520(12) -0.0080(9) -0.0135(9) 0.0027(8) C28 0.0610(14) 0.0604(19) 0.0607(14) 0.0049(13) -0.0203(11) 0.0057(13) C29 0.0440(13) 0.092(2) 0.0655(16) -0.0128(14) -0.0049(12) 0.0142(13) C30 0.0421(12) 0.0450(13) 0.0498(13) 0.0146(10) 0.0088(10) 0.0013(9) C31 0.0498(15) 0.0751(19) 0.103(2) 0.0347(17) 0.0343(15) -0.0014(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.8698(16) . ? Cu1 N2 1.9352(14) . ? Cu1 N1 1.9398(14) . ? F1 C1 1.336(2) . ? F2 C1 1.342(2) . ? F3 C1 1.338(2) . ? F4 C5 1.334(2) . ? F5 C5 1.325(2) . ? F6 C5 1.335(2) . ? N1 C2 1.313(2) . ? N1 C6 1.442(2) . ? N2 C4 1.315(2) . ? N2 C18 1.444(2) . ? N3 C30 1.129(3) . ? C1 C2 1.538(2) . ? C2 C3 1.402(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9500 . ? C4 C5 1.540(2) . ? C6 C7 1.403(3) . ? C6 C11 1.408(3) . ? C7 C8 1.397(3) . ? C7 C12 1.518(3) . ? C8 C9 1.377(3) . ? C8 H8 0.9500 . ? C9 C10 1.371(4) . ? C9 H9 0.9500 . ? C10 C11 1.398(3) . ? C10 H10 0.9500 . ? C11 C15 1.515(3) . ? C12 C13 1.521(3) . ? C12 C14 1.535(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(4) . ? C15 C17 1.525(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.400(3) . ? C18 C19 1.405(3) . ? C19 C20 1.391(3) . ? C19 C24 1.517(3) . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.363(4) . ? C21 H21 0.9500 . ? C22 C23 1.396(3) . ? C22 H22 0.9500 . ? C23 C27 1.522(3) . ? C24 C25 1.526(3) . ? C24 C26 1.532(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.530(3) . ? C27 C28 1.537(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.458(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 131.78(7) . . ? N3 Cu1 N1 128.93(7) . . ? N2 Cu1 N1 98.98(6) . . ? C2 N1 C6 124.74(14) . . ? C2 N1 Cu1 120.87(11) . . ? C6 N1 Cu1 114.28(11) . . ? C4 N2 C18 125.00(14) . . ? C4 N2 Cu1 120.91(11) . . ? C18 N2 Cu1 114.08(11) . . ? C30 N3 Cu1 171.81(18) . . ? F1 C1 F3 106.47(15) . . ? F1 C1 F2 106.30(14) . . ? F3 C1 F2 105.90(15) . . ? F1 C1 C2 112.36(15) . . ? F3 C1 C2 113.57(15) . . ? F2 C1 C2 111.70(14) . . ? N1 C2 C3 126.11(15) . . ? N1 C2 C1 118.46(15) . . ? C3 C2 C1 115.42(14) . . ? C4 C3 C2 126.98(16) . . ? C4 C3 H3 116.5 . . ? C2 C3 H3 116.5 . . ? N2 C4 C3 126.10(15) . . ? N2 C4 C5 118.56(15) . . ? C3 C4 C5 115.26(15) . . ? F5 C5 F4 106.78(16) . . ? F5 C5 F6 106.90(17) . . ? F4 C5 F6 105.58(15) . . ? F5 C5 C4 111.27(14) . . ? F4 C5 C4 113.22(16) . . ? F6 C5 C4 112.63(15) . . ? C7 C6 C11 121.87(16) . . ? C7 C6 N1 119.14(16) . . ? C11 C6 N1 118.32(16) . . ? C8 C7 C6 117.47(19) . . ? C8 C7 C12 120.48(19) . . ? C6 C7 C12 121.97(16) . . ? C9 C8 C7 121.6(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.87(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.7(2) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 117.45(19) . . ? C10 C11 C15 120.87(19) . . ? C6 C11 C15 121.61(17) . . ? C7 C12 C13 113.19(18) . . ? C7 C12 C14 109.28(17) . . ? C13 C12 C14 111.10(17) . . ? C7 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.4(2) . . ? C11 C15 C17 113.9(2) . . ? C16 C15 C17 109.8(2) . . ? C11 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.38(17) . . ? C23 C18 N2 119.54(16) . . ? C19 C18 N2 118.45(15) . . ? C20 C19 C18 118.06(18) . . ? C20 C19 C24 120.55(17) . . ? C18 C19 C24 121.26(16) . . ? C21 C20 C19 121.1(2) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.9(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.7(2) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C18 117.77(19) . . ? C22 C23 C27 119.61(18) . . ? C18 C23 C27 122.53(17) . . ? C19 C24 C25 113.55(17) . . ? C19 C24 C26 109.14(16) . . ? C25 C24 C26 110.54(17) . . ? C19 C24 H24 107.8 . . ? C25 C24 H24 107.8 . . ? C26 C24 H24 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.9(2) . . ? C23 C27 C28 112.31(18) . . ? C29 C27 C28 110.05(19) . . ? C23 C27 H27 107.8 . . ? C29 C27 H27 107.8 . . ? C28 C27 H27 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 178.6(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 C2 175.80(13) . . . . ? N2 Cu1 N1 C2 1.62(14) . . . . ? N3 Cu1 N1 C6 -0.59(15) . . . . ? N2 Cu1 N1 C6 -174.77(12) . . . . ? N3 Cu1 N2 C4 -174.28(12) . . . . ? N1 Cu1 N2 C4 -0.36(13) . . . . ? N3 Cu1 N2 C18 6.74(16) . . . . ? N1 Cu1 N2 C18 -179.34(11) . . . . ? N2 Cu1 N3 C30 89.2(14) . . . . ? N1 Cu1 N3 C30 -83.1(14) . . . . ? C6 N1 C2 C3 174.85(16) . . . . ? Cu1 N1 C2 C3 -1.1(2) . . . . ? C6 N1 C2 C1 -4.1(2) . . . . ? Cu1 N1 C2 C1 179.89(11) . . . . ? F1 C1 C2 N1 -55.7(2) . . . . ? F3 C1 C2 N1 -176.66(15) . . . . ? F2 C1 C2 N1 63.6(2) . . . . ? F1 C1 C2 C3 125.21(16) . . . . ? F3 C1 C2 C3 4.3(2) . . . . ? F2 C1 C2 C3 -115.42(17) . . . . ? N1 C2 C3 C4 -1.1(3) . . . . ? C1 C2 C3 C4 177.90(16) . . . . ? C18 N2 C4 C3 177.32(16) . . . . ? Cu1 N2 C4 C3 -1.5(2) . . . . ? C18 N2 C4 C5 -5.9(2) . . . . ? Cu1 N2 C4 C5 175.22(12) . . . . ? C2 C3 C4 N2 2.7(3) . . . . ? C2 C3 C4 C5 -174.20(16) . . . . ? N2 C4 C5 F5 -60.6(2) . . . . ? C3 C4 C5 F5 116.47(18) . . . . ? N2 C4 C5 F4 179.07(15) . . . . ? C3 C4 C5 F4 -3.8(2) . . . . ? N2 C4 C5 F6 59.4(2) . . . . ? C3 C4 C5 F6 -123.52(17) . . . . ? C2 N1 C6 C7 97.8(2) . . . . ? Cu1 N1 C6 C7 -85.99(18) . . . . ? C2 N1 C6 C11 -91.4(2) . . . . ? Cu1 N1 C6 C11 84.82(17) . . . . ? C11 C6 C7 C8 1.7(3) . . . . ? N1 C6 C7 C8 172.15(17) . . . . ? C11 C6 C7 C12 -175.01(17) . . . . ? N1 C6 C7 C12 -4.5(3) . . . . ? C6 C7 C8 C9 -1.6(3) . . . . ? C12 C7 C8 C9 175.1(2) . . . . ? C7 C8 C9 C10 1.0(4) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C9 C10 C11 C6 0.4(3) . . . . ? C9 C10 C11 C15 -176.6(2) . . . . ? C7 C6 C11 C10 -1.1(3) . . . . ? N1 C6 C11 C10 -171.65(17) . . . . ? C7 C6 C11 C15 175.86(18) . . . . ? N1 C6 C11 C15 5.3(3) . . . . ? C8 C7 C12 C13 51.8(3) . . . . ? C6 C7 C12 C13 -131.6(2) . . . . ? C8 C7 C12 C14 -72.6(2) . . . . ? C6 C7 C12 C14 104.0(2) . . . . ? C10 C11 C15 C16 82.0(3) . . . . ? C6 C11 C15 C16 -94.9(2) . . . . ? C10 C11 C15 C17 -42.9(3) . . . . ? C6 C11 C15 C17 140.2(2) . . . . ? C4 N2 C18 C23 100.0(2) . . . . ? Cu1 N2 C18 C23 -81.02(17) . . . . ? C4 N2 C18 C19 -88.9(2) . . . . ? Cu1 N2 C18 C19 90.00(17) . . . . ? C23 C18 C19 C20 -0.5(3) . . . . ? N2 C18 C19 C20 -171.30(16) . . . . ? C23 C18 C19 C24 175.45(17) . . . . ? N2 C18 C19 C24 4.6(3) . . . . ? C18 C19 C20 C21 1.3(3) . . . . ? C24 C19 C20 C21 -174.6(2) . . . . ? C19 C20 C21 C22 -0.9(4) . . . . ? C20 C21 C22 C23 -0.4(4) . . . . ? C21 C22 C23 C18 1.2(3) . . . . ? C21 C22 C23 C27 177.9(2) . . . . ? C19 C18 C23 C22 -0.8(3) . . . . ? N2 C18 C23 C22 169.95(17) . . . . ? C19 C18 C23 C27 -177.40(18) . . . . ? N2 C18 C23 C27 -6.7(3) . . . . ? C20 C19 C24 C25 -41.5(3) . . . . ? C18 C19 C24 C25 142.74(19) . . . . ? C20 C19 C24 C26 82.3(2) . . . . ? C18 C19 C24 C26 -93.5(2) . . . . ? C22 C23 C27 C29 -65.7(3) . . . . ? C18 C23 C27 C29 110.8(2) . . . . ? C22 C23 C27 C28 57.8(3) . . . . ? C18 C23 C27 C28 -125.6(2) . . . . ? Cu1 N3 C30 C31 -15(13) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.346 _refine_diff_density_min -0.148 _refine_diff_density_rms 0.040 #====END data_06199m _database_code_depnum_ccdc_archive 'CCDC 617543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common LCu(CO) _chemical_melting_point ? _chemical_formula_moiety 'C30 H41 Cu N2 O' _chemical_formula_sum 'C30 H41 Cu N2 O' _chemical_formula_weight 509.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 30.688(5) _cell_length_b 9.7321(15) _cell_length_c 39.461(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.026(3) _cell_angle_gamma 90.00 _cell_volume 11720(3) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3632 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6156 _exptl_absorpt_correction_T_max 0.7488 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99731 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 25.05 _reflns_number_total 20760 _reflns_number_gt 15502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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. Four molecules of the complex (A-D) occupy the asymmetric unit. Therefore, Z = 16 and Z' = 4. CheckCIF alerts (http://checkcif.iucr.org/) for O1 positions are due to the terminal nature of the CO ligands. In the case of O1D, this atom points into a hydrophobic cavity, with no observable interaction with H-atoms. Likewise, large Ueq(max)/Ueq(min) ratios for C and H atoms are due to the terminal methyl groups of iso-propyl substituents on the phenyl rings. No further modifications of refinement parameters can be made to alleviate alerts for the CO and the iso-propyl methyl groups. ; _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^)+(0.0299P)^2^+11.2071P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20760 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Cu1A Cu 0.593773(12) -0.34753(4) 0.213406(10) 0.03413(10) Uani 1 1 d . . . O1A O 0.55434(10) -0.6133(3) 0.19572(7) 0.0708(8) Uani 1 1 d . . . N1A N 0.62801(8) -0.3185(3) 0.25641(6) 0.0332(6) Uani 1 1 d . . . N2A N 0.59753(8) -0.1674(3) 0.19426(6) 0.0305(6) Uani 1 1 d . . . C1A C 0.67024(11) -0.1769(4) 0.29970(8) 0.0507(9) Uani 1 1 d . . . H1AA H 0.6528 -0.2046 0.3180 0.076 Uiso 1 1 calc R . . H1AB H 0.6788 -0.0802 0.3027 0.076 Uiso 1 1 calc R . . H1AC H 0.6966 -0.2342 0.3004 0.076 Uiso 1 1 calc R . . C2A C 0.64333(10) -0.1947(3) 0.26570(8) 0.0349(8) Uani 1 1 d . . . C3A C 0.63630(10) -0.0763(3) 0.24545(7) 0.0343(7) Uani 1 1 d . . . H3AA H 0.6467 0.0071 0.2559 0.041 Uiso 1 1 calc R . . C4A C 0.61632(10) -0.0640(3) 0.21232(7) 0.0311(7) Uani 1 1 d . . . C5A C 0.61755(12) 0.0771(3) 0.19606(8) 0.0434(8) Uani 1 1 d . . . H5AA H 0.5879 0.1036 0.1868 0.065 Uiso 1 1 calc R . . H5AB H 0.6366 0.0744 0.1776 0.065 Uiso 1 1 calc R . . H5AC H 0.6290 0.1442 0.2133 0.065 Uiso 1 1 calc R . . C6A C 0.63895(11) -0.4325(3) 0.27871(8) 0.0413(8) Uani 1 1 d . . . C7A C 0.67634(12) -0.5106(4) 0.27432(11) 0.0605(11) Uani 1 1 d . . . C8A C 0.68605(14) -0.6226(5) 0.29531(13) 0.0787(14) Uani 1 1 d . . . H8AA H 0.7113 -0.6763 0.2925 0.094 Uiso 1 1 calc R . . C9A C 0.66006(15) -0.6573(5) 0.31985(12) 0.0777(14) Uani 1 1 d . . . H9AA H 0.6674 -0.7342 0.3341 0.093 Uiso 1 1 calc R . . C10A C 0.62323(14) -0.5816(4) 0.32406(10) 0.0648(12) Uani 1 1 d . . . H10A H 0.6052 -0.6077 0.3412 0.078 Uiso 1 1 calc R . . C11A C 0.61165(11) -0.4672(4) 0.30374(8) 0.0453(9) Uani 1 1 d . . . C12A C 0.70533(14) -0.4756(5) 0.24649(15) 0.0887(17) Uani 1 1 d . . . H12A H 0.6964 -0.3828 0.2373 0.106 Uiso 1 1 calc R . . C13A C 0.69925(18) -0.5765(7) 0.21734(15) 0.116(2) Uani 1 1 d . . . H13A H 0.6681 -0.5822 0.2089 0.173 Uiso 1 1 calc R . . H13B H 0.7098 -0.6673 0.2253 0.173 Uiso 1 1 calc R . . H13C H 0.7159 -0.5456 0.1989 0.173 Uiso 1 1 calc R . . C14A C 0.75383(16) -0.4676(7) 0.26077(19) 0.141(3) Uani 1 1 d . . . H14A H 0.7568 -0.4093 0.2811 0.212 Uiso 1 1 calc R . . H14B H 0.7709 -0.4283 0.2435 0.212 Uiso 1 1 calc R . . H14C H 0.7647 -0.5600 0.2668 0.212 Uiso 1 1 calc R . . C15A C 0.57014(12) -0.3870(4) 0.30777(9) 0.0506(10) Uani 1 1 d . . . H15A H 0.5713 -0.3004 0.2942 0.061 Uiso 1 1 calc R . . C16A C 0.52993(12) -0.4675(4) 0.29298(11) 0.0630(11) Uani 1 1 d . . . H16A H 0.5316 -0.4837 0.2686 0.095 Uiso 1 1 calc R . . H16B H 0.5034 -0.4147 0.2960 0.095 Uiso 1 1 calc R . . H16C H 0.5289 -0.5557 0.3048 0.095 Uiso 1 1 calc R . . C17A C 0.56546(16) -0.3463(5) 0.34451(10) 0.0826(14) Uani 1 1 d . . . H17A H 0.5926 -0.3028 0.3545 0.124 Uiso 1 1 calc R . . H17B H 0.5597 -0.4285 0.3577 0.124 Uiso 1 1 calc R . . H17C H 0.5411 -0.2815 0.3450 0.124 Uiso 1 1 calc R . . C18A C 0.58282(10) -0.1439(3) 0.15885(7) 0.0328(7) Uani 1 1 d . . . C19A C 0.61299(10) -0.1572(3) 0.13469(8) 0.0384(8) Uani 1 1 d . . . C20A C 0.59805(12) -0.1394(4) 0.10044(8) 0.0482(9) Uani 1 1 d . . . H20A H 0.6180 -0.1487 0.0837 0.058 Uiso 1 1 calc R . . C21A C 0.55504(13) -0.1087(4) 0.09044(9) 0.0526(10) Uani 1 1 d . . . H21A H 0.5455 -0.0967 0.0669 0.063 Uiso 1 1 calc R . . C22A C 0.52577(12) -0.0952(4) 0.11410(9) 0.0482(9) Uani 1 1 d . . . H22A H 0.4960 -0.0741 0.1068 0.058 Uiso 1 1 calc R . . C23A C 0.53886(10) -0.1118(3) 0.14886(8) 0.0389(8) Uani 1 1 d . . . C24A C 0.66063(11) -0.1935(4) 0.14489(9) 0.0501(9) Uani 1 1 d . . . H24A H 0.6666 -0.1791 0.1700 0.060 Uiso 1 1 calc R . . C25A C 0.66927(14) -0.3437(5) 0.13779(12) 0.0813(14) Uani 1 1 d . . . H25A H 0.6503 -0.4013 0.1503 0.122 Uiso 1 1 calc R . . H25B H 0.7000 -0.3652 0.1451 0.122 Uiso 1 1 calc R . . H25C H 0.6631 -0.3615 0.1133 0.122 Uiso 1 1 calc R . . C26A C 0.69273(13) -0.1028(5) 0.12768(11) 0.0776(13) Uani 1 1 d . . . H26A H 0.6863 -0.0058 0.1317 0.116 Uiso 1 1 calc R . . H26B H 0.6896 -0.1209 0.1031 0.116 Uiso 1 1 calc R . . H26C H 0.7228 -0.1236 0.1372 0.116 Uiso 1 1 calc R . . C27A C 0.50593(11) -0.0969(4) 0.17470(10) 0.0520(10) Uani 1 1 d . . . H27A H 0.5225 -0.0986 0.1979 0.062 Uiso 1 1 calc R . . C28A C 0.48101(15) 0.0390(5) 0.17108(13) 0.0844(15) Uani 1 1 d . . . H28A H 0.5019 0.1153 0.1720 0.127 Uiso 1 1 calc R . . H28B H 0.4625 0.0482 0.1897 0.127 Uiso 1 1 calc R . . H28C H 0.4626 0.0408 0.1492 0.127 Uiso 1 1 calc R . . C29A C 0.47397(15) -0.2156(5) 0.17262(14) 0.0930(16) Uani 1 1 d . . . H29A H 0.4902 -0.3025 0.1747 0.140 Uiso 1 1 calc R . . H29B H 0.4558 -0.2130 0.1507 0.140 Uiso 1 1 calc R . . H29C H 0.4552 -0.2083 0.1911 0.140 Uiso 1 1 calc R . . C30A C 0.56896(12) -0.5083(4) 0.20116(9) 0.0464(9) Uani 1 1 d . . . Cu1B Cu 0.513390(12) 0.11054(4) 0.394017(9) 0.02884(9) Uani 1 1 d . . . O1B O 0.54800(9) -0.1550(3) 0.41704(7) 0.0622(7) Uani 1 1 d . . . N1B N 0.47827(8) 0.1558(2) 0.35259(6) 0.0302(6) Uani 1 1 d . . . N2B N 0.51483(8) 0.2880(2) 0.41524(6) 0.0286(6) Uani 1 1 d . . . C1B C 0.43349(11) 0.3079(3) 0.31349(8) 0.0466(9) Uani 1 1 d . . . H1BA H 0.4075 0.2488 0.3124 0.070 Uiso 1 1 calc R . . H1BB H 0.4500 0.2878 0.2941 0.070 Uiso 1 1 calc R . . H1BC H 0.4244 0.4044 0.3127 0.070 Uiso 1 1 calc R . . C2B C 0.46197(10) 0.2811(3) 0.34618(7) 0.0303(7) Uani 1 1 d . . . C3B C 0.47029(10) 0.3919(3) 0.36855(8) 0.0327(7) Uani 1 1 d . . . H3BA H 0.4577 0.4769 0.3608 0.039 Uiso 1 1 calc R . . C4B C 0.49442(9) 0.3958(3) 0.40064(8) 0.0298(7) Uani 1 1 d . . . C5B C 0.49701(12) 0.5319(3) 0.41916(8) 0.0432(8) Uani 1 1 d . . . H5BA H 0.5278 0.5589 0.4242 0.065 Uiso 1 1 calc R . . H5BB H 0.4836 0.5230 0.4405 0.065 Uiso 1 1 calc R . . H5BC H 0.4813 0.6020 0.4048 0.065 Uiso 1 1 calc R . . C6B C 0.46869(11) 0.0484(3) 0.32799(8) 0.0375(8) Uani 1 1 d . . . C7B C 0.43297(12) -0.0390(3) 0.33135(10) 0.0489(10) Uani 1 1 d . . . C8B C 0.42608(15) -0.1474(4) 0.30848(12) 0.0692(13) Uani 1 1 d . . . H8BA H 0.4022 -0.2082 0.3102 0.083 Uiso 1 1 calc R . . C9B C 0.45328(17) -0.1681(4) 0.28332(12) 0.0794(15) Uani 1 1 d . . . H9BA H 0.4478 -0.2424 0.2678 0.095 Uiso 1 1 calc R . . C10B C 0.48809(15) -0.0824(4) 0.28044(10) 0.0665(12) Uani 1 1 d . . . H10B H 0.5066 -0.0982 0.2630 0.080 Uiso 1 1 calc R . . C11B C 0.49686(12) 0.0278(3) 0.30279(9) 0.0460(9) Uani 1 1 d . . . C12B C 0.40368(12) -0.0197(4) 0.35937(10) 0.0581(11) Uani 1 1 d . . . H12B H 0.4107 0.0721 0.3700 0.070 Uiso 1 1 calc R . . C13B C 0.41279(14) -0.1288(5) 0.38731(12) 0.0880(16) Uani 1 1 d . . . H13D H 0.4432 -0.1205 0.3976 0.132 Uiso 1 1 calc R . . H13E H 0.4081 -0.2205 0.3773 0.132 Uiso 1 1 calc R . . H13F H 0.3929 -0.1150 0.4049 0.132 Uiso 1 1 calc R . . C14B C 0.35476(13) -0.0198(5) 0.34625(12) 0.0805(14) Uani 1 1 d . . . H14D H 0.3490 0.0521 0.3290 0.121 Uiso 1 1 calc R . . H14E H 0.3374 -0.0021 0.3653 0.121 Uiso 1 1 calc R . . H14F H 0.3467 -0.1094 0.3361 0.121 Uiso 1 1 calc R . . C15B C 0.53690(12) 0.1171(4) 0.30110(9) 0.0503(9) Uani 1 1 d . . . H15B H 0.5324 0.2033 0.3141 0.060 Uiso 1 1 calc R . . C16B C 0.57719(12) 0.0448(4) 0.31872(9) 0.0567(10) Uani 1 1 d . . . H16D H 0.5724 0.0241 0.3424 0.085 Uiso 1 1 calc R . . H16E H 0.6028 0.1047 0.3184 0.085 Uiso 1 1 calc R . . H16F H 0.5822 -0.0409 0.3067 0.085 Uiso 1 1 calc R . . C17B C 0.54511(15) 0.1589(5) 0.26469(9) 0.0742(13) Uani 1 1 d . . . H17D H 0.5187 0.2023 0.2533 0.111 Uiso 1 1 calc R . . H17E H 0.5522 0.0770 0.2519 0.111 Uiso 1 1 calc R . . H17F H 0.5696 0.2238 0.2657 0.111 Uiso 1 1 calc R . . C18B C 0.53583(10) 0.2956(3) 0.44956(7) 0.0298(7) Uani 1 1 d . . . C19B C 0.51097(10) 0.2709(3) 0.47695(8) 0.0336(7) Uani 1 1 d . . . C20B C 0.53300(12) 0.2614(3) 0.50943(8) 0.0419(8) Uani 1 1 d . . . H20B H 0.5168 0.2439 0.5282 0.050 Uiso 1 1 calc R . . C21B C 0.57780(13) 0.2768(3) 0.51497(9) 0.0476(9) Uani 1 1 d . . . H21B H 0.5923 0.2681 0.5373 0.057 Uiso 1 1 calc R . . C22B C 0.60142(11) 0.3046(3) 0.48817(8) 0.0423(8) Uani 1 1 d . . . H22B H 0.6322 0.3166 0.4923 0.051 Uiso 1 1 calc R . . C23B C 0.58139(10) 0.3157(3) 0.45511(7) 0.0312(7) Uani 1 1 d . . . C24B C 0.46152(11) 0.2511(3) 0.47077(9) 0.0422(8) Uani 1 1 d . . . H24B H 0.4518 0.2831 0.4471 0.051 Uiso 1 1 calc R . . C25B C 0.43697(12) 0.3363(4) 0.49532(10) 0.0548(10) Uani 1 1 d . . . H25D H 0.4465 0.4323 0.4947 0.082 Uiso 1 1 calc R . . H25E H 0.4433 0.3001 0.5185 0.082 Uiso 1 1 calc R . . H25F H 0.4054 0.3309 0.4884 0.082 Uiso 1 1 calc R . . C26B C 0.44956(13) 0.0994(4) 0.47298(12) 0.0673(12) Uani 1 1 d . . . H26D H 0.4645 0.0470 0.4564 0.101 Uiso 1 1 calc R . . H26E H 0.4178 0.0885 0.4679 0.101 Uiso 1 1 calc R . . H26F H 0.4587 0.0653 0.4960 0.101 Uiso 1 1 calc R . . C27B C 0.60817(10) 0.3446(3) 0.42549(8) 0.0417(8) Uani 1 1 d . . . H27B H 0.5872 0.3694 0.4053 0.050 Uiso 1 1 calc R . . C28B C 0.63316(12) 0.2170(4) 0.41627(10) 0.0619(11) Uani 1 1 d . . . H28D H 0.6123 0.1439 0.4089 0.093 Uiso 1 1 calc R . . H28E H 0.6523 0.1860 0.4362 0.093 Uiso 1 1 calc R . . H28F H 0.6509 0.2390 0.3978 0.093 Uiso 1 1 calc R . . C29B C 0.63981(15) 0.4650(4) 0.43254(11) 0.0797(14) Uani 1 1 d . . . H29D H 0.6233 0.5480 0.4370 0.119 Uiso 1 1 calc R . . H29E H 0.6558 0.4803 0.4127 0.119 Uiso 1 1 calc R . . H29F H 0.6606 0.4440 0.4524 0.119 Uiso 1 1 calc R . . C30B C 0.53514(10) -0.0506(3) 0.40812(8) 0.0356(7) Uani 1 1 d . . . Cu1C Cu 0.286894(13) 0.25788(4) 0.159133(10) 0.03436(10) Uani 1 1 d . . . O1C O 0.25185(9) 0.5252(3) 0.13817(6) 0.0577(7) Uani 1 1 d . . . N1C N 0.32170(8) 0.2156(3) 0.20117(6) 0.0337(6) Uani 1 1 d . . . N2C N 0.29112(9) 0.0852(3) 0.13629(6) 0.0372(6) Uani 1 1 d . . . C1C C 0.36876(11) 0.0682(4) 0.23997(8) 0.0482(9) Uani 1 1 d . . . H1CA H 0.3523 0.0905 0.2593 0.072 Uiso 1 1 calc R . . H1CB H 0.3950 0.1262 0.2408 0.072 Uiso 1 1 calc R . . H1CC H 0.3775 -0.0287 0.2413 0.072 Uiso 1 1 calc R . . C2C C 0.34031(10) 0.0936(3) 0.20710(8) 0.0363(8) Uani 1 1 d . . . C3C C 0.33529(10) -0.0161(3) 0.18375(8) 0.0384(8) Uani 1 1 d . . . H3CA H 0.3485 -0.1001 0.1916 0.046 Uiso 1 1 calc R . . C4C C 0.31376(11) -0.0200(3) 0.15077(8) 0.0383(8) Uani 1 1 d . . . C5C C 0.31700(13) -0.1523(3) 0.13101(9) 0.0556(10) Uani 1 1 d . . . H5CA H 0.3290 -0.1328 0.1095 0.083 Uiso 1 1 calc R . . H5CB H 0.2878 -0.1930 0.1263 0.083 Uiso 1 1 calc R . . H5CC H 0.3363 -0.2168 0.1445 0.083 Uiso 1 1 calc R . . C6C C 0.33096(11) 0.3240(3) 0.22570(8) 0.0388(8) Uani 1 1 d . . . C7C C 0.30282(11) 0.3450(3) 0.25121(8) 0.0411(8) Uani 1 1 d . . . C8C C 0.31247(13) 0.4527(4) 0.27388(10) 0.0559(10) Uani 1 1 d . . . H8CA H 0.2941 0.4688 0.2914 0.067 Uiso 1 1 calc R . . C9C C 0.34816(15) 0.5366(4) 0.27144(12) 0.0681(13) Uani 1 1 d . . . H9CA H 0.3542 0.6093 0.2873 0.082 Uiso 1 1 calc R . . C10C C 0.37493(14) 0.5159(4) 0.24624(12) 0.0662(12) Uani 1 1 d . . . H10C H 0.3992 0.5754 0.2448 0.079 Uiso 1 1 calc R . . C11C C 0.36742(12) 0.4096(4) 0.22259(10) 0.0514(10) Uani 1 1 d . . . C12C C 0.26194(11) 0.2601(3) 0.25280(8) 0.0422(8) Uani 1 1 d . . . H12C H 0.2648 0.1758 0.2387 0.051 Uiso 1 1 calc R . . C13C C 0.25433(14) 0.2138(4) 0.28889(9) 0.0639(11) Uani 1 1 d . . . H13G H 0.2805 0.1662 0.2994 0.096 Uiso 1 1 calc R . . H13H H 0.2292 0.1514 0.2877 0.096 Uiso 1 1 calc R . . H13I H 0.2485 0.2943 0.3026 0.096 Uiso 1 1 calc R . . C14C C 0.22230(12) 0.3402(4) 0.23694(10) 0.0560(10) Uani 1 1 d . . . H14G H 0.2258 0.3598 0.2130 0.084 Uiso 1 1 calc R . . H14H H 0.2199 0.4267 0.2493 0.084 Uiso 1 1 calc R . . H14I H 0.1957 0.2854 0.2383 0.084 Uiso 1 1 calc R . . C15C C 0.39653(12) 0.3905(5) 0.19460(11) 0.0651(12) Uani 1 1 d . . . H15C H 0.3897 0.2985 0.1841 0.078 Uiso 1 1 calc R . . C16C C 0.38700(14) 0.4992(6) 0.16653(12) 0.0962(18) Uani 1 1 d . . . H16G H 0.3564 0.4912 0.1567 0.144 Uiso 1 1 calc R . . H16H H 0.4065 0.4847 0.1487 0.144 Uiso 1 1 calc R . . H16I H 0.3920 0.5911 0.1763 0.144 Uiso 1 1 calc R . . C17C C 0.44580(13) 0.3927(5) 0.20731(13) 0.0892(16) Uani 1 1 d . . . H17G H 0.4521 0.3214 0.2247 0.134 Uiso 1 1 calc R . . H17H H 0.4537 0.4828 0.2172 0.134 Uiso 1 1 calc R . . H17I H 0.4629 0.3751 0.1881 0.134 Uiso 1 1 calc R . . C18C C 0.27335(12) 0.0729(3) 0.10136(8) 0.0388(8) Uani 1 1 d . . . C19C C 0.23111(12) 0.0180(3) 0.09320(8) 0.0411(8) Uani 1 1 d . . . C20C C 0.21472(13) 0.0100(4) 0.05911(9) 0.0517(9) Uani 1 1 d . . . H20C H 0.1863 -0.0270 0.0531 0.062 Uiso 1 1 calc R . . C21C C 0.23914(15) 0.0552(4) 0.03373(9) 0.0616(11) Uani 1 1 d . . . H21C H 0.2277 0.0471 0.0105 0.074 Uiso 1 1 calc R . . C22C C 0.27986(14) 0.1117(4) 0.04197(9) 0.0579(10) Uani 1 1 d . . . H22C H 0.2960 0.1442 0.0243 0.069 Uiso 1 1 calc R . . C23C C 0.29790(12) 0.1221(3) 0.07571(9) 0.0465(9) Uani 1 1 d . . . C24C C 0.20338(12) -0.0268(4) 0.12073(9) 0.0500(9) Uani 1 1 d . . . H24C H 0.2235 -0.0399 0.1421 0.060 Uiso 1 1 calc R . . C25C C 0.17928(16) -0.1623(4) 0.11321(12) 0.0802(14) Uani 1 1 d . . . H25G H 0.2004 -0.2339 0.1087 0.120 Uiso 1 1 calc R . . H25H H 0.1578 -0.1513 0.0932 0.120 Uiso 1 1 calc R . . H25I H 0.1641 -0.1888 0.1329 0.120 Uiso 1 1 calc R . . C26C C 0.17115(16) 0.0856(5) 0.12753(13) 0.0856(15) Uani 1 1 d . . . H26G H 0.1873 0.1694 0.1348 0.128 Uiso 1 1 calc R . . H26H H 0.1536 0.0559 0.1455 0.128 Uiso 1 1 calc R . . H26I H 0.1518 0.1043 0.1067 0.128 Uiso 1 1 calc R . . C27C C 0.34274(12) 0.1878(4) 0.08436(10) 0.0558(10) Uani 1 1 d . . . H27C H 0.3508 0.1798 0.1095 0.067 Uiso 1 1 calc R . . C28C C 0.37824(17) 0.1192(6) 0.06648(17) 0.122(2) Uani 1 1 d . . . H28G H 0.3810 0.0229 0.0736 0.183 Uiso 1 1 calc R . . H28H H 0.4062 0.1666 0.0725 0.183 Uiso 1 1 calc R . . H28I H 0.3705 0.1236 0.0418 0.183 Uiso 1 1 calc R . . C29C C 0.34210(14) 0.3391(4) 0.07496(12) 0.0769(13) Uani 1 1 d . . . H29G H 0.3186 0.3854 0.0855 0.115 Uiso 1 1 calc R . . H29H H 0.3371 0.3487 0.0501 0.115 Uiso 1 1 calc R . . H29I H 0.3703 0.3809 0.0832 0.115 Uiso 1 1 calc R . . C30C C 0.26385(11) 0.4201(4) 0.14603(8) 0.0381(8) Uani 1 1 d . . . Cu1D Cu 0.178071(12) 0.16340(4) 0.528119(11) 0.03748(11) Uani 1 1 d . . . O1D O 0.18084(13) 0.4603(3) 0.53014(10) 0.1061(12) Uani 1 1 d . . . N1D N 0.12548(8) 0.0552(3) 0.52525(6) 0.0338(6) Uani 1 1 d . . . N2D N 0.21973(8) 0.0168(2) 0.53300(6) 0.0302(6) Uani 1 1 d . . . C1D C 0.08270(10) -0.1574(3) 0.52181(8) 0.0413(8) Uani 1 1 d . . . H1DA H 0.0661 -0.1308 0.5002 0.062 Uiso 1 1 calc R . . H1DB H 0.0658 -0.1343 0.5408 0.062 Uiso 1 1 calc R . . H1DC H 0.0882 -0.2565 0.5218 0.062 Uiso 1 1 calc R . . C2D C 0.12580(10) -0.0812(3) 0.52594(7) 0.0301(7) Uani 1 1 d . . . C3D C 0.16434(10) -0.1587(3) 0.53045(7) 0.0316(7) Uani 1 1 d . . . H3DA H 0.1603 -0.2554 0.5307 0.038 Uiso 1 1 calc R . . C4D C 0.20809(9) -0.1142(3) 0.53468(7) 0.0289(7) Uani 1 1 d . . . C5D C 0.24298(10) -0.2219(3) 0.54154(8) 0.0354(7) Uani 1 1 d . . . H5DA H 0.2601 -0.2030 0.5634 0.053 Uiso 1 1 calc R . . H5DB H 0.2624 -0.2204 0.5233 0.053 Uiso 1 1 calc R . . H5DC H 0.2292 -0.3126 0.5423 0.053 Uiso 1 1 calc R . . C6D C 0.08522(10) 0.1309(3) 0.52388(9) 0.0382(8) Uani 1 1 d . . . C7D C 0.07044(11) 0.1749(4) 0.55455(9) 0.0465(9) Uani 1 1 d . . . C8D C 0.03469(12) 0.2633(4) 0.55260(11) 0.0617(11) Uani 1 1 d . . . H8DA H 0.0239 0.2937 0.5730 0.074 Uiso 1 1 calc R . . C9D C 0.01457(12) 0.3076(4) 0.52188(12) 0.0638(12) Uani 1 1 d . . . H9DA H -0.0092 0.3704 0.5212 0.077 Uiso 1 1 calc R . . C10D C 0.02884(11) 0.2612(4) 0.49210(11) 0.0561(10) Uani 1 1 d . . . H10D H 0.0143 0.2910 0.4709 0.067 Uiso 1 1 calc R . . C11D C 0.06421(10) 0.1713(3) 0.49226(9) 0.0419(8) Uani 1 1 d . . . C12D C 0.09263(13) 0.1277(4) 0.58880(9) 0.0580(11) Uani 1 1 d . . . H12D H 0.1154 0.0591 0.5839 0.070 Uiso 1 1 calc R . . C13D C 0.11646(18) 0.2442(5) 0.60809(12) 0.1039(19) Uani 1 1 d . . . H13J H 0.1379 0.2843 0.5942 0.156 Uiso 1 1 calc R . . H13K H 0.1317 0.2092 0.6294 0.156 Uiso 1 1 calc R . . H13L H 0.0953 0.3148 0.6132 0.156 Uiso 1 1 calc R . . C14D C 0.06136(17) 0.0542(7) 0.61034(12) 0.116(2) Uani 1 1 d . . . H14J H 0.0473 -0.0225 0.5973 0.173 Uiso 1 1 calc R . . H14K H 0.0389 0.1188 0.6164 0.173 Uiso 1 1 calc R . . H14L H 0.0778 0.0190 0.6312 0.173 Uiso 1 1 calc R . . C15D C 0.07953(12) 0.1206(4) 0.45908(9) 0.0515(10) Uani 1 1 d . . . H15D H 0.1010 0.0445 0.4648 0.062 Uiso 1 1 calc R . . C16D C 0.10317(15) 0.2331(5) 0.44124(11) 0.0857(15) Uani 1 1 d . . . H16J H 0.1292 0.2623 0.4560 0.129 Uiso 1 1 calc R . . H16K H 0.0835 0.3117 0.4366 0.129 Uiso 1 1 calc R . . H16L H 0.1120 0.1975 0.4197 0.129 Uiso 1 1 calc R . . C17D C 0.04179(13) 0.0622(4) 0.43495(10) 0.0653(11) Uani 1 1 d . . . H17J H 0.0267 -0.0095 0.4467 0.098 Uiso 1 1 calc R . . H17K H 0.0534 0.0228 0.4149 0.098 Uiso 1 1 calc R . . H17L H 0.0211 0.1359 0.4278 0.098 Uiso 1 1 calc R . . C18D C 0.26531(10) 0.0539(3) 0.53587(8) 0.0329(7) Uani 1 1 d . . . C19D C 0.28558(10) 0.1014(3) 0.56705(8) 0.0402(8) Uani 1 1 d . . . C20D C 0.32880(11) 0.1459(4) 0.56821(10) 0.0536(10) Uani 1 1 d . . . H20D H 0.3432 0.1785 0.5891 0.064 Uiso 1 1 calc R . . C21D C 0.35101(12) 0.1437(4) 0.53982(11) 0.0634(12) Uani 1 1 d . . . H21D H 0.3805 0.1749 0.5412 0.076 Uiso 1 1 calc R . . C22D C 0.33055(12) 0.0962(4) 0.50946(10) 0.0580(11) Uani 1 1 d . . . H22D H 0.3462 0.0947 0.4899 0.070 Uiso 1 1 calc R . . C23D C 0.28745(10) 0.0503(3) 0.50659(8) 0.0403(8) Uani 1 1 d . . . C24D C 0.26230(11) 0.1044(4) 0.59897(9) 0.0532(10) Uani 1 1 d . . . H24D H 0.2314 0.0743 0.5925 0.064 Uiso 1 1 calc R . . C25D C 0.26067(16) 0.2494(5) 0.61391(11) 0.0880(16) Uani 1 1 d . . . H25J H 0.2485 0.3132 0.5962 0.132 Uiso 1 1 calc R . . H25K H 0.2904 0.2787 0.6224 0.132 Uiso 1 1 calc R . . H25L H 0.2421 0.2492 0.6327 0.132 Uiso 1 1 calc R . . C26D C 0.28274(12) 0.0043(4) 0.62566(9) 0.0565(10) Uani 1 1 d . . . H26J H 0.2802 -0.0895 0.6166 0.085 Uiso 1 1 calc R . . H26K H 0.2674 0.0106 0.6462 0.085 Uiso 1 1 calc R . . H26L H 0.3137 0.0273 0.6314 0.085 Uiso 1 1 calc R . . C27D C 0.26480(11) 0.0042(4) 0.47244(8) 0.0480(9) Uani 1 1 d . . . H27D H 0.2409 -0.0608 0.4771 0.058 Uiso 1 1 calc R . . C28D C 0.29486(14) -0.0716(5) 0.45001(10) 0.0716(13) Uani 1 1 d . . . H28J H 0.3105 -0.1449 0.4632 0.107 Uiso 1 1 calc R . . H28K H 0.3161 -0.0067 0.4421 0.107 Uiso 1 1 calc R . . H28L H 0.2772 -0.1114 0.4303 0.107 Uiso 1 1 calc R . . C29D C 0.24321(14) 0.1280(4) 0.45334(9) 0.0637(11) Uani 1 1 d . . . H29J H 0.2224 0.1712 0.4673 0.096 Uiso 1 1 calc R . . H29K H 0.2276 0.0972 0.4317 0.096 Uiso 1 1 calc R . . H29L H 0.2658 0.1947 0.4488 0.096 Uiso 1 1 calc R . . C30D C 0.18124(13) 0.3456(4) 0.52851(11) 0.0601(11) 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 Cu1A 0.0373(2) 0.0318(2) 0.0334(2) 0.00053(17) 0.00411(17) -0.00537(18) O1A 0.093(2) 0.0437(16) 0.078(2) -0.0117(15) 0.0173(17) -0.0257(16) N1A 0.0294(14) 0.0383(16) 0.0320(15) 0.0052(12) 0.0036(11) -0.0014(12) N2A 0.0347(14) 0.0315(14) 0.0252(14) -0.0026(12) 0.0028(11) -0.0036(12) C1A 0.047(2) 0.061(2) 0.042(2) 0.0036(19) -0.0072(17) -0.0102(19) C2A 0.0269(16) 0.050(2) 0.0283(17) 0.0019(15) 0.0060(13) -0.0044(15) C3A 0.0373(18) 0.0364(19) 0.0297(18) -0.0056(15) 0.0062(14) -0.0111(15) C4A 0.0305(17) 0.0349(18) 0.0293(18) -0.0023(14) 0.0092(14) -0.0061(14) C5A 0.059(2) 0.0346(19) 0.0368(19) -0.0019(16) 0.0043(17) -0.0088(17) C6A 0.0385(19) 0.043(2) 0.041(2) 0.0092(16) -0.0027(16) -0.0041(16) C7A 0.036(2) 0.059(3) 0.087(3) 0.023(2) 0.008(2) 0.0042(19) C8A 0.047(2) 0.075(3) 0.112(4) 0.037(3) 0.003(3) 0.014(2) C9A 0.077(3) 0.066(3) 0.086(3) 0.036(3) -0.014(3) 0.007(3) C10A 0.076(3) 0.066(3) 0.052(3) 0.023(2) 0.007(2) -0.005(2) C11A 0.053(2) 0.048(2) 0.0341(19) 0.0079(17) 0.0031(17) -0.0058(18) C12A 0.050(3) 0.072(3) 0.152(5) 0.038(3) 0.046(3) 0.022(2) C13A 0.094(4) 0.149(6) 0.111(5) 0.037(4) 0.045(4) 0.014(4) C14A 0.057(3) 0.133(5) 0.242(8) -0.009(5) 0.058(4) -0.012(3) C15A 0.068(3) 0.046(2) 0.041(2) 0.0084(18) 0.0240(19) 0.000(2) C16A 0.055(2) 0.058(3) 0.078(3) 0.003(2) 0.015(2) 0.009(2) C17A 0.108(4) 0.088(3) 0.058(3) -0.004(3) 0.038(3) -0.011(3) C18A 0.0423(19) 0.0257(16) 0.0300(17) -0.0021(14) 0.0024(14) -0.0035(14) C19A 0.0445(19) 0.0391(19) 0.0317(18) -0.0019(15) 0.0040(15) 0.0003(16) C20A 0.058(2) 0.057(2) 0.0296(19) -0.0078(17) 0.0065(17) 0.0007(19) C21A 0.067(3) 0.056(2) 0.033(2) -0.0021(18) -0.0046(19) 0.003(2) C22A 0.046(2) 0.047(2) 0.048(2) -0.0013(18) -0.0112(18) 0.0018(18) C23A 0.0399(19) 0.0363(19) 0.040(2) -0.0030(16) 0.0010(15) -0.0037(15) C24A 0.045(2) 0.071(3) 0.035(2) -0.0046(19) 0.0090(16) 0.0069(19) C25A 0.069(3) 0.078(3) 0.098(4) 0.003(3) 0.011(3) 0.023(3) C26A 0.052(3) 0.104(4) 0.079(3) 0.010(3) 0.015(2) -0.007(3) C27A 0.036(2) 0.067(3) 0.053(2) 0.001(2) 0.0037(17) 0.0047(19) C28A 0.077(3) 0.078(3) 0.103(4) -0.013(3) 0.034(3) 0.015(3) C29A 0.070(3) 0.082(4) 0.133(5) 0.008(3) 0.043(3) -0.015(3) C30A 0.059(2) 0.041(2) 0.040(2) 0.0030(17) 0.0081(17) -0.0056(19) Cu1B 0.0332(2) 0.02323(19) 0.0294(2) -0.00091(16) 0.00019(16) 0.00093(16) O1B 0.0701(18) 0.0348(15) 0.0768(19) 0.0118(14) -0.0153(15) 0.0063(13) N1B 0.0321(14) 0.0263(13) 0.0313(14) -0.0020(11) -0.0003(11) -0.0010(11) N2B 0.0337(14) 0.0251(13) 0.0276(14) -0.0031(11) 0.0054(11) -0.0023(11) C1B 0.054(2) 0.037(2) 0.045(2) 0.0013(17) -0.0082(17) 0.0083(17) C2B 0.0322(17) 0.0293(17) 0.0292(17) 0.0032(14) 0.0018(13) 0.0006(13) C3B 0.0382(18) 0.0244(16) 0.0356(18) 0.0052(14) 0.0046(14) 0.0061(14) C4B 0.0330(17) 0.0233(16) 0.0350(18) -0.0020(14) 0.0127(14) 0.0006(14) C5B 0.065(2) 0.0285(18) 0.0358(19) -0.0011(15) 0.0040(17) 0.0037(17) C6B 0.045(2) 0.0273(17) 0.0356(19) 0.0002(15) -0.0146(16) 0.0045(15) C7B 0.048(2) 0.0327(19) 0.059(2) 0.0009(18) -0.0249(19) -0.0029(17) C8B 0.070(3) 0.036(2) 0.092(3) -0.007(2) -0.039(3) -0.004(2) C9B 0.098(4) 0.045(3) 0.083(3) -0.033(2) -0.047(3) 0.016(3) C10B 0.090(3) 0.054(3) 0.051(3) -0.021(2) -0.017(2) 0.024(2) C11B 0.064(2) 0.0331(19) 0.038(2) -0.0068(16) -0.0082(18) 0.0116(18) C12B 0.045(2) 0.053(2) 0.072(3) 0.010(2) -0.012(2) -0.0174(19) C13B 0.060(3) 0.099(4) 0.100(4) 0.040(3) -0.016(3) -0.023(3) C14B 0.050(3) 0.084(3) 0.103(4) 0.016(3) -0.013(2) -0.005(2) C15B 0.071(3) 0.043(2) 0.038(2) -0.0035(17) 0.0151(19) 0.0128(19) C16B 0.063(3) 0.058(2) 0.050(2) 0.001(2) 0.009(2) -0.001(2) C17B 0.097(3) 0.080(3) 0.049(2) 0.011(2) 0.026(2) 0.038(3) C18B 0.0408(18) 0.0187(15) 0.0297(17) -0.0023(13) 0.0036(14) -0.0024(13) C19B 0.049(2) 0.0228(16) 0.0310(18) -0.0041(14) 0.0113(15) -0.0051(14) C20B 0.068(3) 0.0302(18) 0.0300(19) 0.0002(15) 0.0150(17) -0.0058(17) C21B 0.072(3) 0.037(2) 0.0314(19) 0.0024(16) -0.0065(18) -0.0007(18) C22B 0.045(2) 0.0368(19) 0.043(2) 0.0018(16) -0.0065(17) -0.0016(16) C23B 0.0394(18) 0.0232(16) 0.0304(17) -0.0012(13) 0.0001(14) -0.0012(14) C24B 0.050(2) 0.0381(19) 0.042(2) -0.0039(16) 0.0180(16) -0.0055(16) C25B 0.061(2) 0.040(2) 0.068(3) -0.0022(19) 0.030(2) -0.0023(19) C26B 0.056(2) 0.047(2) 0.103(3) -0.026(2) 0.028(2) -0.014(2) C27B 0.0352(18) 0.047(2) 0.043(2) 0.0023(17) 0.0054(15) -0.0038(16) C28B 0.049(2) 0.069(3) 0.072(3) -0.003(2) 0.024(2) 0.006(2) C29B 0.093(3) 0.069(3) 0.081(3) -0.002(3) 0.025(3) -0.039(3) C30B 0.0390(19) 0.0339(19) 0.0325(18) -0.0024(16) -0.0026(15) -0.0022(15) Cu1C 0.0425(2) 0.0274(2) 0.0322(2) 0.00221(17) -0.00102(17) 0.00685(17) O1C 0.0733(18) 0.0363(15) 0.0625(17) 0.0090(13) 0.0016(14) 0.0182(13) N1C 0.0363(15) 0.0297(14) 0.0339(15) 0.0018(12) -0.0027(12) 0.0007(12) N2C 0.0520(17) 0.0304(15) 0.0290(15) 0.0010(12) 0.0033(13) 0.0085(13) C1C 0.053(2) 0.042(2) 0.045(2) 0.0054(17) -0.0134(17) 0.0084(17) C2C 0.0339(18) 0.0338(18) 0.0405(19) 0.0077(16) 0.0007(15) 0.0043(15) C3C 0.047(2) 0.0299(18) 0.0379(19) 0.0086(15) 0.0044(16) 0.0116(15) C4C 0.053(2) 0.0294(18) 0.0340(19) 0.0056(15) 0.0090(16) 0.0083(16) C5C 0.084(3) 0.035(2) 0.048(2) -0.0015(17) 0.005(2) 0.018(2) C6C 0.045(2) 0.0267(17) 0.040(2) 0.0049(15) -0.0169(16) 0.0012(15) C7C 0.053(2) 0.0304(18) 0.0361(19) -0.0037(15) -0.0105(16) 0.0091(16) C8C 0.066(3) 0.049(2) 0.049(2) -0.0127(19) -0.015(2) 0.010(2) C9C 0.078(3) 0.037(2) 0.079(3) -0.016(2) -0.039(3) 0.006(2) C10C 0.059(3) 0.045(2) 0.086(3) 0.005(2) -0.033(2) -0.012(2) C11C 0.048(2) 0.039(2) 0.062(3) 0.0051(19) -0.0206(19) -0.0048(17) C12C 0.058(2) 0.0325(19) 0.0351(19) -0.0034(15) 0.0024(17) 0.0058(17) C13C 0.081(3) 0.065(3) 0.046(2) 0.008(2) 0.008(2) 0.013(2) C14C 0.054(2) 0.047(2) 0.065(3) 0.009(2) -0.0039(19) -0.0020(19) C15C 0.050(2) 0.065(3) 0.078(3) 0.014(2) -0.002(2) -0.018(2) C16C 0.059(3) 0.132(5) 0.093(4) 0.049(3) -0.010(3) -0.024(3) C17C 0.057(3) 0.092(4) 0.115(4) 0.024(3) -0.009(3) 0.000(3) C18C 0.062(2) 0.0278(18) 0.0270(18) 0.0010(14) 0.0043(16) 0.0133(16) C19C 0.057(2) 0.0298(18) 0.0352(19) 0.0001(15) 0.0014(17) 0.0067(16) C20C 0.067(3) 0.042(2) 0.044(2) 0.0003(18) -0.0045(19) -0.0029(19) C21C 0.096(3) 0.056(3) 0.031(2) 0.0018(18) -0.004(2) -0.002(2) C22C 0.082(3) 0.058(3) 0.035(2) 0.0050(19) 0.013(2) -0.004(2) C23C 0.064(2) 0.038(2) 0.038(2) 0.0058(16) 0.0061(18) 0.0058(18) C24C 0.056(2) 0.048(2) 0.045(2) 0.0005(18) 0.0036(18) 0.0027(19) C25C 0.101(4) 0.059(3) 0.085(3) 0.004(3) 0.032(3) -0.014(3) C26C 0.096(4) 0.068(3) 0.100(4) 0.000(3) 0.044(3) 0.018(3) C27C 0.060(2) 0.062(3) 0.045(2) 0.012(2) 0.0050(19) -0.001(2) C28C 0.077(4) 0.093(4) 0.199(7) -0.015(4) 0.036(4) 0.020(3) C29C 0.073(3) 0.067(3) 0.091(3) 0.002(3) 0.009(3) -0.013(2) C30C 0.043(2) 0.041(2) 0.0301(18) -0.0025(16) -0.0006(15) 0.0044(16) Cu1D 0.0320(2) 0.0279(2) 0.0511(3) 0.00064(19) -0.00212(18) -0.00611(17) O1D 0.158(3) 0.0290(17) 0.133(3) -0.0026(19) 0.023(3) -0.011(2) N1D 0.0298(14) 0.0341(15) 0.0362(15) -0.0004(12) -0.0023(12) -0.0048(12) N2D 0.0284(14) 0.0297(14) 0.0317(14) -0.0009(11) -0.0003(11) -0.0061(11) C1D 0.0375(18) 0.0404(19) 0.045(2) 0.0073(16) -0.0018(15) -0.0082(16) C2D 0.0334(17) 0.0342(18) 0.0221(16) 0.0029(14) -0.0002(13) -0.0112(14) C3D 0.0384(18) 0.0259(16) 0.0296(17) -0.0014(14) -0.0004(14) -0.0071(14) C4D 0.0330(17) 0.0331(17) 0.0206(15) -0.0022(13) 0.0026(13) -0.0056(14) C5D 0.0375(18) 0.0329(18) 0.0355(18) -0.0006(15) 0.0018(14) -0.0022(14) C6D 0.0291(17) 0.0312(18) 0.053(2) -0.0009(16) -0.0024(15) -0.0070(14) C7D 0.0386(19) 0.044(2) 0.056(2) -0.0141(18) 0.0010(17) -0.0015(17) C8D 0.045(2) 0.062(3) 0.077(3) -0.027(2) 0.002(2) 0.001(2) C9D 0.036(2) 0.050(2) 0.102(4) -0.013(2) -0.006(2) 0.0082(18) C10D 0.040(2) 0.050(2) 0.075(3) 0.006(2) -0.012(2) -0.0030(18) C11D 0.0327(18) 0.0377(19) 0.053(2) 0.0080(17) -0.0065(16) -0.0065(16) C12D 0.055(2) 0.074(3) 0.044(2) -0.016(2) -0.0006(19) 0.005(2) C13D 0.117(4) 0.097(4) 0.086(4) -0.026(3) -0.046(3) 0.001(3) C14D 0.089(4) 0.195(7) 0.061(3) 0.028(4) -0.001(3) -0.014(4) C15D 0.047(2) 0.059(2) 0.046(2) 0.0157(19) -0.0040(17) -0.0045(19) C16D 0.084(3) 0.104(4) 0.068(3) 0.025(3) 0.004(3) -0.029(3) C17D 0.070(3) 0.069(3) 0.054(3) 0.000(2) -0.008(2) -0.002(2) C18D 0.0281(16) 0.0277(16) 0.0419(19) 0.0028(14) -0.0003(14) -0.0056(13) C19D 0.0339(18) 0.0419(19) 0.043(2) -0.0030(16) -0.0049(15) -0.0040(16) C20D 0.041(2) 0.053(2) 0.064(3) 0.000(2) -0.0110(19) -0.0138(18) C21D 0.036(2) 0.074(3) 0.080(3) 0.018(2) 0.003(2) -0.024(2) C22D 0.044(2) 0.075(3) 0.056(3) 0.018(2) 0.0126(19) -0.012(2) C23D 0.0347(18) 0.043(2) 0.043(2) 0.0085(16) 0.0051(16) -0.0087(15) C24D 0.038(2) 0.076(3) 0.044(2) -0.020(2) -0.0043(17) -0.0029(19) C25D 0.103(4) 0.090(4) 0.067(3) -0.030(3) -0.009(3) 0.036(3) C26D 0.059(2) 0.070(3) 0.041(2) -0.012(2) 0.0072(18) -0.014(2) C27D 0.049(2) 0.059(2) 0.037(2) 0.0062(18) 0.0120(17) -0.0054(18) C28D 0.085(3) 0.081(3) 0.052(3) 0.001(2) 0.022(2) 0.008(3) C29D 0.080(3) 0.068(3) 0.041(2) 0.009(2) -0.001(2) 0.002(2) C30D 0.061(3) 0.039(2) 0.079(3) -0.003(2) 0.004(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1A C30A 1.785(4) . ? Cu1A N2A 1.917(2) . ? Cu1A N1A 1.921(2) . ? O1A C30A 1.128(4) . ? N1A C2A 1.331(4) . ? N1A C6A 1.434(4) . ? N2A C4A 1.330(4) . ? N2A C18A 1.441(4) . ? C1A C2A 1.510(4) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C3A 1.406(4) . ? C3A C4A 1.390(4) . ? C3A H3AA 0.9500 . ? C4A C5A 1.517(4) . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C6A C11A 1.401(4) . ? C6A C7A 1.402(5) . ? C7A C8A 1.382(5) . ? C7A C12A 1.523(6) . ? C8A C9A 1.360(6) . ? C8A H8AA 0.9500 . ? C9A C10A 1.374(6) . ? C9A H9AA 0.9500 . ? C10A C11A 1.396(5) . ? C10A H10A 0.9500 . ? C11A C15A 1.517(5) . ? C12A C13A 1.509(7) . ? C12A C14A 1.537(7) . ? C12A H12A 1.0000 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A C17A 1.524(5) . ? C15A C16A 1.525(5) . ? C15A H15A 1.0000 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A C23A 1.401(4) . ? C18A C19A 1.403(4) . ? C19A C20A 1.392(4) . ? C19A C24A 1.517(5) . ? C20A C21A 1.370(5) . ? C20A H20A 0.9500 . ? C21A C22A 1.368(5) . ? C21A H21A 0.9500 . ? C22A C23A 1.398(5) . ? C22A H22A 0.9500 . ? C23A C27A 1.516(5) . ? C24A C25A 1.517(5) . ? C24A C26A 1.533(5) . ? C24A H24A 1.0000 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A C29A 1.512(5) . ? C27A C28A 1.527(5) . ? C27A H27A 1.0000 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? Cu1B C30B 1.771(3) . ? Cu1B N1B 1.913(2) . ? Cu1B N2B 1.918(2) . ? O1B C30B 1.132(4) . ? N1B C2B 1.332(4) . ? N1B C6B 1.436(4) . ? N2B C4B 1.322(4) . ? N2B C18B 1.439(4) . ? C1B C2B 1.503(4) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C2B C3B 1.400(4) . ? C3B C4B 1.399(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.511(4) . ? C5B H5BA 0.9800 . ? C5B H5BB 0.9800 . ? C5B H5BC 0.9800 . ? C6B C11B 1.399(5) . ? C6B C7B 1.405(5) . ? C7B C8B 1.390(5) . ? C7B C12B 1.508(5) . ? C8B C9B 1.377(6) . ? C8B H8BA 0.9500 . ? C9B C10B 1.369(6) . ? C9B H9BA 0.9500 . ? C10B C11B 1.397(5) . ? C10B H10B 0.9500 . ? C11B C15B 1.512(5) . ? C12B C13B 1.535(5) . ? C12B C14B 1.536(5) . ? C12B H12B 1.0000 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B C16B 1.526(5) . ? C15B C17B 1.539(5) . ? C15B H15B 1.0000 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B C23B 1.406(4) . ? C18B C19B 1.408(4) . ? C19B C20B 1.388(4) . ? C19B C24B 1.524(4) . ? C20B C21B 1.378(5) . ? C20B H20B 0.9500 . ? C21B C22B 1.370(5) . ? C21B H21B 0.9500 . ? C22B C23B 1.387(4) . ? C22B H22B 0.9500 . ? C23B C27B 1.524(4) . ? C24B C26B 1.527(5) . ? C24B C25B 1.531(4) . ? C24B H24B 1.0000 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B C28B 1.524(5) . ? C27B C29B 1.529(5) . ? C27B H27B 1.0000 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? Cu1C C30C 1.784(4) . ? Cu1C N2C 1.918(3) . ? Cu1C N1C 1.921(2) . ? O1C C30C 1.120(4) . ? N1C C2C 1.328(4) . ? N1C C6C 1.439(4) . ? N2C C4C 1.332(4) . ? N2C C18C 1.433(4) . ? C1C C2C 1.506(4) . ? C1C H1CA 0.9800 . ? C1C H1CB 0.9800 . ? C1C H1CC 0.9800 . ? C2C C3C 1.408(4) . ? C3C C4C 1.397(4) . ? C3C H3CA 0.9500 . ? C4C C5C 1.514(4) . ? C5C H5CA 0.9800 . ? C5C H5CB 0.9800 . ? C5C H5CC 0.9800 . ? C6C C7C 1.408(5) . ? C6C C11C 1.410(5) . ? C7C C8C 1.390(5) . ? C7C C12C 1.509(5) . ? C8C C9C 1.377(6) . ? C8C H8CA 0.9500 . ? C9C C10C 1.369(6) . ? C9C H9CA 0.9500 . ? C10C C11C 1.397(5) . ? C10C H10C 0.9500 . ? C11C C15C 1.503(5) . ? C12C C14C 1.523(5) . ? C12C C13C 1.535(5) . ? C12C H12C 1.0000 . ? C13C H13G 0.9800 . ? C13C H13H 0.9800 . ? C13C H13I 0.9800 . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C14C H14I 0.9800 . ? C15C C16C 1.537(6) . ? C15C C17C 1.543(5) . ? C15C H15C 1.0000 . ? C16C H16G 0.9800 . ? C16C H16H 0.9800 . ? C16C H16I 0.9800 . ? C17C H17G 0.9800 . ? C17C H17H 0.9800 . ? C17C H17I 0.9800 . ? C18C C23C 1.408(5) . ? C18C C19C 1.408(5) . ? C19C C20C 1.388(5) . ? C19C C24C 1.513(5) . ? C20C C21C 1.384(5) . ? C20C H20C 0.9500 . ? C21C C22C 1.373(5) . ? C21C H21C 0.9500 . ? C22C C23C 1.391(5) . ? C22C H22C 0.9500 . ? C23C C27C 1.523(5) . ? C24C C26C 1.518(5) . ? C24C C25C 1.526(5) . ? C24C H24C 1.0000 . ? C25C H25G 0.9800 . ? C25C H25H 0.9800 . ? C25C H25I 0.9800 . ? C26C H26G 0.9800 . ? C26C H26H 0.9800 . ? C26C H26I 0.9800 . ? C27C C28C 1.514(6) . ? C27C C29C 1.518(5) . ? C27C H27C 1.0000 . ? C28C H28G 0.9800 . ? C28C H28H 0.9800 . ? C28C H28I 0.9800 . ? C29C H29G 0.9800 . ? C29C H29H 0.9800 . ? C29C H29I 0.9800 . ? Cu1D C30D 1.776(4) . ? Cu1D N2D 1.912(2) . ? Cu1D N1D 1.920(2) . ? O1D C30D 1.118(4) . ? N1D C2D 1.328(4) . ? N1D C6D 1.434(4) . ? N2D C4D 1.328(4) . ? N2D C18D 1.438(4) . ? C1D C2D 1.510(4) . ? C1D H1DA 0.9800 . ? C1D H1DB 0.9800 . ? C1D H1DC 0.9800 . ? C2D C3D 1.398(4) . ? C3D C4D 1.404(4) . ? C3D H3DA 0.9500 . ? C4D C5D 1.502(4) . ? C5D H5DA 0.9800 . ? C5D H5DB 0.9800 . ? C5D H5DC 0.9800 . ? C6D C11D 1.400(4) . ? C6D C7D 1.403(5) . ? C7D C8D 1.390(5) . ? C7D C12D 1.519(5) . ? C8D C9D 1.371(6) . ? C8D H8DA 0.9500 . ? C9D C10D 1.373(5) . ? C9D H9DA 0.9500 . ? C10D C11D 1.394(5) . ? C10D H10D 0.9500 . ? C11D C15D 1.519(5) . ? C12D C13D 1.511(6) . ? C12D C14D 1.525(6) . ? C12D H12D 1.0000 . ? C13D H13J 0.9800 . ? C13D H13K 0.9800 . ? C13D H13L 0.9800 . ? C14D H14J 0.9800 . ? C14D H14K 0.9800 . ? C14D H14L 0.9800 . ? C15D C16D 1.525(5) . ? C15D C17D 1.530(5) . ? C15D H15D 1.0000 . ? C16D H16J 0.9800 . ? C16D H16K 0.9800 . ? C16D H16L 0.9800 . ? C17D H17J 0.9800 . ? C17D H17K 0.9800 . ? C17D H17L 0.9800 . ? C18D C19D 1.398(4) . ? C18D C23D 1.401(4) . ? C19D C20D 1.391(4) . ? C19D C24D 1.512(5) . ? C20D C21D 1.371(5) . ? C20D H20D 0.9500 . ? C21D C22D 1.373(5) . ? C21D H21D 0.9500 . ? C22D C23D 1.389(5) . ? C22D H22D 0.9500 . ? C23D C27D 1.518(5) . ? C24D C26D 1.521(5) . ? C24D C25D 1.532(5) . ? C24D H24D 1.0000 . ? C25D H25J 0.9800 . ? C25D H25K 0.9800 . ? C25D H25L 0.9800 . ? C26D H26J 0.9800 . ? C26D H26K 0.9800 . ? C26D H26L 0.9800 . ? C27D C28D 1.533(5) . ? C27D C29D 1.535(5) . ? C27D H27D 1.0000 . ? C28D H28J 0.9800 . ? C28D H28K 0.9800 . ? C28D H28L 0.9800 . ? C29D H29J 0.9800 . ? C29D H29K 0.9800 . ? C29D H29L 0.9800 . ? 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 C30A Cu1A N2A 137.45(13) . . ? C30A Cu1A N1A 123.13(14) . . ? N2A Cu1A N1A 99.42(10) . . ? C2A N1A C6A 118.6(3) . . ? C2A N1A Cu1A 121.4(2) . . ? C6A N1A Cu1A 120.0(2) . . ? C4A N2A C18A 118.3(2) . . ? C4A N2A Cu1A 121.5(2) . . ? C18A N2A Cu1A 120.10(19) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? N1A C2A C3A 123.8(3) . . ? N1A C2A C1A 119.6(3) . . ? C3A C2A C1A 116.6(3) . . ? C4A C3A C2A 129.2(3) . . ? C4A C3A H3AA 115.4 . . ? C2A C3A H3AA 115.4 . . ? N2A C4A C3A 124.2(3) . . ? N2A C4A C5A 119.1(3) . . ? C3A C4A C5A 116.6(3) . . ? C4A C5A H5AA 109.5 . . ? C4A C5A H5AB 109.5 . . ? H5AA C5A H5AB 109.5 . . ? C4A C5A H5AC 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? C11A C6A C7A 120.9(3) . . ? C11A C6A N1A 120.0(3) . . ? C7A C6A N1A 119.0(3) . . ? C8A C7A C6A 118.8(4) . . ? C8A C7A C12A 120.2(4) . . ? C6A C7A C12A 121.0(3) . . ? C9A C8A C7A 121.1(4) . . ? C9A C8A H8AA 119.4 . . ? C7A C8A H8AA 119.4 . . ? C8A C9A C10A 120.3(4) . . ? C8A C9A H9AA 119.8 . . ? C10A C9A H9AA 119.8 . . ? C9A C10A C11A 121.4(4) . . ? C9A C10A H10A 119.3 . . ? C11A C10A H10A 119.3 . . ? C10A C11A C6A 117.5(3) . . ? C10A C11A C15A 121.1(3) . . ? C6A C11A C15A 121.4(3) . . ? C13A C12A C7A 111.7(4) . . ? C13A C12A C14A 110.5(4) . . ? C7A C12A C14A 111.3(5) . . ? C13A C12A H12A 107.7 . . ? C7A C12A H12A 107.7 . . ? C14A C12A H12A 107.7 . . ? C12A C13A H13A 109.5 . . ? C12A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C12A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C11A C15A C17A 113.4(3) . . ? C11A C15A C16A 110.5(3) . . ? C17A C15A C16A 110.1(3) . . ? C11A C15A H15A 107.5 . . ? C17A C15A H15A 107.5 . . ? C16A C15A H15A 107.5 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15A C17A H17A 109.5 . . ? C15A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C15A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C23A C18A C19A 120.9(3) . . ? C23A C18A N2A 120.2(3) . . ? C19A C18A N2A 118.9(3) . . ? C20A C19A C18A 118.4(3) . . ? C20A C19A C24A 119.8(3) . . ? C18A C19A C24A 121.8(3) . . ? C21A C20A C19A 121.0(3) . . ? C21A C20A H20A 119.5 . . ? C19A C20A H20A 119.5 . . ? C22A C21A C20A 120.4(3) . . ? C22A C21A H21A 119.8 . . ? C20A C21A H21A 119.8 . . ? C21A C22A C23A 121.1(3) . . ? C21A C22A H22A 119.4 . . ? C23A C22A H22A 119.4 . . ? C22A C23A C18A 118.1(3) . . ? C22A C23A C27A 120.4(3) . . ? C18A C23A C27A 121.5(3) . . ? C25A C24A C19A 111.0(3) . . ? C25A C24A C26A 109.9(3) . . ? C19A C24A C26A 113.2(3) . . ? C25A C24A H24A 107.5 . . ? C19A C24A H24A 107.5 . . ? C26A C24A H24A 107.5 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C24A C26A H26A 109.5 . . ? C24A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C24A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C29A C27A C23A 111.4(3) . . ? C29A C27A C28A 109.9(3) . . ? C23A C27A C28A 112.5(3) . . ? C29A C27A H27A 107.6 . . ? C23A C27A H27A 107.6 . . ? C28A C27A H27A 107.6 . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? O1A C30A Cu1A 175.0(3) . . ? C30B Cu1B N1B 129.24(12) . . ? C30B Cu1B N2B 132.02(12) . . ? N1B Cu1B N2B 98.68(10) . . ? C2B N1B C6B 119.5(2) . . ? C2B N1B Cu1B 122.7(2) . . ? C6B N1B Cu1B 117.86(19) . . ? C4B N2B C18B 120.9(2) . . ? C4B N2B Cu1B 122.4(2) . . ? C18B N2B Cu1B 116.41(18) . . ? C2B C1B H1BA 109.5 . . ? C2B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? C2B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? N1B C2B C3B 123.0(3) . . ? N1B C2B C1B 119.6(3) . . ? C3B C2B C1B 117.3(3) . . ? C4B C3B C2B 129.5(3) . . ? C4B C3B H3BA 115.2 . . ? C2B C3B H3BA 115.2 . . ? N2B C4B C3B 123.7(3) . . ? N2B C4B C5B 119.1(3) . . ? C3B C4B C5B 117.2(3) . . ? C4B C5B H5BA 109.5 . . ? C4B C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? C4B C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? C11B C6B C7B 121.8(3) . . ? C11B C6B N1B 119.1(3) . . ? C7B C6B N1B 118.9(3) . . ? C8B C7B C6B 117.7(4) . . ? C8B C7B C12B 120.6(4) . . ? C6B C7B C12B 121.6(3) . . ? C9B C8B C7B 121.1(4) . . ? C9B C8B H8BA 119.5 . . ? C7B C8B H8BA 119.5 . . ? C10B C9B C8B 120.5(4) . . ? C10B C9B H9BA 119.7 . . ? C8B C9B H9BA 119.7 . . ? C9B C10B C11B 121.0(4) . . ? C9B C10B H10B 119.5 . . ? C11B C10B H10B 119.5 . . ? C10B C11B C6B 117.8(4) . . ? C10B C11B C15B 121.1(4) . . ? C6B C11B C15B 121.0(3) . . ? C7B C12B C13B 111.2(4) . . ? C7B C12B C14B 112.9(3) . . ? C13B C12B C14B 109.8(3) . . ? C7B C12B H12B 107.5 . . ? C13B C12B H12B 107.5 . . ? C14B C12B H12B 107.5 . . ? C12B C13B H13D 109.5 . . ? C12B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C11B C15B C16B 109.8(3) . . ? C11B C15B C17B 114.0(3) . . ? C16B C15B C17B 110.1(3) . . ? C11B C15B H15B 107.6 . . ? C16B C15B H15B 107.6 . . ? C17B C15B H15B 107.6 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C23B C18B C19B 121.0(3) . . ? C23B C18B N2B 119.6(3) . . ? C19B C18B N2B 119.2(3) . . ? C20B C19B C18B 118.0(3) . . ? C20B C19B C24B 121.3(3) . . ? C18B C19B C24B 120.6(3) . . ? C21B C20B C19B 121.4(3) . . ? C21B C20B H20B 119.3 . . ? C19B C20B H20B 119.3 . . ? C22B C21B C20B 119.9(3) . . ? C22B C21B H21B 120.0 . . ? C20B C21B H21B 120.0 . . ? C21B C22B C23B 121.6(3) . . ? C21B C22B H22B 119.2 . . ? C23B C22B H22B 119.2 . . ? C22B C23B C18B 118.1(3) . . ? C22B C23B C27B 121.0(3) . . ? C18B C23B C27B 120.9(3) . . ? C19B C24B C26B 110.8(3) . . ? C19B C24B C25B 112.2(3) . . ? C26B C24B C25B 110.5(3) . . ? C19B C24B H24B 107.7 . . ? C26B C24B H24B 107.7 . . ? C25B C24B H24B 107.7 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C24B C26B H26D 109.5 . . ? C24B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C24B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C23B 111.0(3) . . ? C28B C27B C29B 110.0(3) . . ? C23B C27B C29B 112.7(3) . . ? C28B C27B H27B 107.7 . . ? C23B C27B H27B 107.7 . . ? C29B C27B H27B 107.7 . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O1B C30B Cu1B 178.3(3) . . ? C30C Cu1C N2C 133.12(13) . . ? C30C Cu1C N1C 127.39(13) . . ? N2C Cu1C N1C 99.18(11) . . ? C2C N1C C6C 119.1(3) . . ? C2C N1C Cu1C 122.2(2) . . ? C6C N1C Cu1C 118.46(19) . . ? C4C N2C C18C 118.5(3) . . ? C4C N2C Cu1C 122.0(2) . . ? C18C N2C Cu1C 119.18(19) . . ? C2C C1C H1CA 109.5 . . ? C2C C1C H1CB 109.5 . . ? H1CA C1C H1CB 109.5 . . ? C2C C1C H1CC 109.5 . . ? H1CA C1C H1CC 109.5 . . ? H1CB C1C H1CC 109.5 . . ? N1C C2C C3C 123.2(3) . . ? N1C C2C C1C 119.9(3) . . ? C3C C2C C1C 116.9(3) . . ? C4C C3C C2C 129.7(3) . . ? C4C C3C H3CA 115.1 . . ? C2C C3C H3CA 115.1 . . ? N2C C4C C3C 123.6(3) . . ? N2C C4C C5C 119.5(3) . . ? C3C C4C C5C 116.9(3) . . ? C4C C5C H5CA 109.5 . . ? C4C C5C H5CB 109.5 . . ? H5CA C5C H5CB 109.5 . . ? C4C C5C H5CC 109.5 . . ? H5CA C5C H5CC 109.5 . . ? H5CB C5C H5CC 109.5 . . ? C7C C6C C11C 121.9(3) . . ? C7C C6C N1C 119.6(3) . . ? C11C C6C N1C 118.5(3) . . ? C8C C7C C6C 117.7(3) . . ? C8C C7C C12C 120.5(3) . . ? C6C C7C C12C 121.7(3) . . ? C9C C8C C7C 121.3(4) . . ? C9C C8C H8CA 119.4 . . ? C7C C8C H8CA 119.4 . . ? C10C C9C C8C 120.4(4) . . ? C10C C9C H9CA 119.8 . . ? C8C C9C H9CA 119.8 . . ? C9C C10C C11C 121.7(4) . . ? C9C C10C H10C 119.2 . . ? C11C C10C H10C 119.2 . . ? C10C C11C C6C 117.1(4) . . ? C10C C11C C15C 120.9(4) . . ? C6C C11C C15C 122.0(3) . . ? C7C C12C C14C 109.6(3) . . ? C7C C12C C13C 114.1(3) . . ? C14C C12C C13C 109.8(3) . . ? C7C C12C H12C 107.7 . . ? C14C C12C H12C 107.7 . . ? C13C C12C H12C 107.7 . . ? C12C C13C H13G 109.5 . . ? C12C C13C H13H 109.5 . . ? H13G C13C H13H 109.5 . . ? C12C C13C H13I 109.5 . . ? H13G C13C H13I 109.5 . . ? H13H C13C H13I 109.5 . . ? C12C C14C H14G 109.5 . . ? C12C C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? C12C C14C H14I 109.5 . . ? H14G C14C H14I 109.5 . . ? H14H C14C H14I 109.5 . . ? C11C C15C C16C 111.2(4) . . ? C11C C15C C17C 113.4(4) . . ? C16C C15C C17C 109.3(3) . . ? C11C C15C H15C 107.5 . . ? C16C C15C H15C 107.5 . . ? C17C C15C H15C 107.5 . . ? C15C C16C H16G 109.5 . . ? C15C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C15C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C15C C17C H17G 109.5 . . ? C15C C17C H17H 109.5 . . ? H17G C17C H17H 109.5 . . ? C15C C17C H17I 109.5 . . ? H17G C17C H17I 109.5 . . ? H17H C17C H17I 109.5 . . ? C23C C18C C19C 120.9(3) . . ? C23C C18C N2C 119.0(3) . . ? C19C C18C N2C 120.0(3) . . ? C20C C19C C18C 118.3(3) . . ? C20C C19C C24C 120.4(3) . . ? C18C C19C C24C 121.3(3) . . ? C21C C20C C19C 121.0(4) . . ? C21C C20C H20C 119.5 . . ? C19C C20C H20C 119.5 . . ? C22C C21C C20C 120.3(4) . . ? C22C C21C H21C 119.9 . . ? C20C C21C H21C 119.9 . . ? C21C C22C C23C 121.1(4) . . ? C21C C22C H22C 119.4 . . ? C23C C22C H22C 119.4 . . ? C22C C23C C18C 118.3(3) . . ? C22C C23C C27C 120.3(3) . . ? C18C C23C C27C 121.4(3) . . ? C19C C24C C26C 110.2(3) . . ? C19C C24C C25C 114.0(3) . . ? C26C C24C C25C 110.3(3) . . ? C19C C24C H24C 107.4 . . ? C26C C24C H24C 107.4 . . ? C25C C24C H24C 107.4 . . ? C24C C25C H25G 109.5 . . ? C24C C25C H25H 109.5 . . ? H25G C25C H25H 109.5 . . ? C24C C25C H25I 109.5 . . ? H25G C25C H25I 109.5 . . ? H25H C25C H25I 109.5 . . ? C24C C26C H26G 109.5 . . ? C24C C26C H26H 109.5 . . ? H26G C26C H26H 109.5 . . ? C24C C26C H26I 109.5 . . ? H26G C26C H26I 109.5 . . ? H26H C26C H26I 109.5 . . ? C28C C27C C29C 107.8(4) . . ? C28C C27C C23C 112.8(4) . . ? C29C C27C C23C 111.4(3) . . ? C28C C27C H27C 108.2 . . ? C29C C27C H27C 108.2 . . ? C23C C27C H27C 108.2 . . ? C27C C28C H28G 109.5 . . ? C27C C28C H28H 109.5 . . ? H28G C28C H28H 109.5 . . ? C27C C28C H28I 109.5 . . ? H28G C28C H28I 109.5 . . ? H28H C28C H28I 109.5 . . ? C27C C29C H29G 109.5 . . ? C27C C29C H29H 109.5 . . ? H29G C29C H29H 109.5 . . ? C27C C29C H29I 109.5 . . ? H29G C29C H29I 109.5 . . ? H29H C29C H29I 109.5 . . ? O1C C30C Cu1C 175.8(3) . . ? C30D Cu1D N2D 135.14(15) . . ? C30D Cu1D N1D 126.35(15) . . ? N2D Cu1D N1D 98.39(11) . . ? C2D N1D C6D 121.2(3) . . ? C2D N1D Cu1D 122.8(2) . . ? C6D N1D Cu1D 115.87(19) . . ? C4D N2D C18D 120.1(2) . . ? C4D N2D Cu1D 122.8(2) . . ? C18D N2D Cu1D 117.10(19) . . ? C2D C1D H1DA 109.5 . . ? C2D C1D H1DB 109.5 . . ? H1DA C1D H1DB 109.5 . . ? C2D C1D H1DC 109.5 . . ? H1DA C1D H1DC 109.5 . . ? H1DB C1D H1DC 109.5 . . ? N1D C2D C3D 123.1(3) . . ? N1D C2D C1D 118.9(3) . . ? C3D C2D C1D 117.9(3) . . ? C2D C3D C4D 129.4(3) . . ? C2D C3D H3DA 115.3 . . ? C4D C3D H3DA 115.3 . . ? N2D C4D C3D 123.3(3) . . ? N2D C4D C5D 119.2(3) . . ? C3D C4D C5D 117.5(3) . . ? C4D C5D H5DA 109.5 . . ? C4D C5D H5DB 109.5 . . ? H5DA C5D H5DB 109.5 . . ? C4D C5D H5DC 109.5 . . ? H5DA C5D H5DC 109.5 . . ? H5DB C5D H5DC 109.5 . . ? C11D C6D C7D 121.5(3) . . ? C11D C6D N1D 119.5(3) . . ? C7D C6D N1D 118.7(3) . . ? C8D C7D C6D 117.8(3) . . ? C8D C7D C12D 120.9(3) . . ? C6D C7D C12D 121.3(3) . . ? C9D C8D C7D 121.6(4) . . ? C9D C8D H8DA 119.2 . . ? C7D C8D H8DA 119.2 . . ? C8D C9D C10D 119.9(4) . . ? C8D C9D H9DA 120.0 . . ? C10D C9D H9DA 120.0 . . ? C9D C10D C11D 121.4(4) . . ? C9D C10D H10D 119.3 . . ? C11D C10D H10D 119.3 . . ? C10D C11D C6D 117.8(3) . . ? C10D C11D C15D 120.8(3) . . ? C6D C11D C15D 121.4(3) . . ? C13D C12D C7D 111.7(4) . . ? C13D C12D C14D 111.8(4) . . ? C7D C12D C14D 112.8(3) . . ? C13D C12D H12D 106.7 . . ? C7D C12D H12D 106.7 . . ? C14D C12D H12D 106.7 . . ? C12D C13D H13J 109.5 . . ? C12D C13D H13K 109.5 . . ? H13J C13D H13K 109.5 . . ? C12D C13D H13L 109.5 . . ? H13J C13D H13L 109.5 . . ? H13K C13D H13L 109.5 . . ? C12D C14D H14J 109.5 . . ? C12D C14D H14K 109.5 . . ? H14J C14D H14K 109.5 . . ? C12D C14D H14L 109.5 . . ? H14J C14D H14L 109.5 . . ? H14K C14D H14L 109.5 . . ? C11D C15D C16D 111.7(3) . . ? C11D C15D C17D 112.0(3) . . ? C16D C15D C17D 110.2(3) . . ? C11D C15D H15D 107.6 . . ? C16D C15D H15D 107.6 . . ? C17D C15D H15D 107.6 . . ? C15D C16D H16J 109.5 . . ? C15D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C15D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C15D C17D H17J 109.5 . . ? C15D C17D H17K 109.5 . . ? H17J C17D H17K 109.5 . . ? C15D C17D H17L 109.5 . . ? H17J C17D H17L 109.5 . . ? H17K C17D H17L 109.5 . . ? C19D C18D C23D 121.6(3) . . ? C19D C18D N2D 119.5(3) . . ? C23D C18D N2D 118.7(3) . . ? C20D C19D C18D 117.8(3) . . ? C20D C19D C24D 119.9(3) . . ? C18D C19D C24D 122.3(3) . . ? C21D C20D C19D 121.5(3) . . ? C21D C20D H20D 119.3 . . ? C19D C20D H20D 119.3 . . ? C20D C21D C22D 119.8(3) . . ? C20D C21D H21D 120.1 . . ? C22D C21D H21D 120.1 . . ? C21D C22D C23D 121.6(3) . . ? C21D C22D H22D 119.2 . . ? C23D C22D H22D 119.2 . . ? C22D C23D C18D 117.7(3) . . ? C22D C23D C27D 120.7(3) . . ? C18D C23D C27D 121.5(3) . . ? C19D C24D C26D 111.6(3) . . ? C19D C24D C25D 112.1(4) . . ? C26D C24D C25D 110.6(3) . . ? C19D C24D H24D 107.5 . . ? C26D C24D H24D 107.5 . . ? C25D C24D H24D 107.5 . . ? C24D C25D H25J 109.5 . . ? C24D C25D H25K 109.5 . . ? H25J C25D H25K 109.5 . . ? C24D C25D H25L 109.5 . . ? H25J C25D H25L 109.5 . . ? H25K C25D H25L 109.5 . . ? C24D C26D H26J 109.5 . . ? C24D C26D H26K 109.5 . . ? H26J C26D H26K 109.5 . . ? C24D C26D H26L 109.5 . . ? H26J C26D H26L 109.5 . . ? H26K C26D H26L 109.5 . . ? C23D C27D C28D 114.1(3) . . ? C23D C27D C29D 109.7(3) . . ? C28D C27D C29D 110.4(3) . . ? C23D C27D H27D 107.5 . . ? C28D C27D H27D 107.5 . . ? C29D C27D H27D 107.5 . . ? C27D C28D H28J 109.5 . . ? C27D C28D H28K 109.5 . . ? H28J C28D H28K 109.5 . . ? C27D C28D H28L 109.5 . . ? H28J C28D H28L 109.5 . . ? H28K C28D H28L 109.5 . . ? C27D C29D H29J 109.5 . . ? C27D C29D H29K 109.5 . . ? H29J C29D H29K 109.5 . . ? C27D C29D H29L 109.5 . . ? H29J C29D H29L 109.5 . . ? H29K C29D H29L 109.5 . . ? O1D C30D Cu1D 175.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30A Cu1A N1A C2A -175.0(2) . . . . ? N2A Cu1A N1A C2A 4.9(2) . . . . ? C30A Cu1A N1A C6A 7.3(3) . . . . ? N2A Cu1A N1A C6A -172.7(2) . . . . ? C30A Cu1A N2A C4A 173.7(2) . . . . ? N1A Cu1A N2A C4A -6.2(2) . . . . ? C30A Cu1A N2A C18A -11.0(3) . . . . ? N1A Cu1A N2A C18A 169.1(2) . . . . ? C6A N1A C2A C3A 177.4(3) . . . . ? Cu1A N1A C2A C3A -0.2(4) . . . . ? C6A N1A C2A C1A -2.1(4) . . . . ? Cu1A N1A C2A C1A -179.8(2) . . . . ? N1A C2A C3A C4A -5.6(5) . . . . ? C1A C2A C3A C4A 174.0(3) . . . . ? C18A N2A C4A C3A -172.5(3) . . . . ? Cu1A N2A C4A C3A 2.8(4) . . . . ? C18A N2A C4A C5A 5.9(4) . . . . ? Cu1A N2A C4A C5A -178.8(2) . . . . ? C2A C3A C4A N2A 4.1(5) . . . . ? C2A C3A C4A C5A -174.3(3) . . . . ? C2A N1A C6A C11A 90.4(4) . . . . ? Cu1A N1A C6A C11A -91.9(3) . . . . ? C2A N1A C6A C7A -91.7(4) . . . . ? Cu1A N1A C6A C7A 86.0(4) . . . . ? C11A C6A C7A C8A -0.3(6) . . . . ? N1A C6A C7A C8A -178.3(4) . . . . ? C11A C6A C7A C12A 178.2(4) . . . . ? N1A C6A C7A C12A 0.3(6) . . . . ? C6A C7A C8A C9A 0.0(7) . . . . ? C12A C7A C8A C9A -178.6(5) . . . . ? C7A C8A C9A C10A 0.5(8) . . . . ? C8A C9A C10A C11A -0.6(7) . . . . ? C9A C10A C11A C6A 0.3(6) . . . . ? C9A C10A C11A C15A 178.0(4) . . . . ? C7A C6A C11A C10A 0.2(5) . . . . ? N1A C6A C11A C10A 178.2(3) . . . . ? C7A C6A C11A C15A -177.5(3) . . . . ? N1A C6A C11A C15A 0.5(5) . . . . ? C8A C7A C12A C13A 72.6(6) . . . . ? C6A C7A C12A C13A -106.0(5) . . . . ? C8A C7A C12A C14A -51.4(6) . . . . ? C6A C7A C12A C14A 130.0(5) . . . . ? C10A C11A C15A C17A 50.4(5) . . . . ? C6A C11A C15A C17A -132.0(4) . . . . ? C10A C11A C15A C16A -73.8(4) . . . . ? C6A C11A C15A C16A 103.8(4) . . . . ? C4A N2A C18A C23A -97.1(3) . . . . ? Cu1A N2A C18A C23A 87.5(3) . . . . ? C4A N2A C18A C19A 84.4(4) . . . . ? Cu1A N2A C18A C19A -91.0(3) . . . . ? C23A C18A C19A C20A -0.9(5) . . . . ? N2A C18A C19A C20A 177.6(3) . . . . ? C23A C18A C19A C24A -179.3(3) . . . . ? N2A C18A C19A C24A -0.9(5) . . . . ? C18A C19A C20A C21A 0.5(5) . . . . ? C24A C19A C20A C21A 179.0(3) . . . . ? C19A C20A C21A C22A -0.2(6) . . . . ? C20A C21A C22A C23A 0.2(6) . . . . ? C21A C22A C23A C18A -0.5(5) . . . . ? C21A C22A C23A C27A -179.8(3) . . . . ? C19A C18A C23A C22A 0.9(5) . . . . ? N2A C18A C23A C22A -177.5(3) . . . . ? C19A C18A C23A C27A -179.9(3) . . . . ? N2A C18A C23A C27A 1.7(5) . . . . ? C20A C19A C24A C25A -76.4(4) . . . . ? C18A C19A C24A C25A 102.1(4) . . . . ? C20A C19A C24A C26A 47.8(5) . . . . ? C18A C19A C24A C26A -133.8(4) . . . . ? C22A C23A C27A C29A 70.5(5) . . . . ? C18A C23A C27A C29A -108.7(4) . . . . ? C22A C23A C27A C28A -53.4(5) . . . . ? C18A C23A C27A C28A 127.4(4) . . . . ? N2A Cu1A C30A O1A -175(100) . . . . ? N1A Cu1A C30A O1A 4(4) . . . . ? C30B Cu1B N1B C2B 176.0(2) . . . . ? N2B Cu1B N1B C2B -1.5(2) . . . . ? C30B Cu1B N1B C6B -2.7(3) . . . . ? N2B Cu1B N1B C6B 179.8(2) . . . . ? C30B Cu1B N2B C4B -176.8(2) . . . . ? N1B Cu1B N2B C4B 0.6(2) . . . . ? C30B Cu1B N2B C18B -2.6(3) . . . . ? N1B Cu1B N2B C18B 174.8(2) . . . . ? C6B N1B C2B C3B -179.0(3) . . . . ? Cu1B N1B C2B C3B 2.3(4) . . . . ? C6B N1B C2B C1B 0.6(4) . . . . ? Cu1B N1B C2B C1B -178.1(2) . . . . ? N1B C2B C3B C4B -2.2(5) . . . . ? C1B C2B C3B C4B 178.3(3) . . . . ? C18B N2B C4B C3B -174.4(3) . . . . ? Cu1B N2B C4B C3B -0.5(4) . . . . ? C18B N2B C4B C5B 5.8(4) . . . . ? Cu1B N2B C4B C5B 179.7(2) . . . . ? C2B C3B C4B N2B 1.1(5) . . . . ? C2B C3B C4B C5B -179.1(3) . . . . ? C2B N1B C6B C11B 90.3(4) . . . . ? Cu1B N1B C6B C11B -90.9(3) . . . . ? C2B N1B C6B C7B -94.0(4) . . . . ? Cu1B N1B C6B C7B 84.7(3) . . . . ? C11B C6B C7B C8B -0.5(5) . . . . ? N1B C6B C7B C8B -176.0(3) . . . . ? C11B C6B C7B C12B 177.7(3) . . . . ? N1B C6B C7B C12B 2.2(5) . . . . ? C6B C7B C8B C9B -0.2(5) . . . . ? C12B C7B C8B C9B -178.4(4) . . . . ? C7B C8B C9B C10B 0.5(6) . . . . ? C8B C9B C10B C11B -0.1(6) . . . . ? C9B C10B C11B C6B -0.6(5) . . . . ? C9B C10B C11B C15B 176.1(4) . . . . ? C7B C6B C11B C10B 0.9(5) . . . . ? N1B C6B C11B C10B 176.4(3) . . . . ? C7B C6B C11B C15B -175.7(3) . . . . ? N1B C6B C11B C15B -0.2(5) . . . . ? C8B C7B C12B C13B 72.7(4) . . . . ? C6B C7B C12B C13B -105.5(4) . . . . ? C8B C7B C12B C14B -51.4(5) . . . . ? C6B C7B C12B C14B 130.5(4) . . . . ? C10B C11B C15B C16B -79.4(4) . . . . ? C6B C11B C15B C16B 97.1(4) . . . . ? C10B C11B C15B C17B 44.6(5) . . . . ? C6B C11B C15B C17B -138.9(3) . . . . ? C4B N2B C18B C23B -99.4(3) . . . . ? Cu1B N2B C18B C23B 86.4(3) . . . . ? C4B N2B C18B C19B 86.1(3) . . . . ? Cu1B N2B C18B C19B -88.2(3) . . . . ? C23B C18B C19B C20B -2.6(4) . . . . ? N2B C18B C19B C20B 171.9(3) . . . . ? C23B C18B C19B C24B 179.2(3) . . . . ? N2B C18B C19B C24B -6.4(4) . . . . ? C18B C19B C20B C21B 0.6(5) . . . . ? C24B C19B C20B C21B 178.8(3) . . . . ? C19B C20B C21B C22B 1.3(5) . . . . ? C20B C21B C22B C23B -1.1(5) . . . . ? C21B C22B C23B C18B -0.9(5) . . . . ? C21B C22B C23B C27B -179.1(3) . . . . ? C19B C18B C23B C22B 2.7(4) . . . . ? N2B C18B C23B C22B -171.7(3) . . . . ? C19B C18B C23B C27B -179.0(3) . . . . ? N2B C18B C23B C27B 6.5(4) . . . . ? C20B C19B C24B C26B -75.2(4) . . . . ? C18B C19B C24B C26B 103.0(4) . . . . ? C20B C19B C24B C25B 48.8(4) . . . . ? C18B C19B C24B C25B -133.0(3) . . . . ? C22B C23B C27B C28B 75.0(4) . . . . ? C18B C23B C27B C28B -103.2(3) . . . . ? C22B C23B C27B C29B -48.9(4) . . . . ? C18B C23B C27B C29B 132.9(3) . . . . ? N1B Cu1B C30B O1B -56(10) . . . . ? N2B Cu1B C30B O1B 121(10) . . . . ? C30C Cu1C N1C C2C -174.2(2) . . . . ? N2C Cu1C N1C C2C 0.0(3) . . . . ? C30C Cu1C N1C C6C 0.2(3) . . . . ? N2C Cu1C N1C C6C 174.4(2) . . . . ? C30C Cu1C N2C C4C 173.8(2) . . . . ? N1C Cu1C N2C C4C 0.1(3) . . . . ? C30C Cu1C N2C C18C 0.4(3) . . . . ? N1C Cu1C N2C C18C -173.3(2) . . . . ? C6C N1C C2C C3C -176.2(3) . . . . ? Cu1C N1C C2C C3C -1.8(4) . . . . ? C6C N1C C2C C1C 3.2(4) . . . . ? Cu1C N1C C2C C1C 177.5(2) . . . . ? N1C C2C C3C C4C 4.2(6) . . . . ? C1C C2C C3C C4C -175.1(3) . . . . ? C18C N2C C4C C3C 175.1(3) . . . . ? Cu1C N2C C4C C3C 1.7(5) . . . . ? C18C N2C C4C C5C -4.7(5) . . . . ? Cu1C N2C C4C C5C -178.2(2) . . . . ? C2C C3C C4C N2C -4.2(6) . . . . ? C2C C3C C4C C5C 175.7(3) . . . . ? C2C N1C C6C C7C -93.7(4) . . . . ? Cu1C N1C C6C C7C 91.8(3) . . . . ? C2C N1C C6C C11C 88.6(4) . . . . ? Cu1C N1C C6C C11C -86.0(3) . . . . ? C11C C6C C7C C8C -0.9(5) . . . . ? N1C C6C C7C C8C -178.6(3) . . . . ? C11C C6C C7C C12C 175.2(3) . . . . ? N1C C6C C7C C12C -2.4(4) . . . . ? C6C C7C C8C C9C 0.3(5) . . . . ? C12C C7C C8C C9C -175.9(3) . . . . ? C7C C8C C9C C10C 0.4(6) . . . . ? C8C C9C C10C C11C -0.6(6) . . . . ? C9C C10C C11C C6C 0.0(5) . . . . ? C9C C10C C11C C15C 178.5(4) . . . . ? C7C C6C C11C C10C 0.8(5) . . . . ? N1C C6C C11C C10C 178.4(3) . . . . ? C7C C6C C11C C15C -177.7(3) . . . . ? N1C C6C C11C C15C 0.0(5) . . . . ? C8C C7C C12C C14C 76.9(4) . . . . ? C6C C7C C12C C14C -99.2(4) . . . . ? C8C C7C C12C C13C -46.6(4) . . . . ? C6C C7C C12C C13C 137.3(3) . . . . ? C10C C11C C15C C16C -74.9(5) . . . . ? C6C C11C C15C C16C 103.5(4) . . . . ? C10C C11C C15C C17C 48.8(5) . . . . ? C6C C11C C15C C17C -132.8(4) . . . . ? C4C N2C C18C C23C -93.3(4) . . . . ? Cu1C N2C C18C C23C 80.3(3) . . . . ? C4C N2C C18C C19C 89.6(4) . . . . ? Cu1C N2C C18C C19C -96.8(3) . . . . ? C23C C18C C19C C20C 1.8(5) . . . . ? N2C C18C C19C C20C 178.9(3) . . . . ? C23C C18C C19C C24C -176.1(3) . . . . ? N2C C18C C19C C24C 1.0(5) . . . . ? C18C C19C C20C C21C -0.2(5) . . . . ? C24C C19C C20C C21C 177.7(3) . . . . ? C19C C20C C21C C22C -1.4(6) . . . . ? C20C C21C C22C C23C 1.5(6) . . . . ? C21C C22C C23C C18C 0.1(6) . . . . ? C21C C22C C23C C27C -178.7(4) . . . . ? C19C C18C C23C C22C -1.7(5) . . . . ? N2C C18C C23C C22C -178.8(3) . . . . ? C19C C18C C23C C27C 177.1(3) . . . . ? N2C C18C C23C C27C -0.1(5) . . . . ? C20C C19C C24C C26C -80.1(4) . . . . ? C18C C19C C24C C26C 97.8(4) . . . . ? C20C C19C C24C C25C 44.5(5) . . . . ? C18C C19C C24C C25C -137.6(4) . . . . ? C22C C23C C27C C28C -56.4(5) . . . . ? C18C C23C C27C C28C 124.8(4) . . . . ? C22C C23C C27C C29C 64.9(5) . . . . ? C18C C23C C27C C29C -113.8(4) . . . . ? N2C Cu1C C30C O1C -118(4) . . . . ? N1C Cu1C C30C O1C 54(4) . . . . ? C30D Cu1D N1D C2D -178.3(3) . . . . ? N2D Cu1D N1D C2D -1.8(3) . . . . ? C30D Cu1D N1D C6D -1.1(3) . . . . ? N2D Cu1D N1D C6D 175.4(2) . . . . ? C30D Cu1D N2D C4D 173.8(3) . . . . ? N1D Cu1D N2D C4D -2.2(2) . . . . ? C30D Cu1D N2D C18D -4.4(3) . . . . ? N1D Cu1D N2D C18D 179.6(2) . . . . ? C6D N1D C2D C3D -173.9(3) . . . . ? Cu1D N1D C2D C3D 3.2(4) . . . . ? C6D N1D C2D C1D 5.9(4) . . . . ? Cu1D N1D C2D C1D -177.1(2) . . . . ? N1D C2D C3D C4D -0.5(5) . . . . ? C1D C2D C3D C4D 179.7(3) . . . . ? C18D N2D C4D C3D -176.8(3) . . . . ? Cu1D N2D C4D C3D 5.0(4) . . . . ? C18D N2D C4D C5D 3.4(4) . . . . ? Cu1D N2D C4D C5D -174.8(2) . . . . ? C2D C3D C4D N2D -4.1(5) . . . . ? C2D C3D C4D C5D 175.7(3) . . . . ? C2D N1D C6D C11D -93.6(4) . . . . ? Cu1D N1D C6D C11D 89.2(3) . . . . ? C2D N1D C6D C7D 93.2(4) . . . . ? Cu1D N1D C6D C7D -84.0(3) . . . . ? C11D C6D C7D C8D -1.5(5) . . . . ? N1D C6D C7D C8D 171.6(3) . . . . ? C11D C6D C7D C12D 178.4(3) . . . . ? N1D C6D C7D C12D -8.5(5) . . . . ? C6D C7D C8D C9D -0.6(6) . . . . ? C12D C7D C8D C9D 179.5(4) . . . . ? C7D C8D C9D C10D 2.0(6) . . . . ? C8D C9D C10D C11D -1.3(6) . . . . ? C9D C10D C11D C6D -0.8(5) . . . . ? C9D C10D C11D C15D 179.8(3) . . . . ? C7D C6D C11D C10D 2.2(5) . . . . ? N1D C6D C11D C10D -170.9(3) . . . . ? C7D C6D C11D C15D -178.4(3) . . . . ? N1D C6D C11D C15D 8.5(5) . . . . ? C8D C7D C12D C13D -68.7(5) . . . . ? C6D C7D C12D C13D 111.3(4) . . . . ? C8D C7D C12D C14D 58.1(5) . . . . ? C6D C7D C12D C14D -121.8(4) . . . . ? C10D C11D C15D C16D 73.0(4) . . . . ? C6D C11D C15D C16D -106.4(4) . . . . ? C10D C11D C15D C17D -51.1(4) . . . . ? C6D C11D C15D C17D 129.5(3) . . . . ? C4D N2D C18D C19D -99.5(3) . . . . ? Cu1D N2D C18D C19D 78.8(3) . . . . ? C4D N2D C18D C23D 84.9(4) . . . . ? Cu1D N2D C18D C23D -96.9(3) . . . . ? C23D C18D C19D C20D 0.2(5) . . . . ? N2D C18D C19D C20D -175.3(3) . . . . ? C23D C18D C19D C24D -179.3(3) . . . . ? N2D C18D C19D C24D 5.2(5) . . . . ? C18D C19D C20D C21D 0.0(5) . . . . ? C24D C19D C20D C21D 179.6(4) . . . . ? C19D C20D C21D C22D -0.3(6) . . . . ? C20D C21D C22D C23D 0.3(6) . . . . ? C21D C22D C23D C18D -0.1(6) . . . . ? C21D C22D C23D C27D 177.3(4) . . . . ? C19D C18D C23D C22D -0.2(5) . . . . ? N2D C18D C23D C22D 175.4(3) . . . . ? C19D C18D C23D C27D -177.5(3) . . . . ? N2D C18D C23D C27D -2.0(5) . . . . ? C20D C19D C24D C26D -65.9(4) . . . . ? C18D C19D C24D C26D 113.6(4) . . . . ? C20D C19D C24D C25D 58.7(5) . . . . ? C18D C19D C24D C25D -121.8(4) . . . . ? C22D C23D C27D C28D 36.3(5) . . . . ? C18D C23D C27D C28D -146.4(3) . . . . ? C22D C23D C27D C29D -88.1(4) . . . . ? C18D C23D C27D C29D 89.1(4) . . . . ? N2D Cu1D C30D O1D -137(5) . . . . ? N1D Cu1D C30D O1D 38(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.289 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.051 #====END data_06191n _database_code_depnum_ccdc_archive 'CCDC 617544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (L2)Cu(CO) _chemical_melting_point ? _chemical_formula_moiety 'C30 H35 Cu F6 N2 O' _chemical_formula_sum 'C30 H35 Cu F6 N2 O' _chemical_formula_weight 617.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.339(2) _cell_length_b 15.282(2) _cell_length_c 24.409(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6094.8(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3887 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'cut block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8001 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59729 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.39 _reflns_number_total 6233 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0297P)^2^+10.3188P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6233 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 Cu1 Cu 0.03075(2) 0.70631(2) 0.160561(16) 0.02680(11) Uani 1 1 d . . . O1 O 0.1257(2) 0.8510(2) 0.20611(13) 0.0704(9) Uani 1 1 d . . . F1 F -0.22029(15) 0.6349(2) 0.06459(13) 0.0896(10) Uani 1 1 d . . . F2 F -0.1310(2) 0.65479(18) 0.00349(10) 0.0903(11) Uani 1 1 d . . . F3 F -0.15808(16) 0.52729(15) 0.02967(10) 0.0648(7) Uani 1 1 d . . . F4 F 0.01991(19) 0.40802(14) 0.21584(10) 0.0707(8) Uani 1 1 d . . . F5 F 0.10064(15) 0.40221(15) 0.14845(14) 0.0816(9) Uani 1 1 d . . . F6 F -0.02419(16) 0.37068(13) 0.13813(11) 0.0647(7) Uani 1 1 d . . . N1 N -0.05660(15) 0.69425(16) 0.10776(10) 0.0255(6) Uani 1 1 d . . . N2 N 0.05170(15) 0.58342(16) 0.17465(10) 0.0252(6) Uani 1 1 d . . . C1 C -0.1483(3) 0.6087(2) 0.04706(16) 0.0434(9) Uani 1 1 d . . . C2 C -0.08179(19) 0.6160(2) 0.09168(13) 0.0291(7) Uani 1 1 d . . . C3 C -0.05331(19) 0.5358(2) 0.11178(13) 0.0289(7) Uani 1 1 d . . . H3A H -0.0792 0.4849 0.0977 0.035 Uiso 1 1 calc R . . C4 C 0.00867(18) 0.52195(19) 0.15012(12) 0.0260(7) Uani 1 1 d . . . C5 C 0.0264(2) 0.4252(2) 0.16281(15) 0.0389(8) Uani 1 1 d . . . C6 C -0.0906(2) 0.77471(19) 0.08623(13) 0.0281(7) Uani 1 1 d . . . C7 C -0.0491(2) 0.8181(2) 0.04361(14) 0.0376(9) Uani 1 1 d . . . C8 C -0.0826(3) 0.8974(2) 0.02518(15) 0.0456(10) Uani 1 1 d . . . H8A H -0.0561 0.9282 -0.0036 0.055 Uiso 1 1 calc R . . C9 C -0.1524(3) 0.9313(2) 0.04768(16) 0.0483(10) Uani 1 1 d . . . H9A H -0.1746 0.9844 0.0338 0.058 Uiso 1 1 calc R . . C10 C -0.1907(2) 0.8891(2) 0.09016(16) 0.0423(9) Uani 1 1 d . . . H10A H -0.2387 0.9139 0.1057 0.051 Uiso 1 1 calc R . . C11 C -0.1605(2) 0.8105(2) 0.11102(14) 0.0324(8) Uani 1 1 d . . . C12 C 0.0286(3) 0.7823(3) 0.01956(16) 0.0541(11) Uani 1 1 d . . . H12A H 0.0374 0.7220 0.0343 0.065 Uiso 1 1 calc R . . C13 C 0.1019(3) 0.8385(3) 0.0352(2) 0.0733(14) Uani 1 1 d . . . H13A H 0.1055 0.8425 0.0752 0.110 Uiso 1 1 calc R . . H13B H 0.0952 0.8972 0.0197 0.110 Uiso 1 1 calc R . . H13C H 0.1520 0.8119 0.0208 0.110 Uiso 1 1 calc R . . C14 C 0.0238(4) 0.7771(5) -0.0432(2) 0.107(2) Uani 1 1 d . . . H14A H -0.0300 0.7548 -0.0540 0.160 Uiso 1 1 calc R . . H14B H 0.0665 0.7377 -0.0568 0.160 Uiso 1 1 calc R . . H14C H 0.0319 0.8356 -0.0588 0.160 Uiso 1 1 calc R . . C15 C -0.2002(2) 0.7674(2) 0.16032(15) 0.0363(8) Uani 1 1 d . . . H15A H -0.1906 0.7030 0.1573 0.044 Uiso 1 1 calc R . . C16 C -0.2925(2) 0.7818(3) 0.16405(19) 0.0560(11) Uani 1 1 d . . . H16A H -0.3183 0.7639 0.1296 0.084 Uiso 1 1 calc R . . H16B H -0.3037 0.8439 0.1707 0.084 Uiso 1 1 calc R . . H16C H -0.3148 0.7469 0.1942 0.084 Uiso 1 1 calc R . . C17 C -0.1601(2) 0.7986(3) 0.21340(15) 0.0451(9) Uani 1 1 d . . . H17A H -0.1012 0.7863 0.2121 0.068 Uiso 1 1 calc R . . H17B H -0.1845 0.7678 0.2446 0.068 Uiso 1 1 calc R . . H17C H -0.1686 0.8617 0.2176 0.068 Uiso 1 1 calc R . . C18 C 0.12097(18) 0.56600(19) 0.21013(13) 0.0260(7) Uani 1 1 d . . . C19 C 0.10920(19) 0.5622(2) 0.26680(13) 0.0274(7) Uani 1 1 d . . . C20 C 0.1784(2) 0.5541(2) 0.29959(14) 0.0323(8) Uani 1 1 d . . . H20A H 0.1721 0.5514 0.3382 0.039 Uiso 1 1 calc R . . C21 C 0.2560(2) 0.5500(2) 0.27729(14) 0.0357(8) Uani 1 1 d . . . H21A H 0.3024 0.5444 0.3005 0.043 Uiso 1 1 calc R . . C22 C 0.2658(2) 0.5541(2) 0.22134(15) 0.0381(8) Uani 1 1 d . . . H22A H 0.3194 0.5509 0.2063 0.046 Uiso 1 1 calc R . . C23 C 0.1993(2) 0.5629(2) 0.18626(14) 0.0337(8) Uani 1 1 d . . . C24 C 0.0244(2) 0.5688(2) 0.29202(13) 0.0315(7) Uani 1 1 d . . . H24A H -0.0161 0.5494 0.2638 0.038 Uiso 1 1 calc R . . C25 C 0.0040(2) 0.6629(2) 0.30718(16) 0.0410(9) Uani 1 1 d . . . H25A H 0.0106 0.7004 0.2749 0.062 Uiso 1 1 calc R . . H25B H 0.0411 0.6828 0.3362 0.062 Uiso 1 1 calc R . . H25C H -0.0526 0.6662 0.3202 0.062 Uiso 1 1 calc R . . C26 C 0.0142(2) 0.5096(3) 0.34216(16) 0.0467(9) Uani 1 1 d . . . H26A H 0.0291 0.4494 0.3324 0.070 Uiso 1 1 calc R . . H26B H -0.0429 0.5111 0.3544 0.070 Uiso 1 1 calc R . . H26C H 0.0499 0.5302 0.3717 0.070 Uiso 1 1 calc R . . C27 C 0.2129(2) 0.5706(3) 0.12452(16) 0.0529(11) Uani 1 1 d . . . H27A H 0.1581 0.5676 0.1063 0.064 Uiso 1 1 calc R . . C28 C 0.2509(3) 0.6593(3) 0.1105(2) 0.0833(17) Uani 1 1 d . . . H28A H 0.2569 0.6644 0.0706 0.125 Uiso 1 1 calc R . . H28B H 0.3048 0.6640 0.1278 0.125 Uiso 1 1 calc R . . H28C H 0.2154 0.7063 0.1239 0.125 Uiso 1 1 calc R . . C29 C 0.2647(3) 0.4957(4) 0.10215(17) 0.0679(14) Uani 1 1 d . . . H29A H 0.2412 0.4397 0.1139 0.102 Uiso 1 1 calc R . . H29B H 0.3207 0.5008 0.1162 0.102 Uiso 1 1 calc R . . H29C H 0.2655 0.4984 0.0620 0.102 Uiso 1 1 calc R . . C30 C 0.0873(2) 0.7965(2) 0.18843(15) 0.0389(8) 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 0.02531(19) 0.02429(19) 0.0308(2) 0.00030(17) -0.00622(17) -0.00266(17) O1 0.080(2) 0.0547(19) 0.076(2) -0.0063(16) -0.0219(18) -0.0331(17) F1 0.0432(16) 0.120(3) 0.106(2) -0.046(2) -0.0405(15) 0.0165(16) F2 0.145(3) 0.0744(19) 0.0517(16) 0.0228(14) -0.0594(17) -0.0503(19) F3 0.0823(18) 0.0440(13) 0.0679(16) -0.0088(12) -0.0434(14) -0.0094(12) F4 0.132(2) 0.0305(12) 0.0499(14) 0.0069(10) -0.0146(15) -0.0064(14) F5 0.0551(16) 0.0375(13) 0.152(3) -0.0015(15) 0.0183(17) 0.0176(12) F6 0.0819(18) 0.0239(11) 0.0882(18) -0.0070(11) -0.0421(15) -0.0041(12) N1 0.0255(13) 0.0268(14) 0.0244(13) 0.0024(11) -0.0046(11) -0.0015(11) N2 0.0225(13) 0.0256(13) 0.0276(14) -0.0022(11) -0.0030(10) 0.0032(11) C1 0.053(3) 0.034(2) 0.043(2) 0.0010(17) -0.0220(19) -0.0088(18) C2 0.0249(17) 0.0372(18) 0.0253(17) -0.0024(15) -0.0035(13) -0.0035(14) C3 0.0308(18) 0.0238(16) 0.0320(18) -0.0040(14) -0.0055(14) -0.0043(13) C4 0.0262(16) 0.0239(16) 0.0280(17) -0.0009(13) 0.0005(13) 0.0024(13) C5 0.045(2) 0.0293(17) 0.043(2) -0.0054(16) -0.0113(18) 0.0012(17) C6 0.0329(17) 0.0240(17) 0.0274(17) 0.0043(13) -0.0111(14) -0.0047(13) C7 0.051(2) 0.0367(19) 0.0249(17) 0.0026(15) -0.0043(16) -0.0088(16) C8 0.069(3) 0.037(2) 0.031(2) 0.0110(17) -0.0096(19) -0.013(2) C9 0.059(3) 0.035(2) 0.051(2) 0.0130(19) -0.021(2) 0.0030(19) C10 0.040(2) 0.038(2) 0.049(2) 0.0035(18) -0.0132(18) 0.0014(17) C11 0.0299(18) 0.0291(18) 0.0383(19) 0.0037(15) -0.0097(15) -0.0008(14) C12 0.073(3) 0.048(2) 0.042(2) 0.0027(18) 0.018(2) -0.008(2) C13 0.064(3) 0.079(4) 0.077(3) 0.001(3) 0.009(3) -0.002(3) C14 0.112(5) 0.154(6) 0.053(3) -0.028(4) 0.024(3) -0.017(5) C15 0.0285(17) 0.0300(17) 0.050(2) 0.0034(17) 0.0019(17) 0.0005(13) C16 0.0309(19) 0.062(3) 0.075(3) 0.001(2) 0.001(2) 0.0007(19) C17 0.042(2) 0.051(2) 0.043(2) 0.0088(19) 0.0036(17) -0.0010(19) C18 0.0241(16) 0.0207(15) 0.0332(18) -0.0014(13) -0.0022(13) 0.0021(13) C19 0.0280(17) 0.0239(16) 0.0302(17) -0.0030(13) -0.0029(13) -0.0020(13) C20 0.0331(19) 0.0322(18) 0.0316(18) -0.0033(15) -0.0062(15) -0.0013(15) C21 0.0267(17) 0.0379(19) 0.042(2) -0.0035(17) -0.0120(16) 0.0017(15) C22 0.0253(19) 0.043(2) 0.046(2) -0.0024(17) -0.0021(15) 0.0058(16) C23 0.0259(18) 0.040(2) 0.0351(19) 0.0001(16) -0.0012(14) 0.0055(15) C24 0.0291(17) 0.0381(18) 0.0273(17) -0.0034(14) -0.0015(14) -0.0010(16) C25 0.038(2) 0.041(2) 0.044(2) -0.0007(17) 0.0083(17) 0.0078(16) C26 0.042(2) 0.046(2) 0.053(2) 0.0085(19) 0.0075(19) 0.0016(17) C27 0.032(2) 0.090(3) 0.038(2) 0.009(2) 0.0031(17) 0.012(2) C28 0.082(4) 0.098(4) 0.070(3) 0.032(3) 0.031(3) 0.017(3) C29 0.047(3) 0.114(4) 0.044(3) -0.020(3) 0.005(2) 0.012(3) C30 0.040(2) 0.0339(19) 0.043(2) 0.0061(18) -0.0135(17) -0.0034(18) _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 C30 1.794(4) . ? Cu1 N1 1.932(2) . ? Cu1 N2 1.940(2) . ? O1 C30 1.128(4) . ? F1 C1 1.315(5) . ? F2 C1 1.306(4) . ? F3 C1 1.325(4) . ? F4 C5 1.325(4) . ? F5 C5 1.311(4) . ? F6 C5 1.318(4) . ? N1 C2 1.324(4) . ? N1 C6 1.448(4) . ? N2 C4 1.317(4) . ? N2 C18 1.450(4) . ? C1 C2 1.542(5) . ? C2 C3 1.399(4) . ? C3 C4 1.395(4) . ? C4 C5 1.539(4) . ? C6 C11 1.403(5) . ? C6 C7 1.408(5) . ? C7 C8 1.403(5) . ? C7 C12 1.503(5) . ? C8 C9 1.369(6) . ? C9 C10 1.372(5) . ? C10 C11 1.395(5) . ? C11 C15 1.518(5) . ? C12 C13 1.521(6) . ? C12 C14 1.535(6) . ? C15 C16 1.527(5) . ? C15 C17 1.529(5) . ? C18 C19 1.398(4) . ? C18 C23 1.407(4) . ? C19 C20 1.391(4) . ? C19 C24 1.520(4) . ? C20 C21 1.381(5) . ? C21 C22 1.377(5) . ? C22 C23 1.391(5) . ? C23 C27 1.528(5) . ? C24 C25 1.522(5) . ? C24 C26 1.532(5) . ? C27 C29 1.524(6) . ? C27 C28 1.530(6) . ? 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 C30 Cu1 N1 135.00(13) . . ? C30 Cu1 N2 125.86(13) . . ? N1 Cu1 N2 98.99(10) . . ? C2 N1 C6 122.7(3) . . ? C2 N1 Cu1 120.9(2) . . ? C6 N1 Cu1 116.40(19) . . ? C4 N2 C18 123.9(3) . . ? C4 N2 Cu1 121.1(2) . . ? C18 N2 Cu1 114.93(19) . . ? F2 C1 F1 107.1(4) . . ? F2 C1 F3 105.8(3) . . ? F1 C1 F3 106.3(3) . . ? F2 C1 C2 112.6(3) . . ? F1 C1 C2 112.3(3) . . ? F3 C1 C2 112.3(3) . . ? N1 C2 C3 125.7(3) . . ? N1 C2 C1 119.5(3) . . ? C3 C2 C1 114.8(3) . . ? C4 C3 C2 127.5(3) . . ? N2 C4 C3 125.7(3) . . ? N2 C4 C5 119.6(3) . . ? C3 C4 C5 114.7(3) . . ? F5 C5 F6 106.8(3) . . ? F5 C5 F4 106.4(3) . . ? F6 C5 F4 105.8(3) . . ? F5 C5 C4 112.2(3) . . ? F6 C5 C4 113.4(3) . . ? F4 C5 C4 111.8(3) . . ? C11 C6 C7 121.8(3) . . ? C11 C6 N1 119.1(3) . . ? C7 C6 N1 118.9(3) . . ? C8 C7 C6 117.2(3) . . ? C8 C7 C12 121.2(3) . . ? C6 C7 C12 121.6(3) . . ? C9 C8 C7 121.6(4) . . ? C8 C9 C10 120.3(3) . . ? C9 C10 C11 121.3(4) . . ? C10 C11 C6 117.8(3) . . ? C10 C11 C15 120.8(3) . . ? C6 C11 C15 121.4(3) . . ? C7 C12 C13 111.2(3) . . ? C7 C12 C14 111.4(4) . . ? C13 C12 C14 108.7(4) . . ? C11 C15 C16 114.1(3) . . ? C11 C15 C17 110.7(3) . . ? C16 C15 C17 109.2(3) . . ? C19 C18 C23 122.2(3) . . ? C19 C18 N2 119.4(3) . . ? C23 C18 N2 118.0(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C24 120.9(3) . . ? C18 C19 C24 121.6(3) . . ? C21 C20 C19 121.6(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 121.6(3) . . ? C22 C23 C18 117.4(3) . . ? C22 C23 C27 120.1(3) . . ? C18 C23 C27 122.5(3) . . ? C19 C24 C25 111.1(3) . . ? C19 C24 C26 112.5(3) . . ? C25 C24 C26 109.9(3) . . ? C29 C27 C23 112.1(3) . . ? C29 C27 C28 111.0(4) . . ? C23 C27 C28 110.4(4) . . ? O1 C30 Cu1 177.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 Cu1 N1 C2 174.0(3) . . . . ? N2 Cu1 N1 C2 -1.6(3) . . . . ? C30 Cu1 N1 C6 -4.4(3) . . . . ? N2 Cu1 N1 C6 180.0(2) . . . . ? C30 Cu1 N2 C4 -176.9(2) . . . . ? N1 Cu1 N2 C4 -0.8(3) . . . . ? C30 Cu1 N2 C18 -1.4(3) . . . . ? N1 Cu1 N2 C18 174.7(2) . . . . ? C6 N1 C2 C3 -178.1(3) . . . . ? Cu1 N1 C2 C3 3.5(4) . . . . ? C6 N1 C2 C1 1.8(5) . . . . ? Cu1 N1 C2 C1 -176.5(2) . . . . ? F2 C1 C2 N1 51.3(5) . . . . ? F1 C1 C2 N1 -69.7(4) . . . . ? F3 C1 C2 N1 170.6(3) . . . . ? F2 C1 C2 C3 -128.7(4) . . . . ? F1 C1 C2 C3 110.3(4) . . . . ? F3 C1 C2 C3 -9.5(5) . . . . ? N1 C2 C3 C4 -3.2(6) . . . . ? C1 C2 C3 C4 176.9(3) . . . . ? C18 N2 C4 C3 -173.6(3) . . . . ? Cu1 N2 C4 C3 1.5(4) . . . . ? C18 N2 C4 C5 5.6(5) . . . . ? Cu1 N2 C4 C5 -179.3(2) . . . . ? C2 C3 C4 N2 0.3(6) . . . . ? C2 C3 C4 C5 -179.0(3) . . . . ? N2 C4 C5 F5 -62.8(4) . . . . ? C3 C4 C5 F5 116.5(3) . . . . ? N2 C4 C5 F6 176.1(3) . . . . ? C3 C4 C5 F6 -4.6(5) . . . . ? N2 C4 C5 F4 56.6(4) . . . . ? C3 C4 C5 F4 -124.1(3) . . . . ? C2 N1 C6 C11 87.2(4) . . . . ? Cu1 N1 C6 C11 -94.4(3) . . . . ? C2 N1 C6 C7 -97.4(4) . . . . ? Cu1 N1 C6 C7 81.0(3) . . . . ? C11 C6 C7 C8 -2.6(5) . . . . ? N1 C6 C7 C8 -177.9(3) . . . . ? C11 C6 C7 C12 176.1(3) . . . . ? N1 C6 C7 C12 0.9(5) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C12 C7 C8 C9 -178.6(4) . . . . ? C7 C8 C9 C10 1.6(6) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C6 -1.5(5) . . . . ? C9 C10 C11 C15 176.1(3) . . . . ? C7 C6 C11 C10 3.3(5) . . . . ? N1 C6 C11 C10 178.5(3) . . . . ? C7 C6 C11 C15 -174.3(3) . . . . ? N1 C6 C11 C15 0.9(4) . . . . ? C8 C7 C12 C13 68.8(5) . . . . ? C6 C7 C12 C13 -109.9(4) . . . . ? C8 C7 C12 C14 -52.5(5) . . . . ? C6 C7 C12 C14 128.8(4) . . . . ? C10 C11 C15 C16 32.7(5) . . . . ? C6 C11 C15 C16 -149.7(3) . . . . ? C10 C11 C15 C17 -90.9(4) . . . . ? C6 C11 C15 C17 86.7(4) . . . . ? C4 N2 C18 C19 -95.8(4) . . . . ? Cu1 N2 C18 C19 88.9(3) . . . . ? C4 N2 C18 C23 90.9(4) . . . . ? Cu1 N2 C18 C23 -84.4(3) . . . . ? C23 C18 C19 C20 -0.7(5) . . . . ? N2 C18 C19 C20 -173.7(3) . . . . ? C23 C18 C19 C24 177.8(3) . . . . ? N2 C18 C19 C24 4.8(4) . . . . ? C18 C19 C20 C21 0.0(5) . . . . ? C24 C19 C20 C21 -178.5(3) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C18 -1.0(5) . . . . ? C21 C22 C23 C27 177.8(4) . . . . ? C19 C18 C23 C22 1.2(5) . . . . ? N2 C18 C23 C22 174.3(3) . . . . ? C19 C18 C23 C27 -177.6(3) . . . . ? N2 C18 C23 C27 -4.5(5) . . . . ? C20 C19 C24 C25 85.4(4) . . . . ? C18 C19 C24 C25 -93.0(4) . . . . ? C20 C19 C24 C26 -38.4(4) . . . . ? C18 C19 C24 C26 143.2(3) . . . . ? C22 C23 C27 C29 53.7(5) . . . . ? C18 C23 C27 C29 -127.6(4) . . . . ? C22 C23 C27 C28 -70.6(5) . . . . ? C18 C23 C27 C28 108.1(4) . . . . ? N1 Cu1 C30 O1 -147(7) . . . . ? N2 Cu1 C30 O1 27(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.465 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.070 #====END