# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2129 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Dr. Malcolm A. Halcrow' _publ_contact_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 2336506' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email malcolmh@chem.leeds.ac.uk _publ_requested_journal 'Dalton Transactions' _publ_contact_letter ; The following set of data is for four structures included in a manuscript we have just submitted to the Dalton Transactions office. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Copper Complexes of Pyridine-2,6-dicarbaldimine Derivatives, and of 1,3-Bis-(pyridine-2-yl)pyrazole. Effects of Ligand Bulk and Conformational Strain on the Ground State of a Six-co-ordinate Copper(II) Ion. ; loop_ _publ_author_name _publ_author_address 'Joanne M. Holland' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Xiaoming Liu' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Jing P. Zhao' ; CW EPR Service Centre. Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK ; 'Frank E. Mabbs' ; CW EPR Service Centre. Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Mark Thornton-Pett' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #================================================================= data_mh3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-bis-{N-cyclohexylcarbaldimino}pyridine]copper(II) ditetrafluoroborate nitromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H54 Cu N6, 2B F4, C H3 N O2' _chemical_formula_sum 'C41 H57 B2 Cu F8 N7 O2' _chemical_formula_weight 917.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6323(1) _cell_length_b 17.8182(1) _cell_length_c 19.2083(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.5180(6) _cell_angle_gamma 90.00 _cell_volume 4516.77(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7597 _exptl_absorpt_correction_T_max 0.8682 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; The unit cell was refined using all data ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70847 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8844 _reflns_number_gt 8056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms of the BF~4~^-^ anion centred on B2 are disordered over two orientations: F5-F8, occupancy 0.6 F9-F12, occupancy 0.4 All B-F bonds were restrained to 1.36(2)\%A. The half-occupied atoms C2S-C5S represent a badly disordered region of solvent lying across a crystallographic 2-fold axis. The identity of the solvent occupying this region of the lattic is unclear. All non-H atoms with occupancy >0.5 were refined anisotropically. ; _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^)+(0.0877P)^2^+6.6932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8844 _refine_ls_number_parameters 566 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.006 _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 0.26314(2) 0.031601(17) 0.763824(16) 0.02270(14) Uani 1 1 d . . . N1 N 0.13901(17) -0.02076(12) 0.76467(12) 0.0244(5) Uani 1 1 d . . . C1 C 0.1166(2) -0.08436(15) 0.72716(14) 0.0266(5) Uani 1 1 d . . . C2 C 0.0311(2) -0.12510(18) 0.72909(17) 0.0361(7) Uani 1 1 d . . . H2 H 0.0155 -0.1706 0.7029 0.043 Uiso 1 1 calc R . . C3 C -0.0315(2) -0.0976(2) 0.7705(2) 0.0437(8) Uani 1 1 d . . . H3 H -0.0907 -0.1246 0.7728 0.052 Uiso 1 1 calc R . . C4 C -0.0079(2) -0.03100(19) 0.80848(19) 0.0402(7) Uani 1 1 d . . . H4 H -0.0506 -0.0116 0.8363 0.048 Uiso 1 1 calc R . . C5 C 0.0801(2) 0.00658(16) 0.80468(15) 0.0293(6) Uani 1 1 d . . . C6 C 0.1215(2) 0.07663(17) 0.84184(15) 0.0312(6) Uani 1 1 d . . . H6 H 0.0867 0.1033 0.8712 0.037 Uiso 1 1 calc R . . N2 N 0.20614(17) 0.09973(13) 0.83280(12) 0.0262(5) Uani 1 1 d . . . C7 C 0.2533(2) 0.16865(15) 0.86907(15) 0.0285(6) Uani 1 1 d . . . H7 H 0.3062 0.1848 0.8444 0.034 Uiso 1 1 calc R . . C8 C 0.3073(2) 0.15092(17) 0.94682(17) 0.0367(7) Uani 1 1 d . . . H8A H 0.3579 0.1108 0.9480 0.044 Uiso 1 1 calc R . . H8B H 0.2575 0.1325 0.9725 0.044 Uiso 1 1 calc R . . C9 C 0.3605(2) 0.22111(19) 0.98492(17) 0.0407(7) Uani 1 1 d . . . H9A H 0.3906 0.2095 1.0362 0.049 Uiso 1 1 calc R . . H9B H 0.4160 0.2358 0.9630 0.049 Uiso 1 1 calc R . . C10 C 0.2867(2) 0.28585(18) 0.97923(17) 0.0391(7) Uani 1 1 d . . . H10A H 0.3237 0.3310 1.0018 0.047 Uiso 1 1 calc R . . H10B H 0.2352 0.2731 1.0056 0.047 Uiso 1 1 calc R . . C11 C 0.2345(3) 0.30280(17) 0.90143(19) 0.0421(7) Uani 1 1 d . . . H11A H 0.2854 0.3194 0.8759 0.051 Uiso 1 1 calc R . . H11B H 0.1853 0.3441 0.8994 0.051 Uiso 1 1 calc R . . C12 C 0.1794(2) 0.23355(17) 0.86418(18) 0.0397(7) Uani 1 1 d . . . H12A H 0.1249 0.2192 0.8873 0.048 Uiso 1 1 calc R . . H12B H 0.1479 0.2452 0.8131 0.048 Uiso 1 1 calc R . . C13 C 0.1948(2) -0.10467(15) 0.68944(14) 0.0256(5) Uani 1 1 d . . . H13 H 0.1890 -0.1485 0.6605 0.031 Uiso 1 1 calc R . . N3 N 0.27073(16) -0.06033(12) 0.69770(11) 0.0234(4) Uani 1 1 d . . . C14 C 0.3573(2) -0.07756(15) 0.66751(14) 0.0266(5) Uani 1 1 d . . . H14 H 0.4201 -0.0689 0.7067 0.032 Uiso 1 1 calc R . . C15 C 0.3600(2) -0.02224(16) 0.60757(16) 0.0317(6) Uani 1 1 d . . . H15A H 0.3571 0.0297 0.6252 0.038 Uiso 1 1 calc R . . H15B H 0.3004 -0.0303 0.5666 0.038 Uiso 1 1 calc R . . C16 C 0.4573(3) -0.03310(18) 0.5828(2) 0.0429(8) Uani 1 1 d . . . H16A H 0.4576 0.0020 0.5429 0.051 Uiso 1 1 calc R . . H16B H 0.5166 -0.0214 0.6230 0.051 Uiso 1 1 calc R . . C17 C 0.4655(3) -0.1134(2) 0.5577(2) 0.0487(9) Uani 1 1 d . . . H17A H 0.5309 -0.1199 0.5448 0.058 Uiso 1 1 calc R . . H17B H 0.4102 -0.1232 0.5143 0.058 Uiso 1 1 calc R . . C18 C 0.4588(3) -0.16939(18) 0.6164(2) 0.0446(8) Uani 1 1 d . . . H18A H 0.5185 -0.1633 0.6577 0.054 Uiso 1 1 calc R . . H18B H 0.4599 -0.2211 0.5977 0.054 Uiso 1 1 calc R . . C19 C 0.3622(2) -0.15806(16) 0.64180(17) 0.0347(6) Uani 1 1 d . . . H19A H 0.3022 -0.1687 0.6018 0.042 Uiso 1 1 calc R . . H19B H 0.3615 -0.1933 0.6815 0.042 Uiso 1 1 calc R . . N4 N 0.39256(16) 0.08552(12) 0.76491(11) 0.0234(4) Uani 1 1 d . . . C20 C 0.3915(2) 0.14596(15) 0.72280(14) 0.0261(5) Uani 1 1 d . . . C21 C 0.4794(2) 0.18436(16) 0.72054(17) 0.0335(6) Uani 1 1 d . . . H21 H 0.4764 0.2282 0.6919 0.040 Uiso 1 1 calc R . . C22 C 0.5716(2) 0.15742(18) 0.76091(18) 0.0370(7) Uani 1 1 d . . . H22 H 0.6330 0.1816 0.7589 0.044 Uiso 1 1 calc R . . C23 C 0.5733(2) 0.09517(17) 0.80401(16) 0.0330(6) Uani 1 1 d . . . H23 H 0.6358 0.0759 0.8319 0.040 Uiso 1 1 calc R . . C24 C 0.48212(19) 0.06095(15) 0.80609(14) 0.0262(5) Uani 1 1 d . . . C25 C 0.2926(2) 0.16753(15) 0.67591(14) 0.0272(5) Uani 1 1 d . . . H25 H 0.2861 0.2129 0.6492 0.033 Uiso 1 1 calc R . . N5 N 0.21594(16) 0.12566(12) 0.67116(12) 0.0253(5) Uani 1 1 d . . . C26 C 0.1226(2) 0.14727(16) 0.61765(15) 0.0292(6) Uani 1 1 d . . . H26 H 0.1303 0.1998 0.6014 0.035 Uiso 1 1 calc R . . C27 C 0.1078(2) 0.09473(17) 0.55299(15) 0.0337(6) Uani 1 1 d . . . H27A H 0.1001 0.0425 0.5684 0.040 Uiso 1 1 calc R . . H27B H 0.1681 0.0969 0.5331 0.040 Uiso 1 1 calc R . . C28 C 0.0135(3) 0.1176(2) 0.49493(17) 0.0452(8) Uani 1 1 d . . . H28A H 0.0236 0.1682 0.4767 0.054 Uiso 1 1 calc R . . H28B H 0.0030 0.0820 0.4542 0.054 Uiso 1 1 calc R . . C29 C -0.0798(3) 0.1178(2) 0.5251(2) 0.0530(9) Uani 1 1 d . . . H29A H -0.1386 0.1370 0.4879 0.064 Uiso 1 1 calc R . . H29B H -0.0953 0.0658 0.5369 0.064 Uiso 1 1 calc R . . C30 C -0.0645(3) 0.1661(2) 0.5920(2) 0.0505(9) Uani 1 1 d . . . H30A H -0.1243 0.1611 0.6121 0.061 Uiso 1 1 calc R . . H30B H -0.0592 0.2194 0.5787 0.061 Uiso 1 1 calc R . . C31 C 0.0310(2) 0.1440(2) 0.64939(17) 0.0403(7) Uani 1 1 d . . . H31A H 0.0409 0.1787 0.6908 0.048 Uiso 1 1 calc R . . H31B H 0.0233 0.0925 0.6667 0.048 Uiso 1 1 calc R . . C32 C 0.4785(2) -0.00308(16) 0.85362(14) 0.0285(6) Uani 1 1 d . . . H32 H 0.5395 -0.0241 0.8820 0.034 Uiso 1 1 calc R . . N6 N 0.39345(18) -0.03031(12) 0.85675(12) 0.0275(5) Uani 1 1 d . . . C33 C 0.3937(2) -0.09387(16) 0.90547(15) 0.0324(6) Uani 1 1 d . . . H33 H 0.4650 -0.1047 0.9325 0.039 Uiso 1 1 calc R . . C34 C 0.3321(3) -0.0731(2) 0.95856(17) 0.0464(8) Uani 1 1 d . . . H34A H 0.2632 -0.0575 0.9319 0.056 Uiso 1 1 calc R . . H34B H 0.3646 -0.0303 0.9884 0.056 Uiso 1 1 calc R . . C35 C 0.3246(4) -0.1397(2) 1.00726(19) 0.0595(10) Uani 1 1 d . . . H35A H 0.3928 -0.1518 1.0377 0.071 Uiso 1 1 calc R . . H35B H 0.2808 -0.1260 1.0393 0.071 Uiso 1 1 calc R . . C36 C 0.2811(3) -0.2080(2) 0.9633(2) 0.0569(10) Uani 1 1 d . . . H36A H 0.2806 -0.2508 0.9959 0.068 Uiso 1 1 calc R . . H36B H 0.2102 -0.1975 0.9369 0.068 Uiso 1 1 calc R . . C37 C 0.3419(3) -0.22898(19) 0.91004(19) 0.0485(9) Uani 1 1 d . . . H37A H 0.3087 -0.2716 0.8801 0.058 Uiso 1 1 calc R . . H37B H 0.4106 -0.2452 0.9365 0.058 Uiso 1 1 calc R . . C38 C 0.3502(3) -0.16259(17) 0.86164(16) 0.0373(7) Uani 1 1 d . . . H38A H 0.3942 -0.1765 0.8298 0.045 Uiso 1 1 calc R . . H38B H 0.2822 -0.1505 0.8309 0.045 Uiso 1 1 calc R . . B1 B 0.1394(3) -0.31051(19) 0.6787(2) 0.0378(8) Uani 1 1 d D . . F1 F 0.20239(17) -0.27214(12) 0.73564(12) 0.0554(5) Uani 1 1 d D . . F2 F 0.0889(2) -0.26216(14) 0.62745(14) 0.0846(9) Uani 1 1 d D . . F3 F 0.1920(3) -0.3649(2) 0.65619(18) 0.1133(14) Uani 1 1 d D . . F4 F 0.0669(2) -0.3443(2) 0.7065(2) 0.1127(13) Uani 1 1 d D . . B2 B 0.6891(4) -0.1187(3) 0.8184(3) 0.0646(13) Uani 1 1 d D . . F5 F 0.6315(6) -0.1556(3) 0.8515(4) 0.093(2) Uani 0.60 1 d PD A 1 F6 F 0.7373(5) -0.1644(3) 0.7819(4) 0.127(3) Uani 0.60 1 d PD A 1 F7 F 0.6171(5) -0.0776(3) 0.7604(3) 0.111(2) Uani 0.60 1 d PD A 1 F8 F 0.7332(6) -0.0542(3) 0.8359(5) 0.136(3) Uani 0.60 1 d PD A 1 F9 F 0.6036(7) -0.1495(6) 0.8205(5) 0.078(3) Uiso 0.40 1 d PD A 2 F10 F 0.7719(7) -0.1623(6) 0.8699(6) 0.120(3) Uiso 0.40 1 d PD A 2 F11 F 0.7152(14) -0.1118(11) 0.7633(7) 0.216(8) Uiso 0.40 1 d PD A 2 F12 F 0.7105(7) -0.0605(5) 0.8765(5) 0.089(2) Uiso 0.40 1 d PD A 2 C1S C -0.2530(4) 0.0470(3) 0.6837(3) 0.0745(13) Uani 1 1 d . . . H1S1 H -0.3066 0.0835 0.6642 0.112 Uiso 1 1 calc R . . H1S2 H -0.1930 0.0733 0.7120 0.112 Uiso 1 1 calc R . . H1S3 H -0.2769 0.0112 0.7145 0.112 Uiso 1 1 calc R . . N1S N -0.2267(3) 0.00674(19) 0.62453(17) 0.0523(8) Uani 1 1 d . . . O1S O -0.1386(3) -0.01475(18) 0.63339(19) 0.0701(8) Uani 1 1 d . . . O2S O -0.2890(3) -0.0075(3) 0.57050(17) 0.0848(10) Uani 1 1 d . . . C2S C -0.0280(8) -0.3691(6) 0.4772(6) 0.076(3) Uiso 0.50 1 d P . . C3S C 0.0373(12) -0.4144(9) 0.4948(8) 0.106(4) Uiso 0.50 1 d P . . C4S C -0.0112(14) -0.4936(11) 0.5116(9) 0.097(4) Uiso 0.50 1 d P . . C5S C -0.0778(17) -0.4612(12) 0.4861(12) 0.152(7) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01987(19) 0.0234(2) 0.0261(2) -0.00311(11) 0.00812(13) -0.00322(11) N1 0.0225(11) 0.0266(11) 0.0247(11) 0.0015(8) 0.0069(8) -0.0006(8) C1 0.0236(12) 0.0277(13) 0.0273(13) 0.0012(10) 0.0042(10) -0.0013(10) C2 0.0272(14) 0.0337(15) 0.0475(17) -0.0039(13) 0.0095(12) -0.0092(12) C3 0.0301(15) 0.0455(18) 0.060(2) -0.0040(15) 0.0191(14) -0.0122(13) C4 0.0310(16) 0.0471(19) 0.0485(19) -0.0040(14) 0.0210(14) -0.0051(13) C5 0.0254(13) 0.0329(14) 0.0314(14) 0.0002(11) 0.0103(11) 0.0002(11) C6 0.0301(14) 0.0343(15) 0.0321(14) -0.0031(11) 0.0135(11) 0.0016(11) N2 0.0255(11) 0.0279(11) 0.0259(11) -0.0017(9) 0.0079(9) 0.0004(9) C7 0.0289(13) 0.0278(13) 0.0309(14) -0.0053(11) 0.0112(11) -0.0017(11) C8 0.0349(15) 0.0327(15) 0.0377(16) -0.0027(12) 0.0001(12) 0.0015(12) C9 0.0387(16) 0.0421(17) 0.0366(16) -0.0072(13) 0.0009(13) -0.0043(13) C10 0.0437(17) 0.0370(16) 0.0395(16) -0.0135(13) 0.0155(13) -0.0071(13) C11 0.0457(18) 0.0270(15) 0.0516(19) -0.0060(13) 0.0085(15) 0.0024(13) C12 0.0376(16) 0.0310(15) 0.0445(17) -0.0040(13) -0.0010(13) 0.0052(13) C13 0.0265(13) 0.0242(13) 0.0254(12) 0.0001(10) 0.0050(10) -0.0007(10) N3 0.0227(10) 0.0243(11) 0.0234(10) 0.0005(8) 0.0058(8) -0.0005(8) C14 0.0255(13) 0.0273(13) 0.0282(13) -0.0031(10) 0.0091(10) 0.0004(10) C15 0.0385(16) 0.0280(14) 0.0330(14) 0.0004(11) 0.0170(12) 0.0011(11) C16 0.049(2) 0.0395(18) 0.0504(19) 0.0013(14) 0.0311(16) -0.0010(14) C17 0.059(2) 0.0448(19) 0.055(2) -0.0046(16) 0.0381(18) 0.0063(16) C18 0.0493(19) 0.0326(16) 0.060(2) -0.0031(14) 0.0286(16) 0.0091(14) C19 0.0377(16) 0.0267(14) 0.0425(16) -0.0024(12) 0.0155(13) 0.0021(12) N4 0.0212(10) 0.0242(11) 0.0252(10) -0.0035(8) 0.0068(8) -0.0018(8) C20 0.0262(13) 0.0246(12) 0.0287(13) -0.0042(10) 0.0092(10) -0.0030(10) C21 0.0329(15) 0.0282(14) 0.0412(15) -0.0018(12) 0.0126(12) -0.0079(11) C22 0.0277(14) 0.0369(16) 0.0484(17) -0.0098(13) 0.0130(13) -0.0125(12) C23 0.0221(13) 0.0362(15) 0.0392(15) -0.0082(12) 0.0050(11) -0.0035(11) C24 0.0215(12) 0.0276(13) 0.0286(13) -0.0067(10) 0.0048(10) -0.0020(10) C25 0.0313(14) 0.0228(12) 0.0285(13) 0.0013(10) 0.0095(11) -0.0007(10) N5 0.0235(11) 0.0257(11) 0.0268(11) 0.0016(9) 0.0064(9) 0.0009(9) C26 0.0262(13) 0.0290(14) 0.0303(13) 0.0060(11) 0.0034(11) 0.0019(10) C27 0.0320(15) 0.0361(15) 0.0309(14) 0.0033(12) 0.0041(11) 0.0002(12) C28 0.0400(17) 0.057(2) 0.0324(16) 0.0084(15) -0.0026(13) -0.0018(15) C29 0.0306(16) 0.075(3) 0.0460(19) 0.0139(18) -0.0037(14) -0.0006(16) C30 0.0283(16) 0.069(2) 0.053(2) 0.0134(18) 0.0087(14) 0.0126(16) C31 0.0278(15) 0.0538(19) 0.0387(16) 0.0046(14) 0.0074(12) 0.0078(13) C32 0.0235(13) 0.0306(14) 0.0277(13) -0.0021(11) -0.0004(10) 0.0014(11) N6 0.0270(12) 0.0270(12) 0.0261(11) 0.0009(9) 0.0025(9) 0.0004(9) C33 0.0314(14) 0.0316(14) 0.0297(14) 0.0064(11) -0.0007(11) -0.0013(11) C34 0.065(2) 0.0455(19) 0.0295(15) 0.0023(13) 0.0142(15) -0.0006(16) C35 0.082(3) 0.064(2) 0.0340(18) 0.0126(17) 0.0168(18) -0.006(2) C36 0.060(2) 0.059(2) 0.0464(19) 0.0212(17) 0.0038(17) -0.0197(19) C37 0.058(2) 0.0342(17) 0.0442(18) 0.0121(14) -0.0045(15) -0.0090(15) C38 0.0465(17) 0.0292(15) 0.0327(15) 0.0040(12) 0.0034(13) -0.0012(13) B1 0.0275(16) 0.0310(17) 0.052(2) 0.0020(15) 0.0048(14) 0.0008(13) F1 0.0497(12) 0.0524(12) 0.0543(12) -0.0030(10) -0.0053(9) 0.0013(10) F2 0.111(2) 0.0497(14) 0.0662(16) 0.0038(12) -0.0278(15) 0.0063(14) F3 0.087(2) 0.144(3) 0.092(2) -0.050(2) -0.0085(17) 0.065(2) F4 0.0630(18) 0.150(3) 0.123(3) 0.022(2) 0.0194(18) -0.047(2) B2 0.069(3) 0.047(2) 0.088(4) 0.012(2) 0.039(3) -0.006(2) F5 0.149(6) 0.050(3) 0.118(5) 0.011(3) 0.103(5) 0.006(3) F6 0.135(5) 0.064(3) 0.242(8) 0.038(4) 0.159(6) 0.038(3) F7 0.144(5) 0.105(4) 0.074(3) 0.018(3) 0.012(3) 0.055(4) F8 0.172(7) 0.067(4) 0.157(7) 0.015(4) 0.021(6) -0.058(4) C1S 0.090(4) 0.071(3) 0.070(3) -0.017(2) 0.035(3) -0.006(3) N1S 0.059(2) 0.0497(18) 0.0484(18) 0.0042(14) 0.0146(15) -0.0093(15) O1S 0.068(2) 0.0587(18) 0.087(2) 0.0046(16) 0.0259(17) 0.0028(15) O2S 0.080(2) 0.116(3) 0.0501(18) -0.0028(19) 0.0007(17) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.936(2) . ? Cu1 N4 2.004(2) . ? Cu1 N2 2.085(2) . ? Cu1 N3 2.091(2) . ? Cu1 N5 2.412(2) . ? Cu1 N6 2.443(2) . ? N1 C5 1.335(4) . ? N1 C1 1.337(4) . ? C1 C2 1.381(4) . ? C1 C13 1.476(4) . ? C2 C3 1.394(5) . ? C3 C4 1.388(5) . ? C4 C5 1.392(4) . ? C5 C6 1.478(4) . ? C6 N2 1.277(4) . ? N2 C7 1.477(3) . ? C7 C12 1.521(4) . ? C7 C8 1.523(4) . ? C8 C9 1.536(4) . ? C9 C10 1.516(5) . ? C10 C11 1.516(5) . ? C11 C12 1.526(4) . ? C13 N3 1.280(3) . ? N3 C14 1.472(3) . ? C14 C15 1.523(4) . ? C14 C19 1.524(4) . ? C15 C16 1.529(4) . ? C16 C17 1.522(5) . ? C17 C18 1.526(5) . ? C18 C19 1.528(4) . ? N4 C20 1.345(3) . ? N4 C24 1.350(3) . ? C20 C21 1.390(4) . ? C20 C25 1.472(4) . ? C21 C22 1.387(4) . ? C22 C23 1.381(5) . ? C23 C24 1.394(4) . ? C24 C32 1.470(4) . ? C25 N5 1.268(4) . ? N5 C26 1.473(3) . ? C26 C31 1.521(4) . ? C26 C27 1.528(4) . ? C27 C28 1.531(4) . ? C28 C29 1.524(5) . ? C29 C30 1.517(6) . ? C30 C31 1.533(4) . ? C32 N6 1.272(4) . ? N6 C33 1.469(4) . ? C33 C38 1.520(4) . ? C33 C34 1.520(5) . ? C34 C35 1.530(5) . ? C35 C36 1.514(6) . ? C36 C37 1.515(6) . ? C37 C38 1.526(4) . ? B1 F3 1.340(4) . ? B1 F2 1.359(4) . ? B1 F4 1.374(5) . ? B1 F1 1.389(4) . ? B2 F11 1.205(12) . ? B2 F9 1.298(10) . ? B2 F8 1.302(7) . ? B2 F5 1.305(6) . ? B2 F6 1.348(7) . ? B2 F7 1.481(7) . ? B2 F12 1.498(9) . ? B2 F10 1.516(10) . ? C1S N1S 1.462(5) . ? N1S O2S 1.193(5) . ? N1S O1S 1.231(5) . ? C2S C3S 1.186(17) . ? C2S C5S 1.80(2) . ? C3S C4S 1.62(2) . ? C3S C4S 1.68(2) 3_546 ? C3S C5S 1.75(2) . ? C4S C4S 0.64(3) 3_546 ? C4S C5S 1.08(3) . ? C4S C5S 1.45(3) 3_546 ? 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 N1 Cu1 N4 178.94(9) . . ? N1 Cu1 N2 79.02(9) . . ? N4 Cu1 N2 100.46(9) . . ? N1 Cu1 N3 78.70(9) . . ? N4 Cu1 N3 101.79(8) . . ? N2 Cu1 N3 157.65(9) . . ? N1 Cu1 N5 105.61(8) . . ? N4 Cu1 N5 75.28(8) . . ? N2 Cu1 N5 89.51(8) . . ? N3 Cu1 N5 98.09(8) . . ? N1 Cu1 N6 104.67(9) . . ? N4 Cu1 N6 74.45(8) . . ? N2 Cu1 N6 96.73(8) . . ? N3 Cu1 N6 87.27(8) . . ? N5 Cu1 N6 149.72(8) . . ? C5 N1 C1 122.0(2) . . ? C5 N1 Cu1 118.82(19) . . ? C1 N1 Cu1 119.10(18) . . ? N1 C1 C2 120.8(3) . . ? N1 C1 C13 112.1(2) . . ? C2 C1 C13 127.0(3) . . ? C1 C2 C3 118.1(3) . . ? C4 C3 C2 120.4(3) . . ? C3 C4 C5 118.3(3) . . ? N1 C5 C4 120.4(3) . . ? N1 C5 C6 112.0(2) . . ? C4 C5 C6 127.7(3) . . ? N2 C6 C5 117.1(2) . . ? C6 N2 C7 120.4(2) . . ? C6 N2 Cu1 113.08(19) . . ? C7 N2 Cu1 126.57(17) . . ? N2 C7 C12 113.5(2) . . ? N2 C7 C8 109.6(2) . . ? C12 C7 C8 111.6(2) . . ? C7 C8 C9 110.6(3) . . ? C10 C9 C8 111.1(3) . . ? C9 C10 C11 111.2(3) . . ? C10 C11 C12 110.8(3) . . ? C7 C12 C11 110.2(3) . . ? N3 C13 C1 116.7(2) . . ? C13 N3 C14 121.7(2) . . ? C13 N3 Cu1 113.38(18) . . ? C14 N3 Cu1 124.69(17) . . ? N3 C14 C15 109.7(2) . . ? N3 C14 C19 115.3(2) . . ? C15 C14 C19 110.7(2) . . ? C14 C15 C16 109.9(2) . . ? C17 C16 C15 110.9(3) . . ? C16 C17 C18 111.0(3) . . ? C17 C18 C19 111.4(3) . . ? C14 C19 C18 109.8(2) . . ? C20 N4 C24 119.0(2) . . ? C20 N4 Cu1 120.04(17) . . ? C24 N4 Cu1 120.99(18) . . ? N4 C20 C21 122.2(3) . . ? N4 C20 C25 116.6(2) . . ? C21 C20 C25 121.1(3) . . ? C22 C21 C20 118.7(3) . . ? C23 C22 C21 119.3(3) . . ? C22 C23 C24 119.2(3) . . ? N4 C24 C23 121.5(3) . . ? N4 C24 C32 116.7(2) . . ? C23 C24 C32 121.8(2) . . ? N5 C25 C20 120.1(2) . . ? C25 N5 C26 116.6(2) . . ? C25 N5 Cu1 107.05(17) . . ? C26 N5 Cu1 136.12(17) . . ? N5 C26 C31 111.3(2) . . ? N5 C26 C27 108.8(2) . . ? C31 C26 C27 110.3(2) . . ? C26 C27 C28 110.2(3) . . ? C29 C28 C27 110.7(3) . . ? C30 C29 C28 111.9(3) . . ? C29 C30 C31 112.0(3) . . ? C26 C31 C30 109.6(3) . . ? N6 C32 C24 119.9(2) . . ? C32 N6 C33 117.9(2) . . ? C32 N6 Cu1 107.31(18) . . ? C33 N6 Cu1 134.32(18) . . ? N6 C33 C38 109.3(2) . . ? N6 C33 C34 109.1(2) . . ? C38 C33 C34 111.3(3) . . ? C33 C34 C35 110.8(3) . . ? C36 C35 C34 111.0(3) . . ? C37 C36 C35 111.8(3) . . ? C36 C37 C38 110.9(3) . . ? C33 C38 C37 111.4(3) . . ? F3 B1 F2 116.1(4) . . ? F3 B1 F4 107.7(4) . . ? F2 B1 F4 106.0(3) . . ? F3 B1 F1 109.6(3) . . ? F2 B1 F1 111.1(3) . . ? F4 B1 F1 105.8(3) . . ? F11 B2 F9 122.4(11) . . ? F8 B2 F5 127.9(7) . . ? F8 B2 F6 114.5(6) . . ? F5 B2 F6 112.4(5) . . ? F8 B2 F7 86.2(5) . . ? F5 B2 F7 104.4(6) . . ? F6 B2 F7 103.0(5) . . ? F11 B2 F12 122.6(10) . . ? F9 B2 F12 106.2(7) . . ? F11 B2 F10 106.8(10) . . ? F9 B2 F10 106.9(6) . . ? F12 B2 F10 84.0(6) . . ? O2S N1S O1S 120.8(4) . . ? O2S N1S C1S 121.4(4) . . ? O1S N1S C1S 117.8(4) . . ? C3S C2S C5S 68.1(11) . . ? C2S C3S C4S 109.5(13) . . ? C2S C3S C4S 120.9(14) . 3_546 ? C4S C3S C4S 22.4(10) . 3_546 ? C2S C3S C5S 72.9(11) . . ? C4S C3S C5S 37.3(9) . . ? C4S C3S C5S 50.0(11) 3_546 . ? C4S C4S C5S 111(4) 3_546 . ? C4S C4S C5S 44(3) 3_546 3_546 ? C5S C4S C5S 155.6(16) . 3_546 ? C4S C4S C3S 83(3) 3_546 . ? C5S C4S C3S 77.6(18) . . ? C5S C4S C3S 96.3(13) 3_546 . ? C4S C4S C3S 74(3) 3_546 3_546 ? C5S C4S C3S 110(2) . 3_546 ? C5S C4S C3S 67.6(12) 3_546 3_546 ? C3S C4S C3S 157.6(10) . 3_546 ? C4S C5S C4S 24.4(16) . 3_546 ? C4S C5S C3S 65.1(17) . . ? C4S C5S C3S 62.4(12) 3_546 . ? C4S C5S C2S 104(2) . . ? C4S C5S C2S 100.2(14) 3_546 . ? C3S C5S C2S 39.0(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.991 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.082 #=END data_jmh6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-bis-{N-tert-butylcarbaldimino}pyridine]copper(II) ditetrafluoroborate hemi-acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H46 Cu N6, 2B F4, 0.5C3 H6 O' _chemical_formula_sum 'C31.50 H49 B2 Cu F8 N6 O0.50' _chemical_formula_weight 756.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.12350(10) _cell_length_b 17.0639(2) _cell_length_c 19.9979(3) _cell_angle_alpha 81.6900(8) _cell_angle_beta 75.7200(8) _cell_angle_gamma 89.0990(8) _cell_volume 3639.12(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Lath _exptl_crystal_colour Green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.9235 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; The unit cell was refined using all data ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114065 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16691 _reflns_number_gt 13873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0700P)^2^+1.8581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16691 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _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 0.21954(2) 0.304389(13) 0.671996(12) 0.02601(7) Uani 1 1 d . . . N1 N 0.19899(15) 0.41643(9) 0.64633(8) 0.0244(3) Uani 1 1 d . . . C1 C 0.11310(18) 0.44119(11) 0.61198(10) 0.0252(4) Uani 1 1 d . . . C2 C 0.08969(19) 0.52098(12) 0.59667(11) 0.0305(4) Uani 1 1 d . . . H2 H 0.0271 0.5376 0.5732 0.037 Uiso 1 1 calc R . . C3 C 0.1597(2) 0.57591(12) 0.61646(12) 0.0323(4) Uani 1 1 d . . . H3 H 0.1456 0.6309 0.6066 0.039 Uiso 1 1 calc R . . C4 C 0.25029(19) 0.55022(12) 0.65066(11) 0.0298(4) Uani 1 1 d . . . H4 H 0.3001 0.5872 0.6637 0.036 Uiso 1 1 calc R . . C5 C 0.26711(18) 0.46949(11) 0.66563(10) 0.0258(4) Uani 1 1 d . . . C6 C 0.04746(18) 0.37770(12) 0.59189(10) 0.0270(4) Uani 1 1 d . . . H6 H -0.0120 0.3904 0.5653 0.032 Uiso 1 1 calc R . . N2 N 0.07061(15) 0.30582(10) 0.61028(9) 0.0267(3) Uani 1 1 d . . . C7 C -0.0019(2) 0.24299(12) 0.59048(11) 0.0321(4) Uani 1 1 d . . . C8 C 0.0770(3) 0.17038(16) 0.5827(2) 0.0654(9) Uani 1 1 d . . . H8A H 0.1538 0.1841 0.5466 0.098 Uiso 1 1 calc R . . H8B H 0.0312 0.1291 0.5694 0.098 Uiso 1 1 calc R . . H8C H 0.0970 0.1509 0.6272 0.098 Uiso 1 1 calc R . . C9 C -0.0389(3) 0.26898(16) 0.52260(16) 0.0580(8) Uani 1 1 d . . . H9A H -0.0974 0.3124 0.5285 0.087 Uiso 1 1 calc R . . H9B H -0.0782 0.2243 0.5098 0.087 Uiso 1 1 calc R . . H9C H 0.0351 0.2870 0.4857 0.087 Uiso 1 1 calc R . . C10 C -0.1184(3) 0.2265(2) 0.64887(18) 0.0796(12) Uani 1 1 d . . . H10A H -0.0957 0.2095 0.6930 0.119 Uiso 1 1 calc R . . H10B H -0.1679 0.1846 0.6391 0.119 Uiso 1 1 calc R . . H10C H -0.1671 0.2748 0.6523 0.119 Uiso 1 1 calc R . . C11 C 0.35661(18) 0.43546(12) 0.70427(10) 0.0276(4) Uani 1 1 d . . . H11 H 0.4113 0.4689 0.7176 0.033 Uiso 1 1 calc R . . N3 N 0.35998(15) 0.36038(10) 0.71967(9) 0.0269(3) Uani 1 1 d . . . C12 C 0.45204(19) 0.32648(13) 0.75888(11) 0.0313(4) Uani 1 1 d . . . C13 C 0.5168(2) 0.38840(15) 0.78686(13) 0.0409(5) Uani 1 1 d . . . H13A H 0.5668 0.4246 0.7477 0.061 Uiso 1 1 calc R . . H13B H 0.5708 0.3618 0.8147 0.061 Uiso 1 1 calc R . . H13C H 0.4544 0.4184 0.8160 0.061 Uiso 1 1 calc R . . C14 C 0.5490(2) 0.28496(15) 0.70804(13) 0.0403(5) Uani 1 1 d . . . H14A H 0.5083 0.2433 0.6920 0.060 Uiso 1 1 calc R . . H14B H 0.6112 0.2614 0.7316 0.060 Uiso 1 1 calc R . . H14C H 0.5895 0.3236 0.6679 0.060 Uiso 1 1 calc R . . C15 C 0.3817(2) 0.26676(16) 0.81973(13) 0.0458(6) Uani 1 1 d . . . H15A H 0.3148 0.2935 0.8493 0.069 Uiso 1 1 calc R . . H15B H 0.4388 0.2440 0.8473 0.069 Uiso 1 1 calc R . . H15C H 0.3463 0.2244 0.8017 0.069 Uiso 1 1 calc R . . N4 N 0.23387(16) 0.19157(10) 0.70446(9) 0.0270(3) Uani 1 1 d . . . C16 C 0.31708(19) 0.14872(12) 0.66437(11) 0.0293(4) Uani 1 1 d . . . C17 C 0.3347(2) 0.06897(13) 0.68562(12) 0.0355(5) Uani 1 1 d . . . H17 H 0.3931 0.0395 0.6565 0.043 Uiso 1 1 calc R . . C18 C 0.2657(2) 0.03353(13) 0.74991(13) 0.0394(5) Uani 1 1 d . . . H18 H 0.2773 -0.0206 0.7658 0.047 Uiso 1 1 calc R . . C19 C 0.1795(2) 0.07750(12) 0.79105(12) 0.0346(5) Uani 1 1 d . . . H19 H 0.1311 0.0539 0.8352 0.042 Uiso 1 1 calc R . . C20 C 0.16503(19) 0.15671(12) 0.76652(11) 0.0288(4) Uani 1 1 d . . . C21 C 0.3890(2) 0.19189(12) 0.59784(11) 0.0322(4) Uani 1 1 d . . . H21 H 0.4477 0.1649 0.5665 0.039 Uiso 1 1 calc R . . N5 N 0.37227(16) 0.26549(10) 0.58241(9) 0.0279(3) Uani 1 1 d . . . C22 C 0.4457(2) 0.30794(12) 0.51379(11) 0.0322(4) Uani 1 1 d . . . C23 C 0.3720(3) 0.29830(15) 0.46014(12) 0.0442(6) Uani 1 1 d . . . H23A H 0.3632 0.2419 0.4573 0.066 Uiso 1 1 calc R . . H23B H 0.4159 0.3260 0.4144 0.066 Uiso 1 1 calc R . . H23C H 0.2896 0.3208 0.4743 0.066 Uiso 1 1 calc R . . C24 C 0.5761(2) 0.27515(16) 0.49239(14) 0.0493(6) Uani 1 1 d . . . H24A H 0.6177 0.2756 0.5302 0.074 Uiso 1 1 calc R . . H24B H 0.6238 0.3081 0.4502 0.074 Uiso 1 1 calc R . . H24C H 0.5704 0.2207 0.4830 0.074 Uiso 1 1 calc R . . C25 C 0.4545(2) 0.39526(13) 0.52049(12) 0.0383(5) Uani 1 1 d . . . H25A H 0.3709 0.4169 0.5315 0.057 Uiso 1 1 calc R . . H25B H 0.5033 0.4241 0.4764 0.057 Uiso 1 1 calc R . . H25C H 0.4949 0.4010 0.5579 0.057 Uiso 1 1 calc R . . C26 C 0.0781(2) 0.20726(12) 0.80847(11) 0.0305(4) Uani 1 1 d . . . H26 H 0.0282 0.1854 0.8528 0.037 Uiso 1 1 calc R . . N6 N 0.06944(15) 0.27998(10) 0.78561(9) 0.0272(3) Uani 1 1 d . . . C27 C -0.01792(19) 0.33050(12) 0.82961(11) 0.0306(4) Uani 1 1 d . . . C28 C 0.0460(2) 0.41084(14) 0.82112(14) 0.0417(5) Uani 1 1 d . . . H28A H 0.1258 0.4037 0.8334 0.063 Uiso 1 1 calc R . . H28B H -0.0066 0.4443 0.8519 0.063 Uiso 1 1 calc R . . H28C H 0.0598 0.4363 0.7726 0.063 Uiso 1 1 calc R . . C29 C -0.0538(3) 0.29605(15) 0.90697(13) 0.0466(6) Uani 1 1 d . . . H29A H -0.1006 0.2462 0.9132 0.070 Uiso 1 1 calc R . . H29B H -0.1053 0.3338 0.9335 0.070 Uiso 1 1 calc R . . H29C H 0.0214 0.2861 0.9238 0.070 Uiso 1 1 calc R . . C30 C -0.1335(2) 0.33987(15) 0.80140(15) 0.0448(6) Uani 1 1 d . . . H30A H -0.1101 0.3632 0.7521 0.067 Uiso 1 1 calc R . . H30B H -0.1916 0.3746 0.8279 0.067 Uiso 1 1 calc R . . H30C H -0.1732 0.2878 0.8060 0.067 Uiso 1 1 calc R . . Cu2 Cu 0.28365(2) 0.165027(14) 0.199855(12) 0.02556(7) Uani 1 1 d . . . N7 N 0.41455(15) 0.15913(9) 0.24798(9) 0.0257(3) Uani 1 1 d . . . C31 C 0.38713(19) 0.13554(11) 0.31727(11) 0.0279(4) Uani 1 1 d . . . C32 C 0.4785(2) 0.13051(12) 0.35407(11) 0.0320(4) Uani 1 1 d . . . H32 H 0.4586 0.1124 0.4028 0.038 Uiso 1 1 calc R . . C33 C 0.5996(2) 0.15255(13) 0.31808(12) 0.0360(5) Uani 1 1 d . . . H33 H 0.6634 0.1506 0.3422 0.043 Uiso 1 1 calc R . . C34 C 0.6264(2) 0.17733(12) 0.24697(12) 0.0332(5) Uani 1 1 d . . . H34 H 0.7086 0.1929 0.2218 0.040 Uiso 1 1 calc R . . C35 C 0.53156(19) 0.17921(11) 0.21282(11) 0.0274(4) Uani 1 1 d . . . C36 C 0.2553(2) 0.11522(12) 0.34979(11) 0.0298(4) Uani 1 1 d . . . H36 H 0.2286 0.0964 0.3983 0.036 Uiso 1 1 calc R . . N8 N 0.17747(16) 0.12318(10) 0.31198(9) 0.0289(4) Uani 1 1 d . . . C37 C 0.0431(2) 0.10322(14) 0.34623(11) 0.0342(5) Uani 1 1 d . . . C38 C 0.0210(2) 0.06255(19) 0.42111(13) 0.0516(7) Uani 1 1 d . . . H38A H 0.0726 0.0156 0.4228 0.077 Uiso 1 1 calc R . . H38B H -0.0667 0.0466 0.4389 0.077 Uiso 1 1 calc R . . H38C H 0.0427 0.0992 0.4499 0.077 Uiso 1 1 calc R . . C39 C -0.0031(3) 0.0486(2) 0.30386(15) 0.0567(7) Uani 1 1 d . . . H39A H 0.0040 0.0760 0.2564 0.085 Uiso 1 1 calc R . . H39B H -0.0901 0.0337 0.3258 0.085 Uiso 1 1 calc R . . H39C H 0.0470 0.0009 0.3020 0.085 Uiso 1 1 calc R . . C40 C -0.0264(2) 0.18108(18) 0.34337(17) 0.0562(7) Uani 1 1 d . . . H40A H 0.0091 0.2181 0.3668 0.084 Uiso 1 1 calc R . . H40B H -0.1142 0.1711 0.3668 0.084 Uiso 1 1 calc R . . H40C H -0.0185 0.2040 0.2946 0.084 Uiso 1 1 calc R . . C41 C 0.54973(19) 0.20291(12) 0.13716(11) 0.0288(4) Uani 1 1 d . . . H41 H 0.6300 0.2177 0.1085 0.035 Uiso 1 1 calc R . . N9 N 0.45749(15) 0.20345(10) 0.11066(9) 0.0269(3) Uani 1 1 d . . . C42 C 0.4759(2) 0.22636(12) 0.03349(11) 0.0303(4) Uani 1 1 d . . . C43 C 0.6095(2) 0.25073(16) -0.00498(13) 0.0434(6) Uani 1 1 d . . . H43A H 0.6339 0.2975 0.0121 0.065 Uiso 1 1 calc R . . H43B H 0.6154 0.2632 -0.0551 0.065 Uiso 1 1 calc R . . H43C H 0.6647 0.2071 0.0033 0.065 Uiso 1 1 calc R . . C44 C 0.3900(2) 0.29531(14) 0.02282(12) 0.0415(5) Uani 1 1 d . . . H44A H 0.3035 0.2774 0.0422 0.062 Uiso 1 1 calc R . . H44B H 0.4033 0.3143 -0.0271 0.062 Uiso 1 1 calc R . . H44C H 0.4082 0.3384 0.0466 0.062 Uiso 1 1 calc R . . C45 C 0.4372(2) 0.15414(14) 0.00602(12) 0.0404(5) Uani 1 1 d . . . H45A H 0.4933 0.1106 0.0129 0.061 Uiso 1 1 calc R . . H45B H 0.4413 0.1677 -0.0438 0.061 Uiso 1 1 calc R . . H45C H 0.3521 0.1379 0.0313 0.061 Uiso 1 1 calc R . . N10 N 0.15481(15) 0.17137(10) 0.14980(9) 0.0260(3) Uani 1 1 d . . . C46 C 0.12750(19) 0.10813(12) 0.12246(10) 0.0274(4) Uani 1 1 d . . . C47 C 0.0392(2) 0.11199(13) 0.08358(12) 0.0330(4) Uani 1 1 d . . . H47 H 0.0214 0.0671 0.0643 0.040 Uiso 1 1 calc R . . C48 C -0.0221(2) 0.18197(13) 0.07347(12) 0.0347(5) Uani 1 1 d . . . H48 H -0.0829 0.1856 0.0472 0.042 Uiso 1 1 calc R . . C49 C 0.0055(2) 0.24706(13) 0.10200(12) 0.0337(5) Uani 1 1 d . . . H49 H -0.0356 0.2957 0.0953 0.040 Uiso 1 1 calc R . . C50 C 0.09430(18) 0.23945(12) 0.14043(11) 0.0279(4) Uani 1 1 d . . . C51 C 0.19498(19) 0.03546(12) 0.13737(11) 0.0280(4) Uani 1 1 d . . . H51 H 0.1784 -0.0116 0.1207 0.034 Uiso 1 1 calc R . . N11 N 0.27568(15) 0.03592(10) 0.17272(9) 0.0269(3) Uani 1 1 d . . . C52 C 0.3450(2) -0.03797(12) 0.18701(11) 0.0302(4) Uani 1 1 d . . . C53 C 0.4770(2) -0.02306(14) 0.14262(15) 0.0439(6) Uani 1 1 d . . . H53A H 0.4770 -0.0175 0.0932 0.066 Uiso 1 1 calc R . . H53B H 0.5286 -0.0677 0.1538 0.066 Uiso 1 1 calc R . . H53C H 0.5105 0.0257 0.1523 0.066 Uiso 1 1 calc R . . C54 C 0.2897(2) -0.11176(13) 0.16957(13) 0.0392(5) Uani 1 1 d . . . H54A H 0.2042 -0.1206 0.1977 0.059 Uiso 1 1 calc R . . H54B H 0.3392 -0.1579 0.1799 0.059 Uiso 1 1 calc R . . H54C H 0.2904 -0.1041 0.1200 0.059 Uiso 1 1 calc R . . C55 C 0.3434(3) -0.04932(14) 0.26438(12) 0.0409(5) Uani 1 1 d . . . H55A H 0.3836 -0.0034 0.2747 0.061 Uiso 1 1 calc R . . H55B H 0.3881 -0.0974 0.2757 0.061 Uiso 1 1 calc R . . H55C H 0.2573 -0.0545 0.2923 0.061 Uiso 1 1 calc R . . C56 C 0.13003(19) 0.30536(12) 0.17272(11) 0.0289(4) Uani 1 1 d . . . H56 H 0.0890 0.3545 0.1697 0.035 Uiso 1 1 calc R . . N12 N 0.21606(16) 0.29569(10) 0.20454(9) 0.0285(4) Uani 1 1 d . . . C57 C 0.2513(2) 0.36258(12) 0.23736(12) 0.0341(5) Uani 1 1 d . . . C58 C 0.1709(3) 0.43441(16) 0.23256(18) 0.0599(8) Uani 1 1 d . . . H58A H 0.1765 0.4546 0.1834 0.090 Uiso 1 1 calc R . . H58B H 0.1996 0.4756 0.2548 0.090 Uiso 1 1 calc R . . H58C H 0.0846 0.4196 0.2564 0.090 Uiso 1 1 calc R . . C59 C 0.2395(5) 0.33175(18) 0.31320(18) 0.0898(15) Uani 1 1 d . . . H59A H 0.1544 0.3123 0.3349 0.135 Uiso 1 1 calc R . . H59B H 0.2593 0.3745 0.3368 0.135 Uiso 1 1 calc R . . H59C H 0.2972 0.2883 0.3172 0.135 Uiso 1 1 calc R . . C60 C 0.3839(3) 0.3856(2) 0.1997(3) 0.0987(16) Uani 1 1 d . . . H60A H 0.4382 0.3415 0.2082 0.148 Uiso 1 1 calc R . . H60B H 0.4091 0.4321 0.2170 0.148 Uiso 1 1 calc R . . H60C H 0.3905 0.3983 0.1496 0.148 Uiso 1 1 calc R . . B1 B 0.2542(2) 0.52334(15) 0.40396(14) 0.0338(5) Uani 1 1 d . . . F1 F 0.37144(13) 0.49658(9) 0.37682(8) 0.0491(4) Uani 1 1 d . . . F2 F 0.25968(16) 0.58249(10) 0.44390(9) 0.0574(4) Uani 1 1 d . . . F3 F 0.17868(13) 0.46086(9) 0.44527(8) 0.0455(3) Uani 1 1 d . . . F4 F 0.20135(14) 0.55381(9) 0.34939(8) 0.0484(4) Uani 1 1 d . . . B2 B -0.2168(2) 0.03954(16) 0.02696(14) 0.0364(5) Uani 1 1 d . . . F5 F -0.25570(14) 0.08018(10) 0.08410(8) 0.0526(4) Uani 1 1 d . . . F6 F -0.13275(15) 0.08665(10) -0.02730(8) 0.0570(4) Uani 1 1 d . . . F7 F -0.31580(14) 0.02019(11) 0.00257(8) 0.0560(4) Uani 1 1 d . . . F8 F -0.15704(19) -0.02726(11) 0.04774(9) 0.0704(5) Uani 1 1 d . . . B3 B 0.3210(3) -0.0455(2) 0.48633(18) 0.0631(11) Uani 1 1 d . . . F9 F 0.28729(18) 0.03142(12) 0.49765(9) 0.0748(6) Uani 1 1 d . . . F10 F 0.2457(3) -0.07374(16) 0.44980(12) 0.1008(8) Uani 1 1 d . . . F11 F 0.3040(2) -0.09177(13) 0.55058(11) 0.0877(7) Uani 1 1 d . . . F12 F 0.4435(2) -0.04608(13) 0.44964(16) 0.1239(12) Uani 1 1 d . . . B4 B 0.7801(3) 0.37406(18) 0.18450(18) 0.0471(7) Uani 1 1 d . . . F13 F 0.74053(15) 0.33136(9) 0.13944(8) 0.0517(4) Uani 1 1 d . . . F14 F 0.8121(2) 0.32351(11) 0.23710(10) 0.0705(5) Uani 1 1 d . . . F15 F 0.88953(17) 0.41524(10) 0.14593(12) 0.0737(5) Uani 1 1 d . . . F16 F 0.6937(2) 0.42810(14) 0.20749(11) 0.0865(7) Uani 1 1 d . . . C1S C 0.2576(4) 0.5025(2) 0.00451(17) 0.0731(10) Uani 1 1 d . . . O1S O 0.2476(5) 0.5320(3) 0.05716(17) 0.1514(17) Uani 1 1 d . . . C2S C 0.1598(4) 0.4549(3) -0.0079(3) 0.1107(17) Uani 1 1 d . . . H2S1 H 0.0970 0.4400 0.0360 0.166 Uiso 1 1 calc R . . H2S2 H 0.1954 0.4069 -0.0258 0.166 Uiso 1 1 calc R . . H2S3 H 0.1212 0.4856 -0.0420 0.166 Uiso 1 1 calc R . . C3S C 0.3747(4) 0.5156(2) -0.0504(2) 0.0767(10) Uani 1 1 d . . . H3S1 H 0.4238 0.5579 -0.0407 0.115 Uiso 1 1 calc R . . H3S2 H 0.3560 0.5309 -0.0958 0.115 Uiso 1 1 calc R . . H3S3 H 0.4221 0.4667 -0.0509 0.115 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 0.02810(13) 0.02097(12) 0.02829(13) -0.00087(9) -0.00738(10) 0.00249(9) N1 0.0240(8) 0.0236(8) 0.0242(8) -0.0018(6) -0.0042(6) 0.0009(6) C1 0.0243(9) 0.0253(9) 0.0241(9) -0.0017(7) -0.0035(7) 0.0000(7) C2 0.0298(10) 0.0292(10) 0.0323(11) -0.0005(8) -0.0099(8) 0.0040(8) C3 0.0363(11) 0.0220(9) 0.0369(11) 0.0000(8) -0.0082(9) 0.0021(8) C4 0.0297(10) 0.0258(10) 0.0326(11) -0.0034(8) -0.0053(8) -0.0032(8) C5 0.0244(9) 0.0253(9) 0.0257(9) -0.0021(7) -0.0034(7) 0.0002(7) C6 0.0246(9) 0.0290(10) 0.0267(10) -0.0023(8) -0.0061(8) 0.0016(8) N2 0.0266(8) 0.0251(8) 0.0274(8) -0.0030(7) -0.0050(7) -0.0008(6) C7 0.0341(11) 0.0280(10) 0.0346(11) -0.0047(8) -0.0085(9) -0.0051(8) C8 0.075(2) 0.0368(14) 0.109(3) -0.0310(16) -0.057(2) 0.0133(13) C9 0.084(2) 0.0414(14) 0.0626(18) -0.0055(13) -0.0450(17) -0.0076(14) C10 0.075(2) 0.087(2) 0.064(2) -0.0308(18) 0.0203(17) -0.054(2) C11 0.0260(9) 0.0280(10) 0.0287(10) -0.0043(8) -0.0064(8) -0.0014(8) N3 0.0259(8) 0.0286(8) 0.0262(8) -0.0030(7) -0.0072(7) 0.0021(7) C12 0.0299(10) 0.0322(10) 0.0333(11) 0.0001(9) -0.0134(9) 0.0023(8) C13 0.0413(13) 0.0433(13) 0.0446(13) -0.0056(10) -0.0235(11) 0.0026(10) C14 0.0361(12) 0.0426(13) 0.0452(13) -0.0064(10) -0.0163(10) 0.0119(10) C15 0.0425(13) 0.0528(15) 0.0406(13) 0.0139(11) -0.0188(11) -0.0056(11) N4 0.0288(8) 0.0241(8) 0.0278(8) -0.0016(7) -0.0074(7) 0.0016(6) C16 0.0313(10) 0.0253(9) 0.0309(10) -0.0026(8) -0.0081(8) 0.0027(8) C17 0.0369(11) 0.0262(10) 0.0409(12) -0.0029(9) -0.0062(10) 0.0069(9) C18 0.0472(13) 0.0253(10) 0.0436(13) 0.0017(9) -0.0116(11) 0.0049(9) C19 0.0396(12) 0.0275(10) 0.0334(11) 0.0033(8) -0.0072(9) 0.0002(9) C20 0.0315(10) 0.0251(9) 0.0294(10) -0.0013(8) -0.0083(8) -0.0005(8) C21 0.0329(11) 0.0294(10) 0.0319(11) -0.0043(8) -0.0041(9) 0.0033(8) N5 0.0289(9) 0.0270(8) 0.0276(8) -0.0025(7) -0.0075(7) 0.0019(7) C22 0.0349(11) 0.0292(10) 0.0285(10) 0.0004(8) -0.0030(9) 0.0012(8) C23 0.0586(15) 0.0431(13) 0.0305(12) -0.0018(10) -0.0119(11) -0.0037(11) C24 0.0396(13) 0.0451(14) 0.0492(15) 0.0075(11) 0.0067(11) 0.0054(11) C25 0.0466(13) 0.0303(11) 0.0330(11) -0.0001(9) -0.0025(10) -0.0035(9) C26 0.0323(10) 0.0298(10) 0.0263(10) 0.0000(8) -0.0035(8) -0.0013(8) N6 0.0262(8) 0.0260(8) 0.0280(8) -0.0019(7) -0.0054(7) 0.0010(7) C27 0.0291(10) 0.0289(10) 0.0308(10) -0.0041(8) -0.0020(8) 0.0018(8) C28 0.0395(12) 0.0339(11) 0.0471(14) -0.0135(10) 0.0026(10) -0.0031(10) C29 0.0550(15) 0.0418(13) 0.0341(12) -0.0027(10) 0.0033(11) 0.0092(11) C30 0.0355(12) 0.0447(13) 0.0584(16) -0.0173(12) -0.0145(11) 0.0113(10) Cu2 0.02579(13) 0.02644(13) 0.02557(13) -0.00274(9) -0.00904(10) 0.00033(9) N7 0.0272(8) 0.0226(8) 0.0278(8) -0.0029(6) -0.0081(7) 0.0009(6) C31 0.0336(10) 0.0225(9) 0.0288(10) -0.0035(8) -0.0102(8) 0.0017(8) C32 0.0398(11) 0.0276(10) 0.0315(11) -0.0023(8) -0.0157(9) 0.0028(9) C33 0.0363(11) 0.0333(11) 0.0439(13) -0.0046(9) -0.0209(10) 0.0028(9) C34 0.0281(10) 0.0294(10) 0.0434(12) -0.0026(9) -0.0129(9) 0.0000(8) C35 0.0278(10) 0.0227(9) 0.0321(10) -0.0045(8) -0.0080(8) 0.0012(7) C36 0.0347(11) 0.0286(10) 0.0254(10) -0.0021(8) -0.0072(8) 0.0009(8) N8 0.0297(9) 0.0282(8) 0.0278(9) -0.0028(7) -0.0059(7) -0.0007(7) C37 0.0284(10) 0.0421(12) 0.0293(11) -0.0006(9) -0.0043(8) -0.0015(9) C38 0.0344(12) 0.0778(19) 0.0341(13) 0.0090(12) -0.0022(10) -0.0036(12) C39 0.0417(14) 0.079(2) 0.0455(15) -0.0147(14) 0.0006(12) -0.0251(14) C40 0.0343(13) 0.0591(17) 0.0671(19) 0.0049(14) -0.0056(12) 0.0087(12) C41 0.0253(10) 0.0269(10) 0.0331(11) -0.0044(8) -0.0053(8) -0.0001(8) N9 0.0288(8) 0.0236(8) 0.0265(8) -0.0017(6) -0.0048(7) 0.0003(6) C42 0.0339(11) 0.0293(10) 0.0249(10) -0.0004(8) -0.0041(8) 0.0005(8) C43 0.0399(13) 0.0495(14) 0.0335(12) 0.0020(10) 0.0001(10) -0.0053(11) C44 0.0499(14) 0.0384(12) 0.0324(12) 0.0032(9) -0.0083(10) 0.0075(10) C45 0.0563(15) 0.0368(12) 0.0277(11) -0.0038(9) -0.0096(10) -0.0052(11) N10 0.0259(8) 0.0257(8) 0.0257(8) -0.0019(6) -0.0061(7) -0.0006(6) C46 0.0277(10) 0.0274(10) 0.0266(10) -0.0027(8) -0.0062(8) -0.0010(8) C47 0.0313(11) 0.0353(11) 0.0347(11) -0.0058(9) -0.0121(9) -0.0030(9) C48 0.0314(11) 0.0396(12) 0.0368(11) -0.0032(9) -0.0164(9) -0.0002(9) C49 0.0310(11) 0.0353(11) 0.0358(11) -0.0028(9) -0.0119(9) 0.0046(9) C50 0.0266(10) 0.0287(10) 0.0280(10) -0.0017(8) -0.0075(8) 0.0029(8) C51 0.0296(10) 0.0257(9) 0.0284(10) -0.0043(8) -0.0066(8) -0.0021(8) N11 0.0279(8) 0.0245(8) 0.0271(8) -0.0012(6) -0.0058(7) -0.0006(6) C52 0.0346(11) 0.0233(9) 0.0335(11) -0.0023(8) -0.0111(9) 0.0032(8) C53 0.0368(12) 0.0331(12) 0.0586(16) -0.0020(11) -0.0089(11) 0.0070(10) C54 0.0532(14) 0.0248(10) 0.0434(13) -0.0035(9) -0.0200(11) 0.0021(10) C55 0.0596(15) 0.0298(11) 0.0383(12) -0.0028(9) -0.0232(11) 0.0067(10) C56 0.0305(10) 0.0255(9) 0.0308(10) -0.0032(8) -0.0085(8) 0.0045(8) N12 0.0316(9) 0.0250(8) 0.0292(9) -0.0046(7) -0.0078(7) 0.0019(7) C57 0.0410(12) 0.0259(10) 0.0404(12) -0.0110(9) -0.0160(10) 0.0033(9) C58 0.084(2) 0.0388(14) 0.075(2) -0.0279(14) -0.0440(18) 0.0213(14) C59 0.194(5) 0.0383(15) 0.061(2) -0.0086(14) -0.075(3) -0.006(2) C60 0.0467(17) 0.090(3) 0.167(4) -0.089(3) 0.001(2) -0.0178(17) B1 0.0315(12) 0.0352(12) 0.0348(13) -0.0048(10) -0.0086(10) 0.0014(10) F1 0.0341(7) 0.0545(9) 0.0516(9) 0.0017(7) -0.0030(6) 0.0081(6) F2 0.0672(10) 0.0551(9) 0.0550(9) -0.0220(8) -0.0161(8) -0.0067(8) F3 0.0379(7) 0.0475(8) 0.0469(8) 0.0029(6) -0.0076(6) -0.0060(6) F4 0.0489(8) 0.0566(9) 0.0412(8) -0.0013(7) -0.0178(7) 0.0085(7) B2 0.0343(13) 0.0402(13) 0.0375(13) -0.0092(11) -0.0120(11) 0.0013(10) F5 0.0457(8) 0.0606(9) 0.0552(9) -0.0294(8) -0.0072(7) -0.0028(7) F6 0.0549(9) 0.0680(10) 0.0487(9) -0.0058(8) -0.0140(7) -0.0228(8) F7 0.0435(8) 0.0807(11) 0.0474(9) -0.0132(8) -0.0145(7) -0.0192(8) F8 0.0926(14) 0.0680(11) 0.0475(9) -0.0045(8) -0.0157(9) 0.0358(10) B3 0.058(2) 0.063(2) 0.0472(18) 0.0177(16) 0.0109(15) 0.0281(17) F9 0.0817(13) 0.0783(12) 0.0479(9) 0.0080(9) 0.0028(9) 0.0447(10) F10 0.1151(19) 0.120(2) 0.0761(15) -0.0279(14) -0.0350(14) 0.0525(16) F11 0.0775(13) 0.0964(15) 0.0715(13) 0.0455(11) -0.0188(10) 0.0083(11) F12 0.0893(16) 0.0634(13) 0.159(2) 0.0046(14) 0.0684(16) 0.0206(11) B4 0.0503(17) 0.0390(14) 0.0587(18) -0.0152(13) -0.0219(14) 0.0053(13) F13 0.0540(9) 0.0487(8) 0.0592(9) -0.0172(7) -0.0214(7) -0.0025(7) F14 0.0932(14) 0.0634(11) 0.0640(11) -0.0073(9) -0.0379(10) 0.0047(10) F15 0.0624(11) 0.0463(9) 0.1129(16) -0.0074(10) -0.0245(11) -0.0081(8) F16 0.0805(13) 0.1162(17) 0.0858(14) -0.0609(13) -0.0403(11) 0.0514(13) C1S 0.096(3) 0.070(2) 0.0476(18) -0.0039(15) -0.0108(17) 0.033(2) O1S 0.216(5) 0.168(4) 0.066(2) -0.039(2) -0.016(2) 0.056(3) C2S 0.074(3) 0.104(3) 0.140(4) 0.039(3) -0.031(3) -0.002(2) C3S 0.086(3) 0.064(2) 0.075(2) 0.0057(17) -0.020(2) 0.0033(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. The asymmetric unit contains two complex cations, 4 BF~4~^-^ anions and one acetone molecule, all lying on general positions. No disorder was detected during refinement. All non-H atoms were refined anisotropially. ; 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 N1 1.9317(16) . ? Cu1 N4 1.9579(16) . ? Cu1 N2 2.2949(17) . ? Cu1 N3 2.3037(17) . ? Cu1 N5 2.3115(17) . ? Cu1 N6 2.4496(17) . ? N1 C1 1.338(3) . ? N1 C5 1.345(3) . ? C1 C2 1.387(3) . ? C1 C6 1.471(3) . ? C2 C3 1.387(3) . ? C3 C4 1.384(3) . ? C4 C5 1.387(3) . ? C5 C11 1.469(3) . ? C6 N2 1.270(3) . ? N2 C7 1.505(3) . ? C7 C8 1.511(3) . ? C7 C10 1.514(4) . ? C7 C9 1.518(3) . ? C11 N3 1.276(3) . ? N3 C12 1.498(3) . ? C12 C15 1.526(3) . ? C12 C14 1.530(3) . ? C12 C13 1.530(3) . ? N4 C20 1.346(3) . ? N4 C16 1.348(3) . ? C16 C17 1.392(3) . ? C16 C21 1.471(3) . ? C17 C18 1.382(3) . ? C18 C19 1.388(3) . ? C19 C20 1.391(3) . ? C20 C26 1.472(3) . ? C21 N5 1.271(3) . ? N5 C22 1.501(3) . ? C22 C25 1.522(3) . ? C22 C24 1.529(3) . ? C22 C23 1.530(3) . ? C26 N6 1.270(3) . ? N6 C27 1.494(3) . ? C27 C28 1.522(3) . ? C27 C30 1.524(3) . ? C27 C29 1.529(3) . ? Cu2 N7 1.9274(17) . ? Cu2 N10 1.9337(16) . ? Cu2 N8 2.2781(17) . ? Cu2 N9 2.3132(17) . ? Cu2 N12 2.3491(17) . ? Cu2 N11 2.3519(17) . ? N7 C35 1.341(3) . ? N7 C31 1.345(3) . ? C31 C32 1.389(3) . ? C31 C36 1.474(3) . ? C32 C33 1.390(3) . ? C33 C34 1.382(3) . ? C34 C35 1.388(3) . ? C35 C41 1.473(3) . ? C36 N8 1.276(3) . ? N8 C37 1.504(3) . ? C37 C38 1.519(3) . ? C37 C39 1.519(3) . ? C37 C40 1.527(3) . ? C41 N9 1.265(3) . ? N9 C42 1.500(3) . ? C42 C43 1.528(3) . ? C42 C44 1.528(3) . ? C42 C45 1.528(3) . ? N10 C50 1.346(3) . ? N10 C46 1.348(3) . ? C46 C47 1.390(3) . ? C46 C51 1.471(3) . ? C47 C48 1.380(3) . ? C48 C49 1.391(3) . ? C49 C50 1.387(3) . ? C50 C56 1.480(3) . ? C51 N11 1.273(3) . ? N11 C52 1.496(3) . ? C52 C53 1.521(3) . ? C52 C55 1.527(3) . ? C52 C54 1.530(3) . ? C56 N12 1.270(3) . ? N12 C57 1.498(3) . ? C57 C59 1.506(4) . ? C57 C60 1.511(4) . ? C57 C58 1.512(3) . ? B1 F1 1.381(3) . ? B1 F2 1.385(3) . ? B1 F4 1.397(3) . ? B1 F3 1.399(3) . ? B2 F7 1.372(3) . ? B2 F8 1.374(3) . ? B2 F5 1.396(3) . ? B2 F6 1.403(3) . ? B3 F10 1.372(5) . ? B3 F11 1.379(4) . ? B3 F12 1.380(4) . ? B3 F9 1.394(4) . ? B4 F16 1.365(3) . ? B4 F14 1.375(4) . ? B4 F13 1.390(3) . ? B4 F15 1.406(4) . ? C1S O1S 1.212(5) . ? C1S C2S 1.458(6) . ? C1S C3S 1.478(5) . ? 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 N1 Cu1 N4 176.09(7) . . ? N1 Cu1 N2 77.68(6) . . ? N4 Cu1 N2 103.26(6) . . ? N1 Cu1 N3 77.48(6) . . ? N4 Cu1 N3 101.56(6) . . ? N2 Cu1 N3 155.16(6) . . ? N1 Cu1 N5 106.18(6) . . ? N4 Cu1 N5 77.62(7) . . ? N2 Cu1 N5 92.97(6) . . ? N3 Cu1 N5 93.32(6) . . ? N1 Cu1 N6 100.81(6) . . ? N4 Cu1 N6 75.38(6) . . ? N2 Cu1 N6 93.84(6) . . ? N3 Cu1 N6 91.38(6) . . ? N5 Cu1 N6 152.99(6) . . ? C1 N1 C5 120.03(17) . . ? C1 N1 Cu1 119.87(13) . . ? C5 N1 Cu1 120.04(13) . . ? N1 C1 C2 121.69(18) . . ? N1 C1 C6 114.90(17) . . ? C2 C1 C6 123.41(18) . . ? C1 C2 C3 118.47(19) . . ? C4 C3 C2 119.72(19) . . ? C3 C4 C5 118.82(19) . . ? N1 C5 C4 121.24(18) . . ? N1 C5 C11 115.22(17) . . ? C4 C5 C11 123.52(18) . . ? N2 C6 C1 119.67(18) . . ? C6 N2 C7 117.69(17) . . ? C6 N2 Cu1 107.73(13) . . ? C7 N2 Cu1 134.56(13) . . ? N2 C7 C8 108.56(18) . . ? N2 C7 C10 106.31(19) . . ? C8 C7 C10 111.8(3) . . ? N2 C7 C9 112.94(18) . . ? C8 C7 C9 108.6(2) . . ? C10 C7 C9 108.7(3) . . ? N3 C11 C5 119.15(18) . . ? C11 N3 C12 118.56(17) . . ? C11 N3 Cu1 108.02(13) . . ? C12 N3 Cu1 133.31(13) . . ? N3 C12 C15 107.10(17) . . ? N3 C12 C14 106.52(17) . . ? C15 C12 C14 110.6(2) . . ? N3 C12 C13 113.92(17) . . ? C15 C12 C13 109.32(19) . . ? C14 C12 C13 109.33(19) . . ? C20 N4 C16 119.60(17) . . ? C20 N4 Cu1 121.46(14) . . ? C16 N4 Cu1 118.92(14) . . ? N4 C16 C17 121.68(19) . . ? N4 C16 C21 115.82(17) . . ? C17 C16 C21 122.49(19) . . ? C18 C17 C16 118.7(2) . . ? C17 C18 C19 119.6(2) . . ? C18 C19 C20 118.9(2) . . ? N4 C20 C19 121.44(19) . . ? N4 C20 C26 116.87(17) . . ? C19 C20 C26 121.63(19) . . ? N5 C21 C16 119.70(19) . . ? C21 N5 C22 118.63(18) . . ? C21 N5 Cu1 107.92(14) . . ? C22 N5 Cu1 133.41(13) . . ? N5 C22 C25 108.05(17) . . ? N5 C22 C24 112.16(17) . . ? C25 C22 C24 109.6(2) . . ? N5 C22 C23 106.51(18) . . ? C25 C22 C23 109.44(19) . . ? C24 C22 C23 110.9(2) . . ? N6 C26 C20 120.28(19) . . ? C26 N6 C27 119.36(17) . . ? C26 N6 Cu1 106.00(13) . . ? C27 N6 Cu1 134.59(12) . . ? N6 C27 C28 107.36(17) . . ? N6 C27 C30 107.30(18) . . ? C28 C27 C30 109.79(19) . . ? N6 C27 C29 113.37(17) . . ? C28 C27 C29 109.0(2) . . ? C30 C27 C29 109.9(2) . . ? N7 Cu2 N10 178.84(7) . . ? N7 Cu2 N8 78.33(7) . . ? N10 Cu2 N8 102.82(7) . . ? N7 Cu2 N9 77.29(7) . . ? N10 Cu2 N9 101.56(6) . . ? N8 Cu2 N9 155.62(6) . . ? N7 Cu2 N12 102.92(6) . . ? N10 Cu2 N12 77.22(6) . . ? N8 Cu2 N12 92.75(6) . . ? N9 Cu2 N12 93.06(6) . . ? N7 Cu2 N11 102.67(6) . . ? N10 Cu2 N11 77.23(6) . . ? N8 Cu2 N11 90.49(6) . . ? N9 Cu2 N11 94.42(6) . . ? N12 Cu2 N11 154.33(6) . . ? C35 N7 C31 120.36(18) . . ? C35 N7 Cu2 120.30(14) . . ? C31 N7 Cu2 119.34(14) . . ? N7 C31 C32 121.3(2) . . ? N7 C31 C36 115.11(18) . . ? C32 C31 C36 123.60(19) . . ? C31 C32 C33 118.6(2) . . ? C34 C33 C32 119.6(2) . . ? C33 C34 C35 119.2(2) . . ? N7 C35 C34 121.03(19) . . ? N7 C35 C41 115.11(18) . . ? C34 C35 C41 123.86(19) . . ? N8 C36 C31 119.18(19) . . ? C36 N8 C37 118.44(18) . . ? C36 N8 Cu2 108.01(14) . . ? C37 N8 Cu2 133.53(13) . . ? N8 C37 C38 113.52(18) . . ? N8 C37 C39 107.96(18) . . ? C38 C37 C39 108.7(2) . . ? N8 C37 C40 106.72(19) . . ? C38 C37 C40 110.2(2) . . ? C39 C37 C40 109.6(2) . . ? N9 C41 C35 119.42(18) . . ? C41 N9 C42 119.58(17) . . ? C41 N9 Cu2 107.85(14) . . ? C42 N9 Cu2 132.56(13) . . ? N9 C42 C43 113.80(18) . . ? N9 C42 C44 106.99(17) . . ? C43 C42 C44 109.65(19) . . ? N9 C42 C45 106.51(16) . . ? C43 C42 C45 109.44(19) . . ? C44 C42 C45 110.38(19) . . ? C50 N10 C46 119.67(17) . . ? C50 N10 Cu2 120.26(14) . . ? C46 N10 Cu2 120.04(13) . . ? N10 C46 C47 121.36(19) . . ? N10 C46 C51 115.95(17) . . ? C47 C46 C51 122.68(19) . . ? C48 C47 C46 119.0(2) . . ? C47 C48 C49 119.68(19) . . ? C50 C49 C48 118.6(2) . . ? N10 C50 C49 121.68(19) . . ? N10 C50 C56 115.76(17) . . ? C49 C50 C56 122.56(18) . . ? N11 C51 C46 119.70(18) . . ? C51 N11 C52 119.41(17) . . ? C51 N11 Cu2 106.95(13) . . ? C52 N11 Cu2 133.62(13) . . ? N11 C52 C53 106.29(17) . . ? N11 C52 C55 107.14(17) . . ? C53 C52 C55 110.3(2) . . ? N11 C52 C54 113.50(17) . . ? C53 C52 C54 109.79(19) . . ? C55 C52 C54 109.70(18) . . ? N12 C56 C50 119.46(18) . . ? C56 N12 C57 119.14(17) . . ? C56 N12 Cu2 107.26(13) . . ? C57 N12 Cu2 133.57(13) . . ? N12 C57 C59 107.11(19) . . ? N12 C57 C60 106.5(2) . . ? C59 C57 C60 111.5(3) . . ? N12 C57 C58 114.06(19) . . ? C59 C57 C58 108.5(3) . . ? C60 C57 C58 109.1(3) . . ? F1 B1 F2 110.8(2) . . ? F1 B1 F4 109.3(2) . . ? F2 B1 F4 108.8(2) . . ? F1 B1 F3 110.16(19) . . ? F2 B1 F3 109.2(2) . . ? F4 B1 F3 108.56(19) . . ? F7 B2 F8 110.9(2) . . ? F7 B2 F5 110.8(2) . . ? F8 B2 F5 108.0(2) . . ? F7 B2 F6 108.4(2) . . ? F8 B2 F6 108.4(2) . . ? F5 B2 F6 110.3(2) . . ? F10 B3 F11 109.4(3) . . ? F10 B3 F12 110.2(3) . . ? F11 B3 F12 110.3(3) . . ? F10 B3 F9 109.3(3) . . ? F11 B3 F9 107.7(3) . . ? F12 B3 F9 109.9(3) . . ? F16 B4 F14 114.0(3) . . ? F16 B4 F13 110.5(2) . . ? F14 B4 F13 110.4(2) . . ? F16 B4 F15 108.4(2) . . ? F14 B4 F15 106.4(2) . . ? F13 B4 F15 106.9(3) . . ? O1S C1S C2S 123.4(5) . . ? O1S C1S C3S 118.6(5) . . ? C2S C1S C3S 118.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.784 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.098 #=END data_jmh20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-bis-{N-(2,4,6-trimethylphenyl)carbaldimino}pyridine]copper(I) tetrafluoroborate acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H54 Cu N6, B F4, C2 H3 N' _chemical_formula_sum 'C52 H57 B Cu F4 N7' _chemical_formula_weight 930.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6577(2) _cell_length_b 26.3752(4) _cell_length_c 16.2105(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.1990(10) _cell_angle_gamma 90.00 _cell_volume 4809.96(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Brown _exptl_crystal_colour Needle _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 0.9699 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; The unit cell was refined using all data ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114564 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.45 _reflns_number_total 10968 _reflns_number_gt 8690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The BF4- anion is disordered over three distinct sites: B1A-F4A, occupancy 0.5 B1B-F4B, occupancy 0.3 B1C-F4C, occupancy 0.2 All B-F distances were restrained to 1.38(2)\%A and F...F distances to 2.25(2)\%A. All atoms with occupancy >=0.5 were refined anisotropically. ; _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^)+(0.0494P)^2^+2.2120P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10968 _refine_ls_number_parameters 627 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.252263(19) 0.172835(8) 0.121528(14) 0.02874(7) Uani 1 1 d . . . N1 N 0.10995(13) 0.12888(6) 0.06946(9) 0.0278(3) Uani 1 1 d . . . C1 C 0.07063(16) 0.08655(7) 0.10029(12) 0.0292(4) Uani 1 1 d . . . C2 C -0.01468(16) 0.05514(8) 0.04919(13) 0.0341(4) Uani 1 1 d . . . H2 H -0.0378 0.0248 0.0719 0.041 Uiso 1 1 calc R . . C3 C -0.06572(17) 0.06844(8) -0.03508(13) 0.0380(5) Uani 1 1 d . . . H3 H -0.1253 0.0477 -0.0705 0.046 Uiso 1 1 calc R . . C4 C -0.02877(17) 0.11231(8) -0.06692(13) 0.0362(4) Uani 1 1 d . . . H4 H -0.0637 0.1226 -0.1241 0.043 Uiso 1 1 calc R . . C5 C 0.06039(16) 0.14103(7) -0.01374(12) 0.0304(4) Uani 1 1 d . . . C6 C 0.12008(16) 0.07575(7) 0.19209(12) 0.0314(4) Uani 1 1 d . . . H6 H 0.1796 0.0974 0.2254 0.038 Uiso 1 1 calc R . . N2 N 0.08472(15) 0.03832(6) 0.22702(11) 0.0387(4) Uani 1 1 d . . . C7 C 0.13201(17) 0.02925(7) 0.31638(12) 0.0338(4) Uani 1 1 d . . . C8 C 0.07227(18) 0.04828(7) 0.37385(13) 0.0362(4) Uani 1 1 d . . . C9 C 0.11520(19) 0.03624(8) 0.46012(14) 0.0400(5) Uani 1 1 d . . . H9 H 0.0745 0.0488 0.4996 0.048 Uiso 1 1 calc R . . C10 C 0.2157(2) 0.00647(8) 0.49015(14) 0.0434(5) Uani 1 1 d . . . C11 C 0.2709(2) -0.01269(8) 0.43093(15) 0.0458(5) Uani 1 1 d . . . H11 H 0.3387 -0.0338 0.4505 0.055 Uiso 1 1 calc R . . C12 C 0.23139(19) -0.00242(8) 0.34400(14) 0.0413(5) Uani 1 1 d . . . C13 C -0.0351(2) 0.08160(9) 0.34357(16) 0.0497(6) Uani 1 1 d . . . H13A H -0.0112 0.1141 0.3239 0.075 Uiso 1 1 calc R . . H13B H -0.0717 0.0875 0.3907 0.075 Uiso 1 1 calc R . . H13C H -0.0926 0.0649 0.2963 0.075 Uiso 1 1 calc R . . C14 C 0.2650(3) -0.00425(10) 0.58450(16) 0.0629(7) Uani 1 1 d . . . H14A H 0.2867 -0.0401 0.5927 0.094 Uiso 1 1 calc R . . H14B H 0.2046 0.0037 0.6147 0.094 Uiso 1 1 calc R . . H14C H 0.3355 0.0168 0.6073 0.094 Uiso 1 1 calc R . . C15 C 0.2929(2) -0.02510(11) 0.28200(17) 0.0625(7) Uani 1 1 d . . . H15A H 0.3564 -0.0478 0.3126 0.094 Uiso 1 1 calc R . . H15B H 0.3269 0.0020 0.2546 0.094 Uiso 1 1 calc R . . H15C H 0.2353 -0.0444 0.2383 0.094 Uiso 1 1 calc R . . C16 C 0.10990(17) 0.18615(7) -0.04463(12) 0.0320(4) Uani 1 1 d . . . H16 H 0.0718 0.2010 -0.0982 0.038 Uiso 1 1 calc R . . N3 N 0.20576(13) 0.20497(6) 0.00264(10) 0.0292(3) Uani 1 1 d . . . C17 C 0.25523(16) 0.25049(7) -0.02221(11) 0.0293(4) Uani 1 1 d . . . C18 C 0.37044(17) 0.24813(7) -0.03264(13) 0.0338(4) Uani 1 1 d . . . C19 C 0.42388(18) 0.29290(7) -0.04832(13) 0.0364(4) Uani 1 1 d . . . H19 H 0.5019 0.2917 -0.0560 0.044 Uiso 1 1 calc R . . C20 C 0.36650(19) 0.33957(7) -0.05314(13) 0.0368(4) Uani 1 1 d . . . C21 C 0.25225(18) 0.34032(7) -0.04272(12) 0.0348(4) Uani 1 1 d . . . H21 H 0.2119 0.3719 -0.0467 0.042 Uiso 1 1 calc R . . C22 C 0.19404(17) 0.29668(7) -0.02669(12) 0.0320(4) Uani 1 1 d . . . C23 C 0.4347(2) 0.19832(8) -0.02852(17) 0.0490(6) Uani 1 1 d . . . H23A H 0.5112 0.2038 -0.0416 0.074 Uiso 1 1 calc R . . H23B H 0.3865 0.1748 -0.0703 0.074 Uiso 1 1 calc R . . H23C H 0.4483 0.1840 0.0290 0.074 Uiso 1 1 calc R . . C24 C 0.4277(2) 0.38794(8) -0.06721(17) 0.0512(6) Uani 1 1 d . . . H24A H 0.4075 0.3957 -0.1284 0.077 Uiso 1 1 calc R . . H24B H 0.5140 0.3837 -0.0458 0.077 Uiso 1 1 calc R . . H24C H 0.4014 0.4158 -0.0365 0.077 Uiso 1 1 calc R . . C25 C 0.07188(17) 0.30043(8) -0.01201(14) 0.0383(5) Uani 1 1 d . . . H25A H 0.0568 0.3355 0.0020 0.057 Uiso 1 1 calc R . . H25B H 0.0672 0.2782 0.0354 0.057 Uiso 1 1 calc R . . H25C H 0.0122 0.2900 -0.0639 0.057 Uiso 1 1 calc R . . N4 N 0.41222(13) 0.14434(6) 0.18627(10) 0.0284(3) Uani 1 1 d . . . C26 C 0.46514(16) 0.09959(7) 0.18027(12) 0.0295(4) Uani 1 1 d . . . C27 C 0.57873(17) 0.08822(8) 0.23088(13) 0.0352(4) Uani 1 1 d . . . H27 H 0.6133 0.0561 0.2264 0.042 Uiso 1 1 calc R . . C28 C 0.64034(17) 0.12391(8) 0.28739(13) 0.0376(4) Uani 1 1 d . . . H28 H 0.7183 0.1169 0.3215 0.045 Uiso 1 1 calc R . . C29 C 0.58702(17) 0.17011(7) 0.29386(13) 0.0343(4) Uani 1 1 d . . . H29 H 0.6281 0.1954 0.3321 0.041 Uiso 1 1 calc R . . C30 C 0.47297(16) 0.17887(7) 0.24379(12) 0.0295(4) Uani 1 1 d . . . C31 C 0.39703(17) 0.06288(7) 0.11821(12) 0.0319(4) Uani 1 1 d . . . H31 H 0.3191 0.0711 0.0854 0.038 Uiso 1 1 calc R . . N5 N 0.44209(14) 0.02020(6) 0.10831(10) 0.0323(3) Uani 1 1 d . . . C32 C 0.38075(16) -0.01647(7) 0.04915(12) 0.0309(4) Uani 1 1 d . . . C33 C 0.39556(17) -0.06733(7) 0.07749(13) 0.0338(4) Uani 1 1 d . . . C34 C 0.34035(17) -0.10556(7) 0.02260(14) 0.0371(4) Uani 1 1 d . . . H34 H 0.3473 -0.1396 0.0426 0.045 Uiso 1 1 calc R . . C35 C 0.27530(18) -0.09571(7) -0.06058(14) 0.0373(4) Uani 1 1 d . . . C36 C 0.26602(17) -0.04569(8) -0.08823(13) 0.0355(4) Uani 1 1 d . . . H36 H 0.2244 -0.0386 -0.1458 0.043 Uiso 1 1 calc R . . C37 C 0.31516(16) -0.00544(7) -0.03509(13) 0.0322(4) Uani 1 1 d . . . C38 C 0.46776(19) -0.08134(8) 0.16581(14) 0.0411(5) Uani 1 1 d . . . H38A H 0.4152 -0.0952 0.1985 0.062 Uiso 1 1 calc R . . H38B H 0.5080 -0.0511 0.1947 0.062 Uiso 1 1 calc R . . H38C H 0.5271 -0.1069 0.1617 0.062 Uiso 1 1 calc R . . C39 C 0.2139(2) -0.13847(8) -0.11744(16) 0.0484(5) Uani 1 1 d . . . H39A H 0.1736 -0.1250 -0.1739 0.073 Uiso 1 1 calc R . . H39B H 0.1555 -0.1544 -0.0919 0.073 Uiso 1 1 calc R . . H39C H 0.2730 -0.1637 -0.1233 0.073 Uiso 1 1 calc R . . C40 C 0.29928(19) 0.04763(8) -0.07191(14) 0.0396(5) Uani 1 1 d . . . H40A H 0.2868 0.0460 -0.1340 0.059 Uiso 1 1 calc R . . H40B H 0.3706 0.0677 -0.0467 0.059 Uiso 1 1 calc R . . H40C H 0.2302 0.0636 -0.0588 0.059 Uiso 1 1 calc R . . C41 C 0.40905(16) 0.22577(7) 0.25067(12) 0.0315(4) Uani 1 1 d . . . H41 H 0.4474 0.2525 0.2869 0.038 Uiso 1 1 calc R . . N6 N 0.30079(13) 0.23036(5) 0.20721(9) 0.0284(3) Uani 1 1 d . . . C42 C 0.23819(16) 0.27700(7) 0.21090(11) 0.0299(4) Uani 1 1 d . . . C43 C 0.28489(17) 0.32382(7) 0.19377(12) 0.0325(4) Uani 1 1 d . . . C44 C 0.21465(19) 0.36692(8) 0.19331(13) 0.0383(5) Uani 1 1 d . . . H44 H 0.2448 0.3990 0.1823 0.046 Uiso 1 1 calc R . . C45 C 0.10288(19) 0.36481(8) 0.20829(13) 0.0403(5) Uani 1 1 d . . . C46 C 0.05983(18) 0.31790(8) 0.22470(12) 0.0372(4) Uani 1 1 d . . . H46 H -0.0162 0.3160 0.2357 0.045 Uiso 1 1 calc R . . C47 C 0.12514(17) 0.27337(7) 0.22546(12) 0.0324(4) Uani 1 1 d . . . C48 C 0.40246(18) 0.32903(8) 0.17203(14) 0.0376(4) Uani 1 1 d . . . H48A H 0.4057 0.3619 0.1444 0.056 Uiso 1 1 calc R . . H48B H 0.4108 0.3017 0.1331 0.056 Uiso 1 1 calc R . . H48C H 0.4673 0.3269 0.2245 0.056 Uiso 1 1 calc R . . C49 C 0.0282(2) 0.41229(9) 0.20472(17) 0.0549(6) Uani 1 1 d . . . H49A H 0.0805 0.4417 0.2214 0.082 Uiso 1 1 calc R . . H49B H -0.0224 0.4087 0.2440 0.082 Uiso 1 1 calc R . . H49C H -0.0217 0.4171 0.1464 0.082 Uiso 1 1 calc R . . C50 C 0.07407(18) 0.22299(8) 0.24150(14) 0.0383(4) Uani 1 1 d . . . H50A H 0.0587 0.2023 0.1895 0.057 Uiso 1 1 calc R . . H50B H -0.0005 0.2285 0.2574 0.057 Uiso 1 1 calc R . . H50C H 0.1308 0.2054 0.2881 0.057 Uiso 1 1 calc R . . B1A B 0.7383(9) 0.2081(4) 0.7995(7) 0.047(4) Uani 0.50 1 d PD A 1 F1A F 0.7487(5) 0.15638(18) 0.7848(6) 0.0549(12) Uani 0.50 1 d PD A 1 F2A F 0.6660(6) 0.2138(5) 0.8586(5) 0.050(2) Uani 0.50 1 d PD A 1 F3A F 0.6877(4) 0.23450(14) 0.7244(2) 0.0596(9) Uani 0.50 1 d PD A 1 F4A F 0.8493(3) 0.23001(17) 0.8380(3) 0.0699(12) Uani 0.50 1 d PD A 1 B1B B 0.7541(13) 0.2096(6) 0.8055(9) 0.029(5) Uiso 0.30 1 d PD B 2 F1B F 0.8537(5) 0.2206(2) 0.8718(4) 0.0391(14) Uiso 0.30 1 d PD B 2 F2B F 0.7371(6) 0.2451(2) 0.7430(5) 0.0500(16) Uiso 0.30 1 d PD B 2 F3B F 0.7716(13) 0.1637(4) 0.7694(8) 0.059(3) Uiso 0.30 1 d PD B 2 F4B F 0.6527(9) 0.2070(4) 0.8342(7) 0.048(3) Uiso 0.30 1 d PD B 2 B1C B 0.7654(14) 0.2102(6) 0.8301(10) 0.052(6) Uiso 0.20 1 d PD C 3 F1C F 0.8456(7) 0.2083(3) 0.9096(6) 0.063(2) Uiso 0.20 1 d PD C 3 F2C F 0.7891(11) 0.2507(3) 0.7826(8) 0.079(3) Uiso 0.20 1 d PD C 3 F3C F 0.7764(17) 0.1656(5) 0.7866(11) 0.053(5) Uiso 0.20 1 d PD C 3 F4C F 0.6536(13) 0.2150(9) 0.8436(15) 0.029(4) Uiso 0.20 1 d PD C 3 N1S N 0.7893(2) 0.13511(10) 0.49265(16) 0.0732(7) Uani 1 1 d . . . C1S C 0.7865(2) 0.17433(11) 0.52051(17) 0.0561(6) Uani 1 1 d . . . C2S C 0.7849(3) 0.22520(12) 0.5543(2) 0.0732(8) Uani 1 1 d . . . H2S1 H 0.8658 0.2351 0.5850 0.110 Uiso 1 1 calc R . . H2S2 H 0.7338 0.2259 0.5937 0.110 Uiso 1 1 calc R . . H2S3 H 0.7540 0.2489 0.5072 0.110 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 0.02763(12) 0.02721(12) 0.02825(12) 0.00007(9) 0.00176(9) 0.00076(9) N1 0.0267(7) 0.0278(8) 0.0286(8) -0.0006(6) 0.0065(6) 0.0017(6) C1 0.0265(9) 0.0286(9) 0.0334(10) -0.0020(8) 0.0093(7) 0.0029(7) C2 0.0291(9) 0.0338(10) 0.0405(11) -0.0047(8) 0.0109(8) -0.0027(8) C3 0.0303(10) 0.0414(11) 0.0400(11) -0.0095(9) 0.0049(8) -0.0043(8) C4 0.0309(10) 0.0436(11) 0.0313(10) -0.0032(9) 0.0032(8) 0.0012(8) C5 0.0283(9) 0.0329(10) 0.0293(9) -0.0007(8) 0.0063(7) 0.0034(7) C6 0.0304(9) 0.0288(9) 0.0343(10) -0.0013(8) 0.0075(8) -0.0001(7) N2 0.0427(10) 0.0361(9) 0.0360(9) 0.0033(7) 0.0080(7) -0.0076(7) C7 0.0376(10) 0.0289(9) 0.0349(10) 0.0025(8) 0.0098(8) -0.0083(8) C8 0.0366(10) 0.0308(10) 0.0414(11) -0.0027(8) 0.0106(9) -0.0085(8) C9 0.0499(12) 0.0333(10) 0.0403(12) -0.0030(9) 0.0183(10) -0.0096(9) C10 0.0621(14) 0.0301(10) 0.0368(11) 0.0047(9) 0.0106(10) -0.0066(10) C11 0.0523(13) 0.0367(11) 0.0458(13) 0.0078(10) 0.0082(10) 0.0060(10) C12 0.0469(12) 0.0375(11) 0.0415(12) 0.0031(9) 0.0153(10) 0.0002(9) C13 0.0406(12) 0.0562(14) 0.0499(13) -0.0095(11) 0.0075(10) 0.0038(10) C14 0.098(2) 0.0452(14) 0.0409(13) 0.0080(11) 0.0101(13) 0.0002(13) C15 0.0652(16) 0.0704(18) 0.0563(16) 0.0062(13) 0.0239(13) 0.0222(14) C16 0.0349(10) 0.0336(10) 0.0267(9) 0.0013(8) 0.0067(8) 0.0045(8) N3 0.0300(8) 0.0293(8) 0.0285(8) 0.0005(6) 0.0079(6) 0.0026(6) C17 0.0338(10) 0.0294(9) 0.0241(9) 0.0028(7) 0.0066(7) 0.0035(7) C18 0.0368(10) 0.0305(10) 0.0363(10) 0.0022(8) 0.0136(8) 0.0071(8) C19 0.0381(11) 0.0348(10) 0.0409(11) 0.0027(9) 0.0184(9) 0.0027(8) C20 0.0456(12) 0.0313(10) 0.0350(11) 0.0017(8) 0.0129(9) 0.0005(8) C21 0.0407(11) 0.0279(9) 0.0342(10) 0.0026(8) 0.0072(8) 0.0085(8) C22 0.0331(10) 0.0339(10) 0.0265(9) 0.0006(8) 0.0033(8) 0.0068(8) C23 0.0488(13) 0.0343(11) 0.0736(16) 0.0098(11) 0.0333(12) 0.0118(10) C24 0.0590(14) 0.0314(11) 0.0693(16) 0.0023(11) 0.0277(12) -0.0019(10) C25 0.0325(10) 0.0413(11) 0.0400(11) 0.0004(9) 0.0078(9) 0.0084(8) N4 0.0281(8) 0.0265(8) 0.0302(8) 0.0021(6) 0.0072(6) 0.0011(6) C26 0.0294(9) 0.0285(9) 0.0319(10) 0.0045(8) 0.0105(8) 0.0038(7) C27 0.0327(10) 0.0358(10) 0.0373(10) 0.0030(9) 0.0097(8) 0.0088(8) C28 0.0268(9) 0.0460(12) 0.0372(11) 0.0020(9) 0.0032(8) 0.0060(8) C29 0.0293(9) 0.0369(10) 0.0349(10) 0.0008(8) 0.0049(8) -0.0006(8) C30 0.0283(9) 0.0293(9) 0.0297(9) 0.0037(7) 0.0054(7) -0.0001(7) C31 0.0290(9) 0.0317(10) 0.0351(10) 0.0028(8) 0.0085(8) 0.0036(8) N5 0.0337(8) 0.0290(8) 0.0353(9) 0.0023(7) 0.0109(7) 0.0032(7) C32 0.0276(9) 0.0295(9) 0.0379(10) -0.0017(8) 0.0124(8) 0.0024(7) C33 0.0327(10) 0.0300(10) 0.0409(11) 0.0027(8) 0.0135(8) 0.0075(8) C34 0.0356(10) 0.0273(9) 0.0518(13) 0.0014(9) 0.0172(9) 0.0048(8) C35 0.0342(10) 0.0344(10) 0.0458(12) -0.0050(9) 0.0147(9) 0.0007(8) C36 0.0324(10) 0.0389(11) 0.0360(10) 0.0002(9) 0.0106(8) 0.0018(8) C37 0.0280(9) 0.0320(10) 0.0391(11) 0.0023(8) 0.0130(8) 0.0032(7) C38 0.0440(12) 0.0344(11) 0.0454(12) 0.0061(9) 0.0122(10) 0.0111(9) C39 0.0517(13) 0.0367(12) 0.0554(14) -0.0064(10) 0.0116(11) -0.0051(10) C40 0.0454(12) 0.0336(10) 0.0387(11) 0.0047(9) 0.0089(9) 0.0025(9) C41 0.0317(9) 0.0293(9) 0.0303(10) -0.0011(8) 0.0021(8) -0.0004(7) N6 0.0296(8) 0.0268(8) 0.0276(8) 0.0010(6) 0.0054(6) 0.0021(6) C42 0.0331(10) 0.0293(9) 0.0243(9) -0.0025(7) 0.0021(7) 0.0045(7) C43 0.0365(10) 0.0298(9) 0.0287(9) -0.0026(8) 0.0042(8) 0.0016(8) C44 0.0491(12) 0.0291(10) 0.0352(11) -0.0003(8) 0.0084(9) 0.0046(9) C45 0.0496(12) 0.0358(11) 0.0339(11) -0.0001(9) 0.0081(9) 0.0138(9) C46 0.0381(11) 0.0440(12) 0.0295(10) 0.0002(9) 0.0088(8) 0.0105(9) C47 0.0352(10) 0.0344(10) 0.0251(9) -0.0014(8) 0.0036(8) 0.0039(8) C48 0.0393(11) 0.0328(10) 0.0385(11) -0.0019(8) 0.0063(9) -0.0039(8) C49 0.0652(16) 0.0416(13) 0.0602(15) 0.0045(11) 0.0207(13) 0.0225(11) C50 0.0354(10) 0.0392(11) 0.0403(11) 0.0008(9) 0.0100(9) 0.0018(9) B1A 0.024(4) 0.048(5) 0.067(7) -0.002(3) 0.008(3) 0.004(3) F1A 0.049(3) 0.038(2) 0.076(3) -0.008(2) 0.014(2) 0.002(2) F2A 0.044(2) 0.060(3) 0.046(4) 0.009(3) 0.012(2) 0.0050(19) F3A 0.067(2) 0.064(2) 0.0471(19) 0.0098(16) 0.0147(17) 0.0116(19) F4A 0.0397(18) 0.097(3) 0.072(3) -0.003(2) 0.0123(19) -0.0241(18) N1S 0.0865(18) 0.0651(16) 0.0640(15) -0.0084(13) 0.0128(13) -0.0075(13) C1S 0.0520(14) 0.0663(18) 0.0453(14) -0.0025(13) 0.0046(11) -0.0020(12) C2S 0.0698(19) 0.0725(19) 0.0693(19) -0.0141(15) 0.0041(15) 0.0077(15) _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 N1 2.0186(15) . ? Cu1 N4 2.0292(15) . ? Cu1 N6 2.0344(15) . ? Cu1 N3 2.0442(15) . ? N1 C1 1.352(2) . ? N1 C5 1.359(2) . ? C1 C2 1.389(3) . ? C1 C6 1.476(3) . ? C2 C3 1.385(3) . ? C3 C4 1.381(3) . ? C4 C5 1.388(3) . ? C5 C16 1.467(3) . ? C6 N2 1.260(2) . ? N2 C7 1.429(3) . ? C7 C8 1.395(3) . ? C7 C12 1.403(3) . ? C8 C9 1.393(3) . ? C8 C13 1.503(3) . ? C9 C10 1.389(3) . ? C10 C11 1.384(3) . ? C10 C14 1.513(3) . ? C11 C12 1.390(3) . ? C12 C15 1.503(3) . ? C16 N3 1.278(2) . ? N3 C17 1.435(2) . ? C17 C18 1.398(3) . ? C17 C22 1.404(3) . ? C18 C19 1.389(3) . ? C18 C23 1.505(3) . ? C19 C20 1.393(3) . ? C20 C21 1.386(3) . ? C20 C24 1.508(3) . ? C21 C22 1.395(3) . ? C22 C25 1.507(3) . ? N4 C26 1.347(2) . ? N4 C30 1.362(2) . ? C26 C27 1.395(3) . ? C26 C31 1.470(3) . ? C27 C28 1.377(3) . ? C28 C29 1.384(3) . ? C29 C30 1.383(3) . ? C30 C41 1.463(3) . ? C31 N5 1.270(2) . ? N5 C32 1.417(2) . ? C32 C37 1.409(3) . ? C32 C33 1.414(3) . ? C33 C34 1.386(3) . ? C33 C38 1.504(3) . ? C34 C35 1.387(3) . ? C35 C36 1.388(3) . ? C35 C39 1.512(3) . ? C36 C37 1.392(3) . ? C37 C40 1.514(3) . ? C41 N6 1.280(2) . ? N6 C42 1.440(2) . ? C42 C47 1.402(3) . ? C42 C43 1.406(3) . ? C43 C44 1.400(3) . ? C43 C48 1.508(3) . ? C44 C45 1.388(3) . ? C45 C46 1.387(3) . ? C45 C49 1.518(3) . ? C46 C47 1.398(3) . ? C47 C50 1.506(3) . ? B1A F3A 1.393(11) . ? B1A F1A 1.394(10) . ? B1A F4A 1.406(11) . ? B1A F2A 1.440(11) . ? B1B F2B 1.355(14) . ? B1B F4B 1.380(14) . ? B1B F3B 1.384(15) . ? B1B F1B 1.390(15) . ? B1C F1C 1.380(15) . ? B1C F4C 1.383(16) . ? B1C F2C 1.387(15) . ? B1C F3C 1.393(15) . ? N1S C1S 1.133(3) . ? C1S C2S 1.451(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N4 123.13(6) . . ? N1 Cu1 N6 139.88(6) . . ? N4 Cu1 N6 82.52(6) . . ? N1 Cu1 N3 81.85(6) . . ? N4 Cu1 N3 128.45(6) . . ? N6 Cu1 N3 106.98(6) . . ? C1 N1 C5 117.68(16) . . ? C1 N1 Cu1 129.88(12) . . ? C5 N1 Cu1 111.62(12) . . ? N1 C1 C2 122.10(17) . . ? N1 C1 C6 116.84(16) . . ? C2 C1 C6 121.04(17) . . ? C3 C2 C1 119.51(19) . . ? C4 C3 C2 119.05(18) . . ? C3 C4 C5 118.75(18) . . ? N1 C5 C4 122.82(18) . . ? N1 C5 C16 115.29(16) . . ? C4 C5 C16 121.88(17) . . ? N2 C6 C1 121.13(18) . . ? C6 N2 C7 120.15(17) . . ? C8 C7 C12 121.09(19) . . ? C8 C7 N2 119.31(18) . . ? C12 C7 N2 119.34(18) . . ? C9 C8 C7 118.54(19) . . ? C9 C8 C13 120.70(19) . . ? C7 C8 C13 120.76(19) . . ? C10 C9 C8 121.9(2) . . ? C11 C10 C9 117.8(2) . . ? C11 C10 C14 120.7(2) . . ? C9 C10 C14 121.5(2) . . ? C10 C11 C12 122.8(2) . . ? C11 C12 C7 117.8(2) . . ? C11 C12 C15 120.7(2) . . ? C7 C12 C15 121.5(2) . . ? N3 C16 C5 118.09(17) . . ? C16 N3 C17 120.62(16) . . ? C16 N3 Cu1 112.23(13) . . ? C17 N3 Cu1 125.79(12) . . ? C18 C17 C22 121.56(17) . . ? C18 C17 N3 117.79(16) . . ? C22 C17 N3 120.30(16) . . ? C19 C18 C17 118.38(17) . . ? C19 C18 C23 120.54(18) . . ? C17 C18 C23 121.07(18) . . ? C18 C19 C20 121.97(18) . . ? C21 C20 C19 117.93(18) . . ? C21 C20 C24 120.96(18) . . ? C19 C20 C24 121.10(19) . . ? C20 C21 C22 122.75(18) . . ? C21 C22 C17 117.41(17) . . ? C21 C22 C25 120.07(17) . . ? C17 C22 C25 122.48(18) . . ? C26 N4 C30 118.01(15) . . ? C26 N4 Cu1 131.56(13) . . ? C30 N4 Cu1 110.41(11) . . ? N4 C26 C27 121.86(17) . . ? N4 C26 C31 116.81(16) . . ? C27 C26 C31 121.33(17) . . ? C28 C27 C26 119.56(18) . . ? C27 C28 C29 119.07(18) . . ? C30 C29 C28 118.95(18) . . ? N4 C30 C29 122.51(17) . . ? N4 C30 C41 115.71(16) . . ? C29 C30 C41 121.78(17) . . ? N5 C31 C26 120.21(17) . . ? C31 N5 C32 122.59(16) . . ? C37 C32 C33 119.99(17) . . ? C37 C32 N5 124.35(17) . . ? C33 C32 N5 115.52(17) . . ? C34 C33 C32 119.00(18) . . ? C34 C33 C38 118.82(18) . . ? C32 C33 C38 122.18(18) . . ? C33 C34 C35 122.09(18) . . ? C34 C35 C36 117.92(19) . . ? C34 C35 C39 120.23(19) . . ? C36 C35 C39 121.8(2) . . ? C35 C36 C37 122.69(19) . . ? C36 C37 C32 118.21(17) . . ? C36 C37 C40 118.24(18) . . ? C32 C37 C40 123.51(18) . . ? N6 C41 C30 119.09(17) . . ? C41 N6 C42 119.69(16) . . ? C41 N6 Cu1 111.28(12) . . ? C42 N6 Cu1 127.76(12) . . ? C47 C42 C43 121.53(17) . . ? C47 C42 N6 117.25(16) . . ? C43 C42 N6 121.03(16) . . ? C44 C43 C42 117.26(18) . . ? C44 C43 C48 119.39(18) . . ? C42 C43 C48 123.28(17) . . ? C45 C44 C43 122.77(19) . . ? C46 C45 C44 118.23(18) . . ? C46 C45 C49 120.7(2) . . ? C44 C45 C49 121.0(2) . . ? C45 C46 C47 121.84(19) . . ? C46 C47 C42 118.37(18) . . ? C46 C47 C50 120.24(18) . . ? C42 C47 C50 121.39(17) . . ? F3A B1A F1A 112.1(8) . . ? F3A B1A F4A 108.1(7) . . ? F1A B1A F4A 111.5(8) . . ? F3A B1A F2A 109.9(8) . . ? F1A B1A F2A 108.0(8) . . ? F4A B1A F2A 107.0(8) . . ? F2B B1B F4B 108.4(11) . . ? F2B B1B F3B 107.3(11) . . ? F4B B1B F3B 109.4(12) . . ? F2B B1B F1B 111.3(11) . . ? F4B B1B F1B 111.4(11) . . ? F3B B1B F1B 108.8(12) . . ? F1C B1C F4C 106.9(13) . . ? F1C B1C F2C 111.2(13) . . ? F4C B1C F2C 110.5(13) . . ? F1C B1C F3C 108.3(12) . . ? F4C B1C F3C 111.9(15) . . ? F2C B1C F3C 108.1(13) . . ? N1S C1S C2S 178.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.394 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.050 #=END data_mh31 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[1,3-di{pyridin-2-yl}pyrazole]copper(II) diperchlorate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Cu N8, 2Cl O4' _chemical_formula_sum 'C26 H20 Cl2 Cu N8 O8' _chemical_formula_weight 706.94 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7526(19) _cell_length_b 8.7892(19) _cell_length_c 19.381(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.334(14) _cell_angle_gamma 90.00 _cell_volume 1489.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Lath _exptl_crystal_colour Green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.975 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_correction_T_max 0.7787 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Ten crystals were examined, all of which suffered from high mosaicity that increased at lower temperatures. The crystal used for data collection had a mosaicity of 0.914(3) at 293K, compared to a more normal value of 0.4-0.5. This accounts for the relatively poor quality of the refinement. A dataset from the same crystal collected at 150K could not be solved or refined. The unit cell was refined using all data. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7778 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 26.22 _reflns_number_total 4711 _reflns_number_gt 3077 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. Both perchlorate anions were disordered over two orientations: Anion 1: Cl36-O40, occupancy 0.6 and Cl41-O45, occupancy 0.4 Anion 2: Cl46-O50, occupancy 0.8 and Cl51-O55, occupancy 0.2 All Cl-O bonds were restrained to 1.39(2) /%A, and O...O distances to 2.27(2) /%A. The Uij thermal parameters of all O atoms were restrained to be equal to within 0.04 /%A^2^, with rigid bond restraints also being applied. The pyrazole N(1) and C(3) sites in each ligand could not be distinguished because of the low resolution of the structure, and may in fact be disordered. Therefore C2, C5, C20 and C23 were all refined as C atoms. All non-H atoms except Cl51-O55 were refined anisotropically. ; _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^)+(0.1379P)^2^+1.1265P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 4711 _refine_ls_number_parameters 473 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2601 _refine_ls_wR_factor_gt 0.2276 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24621(13) 0.1375(2) 0.24985(6) 0.0802(5) Uani 1 1 d . . . N2 N 0.2372(8) 0.1317(13) 0.3437(4) 0.085(2) Uani 1 1 d . . . C3 C 0.2876(12) 0.0172(10) 0.3871(5) 0.072(2) Uani 1 1 d . . . C4 C 0.2735(15) 0.0510(15) 0.4531(6) 0.095(3) Uani 1 1 d . . . H4 H 0.3029 -0.0095 0.4907 0.114 Uiso 1 1 calc R . . C5 C 0.2068(16) 0.1930(17) 0.4555(6) 0.103(4) Uani 1 1 d . . . H5 H 0.1794 0.2453 0.4948 0.123 Uiso 1 1 calc R . . C6 C 0.1894(13) 0.2409(11) 0.3899(5) 0.079(3) Uani 1 1 d . . . C7 C 0.3504(11) -0.1104(10) 0.3476(6) 0.078(2) Uani 1 1 d . . . C9 C 0.3948(12) -0.2131(12) 0.2400(7) 0.093(3) Uani 1 1 d . . . H9 H 0.3850 -0.2029 0.1923 0.112 Uiso 1 1 calc R . . N8 N 0.3446(9) -0.0959(9) 0.2813(5) 0.078(2) Uani 1 1 d . . . C10 C 0.4571(13) -0.3410(15) 0.2668(8) 0.105(4) Uani 1 1 d . . . H10 H 0.4952 -0.4171 0.2389 0.126 Uiso 1 1 calc R . . C11 C 0.4613(14) -0.3530(16) 0.3367(8) 0.111(4) Uani 1 1 d . . . H11 H 0.5025 -0.4404 0.3571 0.133 Uiso 1 1 calc R . . C12 C 0.4051(17) -0.2372(13) 0.3796(8) 0.111(4) Uani 1 1 d . . . H12 H 0.4058 -0.2477 0.4273 0.133 Uiso 1 1 calc R . . C13 C 0.1338(11) 0.3756(11) 0.3555(6) 0.076(2) Uani 1 1 d . . . N14 N 0.1498(9) 0.3683(8) 0.2875(5) 0.075(2) Uani 1 1 d . . . C15 C 0.0994(14) 0.4820(14) 0.2516(7) 0.099(3) Uani 1 1 d . . . H15 H 0.1014 0.4768 0.2037 0.119 Uiso 1 1 calc R . . C16 C 0.0406(13) 0.6157(13) 0.2827(8) 0.101(3) Uani 1 1 d . . . H16 H 0.0153 0.6997 0.2554 0.121 Uiso 1 1 calc R . . C17 C 0.0216(14) 0.6213(14) 0.3504(7) 0.103(3) Uani 1 1 d . . . H17 H -0.0209 0.7064 0.3708 0.124 Uiso 1 1 calc R . . C18 C 0.0674(14) 0.4958(13) 0.3897(7) 0.097(3) Uani 1 1 d . . . H18 H 0.0541 0.4925 0.4371 0.116 Uiso 1 1 calc R . . N19 N 0.2509(8) 0.1467(13) 0.1552(4) 0.088(2) Uani 1 1 d . . . C20 C 0.3697(11) 0.1934(11) 0.1113(5) 0.076(2) Uani 1 1 d . . . C21 C 0.3386(16) 0.1763(15) 0.0449(6) 0.107(4) Uani 1 1 d . . . H21 H 0.3990 0.1992 0.0079 0.129 Uiso 1 1 calc R . . C22 C 0.1899(16) 0.1140(19) 0.0442(5) 0.106(4) Uani 1 1 d . . . H22 H 0.1321 0.0885 0.0046 0.128 Uiso 1 1 calc R . . C23 C 0.1426(10) 0.0965(9) 0.1111(5) 0.070(2) Uani 1 1 d . . . C24 C 0.4995(10) 0.2524(10) 0.1487(6) 0.075(2) Uani 1 1 d . . . N25 N 0.4813(8) 0.2379(8) 0.2166(5) 0.079(2) Uani 1 1 d . . . C26 C 0.5940(15) 0.2798(12) 0.2539(7) 0.099(4) Uani 1 1 d . . . H26 H 0.5912 0.2643 0.3013 0.118 Uiso 1 1 calc R . . C27 C 0.7256(15) 0.3496(14) 0.2275(10) 0.102(4) Uani 1 1 d . . . H27 H 0.8021 0.3876 0.2574 0.123 Uiso 1 1 calc R . . C28 C 0.7389(14) 0.3606(13) 0.1575(9) 0.101(4) Uani 1 1 d . . . H28 H 0.8279 0.3981 0.1391 0.122 Uiso 1 1 calc R . . C29 C 0.6217(18) 0.3164(15) 0.1163(8) 0.113(4) Uani 1 1 d . . . H29 H 0.6220 0.3278 0.0686 0.136 Uiso 1 1 calc R . . C30 C 0.0114(12) 0.0365(11) 0.1466(5) 0.079(3) Uani 1 1 d . . . N31 N 0.0194(11) 0.0430(8) 0.2146(5) 0.081(2) Uani 1 1 d . . . C32 C -0.0998(14) -0.0095(12) 0.2523(7) 0.092(3) Uani 1 1 d . . . H32 H -0.0907 -0.0057 0.3003 0.110 Uiso 1 1 calc R . . C33 C -0.2266(15) -0.0649(15) 0.2227(10) 0.105(4) Uani 1 1 d . . . H33 H -0.3101 -0.0945 0.2477 0.126 Uiso 1 1 calc R . . C34 C -0.2249(16) -0.0750(16) 0.1541(9) 0.113(4) Uani 1 1 d . . . H34 H -0.3098 -0.1188 0.1316 0.135 Uiso 1 1 calc R . . C35 C -0.1103(15) -0.0271(15) 0.1142(6) 0.099(3) Uani 1 1 d . . . H35 H -0.1162 -0.0380 0.0665 0.118 Uiso 1 1 calc R . . Cl36 Cl -0.1932(12) 0.1485(12) -0.0675(4) 0.121(3) Uani 0.60 1 d PD A 1 O37 O -0.1402(19) 0.2308(18) -0.0109(6) 0.127(6) Uani 0.60 1 d PDU A 1 O38 O -0.151(2) 0.2258(18) -0.1273(6) 0.141(6) Uani 0.60 1 d PDU A 1 O39 O -0.109(2) 0.0072(15) -0.0706(9) 0.138(7) Uani 0.60 1 d PDU A 1 O40 O -0.343(2) 0.110(3) -0.0696(16) 0.242(19) Uani 0.60 1 d PDU A 1 Cl41 Cl -0.290(2) 0.129(2) -0.0622(6) 0.153(6) Uani 0.40 1 d PD B 2 O42 O -0.341(3) 0.044(3) -0.1193(10) 0.135(9) Uani 0.40 1 d PDU B 2 O43 O -0.335(3) 0.059(2) -0.0030(9) 0.124(8) Uani 0.40 1 d PDU B 2 O44 O -0.357(3) 0.277(2) -0.0678(13) 0.155(11) Uani 0.40 1 d PDU B 2 O45 O -0.134(2) 0.141(4) -0.0633(17) 0.177(18) Uani 0.40 1 d PDU B 2 Cl46 Cl 0.7311(7) 0.0790(6) 0.4374(3) 0.1148(14) Uani 0.80 1 d PD C 3 O47 O 0.8686(14) -0.0125(17) 0.4294(6) 0.146(5) Uani 0.80 1 d PDU C 3 O48 O 0.6454(18) 0.0499(19) 0.3783(6) 0.169(6) Uani 0.80 1 d PDU C 3 O49 O 0.6551(17) 0.0259(16) 0.4951(5) 0.157(6) Uani 0.80 1 d PDU C 3 O50 O 0.780(3) 0.2235(18) 0.4462(11) 0.215(11) Uani 0.80 1 d PDU C 3 Cl51 Cl 0.744(4) 0.184(3) 0.4294(13) 0.158(12) Uiso 0.20 1 d PD D 4 O52 O 0.827(4) 0.214(5) 0.4903(15) 0.100(12) Uiso 0.20 1 d PDU D 4 O53 O 0.601(3) 0.252(5) 0.4306(18) 0.119(13) Uiso 0.20 1 d PDU D 4 O54 O 0.822(4) 0.247(5) 0.3740(16) 0.111(12) Uiso 0.20 1 d PDU D 4 O55 O 0.729(7) 0.029(4) 0.418(3) 0.19(2) Uiso 0.20 1 d PDU D 4 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 0.0700(7) 0.0672(6) 0.1031(8) -0.0013(6) 0.0008(5) -0.0010(5) N2 0.051(4) 0.054(4) 0.149(6) -0.006(7) -0.009(4) -0.007(5) C3 0.067(6) 0.067(5) 0.083(6) 0.015(4) 0.000(4) 0.005(4) C4 0.095(9) 0.090(8) 0.100(9) 0.020(6) -0.009(6) -0.006(6) C5 0.093(9) 0.138(12) 0.077(7) -0.012(6) 0.001(5) -0.011(7) C6 0.087(7) 0.069(6) 0.079(6) -0.007(4) 0.001(5) 0.004(5) C7 0.067(6) 0.056(5) 0.109(8) 0.003(5) -0.010(5) 0.002(4) C9 0.052(5) 0.070(7) 0.157(10) -0.011(6) -0.010(6) -0.013(5) N8 0.061(5) 0.058(4) 0.116(7) -0.002(4) -0.003(4) -0.002(3) C10 0.075(7) 0.074(8) 0.166(11) -0.023(8) -0.007(7) 0.003(6) C11 0.089(7) 0.067(6) 0.173(12) 0.011(9) -0.019(7) 0.019(7) C12 0.119(10) 0.066(6) 0.148(10) 0.014(6) -0.005(8) 0.026(6) C13 0.066(6) 0.066(5) 0.097(7) -0.008(5) 0.003(5) -0.011(4) N14 0.057(5) 0.045(4) 0.122(7) 0.008(4) 0.002(4) -0.003(3) C15 0.083(8) 0.089(8) 0.128(9) 0.001(7) 0.011(6) -0.016(6) C16 0.086(7) 0.057(6) 0.158(11) -0.002(7) -0.011(6) 0.011(5) C17 0.102(8) 0.062(6) 0.145(10) -0.010(7) 0.000(7) 0.023(6) C18 0.081(7) 0.083(7) 0.127(9) -0.019(6) 0.011(6) 0.003(6) N19 0.049(4) 0.057(4) 0.158(7) -0.014(7) 0.003(4) 0.002(5) C20 0.059(5) 0.084(6) 0.087(6) 0.000(4) 0.017(4) -0.008(4) C21 0.110(10) 0.114(11) 0.100(8) 0.006(6) 0.027(6) -0.011(8) C22 0.116(10) 0.123(11) 0.079(6) -0.019(7) -0.011(6) 0.006(8) C23 0.053(5) 0.067(6) 0.088(6) -0.005(4) -0.008(4) 0.001(4) C24 0.045(5) 0.062(5) 0.118(8) 0.001(5) 0.009(5) 0.004(4) N25 0.040(4) 0.065(4) 0.131(7) -0.002(4) -0.006(4) 0.012(3) C26 0.086(9) 0.060(6) 0.147(10) 0.012(6) -0.016(7) 0.008(6) C27 0.072(8) 0.071(7) 0.162(12) -0.003(8) -0.013(8) 0.003(5) C28 0.049(6) 0.071(7) 0.185(14) -0.005(8) 0.010(7) -0.009(5) C29 0.104(11) 0.100(9) 0.138(11) 0.007(7) 0.030(8) 0.008(7) C30 0.066(6) 0.071(6) 0.101(7) -0.002(5) 0.001(5) -0.005(4) N31 0.086(6) 0.049(4) 0.108(6) 0.001(4) 0.003(5) -0.002(4) C32 0.076(7) 0.066(6) 0.134(9) -0.005(6) 0.016(6) 0.015(5) C33 0.066(7) 0.086(8) 0.161(12) 0.008(8) -0.002(7) -0.023(6) C34 0.063(8) 0.104(10) 0.169(14) -0.025(9) -0.015(8) -0.006(6) C35 0.079(8) 0.116(9) 0.100(8) -0.001(6) -0.014(6) -0.016(7) Cl36 0.111(7) 0.149(7) 0.103(5) 0.003(5) 0.001(4) 0.038(7) O37 0.139(14) 0.169(15) 0.073(8) -0.019(8) -0.004(8) 0.036(11) O38 0.171(18) 0.156(14) 0.093(10) 0.006(10) -0.017(10) -0.021(13) O39 0.162(17) 0.094(10) 0.158(14) -0.009(10) -0.002(11) 0.043(11) O40 0.21(3) 0.19(3) 0.33(4) -0.02(3) -0.01(3) 0.09(2) Cl41 0.129(11) 0.223(17) 0.105(7) -0.038(10) 0.002(8) 0.018(15) O42 0.15(2) 0.13(2) 0.130(19) -0.034(15) 0.012(16) -0.007(17) O43 0.14(2) 0.135(18) 0.092(15) -0.003(13) -0.014(13) 0.034(16) O44 0.15(3) 0.072(13) 0.25(3) -0.017(15) 0.02(2) 0.010(15) O45 0.12(3) 0.22(3) 0.19(3) 0.02(3) -0.04(2) -0.11(3) Cl46 0.125(4) 0.123(4) 0.096(3) -0.001(2) -0.002(2) 0.008(3) O47 0.119(10) 0.184(13) 0.137(10) 0.022(9) 0.017(7) 0.054(10) O48 0.174(15) 0.224(17) 0.108(9) 0.020(10) -0.023(8) -0.004(12) O49 0.212(17) 0.167(12) 0.095(8) 0.000(8) 0.031(8) 0.050(11) O50 0.17(2) 0.20(2) 0.27(3) -0.001(18) 0.019(19) -0.053(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.824(8) . ? Cu1 N19 1.838(9) . ? Cu1 N31 2.233(9) . ? Cu1 N8 2.297(8) . ? Cu1 N14 2.326(8) . ? Cu1 N25 2.353(9) . ? N2 C3 1.372(14) . ? N2 C6 1.389(14) . ? C3 C4 1.324(15) . ? C3 C7 1.476(14) . ? C4 C5 1.379(18) . ? C5 C6 1.341(14) . ? C6 C13 1.435(14) . ? C7 N8 1.292(13) . ? C7 C12 1.353(15) . ? C9 C10 1.344(17) . ? C9 N8 1.386(14) . ? C10 C11 1.359(16) . ? C11 C12 1.415(19) . ? C13 N14 1.333(12) . ? C13 C18 1.387(15) . ? N14 C15 1.285(14) . ? C15 C16 1.427(18) . ? C16 C17 1.331(16) . ? C17 C18 1.391(17) . ? N19 C23 1.326(11) . ? N19 C20 1.430(13) . ? C20 C21 1.313(14) . ? C20 C24 1.421(14) . ? C21 C22 1.411(18) . ? C22 C23 1.385(15) . ? C23 C30 1.461(14) . ? C24 N25 1.339(12) . ? C24 C29 1.382(18) . ? N25 C26 1.254(14) . ? C26 C27 1.42(2) . ? C27 C28 1.370(19) . ? C28 C29 1.332(19) . ? C30 N31 1.318(12) . ? C30 C35 1.336(15) . ? N31 C32 1.378(15) . ? C32 C33 1.322(16) . ? C33 C34 1.33(2) . ? C34 C35 1.36(2) . ? Cl36 O40 1.355(16) . ? Cl36 O37 1.379(13) . ? Cl36 O38 1.405(14) . ? Cl36 O39 1.447(14) . ? Cl41 O45 1.373(17) . ? Cl41 O43 1.375(17) . ? Cl41 O42 1.394(17) . ? Cl41 O44 1.425(17) . ? Cl46 O50 1.347(14) . ? Cl46 O48 1.367(11) . ? Cl46 O49 1.405(12) . ? Cl46 O47 1.461(11) . ? Cl51 O52 1.381(19) . ? Cl51 O55 1.387(19) . ? Cl51 O53 1.395(19) . ? Cl51 O54 1.406(19) . ? 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 N2 Cu1 N19 178.5(5) . . ? N2 Cu1 N31 102.7(3) . . ? N19 Cu1 N31 76.5(3) . . ? N2 Cu1 N8 75.0(4) . . ? N19 Cu1 N8 106.3(4) . . ? N31 Cu1 N8 93.9(3) . . ? N2 Cu1 N14 71.4(4) . . ? N19 Cu1 N14 107.3(4) . . ? N31 Cu1 N14 95.2(3) . . ? N8 Cu1 N14 146.4(3) . . ? N2 Cu1 N25 110.9(3) . . ? N19 Cu1 N25 69.8(3) . . ? N31 Cu1 N25 146.3(3) . . ? N8 Cu1 N25 94.9(3) . . ? N14 Cu1 N25 95.2(3) . . ? C3 N2 C6 102.1(8) . . ? C3 N2 Cu1 127.3(8) . . ? C6 N2 Cu1 130.5(8) . . ? C4 C3 N2 112.8(10) . . ? C4 C3 C7 136.3(10) . . ? N2 C3 C7 110.9(9) . . ? C3 C4 C5 107.0(10) . . ? C6 C5 C4 106.5(11) . . ? C5 C6 N2 111.7(10) . . ? C5 C6 C13 136.3(11) . . ? N2 C6 C13 112.1(9) . . ? N8 C7 C12 122.4(11) . . ? N8 C7 C3 116.1(8) . . ? C12 C7 C3 121.4(11) . . ? C10 C9 N8 122.1(12) . . ? C7 N8 C9 120.0(9) . . ? C7 N8 Cu1 110.6(6) . . ? C9 N8 Cu1 129.4(8) . . ? C9 C10 C11 116.4(13) . . ? C10 C11 C12 122.3(12) . . ? C7 C12 C11 116.7(12) . . ? N14 C13 C18 124.9(10) . . ? N14 C13 C6 111.9(8) . . ? C18 C13 C6 123.2(10) . . ? C15 N14 C13 116.8(9) . . ? C15 N14 Cu1 129.0(8) . . ? C13 N14 Cu1 114.0(6) . . ? N14 C15 C16 122.2(12) . . ? C17 C16 C15 120.6(12) . . ? C16 C17 C18 117.8(12) . . ? C13 C18 C17 117.3(12) . . ? C23 N19 C20 103.3(8) . . ? C23 N19 Cu1 125.8(8) . . ? C20 N19 Cu1 130.7(6) . . ? C21 C20 C24 132.2(10) . . ? C21 C20 N19 115.1(9) . . ? C24 C20 N19 112.8(9) . . ? C20 C21 C22 102.0(10) . . ? C23 C22 C21 110.2(9) . . ? N19 C23 C22 109.5(10) . . ? N19 C23 C30 111.8(9) . . ? C22 C23 C30 138.7(9) . . ? N25 C24 C29 127.7(11) . . ? N25 C24 C20 110.0(8) . . ? C29 C24 C20 122.3(11) . . ? C26 N25 C24 114.6(11) . . ? C26 N25 Cu1 128.9(10) . . ? C24 N25 Cu1 116.4(6) . . ? N25 C26 C27 123.4(14) . . ? C28 C27 C26 119.4(13) . . ? C29 C28 C27 118.6(13) . . ? C28 C29 C24 116.0(14) . . ? N31 C30 C35 119.8(11) . . ? N31 C30 C23 116.4(8) . . ? C35 C30 C23 123.8(11) . . ? C30 N31 C32 120.4(9) . . ? C30 N31 Cu1 109.4(6) . . ? C32 N31 Cu1 130.2(8) . . ? C33 C32 N31 122.2(13) . . ? C32 C33 C34 114.5(14) . . ? C33 C34 C35 125.8(12) . . ? C30 C35 C34 117.1(12) . . ? O40 Cl36 O37 116.7(14) . . ? O40 Cl36 O38 112.6(13) . . ? O37 Cl36 O38 108.1(11) . . ? O40 Cl36 O39 106.1(14) . . ? O37 Cl36 O39 109.1(10) . . ? O38 Cl36 O39 103.3(11) . . ? O45 Cl41 O43 111.7(16) . . ? O45 Cl41 O42 108.3(15) . . ? O43 Cl41 O42 109.2(15) . . ? O45 Cl41 O44 109.5(16) . . ? O43 Cl41 O44 109.9(14) . . ? O42 Cl41 O44 108.1(14) . . ? O50 Cl46 O48 116.2(11) . . ? O50 Cl46 O49 111.7(10) . . ? O48 Cl46 O49 110.1(10) . . ? O50 Cl46 O47 106.0(11) . . ? O48 Cl46 O47 103.5(8) . . ? O49 Cl46 O47 108.7(8) . . ? O52 Cl51 O55 111.7(18) . . ? O52 Cl51 O53 110.0(17) . . ? O55 Cl51 O53 110.0(18) . . ? O52 Cl51 O54 109.1(17) . . ? O55 Cl51 O54 107.8(17) . . ? O53 Cl51 O54 108.1(17) . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 0.738 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.152