Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Malcolm A. Halcrow' _publ_contact_author_address ; Department of Chemistry University of Leeds Woodhouse Lane LEEDS LS2 9JT UNITED KINGDOM ; _publ_contact_author_email M.A.HALCROW@LEEDS.AC.UK _publ_section_title ; Four Copper(II) Pyrazolido Complexes Derived from Reactions of 3{5}-Substituted Pyrazoles with CuF2 or Cu(OH)2 ; loop_ _publ_author_name 'Malcolm A. Halcrow' 'George Christou' 'Dolos Foguet-Albiol' 'Leigh F. Jones' 'Colin A. Kilner' ; R.M.Kowalczyk ; 'Patrick C. McGowan' 'Q. Folashade Mokuolu' 'Joanne Wolowska' data_1 _database_code_depnum_ccdc_archive 'CCDC 632224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis[3{5}-(pyrid-2-yl)pyrazolido]dicopper(II) dichloroform hemihydrate solvate ; _chemical_name_common ; Tetrakis(3(5)-(pyrid-2-yl)pyrazolido)dicopper(ii) dichloroform hemihydrate solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 Cu2 N12, 2[C H Cl3], 0.5[H2 O]' _chemical_formula_sum 'C34 H27 Cl6 Cu2 N12 O0.50' _chemical_formula_weight 951.46 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 27.6069(3) _cell_length_b 17.8695(2) _cell_length_c 32.0957(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15833.5(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 82877 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.44 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Green _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7664 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.910 _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 ; 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_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 '\w and \f scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82877 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.44 _reflns_number_total 18006 _reflns_number_gt 11523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 asymmetric unit contains two molecules of the complex compound (labelled 'A' and 'B'), four molecules of chloroform and one molecule of water. The final model contains no disorder; although solvent molecule C59-Cl62 exhibits some slightly high thermal parameters, attempts to resolve a second partial solvent molecule in this site were unsuccessful. All non-H atoms were refined anisotropically, and all C-bound H atoms were placed incalculated positions and refined using a riding model. The H atoms in the water molecule (O63) were located in the Fourier map and allowed to refine freely with a common isotropic thermal parameter, subject to the restraints O---H = 0.85(1)\%A and H...H = 1.39(2)\%A. The highest residual Fourier peak of +1.0 e.\%A^-3^ lies within the solvent molecule C55-Cl58. ; _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^)+(0.0863P)^2^+5.6680P] 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 18006 _refine_ls_number_parameters 989 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cu1A Cu 0.661844(17) 0.04344(3) 0.396947(16) 0.02668(13) Uani 1 1 d . . . Cu2A Cu 0.656406(16) 0.10073(2) 0.508660(15) 0.02368(12) Uani 1 1 d . . . N3A N 0.66367(11) 0.14488(17) 0.42129(10) 0.0261(7) Uani 1 1 d . . . N4A N 0.66268(11) 0.17048(17) 0.46064(10) 0.0260(7) Uani 1 1 d . . . C5A C 0.66284(14) 0.2457(2) 0.45897(13) 0.0296(9) Uani 1 1 d . . . H5A H 0.6621 0.2779 0.4825 0.036 Uiso 1 1 calc R . . C6A C 0.66431(15) 0.2695(2) 0.41781(13) 0.0325(10) Uani 1 1 d . . . H6A H 0.6649 0.3194 0.4077 0.039 Uiso 1 1 calc R . . C7A C 0.66473(14) 0.2037(2) 0.39490(13) 0.0283(9) Uani 1 1 d . . . C8A C 0.66596(14) 0.1857(2) 0.35043(13) 0.0299(9) Uani 1 1 d . . . N9A N 0.66421(12) 0.11121(18) 0.34237(11) 0.0299(8) Uani 1 1 d . . . C10A C 0.66517(16) 0.0886(3) 0.30257(14) 0.0369(10) Uani 1 1 d . . . H10A H 0.6643 0.0365 0.2969 0.044 Uiso 1 1 calc R . . C11A C 0.66742(18) 0.1376(3) 0.26960(14) 0.0447(12) Uani 1 1 d . . . H11A H 0.6680 0.1195 0.2418 0.054 Uiso 1 1 calc R . . C12A C 0.66890(19) 0.2139(3) 0.27763(16) 0.0512(13) Uani 1 1 d . . . H12A H 0.6707 0.2489 0.2554 0.061 Uiso 1 1 calc R . . C13A C 0.66772(18) 0.2381(3) 0.31877(14) 0.0422(11) Uani 1 1 d . . . H13A H 0.6681 0.2900 0.3251 0.051 Uiso 1 1 calc R . . N14A N 0.61563(11) 0.02992(17) 0.47866(10) 0.0259(7) Uani 1 1 d . . . N15A N 0.61644(11) 0.00246(17) 0.43939(10) 0.0257(7) Uani 1 1 d . . . C16A C 0.58336(15) -0.0519(2) 0.43719(14) 0.0340(10) Uani 1 1 d . . . H16A H 0.5768 -0.0806 0.4129 0.041 Uiso 1 1 calc R . . C17A C 0.55992(16) -0.0608(2) 0.47500(15) 0.0379(10) Uani 1 1 d . . . H17A H 0.5348 -0.0951 0.4818 0.045 Uiso 1 1 calc R . . C18A C 0.58166(14) -0.0077(2) 0.50077(13) 0.0290(9) Uani 1 1 d . . . C19A C 0.57691(14) 0.0147(2) 0.54442(13) 0.0290(9) Uani 1 1 d . . . N20A N 0.60911(11) 0.06811(17) 0.55615(10) 0.0267(7) Uani 1 1 d . . . C21A C 0.60867(16) 0.0921(2) 0.59566(14) 0.0355(10) Uani 1 1 d . . . H21A H 0.6308 0.1301 0.6037 0.043 Uiso 1 1 calc R . . C22A C 0.57710(18) 0.0635(3) 0.62530(15) 0.0448(12) Uani 1 1 d . . . H22A H 0.5782 0.0802 0.6534 0.054 Uiso 1 1 calc R . . C23A C 0.54406(18) 0.0101(3) 0.61293(16) 0.0476(12) Uani 1 1 d . . . H23A H 0.5215 -0.0095 0.6324 0.057 Uiso 1 1 calc R . . C24A C 0.54367(17) -0.0152(3) 0.57219(15) 0.0401(11) Uani 1 1 d . . . H24A H 0.5211 -0.0522 0.5634 0.048 Uiso 1 1 calc R . . N25A N 0.66690(12) -0.04724(18) 0.36374(11) 0.0293(8) Uani 1 1 d . . . N26A N 0.63324(14) -0.08831(19) 0.34302(11) 0.0373(9) Uani 1 1 d . . . C27A C 0.6589(2) -0.1388(3) 0.32069(14) 0.0442(12) Uani 1 1 d . . . H27A H 0.6447 -0.1752 0.3029 0.053 Uiso 1 1 calc R . . C28A C 0.7080(2) -0.1310(2) 0.32680(15) 0.0460(12) Uani 1 1 d . . . H28A H 0.7334 -0.1597 0.3148 0.055 Uiso 1 1 calc R . . C29A C 0.71183(17) -0.0716(2) 0.35448(13) 0.0340(10) Uani 1 1 d . . . C30A C 0.75270(15) -0.0321(2) 0.37301(13) 0.0318(9) Uani 1 1 d . . . N31A N 0.73938(12) 0.02304(18) 0.40016(11) 0.0303(8) Uani 1 1 d . . . C32A C 0.77467(16) 0.0620(3) 0.41938(15) 0.0410(11) Uani 1 1 d . . . H32A H 0.7656 0.1014 0.4377 0.049 Uiso 1 1 calc R . . C33A C 0.82338(17) 0.0475(3) 0.41380(17) 0.0501(13) Uani 1 1 d . . . H33A H 0.8473 0.0741 0.4291 0.060 Uiso 1 1 calc R . . C34A C 0.83630(17) -0.0067(3) 0.38536(19) 0.0557(15) Uani 1 1 d . . . H34A H 0.8695 -0.0161 0.3797 0.067 Uiso 1 1 calc R . . C35A C 0.80088(17) -0.0472(2) 0.36514(17) 0.0457(12) Uani 1 1 d . . . H35A H 0.8096 -0.0853 0.3459 0.055 Uiso 1 1 calc R . . N36A N 0.69830(11) 0.15686(16) 0.54559(10) 0.0245(7) Uani 1 1 d . . . N37A N 0.69330(12) 0.22480(18) 0.56373(11) 0.0308(8) Uani 1 1 d . . . C38A C 0.73186(15) 0.2334(2) 0.58860(14) 0.0354(10) Uani 1 1 d . . . H38A H 0.7374 0.2762 0.6054 0.043 Uiso 1 1 calc R . . C39A C 0.76264(14) 0.1723(2) 0.58684(13) 0.0304(9) Uani 1 1 d . . . H39A H 0.7923 0.1649 0.6012 0.036 Uiso 1 1 calc R . . C40A C 0.73978(13) 0.1243(2) 0.55901(12) 0.0253(8) Uani 1 1 d . . . C41A C 0.75080(14) 0.0497(2) 0.54237(12) 0.0263(8) Uani 1 1 d . . . N42A N 0.71756(11) 0.02292(17) 0.51498(10) 0.0247(7) Uani 1 1 d . . . C43A C 0.72474(15) -0.0450(2) 0.49857(14) 0.0336(10) Uani 1 1 d . . . H43A H 0.7013 -0.0638 0.4796 0.040 Uiso 1 1 calc R . . C44A C 0.76393(16) -0.0888(2) 0.50767(16) 0.0422(11) Uani 1 1 d . . . H44A H 0.7675 -0.1369 0.4955 0.051 Uiso 1 1 calc R . . C45A C 0.79820(17) -0.0614(3) 0.53496(17) 0.0481(13) Uani 1 1 d . . . H45A H 0.8259 -0.0906 0.5417 0.058 Uiso 1 1 calc R . . C46A C 0.79212(16) 0.0087(2) 0.55251(15) 0.0396(11) Uani 1 1 d . . . H46A H 0.8156 0.0285 0.5711 0.048 Uiso 1 1 calc R . . Cu1B Cu 0.458549(17) 0.33027(3) 0.502541(15) 0.02590(12) Uani 1 1 d . . . Cu2B Cu 0.438835(17) 0.29443(3) 0.384106(15) 0.02696(13) Uani 1 1 d . . . N3B N 0.43754(11) 0.39654(17) 0.45699(10) 0.0246(7) Uani 1 1 d . . . N4B N 0.42782(11) 0.38722(17) 0.41596(10) 0.0247(7) Uani 1 1 d . . . C5B C 0.41437(14) 0.4546(2) 0.40094(13) 0.0278(9) Uani 1 1 d . . . H5B H 0.4056 0.4640 0.3728 0.033 Uiso 1 1 calc R . . C6B C 0.41512(14) 0.5081(2) 0.43188(13) 0.0284(9) Uani 1 1 d . . . H6B H 0.4074 0.5597 0.4297 0.034 Uiso 1 1 calc R . . C7B C 0.42981(13) 0.4690(2) 0.46692(12) 0.0254(8) Uani 1 1 d . . . C8B C 0.43964(13) 0.4905(2) 0.50979(12) 0.0256(8) Uani 1 1 d . . . N9B N 0.45526(11) 0.43309(18) 0.53412(10) 0.0277(7) Uani 1 1 d . . . C10B C 0.46693(14) 0.4476(3) 0.57402(13) 0.0330(10) Uani 1 1 d . . . H10B H 0.4780 0.4078 0.5912 0.040 Uiso 1 1 calc R . . C11B C 0.46323(15) 0.5190(3) 0.59092(13) 0.0361(10) Uani 1 1 d . . . H11B H 0.4716 0.5276 0.6192 0.043 Uiso 1 1 calc R . . C12B C 0.44723(15) 0.5774(2) 0.56614(14) 0.0354(10) Uani 1 1 d . . . H12B H 0.4449 0.6267 0.5771 0.043 Uiso 1 1 calc R . . C13B C 0.43465(14) 0.5632(2) 0.52490(13) 0.0312(9) Uani 1 1 d . . . H13B H 0.4229 0.6021 0.5075 0.037 Uiso 1 1 calc R . . N14B N 0.48393(11) 0.25012(17) 0.42439(10) 0.0274(7) Uani 1 1 d . . . N15B N 0.49210(11) 0.25706(17) 0.46571(10) 0.0271(7) Uani 1 1 d . . . C16B C 0.52806(14) 0.2093(2) 0.47607(14) 0.0311(9) Uani 1 1 d . . . H16B H 0.5408 0.2032 0.5033 0.037 Uiso 1 1 calc R . . C17B C 0.54347(14) 0.1708(2) 0.44144(14) 0.0346(10) Uani 1 1 d . . . H17B H 0.5681 0.1337 0.4399 0.041 Uiso 1 1 calc R . . C18B C 0.51508(14) 0.1982(2) 0.40942(13) 0.0292(9) Uani 1 1 d . . . C19B C 0.51189(14) 0.1822(2) 0.36465(14) 0.0314(9) Uani 1 1 d . . . N20B N 0.47769(12) 0.22245(18) 0.34465(11) 0.0310(8) Uani 1 1 d . . . C21B C 0.47210(17) 0.2122(2) 0.30345(14) 0.0377(10) Uani 1 1 d . . . H21B H 0.4480 0.2403 0.2892 0.045 Uiso 1 1 calc R . . C22B C 0.50007(17) 0.1626(3) 0.28105(16) 0.0454(12) Uani 1 1 d . . . H22B H 0.4956 0.1576 0.2518 0.054 Uiso 1 1 calc R . . C23B C 0.53443(18) 0.1205(3) 0.30123(17) 0.0499(13) Uani 1 1 d . . . H23B H 0.5534 0.0850 0.2864 0.060 Uiso 1 1 calc R . . C24B C 0.54097(16) 0.1308(2) 0.34363(16) 0.0422(12) Uani 1 1 d . . . H24B H 0.5650 0.1032 0.3582 0.051 Uiso 1 1 calc R . . N25B N 0.47408(11) 0.27620(18) 0.55412(11) 0.0299(8) Uani 1 1 d . . . N26B N 0.51576(12) 0.2660(2) 0.57589(11) 0.0336(8) Uani 1 1 d . . . C27B C 0.50338(15) 0.2317(2) 0.61120(13) 0.0317(9) Uani 1 1 d . . . H27B H 0.5258 0.2181 0.6324 0.038 Uiso 1 1 calc R . . C28B C 0.45414(14) 0.2181(2) 0.61335(13) 0.0287(9) Uani 1 1 d . . . H28B H 0.4365 0.1944 0.6351 0.034 Uiso 1 1 calc R . . C29B C 0.43649(13) 0.2474(2) 0.57590(12) 0.0242(8) Uani 1 1 d . . . C30B C 0.38768(13) 0.2528(2) 0.55793(12) 0.0249(8) Uani 1 1 d . . . N31B N 0.38601(11) 0.28712(17) 0.52055(10) 0.0259(7) Uani 1 1 d . . . C32B C 0.34304(14) 0.2929(2) 0.50130(13) 0.0288(9) Uani 1 1 d . . . H32B H 0.3420 0.3161 0.4747 0.035 Uiso 1 1 calc R . . C33B C 0.30054(14) 0.2670(2) 0.51823(14) 0.0323(10) Uani 1 1 d . . . H33B H 0.2707 0.2724 0.5037 0.039 Uiso 1 1 calc R . . C34B C 0.30220(15) 0.2328(2) 0.55705(14) 0.0357(10) Uani 1 1 d . . . H34B H 0.2733 0.2151 0.5698 0.043 Uiso 1 1 calc R . . C35B C 0.34638(14) 0.2248(2) 0.57691(13) 0.0315(9) Uani 1 1 d . . . H35B H 0.3484 0.2004 0.6032 0.038 Uiso 1 1 calc R . . N36B N 0.39864(13) 0.32632(18) 0.33728(10) 0.0308(8) Uani 1 1 d . . . N37B N 0.40537(15) 0.38193(19) 0.30935(11) 0.0389(9) Uani 1 1 d . . . C38B C 0.3682(2) 0.3762(3) 0.28250(15) 0.0522(14) Uani 1 1 d . . . H38B H 0.3635 0.4085 0.2594 0.063 Uiso 1 1 calc R . . C39B C 0.33760(18) 0.3173(3) 0.29268(15) 0.0479(12) Uani 1 1 d . . . H39B H 0.3089 0.3020 0.2787 0.057 Uiso 1 1 calc R . . C40B C 0.35852(15) 0.2861(2) 0.32789(13) 0.0319(9) Uani 1 1 d . . . C41B C 0.34708(14) 0.2218(2) 0.35399(13) 0.0315(9) Uani 1 1 d . . . N42B N 0.37584(12) 0.21421(17) 0.38800(11) 0.0301(8) Uani 1 1 d . . . C43B C 0.36823(16) 0.1555(2) 0.41330(15) 0.0383(11) Uani 1 1 d . . . H43B H 0.3879 0.1504 0.4374 0.046 Uiso 1 1 calc R . . C44B C 0.33297(17) 0.1024(2) 0.40577(17) 0.0442(12) Uani 1 1 d . . . H44B H 0.3289 0.0611 0.4241 0.053 Uiso 1 1 calc R . . C45B C 0.30376(17) 0.1103(3) 0.37126(17) 0.0466(13) Uani 1 1 d . . . H45B H 0.2790 0.0748 0.3656 0.056 Uiso 1 1 calc R . . C46B C 0.31083(16) 0.1706(2) 0.34495(15) 0.0398(11) Uani 1 1 d . . . H46B H 0.2911 0.1768 0.3210 0.048 Uiso 1 1 calc R . . C47 C 0.61398(18) 0.3479(3) 0.65087(15) 0.0467(12) Uani 1 1 d . . . H47 H 0.6039 0.3415 0.6212 0.056 Uiso 1 1 calc R . . Cl48 Cl 0.66628(5) 0.40413(8) 0.65213(5) 0.0619(4) Uani 1 1 d . . . Cl49 Cl 0.62617(6) 0.25872(7) 0.67198(4) 0.0663(4) Uani 1 1 d . . . Cl50 Cl 0.56692(5) 0.39191(8) 0.67772(5) 0.0628(4) Uani 1 1 d . . . C51 C 0.8513(2) 0.1156(3) 0.30088(17) 0.0550(14) Uani 1 1 d . . . H51 H 0.8498 0.0603 0.3055 0.066 Uiso 1 1 calc R . . Cl52 Cl 0.86645(6) 0.13099(10) 0.24882(5) 0.0789(5) Uani 1 1 d . . . Cl53 Cl 0.89646(6) 0.15212(8) 0.33373(5) 0.0682(4) Uani 1 1 d . . . Cl54 Cl 0.79491(6) 0.15352(9) 0.31376(6) 0.0838(5) Uani 1 1 d . . . C55 C 0.6928(2) 0.4634(4) 0.2099(2) 0.0781(19) Uani 1 1 d . . . H55 H 0.6750 0.5061 0.1967 0.094 Uiso 1 1 calc R . . Cl56 Cl 0.71573(6) 0.40718(9) 0.16934(5) 0.0783(5) Uani 1 1 d . . . Cl57 Cl 0.65229(9) 0.41596(10) 0.24045(7) 0.1079(8) Uani 1 1 d . . . Cl58 Cl 0.74084(7) 0.50118(13) 0.23862(7) 0.1136(8) Uani 1 1 d . . . C59 C 0.5146(2) 0.4048(3) 0.2803(2) 0.0702(17) Uani 1 1 d . . . H59 H 0.4823 0.3990 0.2940 0.084 Uiso 1 1 calc R . . Cl60 Cl 0.53059(7) 0.49956(9) 0.28063(7) 0.0978(7) Uani 1 1 d . . . Cl61 Cl 0.51141(11) 0.36869(18) 0.23037(7) 0.1552(12) Uani 1 1 d . . . Cl62 Cl 0.55815(6) 0.35513(9) 0.30933(7) 0.0901(6) Uani 1 1 d . . . O63 O 0.60983(10) 0.31449(15) 0.55429(10) 0.0325(7) Uani 1 1 d D . . H63A H 0.5823(6) 0.2937(19) 0.5535(16) 0.056(11) Uiso 1 1 d D . . H63B H 0.6318(9) 0.2816(16) 0.5554(16) 0.056(11) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1A 0.0291(3) 0.0230(2) 0.0279(3) -0.0024(2) -0.0017(2) -0.0008(2) Cu2A 0.0238(2) 0.0213(2) 0.0260(3) -0.00013(19) -0.0036(2) -0.00049(19) N3A 0.0292(18) 0.0229(16) 0.0261(18) -0.0003(14) -0.0018(14) -0.0007(14) N4A 0.0261(17) 0.0216(16) 0.0303(19) -0.0009(14) -0.0023(14) -0.0010(13) C5A 0.033(2) 0.024(2) 0.031(2) -0.0008(17) -0.0006(18) -0.0041(17) C6A 0.041(2) 0.021(2) 0.035(2) 0.0037(18) -0.003(2) -0.0048(18) C7A 0.028(2) 0.031(2) 0.025(2) 0.0015(17) 0.0004(17) -0.0012(17) C8A 0.029(2) 0.030(2) 0.032(2) 0.0055(18) -0.0030(18) -0.0018(17) N9A 0.0330(19) 0.0305(18) 0.0261(19) -0.0004(15) -0.0019(15) 0.0011(15) C10A 0.042(3) 0.037(2) 0.032(2) -0.0024(19) -0.005(2) 0.001(2) C11A 0.057(3) 0.052(3) 0.025(2) -0.002(2) -0.005(2) -0.002(2) C12A 0.069(4) 0.048(3) 0.036(3) 0.011(2) 0.000(3) -0.005(3) C13A 0.060(3) 0.033(2) 0.035(3) 0.006(2) -0.002(2) -0.001(2) N14A 0.0262(17) 0.0250(16) 0.0267(18) 0.0010(14) -0.0035(14) 0.0017(14) N15A 0.0249(17) 0.0235(16) 0.0287(19) -0.0040(14) -0.0058(14) -0.0010(13) C16A 0.032(2) 0.031(2) 0.039(3) -0.0071(19) -0.008(2) -0.0046(18) C17A 0.036(2) 0.036(2) 0.042(3) -0.002(2) 0.003(2) -0.015(2) C18A 0.0214(19) 0.026(2) 0.039(2) 0.0061(18) -0.0013(18) -0.0023(16) C19A 0.024(2) 0.026(2) 0.036(2) 0.0046(18) 0.0025(18) 0.0031(16) N20A 0.0254(17) 0.0244(16) 0.0302(19) -0.0006(15) 0.0010(15) 0.0024(13) C21A 0.043(3) 0.030(2) 0.033(3) -0.0036(19) 0.002(2) -0.0006(19) C22A 0.055(3) 0.041(3) 0.038(3) -0.002(2) 0.015(2) -0.005(2) C23A 0.051(3) 0.048(3) 0.044(3) 0.009(2) 0.017(2) -0.007(2) C24A 0.040(2) 0.038(2) 0.042(3) 0.003(2) 0.005(2) -0.008(2) N25A 0.0357(19) 0.0256(17) 0.0267(19) 0.0020(14) -0.0064(15) -0.0014(15) N26A 0.049(2) 0.035(2) 0.028(2) -0.0043(16) -0.0093(17) -0.0131(17) C27A 0.077(4) 0.035(2) 0.021(2) -0.0029(19) 0.003(2) -0.018(2) C28A 0.071(4) 0.028(2) 0.039(3) -0.003(2) 0.018(3) -0.004(2) C29A 0.051(3) 0.022(2) 0.029(2) 0.0047(18) -0.001(2) 0.0042(19) C30A 0.036(2) 0.026(2) 0.034(2) 0.0070(18) 0.0021(19) 0.0064(18) N31A 0.0326(18) 0.0292(18) 0.0291(19) 0.0012(15) -0.0057(15) -0.0010(15) C32A 0.038(3) 0.046(3) 0.039(3) 0.002(2) -0.008(2) -0.010(2) C33A 0.032(2) 0.062(3) 0.056(3) 0.010(3) -0.012(2) -0.007(2) C34A 0.028(2) 0.059(3) 0.080(4) 0.023(3) 0.000(3) 0.007(2) C35A 0.042(3) 0.033(2) 0.062(3) 0.011(2) 0.009(2) 0.014(2) N36A 0.0232(16) 0.0234(16) 0.0269(18) -0.0004(14) -0.0011(14) 0.0015(13) N37A 0.0278(18) 0.0269(17) 0.038(2) -0.0084(15) -0.0017(16) -0.0008(14) C38A 0.034(2) 0.034(2) 0.039(3) -0.009(2) 0.000(2) -0.0056(19) C39A 0.025(2) 0.035(2) 0.032(2) -0.0006(19) -0.0048(18) -0.0022(17) C40A 0.0211(19) 0.028(2) 0.027(2) 0.0022(17) 0.0004(17) -0.0032(16) C41A 0.0249(19) 0.028(2) 0.026(2) 0.0039(17) -0.0024(17) 0.0018(16) N42A 0.0244(16) 0.0240(16) 0.0256(18) 0.0005(14) 0.0010(14) 0.0014(13) C43A 0.035(2) 0.028(2) 0.038(3) -0.0027(19) -0.005(2) 0.0022(18) C44A 0.039(3) 0.031(2) 0.057(3) -0.006(2) -0.005(2) 0.007(2) C45A 0.036(3) 0.039(3) 0.069(4) -0.003(2) -0.012(3) 0.011(2) C46A 0.034(2) 0.038(2) 0.046(3) -0.001(2) -0.011(2) 0.0068(19) Cu1B 0.0246(2) 0.0292(3) 0.0238(3) 0.0048(2) -0.0003(2) 0.0016(2) Cu2B 0.0316(3) 0.0243(2) 0.0251(3) 0.0014(2) -0.0014(2) 0.0021(2) N3B 0.0251(16) 0.0266(16) 0.0220(17) 0.0001(13) -0.0016(14) 0.0006(14) N4B 0.0248(17) 0.0286(17) 0.0207(17) 0.0022(14) -0.0052(14) 0.0018(13) C5B 0.029(2) 0.026(2) 0.029(2) 0.0046(17) -0.0046(17) 0.0042(17) C6B 0.029(2) 0.026(2) 0.031(2) 0.0033(17) 0.0036(18) 0.0039(17) C7B 0.0242(19) 0.0238(19) 0.028(2) 0.0007(16) 0.0024(17) 0.0010(16) C8B 0.0195(18) 0.030(2) 0.027(2) 0.0014(17) 0.0040(17) -0.0031(16) N9B 0.0212(16) 0.0369(18) 0.0249(18) -0.0008(15) 0.0037(14) -0.0032(14) C10B 0.024(2) 0.050(3) 0.025(2) 0.002(2) -0.0004(17) -0.0047(19) C11B 0.034(2) 0.050(3) 0.024(2) -0.010(2) 0.0027(19) -0.011(2) C12B 0.037(2) 0.032(2) 0.037(3) -0.008(2) 0.008(2) -0.0084(19) C13B 0.028(2) 0.034(2) 0.032(2) -0.0006(19) 0.0043(18) -0.0048(18) N14B 0.0271(17) 0.0252(17) 0.0299(19) 0.0006(14) 0.0019(15) 0.0019(14) N15B 0.0294(17) 0.0239(16) 0.0280(19) 0.0053(14) -0.0046(15) -0.0038(14) C16B 0.026(2) 0.026(2) 0.041(3) 0.0035(19) -0.0052(19) -0.0010(17) C17B 0.025(2) 0.029(2) 0.050(3) -0.001(2) -0.002(2) 0.0032(17) C18B 0.028(2) 0.0231(19) 0.036(2) -0.0022(17) 0.0042(19) 0.0008(17) C19B 0.029(2) 0.028(2) 0.037(2) -0.0037(18) 0.0046(19) -0.0032(17) N20B 0.0330(18) 0.0284(17) 0.032(2) -0.0021(15) -0.0006(16) -0.0003(15) C21B 0.043(3) 0.036(2) 0.033(3) -0.005(2) 0.000(2) 0.002(2) C22B 0.046(3) 0.053(3) 0.037(3) -0.014(2) 0.007(2) -0.004(2) C23B 0.042(3) 0.055(3) 0.054(3) -0.020(3) 0.011(2) 0.001(2) C24B 0.031(2) 0.034(2) 0.061(3) -0.015(2) 0.003(2) 0.0024(19) N25B 0.0231(17) 0.0378(19) 0.0287(19) 0.0075(15) -0.0025(15) 0.0016(14) N26B 0.0228(17) 0.044(2) 0.034(2) 0.0069(17) -0.0044(15) 0.0004(15) C27B 0.032(2) 0.033(2) 0.030(2) 0.0026(18) -0.0060(19) 0.0002(18) C28B 0.030(2) 0.031(2) 0.025(2) 0.0037(17) -0.0045(18) -0.0026(17) C29B 0.0230(19) 0.0249(19) 0.025(2) 0.0026(16) -0.0014(16) -0.0010(16) C30B 0.0257(19) 0.0221(19) 0.027(2) -0.0043(16) -0.0014(17) 0.0026(16) N31B 0.0269(17) 0.0250(16) 0.0257(18) 0.0009(14) 0.0005(14) 0.0008(14) C32B 0.026(2) 0.032(2) 0.028(2) 0.0042(17) -0.0046(17) -0.0020(17) C33B 0.025(2) 0.036(2) 0.036(3) 0.0014(19) -0.0069(18) 0.0003(18) C34B 0.025(2) 0.038(2) 0.044(3) 0.006(2) 0.001(2) -0.0044(18) C35B 0.032(2) 0.033(2) 0.030(2) 0.0033(18) 0.0011(18) -0.0040(18) N36B 0.042(2) 0.0258(17) 0.0246(18) 0.0036(14) -0.0023(16) 0.0045(15) N37B 0.058(2) 0.033(2) 0.026(2) 0.0048(16) -0.0050(18) 0.0016(18) C38B 0.080(4) 0.045(3) 0.031(3) 0.007(2) -0.018(3) 0.011(3) C39B 0.050(3) 0.052(3) 0.041(3) 0.004(2) -0.021(2) 0.002(2) C40B 0.033(2) 0.035(2) 0.028(2) -0.0052(18) -0.0019(18) 0.0058(18) C41B 0.029(2) 0.032(2) 0.033(2) -0.0074(18) 0.0033(19) 0.0036(18) N42B 0.0333(18) 0.0259(18) 0.031(2) -0.0009(15) 0.0071(16) 0.0053(14) C43B 0.039(2) 0.031(2) 0.045(3) 0.003(2) 0.004(2) 0.0046(19) C44B 0.044(3) 0.032(2) 0.057(3) 0.007(2) 0.017(2) 0.001(2) C45B 0.039(3) 0.039(3) 0.062(4) -0.014(2) 0.016(3) -0.004(2) C46B 0.031(2) 0.047(3) 0.041(3) -0.013(2) 0.003(2) 0.002(2) C47 0.062(3) 0.048(3) 0.030(3) 0.000(2) -0.004(2) 0.005(2) Cl48 0.0588(8) 0.0760(9) 0.0510(8) 0.0157(7) 0.0026(7) -0.0035(7) Cl49 0.1062(12) 0.0447(7) 0.0478(8) 0.0000(6) -0.0283(8) 0.0062(7) Cl50 0.0659(9) 0.0652(8) 0.0574(9) 0.0053(7) 0.0176(7) 0.0054(7) C51 0.066(3) 0.044(3) 0.056(3) 0.005(3) -0.010(3) -0.001(3) Cl52 0.0902(12) 0.0912(11) 0.0555(9) 0.0202(8) -0.0105(8) -0.0236(9) Cl53 0.0647(9) 0.0717(9) 0.0684(10) -0.0103(8) -0.0193(8) -0.0059(7) Cl54 0.0603(9) 0.0785(11) 0.1127(15) -0.0150(10) -0.0106(9) 0.0059(8) C55 0.081(5) 0.082(4) 0.072(5) 0.004(4) 0.005(4) -0.002(4) Cl56 0.0867(11) 0.0813(11) 0.0669(11) -0.0266(8) 0.0093(9) 0.0005(9) Cl57 0.1354(18) 0.0676(11) 0.1207(17) 0.0023(11) 0.0652(14) -0.0127(11) Cl58 0.0811(13) 0.150(2) 0.1099(16) -0.0669(15) -0.0190(12) 0.0041(12) C59 0.070(4) 0.066(4) 0.075(4) 0.001(3) 0.019(3) -0.015(3) Cl60 0.0789(11) 0.0545(9) 0.160(2) 0.0330(11) 0.0231(12) 0.0013(8) Cl61 0.189(3) 0.210(3) 0.0669(13) -0.0255(16) 0.0471(16) -0.092(2) Cl62 0.0709(10) 0.0596(9) 0.1398(18) 0.0240(10) 0.0157(11) 0.0008(8) O63 0.0287(15) 0.0254(14) 0.0434(19) 0.0016(13) 0.0011(15) 0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1A N25A 1.945(3) . ? Cu1A N3A 1.975(3) . ? Cu1A N15A 1.991(3) . ? Cu1A N9A 2.130(3) . ? Cu1A N31A 2.174(3) . ? Cu1A Cu2A 3.7318(7) . ? Cu2A N36A 1.936(3) . ? Cu2A N14A 1.948(3) . ? Cu2A N4A 1.990(3) . ? Cu2A N20A 2.090(3) . ? Cu2A N42A 2.196(3) . ? N3A N4A 1.344(4) . ? N3A C7A 1.351(5) . ? N4A C5A 1.346(5) . ? C5A C6A 1.388(6) . ? C6A C7A 1.386(6) . ? C7A C8A 1.464(6) . ? C8A N9A 1.356(5) . ? C8A C13A 1.382(6) . ? N9A C10A 1.340(5) . ? C10A C11A 1.374(6) . ? C11A C12A 1.389(7) . ? C12A C13A 1.390(7) . ? N14A N15A 1.353(4) . ? N14A C18A 1.355(5) . ? N15A C16A 1.335(5) . ? C16A C17A 1.385(6) . ? C17A C18A 1.394(6) . ? C18A C19A 1.463(6) . ? C19A N20A 1.357(5) . ? C19A C24A 1.386(6) . ? N20A C21A 1.339(5) . ? C21A C22A 1.388(6) . ? C22A C23A 1.379(7) . ? C23A C24A 1.383(7) . ? N25A C29A 1.348(5) . ? N25A N26A 1.358(4) . ? N26A C27A 1.352(6) . ? C27A C28A 1.377(7) . ? C28A C29A 1.388(6) . ? C29A C30A 1.458(6) . ? C30A N31A 1.366(5) . ? C30A C35A 1.381(6) . ? N31A C32A 1.347(5) . ? C32A C33A 1.381(6) . ? C33A C34A 1.377(8) . ? C34A C35A 1.379(7) . ? N36A N37A 1.353(4) . ? N36A C40A 1.355(5) . ? N37A C38A 1.339(5) . ? C38A C39A 1.384(6) . ? C39A C40A 1.389(5) . ? C40A C41A 1.468(5) . ? C41A N42A 1.358(5) . ? C41A C46A 1.395(5) . ? N42A C43A 1.338(5) . ? C43A C44A 1.366(6) . ? C44A C45A 1.379(6) . ? C45A C46A 1.384(6) . ? Cu1B N25B 1.964(3) . ? Cu1B N3B 1.969(3) . ? Cu1B N15B 1.992(3) . ? Cu1B N9B 2.100(3) . ? Cu1B N31B 2.222(3) . ? Cu1B Cu2B 3.8931(7) . ? Cu2B N36B 1.953(3) . ? Cu2B N14B 1.962(3) . ? Cu2B N4B 1.972(3) . ? Cu2B N20B 2.100(3) . ? Cu2B N42B 2.257(3) . ? N3B C7B 1.351(5) . ? N3B N4B 1.354(4) . ? N4B C5B 1.350(5) . ? C5B C6B 1.378(6) . ? C6B C7B 1.384(5) . ? C7B C8B 1.454(5) . ? C8B N9B 1.360(5) . ? C8B C13B 1.392(5) . ? N9B C10B 1.345(5) . ? C10B C11B 1.390(6) . ? C11B C12B 1.385(6) . ? C12B C13B 1.392(6) . ? N14B N15B 1.351(4) . ? N14B C18B 1.354(5) . ? N15B C16B 1.351(5) . ? C16B C17B 1.375(6) . ? C17B C18B 1.382(6) . ? C18B C19B 1.468(6) . ? C19B N20B 1.350(5) . ? C19B C24B 1.393(6) . ? N20B C21B 1.344(5) . ? C21B C22B 1.378(6) . ? C22B C23B 1.373(7) . ? C23B C24B 1.385(7) . ? N25B C29B 1.353(5) . ? N25B N26B 1.358(4) . ? N26B C27B 1.334(5) . ? C27B C28B 1.383(5) . ? C28B C29B 1.399(5) . ? C29B C30B 1.469(5) . ? C30B N31B 1.348(5) . ? C30B C35B 1.387(5) . ? N31B C32B 1.342(5) . ? C32B C33B 1.374(6) . ? C33B C34B 1.389(6) . ? C34B C35B 1.384(6) . ? N36B N37B 1.351(5) . ? N36B C40B 1.354(5) . ? N37B C38B 1.343(6) . ? C38B C39B 1.388(7) . ? C39B C40B 1.386(6) . ? C40B C41B 1.457(6) . ? C41B N42B 1.357(5) . ? C41B C46B 1.387(6) . ? N42B C43B 1.343(5) . ? C43B C44B 1.381(6) . ? C44B C45B 1.378(7) . ? C45B C46B 1.382(7) . ? C47 Cl50 1.746(5) . ? C47 Cl48 1.759(5) . ? C47 Cl49 1.765(5) . ? C51 Cl52 1.744(6) . ? C51 Cl54 1.749(6) . ? C51 Cl53 1.758(6) . ? C55 Cl57 1.712(7) . ? C55 Cl58 1.751(7) . ? C55 Cl56 1.761(7) . ? C59 Cl61 1.730(7) . ? C59 Cl60 1.749(6) . ? C59 Cl62 1.762(7) . ? O63 H63B 0.846(10) . ? O63 H63A 0.847(10) . ? 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 N25A Cu1A N3A 168.54(14) . . ? N25A Cu1A N15A 96.53(13) . . ? N3A Cu1A N15A 94.76(13) . . ? N25A Cu1A N9A 91.20(13) . . ? N3A Cu1A N9A 78.62(13) . . ? N15A Cu1A N9A 142.28(13) . . ? N25A Cu1A N31A 79.38(13) . . ? N3A Cu1A N31A 96.32(13) . . ? N15A Cu1A N31A 121.72(13) . . ? N9A Cu1A N31A 95.98(13) . . ? N36A Cu2A N14A 169.81(13) . . ? N36A Cu2A N4A 95.60(13) . . ? N14A Cu2A N4A 94.27(13) . . ? N36A Cu2A N20A 94.08(13) . . ? N14A Cu2A N20A 79.53(13) . . ? N4A Cu2A N20A 142.56(12) . . ? N36A Cu2A N42A 79.18(12) . . ? N14A Cu2A N42A 94.51(12) . . ? N4A Cu2A N42A 113.65(12) . . ? N20A Cu2A N42A 103.67(12) . . ? N4A N3A C7A 109.0(3) . . ? N4A N3A Cu1A 133.2(2) . . ? C7A N3A Cu1A 117.9(3) . . ? N3A N4A C5A 107.6(3) . . ? N3A N4A Cu2A 121.1(2) . . ? C5A N4A Cu2A 131.1(3) . . ? N4A C5A C6A 110.1(4) . . ? C7A C6A C5A 104.2(3) . . ? N3A C7A C6A 109.1(4) . . ? N3A C7A C8A 116.1(3) . . ? C6A C7A C8A 134.8(4) . . ? N9A C8A C13A 121.7(4) . . ? N9A C8A C7A 113.7(3) . . ? C13A C8A C7A 124.6(4) . . ? C10A N9A C8A 118.5(4) . . ? C10A N9A Cu1A 127.8(3) . . ? C8A N9A Cu1A 113.7(3) . . ? N9A C10A C11A 122.9(4) . . ? C10A C11A C12A 118.9(4) . . ? C11A C12A C13A 118.7(4) . . ? C8A C13A C12A 119.3(4) . . ? N15A N14A C18A 108.6(3) . . ? N15A N14A Cu2A 133.4(3) . . ? C18A N14A Cu2A 117.6(3) . . ? C16A N15A N14A 107.6(3) . . ? C16A N15A Cu1A 131.5(3) . . ? N14A N15A Cu1A 121.0(2) . . ? N15A C16A C17A 110.9(4) . . ? C16A C17A C18A 103.9(4) . . ? N14A C18A C17A 109.0(4) . . ? N14A C18A C19A 115.3(3) . . ? C17A C18A C19A 135.7(4) . . ? N20A C19A C24A 121.8(4) . . ? N20A C19A C18A 113.6(3) . . ? C24A C19A C18A 124.7(4) . . ? C21A N20A C19A 118.8(4) . . ? C21A N20A Cu2A 127.4(3) . . ? C19A N20A Cu2A 113.8(3) . . ? N20A C21A C22A 122.5(4) . . ? C23A C22A C21A 118.2(4) . . ? C22A C23A C24A 120.2(4) . . ? C23A C24A C19A 118.5(4) . . ? C29A N25A N26A 110.3(3) . . ? C29A N25A Cu1A 117.1(3) . . ? N26A N25A Cu1A 132.0(3) . . ? C27A N26A N25A 105.2(4) . . ? N26A C27A C28A 111.8(4) . . ? C27A C28A C29A 104.1(4) . . ? N25A C29A C28A 108.5(4) . . ? N25A C29A C30A 117.7(4) . . ? C28A C29A C30A 133.7(4) . . ? N31A C30A C35A 121.2(4) . . ? N31A C30A C29A 113.7(4) . . ? C35A C30A C29A 125.2(4) . . ? C32A N31A C30A 118.0(4) . . ? C32A N31A Cu1A 130.3(3) . . ? C30A N31A Cu1A 110.8(3) . . ? N31A C32A C33A 123.2(5) . . ? C34A C33A C32A 118.0(5) . . ? C33A C34A C35A 119.8(5) . . ? C34A C35A C30A 119.6(5) . . ? N37A N36A C40A 109.5(3) . . ? N37A N36A Cu2A 131.8(2) . . ? C40A N36A Cu2A 118.5(2) . . ? C38A N37A N36A 106.1(3) . . ? N37A C38A C39A 111.9(4) . . ? C38A C39A C40A 103.5(4) . . ? N36A C40A C39A 108.9(3) . . ? N36A C40A C41A 116.7(3) . . ? C39A C40A C41A 134.4(4) . . ? N42A C41A C46A 121.2(4) . . ? N42A C41A C40A 114.6(3) . . ? C46A C41A C40A 124.2(4) . . ? C43A N42A C41A 118.3(3) . . ? C43A N42A Cu2A 130.7(3) . . ? C41A N42A Cu2A 110.8(2) . . ? N42A C43A C44A 123.5(4) . . ? C43A C44A C45A 118.5(4) . . ? C44A C45A C46A 119.7(4) . . ? C45A C46A C41A 118.7(4) . . ? N25B Cu1B N3B 170.43(14) . . ? N25B Cu1B N15B 94.34(13) . . ? N3B Cu1B N15B 95.23(13) . . ? N25B Cu1B N9B 91.89(14) . . ? N3B Cu1B N9B 79.61(13) . . ? N15B Cu1B N9B 151.78(12) . . ? N25B Cu1B N31B 78.86(12) . . ? N3B Cu1B N31B 97.84(12) . . ? N15B Cu1B N31B 110.21(12) . . ? N9B Cu1B N31B 98.00(12) . . ? N36B Cu2B N14B 170.21(14) . . ? N36B Cu2B N4B 93.79(13) . . ? N14B Cu2B N4B 95.48(13) . . ? N36B Cu2B N20B 90.28(14) . . ? N14B Cu2B N20B 79.98(13) . . ? N4B Cu2B N20B 155.06(13) . . ? N36B Cu2B N42B 77.89(13) . . ? N14B Cu2B N42B 101.31(13) . . ? N4B Cu2B N42B 112.74(12) . . ? N20B Cu2B N42B 92.18(12) . . ? C7B N3B N4B 108.4(3) . . ? C7B N3B Cu1B 116.6(3) . . ? N4B N3B Cu1B 135.0(2) . . ? C5B N4B N3B 107.0(3) . . ? C5B N4B Cu2B 127.4(3) . . ? N3B N4B Cu2B 125.2(2) . . ? N4B C5B C6B 110.9(4) . . ? C5B C6B C7B 103.9(3) . . ? N3B C7B C6B 109.8(4) . . ? N3B C7B C8B 116.6(3) . . ? C6B C7B C8B 133.6(4) . . ? N9B C8B C13B 122.3(4) . . ? N9B C8B C7B 113.8(3) . . ? C13B C8B C7B 123.9(4) . . ? C10B N9B C8B 118.5(4) . . ? C10B N9B Cu1B 128.1(3) . . ? C8B N9B Cu1B 113.4(3) . . ? N9B C10B C11B 122.1(4) . . ? C12B C11B C10B 119.4(4) . . ? C11B C12B C13B 119.2(4) . . ? C12B C13B C8B 118.5(4) . . ? N15B N14B C18B 107.8(3) . . ? N15B N14B Cu2B 135.7(3) . . ? C18B N14B Cu2B 116.5(3) . . ? N14B N15B C16B 107.8(3) . . ? N14B N15B Cu1B 124.4(2) . . ? C16B N15B Cu1B 127.6(3) . . ? N15B C16B C17B 110.2(4) . . ? C16B C17B C18B 104.4(4) . . ? N14B C18B C17B 109.8(4) . . ? N14B C18B C19B 116.3(4) . . ? C17B C18B C19B 133.9(4) . . ? N20B C19B C24B 121.6(4) . . ? N20B C19B C18B 113.8(3) . . ? C24B C19B C18B 124.6(4) . . ? C21B N20B C19B 118.4(4) . . ? C21B N20B Cu2B 128.2(3) . . ? C19B N20B Cu2B 113.4(3) . . ? N20B C21B C22B 122.4(4) . . ? C23B C22B C21B 119.6(5) . . ? C22B C23B C24B 118.7(4) . . ? C23B C24B C19B 119.2(5) . . ? C29B N25B N26B 109.5(3) . . ? C29B N25B Cu1B 117.1(3) . . ? N26B N25B Cu1B 133.2(3) . . ? C27B N26B N25B 106.4(3) . . ? N26B C27B C28B 112.0(4) . . ? C27B C28B C29B 103.5(4) . . ? N25B C29B C28B 108.6(3) . . ? N25B C29B C30B 118.4(3) . . ? C28B C29B C30B 133.0(4) . . ? N31B C30B C35B 121.8(4) . . ? N31B C30B C29B 114.2(3) . . ? C35B C30B C29B 123.9(4) . . ? C32B N31B C30B 118.4(3) . . ? C32B N31B Cu1B 130.6(3) . . ? C30B N31B Cu1B 111.0(2) . . ? N31B C32B C33B 123.2(4) . . ? C32B C33B C34B 118.4(4) . . ? C35B C34B C33B 119.2(4) . . ? C34B C35B C30B 119.0(4) . . ? N37B N36B C40B 110.8(3) . . ? N37B N36B Cu2B 130.3(3) . . ? C40B N36B Cu2B 118.7(3) . . ? C38B N37B N36B 105.3(4) . . ? N37B C38B C39B 111.8(4) . . ? C40B C39B C38B 104.1(4) . . ? N36B C40B C39B 108.0(4) . . ? N36B C40B C41B 117.9(4) . . ? C39B C40B C41B 134.1(4) . . ? N42B C41B C46B 121.7(4) . . ? N42B C41B C40B 114.5(4) . . ? C46B C41B C40B 123.8(4) . . ? C43B N42B C41B 118.2(4) . . ? C43B N42B Cu2B 130.5(3) . . ? C41B N42B Cu2B 110.1(3) . . ? N42B C43B C44B 122.8(5) . . ? C45B C44B C43B 118.8(4) . . ? C44B C45B C46B 119.3(4) . . ? C45B C46B C41B 119.2(5) . . ? Cl50 C47 Cl48 110.0(3) . . ? Cl50 C47 Cl49 111.0(3) . . ? Cl48 C47 Cl49 110.5(3) . . ? Cl52 C51 Cl54 112.2(3) . . ? Cl52 C51 Cl53 110.3(3) . . ? Cl54 C51 Cl53 110.2(3) . . ? Cl57 C55 Cl58 112.6(4) . . ? Cl57 C55 Cl56 112.1(4) . . ? Cl58 C55 Cl56 109.7(4) . . ? Cl61 C59 Cl60 112.3(4) . . ? Cl61 C59 Cl62 109.6(4) . . ? Cl60 C59 Cl62 108.2(3) . . ? H63A O63 H63B 109.9(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C47 H47 O63 1.00 2.21 3.159(6) 158.8 . C59 H59 N37B 1.00 2.20 3.182(7) 166.7 . O63 H63B N37A 0.846(10) 1.996(13) 2.823(4) 166(4) . O63 H63A N26B 0.847(10) 2.03(2) 2.824(4) 155(5) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.015 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.108 #=END data_c:\datasets\leeds\newsmc~1\smcufph _database_code_depnum_ccdc_archive 'CCDC 632225' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Octakis[3{5}-phenylpyrazolido]tetracopper(II) hemi-pentane solvate ; _chemical_name_common ;Octakis(3(5)-phenylpyrazolido)tetracopper(ii) hemi-pentane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C72 H56 Cu4 N16, 0.5[C5 H12]' _chemical_formula_sum 'C74.50 H62 Cu4 N16' _chemical_formula_weight 1435.56 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.978(4) _cell_length_b 17.233(3) _cell_length_c 22.798(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.117(8) _cell_angle_gamma 90.00 _cell_volume 6805(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 166799 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.31 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2948 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.429 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 2.5 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 166799 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 29.31 _reflns_number_total 18446 _reflns_number_gt 12313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _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 asymmetric unit contains one complex molecule lying on a general position, and a disordered region of solvent about the crystallographic inversion centre 1-x, 1-y, -z. Two of the phenylpyrazolido ligands in the model are disordered, each over three equally occupied orientations labelled 'A', 'B' and 'C'. These are N5-C15 and N82-C92. In addition, the phenyl group C76-C81, attached to a third phenylpyrazolido ligand, is also disordered over two sites: C76A-C81A (refined occupancy 0.55) and C76B-C81B (0.45). The following restraints were applied to these disordered groups: phenyl C-C = 1.39(2)\%A phenyl 1,3-C...C = 2.41(1)\%A C{pyrazole}-C{phenyl} = 1.46(1)\%A pyrazole N-N = 1.34(1)\%A pyrazole C-N = 1.34(1)\%A pyrazole C=N = 1.35(1)\%A pyrazole C-C = 1.37(1)\%A pyrazole C=C = 1.39(1)\%A. Although the geometries and thermal parameters on the three disordered residues in this structure are sensible, the short intramolecular contacts H81B...H88A (2.0\%A) and H81B...H88C (1.6\%A) imply that these disorder sites cannot be simultaneously occupied in the same molecule. Although these are from calculated, ratehr than actual, H atom positions it is clear that sites N82C-C92C (occupancy 0.33), and possibly H81A...H88A, cannot coexist with C76B-C81B in the same molecule. The relative occupancies of these groups do not quite agree with this model. So, either the actual positions of H81B and H88A are in fact far enough apart to permit them both to be occupied at once, or the model does not perfectly reflect the actual relative occupancies of each disorder site. Two partial pentane solvent orientations were refined. C73A-C77A, occupancy 0.25 (ie C76A corresponds to a CH2 group here, with H atoms H67A and H67B). C76A, C74B-C77B, occupancy 0.25 (ie C76A corresponds to a CH3 group here, with H atoms H67C-H67E). So, C76A has total occupancy 0.50, leaving a total solvent content of 0.5 molecules of pentane per asymmetric unit. The C-C bonds in the disordered solvent were restrained to 1.54(1)\%A, and 1,3-C...C distances to 2.51(1)\%A. All non-H atoms with occupancies >0.50 were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0555P)^2^+5.1252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18445 _refine_ls_number_parameters 953 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.265518(19) 0.205522(18) 0.099850(15) 0.03094(8) Uani 1 1 d . . . Cu2 Cu 0.381256(18) 0.058327(18) 0.165465(14) 0.02895(8) Uani 1 1 d . A . Cu3 Cu 0.291881(18) -0.046958(18) 0.036050(14) 0.02943(8) Uani 1 1 d . . . Cu4 Cu 0.194016(19) 0.106664(19) -0.037841(15) 0.03230(8) Uani 1 1 d . A . N5A N 0.3067(18) 0.1955(7) 0.1912(9) 0.030(4) Uiso 0.33 1 d PD A 1 N6A N 0.3531(17) 0.1351(9) 0.2216(5) 0.027(5) Uiso 0.33 1 d PD A 1 C7A C 0.3748(6) 0.1418(6) 0.2863(4) 0.020(3) Uiso 0.33 1 d PD A 1 C8A C 0.3362(6) 0.2058(7) 0.2971(5) 0.023(3) Uiso 0.33 1 d PD A 1 H8A H 0.3395 0.2251 0.3372 0.028 Uiso 0.33 1 calc PR A 1 C9A C 0.2926(7) 0.2347(8) 0.2368(5) 0.021(3) Uiso 0.33 1 d PD A 1 H9A H 0.2572 0.2765 0.2283 0.025 Uiso 0.33 1 calc PR A 1 C10A C 0.4333(6) 0.0885(6) 0.3344(4) 0.031(3) Uiso 0.33 1 d PD A 1 C11A C 0.4559(9) 0.0165(8) 0.3178(5) 0.036(5) Uiso 0.33 1 d PD A 1 H11A H 0.4332 0.0001 0.2742 0.043 Uiso 0.33 1 calc PR A 1 C12A C 0.5093(7) -0.0303(6) 0.3621(5) 0.043(4) Uiso 0.33 1 d PD A 1 H12A H 0.5196 -0.0797 0.3490 0.051 Uiso 0.33 1 calc PR A 1 C13A C 0.5499(6) -0.0075(6) 0.4274(5) 0.046(3) Uiso 0.33 1 d PD A 1 H13A H 0.5908 -0.0378 0.4571 0.055 Uiso 0.33 1 calc PR A 1 C14A C 0.5265(6) 0.0608(5) 0.4448(4) 0.047(2) Uiso 0.33 1 d PD A 1 H14A H 0.5487 0.0762 0.4887 0.056 Uiso 0.33 1 calc PR A 1 C15A C 0.4719(5) 0.1071(5) 0.4004(4) 0.038(2) Uiso 0.33 1 d PD A 1 H15A H 0.4592 0.1547 0.4149 0.045 Uiso 0.33 1 calc PR A 1 N5B N 0.3138(11) 0.1860(15) 0.1985(6) 0.032(4) Uiso 0.33 1 d PD A 2 N6B N 0.3657(6) 0.1277(10) 0.2232(5) 0.025(3) Uiso 0.33 1 d PD A 2 C7B C 0.3854(9) 0.1296(9) 0.2874(5) 0.020(5) Uiso 0.33 1 d PD A 2 C8B C 0.3450(7) 0.1872(6) 0.3037(4) 0.022(2) Uiso 0.33 1 d PD A 2 H8B H 0.3482 0.1999 0.3452 0.026 Uiso 0.33 1 calc PR A 2 C9B C 0.2991(8) 0.2214(6) 0.2458(5) 0.022(3) Uiso 0.33 1 d PD A 2 H9B H 0.2636 0.2626 0.2400 0.026 Uiso 0.33 1 calc PR A 2 C10B C 0.4371(7) 0.0704(7) 0.3286(5) 0.040(4) Uiso 0.33 1 d PD A 2 C11B C 0.4855(6) 0.0324(6) 0.3097(4) 0.048(2) Uiso 0.33 1 d PD A 2 H11B H 0.4836 0.0428 0.2682 0.057 Uiso 0.33 1 calc PR A 2 C12B C 0.5395(7) -0.0225(7) 0.3488(5) 0.064(4) Uiso 0.33 1 d PD A 2 H12B H 0.5754 -0.0467 0.3355 0.076 Uiso 0.33 1 calc PR A 2 C13B C 0.5376(7) -0.0394(7) 0.4073(6) 0.074(4) Uiso 0.33 1 d PD A 2 H13B H 0.5758 -0.0727 0.4365 0.088 Uiso 0.33 1 calc PR A 2 C14B C 0.4813(7) -0.0087(7) 0.4238(5) 0.080(4) Uiso 0.33 1 d PD A 2 H14B H 0.4771 -0.0266 0.4616 0.096 Uiso 0.33 1 calc PR A 2 C15B C 0.4295(7) 0.0488(7) 0.3857(5) 0.081(4) Uiso 0.33 1 d PD A 2 H15B H 0.3918 0.0716 0.3978 0.098 Uiso 0.33 1 calc PR A 2 N5C N 0.3002(10) 0.1848(12) 0.1927(9) 0.022(3) Uiso 0.33 1 d PD A 3 N6C N 0.3525(16) 0.1274(12) 0.2203(7) 0.027(6) Uiso 0.33 1 d PD A 3 C7C C 0.3836(16) 0.1337(14) 0.2853(7) 0.050(10) Uiso 0.33 1 d PD A 3 C8C C 0.3532(8) 0.2011(10) 0.2997(7) 0.039(4) Uiso 0.33 1 d PD A 3 H8C H 0.3623 0.2207 0.3411 0.047 Uiso 0.33 1 calc PR A 3 C9C C 0.3070(9) 0.2333(11) 0.2412(7) 0.049(6) Uiso 0.33 1 d PD A 3 H9C H 0.2833 0.2829 0.2357 0.058 Uiso 0.33 1 calc PR A 3 C10C C 0.4455(7) 0.0842(7) 0.3305(4) 0.027(3) Uiso 0.33 1 d PD A 3 C11C C 0.4608(9) 0.0098(7) 0.3151(5) 0.032(5) Uiso 0.33 1 d PD A 3 H11C H 0.4295 -0.0119 0.2745 0.038 Uiso 0.33 1 calc PR A 3 C12C C 0.5220(8) -0.0332(6) 0.3591(5) 0.034(3) Uiso 0.33 1 d PD A 3 H12C H 0.5332 -0.0831 0.3474 0.040 Uiso 0.33 1 calc PR A 3 C13C C 0.5662(6) -0.0042(5) 0.4192(4) 0.039(3) Uiso 0.33 1 d PD A 3 H13C H 0.6060 -0.0346 0.4498 0.047 Uiso 0.33 1 calc PR A 3 C14C C 0.5515(6) 0.0712(5) 0.4345(4) 0.050(2) Uiso 0.33 1 d PD A 3 H14C H 0.5822 0.0923 0.4756 0.060 Uiso 0.33 1 calc PR A 3 C15C C 0.4926(5) 0.1152(5) 0.3904(4) 0.037(2) Uiso 0.33 1 d PD A 3 H15C H 0.4842 0.1667 0.4009 0.045 Uiso 0.33 1 calc PR A 3 N16 N 0.36952(13) 0.19800(13) 0.09856(10) 0.0339(5) Uani 1 1 d . A . N17 N 0.42498(13) 0.14685(13) 0.13627(10) 0.0321(5) Uani 1 1 d . . . C18 C 0.49193(16) 0.16364(16) 0.13108(13) 0.0342(6) Uani 1 1 d . A . C19 C 0.47977(18) 0.22569(17) 0.08905(15) 0.0431(7) Uani 1 1 d . . . H19 H 0.5164 0.2496 0.0763 0.052 Uiso 1 1 calc R A . C20 C 0.40287(18) 0.24507(17) 0.06991(14) 0.0420(7) Uani 1 1 d . A . H20 H 0.3772 0.2857 0.0408 0.050 Uiso 1 1 calc R . . C21 C 0.56307(16) 0.11993(16) 0.16724(14) 0.0365(6) Uani 1 1 d . . . C22 C 0.60676(17) 0.09085(18) 0.13529(16) 0.0446(7) Uani 1 1 d . A . H22 H 0.5901 0.0997 0.0905 0.054 Uiso 1 1 calc R . . C23 C 0.67417(19) 0.0493(2) 0.16844(19) 0.0575(9) Uani 1 1 d . . . H23 H 0.7035 0.0300 0.1464 0.069 Uiso 1 1 calc R A . C24 C 0.6983(2) 0.0360(2) 0.2332(2) 0.0646(11) Uani 1 1 d . A . H24 H 0.7440 0.0070 0.2558 0.077 Uiso 1 1 calc R . . C25 C 0.6560(2) 0.0651(2) 0.26585(18) 0.0629(10) Uani 1 1 d . . . H25 H 0.6729 0.0560 0.3106 0.075 Uiso 1 1 calc R A . C26 C 0.58874(19) 0.1077(2) 0.23280(15) 0.0500(8) Uani 1 1 d . A . H26 H 0.5605 0.1284 0.2553 0.060 Uiso 1 1 calc R . . N27 N 0.28980(12) -0.00692(12) 0.15387(10) 0.0303(5) Uani 1 1 d . . . N28 N 0.25961(12) -0.06281(12) 0.10720(10) 0.0290(4) Uani 1 1 d . A . C29 C 0.20463(14) -0.10172(15) 0.11823(12) 0.0301(5) Uani 1 1 d . . . C30 C 0.19852(16) -0.07106(17) 0.17253(13) 0.0356(6) Uani 1 1 d . A . H30 H 0.1646 -0.0872 0.1913 0.043 Uiso 1 1 calc R . . C31 C 0.25241(15) -0.01217(16) 0.19311(12) 0.0344(6) Uani 1 1 d . A . H31 H 0.2619 0.0199 0.2294 0.041 Uiso 1 1 calc R . . C32 C 0.16103(15) -0.16581(16) 0.07633(12) 0.0331(6) Uani 1 1 d . A . C33 C 0.08087(16) -0.16773(18) 0.05410(14) 0.0423(7) Uani 1 1 d . . . H33 H 0.0550 -0.1277 0.0661 0.051 Uiso 1 1 calc R A . C34 C 0.0386(2) -0.2273(2) 0.01472(17) 0.0574(9) Uani 1 1 d . A . H34 H -0.0160 -0.2279 -0.0003 0.069 Uiso 1 1 calc R . . C35 C 0.0757(2) -0.2856(2) -0.00277(18) 0.0642(10) Uani 1 1 d . . . H35 H 0.0465 -0.3261 -0.0302 0.077 Uiso 1 1 calc R A . C36 C 0.1554(2) -0.28548(19) 0.01953(17) 0.0559(9) Uani 1 1 d . A . H36 H 0.1808 -0.3262 0.0077 0.067 Uiso 1 1 calc R . . C37 C 0.19872(18) -0.22559(17) 0.05947(14) 0.0423(7) Uani 1 1 d . . . H37 H 0.2534 -0.2256 0.0750 0.051 Uiso 1 1 calc R A . N38 N 0.43558(13) -0.02984(13) 0.14590(10) 0.0341(5) Uani 1 1 d . . . N39 N 0.39643(13) -0.07777(13) 0.09556(10) 0.0310(5) Uani 1 1 d . A . C40 C 0.43629(16) -0.14484(16) 0.10347(13) 0.0342(6) Uani 1 1 d . . . C41 C 0.50306(17) -0.13958(18) 0.16049(14) 0.0419(7) Uani 1 1 d . A . H41 H 0.5421 -0.1778 0.1786 0.050 Uiso 1 1 calc R . . C42 C 0.50012(17) -0.06714(18) 0.18479(14) 0.0410(7) Uani 1 1 d . A . H42 H 0.5381 -0.0465 0.2234 0.049 Uiso 1 1 calc R . . C43 C 0.40761(18) -0.20903(16) 0.05754(15) 0.0407(7) Uani 1 1 d . A . C44 C 0.35796(19) -0.19702(19) -0.00675(15) 0.0466(7) Uani 1 1 d . . . H44 H 0.3435 -0.1455 -0.0217 0.056 Uiso 1 1 calc R A . C45 C 0.3292(2) -0.2585(2) -0.0494(2) 0.0678(10) Uani 1 1 d . A . H45 H 0.2944 -0.2490 -0.0927 0.081 Uiso 1 1 calc R . . C46 C 0.3514(3) -0.3331(3) -0.0285(3) 0.0904(15) Uani 1 1 d . . . H46 H 0.3327 -0.3756 -0.0572 0.108 Uiso 1 1 calc R A . C47 C 0.4008(3) -0.3453(2) 0.0345(3) 0.0938(16) Uani 1 1 d . A . H47 H 0.4163 -0.3969 0.0487 0.113 Uiso 1 1 calc R . . C48 C 0.4291(3) -0.2848(2) 0.0782(2) 0.0663(10) Uani 1 1 d . . . H48 H 0.4627 -0.2951 0.1216 0.080 Uiso 1 1 calc R A . N49 N 0.19259(13) -0.05916(14) -0.03998(10) 0.0349(5) Uani 1 1 d . A . N50 N 0.15325(13) 0.00454(13) -0.07220(10) 0.0342(5) Uani 1 1 d . . . C51 C 0.09700(16) -0.01835(18) -0.12906(13) 0.0400(7) Uani 1 1 d . A . C52 C 0.09938(19) -0.09880(19) -0.13304(15) 0.0489(8) Uani 1 1 d . . . H52 H 0.0667 -0.1311 -0.1671 0.059 Uiso 1 1 calc R A . C53 C 0.15955(18) -0.12144(18) -0.07674(14) 0.0436(7) Uani 1 1 d . A . H53 H 0.1755 -0.1736 -0.0655 0.052 Uiso 1 1 calc R . . C54 C 0.04758(19) 0.0390(2) -0.17529(14) 0.0482(8) Uani 1 1 d . . . C55 C 0.03219(18) 0.1110(2) -0.15610(16) 0.0510(8) Uani 1 1 d . A . H55 H 0.0512 0.1228 -0.1116 0.061 Uiso 1 1 calc R . . C56 C -0.0105(2) 0.1660(2) -0.20084(19) 0.0669(11) Uani 1 1 d . . . H56 H -0.0183 0.2159 -0.1867 0.080 Uiso 1 1 calc R A . C57 C -0.0416(3) 0.1492(3) -0.2650(2) 0.0993(18) Uani 1 1 d . A . H57 H -0.0703 0.1874 -0.2955 0.119 Uiso 1 1 calc R . . C58 C -0.0311(4) 0.0769(4) -0.2851(2) 0.135(3) Uani 1 1 d . . . H58 H -0.0550 0.0640 -0.3294 0.162 Uiso 1 1 calc R A . C59 C 0.0146(3) 0.0221(3) -0.24072(18) 0.1000(19) Uani 1 1 d . A . H59 H 0.0232 -0.0272 -0.2553 0.120 Uiso 1 1 calc R . . N60 N 0.33383(13) 0.03235(13) -0.00482(10) 0.0318(5) Uani 1 1 d . A . N61 N 0.28724(13) 0.08058(13) -0.05268(10) 0.0333(5) Uani 1 1 d . . . C62 C 0.33114(17) 0.11604(16) -0.07897(14) 0.0372(6) Uani 1 1 d . A . C63 C 0.40733(18) 0.09181(17) -0.04711(14) 0.0406(7) Uani 1 1 d . . . H63 H 0.4506 0.1076 -0.0551 0.049 Uiso 1 1 calc R A . C64 C 0.40645(16) 0.03960(16) -0.00119(13) 0.0348(6) Uani 1 1 d . A . H64 H 0.4503 0.0129 0.0284 0.042 Uiso 1 1 calc R . . C65 C 0.2951(2) 0.16360(19) -0.13763(17) 0.0519(9) Uani 1 1 d . . . C66 C 0.3350(3) 0.2272(2) -0.1474(2) 0.0818(15) Uani 1 1 d . A . H66 H 0.3839 0.2421 -0.1158 0.098 Uiso 1 1 calc R . . C67 C 0.3003(4) 0.2685(3) -0.2057(3) 0.117(3) Uani 1 1 d . . . H67 H 0.3268 0.3113 -0.2136 0.141 Uiso 1 1 calc R A . C68 C 0.2291(5) 0.2481(4) -0.2513(3) 0.118(3) Uani 1 1 d . A . H68 H 0.2066 0.2770 -0.2900 0.141 Uiso 1 1 calc R . . C69 C 0.1908(3) 0.1870(3) -0.24115(19) 0.0890(17) Uani 1 1 d . . . H69 H 0.1415 0.1733 -0.2729 0.107 Uiso 1 1 calc R A . C70 C 0.2230(2) 0.1436(2) -0.18459(16) 0.0617(10) Uani 1 1 d . A . H70 H 0.1958 0.1004 -0.1782 0.074 Uiso 1 1 calc R . . N71 N 0.14859(13) 0.10252(13) 0.02749(10) 0.0330(5) Uani 1 1 d . . . N72 N 0.16305(12) 0.15579(13) 0.07631(10) 0.0321(5) Uani 1 1 d . A . C73 C 0.11786(15) 0.13721(17) 0.10764(12) 0.0341(6) Uani 1 1 d D . . C74 C 0.07464(16) 0.07169(18) 0.07955(13) 0.0378(6) Uani 1 1 d . A . H74 H 0.0385 0.0459 0.0918 0.045 Uiso 1 1 calc R . . C75 C 0.09559(15) 0.05189(17) 0.02985(13) 0.0351(6) Uani 1 1 d . A . H75 H 0.0756 0.0090 0.0017 0.042 Uiso 1 1 calc R . . C76A C 0.1143(5) 0.1766(5) 0.1633(3) 0.0319(16) Uani 0.55 1 d PD A 1 C77A C 0.1212(4) 0.1373(4) 0.2194(3) 0.0405(14) Uani 0.55 1 d PD A 1 H77A H 0.1264 0.0825 0.2220 0.049 Uiso 0.55 1 calc PR A 1 C78A C 0.1202(4) 0.1797(4) 0.2712(3) 0.0529(17) Uani 0.55 1 d PD A 1 H78A H 0.1238 0.1533 0.3089 0.063 Uiso 0.55 1 calc PR A 1 C79A C 0.1141(4) 0.2600(4) 0.2681(3) 0.0484(15) Uani 0.55 1 d PD A 1 H79A H 0.1168 0.2884 0.3047 0.058 Uiso 0.55 1 calc PR A 1 C80A C 0.1043(3) 0.2993(3) 0.2123(3) 0.0453(14) Uani 0.55 1 d PD A 1 H80A H 0.0976 0.3541 0.2095 0.054 Uiso 0.55 1 calc PR A 1 C81A C 0.1043(3) 0.2566(3) 0.1600(2) 0.0363(12) Uani 0.55 1 d PD A 1 H81A H 0.0973 0.2829 0.1214 0.044 Uiso 0.55 1 calc PR A 1 C76B C 0.1188(9) 0.1950(5) 0.1571(5) 0.035(3) Uiso 0.45 1 d PD A 2 C77B C 0.1144(6) 0.1657(4) 0.2125(4) 0.041(2) Uiso 0.45 1 d PD A 2 H77B H 0.1109 0.1113 0.2173 0.049 Uiso 0.45 1 calc PR A 2 C78B C 0.1151(6) 0.2160(5) 0.2618(4) 0.052(3) Uiso 0.45 1 d PD A 2 H78B H 0.1118 0.1956 0.2993 0.062 Uiso 0.45 1 calc PR A 2 C79B C 0.1205(6) 0.2948(5) 0.2546(4) 0.051(2) Uiso 0.45 1 d PD A 2 H79B H 0.1223 0.3290 0.2879 0.062 Uiso 0.45 1 calc PR A 2 C80B C 0.1235(6) 0.3244(4) 0.1992(4) 0.061(3) Uiso 0.45 1 d PD A 2 H80B H 0.1273 0.3789 0.1947 0.073 Uiso 0.45 1 calc PR A 2 C81B C 0.1210(5) 0.2758(4) 0.1503(4) 0.043(2) Uiso 0.45 1 d PD A 2 H81B H 0.1208 0.2971 0.1118 0.052 Uiso 0.45 1 calc PR A 2 N82A N 0.2013(16) 0.2242(10) -0.0398(7) 0.038(8) Uiso 0.33 1 d PD A 1 N83A N 0.2288(15) 0.2657(6) 0.0155(9) 0.030(5) Uiso 0.33 1 d PD A 1 C84A C 0.2348(7) 0.3421(5) 0.0055(4) 0.029(3) Uiso 0.33 1 d PD A 1 C85A C 0.2142(6) 0.3503(5) -0.0598(4) 0.033(2) Uiso 0.33 1 d PD A 1 H85A H 0.2119 0.3970 -0.0827 0.040 Uiso 0.33 1 calc PR A 1 C86A C 0.1979(6) 0.2772(5) -0.0843(5) 0.035(3) Uiso 0.33 1 d PD A 1 H86A H 0.1856 0.2649 -0.1280 0.042 Uiso 0.33 1 calc PR A 1 C87A C 0.2520(7) 0.4033(5) 0.0536(4) 0.035(3) Uiso 0.33 1 d PD A 1 C88A C 0.2387(6) 0.3902(4) 0.1087(4) 0.035(2) Uiso 0.33 1 d PD A 1 H88A H 0.2217 0.3406 0.1160 0.042 Uiso 0.33 1 calc PR A 1 C89A C 0.2503(6) 0.4498(5) 0.1531(4) 0.038(2) Uiso 0.33 1 d PD A 1 H89A H 0.2416 0.4408 0.1906 0.046 Uiso 0.33 1 calc PR A 1 C90A C 0.2747(6) 0.5221(4) 0.1423(4) 0.039(2) Uiso 0.33 1 d PD A 1 H90A H 0.2807 0.5635 0.1716 0.047 Uiso 0.33 1 calc PR A 1 C91A C 0.2903(7) 0.5336(5) 0.0878(5) 0.055(3) Uiso 0.33 1 d PD A 1 H91A H 0.3083 0.5826 0.0807 0.066 Uiso 0.33 1 calc PR A 1 C92A C 0.2793(6) 0.4738(5) 0.0446(4) 0.041(3) Uiso 0.33 1 d PD A 1 H92A H 0.2909 0.4817 0.0082 0.049 Uiso 0.33 1 calc PR A 1 N82B N 0.1921(8) 0.2126(6) -0.0403(4) 0.022(3) Uiso 0.33 1 d PD A 2 N83B N 0.2148(6) 0.2568(5) 0.0136(6) 0.022(2) Uiso 0.33 1 d PD A 2 C84B C 0.2045(9) 0.3335(6) 0.0032(5) 0.032(5) Uiso 0.33 1 d PD A 2 C85B C 0.1622(7) 0.3377(6) -0.0633(5) 0.052(3) Uiso 0.33 1 d PD A 2 H85B H 0.1380 0.3827 -0.0871 0.062 Uiso 0.33 1 calc PR A 2 C86B C 0.1620(8) 0.2652(6) -0.0877(6) 0.040(4) Uiso 0.33 1 d PD A 2 H86B H 0.1432 0.2535 -0.1322 0.048 Uiso 0.33 1 calc PR A 2 C87B C 0.2188(7) 0.3936(6) 0.0526(5) 0.039(4) Uiso 0.33 1 d PD A 2 C88B C 0.1595(5) 0.4482(6) 0.0453(5) 0.064(3) Uiso 0.33 1 d PD A 2 H88B H 0.1104 0.4438 0.0103 0.076 Uiso 0.33 1 calc PR A 2 C89B C 0.1735(6) 0.5079(6) 0.0895(5) 0.070(3) Uiso 0.33 1 d PD A 2 H89B H 0.1347 0.5457 0.0832 0.084 Uiso 0.33 1 calc PR A 2 C90B C 0.2436(7) 0.5131(7) 0.1428(6) 0.044(4) Uiso 0.33 1 d PD A 2 H90B H 0.2532 0.5551 0.1720 0.052 Uiso 0.33 1 calc PR A 2 C91B C 0.2991(6) 0.4567(6) 0.1529(5) 0.067(3) Uiso 0.33 1 d PD A 2 H91B H 0.3459 0.4580 0.1905 0.080 Uiso 0.33 1 calc PR A 2 C92B C 0.2862(5) 0.3978(5) 0.1076(5) 0.057(3) Uiso 0.33 1 d PD A 2 H92B H 0.3249 0.3596 0.1148 0.068 Uiso 0.33 1 calc PR A 2 N82C N 0.2105(11) 0.2233(8) -0.0345(6) 0.025(4) Uiso 0.33 1 d P A 3 N83C N 0.2318(13) 0.2635(8) 0.0231(7) 0.027(4) Uiso 0.33 1 d P A 3 C84C C 0.2137(12) 0.3360(8) -0.0009(7) 0.036(6) Uiso 0.33 1 d P A 3 C85C C 0.1863(7) 0.3426(5) -0.0682(4) 0.0230(18) Uiso 0.33 1 d P A 3 H85C H 0.1764 0.3887 -0.0932 0.028 Uiso 0.33 1 calc PR A 3 C86C C 0.1772(10) 0.2670(7) -0.0894(6) 0.027(3) Uiso 0.33 1 d P A 3 H86C H 0.1532 0.2490 -0.1325 0.032 Uiso 0.33 1 calc PR A 3 C87C C 0.2314(9) 0.3981(5) 0.0502(5) 0.028(4) Uiso 0.33 1 d PD A 3 C88C C 0.2113(5) 0.3867(4) 0.1016(4) 0.029(2) Uiso 0.33 1 d PD A 3 H88C H 0.1922 0.3377 0.1076 0.035 Uiso 0.33 1 calc PR A 3 C89C C 0.2192(6) 0.4475(5) 0.1448(4) 0.037(2) Uiso 0.33 1 d PD A 3 H89C H 0.2084 0.4392 0.1815 0.045 Uiso 0.33 1 calc PR A 3 C90C C 0.2429(10) 0.5200(6) 0.1332(6) 0.057(6) Uiso 0.33 1 d PD A 3 H90C H 0.2440 0.5626 0.1600 0.068 Uiso 0.33 1 calc PR A 3 C91C C 0.2650(6) 0.5306(4) 0.0830(4) 0.037(2) Uiso 0.33 1 d PD A 3 H91C H 0.2868 0.5787 0.0784 0.044 Uiso 0.33 1 calc PR A 3 C92C C 0.2552(6) 0.4704(5) 0.0388(4) 0.032(2) Uiso 0.33 1 d PD A 3 H92C H 0.2649 0.4791 0.0016 0.038 Uiso 0.33 1 calc PR A 3 C93A C 0.6058(18) 0.529(2) 0.1262(7) 0.142(11) Uiso 0.25 1 d PD B 1 H93A H 0.6456 0.5395 0.1692 0.213 Uiso 0.25 1 calc PR B 1 H93B H 0.6051 0.4731 0.1172 0.213 Uiso 0.25 1 calc PR B 1 H93C H 0.5553 0.5445 0.1243 0.213 Uiso 0.25 1 calc PR B 1 C94A C 0.6235(13) 0.5744(17) 0.0762(8) 0.142(11) Uiso 0.25 1 d PD B 1 H94A H 0.6257 0.6306 0.0859 0.171 Uiso 0.25 1 calc PR B 1 H94B H 0.6744 0.5584 0.0778 0.171 Uiso 0.25 1 calc PR B 1 C95A C 0.5619(7) 0.5592(8) 0.0104(4) 0.061(4) Uiso 0.25 1 d PD B 1 H95A H 0.5350 0.6088 -0.0069 0.073 Uiso 0.25 1 calc PR B 1 H95B H 0.5873 0.5427 -0.0178 0.073 Uiso 0.25 1 calc PR B 1 C96A C 0.5025(7) 0.4999(8) 0.0057(4) 0.137(4) Uiso 0.50 1 d PRD . . H96A H 0.5303 0.4525 0.0276 0.164 Uiso 0.25 1 d PR B 1 H96B H 0.4742 0.5194 0.0308 0.164 Uiso 0.25 1 d PR B 1 H96C H 0.4647 0.4651 -0.0255 0.205 Uiso 0.25 1 d PR B 2 H96D H 0.5474 0.5055 -0.0049 0.205 Uiso 0.25 1 d PR B 2 H96E H 0.4789 0.5508 0.0042 0.205 Uiso 0.25 1 d PR B 2 C97A C 0.4448(10) 0.4775(12) -0.0599(7) 0.104(7) Uiso 0.25 1 d PD B 1 H97A H 0.4098 0.4380 -0.0560 0.156 Uiso 0.25 1 calc PR B 1 H97B H 0.4719 0.4564 -0.0849 0.156 Uiso 0.25 1 calc PR B 1 H97C H 0.4150 0.5233 -0.0817 0.156 Uiso 0.25 1 calc PR B 1 C94B C 0.5271(8) 0.4649(7) 0.0716(5) 0.063(4) Uiso 0.25 1 d PD B 2 H94C H 0.4802 0.4584 0.0799 0.076 Uiso 0.25 1 calc PR B 2 H94D H 0.5472 0.4122 0.0701 0.076 Uiso 0.25 1 calc PR B 2 C95B C 0.5834(9) 0.5041(10) 0.1257(4) 0.079(5) Uiso 0.25 1 d PD B 2 H95C H 0.6174 0.4635 0.1538 0.095 Uiso 0.25 1 calc PR B 2 H95D H 0.5552 0.5272 0.1496 0.095 Uiso 0.25 1 calc PR B 2 C96B C 0.6349(7) 0.5656(7) 0.1202(5) 0.052(3) Uiso 0.25 1 d PD B 2 H96F H 0.6888 0.5466 0.1401 0.062 Uiso 0.25 1 calc PR B 2 H96G H 0.6313 0.6114 0.1450 0.062 Uiso 0.25 1 calc PR B 2 C97B C 0.6173(9) 0.5910(9) 0.0518(6) 0.063(4) Uiso 0.25 1 d PD B 2 H97D H 0.6523 0.6331 0.0525 0.094 Uiso 0.25 1 calc PR B 2 H97E H 0.5638 0.6093 0.0313 0.094 Uiso 0.25 1 calc PR B 2 H97F H 0.6243 0.5470 0.0275 0.094 Uiso 0.25 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03635(18) 0.03031(17) 0.02772(16) 0.00127(12) 0.01468(13) 0.00329(13) Cu2 0.03275(17) 0.02759(16) 0.02740(15) 0.00024(12) 0.01320(13) -0.00124(13) Cu3 0.03327(17) 0.03148(17) 0.02457(15) 0.00118(12) 0.01286(13) 0.00062(13) Cu4 0.03806(18) 0.03402(18) 0.02846(16) -0.00071(13) 0.01731(14) 0.00682(14) N16 0.0372(12) 0.0331(12) 0.0317(11) 0.0051(9) 0.0144(10) 0.0001(10) N17 0.0338(12) 0.0308(12) 0.0327(11) 0.0008(9) 0.0147(9) -0.0005(9) C18 0.0363(14) 0.0334(14) 0.0352(14) -0.0049(11) 0.0168(12) -0.0064(11) C19 0.0442(17) 0.0401(16) 0.0516(17) 0.0048(13) 0.0262(14) -0.0066(13) C20 0.0487(17) 0.0377(16) 0.0420(16) 0.0100(13) 0.0208(14) -0.0020(13) C21 0.0347(14) 0.0317(14) 0.0425(15) -0.0075(12) 0.0151(12) -0.0077(11) C22 0.0400(16) 0.0442(17) 0.0503(18) -0.0134(14) 0.0193(14) -0.0069(13) C23 0.0443(18) 0.051(2) 0.074(2) -0.0260(18) 0.0210(17) -0.0026(16) C24 0.0442(19) 0.051(2) 0.080(3) -0.0168(19) 0.0066(18) 0.0083(16) C25 0.058(2) 0.066(2) 0.0474(19) -0.0035(17) 0.0043(17) 0.0072(18) C26 0.0467(18) 0.056(2) 0.0448(17) -0.0059(15) 0.0164(14) 0.0056(15) N27 0.0346(12) 0.0313(11) 0.0254(10) 0.0000(9) 0.0125(9) -0.0009(9) N28 0.0323(11) 0.0294(11) 0.0248(10) 0.0009(8) 0.0113(9) -0.0008(9) C29 0.0291(13) 0.0320(13) 0.0280(12) 0.0053(10) 0.0103(10) 0.0018(11) C30 0.0327(14) 0.0443(16) 0.0336(14) 0.0032(12) 0.0173(12) -0.0019(12) C31 0.0370(14) 0.0397(15) 0.0282(13) -0.0025(11) 0.0152(11) -0.0008(12) C32 0.0352(14) 0.0339(14) 0.0276(12) 0.0059(10) 0.0100(11) -0.0011(11) C33 0.0344(15) 0.0415(16) 0.0421(16) 0.0052(13) 0.0066(12) -0.0016(13) C34 0.0415(18) 0.050(2) 0.060(2) 0.0031(16) 0.0004(16) -0.0070(15) C35 0.061(2) 0.045(2) 0.060(2) -0.0070(16) -0.0015(18) -0.0108(17) C36 0.070(2) 0.0353(17) 0.057(2) -0.0042(14) 0.0201(18) 0.0016(16) C37 0.0458(17) 0.0357(15) 0.0435(16) 0.0016(12) 0.0163(13) 0.0002(13) N38 0.0337(12) 0.0348(12) 0.0332(11) 0.0021(9) 0.0129(10) 0.0026(10) N39 0.0361(12) 0.0298(11) 0.0295(11) 0.0013(9) 0.0160(9) 0.0019(9) C40 0.0400(15) 0.0343(14) 0.0356(14) 0.0048(11) 0.0228(12) 0.0041(12) C41 0.0418(16) 0.0414(17) 0.0436(16) 0.0072(13) 0.0185(13) 0.0125(13) C42 0.0367(15) 0.0435(17) 0.0377(15) 0.0012(12) 0.0100(12) 0.0041(13) C43 0.0510(17) 0.0337(15) 0.0473(17) -0.0039(13) 0.0302(14) 0.0002(13) C44 0.0561(19) 0.0465(18) 0.0470(17) -0.0098(14) 0.0308(15) -0.0004(15) C45 0.079(3) 0.070(3) 0.061(2) -0.021(2) 0.036(2) -0.010(2) C46 0.119(4) 0.063(3) 0.091(4) -0.039(3) 0.046(3) -0.026(3) C47 0.140(5) 0.031(2) 0.117(4) -0.014(2) 0.059(4) -0.004(2) C48 0.092(3) 0.0407(19) 0.068(2) -0.0008(17) 0.035(2) 0.0035(19) N49 0.0386(12) 0.0374(13) 0.0279(11) -0.0004(9) 0.0128(10) 0.0005(10) N50 0.0355(12) 0.0403(13) 0.0275(11) -0.0014(9) 0.0137(9) 0.0060(10) C51 0.0368(15) 0.0510(18) 0.0285(13) -0.0043(12) 0.0094(12) 0.0029(13) C52 0.0530(19) 0.0447(18) 0.0363(16) -0.0052(13) 0.0055(14) -0.0044(15) C53 0.0493(18) 0.0377(16) 0.0375(15) -0.0020(12) 0.0113(13) -0.0034(13) C54 0.0481(18) 0.056(2) 0.0328(15) 0.0013(14) 0.0089(13) 0.0090(15) C55 0.0384(17) 0.066(2) 0.0431(17) -0.0035(15) 0.0109(14) 0.0132(15) C56 0.056(2) 0.071(3) 0.063(2) 0.0030(19) 0.0131(18) 0.0262(19) C57 0.120(4) 0.101(4) 0.057(3) 0.024(3) 0.016(3) 0.059(3) C58 0.197(7) 0.126(5) 0.040(2) 0.012(3) 0.005(3) 0.083(5) C59 0.140(4) 0.088(3) 0.0366(19) -0.004(2) 0.000(2) 0.049(3) N60 0.0363(12) 0.0337(12) 0.0294(11) 0.0031(9) 0.0173(9) 0.0043(9) N61 0.0422(13) 0.0308(11) 0.0332(11) 0.0050(9) 0.0218(10) 0.0091(10) C62 0.0504(17) 0.0295(14) 0.0429(15) 0.0060(11) 0.0305(14) 0.0090(12) C63 0.0450(17) 0.0373(15) 0.0509(17) 0.0059(13) 0.0313(14) 0.0020(13) C64 0.0371(14) 0.0363(15) 0.0345(14) 0.0011(11) 0.0182(12) 0.0018(12) C65 0.073(2) 0.0459(18) 0.060(2) 0.0236(15) 0.0510(19) 0.0313(17) C66 0.092(3) 0.065(2) 0.127(4) 0.056(3) 0.083(3) 0.045(2) C67 0.144(5) 0.099(4) 0.170(6) 0.100(4) 0.128(5) 0.082(4) C68 0.179(6) 0.122(5) 0.098(4) 0.078(4) 0.104(4) 0.112(5) C69 0.132(4) 0.098(3) 0.047(2) 0.029(2) 0.047(2) 0.078(3) C70 0.088(3) 0.067(2) 0.0395(17) 0.0132(16) 0.0352(19) 0.041(2) N71 0.0341(12) 0.0376(13) 0.0283(11) -0.0032(9) 0.0139(9) 0.0049(10) N72 0.0336(12) 0.0373(12) 0.0255(10) -0.0013(9) 0.0121(9) 0.0061(10) C73 0.0267(13) 0.0473(16) 0.0271(12) 0.0000(11) 0.0097(10) 0.0101(12) C74 0.0285(13) 0.0538(18) 0.0334(14) -0.0026(12) 0.0151(11) -0.0006(12) C75 0.0323(14) 0.0401(15) 0.0336(13) -0.0034(12) 0.0141(11) 0.0013(12) C76A 0.022(3) 0.050(4) 0.027(3) -0.004(3) 0.013(2) 0.007(4) C77A 0.042(3) 0.055(4) 0.030(3) 0.005(3) 0.021(2) 0.014(3) C78A 0.057(4) 0.079(5) 0.031(3) 0.002(3) 0.026(3) 0.018(4) C79A 0.060(4) 0.055(5) 0.038(3) -0.011(3) 0.028(3) 0.011(4) C80A 0.039(3) 0.052(4) 0.049(4) -0.010(3) 0.022(3) 0.011(3) C81A 0.030(3) 0.047(4) 0.034(3) -0.004(2) 0.016(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N5A 1.909(17) . ? Cu1 N5B 2.080(13) . ? Cu1 N5C 1.97(2) . ? Cu1 N16 1.990(2) . ? Cu1 N72 1.988(2) . ? Cu1 N83A 2.040(16) . ? Cu1 N83B 2.006(12) . ? Cu1 N83C 1.886(14) . ? Cu2 N6A 2.058(17) . ? Cu2 N6B 1.888(15) . ? Cu2 N6C 1.96(3) . ? Cu2 N17 1.977(2) . ? Cu2 N27 1.993(2) . ? Cu2 N38 1.987(2) . ? Cu3 N28 1.973(2) . ? Cu3 N39 1.965(2) . ? Cu3 N49 1.983(2) . ? Cu3 N60 1.994(2) . ? Cu4 N50 1.953(2) . ? Cu4 N61 1.984(2) . ? Cu4 N71 2.004(2) . ? Cu4 N82A 2.033(17) . ? Cu4 N82B 1.827(10) . ? Cu4 N82C 2.030(15) . ? Cu1 Cu2 3.2881(6) . ? Cu2 Cu3 3.2839(7) . ? Cu3 Cu4 3.2771(7) . ? Cu1 Cu4 3.3342(7) . ? N5A C9A 1.355(8) . ? N5A N6A 1.357(9) . ? N6A C7A 1.363(8) . ? C7A C8A 1.401(9) . ? C7A C10A 1.511(8) . ? C8A C9A 1.375(9) . ? C10A C11A 1.415(12) . ? C10A C15A 1.417(10) . ? C11A C12A 1.363(12) . ? C12A C13A 1.423(11) . ? C13A C14A 1.372(11) . ? C14A C15A 1.371(10) . ? N5B N6B 1.359(9) . ? N5B C9B 1.363(8) . ? N6B C7B 1.354(8) . ? C7B C8B 1.394(8) . ? C7B C10B 1.460(8) . ? C8B C9B 1.381(9) . ? C10B C11B 1.335(12) . ? C10B C15B 1.418(12) . ? C11B C12B 1.411(11) . ? C12B C13B 1.378(12) . ? C13B C14B 1.375(12) . ? C14B C15B 1.417(12) . ? N5C C9C 1.349(9) . ? N5C N6C 1.360(9) . ? N6C C7C 1.357(9) . ? C7C C8C 1.395(9) . ? C7C C10C 1.477(9) . ? C8C C9C 1.378(9) . ? C10C C11C 1.390(12) . ? C10C C15C 1.397(11) . ? C11C C12C 1.397(11) . ? C12C C13C 1.376(11) . ? C13C C14C 1.403(10) . ? C14C C15C 1.384(10) . ? N16 C20 1.350(4) . ? N16 N17 1.373(3) . ? N17 C18 1.355(3) . ? C18 C19 1.391(4) . ? C18 C21 1.470(4) . ? C19 C20 1.383(4) . ? C21 C26 1.386(4) . ? C21 C22 1.401(4) . ? C22 C23 1.390(5) . ? C23 C24 1.375(6) . ? C24 C25 1.392(6) . ? C25 C26 1.397(5) . ? N27 C31 1.353(3) . ? N27 N28 1.375(3) . ? N28 C29 1.348(3) . ? C29 C30 1.394(4) . ? C29 C32 1.474(4) . ? C30 C31 1.380(4) . ? C32 C33 1.394(4) . ? C32 C37 1.395(4) . ? C33 C34 1.383(4) . ? C34 C35 1.376(5) . ? C35 C36 1.386(5) . ? C36 C37 1.399(4) . ? N38 C42 1.346(4) . ? N38 N39 1.362(3) . ? N39 C40 1.352(3) . ? C40 C41 1.399(4) . ? C40 C43 1.466(4) . ? C41 C42 1.376(4) . ? C43 C48 1.392(5) . ? C43 C44 1.397(4) . ? C44 C45 1.390(5) . ? C45 C46 1.377(6) . ? C46 C47 1.373(7) . ? C47 C48 1.389(6) . ? N49 C53 1.348(4) . ? N49 N50 1.362(3) . ? N50 C51 1.358(3) . ? C51 C52 1.391(4) . ? C51 C54 1.469(4) . ? C52 C53 1.381(4) . ? C54 C55 1.386(5) . ? C54 C59 1.392(5) . ? C55 C56 1.387(5) . ? C56 C57 1.367(6) . ? C57 C58 1.370(7) . ? C58 C59 1.396(6) . ? N60 C64 1.352(3) . ? N60 N61 1.369(3) . ? N61 C62 1.355(3) . ? C62 C63 1.391(4) . ? C62 C65 1.477(4) . ? C63 C64 1.386(4) . ? C65 C70 1.393(5) . ? C65 C66 1.401(5) . ? C66 C67 1.411(7) . ? C67 C68 1.372(9) . ? C68 C69 1.352(8) . ? C69 C70 1.397(5) . ? N71 C75 1.349(4) . ? N71 N72 1.381(3) . ? N72 C73 1.360(3) . ? C73 C74 1.389(4) . ? C73 C76A 1.466(5) . ? C73 C76B 1.499(7) . ? C74 C75 1.388(4) . ? C76A C81A 1.388(9) . ? C76A C77A 1.404(9) . ? C77A C78A 1.395(7) . ? C78A C79A 1.389(9) . ? C79A C80A 1.385(8) . ? C80A C81A 1.402(7) . ? C76B C77B 1.394(10) . ? C76B C81B 1.404(10) . ? C77B C78B 1.413(10) . ? C78B C79B 1.377(10) . ? C79B C80B 1.386(10) . ? C80B C81B 1.378(10) . ? N82A C86A 1.347(10) . ? N82A N83A 1.355(10) . ? N83A C84A 1.350(9) . ? C84A C85A 1.383(8) . ? C84A C87A 1.459(8) . ? C85A C86A 1.360(8) . ? C87A C92A 1.370(10) . ? C87A C88A 1.398(10) . ? C88A C89A 1.394(10) . ? C89A C90A 1.385(10) . ? C90A C91A 1.404(11) . ? C91A C92A 1.383(10) . ? N82B C86B 1.346(9) . ? N82B N83B 1.356(8) . ? N83B C84B 1.344(9) . ? C84B C85B 1.398(9) . ? C84B C87B 1.471(8) . ? C85B C86B 1.367(9) . ? C87B C92B 1.379(11) . ? C87B C88B 1.423(11) . ? C88B C89B 1.386(11) . ? C89B C90B 1.391(12) . ? C90B C91B 1.382(12) . ? C91B C92B 1.397(11) . ? N82C C86C 1.374(15) . ? N82C N83C 1.390(14) . ? N83C C84C 1.351(17) . ? C84C C85C 1.409(16) . ? C84C C87C 1.514(15) . ? C85C C86C 1.377(14) . ? C87C C92C 1.386(11) . ? C87C C88C 1.386(11) . ? C88C C89C 1.404(9) . ? C89C C90C 1.390(12) . ? C90C C91C 1.383(12) . ? C91C C92C 1.406(10) . ? C93A C94A 1.532(10) . ? C94A C95A 1.502(9) . ? C95A C96A 1.492(9) . ? C96A C97A 1.499(9) . ? C96A C94B 1.504(9) . ? C94B C95B 1.430(8) . ? C95B C96B 1.482(8) . ? C96B C97B 1.519(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5A Cu1 N16 92.5(8) . . ? N5A Cu1 N72 100.1(8) . . ? N5A Cu1 N83A 154.6(6) . . ? N5A Cu1 N83B 158.0(4) . . ? N5A Cu1 N83C 153.2(6) . . ? N5B Cu1 N16 90.2(5) . . ? N5B Cu1 N72 99.9(8) . . ? N5B Cu1 N83A 158.6(9) . . ? N5B Cu1 N83B 162.5(6) . . ? N5B Cu1 N83C 157.2(9) . . ? N5C Cu1 N16 96.0(4) . . ? N5C Cu1 N72 94.2(4) . . ? N5C Cu1 N83A 159.6(7) . . ? N5C Cu1 N83B 161.1(6) . . ? N5C Cu1 N83C 158.2(7) . . ? N16 Cu1 N72 146.58(9) . . ? N16 Cu1 N83A 88.7(7) . . ? N16 Cu1 N83B 95.5(3) . . ? N16 Cu1 N83C 89.0(7) . . ? N72 Cu1 N83A 92.6(7) . . ? N72 Cu1 N83B 84.3(3) . . ? N72 Cu1 N83C 93.1(7) . . ? N6A Cu2 N17 88.0(6) . . ? N6A Cu2 N27 90.7(8) . . ? N6A Cu2 N38 157.2(5) . . ? N6B Cu2 N17 87.3(4) . . ? N6B Cu2 N27 94.2(4) . . ? N6B Cu2 N38 152.1(3) . . ? N6C Cu2 N17 90.6(6) . . ? N6C Cu2 N27 88.4(7) . . ? N6C Cu2 N38 156.0(6) . . ? N17 Cu2 N27 148.55(9) . . ? N17 Cu2 N38 100.76(9) . . ? N27 Cu2 N38 92.44(9) . . ? N28 Cu3 N39 87.71(9) . . ? N28 Cu3 N49 101.58(9) . . ? N28 Cu3 N60 142.78(9) . . ? N39 Cu3 N49 154.97(9) . . ? N39 Cu3 N60 91.40(9) . . ? N49 Cu3 N60 94.73(9) . . ? N50 Cu4 N61 87.83(9) . . ? N50 Cu4 N71 92.62(9) . . ? N50 Cu4 N82A 155.3(6) . . ? N50 Cu4 N82B 152.7(4) . . ? N50 Cu4 N82C 159.5(4) . . ? N61 Cu4 N71 143.43(9) . . ? N61 Cu4 N82A 98.6(8) . . ? N61 Cu4 N82B 103.3(4) . . ? N61 Cu4 N82C 95.5(5) . . ? N71 Cu4 N82A 96.0(6) . . ? N71 Cu4 N82B 92.8(3) . . ? N71 Cu4 N82C 96.5(4) . . ? N5A N6A C7A 109.6(15) . . ? N5A N6A Cu2 117.0(8) . . ? C7A N6A Cu2 133.3(13) . . ? N6A C7A C8A 108.0(11) . . ? N6A C7A C10A 122.8(12) . . ? C8A C7A C10A 129.2(9) . . ? C9A C8A C7A 104.6(8) . . ? N5A C9A C8A 111.1(13) . . ? C11A C10A C15A 113.6(6) . . ? C11A C10A C7A 123.5(8) . . ? C15A C10A C7A 122.8(8) . . ? C12A C11A C10A 122.3(7) . . ? C11A C12A C13A 122.2(8) . . ? C14A C13A C12A 116.0(7) . . ? C15A C14A C13A 121.5(7) . . ? C14A C15A C10A 124.0(7) . . ? N6B N5B C9B 110.5(13) . . ? N6B N5B Cu1 119.5(7) . . ? C9B N5B Cu1 129.9(10) . . ? C7B N6B N5B 105.3(12) . . ? C7B N6B Cu2 135.8(11) . . ? N5B N6B Cu2 118.2(7) . . ? N6B C7B C8B 111.5(10) . . ? N6B C7B C10B 119.6(11) . . ? C8B C7B C10B 128.6(10) . . ? C9B C8B C7B 104.5(8) . . ? N5B C9B C8B 108.2(11) . . ? C11B C10B C15B 120.6(7) . . ? C11B C10B C7B 120.4(10) . . ? C15B C10B C7B 118.7(10) . . ? C10B C11B C12B 122.9(7) . . ? C13B C12B C11B 117.0(8) . . ? C14B C13B C12B 120.8(8) . . ? C13B C14B C15B 121.6(8) . . ? C14B C15B C10B 116.2(8) . . ? C9C N5C N6C 105(2) . . ? C9C N5C Cu1 130.1(19) . . ? N6C N5C Cu1 119.3(9) . . ? C7C N6C N5C 111(2) . . ? C7C N6C Cu2 129.5(19) . . ? N5C N6C Cu2 119.1(10) . . ? N6C C7C C8C 106.6(15) . . ? N6C C7C C10C 125.7(16) . . ? C8C C7C C10C 127.2(15) . . ? C9C C8C C7C 105.5(13) . . ? N5C C9C C8C 110.8(18) . . ? C11C C10C C15C 118.9(7) . . ? C11C C10C C7C 123.0(11) . . ? C15C C10C C7C 118.0(12) . . ? C10C C11C C12C 120.4(7) . . ? C13C C12C C11C 120.7(8) . . ? C12C C13C C14C 118.9(7) . . ? C15C C14C C13C 120.6(7) . . ? C14C C15C C10C 120.3(7) . . ? C20 N16 N17 107.3(2) . . ? C20 N16 Cu1 129.2(2) . . ? N17 N16 Cu1 122.95(16) . . ? C18 N17 N16 108.4(2) . . ? C18 N17 Cu2 137.03(19) . . ? N16 N17 Cu2 112.72(16) . . ? N17 C18 C19 109.1(2) . . ? N17 C18 C21 121.4(2) . . ? C19 C18 C21 129.5(3) . . ? C20 C19 C18 105.1(2) . . ? N16 C20 C19 110.2(3) . . ? C26 C21 C22 119.0(3) . . ? C26 C21 C18 121.3(3) . . ? C22 C21 C18 119.7(3) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C25 120.2(3) . . ? C24 C25 C26 120.0(3) . . ? C21 C26 C25 120.2(3) . . ? C31 N27 N28 107.4(2) . . ? C31 N27 Cu2 127.85(18) . . ? N28 N27 Cu2 124.26(16) . . ? C29 N28 N27 108.3(2) . . ? C29 N28 Cu3 138.28(17) . . ? N27 N28 Cu3 111.60(15) . . ? N28 C29 C30 109.2(2) . . ? N28 C29 C32 121.6(2) . . ? C30 C29 C32 129.2(2) . . ? C31 C30 C29 105.2(2) . . ? N27 C31 C30 109.9(2) . . ? C33 C32 C37 119.3(3) . . ? C33 C32 C29 119.6(3) . . ? C37 C32 C29 121.1(2) . . ? C34 C33 C32 120.7(3) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 120.2(3) . . ? C35 C36 C37 120.2(3) . . ? C32 C37 C36 119.5(3) . . ? C42 N38 N39 107.6(2) . . ? C42 N38 Cu2 129.3(2) . . ? N39 N38 Cu2 119.91(16) . . ? C40 N39 N38 108.9(2) . . ? C40 N39 Cu3 132.45(19) . . ? N38 N39 Cu3 117.86(16) . . ? N39 C40 C41 108.3(2) . . ? N39 C40 C43 121.7(2) . . ? C41 C40 C43 130.0(3) . . ? C42 C41 C40 105.2(3) . . ? N38 C42 C41 110.1(3) . . ? C48 C43 C44 118.2(3) . . ? C48 C43 C40 119.6(3) . . ? C44 C43 C40 122.1(3) . . ? C45 C44 C43 121.7(3) . . ? C46 C45 C44 119.5(4) . . ? C47 C46 C45 119.2(4) . . ? C46 C47 C48 122.2(4) . . ? C47 C48 C43 119.2(4) . . ? C53 N49 N50 107.1(2) . . ? C53 N49 Cu3 131.5(2) . . ? N50 N49 Cu3 120.13(17) . . ? C51 N50 N49 108.9(2) . . ? C51 N50 Cu4 132.3(2) . . ? N49 N50 Cu4 118.04(17) . . ? N50 C51 C52 108.5(3) . . ? N50 C51 C54 120.8(3) . . ? C52 C51 C54 130.6(3) . . ? C53 C52 C51 104.9(3) . . ? N49 C53 C52 110.5(3) . . ? C55 C54 C59 117.7(3) . . ? C55 C54 C51 122.0(3) . . ? C59 C54 C51 120.3(3) . . ? C54 C55 C56 121.1(3) . . ? C57 C56 C55 120.6(4) . . ? C56 C57 C58 119.5(4) . . ? C57 C58 C59 120.4(4) . . ? C54 C59 C58 120.6(4) . . ? C64 N60 N61 107.6(2) . . ? C64 N60 Cu3 128.77(18) . . ? N61 N60 Cu3 122.50(17) . . ? C62 N61 N60 108.2(2) . . ? C62 N61 Cu4 136.54(18) . . ? N60 N61 Cu4 109.40(15) . . ? N61 C62 C63 109.3(2) . . ? N61 C62 C65 120.6(3) . . ? C63 C62 C65 129.6(3) . . ? C64 C63 C62 105.0(2) . . ? N60 C64 C63 109.9(2) . . ? C70 C65 C66 119.7(3) . . ? C70 C65 C62 120.3(3) . . ? C66 C65 C62 119.9(4) . . ? C65 C66 C67 118.1(5) . . ? C68 C67 C66 121.3(5) . . ? C69 C68 C67 120.2(4) . . ? C68 C69 C70 120.8(5) . . ? C65 C70 C69 119.9(4) . . ? C75 N71 N72 107.7(2) . . ? C75 N71 Cu4 127.36(18) . . ? N72 N71 Cu4 124.83(17) . . ? C73 N72 N71 107.9(2) . . ? C73 N72 Cu1 135.82(18) . . ? N71 N72 Cu1 110.77(16) . . ? N72 C73 C74 109.2(2) . . ? N72 C73 C76A 127.5(4) . . ? C74 C73 C76A 123.3(4) . . ? N72 C73 C76B 115.0(5) . . ? C74 C73 C76B 135.2(5) . . ? C75 C74 C73 105.3(2) . . ? N71 C75 C74 109.9(2) . . ? C81A C76A C77A 119.2(4) . . ? C81A C76A C73 117.8(6) . . ? C77A C76A C73 123.0(6) . . ? C78A C77A C76A 119.3(6) . . ? C79A C78A C77A 120.5(5) . . ? C80A C79A C78A 120.8(5) . . ? C79A C80A C81A 118.5(5) . . ? C76A C81A C80A 121.5(5) . . ? C77B C76B C81B 118.3(6) . . ? C77B C76B C73 117.1(7) . . ? C81B C76B C73 124.6(7) . . ? C76B C77B C78B 120.9(6) . . ? C79B C78B C77B 119.1(6) . . ? C78B C79B C80B 120.3(7) . . ? C81B C80B C79B 120.8(7) . . ? C80B C81B C76B 120.4(6) . . ? C86A N82A N83A 103.0(15) . . ? C86A N82A Cu4 135.2(12) . . ? N83A N82A Cu4 120.6(9) . . ? C84A N83A N82A 112.6(14) . . ? C84A N83A Cu1 129.5(13) . . ? N82A N83A Cu1 117.6(8) . . ? N83A C84A C85A 106.0(9) . . ? N83A C84A C87A 125.9(10) . . ? C85A C84A C87A 127.9(8) . . ? C86A C85A C84A 105.3(8) . . ? N82A C86A C85A 112.7(12) . . ? C92A C87A C88A 119.8(6) . . ? C92A C87A C84A 120.7(8) . . ? C88A C87A C84A 119.5(8) . . ? C89A C88A C87A 120.0(6) . . ? C90A C89A C88A 120.0(6) . . ? C89A C90A C91A 119.3(6) . . ? C92A C91A C90A 120.1(7) . . ? C87A C92A C91A 120.6(7) . . ? C86B N82B N83B 102.9(10) . . ? C86B N82B Cu4 133.9(8) . . ? N83B N82B Cu4 122.6(7) . . ? C84B N83B N82B 115.0(10) . . ? C84B N83B Cu1 125.6(7) . . ? N82B N83B Cu1 119.2(7) . . ? N83B C84B C85B 102.7(9) . . ? N83B C84B C87B 126.2(10) . . ? C85B C84B C87B 129.7(10) . . ? C86B C85B C84B 107.4(10) . . ? N82B C86B C85B 111.0(10) . . ? C92B C87B C88B 117.8(6) . . ? C92B C87B C84B 123.0(10) . . ? C88B C87B C84B 119.1(10) . . ? C89B C88B C87B 119.8(7) . . ? C88B C89B C90B 120.9(7) . . ? C91B C90B C89B 119.5(7) . . ? C90B C91B C92B 119.7(7) . . ? C87B C92B C91B 121.8(7) . . ? C86C N82C N83C 115.8(12) . . ? C86C N82C Cu4 120.1(11) . . ? N83C N82C Cu4 120.7(10) . . ? C84C N83C N82C 98.8(13) . . ? C84C N83C Cu1 143.0(12) . . ? N82C N83C Cu1 118.0(9) . . ? N83C C84C C85C 115.7(12) . . ? N83C C84C C87C 113.8(13) . . ? C85C C84C C87C 130.4(12) . . ? C86C C85C C84C 104.1(10) . . ? N82C C86C C85C 104.7(12) . . ? C92C C87C C88C 120.6(6) . . ? C92C C87C C84C 118.5(10) . . ? C88C C87C C84C 119.9(11) . . ? C87C C88C C89C 120.1(7) . . ? C90C C89C C88C 119.1(7) . . ? C91C C90C C89C 120.6(7) . . ? C90C C91C C92C 120.0(7) . . ? C87C C92C C91C 119.1(6) . . ? C95A C94A C93A 109.6(8) . . ? C96A C95A C94A 116.7(7) . . ? C95A C96A C97A 118.1(7) . . ? C95A C96A C94B 106.6(5) . . ? C97A C96A C94B 134.0(10) . . ? C95B C94B C96A 119.4(8) . . ? C94B C95B C96B 123.4(7) . . ? C95B C96B C97B 114.7(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.835 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.072 #=END data_c:\datasets\leeds\smcuf2~3\smcupyf2 _database_code_depnum_ccdc_archive 'CCDC 632226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Pentakis[3{5}-(4-fluorophenyl)pyrazolido]tetrakis[5-(4-fluorophenyl)pyrazole] trifluorotetracopper(II) dichloromethane (1/0.75) 3{5}-(4-fluorophenyl)pyrazole (1/0.25) solvate ; _chemical_name_common ; Pentakis(3(5)-(4-fluorophenyl)pyrazolido)tetrakis(5-(4- fluorophenyl)pyrazole) trifluorotetracopper(ii) dichloromethane (1/0.75) 3(5)-(4-fluorophenyl)pyrazole (1/0.25) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C81 H58 Cu4 F12 N18, 0.75[C H2 Cl2], 0.25[C9 H7 F N2]' _chemical_formula_sum 'C84 H61.25 Cl1.50 Cu4 F12.25 N18.50' _chemical_formula_weight 1869.85 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' 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' Cl Cl 0.1484 0.1585 '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 17.0552(1) _cell_length_b 20.9288(1) _cell_length_c 25.8492(2) _cell_angle_alpha 90.5532(2) _cell_angle_beta 103.5682(3) _cell_angle_gamma 106.7792(4) _cell_volume 8557.65(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 171105 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Blue _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3786 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_T_max 0.986 _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 ; 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_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 diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 171105 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.51 _reflns_number_total 39023 _reflns_number_gt 27281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 asymmetric unit contains two molecules of the complex, labelled 'A' and 'B'. Where required, partial disorder sites of atoms in molecule 'A' are given the label 'C', and those in molecule 'B' are labelled as 'D'. The asymmetric unit also contains four weakly occupied dichloromethane environments C1S-Cl3S (fully occupied), C4S-Cl6S (occupancy 0.2), C7S-Cl9S (0.1) and C10S-Cl12S (0.2); and, two weakly occupied 3{5}-(4-fluorophenyl)pyrazole sites N1E-F12E (occupancy 0.3) and N13E-F24E (0.2). Partial molecules N1E-F12E, N13E-F24E and C10S-Cl12S occupy the same region of space in the lattice, so these sites cannot be simultaneously occupied. The same is true of C4S-Cl6S C7S-Cl9S and partial ligand [N11B, N12B, C51B-C59B, F60B]. The two complex molecules show extensive, and similar, patterns of disorder. The following 4-fluorophenyl substituents are disordered, each over two equally occupied sites: [C34A-C39A, F40A] and [C34C-C39C, F40C] [C44A-C49A, F50A] and [C44C-C49C, F50C] [C44B-C49B, F50B] and [C44D-C49D, F50D] [C74A-C79A, F80A] and [C74C-C79C, F80C] [C74B-C79B, F80B] and [C74D-C79D, F80D] The following 5-(4-fluorophenyl)pyrazole ligands are disordered, each over two equally occupied sites: [N11B, N12B, C51B-C59B, F60B] (occupancy 0.50) and [N11D, N12D, C51D-C59D, F60D] (0.50) [N13A, N14A, C61A-C69A, F70A] (occupancy 0.50) and [N13C, N14C, C61C-C69C, F70C] (0.50) [N13B, N14B, C61B-C69B, F70B] (occupancy 0.50) and [N13D, N14D, C61D-C69D, F70D] (0.50) The following restraints were applied to the disordered groups and weakly occupied pyrazole and solvent sites in the model: Intra-pyrazole N-N = 1.34(1)\%A Intra-pyrazole N-C = 1.35(1)\%A Intra-pyrazole N=C = 1.34(1)\%A Intra-pyrazole C-C = 1.39(1)\%A Intra-pyrazole C=C = 1.37(1)\%A C-F = 1.33(1)\%A C-Cl = 1.78(2)\%A Cl...Cl = 2.91(2)\%A and all disordered or partially occupied C~6~H~4~ groups were refined as rigid hexagons. All atoms with occupancy >=0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The largest residual Fourier hole of -1.3 e.\%A^-3^ is 0.8\%A from Cu2A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+5.9930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 39023 _refine_ls_number_parameters 2660 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1A Cu 0.15002(3) 0.24401(2) 0.779403(18) 0.03908(10) Uani 1 1 d . C . Cu2A Cu 0.26441(3) 0.23295(2) 0.670746(19) 0.04259(11) Uani 1 1 d . . . Cu3A Cu 0.11857(3) 0.30615(2) 0.624626(18) 0.03731(10) Uani 1 1 d . C . Cu4A Cu 0.00855(3) 0.17777(2) 0.668529(18) 0.03933(10) Uani 1 1 d . C . F1A F 0.14599(13) 0.23869(10) 0.69169(8) 0.0403(4) Uani 1 1 d . C . F2A F 0.23912(12) 0.32946(10) 0.78257(8) 0.0407(5) Uani 1 1 d . . . F3A F 0.23014(15) 0.14160(11) 0.69092(9) 0.0512(6) Uani 1 1 d . . . N1A N 0.20079(19) 0.21286(15) 0.59406(13) 0.0417(7) Uani 1 1 d . D . N2A N 0.13462(19) 0.23816(15) 0.57820(13) 0.0434(7) Uani 1 1 d . . . C1A C 0.0986(3) 0.21827(19) 0.52632(16) 0.0481(9) Uani 1 1 d . . . H1A H 0.0506 0.2288 0.5058 0.058 Uiso 1 1 calc R . . C2A C 0.1412(3) 0.18042(19) 0.50712(16) 0.0468(9) Uani 1 1 d . . . H2A H 0.1294 0.1606 0.4719 0.056 Uiso 1 1 calc R D . C3A C 0.2059(2) 0.17774(18) 0.55124(15) 0.0416(8) Uani 1 1 d . D . C4A C 0.2720(2) 0.14547(18) 0.55362(16) 0.0426(8) Uani 1 1 d . . . C5A C 0.3509(3) 0.1694(2) 0.58823(18) 0.0515(10) Uani 1 1 d . . . H5A H 0.3636 0.2088 0.6111 0.062 Uiso 1 1 calc R . . C6A C 0.4124(3) 0.1372(2) 0.5905(2) 0.0600(11) Uani 1 1 d . . . H6A H 0.4662 0.1535 0.6150 0.072 Uiso 1 1 calc R D . C7A C 0.3928(3) 0.0812(2) 0.5561(2) 0.0587(11) Uani 1 1 d . . . C8A C 0.3159(3) 0.0558(2) 0.5207(2) 0.0583(11) Uani 1 1 d . . . H8A H 0.3041 0.0168 0.4975 0.070 Uiso 1 1 calc R D . C9A C 0.2563(3) 0.0883(2) 0.51959(17) 0.0496(9) Uani 1 1 d . . . H9A H 0.2027 0.0714 0.4950 0.060 Uiso 1 1 calc R . . F10A F 0.45265(19) 0.04915(16) 0.55832(15) 0.0870(10) Uani 1 1 d . . . N3A N 0.24034(18) 0.35692(15) 0.63683(12) 0.0391(7) Uani 1 1 d . . . N4A N 0.30057(19) 0.32880(16) 0.65988(13) 0.0434(7) Uani 1 1 d . . . C11A C 0.3754(2) 0.3763(2) 0.66996(17) 0.0485(9) Uani 1 1 d . . . H11E H 0.4284 0.3694 0.6855 0.058 Uiso 1 1 calc R D . C12A C 0.3642(2) 0.4369(2) 0.65428(17) 0.0494(9) Uani 1 1 d . D . H12A H 0.4063 0.4789 0.6570 0.059 Uiso 1 1 calc R . . C13A C 0.2769(2) 0.42218(18) 0.63353(15) 0.0404(8) Uani 1 1 d . D . C14A C 0.2264(2) 0.46516(19) 0.60940(15) 0.0405(8) Uani 1 1 d . . . C15A C 0.2395(2) 0.52879(18) 0.63322(16) 0.0454(9) Uani 1 1 d . . . H15E H 0.2832 0.5452 0.6648 0.054 Uiso 1 1 calc R . . C16A C 0.1892(2) 0.56844(19) 0.61105(17) 0.0474(9) Uani 1 1 d . . . H16A H 0.1979 0.6118 0.6270 0.057 Uiso 1 1 calc R D . C17A C 0.1265(2) 0.54278(19) 0.56519(17) 0.0460(9) Uani 1 1 d . . . C18A C 0.1110(2) 0.4803(2) 0.53996(16) 0.0478(9) Uani 1 1 d . . . H18A H 0.0674 0.4644 0.5082 0.057 Uiso 1 1 calc R D . C19A C 0.1617(2) 0.44170(19) 0.56286(15) 0.0428(8) Uani 1 1 d . . . H19A H 0.1524 0.3984 0.5466 0.051 Uiso 1 1 calc R . . F20A F 0.07722(15) 0.58190(12) 0.54270(10) 0.0570(6) Uani 1 1 d . . . N5A N -0.05175(19) 0.21584(15) 0.60689(12) 0.0399(7) Uani 1 1 d . . . N6A N -0.00554(19) 0.27323(15) 0.59148(12) 0.0404(7) Uani 1 1 d . C . C21A C -0.0566(2) 0.29483(19) 0.55301(15) 0.0436(8) Uani 1 1 d . . . H21A H -0.0395 0.3339 0.5350 0.052 Uiso 1 1 calc R D . C22A C -0.1381(2) 0.25187(18) 0.54324(15) 0.0429(8) Uani 1 1 d . D . H22A H -0.1869 0.2555 0.5182 0.051 Uiso 1 1 calc R . . C23A C -0.1330(2) 0.20208(18) 0.57830(15) 0.0404(8) Uani 1 1 d . D . C24A C -0.2014(2) 0.14487(19) 0.58711(17) 0.0461(9) Uani 1 1 d . . . C25A C -0.1927(3) 0.1102(2) 0.6325(2) 0.0629(12) Uani 1 1 d . . . H25A H -0.1416 0.1245 0.6597 0.076 Uiso 1 1 calc R . . C26A C -0.2568(3) 0.0555(3) 0.6388(2) 0.0779(15) Uani 1 1 d . . . H26A H -0.2490 0.0300 0.6688 0.093 Uiso 1 1 calc R D . C27A C -0.3330(3) 0.0385(2) 0.6003(2) 0.0654(13) Uani 1 1 d . . . C28A C -0.3457(3) 0.0725(2) 0.5563(2) 0.0556(11) Uani 1 1 d . . . H28A H -0.3987 0.0604 0.5307 0.067 Uiso 1 1 calc R D . C29A C -0.2788(2) 0.1257(2) 0.54982(18) 0.0481(9) Uani 1 1 d . . . H29A H -0.2862 0.1496 0.5189 0.058 Uiso 1 1 calc R . . F30A F -0.39663(18) -0.01518(14) 0.60796(16) 0.0878(10) Uani 1 1 d . . . N7A N 0.05103(19) 0.27845(15) 0.76246(12) 0.0395(7) Uani 1 1 d . . . N8A N -0.00629(19) 0.24830(15) 0.71554(13) 0.0426(7) Uani 1 1 d . C . C31A C -0.0721(3) 0.2726(2) 0.70915(17) 0.0501(9) Uani 1 1 d . . . H31A H -0.1204 0.2602 0.6797 0.060 Uiso 1 1 calc R D . C32A C -0.0601(3) 0.3182(2) 0.75133(17) 0.0546(10) Uani 1 1 d . A . H32A H -0.0971 0.3427 0.7564 0.066 Uiso 1 1 calc R . . C33A C 0.0181(2) 0.32078(19) 0.78508(15) 0.0465(9) Uani 1 1 d D A . C34A C 0.0701(11) 0.3564(11) 0.8374(6) 0.040(4) Uani 0.50 1 d PGD A 1 C35A C 0.0165(9) 0.3807(11) 0.8596(7) 0.053(4) Uani 0.50 1 d PG A 1 H35A H -0.0420 0.3693 0.8424 0.064 Uiso 0.50 1 calc PR A 1 C36A C 0.0485(9) 0.4217(9) 0.9070(6) 0.108(9) Uani 0.50 1 d PG A 1 H36A H 0.0119 0.4383 0.9222 0.130 Uiso 0.50 1 calc PR A 1 C37A C 0.1341(9) 0.4384(7) 0.9322(4) 0.069(8) Uani 0.50 1 d PGD A 1 C38A C 0.1877(8) 0.4141(9) 0.9100(6) 0.053(5) Uani 0.50 1 d PG A 1 H38A H 0.2461 0.4255 0.9273 0.064 Uiso 0.50 1 calc PR A 1 C39A C 0.1557(10) 0.3731(10) 0.8626(6) 0.051(5) Uani 0.50 1 d PG A 1 H39A H 0.1923 0.3565 0.8475 0.061 Uiso 0.50 1 calc PR A 1 F40A F 0.174(2) 0.4736(16) 0.9797(8) 0.130(12) Uani 0.50 1 d PD A 1 C34C C 0.0514(12) 0.3625(11) 0.8367(5) 0.030(3) Uani 0.50 1 d PGD A 2 C35C C 0.0053(9) 0.3908(11) 0.8628(6) 0.053(4) Uani 0.50 1 d PG A 2 H35C H -0.0531 0.3840 0.8475 0.064 Uiso 0.50 1 calc PR A 2 C36C C 0.0448(9) 0.4292(8) 0.9111(5) 0.057(4) Uani 0.50 1 d PG A 2 H36C H 0.0133 0.4485 0.9289 0.069 Uiso 0.50 1 calc PR A 2 C37C C 0.1304(9) 0.4392(8) 0.9334(5) 0.090(10) Uani 0.50 1 d PGD A 2 C38C C 0.1765(8) 0.4109(10) 0.9074(6) 0.077(7) Uani 0.50 1 d PG A 2 H38C H 0.2350 0.4177 0.9226 0.092 Uiso 0.50 1 calc PR A 2 C39C C 0.1370(11) 0.3725(10) 0.8590(5) 0.036(3) Uani 0.50 1 d PG A 2 H39C H 0.1685 0.3532 0.8412 0.044 Uiso 0.50 1 calc PR A 2 F40C F 0.1648(17) 0.4827(12) 0.9770(7) 0.080(4) Uani 0.50 1 d PD A 2 N9A N 0.0700(2) 0.15294(15) 0.77838(13) 0.0444(7) Uani 1 1 d . . . N10A N 0.0284(2) 0.12278(15) 0.72878(13) 0.0449(7) Uani 1 1 d . C . C41A C -0.0061(3) 0.0574(2) 0.73358(17) 0.0529(10) Uani 1 1 d . . . H41A H -0.0384 0.0248 0.7048 0.063 Uiso 1 1 calc R D . C42A C 0.0128(3) 0.0448(2) 0.78674(18) 0.0601(12) Uani 1 1 d . B . H42A H -0.0034 0.0031 0.8015 0.072 Uiso 1 1 calc R . . C43A C 0.0605(3) 0.1063(2) 0.81391(15) 0.0495(9) Uani 1 1 d D B . C44A C 0.0955(13) 0.1250(9) 0.8720(3) 0.052(10) Uani 0.50 1 d PGD B 1 C45A C 0.0981(15) 0.1831(9) 0.8997(6) 0.059(5) Uani 0.50 1 d PG B 1 H45A H 0.0738 0.2147 0.8814 0.071 Uiso 0.50 1 calc PR B 1 C46A C 0.1363(15) 0.1951(10) 0.9540(6) 0.078(6) Uani 0.50 1 d PG B 1 H46A H 0.1381 0.2349 0.9730 0.093 Uiso 0.50 1 calc PR B 1 C47A C 0.1718(16) 0.1490(13) 0.9808(3) 0.095(7) Uani 0.50 1 d PGD B 1 C48A C 0.1691(18) 0.0908(12) 0.9531(6) 0.101(8) Uani 0.50 1 d PG B 1 H48A H 0.1934 0.0592 0.9713 0.121 Uiso 0.50 1 calc PR B 1 C49A C 0.1310(15) 0.0788(8) 0.8987(6) 0.125(11) Uani 0.50 1 d PG B 1 H49A H 0.1292 0.0390 0.8798 0.149 Uiso 0.50 1 calc PR B 1 F50A F 0.2060(13) 0.1630(8) 1.0335(4) 0.116(5) Uani 0.50 1 d PD B 1 C44C C 0.0965(13) 0.1232(8) 0.8709(3) 0.069(12) Uani 0.50 1 d PGD B 2 C45C C 0.0930(17) 0.1848(9) 0.8891(6) 0.077(7) Uani 0.50 1 d PG B 2 H45C H 0.0710 0.2126 0.8645 0.092 Uiso 0.50 1 calc PR B 2 C46C C 0.1215(17) 0.2056(8) 0.9432(6) 0.102(9) Uani 0.50 1 d PG B 2 H46C H 0.1190 0.2477 0.9557 0.122 Uiso 0.50 1 calc PR B 2 C47C C 0.1536(17) 0.1650(10) 0.9791(3) 0.089(7) Uani 0.50 1 d PGD B 2 C48C C 0.1572(16) 0.1034(10) 0.9609(5) 0.091(7) Uani 0.50 1 d PG B 2 H48C H 0.1791 0.0756 0.9855 0.109 Uiso 0.50 1 calc PR B 2 C49C C 0.1286(12) 0.0825(7) 0.9068(5) 0.056(4) Uani 0.50 1 d PG B 2 H49C H 0.1311 0.0405 0.8943 0.067 Uiso 0.50 1 calc PR B 2 F50C F 0.1855(18) 0.1854(9) 1.0311(4) 0.161(10) Uani 0.50 1 d PD B 2 N11A N 0.2520(2) 0.15157(17) 0.79992(14) 0.0525(8) Uani 1 1 d . C . H11A H 0.2299 0.1327 0.7671 0.063 Uiso 1 1 calc R . . N12A N 0.2442(2) 0.20903(15) 0.81706(13) 0.0455(7) Uani 1 1 d . . . C51A C 0.2867(3) 0.2205(2) 0.86803(16) 0.0522(10) Uani 1 1 d . C 1 H51A H 0.2921 0.2586 0.8905 0.063 Uiso 1 1 calc R . . C52A C 0.3215(3) 0.1711(2) 0.88402(19) 0.0642(12) Uani 1 1 d . . . H52A H 0.3548 0.1679 0.9184 0.077 Uiso 1 1 calc R C 1 C53A C 0.2980(3) 0.1259(2) 0.83927(18) 0.0556(10) Uani 1 1 d . C . C54A C 0.3108(3) 0.0604(2) 0.8317(2) 0.0609(11) Uani 1 1 d . . . C55A C 0.2955(4) 0.0288(3) 0.7815(2) 0.0736(14) Uani 1 1 d . C . H55A H 0.2781 0.0507 0.7508 0.088 Uiso 1 1 calc R . . C56A C 0.3050(4) -0.0337(3) 0.7750(3) 0.0851(17) Uani 1 1 d . . . H56A H 0.2969 -0.0540 0.7404 0.102 Uiso 1 1 calc R C . C57A C 0.3262(4) -0.0658(3) 0.8192(3) 0.0862(17) Uani 1 1 d . C . C58A C 0.3403(5) -0.0377(3) 0.8695(3) 0.104(2) Uani 1 1 d . . . H58A H 0.3546 -0.0615 0.8996 0.124 Uiso 1 1 calc R C . C59A C 0.3333(5) 0.0264(3) 0.8762(2) 0.094(2) Uani 1 1 d . C . H59A H 0.3439 0.0470 0.9111 0.113 Uiso 1 1 calc R . . F60A F 0.3342(3) -0.12769(18) 0.81345(19) 0.1232(15) Uani 1 1 d . . . N13A N 0.3760(18) 0.299(2) 0.7713(14) 0.044(6) Uani 0.50 1 d PD D 1 H13A H 0.3378 0.3179 0.7761 0.053 Uiso 0.50 1 calc PR D 1 N14A N 0.3700(13) 0.2535(14) 0.7324(9) 0.045(6) Uani 0.50 1 d PD D 1 C61A C 0.4400(13) 0.2364(12) 0.7349(9) 0.077(9) Uani 0.50 1 d PD D 1 H61A H 0.4516 0.2109 0.7087 0.092 Uiso 0.50 1 calc PR D 1 C62A C 0.4924(10) 0.2641(11) 0.7845(8) 0.060(6) Uani 0.50 1 d PD D 1 H62A H 0.5421 0.2542 0.8028 0.072 Uiso 0.50 1 calc PR D 1 C63A C 0.4563(18) 0.3093(14) 0.8013(8) 0.038(5) Uani 0.50 1 d PD D 1 C64A C 0.4848(10) 0.3535(9) 0.8509(5) 0.031(2) Uani 0.50 1 d PGD D 1 C65A C 0.5665(10) 0.3595(9) 0.8803(7) 0.049(4) Uani 0.50 1 d PG D 1 H65A H 0.5986 0.3348 0.8684 0.058 Uiso 0.50 1 calc PR D 1 C66A C 0.6010(9) 0.4015(8) 0.9271(6) 0.048(4) Uani 0.50 1 d PG D 1 H66A H 0.6568 0.4056 0.9472 0.057 Uiso 0.50 1 calc PR D 1 C67A C 0.5539(11) 0.4376(7) 0.9445(5) 0.040(3) Uani 0.50 1 d PGD D 1 C68A C 0.4723(11) 0.4316(8) 0.9152(6) 0.043(4) Uani 0.50 1 d PG D 1 H68A H 0.4401 0.4563 0.9271 0.052 Uiso 0.50 1 calc PR D 1 C69A C 0.4377(9) 0.3896(9) 0.8684(5) 0.038(3) Uani 0.50 1 d PG D 1 H69A H 0.3819 0.3855 0.8483 0.046 Uiso 0.50 1 calc PR D 1 F70A F 0.5800(19) 0.4746(14) 0.9910(8) 0.071(4) Uani 0.50 1 d PD D 1 N13C N 0.3823(14) 0.2963(19) 0.7784(13) 0.033(4) Uani 0.50 1 d PD D 2 H13C H 0.3464 0.3176 0.7828 0.039 Uiso 0.50 1 calc PR D 2 N14C N 0.3601(14) 0.2504(14) 0.7363(10) 0.045(5) Uani 0.50 1 d PD D 2 C61C C 0.4311(11) 0.2332(7) 0.7456(8) 0.041(4) Uani 0.50 1 d PD D 2 H61C H 0.4382 0.1978 0.7257 0.049 Uiso 0.50 1 calc PR D 2 C62C C 0.4941(11) 0.2728(12) 0.7878(7) 0.076(8) Uani 0.50 1 d PD D 2 H62C H 0.5518 0.2737 0.7968 0.092 Uiso 0.50 1 calc PR D 2 C63C C 0.4588(15) 0.3105(14) 0.8142(8) 0.035(4) Uani 0.50 1 d PD D 2 C64C C 0.4916(10) 0.3562(9) 0.8632(5) 0.039(3) Uani 0.50 1 d PGD D 2 C65C C 0.5757(10) 0.3732(9) 0.8917(6) 0.040(3) Uani 0.50 1 d PG D 2 H65C H 0.6142 0.3553 0.8796 0.048 Uiso 0.50 1 calc PR D 2 C66C C 0.6035(9) 0.4163(9) 0.9379(6) 0.050(3) Uani 0.50 1 d PG D 2 H66C H 0.6610 0.4279 0.9574 0.059 Uiso 0.50 1 calc PR D 2 C67C C 0.5473(11) 0.4424(8) 0.9556(5) 0.049(4) Uani 0.50 1 d PGD D 2 C68C C 0.4632(11) 0.4254(9) 0.9270(6) 0.041(3) Uani 0.50 1 d PG D 2 H68C H 0.4247 0.4433 0.9391 0.050 Uiso 0.50 1 calc PR D 2 C69C C 0.4353(9) 0.3823(9) 0.8808(5) 0.038(3) Uani 0.50 1 d PG D 2 H69C H 0.3779 0.3707 0.8613 0.045 Uiso 0.50 1 calc PR D 2 F70C F 0.5807(17) 0.4866(12) 0.9983(8) 0.064(3) Uani 0.50 1 d PD D 2 N15A N 0.16236(18) 0.40520(14) 0.71776(12) 0.0376(6) Uani 1 1 d . D . H15A H 0.2051 0.3906 0.7328 0.045 Uiso 1 1 calc R . . N16A N 0.10354(18) 0.37549(15) 0.67283(12) 0.0395(7) Uani 1 1 d . . . C71A C 0.0516(2) 0.4132(2) 0.66274(17) 0.0463(9) Uani 1 1 d . D . H71A H 0.0039 0.4046 0.6331 0.056 Uiso 1 1 calc R . . C72A C 0.0765(2) 0.4667(2) 0.70127(17) 0.0465(9) Uani 1 1 d . . . H72A H 0.0501 0.5007 0.7029 0.056 Uiso 1 1 calc R D . C73A C 0.1481(2) 0.45989(18) 0.73687(15) 0.0416(8) Uani 1 1 d D D . C74A C 0.2072(13) 0.4993(9) 0.7862(6) 0.034(4) Uani 0.50 1 d PGD D 1 C75A C 0.1748(10) 0.5431(11) 0.8092(8) 0.049(5) Uani 0.50 1 d PG D 1 H75A H 0.1199 0.5459 0.7931 0.059 Uiso 0.50 1 calc PR D 1 C76A C 0.2228(11) 0.5828(11) 0.8557(8) 0.067(6) Uani 0.50 1 d PG D 1 H76A H 0.2007 0.6127 0.8714 0.081 Uiso 0.50 1 calc PR D 1 C77A C 0.3031(10) 0.5787(8) 0.8792(5) 0.100(10) Uani 0.50 1 d PGD D 1 C78A C 0.3355(9) 0.5350(7) 0.8562(7) 0.056(5) Uani 0.50 1 d PG D 1 H78A H 0.3904 0.5322 0.8723 0.068 Uiso 0.50 1 calc PR D 1 C79A C 0.2875(13) 0.4953(8) 0.8097(7) 0.049(5) Uani 0.50 1 d PG D 1 H79A H 0.3096 0.4654 0.7940 0.059 Uiso 0.50 1 calc PR D 1 F80A F 0.3518(18) 0.6170(16) 0.9229(9) 0.109(8) Uani 0.50 1 d PD D 1 C74C C 0.1959(15) 0.5022(10) 0.7851(6) 0.051(6) Uani 0.50 1 d PGD D 2 C75C C 0.1635(10) 0.5406(11) 0.8136(9) 0.055(5) Uani 0.50 1 d PG D 2 H75C H 0.1072 0.5422 0.8005 0.066 Uiso 0.50 1 calc PR D 2 C76C C 0.2133(10) 0.5767(10) 0.8613(8) 0.064(6) Uani 0.50 1 d PG D 2 H76C H 0.1911 0.6030 0.8808 0.077 Uiso 0.50 1 calc PR D 2 C77C C 0.2956(10) 0.5744(8) 0.8805(5) 0.060(6) Uani 0.50 1 d PGD D 2 C78C C 0.3281(9) 0.5360(9) 0.8520(7) 0.090(9) Uani 0.50 1 d PG D 2 H78C H 0.3844 0.5344 0.8651 0.108 Uiso 0.50 1 calc PR D 2 C79C C 0.2783(15) 0.4999(11) 0.8043(7) 0.053(5) Uani 0.50 1 d PG D 2 H79C H 0.3005 0.4737 0.7849 0.064 Uiso 0.50 1 calc PR D 2 F80C F 0.3404(18) 0.6087(16) 0.9269(9) 0.109(8) Uani 0.50 1 d PD D 2 N17A N 0.0801(2) 0.07852(15) 0.62768(13) 0.0434(7) Uani 1 1 d . D . H17A H 0.1282 0.0958 0.6517 0.052 Uiso 1 1 calc R . . N18A N 0.0143(2) 0.10413(15) 0.61945(13) 0.0431(7) Uani 1 1 d . . . C81A C -0.0451(3) 0.06373(19) 0.58106(15) 0.0464(9) Uani 1 1 d . D . H81A H -0.0991 0.0693 0.5668 0.056 Uiso 1 1 calc R . . C82A C -0.0189(3) 0.0125(2) 0.56436(16) 0.0476(9) Uani 1 1 d . . . H82A H -0.0506 -0.0230 0.5377 0.057 Uiso 1 1 calc R D . C83A C 0.0632(2) 0.02324(17) 0.59453(14) 0.0405(8) Uani 1 1 d . D . C84A C 0.1234(3) -0.01403(18) 0.59284(15) 0.0425(8) Uani 1 1 d . . . C85A C 0.2055(3) 0.00561(19) 0.62448(16) 0.0466(9) Uani 1 1 d . D . H85A H 0.2236 0.0440 0.6492 0.056 Uiso 1 1 calc R . . C86A C 0.2612(3) -0.0293(2) 0.62088(17) 0.0515(10) Uani 1 1 d . . . H86A H 0.3173 -0.0155 0.6427 0.062 Uiso 1 1 calc R D . C87A C 0.2336(3) -0.0853(2) 0.58454(18) 0.0529(10) Uani 1 1 d . D . C88A C 0.1535(3) -0.10695(19) 0.55297(16) 0.0513(10) Uani 1 1 d . . . H88A H 0.1362 -0.1454 0.5284 0.062 Uiso 1 1 calc R D . C89A C 0.0977(3) -0.07161(18) 0.55747(16) 0.0474(9) Uani 1 1 d . D . H89A H 0.0411 -0.0867 0.5363 0.057 Uiso 1 1 calc R . . F90A F 0.28896(18) -0.11931(13) 0.58006(11) 0.0645(7) Uani 1 1 d . . . Cu1B Cu 0.21134(3) 0.33073(2) 0.207584(18) 0.04158(10) Uani 1 1 d . . . Cu2B Cu 0.25577(3) 0.24961(2) 0.338259(19) 0.04464(11) Uani 1 1 d . F . Cu3B Cu 0.11603(3) 0.32688(2) 0.346093(19) 0.04007(10) Uani 1 1 d . F . Cu4B Cu 0.25079(3) 0.44417(2) 0.305088(18) 0.03996(10) Uani 1 1 d . F . F1B F 0.21378(12) 0.33282(10) 0.29564(8) 0.0413(5) Uani 1 1 d . F . F2B F 0.12711(13) 0.24279(11) 0.20524(9) 0.0478(5) Uani 1 1 d . . . F3B F 0.36514(13) 0.29989(13) 0.32834(9) 0.0537(6) Uani 1 1 d . . . N1B N 0.26678(19) 0.29854(16) 0.40752(13) 0.0428(7) Uani 1 1 d . . . N2B N 0.21312(19) 0.33558(16) 0.40776(13) 0.0429(7) Uani 1 1 d . F . C1B C 0.2319(2) 0.3665(2) 0.45638(16) 0.0469(9) Uani 1 1 d . . . H1B H 0.2040 0.3958 0.4669 0.056 Uiso 1 1 calc R F . C2B C 0.2985(3) 0.3494(2) 0.48945(17) 0.0498(9) Uani 1 1 d . F . H2B H 0.3243 0.3638 0.5260 0.060 Uiso 1 1 calc R . . C3B C 0.3188(2) 0.30621(19) 0.45674(15) 0.0431(8) Uani 1 1 d . F . C4B C 0.3848(2) 0.2731(2) 0.47020(16) 0.0436(8) Uani 1 1 d . . . C5B C 0.3767(3) 0.2124(2) 0.44399(17) 0.0504(10) Uani 1 1 d . . . H5B H 0.3262 0.1908 0.4178 0.060 Uiso 1 1 calc R . . C6B C 0.4415(3) 0.1826(2) 0.4555(2) 0.0596(11) Uani 1 1 d . . . H6B H 0.4366 0.1417 0.4369 0.072 Uiso 1 1 calc R F . C7B C 0.5129(3) 0.2146(3) 0.4947(2) 0.0657(13) Uani 1 1 d . . . C8B C 0.5226(3) 0.2734(3) 0.5230(2) 0.0678(14) Uani 1 1 d . . . H8B H 0.5721 0.2936 0.5505 0.081 Uiso 1 1 calc R F . C9B C 0.4576(3) 0.3021(2) 0.51000(18) 0.0540(10) Uani 1 1 d . . . H9B H 0.4631 0.3430 0.5289 0.065 Uiso 1 1 calc R . . F10B F 0.5772(2) 0.18657(18) 0.50588(16) 0.1004(12) Uani 1 1 d . . . N3B N 0.08517(19) 0.22804(15) 0.34581(13) 0.0422(7) Uani 1 1 d . . . N4B N 0.1412(2) 0.19614(16) 0.33764(14) 0.0469(8) Uani 1 1 d . F . C11B C 0.0999(3) 0.1298(2) 0.32967(18) 0.0535(10) Uani 1 1 d . . . H11F H 0.1244 0.0959 0.3236 0.064 Uiso 1 1 calc R F . C12B C 0.0171(3) 0.1184(2) 0.33170(19) 0.0547(10) Uani 1 1 d . F . H12B H -0.0258 0.0766 0.3269 0.066 Uiso 1 1 calc R . . C13B C 0.0098(3) 0.1816(2) 0.34238(16) 0.0464(9) Uani 1 1 d . F . C14B C -0.0625(2) 0.20155(19) 0.34950(17) 0.0454(9) Uani 1 1 d . . . C15B C -0.0543(3) 0.2491(2) 0.39065(17) 0.0505(10) Uani 1 1 d . . . H15F H -0.0005 0.2685 0.4146 0.061 Uiso 1 1 calc R . . C16B C -0.1227(3) 0.2683(2) 0.3971(2) 0.0569(11) Uani 1 1 d . . . H16B H -0.1169 0.3004 0.4250 0.068 Uiso 1 1 calc R F . C17B C -0.1989(3) 0.2395(2) 0.3617(2) 0.0626(12) Uani 1 1 d . . . C18B C -0.2111(3) 0.1929(2) 0.3212(2) 0.0621(12) Uani 1 1 d . . . H18B H -0.2654 0.1738 0.2978 0.075 Uiso 1 1 calc R F . C19B C -0.1424(3) 0.1741(2) 0.31494(19) 0.0541(10) Uani 1 1 d . . . H19B H -0.1495 0.1420 0.2867 0.065 Uiso 1 1 calc R . . F20B F -0.26713(18) 0.25803(14) 0.36834(15) 0.0809(9) Uani 1 1 d . . . N5B N 0.18265(19) 0.47172(15) 0.34889(12) 0.0410(7) Uani 1 1 d . . . N6B N 0.1225(2) 0.42134(15) 0.36256(13) 0.0422(7) Uani 1 1 d . F . C21B C 0.0811(2) 0.4485(2) 0.39030(16) 0.0475(9) Uani 1 1 d . . . H21B H 0.0360 0.4241 0.4047 0.057 Uiso 1 1 calc R F . C22B C 0.1139(3) 0.5172(2) 0.39474(16) 0.0474(9) Uani 1 1 d . F . H22B H 0.0968 0.5488 0.4125 0.057 Uiso 1 1 calc R . . C23B C 0.1776(2) 0.53038(19) 0.36764(15) 0.0426(8) Uani 1 1 d . F . C24B C 0.2309(2) 0.5964(2) 0.35747(16) 0.0472(9) Uani 1 1 d . . . C25B C 0.2353(3) 0.6545(2) 0.38641(19) 0.0546(11) Uani 1 1 d . . . H25B H 0.2034 0.6511 0.4124 0.066 Uiso 1 1 calc R . . C26B C 0.2844(3) 0.7165(2) 0.3784(2) 0.0634(13) Uani 1 1 d . . . H26B H 0.2860 0.7556 0.3980 0.076 Uiso 1 1 calc R F . C27B C 0.3302(3) 0.7203(2) 0.3418(2) 0.0651(13) Uani 1 1 d . . . C28B C 0.3287(3) 0.6655(2) 0.3111(2) 0.0673(13) Uani 1 1 d . . . H28B H 0.3615 0.6701 0.2855 0.081 Uiso 1 1 calc R F . C29B C 0.2774(3) 0.6034(2) 0.31905(19) 0.0601(11) Uiso 1 1 d . . . H29B H 0.2740 0.5649 0.2978 0.072 Uiso 1 1 calc R . . F30B F 0.3811(2) 0.78141(14) 0.33348(15) 0.0875(10) Uani 1 1 d . . . N7B N 0.13346(19) 0.38668(16) 0.19943(12) 0.0427(7) Uani 1 1 d . F . N8B N 0.15199(19) 0.43259(16) 0.24136(13) 0.0418(7) Uani 1 1 d . . . C31B C 0.0992(3) 0.4703(2) 0.22997(17) 0.0501(9) Uani 1 1 d . . . H31B H 0.0986 0.5058 0.2528 0.060 Uiso 1 1 calc R . . C32B C 0.0461(3) 0.4492(2) 0.17983(18) 0.0557(11) Uani 1 1 d . . . H32B H 0.0028 0.4670 0.1617 0.067 Uiso 1 1 calc R F . C33B C 0.0694(2) 0.3960(2) 0.16126(16) 0.0467(9) Uani 1 1 d . F . C34B C 0.0342(3) 0.3568(3) 0.10893(18) 0.0608(12) Uani 1 1 d . . . C35B C 0.0479(3) 0.2961(3) 0.09884(19) 0.0649(12) Uani 1 1 d . . . H35B H 0.0804 0.2780 0.1265 0.078 Uiso 1 1 calc R . . C36B C 0.0142(4) 0.2615(3) 0.0484(2) 0.0838(17) Uani 1 1 d . . . H36B H 0.0241 0.2203 0.0412 0.101 Uiso 1 1 calc R F . C37B C -0.0330(5) 0.2878(4) 0.0098(2) 0.108(2) Uani 1 1 d . . . C38B C -0.0486(6) 0.3471(4) 0.0177(3) 0.121(3) Uani 1 1 d . . . H38B H -0.0816 0.3644 -0.0103 0.145 Uiso 1 1 calc R F . C39B C -0.0148(4) 0.3814(3) 0.0679(2) 0.092(2) Uani 1 1 d . . . H39B H -0.0253 0.4226 0.0744 0.110 Uiso 1 1 calc R . . F40B F -0.0670(4) 0.2529(3) -0.03940(16) 0.164(2) Uani 1 1 d . . . N9B N 0.30546(19) 0.41482(16) 0.21152(13) 0.0423(7) Uani 1 1 d . E . N10B N 0.32938(19) 0.45330(16) 0.25843(13) 0.0439(7) Uani 1 1 d . . . C41B C 0.4034(3) 0.4992(2) 0.25996(18) 0.0524(10) Uani 1 1 d . . . H41B H 0.4341 0.5325 0.2885 0.063 Uiso 1 1 calc R . . C42B C 0.4287(3) 0.4912(2) 0.21397(18) 0.0552(11) Uani 1 1 d . . . H42B H 0.4787 0.5167 0.2049 0.066 Uiso 1 1 calc R F . C43B C 0.3645(3) 0.4373(2) 0.18365(15) 0.0480(9) Uani 1 1 d D E . C44B C 0.3538(12) 0.3995(7) 0.1324(3) 0.040(3) Uani 0.50 1 d PGD E 1 C45B C 0.2752(10) 0.3876(9) 0.0968(6) 0.064(6) Uani 0.50 1 d PG E 1 H45B H 0.2293 0.3946 0.1086 0.077 Uiso 0.50 1 calc PR E 1 C46B C 0.2636(11) 0.3657(8) 0.0438(5) 0.066(6) Uani 0.50 1 d PG E 1 H46B H 0.2098 0.3576 0.0195 0.080 Uiso 0.50 1 calc PR E 1 C47B C 0.3306(15) 0.3555(9) 0.0265(3) 0.073(6) Uani 0.50 1 d PGD E 1 C48B C 0.4092(12) 0.3673(11) 0.0621(6) 0.065(6) Uani 0.50 1 d PG E 1 H48B H 0.4550 0.3603 0.0503 0.078 Uiso 0.50 1 calc PR E 1 C49B C 0.4208(10) 0.3893(9) 0.1151(5) 0.067(6) Uani 0.50 1 d PG E 1 H49B H 0.4746 0.3974 0.1394 0.081 Uiso 0.50 1 calc PR E 1 F50B F 0.320(2) 0.3271(12) -0.0227(6) 0.078(4) Uani 0.50 1 d PD E 1 C44D C 0.3550(11) 0.4157(6) 0.1280(3) 0.038(3) Uani 0.50 1 d PGD E 2 C45D C 0.2783(9) 0.3957(9) 0.0898(6) 0.045(3) Uani 0.50 1 d PG E 2 H45D H 0.2299 0.4043 0.0968 0.053 Uiso 0.50 1 calc PR E 2 C46D C 0.2724(10) 0.3632(9) 0.0412(5) 0.071(7) Uani 0.50 1 d PG E 2 H46D H 0.2200 0.3496 0.0151 0.085 Uiso 0.50 1 calc PR E 2 C47D C 0.3433(13) 0.3507(9) 0.0309(4) 0.068(6) Uani 0.50 1 d PGD E 2 C48D C 0.4200(10) 0.3707(12) 0.0691(7) 0.096(10) Uani 0.50 1 d PG E 2 H48D H 0.4684 0.3622 0.0620 0.116 Uiso 0.50 1 calc PR E 2 C49D C 0.4259(9) 0.4032(10) 0.1176(5) 0.056(4) Uani 0.50 1 d PG E 2 H49D H 0.4783 0.4169 0.1437 0.068 Uiso 0.50 1 calc PR E 2 F50D F 0.340(2) 0.3257(18) -0.0177(7) 0.123(12) Uani 0.50 1 d PD E 2 N11B N 0.3589(5) 0.2909(4) 0.2197(3) 0.0403(18) Uani 0.50 1 d PD F 1 H11B H 0.3796 0.3109 0.2522 0.048 Uiso 0.50 1 calc PR F 1 N12B N 0.2788(11) 0.2832(15) 0.1925(8) 0.043(4) Uani 0.50 1 d PD F 1 C51B C 0.2780(10) 0.2485(9) 0.1487(8) 0.056(7) Uani 0.50 1 d PD F 1 H51B H 0.2282 0.2329 0.1206 0.067 Uiso 0.50 1 calc PR F 1 C52B C 0.3525(8) 0.2362(7) 0.1459(4) 0.060(4) Uani 0.50 1 d PD F 1 H52B H 0.3640 0.2132 0.1180 0.072 Uiso 0.50 1 calc PR F 1 C53B C 0.4055(4) 0.2660(4) 0.1942(3) 0.0504(19) Uani 0.50 1 d PD F 1 C54B C 0.4963(4) 0.2780(4) 0.2161(3) 0.0498(19) Uani 0.50 1 d PD F 1 C55B C 0.5475(6) 0.2704(6) 0.1828(4) 0.083(4) Uani 0.50 1 d PD F 1 H55B H 0.5238 0.2587 0.1457 0.100 Uiso 0.50 1 calc PR F 1 C56B C 0.6317(8) 0.2801(13) 0.2041(7) 0.071(8) Uani 0.50 1 d PD F 1 H56B H 0.6638 0.2640 0.1845 0.085 Uiso 0.50 1 calc PR F 1 C57B C 0.6705(4) 0.3135(5) 0.2545(3) 0.051(2) Uani 0.50 1 d PD F 1 C58B C 0.6204(5) 0.3174(5) 0.2882(4) 0.067(3) Uani 0.50 1 d PD F 1 H58B H 0.6451 0.3310 0.3250 0.081 Uiso 0.50 1 calc PR F 1 C59B C 0.5340(5) 0.3013(5) 0.2683(3) 0.059(2) Uani 0.50 1 d PD F 1 H59B H 0.5000 0.3066 0.2914 0.071 Uiso 0.50 1 calc PR F 1 F60B F 0.7539(3) 0.3290(3) 0.2737(2) 0.0741(16) Uani 0.50 1 d PD F 1 N11D N 0.3515(6) 0.2599(4) 0.2279(4) 0.042(2) Uani 0.50 1 d PD F 2 H11D H 0.3703 0.2759 0.2616 0.051 Uiso 0.50 1 calc PR F 2 N12D N 0.2901(13) 0.2754(14) 0.1919(6) 0.033(3) Uani 0.50 1 d PD F 2 C51D C 0.2787(11) 0.2433(10) 0.1445(6) 0.048(6) Uani 0.50 1 d PD F 2 H51D H 0.2396 0.2456 0.1122 0.058 Uiso 0.50 1 calc PR F 2 C52D C 0.3352(8) 0.2060(6) 0.1517(4) 0.053(3) Uani 0.50 1 d PD F 2 H52D H 0.3422 0.1783 0.1249 0.063 Uiso 0.50 1 calc PR F 2 C53D C 0.3796(4) 0.2161(4) 0.2045(3) 0.0403(16) Uani 0.50 1 d PD F 2 C54D C 0.4397(4) 0.1839(3) 0.2348(3) 0.0440(17) Uani 0.50 1 d PD F 2 C55D C 0.4528(6) 0.1302(5) 0.2092(3) 0.062(2) Uani 0.50 1 d PD F 2 H55D H 0.4264 0.1176 0.1724 0.074 Uiso 0.50 1 calc PR F 2 C56D C 0.5045(5) 0.0950(5) 0.2376(4) 0.062(2) Uani 0.50 1 d PD F 2 H56D H 0.5148 0.0591 0.2204 0.074 Uiso 0.50 1 calc PR F 2 C57D C 0.5397(4) 0.1132(4) 0.2904(4) 0.059(2) Uani 0.50 1 d PD F 2 C58D C 0.5311(5) 0.1654(4) 0.3168(4) 0.061(2) Uani 0.50 1 d PD F 2 H58D H 0.5588 0.1774 0.3535 0.073 Uiso 0.50 1 calc PR F 2 C59D C 0.4796(5) 0.2014(4) 0.2882(3) 0.0495(19) Uani 0.50 1 d PD F 2 H59D H 0.4722 0.2384 0.3059 0.059 Uiso 0.50 1 calc PR F 2 F60D F 0.5897(4) 0.0780(3) 0.3162(3) 0.093(2) Uani 0.50 1 d PD F 2 N13B N 0.215(2) 0.1562(15) 0.2441(11) 0.040(5) Uani 0.50 1 d PD F 1 H13B H 0.1713 0.1701 0.2295 0.048 Uiso 0.50 1 calc PR F 1 N14B N 0.2705(9) 0.1838(7) 0.2903(11) 0.043(4) Uani 0.50 1 d PD F 1 C61B C 0.3228(8) 0.1462(5) 0.2994(5) 0.061(3) Uani 0.50 1 d PD F 1 H61B H 0.3687 0.1528 0.3300 0.073 Uiso 0.50 1 calc PR F 1 C62B C 0.3017(10) 0.0963(6) 0.2585(6) 0.074(4) Uani 0.50 1 d PD F 1 H62B H 0.3291 0.0632 0.2559 0.088 Uiso 0.50 1 calc PR F 1 C63B C 0.2327(12) 0.1048(9) 0.2224(6) 0.053(6) Uani 0.50 1 d PD F 1 C64B C 0.1875(13) 0.0681(10) 0.1701(6) 0.057(6) Uani 0.50 1 d PGD F 1 C65B C 0.1214(13) 0.0882(7) 0.1396(6) 0.057(5) Uani 0.50 1 d PG F 1 H65B H 0.1084 0.1259 0.1521 0.069 Uiso 0.50 1 calc PR F 1 C66B C 0.0743(10) 0.0533(7) 0.0910(5) 0.063(4) Uani 0.50 1 d PG F 1 H66B H 0.0291 0.0671 0.0702 0.075 Uiso 0.50 1 calc PR F 1 C67B C 0.0932(10) -0.0018(7) 0.0727(4) 0.067(5) Uani 0.50 1 d PGD F 1 C68B C 0.1593(13) -0.0219(9) 0.1032(6) 0.095(8) Uani 0.50 1 d PG F 1 H68B H 0.1723 -0.0596 0.0907 0.114 Uiso 0.50 1 calc PR F 1 C69B C 0.2064(12) 0.0130(12) 0.1518(7) 0.087(7) Uani 0.50 1 d PG F 1 H69B H 0.2516 -0.0008 0.1727 0.104 Uiso 0.50 1 calc PR F 1 F70B F 0.0534(12) -0.0393(10) 0.0265(6) 0.117(7) Uani 0.50 1 d PD F 1 N13D N 0.204(3) 0.1481(15) 0.2413(11) 0.045(6) Uani 0.50 1 d PD F 2 H13D H 0.1709 0.1700 0.2232 0.054 Uiso 0.50 1 calc PR F 2 N14D N 0.2524(9) 0.1668(7) 0.2912(10) 0.037(3) Uani 0.50 1 d PD F 2 C61D C 0.2940(6) 0.1219(5) 0.3045(4) 0.040(2) Uani 0.50 1 d PD F 2 H61D H 0.3331 0.1231 0.3376 0.047 Uiso 0.50 1 calc PR F 2 C62D C 0.2713(7) 0.0730(5) 0.2624(4) 0.043(2) Uani 0.50 1 d PD F 2 H62D H 0.2915 0.0354 0.2610 0.052 Uiso 0.50 1 calc PR F 2 C63D C 0.2131(11) 0.0908(9) 0.2230(5) 0.041(4) Uani 0.50 1 d PD F 2 C64D C 0.1683(14) 0.0588(11) 0.1690(6) 0.044(4) Uani 0.50 1 d PGD F 2 C65D C 0.1106(14) 0.0804(9) 0.1315(7) 0.069(5) Uani 0.50 1 d PG F 2 H65D H 0.0974 0.1199 0.1397 0.083 Uiso 0.50 1 calc PR F 2 C66D C 0.0721(13) 0.0444(10) 0.0822(6) 0.130(10) Uani 0.50 1 d PG F 2 H66D H 0.0327 0.0592 0.0565 0.156 Uiso 0.50 1 calc PR F 2 C67D C 0.0913(15) -0.0134(10) 0.0703(6) 0.156(14) Uani 0.50 1 d PGD F 2 C68D C 0.1490(18) -0.0351(11) 0.1078(8) 0.128(11) Uani 0.50 1 d PG F 2 H68D H 0.1622 -0.0746 0.0996 0.154 Uiso 0.50 1 calc PR F 2 C69D C 0.1875(15) 0.0010(12) 0.1571(7) 0.096(8) Uani 0.50 1 d PG F 2 H69D H 0.2269 -0.0138 0.1828 0.115 Uiso 0.50 1 calc PR F 2 F70D F 0.0522(17) -0.0452(13) 0.0218(7) 0.180(11) Uani 0.50 1 d PD F 2 N15B N 0.0033(2) 0.26991(16) 0.24094(14) 0.0453(7) Uani 1 1 d . F . H15B H 0.0392 0.2486 0.2368 0.054 Uiso 1 1 calc R . . N16B N 0.01853(19) 0.31632(16) 0.28162(13) 0.0442(7) Uani 1 1 d . . . C71B C -0.0506(3) 0.3355(2) 0.27387(18) 0.0502(9) Uani 1 1 d . F . H71B H -0.0586 0.3680 0.2964 0.060 Uiso 1 1 calc R . . C72B C -0.1098(3) 0.3015(2) 0.22830(18) 0.0540(10) Uani 1 1 d . . . H72B H -0.1645 0.3059 0.2143 0.065 Uiso 1 1 calc R F . C73B C -0.0731(2) 0.2600(2) 0.20760(16) 0.0503(10) Uani 1 1 d D F . C74B C -0.1071(18) 0.2056(11) 0.1651(8) 0.063(7) Uani 0.50 1 d PGD F 1 C75B C -0.0792(16) 0.1493(12) 0.1665(8) 0.119(12) Uani 0.50 1 d PG F 1 H75B H -0.0384 0.1439 0.1969 0.142 Uiso 0.50 1 calc PR F 1 C76B C -0.1111(17) 0.1009(9) 0.1236(11) 0.156(16) Uani 0.50 1 d PG F 1 H76B H -0.0920 0.0624 0.1246 0.187 Uiso 0.50 1 calc PR F 1 C77B C -0.1708(17) 0.1087(11) 0.0792(8) 0.154(14) Uani 0.50 1 d PGD F 1 C78B C -0.1987(14) 0.1650(12) 0.0778(8) 0.145(14) Uani 0.50 1 d PG F 1 H78B H -0.2395 0.1704 0.0475 0.174 Uiso 0.50 1 calc PR F 1 C79B C -0.1669(17) 0.2134(10) 0.1208(10) 0.092(10) Uani 0.50 1 d PG F 1 H79B H -0.1859 0.2519 0.1198 0.110 Uiso 0.50 1 calc PR F 1 F80B F -0.203(3) 0.0630(18) 0.0377(12) 0.203(19) Uani 0.50 1 d PD F 1 C74D C -0.1032(15) 0.2147(10) 0.1589(6) 0.054(5) Uani 0.50 1 d PGD F 2 C75D C -0.0719(13) 0.1604(9) 0.1580(5) 0.058(4) Uani 0.50 1 d PG F 2 H75D H -0.0309 0.1544 0.1880 0.069 Uiso 0.50 1 calc PR F 2 C76D C -0.1004(11) 0.1148(7) 0.1133(7) 0.074(4) Uani 0.50 1 d PG F 2 H76D H -0.0790 0.0778 0.1126 0.089 Uiso 0.50 1 calc PR F 2 C77D C -0.1603(11) 0.1236(9) 0.0694(6) 0.085(5) Uani 0.50 1 d PGD F 2 C78D C -0.1917(10) 0.1778(9) 0.0703(6) 0.081(5) Uani 0.50 1 d PG F 2 H78D H -0.2326 0.1838 0.0403 0.097 Uiso 0.50 1 calc PR F 2 C79D C -0.1631(12) 0.2234(8) 0.1150(8) 0.065(5) Uani 0.50 1 d PG F 2 H79D H -0.1846 0.2605 0.1156 0.077 Uiso 0.50 1 calc PR F 2 F80D F -0.188(2) 0.0805(15) 0.0261(9) 0.131(6) Uani 0.50 1 d PD F 2 N17B N 0.40685(18) 0.42268(17) 0.37387(12) 0.0422(7) Uani 1 1 d . F . H17B H 0.3969 0.3845 0.3552 0.051 Uiso 1 1 calc R . . N18B N 0.3521(2) 0.45968(18) 0.36815(13) 0.0466(8) Uani 1 1 d . . . C81B C 0.3908(2) 0.5132(2) 0.40301(16) 0.0469(9) Uani 1 1 d . F . H81B H 0.3674 0.5482 0.4081 0.056 Uiso 1 1 calc R . . C82B C 0.4702(3) 0.5107(2) 0.43090(16) 0.0486(9) Uani 1 1 d . . . H82B H 0.5106 0.5428 0.4576 0.058 Uiso 1 1 calc R F . C83B C 0.4778(2) 0.4517(2) 0.41148(15) 0.0415(8) Uani 1 1 d . F . C84B C 0.5483(2) 0.42249(19) 0.42786(15) 0.0423(8) Uani 1 1 d . . . C85B C 0.5455(3) 0.3611(2) 0.40567(18) 0.0512(10) Uani 1 1 d . F . H85B H 0.4977 0.3374 0.3783 0.061 Uiso 1 1 calc R . . C86B C 0.6113(3) 0.3336(2) 0.4227(2) 0.0582(11) Uani 1 1 d . . . H86B H 0.6092 0.2916 0.4074 0.070 Uiso 1 1 calc R F . C87B C 0.6792(3) 0.3691(2) 0.46234(18) 0.0528(10) Uani 1 1 d . F . C88B C 0.6855(2) 0.4299(2) 0.48505(16) 0.0519(10) Uani 1 1 d . . . H88B H 0.7339 0.4533 0.5123 0.062 Uiso 1 1 calc R F . C89B C 0.6199(2) 0.4567(2) 0.46748(16) 0.0475(9) Uani 1 1 d . F . H89B H 0.6236 0.4993 0.4827 0.057 Uiso 1 1 calc R . . F90B F 0.74399(15) 0.34195(14) 0.47987(11) 0.0656(7) Uani 1 1 d . . . N1E N 0.7988(8) 0.1832(7) 0.8440(5) 0.074(4) Uiso 0.30 1 d PD G 3 H1E H 0.7763 0.1987 0.8669 0.089 Uiso 0.30 1 calc PR G 3 N2E N 0.8824(9) 0.1901(10) 0.8512(6) 0.078(6) Uiso 0.30 1 d PD G 3 C3E C 0.8884(9) 0.1665(8) 0.8051(5) 0.046(4) Uiso 0.30 1 d PD G 3 H3E H 0.9405 0.1728 0.7956 0.055 Uiso 0.30 1 calc PR G 3 C4E C 0.8116(8) 0.1320(7) 0.7725(5) 0.050(3) Uiso 0.30 1 d PD G 3 H4E H 0.7997 0.1034 0.7410 0.060 Uiso 0.30 1 calc PR G 3 C5E C 0.7558(5) 0.1492(7) 0.7967(5) 0.055(3) Uiso 0.30 1 d PD G 3 C6E C 0.6633(3) 0.1204(4) 0.7758(3) 0.053(3) Uiso 0.30 1 d PGD G 3 C7E C 0.6305(4) 0.0940(4) 0.7229(3) 0.054(3) Uiso 0.30 1 d PG G 3 H7E H 0.6675 0.0904 0.7015 0.065 Uiso 0.30 1 calc PR G 3 C8E C 0.5436(4) 0.0729(3) 0.7015(2) 0.054(3) Uiso 0.30 1 d PG G 3 H8E H 0.5212 0.0548 0.6654 0.065 Uiso 0.30 1 calc PR G 3 C9E C 0.4895(3) 0.0782(3) 0.7329(2) 0.034(2) Uiso 0.30 1 d PGD G 3 C10E C 0.5222(3) 0.1046(3) 0.7857(2) 0.063(4) Uiso 0.30 1 d PG G 3 H10E H 0.4852 0.1082 0.8072 0.076 Uiso 0.30 1 calc PR G 3 C11E C 0.6092(3) 0.1257(3) 0.8072(2) 0.068(4) Uiso 0.30 1 d PG G 3 H11C H 0.6316 0.1438 0.8433 0.081 Uiso 0.30 1 calc PR G 3 F12E F 0.4076(3) 0.0642(4) 0.7112(3) 0.075(3) Uiso 0.30 1 d PGD G 3 N13E N 0.6762(9) 0.2738(7) 0.9869(4) 0.074(6) Uiso 0.20 1 d PGD G 3 H13E H 0.6779 0.3061 1.0096 0.088 Uiso 0.20 1 calc PR G 3 N14E N 0.7263(14) 0.2732(11) 0.9543(9) 0.089(7) Uiso 0.20 1 d PD G 3 C15E C 0.7165(13) 0.2124(9) 0.9334(10) 0.065(6) Uiso 0.20 1 d PD G 3 H15G H 0.7508 0.2006 0.9132 0.078 Uiso 0.20 1 calc PR G 3 C16E C 0.6474(11) 0.1694(8) 0.9467(7) 0.046(4) Uiso 0.20 1 d PD G 3 H16E H 0.6229 0.1226 0.9380 0.055 Uiso 0.20 1 calc PR G 3 C17E C 0.6232(11) 0.2122(7) 0.9758(8) 0.063(6) Uiso 0.20 1 d PD G 3 C18E C 0.5534(6) 0.1801(5) 1.0000(4) 0.062(6) Uiso 0.20 1 d PGD G 3 C19E C 0.5095(6) 0.2209(4) 1.0147(3) 0.062(6) Uiso 0.20 1 d PG G 3 H19E H 0.5280 0.2677 1.0116 0.074 Uiso 0.20 1 calc PR G 3 C20E C 0.4387(8) 0.1931(5) 1.0341(5) 0.091(9) Uiso 0.20 1 d PG G 3 H20E H 0.4087 0.2210 1.0442 0.109 Uiso 0.20 1 calc PR G 3 C21E C 0.4117(6) 0.1245(5) 1.0386(4) 0.072(7) Uiso 0.20 1 d PGD G 3 C22E C 0.4556(8) 0.0837(4) 1.0238(6) 0.084(8) Uiso 0.20 1 d PG G 3 H22E H 0.4371 0.0369 1.0269 0.100 Uiso 0.20 1 calc PR G 3 C23E C 0.5265(9) 0.1115(5) 1.0045(7) 0.108(11) Uiso 0.20 1 d PG G 3 H23E H 0.5565 0.0836 0.9944 0.130 Uiso 0.20 1 calc PR G 3 F24E F 0.3532(7) 0.0835(5) 1.0572(5) 0.106(6) Uiso 0.20 1 d PGD G 3 C1S C 0.7651(4) 0.4455(3) 0.8471(2) 0.0836(16) Uani 1 1 d G . . H1S1 H 0.7940 0.4767 0.8242 0.100 Uiso 1 1 calc R . . H1S2 H 0.7078 0.4499 0.8429 0.100 Uiso 1 1 calc R . . Cl2S Cl 0.82202(10) 0.46527(8) 0.91375(6) 0.0867(4) Uani 1 1 d . . . Cl3S Cl 0.75792(11) 0.36112(11) 0.82752(8) 0.1111(6) Uani 1 1 d . . . C4S C 0.6476(11) 0.3371(9) 0.2504(7) 0.036(4) Uiso 0.20 1 d PD H 3 H4S1 H 0.7004 0.3736 0.2522 0.043 Uiso 0.20 1 calc PR H 3 H4S2 H 0.6568 0.3131 0.2830 0.043 Uiso 0.20 1 calc PR H 3 Cl5S Cl 0.6310(10) 0.2817(10) 0.1956(7) 0.084(5) Uiso 0.20 1 d PD H 3 Cl6S Cl 0.5648(4) 0.3745(3) 0.2516(2) 0.0483(15) Uiso 0.20 1 d PD H 3 C7S C 0.6498(17) 0.3223(18) 0.2308(11) 0.036(9) Uiso 0.10 1 d PD I 4 H7S1 H 0.6633 0.2911 0.2577 0.043 Uiso 0.10 1 calc PR I 4 H7S2 H 0.7031 0.3571 0.2303 0.043 Uiso 0.10 1 calc PR I 4 Cl8S Cl 0.6039(11) 0.2773(8) 0.1661(7) 0.080(4) Uiso 0.10 1 d PD I 4 Cl9S Cl 0.5780(8) 0.3606(6) 0.2489(5) 0.048(3) Uiso 0.10 1 d PD I 4 C10S C 0.8667(12) 0.1515(11) 0.7970(7) 0.036(5) Uiso 0.20 1 d PD J 4 H1S3 H 0.9060 0.1794 0.7776 0.043 Uiso 0.20 1 calc PR J 4 H1S4 H 0.8849 0.1117 0.8078 0.043 Uiso 0.20 1 calc PR J 4 Cl11S Cl 0.7611(8) 0.1280(6) 0.7578(4) 0.125(3) Uiso 0.20 1 d PD J 4 Cl12S Cl 0.8612(8) 0.1993(6) 0.8544(4) 0.110(4) Uiso 0.20 1 d PD J 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 Cu1A 0.0397(2) 0.0340(2) 0.0386(2) 0.00368(17) 0.00533(18) 0.00706(18) Cu2A 0.0416(2) 0.0379(2) 0.0444(3) -0.00342(19) -0.00077(19) 0.01537(19) Cu3A 0.0338(2) 0.0342(2) 0.0413(2) 0.00273(17) 0.00509(18) 0.00954(17) Cu4A 0.0407(2) 0.0343(2) 0.0385(2) 0.00262(17) 0.00330(18) 0.00955(18) F1A 0.0431(11) 0.0353(10) 0.0400(11) 0.0035(8) 0.0073(9) 0.0106(9) F2A 0.0375(10) 0.0345(10) 0.0466(12) 0.0032(9) 0.0080(9) 0.0077(8) F3A 0.0570(13) 0.0388(11) 0.0499(13) -0.0052(9) -0.0062(10) 0.0181(10) N1A 0.0413(16) 0.0388(16) 0.0430(17) -0.0004(13) 0.0047(13) 0.0139(13) N2A 0.0397(16) 0.0407(16) 0.0477(18) 0.0008(14) 0.0038(14) 0.0147(14) C1A 0.048(2) 0.042(2) 0.046(2) -0.0026(17) -0.0004(18) 0.0104(17) C2A 0.051(2) 0.042(2) 0.039(2) -0.0025(16) 0.0013(17) 0.0090(17) C3A 0.043(2) 0.0339(18) 0.043(2) 0.0011(15) 0.0076(16) 0.0067(15) C4A 0.042(2) 0.0383(19) 0.047(2) 0.0063(16) 0.0143(17) 0.0097(16) C5A 0.047(2) 0.048(2) 0.058(3) -0.0007(19) 0.0167(19) 0.0089(18) C6A 0.037(2) 0.061(3) 0.081(3) 0.008(2) 0.016(2) 0.0134(19) C7A 0.049(2) 0.059(3) 0.079(3) 0.006(2) 0.029(2) 0.023(2) C8A 0.058(3) 0.050(2) 0.073(3) -0.005(2) 0.028(2) 0.018(2) C9A 0.049(2) 0.044(2) 0.054(2) -0.0019(18) 0.0165(19) 0.0089(18) F10A 0.0636(17) 0.089(2) 0.127(3) 0.0004(19) 0.0374(18) 0.0397(16) N3A 0.0362(15) 0.0372(15) 0.0441(17) 0.0007(13) 0.0089(13) 0.0124(13) N4A 0.0360(16) 0.0417(17) 0.0509(19) 0.0005(14) 0.0050(14) 0.0139(13) C11A 0.0345(19) 0.052(2) 0.055(2) 0.0014(18) 0.0069(17) 0.0114(17) C12A 0.0359(19) 0.049(2) 0.056(2) 0.0077(18) 0.0097(17) 0.0034(17) C13A 0.0397(19) 0.0398(19) 0.0395(19) 0.0023(15) 0.0095(15) 0.0089(15) C14A 0.0345(18) 0.0431(19) 0.042(2) 0.0070(15) 0.0118(15) 0.0070(15) C15A 0.041(2) 0.0375(19) 0.050(2) 0.0045(16) 0.0070(17) 0.0039(16) C16A 0.047(2) 0.0356(19) 0.055(2) 0.0058(17) 0.0074(18) 0.0094(17) C17A 0.0370(19) 0.044(2) 0.056(2) 0.0140(18) 0.0093(17) 0.0123(16) C18A 0.041(2) 0.051(2) 0.045(2) 0.0067(17) 0.0057(17) 0.0063(17) C19A 0.0412(19) 0.0393(19) 0.043(2) 0.0010(15) 0.0108(16) 0.0047(16) F20A 0.0475(13) 0.0546(14) 0.0664(16) 0.0119(12) 0.0039(11) 0.0192(11) N5A 0.0358(15) 0.0371(15) 0.0420(17) 0.0027(13) 0.0047(13) 0.0077(13) N6A 0.0368(15) 0.0364(15) 0.0434(17) 0.0041(13) 0.0050(13) 0.0081(13) C21A 0.045(2) 0.042(2) 0.043(2) 0.0086(16) 0.0058(16) 0.0160(17) C22A 0.0393(19) 0.0409(19) 0.045(2) 0.0026(16) 0.0049(16) 0.0118(16) C23A 0.0354(18) 0.0408(19) 0.043(2) 0.0007(15) 0.0049(15) 0.0127(15) C24A 0.0377(19) 0.041(2) 0.059(2) 0.0015(17) 0.0103(17) 0.0108(16) C25A 0.039(2) 0.068(3) 0.069(3) 0.018(2) 0.005(2) 0.003(2) C26A 0.066(3) 0.069(3) 0.095(4) 0.033(3) 0.024(3) 0.010(3) C27A 0.046(2) 0.044(2) 0.103(4) 0.003(2) 0.025(3) 0.0029(19) C28A 0.037(2) 0.048(2) 0.078(3) -0.011(2) 0.011(2) 0.0098(18) C29A 0.0373(19) 0.045(2) 0.060(3) -0.0051(18) 0.0086(18) 0.0123(17) F30A 0.0597(17) 0.0569(17) 0.139(3) 0.0134(17) 0.0331(18) -0.0015(14) N7A 0.0384(16) 0.0377(15) 0.0398(16) 0.0054(13) 0.0105(13) 0.0065(13) N8A 0.0363(16) 0.0417(17) 0.0462(18) 0.0037(14) 0.0069(13) 0.0086(13) C31A 0.042(2) 0.057(2) 0.052(2) 0.0071(19) 0.0100(18) 0.0170(19) C32A 0.050(2) 0.066(3) 0.052(2) 0.002(2) 0.0144(19) 0.022(2) C33A 0.047(2) 0.044(2) 0.051(2) 0.0070(17) 0.0165(18) 0.0136(17) C34A 0.044(10) 0.035(5) 0.057(7) 0.005(5) 0.030(6) 0.025(7) C35A 0.055(7) 0.049(7) 0.065(9) -0.006(5) 0.010(6) 0.033(6) C36A 0.16(2) 0.102(16) 0.102(17) -0.010(13) 0.074(16) 0.067(16) C37A 0.13(2) 0.049(10) 0.026(8) -0.014(7) 0.024(10) 0.028(11) C38A 0.073(8) 0.052(9) 0.033(8) -0.014(7) 0.008(6) 0.020(7) C39A 0.042(8) 0.050(8) 0.055(9) -0.002(6) 0.005(6) 0.009(6) F40A 0.19(2) 0.138(17) 0.073(11) -0.041(10) 0.006(10) 0.087(11) C34C 0.030(6) 0.038(6) 0.038(5) 0.006(4) 0.016(4) 0.029(4) C35C 0.077(8) 0.064(9) 0.047(6) -0.005(6) 0.032(6) 0.051(6) C36C 0.076(10) 0.072(9) 0.034(6) -0.007(6) 0.012(6) 0.038(8) C37C 0.077(14) 0.12(2) 0.084(19) 0.002(16) 0.004(12) 0.056(15) C38C 0.060(9) 0.079(14) 0.068(14) 0.021(11) -0.007(8) 0.003(8) C39C 0.033(7) 0.047(7) 0.031(6) 0.003(5) 0.010(4) 0.013(5) F40C 0.107(8) 0.081(6) 0.050(7) -0.021(5) 0.002(5) 0.042(8) N9A 0.0473(18) 0.0368(16) 0.0406(17) 0.0043(13) 0.0032(14) 0.0057(14) N10A 0.0474(18) 0.0349(16) 0.0428(18) 0.0022(13) 0.0028(14) 0.0043(14) C41A 0.058(2) 0.0358(19) 0.052(2) 0.0048(17) 0.0014(19) 0.0030(18) C42A 0.068(3) 0.039(2) 0.057(3) 0.0126(19) 0.006(2) -0.003(2) C43A 0.055(2) 0.044(2) 0.044(2) 0.0095(17) 0.0111(19) 0.0078(18) C44A 0.064(18) 0.058(18) 0.021(8) 0.001(8) -0.002(8) 0.010(12) C45A 0.080(10) 0.069(10) 0.029(7) 0.003(5) 0.017(6) 0.020(8) C46A 0.087(9) 0.097(13) 0.027(7) -0.021(9) 0.003(7) 0.003(10) C47A 0.087(11) 0.109(17) 0.078(14) 0.020(11) 0.018(9) 0.016(12) C48A 0.104(14) 0.098(14) 0.084(16) 0.025(11) 0.006(13) 0.017(12) C49A 0.15(2) 0.117(18) 0.050(9) 0.031(10) 0.002(12) -0.038(15) F50A 0.149(9) 0.131(13) 0.044(5) 0.011(5) 0.001(5) 0.024(9) C44C 0.064(19) 0.050(17) 0.082(19) 0.024(12) 0.025(13) -0.005(13) C45C 0.099(13) 0.078(13) 0.028(6) 0.007(7) 0.016(7) -0.012(9) C46C 0.15(2) 0.089(11) 0.046(11) 0.023(8) 0.024(11) 0.004(12) C47C 0.128(18) 0.091(11) 0.012(6) 0.004(5) 0.002(6) -0.010(11) C48C 0.14(2) 0.079(11) 0.026(6) 0.013(7) -0.003(8) 0.002(11) C49C 0.071(10) 0.044(7) 0.034(6) 0.014(5) -0.002(6) 0.001(7) F50C 0.31(3) 0.101(9) 0.033(5) -0.005(4) -0.006(7) 0.038(10) N11A 0.061(2) 0.0465(19) 0.0441(19) -0.0015(15) -0.0046(16) 0.0217(17) N12A 0.0478(18) 0.0375(16) 0.0455(18) 0.0032(13) 0.0041(14) 0.0103(14) C51A 0.058(2) 0.044(2) 0.042(2) 0.0006(17) -0.0003(19) 0.0078(19) C52A 0.074(3) 0.069(3) 0.045(2) 0.001(2) -0.005(2) 0.030(3) C53A 0.058(3) 0.054(2) 0.055(3) 0.008(2) 0.008(2) 0.022(2) C54A 0.060(3) 0.059(3) 0.069(3) 0.008(2) 0.012(2) 0.029(2) C55A 0.091(4) 0.063(3) 0.069(3) 0.002(2) 0.005(3) 0.039(3) C56A 0.098(4) 0.060(3) 0.094(4) -0.003(3) 0.008(3) 0.030(3) C57A 0.104(5) 0.058(3) 0.104(5) 0.008(3) 0.018(4) 0.042(3) C58A 0.144(6) 0.088(4) 0.103(5) 0.036(4) 0.028(5) 0.073(5) C59A 0.135(6) 0.097(4) 0.071(4) 0.017(3) 0.012(4) 0.076(4) F60A 0.172(4) 0.074(2) 0.149(4) 0.020(2) 0.043(3) 0.072(3) N13A 0.040(8) 0.043(8) 0.044(11) 0.008(6) -0.006(5) 0.016(6) N14A 0.044(9) 0.052(11) 0.034(6) -0.020(7) -0.013(7) 0.024(8) C61A 0.066(11) 0.129(17) 0.049(9) -0.028(9) -0.012(8) 0.072(12) C62A 0.049(11) 0.065(9) 0.087(13) -0.006(8) 0.027(9) 0.041(8) C63A 0.050(8) 0.047(6) 0.016(9) -0.011(6) -0.004(6) 0.022(5) C64A 0.026(5) 0.048(6) 0.012(5) -0.004(4) -0.006(3) 0.008(4) C65A 0.041(6) 0.066(9) 0.024(7) -0.038(5) -0.007(5) 0.006(6) C66A 0.035(5) 0.065(10) 0.032(7) -0.038(5) -0.002(4) 0.008(5) C67A 0.056(7) 0.038(5) 0.019(5) -0.020(4) 0.013(5) 0.000(5) C68A 0.054(6) 0.055(7) 0.030(8) 0.001(5) 0.024(5) 0.019(5) C69A 0.047(6) 0.041(6) 0.019(6) 0.002(5) 0.006(4) 0.004(4) F70A 0.084(6) 0.072(8) 0.044(6) -0.049(4) -0.016(5) 0.030(5) N13C 0.030(7) 0.036(8) 0.031(7) -0.006(8) 0.001(6) 0.015(5) N14C 0.037(6) 0.039(8) 0.064(10) 0.005(6) 0.018(6) 0.015(5) C61C 0.043(7) 0.036(5) 0.043(8) -0.013(5) 0.008(6) 0.013(5) C62C 0.058(12) 0.095(14) 0.054(9) -0.034(9) -0.041(7) 0.034(9) C63C 0.030(6) 0.055(7) 0.019(9) -0.001(6) 0.000(6) 0.015(5) C64C 0.047(8) 0.038(5) 0.019(7) -0.010(5) -0.003(5) 0.006(5) C65C 0.034(5) 0.050(7) 0.023(7) -0.028(5) -0.010(4) 0.008(5) C66C 0.054(6) 0.056(8) 0.028(6) -0.037(5) -0.002(5) 0.011(5) C67C 0.054(7) 0.069(8) 0.033(7) -0.004(6) 0.018(6) 0.025(6) C68C 0.046(6) 0.053(6) 0.022(6) 0.003(5) 0.016(4) 0.005(5) C69C 0.041(5) 0.042(6) 0.032(8) 0.008(6) 0.009(4) 0.015(4) F70C 0.068(5) 0.064(9) 0.050(6) -0.035(4) 0.004(5) 0.014(6) N15A 0.0353(15) 0.0355(15) 0.0424(17) 0.0063(12) 0.0096(13) 0.0113(12) N16A 0.0336(15) 0.0370(15) 0.0446(17) 0.0037(13) 0.0056(13) 0.0090(12) C71A 0.0390(19) 0.046(2) 0.053(2) 0.0060(17) 0.0061(17) 0.0153(17) C72A 0.043(2) 0.043(2) 0.056(2) 0.0050(17) 0.0101(18) 0.0181(17) C73A 0.0404(19) 0.0356(18) 0.049(2) 0.0038(16) 0.0141(17) 0.0100(15) C74A 0.039(9) 0.021(6) 0.043(8) -0.004(5) 0.015(5) 0.008(5) C75A 0.037(5) 0.059(11) 0.053(10) 0.004(8) 0.014(6) 0.015(6) C76A 0.091(14) 0.052(9) 0.056(10) 0.003(8) 0.020(10) 0.014(9) C77A 0.13(2) 0.090(18) 0.10(2) 0.026(14) 0.057(16) 0.040(15) C78A 0.060(9) 0.037(7) 0.064(10) -0.014(7) 0.002(8) 0.013(7) C79A 0.024(6) 0.042(9) 0.067(10) 0.008(7) -0.008(6) 0.006(6) F80A 0.099(9) 0.077(8) 0.101(16) -0.033(8) -0.036(9) 0.001(7) C74C 0.032(6) 0.061(12) 0.063(12) 0.014(9) 0.008(6) 0.021(6) C75C 0.085(12) 0.044(9) 0.051(9) 0.001(7) 0.030(9) 0.033(8) C76C 0.077(11) 0.063(12) 0.055(10) -0.016(9) 0.014(9) 0.029(9) C77C 0.065(9) 0.041(8) 0.048(9) -0.024(7) -0.024(7) 0.008(7) C78C 0.046(10) 0.109(17) 0.084(15) 0.019(12) -0.023(10) 0.005(11) C79C 0.058(13) 0.043(8) 0.064(9) 0.003(7) 0.015(9) 0.023(8) F80C 0.157(19) 0.101(14) 0.059(9) -0.032(8) -0.019(9) 0.061(13) N17A 0.0473(17) 0.0361(16) 0.0405(17) 0.0018(13) 0.0001(14) 0.0114(14) N18A 0.0455(17) 0.0379(16) 0.0426(17) 0.0040(13) -0.0006(14) 0.0164(14) C81A 0.047(2) 0.042(2) 0.041(2) -0.0004(16) -0.0033(17) 0.0112(17) C82A 0.047(2) 0.040(2) 0.046(2) -0.0019(16) 0.0014(17) 0.0074(17) C83A 0.051(2) 0.0302(17) 0.0359(19) 0.0033(14) 0.0071(16) 0.0090(15) C84A 0.053(2) 0.0336(18) 0.0382(19) 0.0058(15) 0.0101(17) 0.0100(16) C85A 0.052(2) 0.040(2) 0.046(2) 0.0017(16) 0.0092(18) 0.0125(17) C86A 0.054(2) 0.046(2) 0.052(2) 0.0050(18) 0.0108(19) 0.0142(19) C87A 0.067(3) 0.048(2) 0.054(2) 0.0119(19) 0.022(2) 0.028(2) C88A 0.075(3) 0.0357(19) 0.043(2) 0.0058(16) 0.014(2) 0.018(2) C89A 0.061(2) 0.0344(18) 0.042(2) 0.0027(15) 0.0092(18) 0.0103(18) F90A 0.0772(17) 0.0640(16) 0.0657(16) 0.0063(13) 0.0239(14) 0.0370(14) Cu1B 0.0400(2) 0.0399(2) 0.0418(2) 0.00259(19) 0.01104(19) 0.00662(19) Cu2B 0.0384(2) 0.0522(3) 0.0438(3) -0.0025(2) 0.0062(2) 0.0176(2) Cu3B 0.0348(2) 0.0394(2) 0.0458(3) 0.00447(19) 0.01046(19) 0.01051(18) Cu4B 0.0346(2) 0.0427(2) 0.0404(2) 0.00003(19) 0.00936(18) 0.00828(19) F1B 0.0351(10) 0.0427(11) 0.0434(12) 0.0036(9) 0.0087(9) 0.0084(9) F2B 0.0410(11) 0.0433(12) 0.0553(14) 0.0031(10) 0.0104(10) 0.0082(9) F3B 0.0341(11) 0.0756(16) 0.0490(13) -0.0155(12) 0.0050(10) 0.0176(11) N1B 0.0384(16) 0.0495(18) 0.0427(17) 0.0024(14) 0.0105(13) 0.0160(14) N2B 0.0389(16) 0.0470(17) 0.0457(18) 0.0017(14) 0.0111(14) 0.0167(14) C1B 0.042(2) 0.051(2) 0.046(2) -0.0002(17) 0.0124(17) 0.0110(17) C2B 0.048(2) 0.055(2) 0.044(2) -0.0009(18) 0.0136(18) 0.0091(19) C3B 0.0399(19) 0.047(2) 0.039(2) 0.0044(16) 0.0106(16) 0.0064(16) C4B 0.0402(19) 0.046(2) 0.044(2) 0.0138(16) 0.0136(16) 0.0097(16) C5B 0.046(2) 0.055(2) 0.049(2) 0.0115(19) 0.0082(18) 0.0147(19) C6B 0.060(3) 0.057(3) 0.067(3) 0.020(2) 0.015(2) 0.026(2) C7B 0.052(3) 0.064(3) 0.085(4) 0.026(3) 0.010(2) 0.027(2) C8B 0.051(3) 0.061(3) 0.077(3) 0.019(2) -0.008(2) 0.013(2) C9B 0.048(2) 0.052(2) 0.053(2) 0.0134(19) 0.0026(19) 0.0093(19) F10B 0.073(2) 0.094(2) 0.136(3) 0.024(2) -0.004(2) 0.0506(19) N3B 0.0404(16) 0.0378(16) 0.0487(18) 0.0073(13) 0.0111(14) 0.0119(13) N4B 0.0464(18) 0.0433(17) 0.054(2) 0.0064(15) 0.0121(15) 0.0175(15) C11B 0.062(3) 0.037(2) 0.066(3) 0.0104(19) 0.022(2) 0.0174(19) C12B 0.059(3) 0.040(2) 0.066(3) 0.0079(19) 0.023(2) 0.0079(19) C13B 0.048(2) 0.043(2) 0.048(2) 0.0081(17) 0.0140(18) 0.0116(17) C14B 0.044(2) 0.0374(19) 0.055(2) 0.0091(17) 0.0183(18) 0.0079(16) C15B 0.055(2) 0.041(2) 0.053(2) 0.0062(17) 0.0159(19) 0.0076(18) C16B 0.071(3) 0.042(2) 0.066(3) 0.010(2) 0.034(2) 0.016(2) C17B 0.060(3) 0.045(2) 0.096(4) 0.017(2) 0.042(3) 0.018(2) C18B 0.047(2) 0.048(2) 0.088(4) 0.001(2) 0.020(2) 0.0066(19) C19B 0.047(2) 0.043(2) 0.069(3) -0.0004(19) 0.020(2) 0.0048(18) F20B 0.0661(17) 0.0597(16) 0.136(3) 0.0103(17) 0.0531(18) 0.0260(14) N5B 0.0399(16) 0.0411(16) 0.0419(17) 0.0036(13) 0.0105(13) 0.0113(13) N6B 0.0431(17) 0.0403(16) 0.0467(18) 0.0038(13) 0.0155(14) 0.0144(14) C21B 0.043(2) 0.058(2) 0.050(2) 0.0070(18) 0.0160(17) 0.0224(19) C22B 0.047(2) 0.057(2) 0.045(2) 0.0020(18) 0.0102(17) 0.0269(19) C23B 0.045(2) 0.0421(19) 0.041(2) 0.0005(15) 0.0035(16) 0.0201(17) C24B 0.045(2) 0.044(2) 0.048(2) 0.0025(17) -0.0009(17) 0.0162(17) C25B 0.049(2) 0.049(2) 0.065(3) -0.004(2) 0.003(2) 0.0227(19) C26B 0.055(3) 0.046(2) 0.080(3) -0.010(2) -0.004(2) 0.020(2) C27B 0.055(3) 0.040(2) 0.079(3) 0.005(2) -0.013(2) 0.005(2) C28B 0.070(3) 0.053(3) 0.067(3) 0.007(2) 0.015(2) 0.002(2) F30B 0.0758(19) 0.0451(15) 0.114(3) 0.0092(15) -0.0017(18) -0.0046(14) N7B 0.0397(16) 0.0414(17) 0.0407(17) 0.0031(13) 0.0079(13) 0.0042(13) N8B 0.0410(16) 0.0447(17) 0.0413(17) 0.0051(13) 0.0136(14) 0.0126(14) C31B 0.048(2) 0.058(2) 0.051(2) 0.0086(19) 0.0170(19) 0.0220(19) C32B 0.046(2) 0.068(3) 0.055(3) 0.017(2) 0.0104(19) 0.022(2) C33B 0.041(2) 0.050(2) 0.043(2) 0.0071(17) 0.0080(17) 0.0062(17) C34B 0.055(3) 0.070(3) 0.045(2) 0.011(2) 0.005(2) 0.005(2) C35B 0.062(3) 0.072(3) 0.049(3) -0.003(2) 0.002(2) 0.009(2) C36B 0.099(4) 0.076(4) 0.058(3) -0.008(3) 0.005(3) 0.010(3) C37B 0.139(6) 0.094(5) 0.053(3) -0.008(3) -0.018(4) 0.014(4) C38B 0.151(7) 0.099(5) 0.066(4) 0.012(4) -0.037(4) 0.017(5) C39B 0.101(4) 0.079(4) 0.064(3) 0.007(3) -0.023(3) 0.013(3) F40B 0.233(6) 0.151(4) 0.057(2) -0.026(2) -0.038(3) 0.041(4) N9B 0.0405(16) 0.0420(17) 0.0426(17) 0.0010(13) 0.0147(14) 0.0063(13) N10B 0.0400(16) 0.0416(17) 0.0447(18) -0.0019(14) 0.0124(14) 0.0026(14) C41B 0.041(2) 0.049(2) 0.060(3) -0.0029(19) 0.0168(19) -0.0011(18) C42B 0.045(2) 0.053(2) 0.062(3) 0.003(2) 0.024(2) -0.0008(19) C43B 0.046(2) 0.049(2) 0.050(2) 0.0059(18) 0.0192(18) 0.0097(18) C44B 0.064(6) 0.018(7) 0.042(5) 0.020(4) 0.022(5) 0.008(5) C45B 0.084(12) 0.055(9) 0.044(8) 0.024(7) 0.020(8) 0.004(7) C46B 0.073(10) 0.053(9) 0.083(16) 0.032(9) 0.034(10) 0.023(8) C47B 0.080(11) 0.061(11) 0.084(15) 0.013(9) 0.028(9) 0.026(10) C48B 0.087(12) 0.080(12) 0.034(6) -0.012(7) 0.037(7) 0.016(9) C49B 0.065(10) 0.067(11) 0.068(11) -0.018(7) 0.045(8) -0.003(6) F50B 0.100(12) 0.098(8) 0.036(5) -0.015(4) 0.030(5) 0.020(6) C44D 0.053(6) 0.017(7) 0.052(6) 0.022(4) 0.030(5) 0.009(5) C45D 0.055(8) 0.051(7) 0.037(7) 0.013(6) 0.023(6) 0.020(6) C46D 0.081(13) 0.102(15) 0.021(7) -0.007(7) 0.005(7) 0.018(10) C47D 0.097(12) 0.080(12) 0.020(6) -0.005(6) 0.028(7) 0.004(10) C48D 0.059(10) 0.105(19) 0.13(2) 0.012(16) 0.048(11) 0.007(10) C49D 0.058(9) 0.057(8) 0.053(9) 0.005(6) 0.019(7) 0.012(6) F50D 0.12(2) 0.161(16) 0.078(11) -0.019(9) 0.046(10) 0.013(10) N11B 0.026(4) 0.057(5) 0.039(4) -0.005(4) 0.007(3) 0.013(4) N12B 0.035(6) 0.047(10) 0.044(7) -0.003(5) 0.006(5) 0.012(5) C51B 0.044(10) 0.048(9) 0.086(16) 0.030(9) 0.033(9) 0.016(7) C52B 0.063(8) 0.079(9) 0.045(6) -0.003(6) 0.014(5) 0.033(7) C53B 0.053(5) 0.048(5) 0.052(5) 0.003(4) 0.016(4) 0.016(4) C54B 0.046(4) 0.056(5) 0.053(5) 0.004(4) 0.016(4) 0.021(4) C55B 0.089(8) 0.118(10) 0.052(6) -0.017(6) 0.001(5) 0.060(7) C56B 0.041(7) 0.078(10) 0.100(15) -0.017(9) 0.049(8) 0.003(5) C57B 0.040(4) 0.081(6) 0.044(5) 0.005(4) 0.013(4) 0.036(5) C58B 0.048(5) 0.077(7) 0.076(7) -0.013(5) 0.010(5) 0.024(5) C59B 0.045(5) 0.080(6) 0.057(5) -0.004(5) 0.020(4) 0.021(4) F60B 0.047(3) 0.105(5) 0.078(4) 0.011(3) 0.023(3) 0.030(3) N11D 0.039(4) 0.043(5) 0.046(4) 0.003(4) 0.009(3) 0.015(4) N12D 0.047(7) 0.031(5) 0.034(6) -0.001(4) 0.023(5) 0.021(5) C51D 0.066(12) 0.060(9) 0.012(5) -0.016(6) -0.004(5) 0.023(8) C52D 0.051(6) 0.066(8) 0.045(6) 0.000(5) 0.012(4) 0.023(6) C53D 0.040(4) 0.038(4) 0.046(4) -0.001(3) 0.015(3) 0.013(3) C54D 0.039(4) 0.039(4) 0.054(5) 0.002(3) 0.012(3) 0.012(3) C55D 0.064(6) 0.072(6) 0.057(5) -0.002(4) 0.016(4) 0.033(5) C56D 0.054(5) 0.069(6) 0.082(7) 0.011(5) 0.025(5) 0.042(5) C57D 0.022(3) 0.049(5) 0.100(7) -0.003(5) -0.006(4) 0.019(3) C58D 0.034(4) 0.062(5) 0.070(6) -0.012(5) -0.005(4) 0.004(4) C59D 0.044(4) 0.042(4) 0.065(5) -0.004(4) 0.009(4) 0.020(3) F60D 0.079(4) 0.082(4) 0.111(5) -0.007(4) -0.022(4) 0.053(4) N13B 0.036(9) 0.029(5) 0.049(11) 0.004(6) 0.004(6) 0.006(7) N14B 0.031(6) 0.033(7) 0.051(6) -0.003(6) -0.001(6) 0.000(6) C61B 0.053(8) 0.044(7) 0.078(8) -0.004(6) 0.006(6) 0.010(5) C62B 0.091(12) 0.058(9) 0.071(9) 0.003(7) 0.008(8) 0.031(8) C63B 0.066(12) 0.035(8) 0.050(7) 0.004(5) 0.012(6) 0.004(8) C64B 0.058(11) 0.041(8) 0.057(8) 0.008(5) 0.013(6) -0.010(7) C65B 0.074(11) 0.044(6) 0.034(6) -0.016(5) -0.002(6) 0.000(6) C66B 0.071(9) 0.056(6) 0.055(8) -0.007(6) -0.003(6) 0.025(6) C67B 0.085(10) 0.059(7) 0.031(5) -0.035(5) 0.002(6) -0.010(6) C68B 0.18(2) 0.061(8) 0.060(10) -0.020(7) 0.019(13) 0.062(12) C69B 0.141(19) 0.072(11) 0.053(9) 0.002(7) 0.004(10) 0.057(14) F70B 0.118(10) 0.107(9) 0.092(9) -0.079(8) -0.047(8) 0.044(8) N13D 0.040(10) 0.050(12) 0.034(8) -0.006(6) 0.003(5) 0.003(8) N14D 0.031(6) 0.028(6) 0.047(6) 0.000(6) 0.007(6) 0.000(5) C61D 0.037(5) 0.040(6) 0.039(4) 0.000(4) 0.009(4) 0.007(4) C62D 0.059(7) 0.038(6) 0.043(5) 0.009(4) 0.022(5) 0.021(5) C63D 0.043(7) 0.029(7) 0.047(6) 0.007(4) 0.020(4) 0.000(6) C64D 0.047(8) 0.033(6) 0.049(7) -0.004(5) 0.024(5) -0.003(7) C65D 0.053(8) 0.083(11) 0.055(10) -0.031(8) -0.002(7) 0.009(8) C66D 0.080(12) 0.20(2) 0.063(9) -0.088(12) 0.000(8) -0.008(12) C67D 0.17(3) 0.072(12) 0.24(4) -0.041(17) 0.11(3) 0.009(16) C68D 0.14(2) 0.120(19) 0.11(2) -0.016(14) -0.013(16) 0.056(15) C69D 0.122(13) 0.067(11) 0.097(16) -0.020(11) 0.023(12) 0.031(10) F70D 0.23(2) 0.168(18) 0.097(11) -0.073(11) 0.043(11) -0.011(14) N15B 0.0365(16) 0.0436(17) 0.053(2) 0.0076(15) 0.0122(14) 0.0066(14) N16B 0.0387(16) 0.0430(17) 0.0517(19) 0.0112(14) 0.0131(14) 0.0117(14) C71B 0.043(2) 0.057(2) 0.054(2) 0.0132(19) 0.0147(18) 0.0173(19) C72B 0.038(2) 0.062(3) 0.061(3) 0.018(2) 0.0118(19) 0.0127(19) C73B 0.039(2) 0.052(2) 0.053(2) 0.0105(19) 0.0077(18) 0.0066(18) C74B 0.055(12) 0.065(11) 0.060(9) 0.008(8) 0.011(8) 0.006(8) C75B 0.070(13) 0.072(15) 0.18(3) -0.013(15) -0.012(16) 0.003(11) C76B 0.11(2) 0.101(17) 0.21(3) -0.065(19) -0.02(2) 0.002(15) C77B 0.14(2) 0.13(2) 0.16(3) -0.030(18) 0.06(2) -0.025(17) C78B 0.16(2) 0.123(19) 0.071(12) -0.028(13) -0.047(14) -0.014(15) C79B 0.12(2) 0.060(9) 0.097(18) 0.016(10) 0.013(13) 0.033(10) F80B 0.161(19) 0.15(2) 0.23(3) -0.13(2) 0.003(17) -0.012(13) C74D 0.040(9) 0.050(7) 0.060(10) 0.006(7) 0.008(8) 0.000(6) C75D 0.045(7) 0.035(6) 0.072(8) -0.002(6) -0.008(6) -0.003(5) C76D 0.055(8) 0.041(6) 0.107(12) -0.021(7) 0.007(8) -0.003(6) C77D 0.067(9) 0.068(8) 0.089(10) -0.045(8) -0.007(8) -0.004(7) C78D 0.060(8) 0.089(10) 0.090(12) 0.010(10) 0.008(8) 0.024(7) C79D 0.050(8) 0.082(11) 0.038(6) -0.002(8) -0.013(6) 0.002(7) F80D 0.113(11) 0.132(14) 0.113(8) -0.065(8) -0.006(8) 0.014(11) N17B 0.0326(15) 0.0519(18) 0.0400(17) -0.0027(14) 0.0092(13) 0.0095(14) N18B 0.0380(16) 0.059(2) 0.0432(18) -0.0024(15) 0.0093(14) 0.0162(15) C81B 0.042(2) 0.051(2) 0.044(2) -0.0039(17) 0.0100(17) 0.0092(17) C82B 0.043(2) 0.053(2) 0.043(2) -0.0025(17) 0.0051(17) 0.0091(18) C83B 0.0338(18) 0.049(2) 0.0373(19) 0.0030(16) 0.0086(15) 0.0059(16) C84B 0.0369(18) 0.048(2) 0.0379(19) 0.0062(16) 0.0092(15) 0.0058(16) C85B 0.040(2) 0.049(2) 0.056(2) 0.0062(19) 0.0020(18) 0.0081(18) C86B 0.050(2) 0.047(2) 0.072(3) 0.008(2) 0.009(2) 0.0111(19) C87B 0.040(2) 0.059(3) 0.058(3) 0.019(2) 0.0075(19) 0.0161(19) C88B 0.0356(19) 0.072(3) 0.041(2) 0.0082(19) 0.0065(16) 0.0089(19) C89B 0.0382(19) 0.057(2) 0.042(2) 0.0045(18) 0.0095(16) 0.0076(18) F90B 0.0468(13) 0.0728(17) 0.0765(18) 0.0214(14) 0.0037(12) 0.0255(13) C1S 0.072(3) 0.102(4) 0.074(4) 0.021(3) 0.022(3) 0.017(3) Cl2S 0.0928(10) 0.0940(10) 0.0723(9) 0.0001(7) 0.0239(8) 0.0239(8) Cl3S 0.0809(10) 0.1415(16) 0.1043(13) -0.0383(12) 0.0226(9) 0.0253(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1A F2A 1.971(2) . ? Cu1A N7A 1.981(3) . ? Cu1A N9A 1.994(3) . ? Cu1A N12A 2.006(3) . ? Cu1A F1A 2.253(2) . ? Cu2A F3A 1.946(2) . ? Cu2A N4A 1.965(3) . ? Cu2A N1A 1.999(3) . ? Cu2A N14C 2.003(19) . ? Cu2A N14A 2.040(15) . ? Cu2A F1A 2.245(2) . ? Cu3A N2A 1.971(3) . ? Cu3A N3A 1.988(3) . ? Cu3A N6A 1.996(3) . ? Cu3A N16A 2.013(3) . ? Cu3A F1A 2.295(2) . ? Cu4A N10A 1.969(3) . ? Cu4A N5A 1.990(3) . ? Cu4A N8A 2.011(3) . ? Cu4A N18A 2.025(3) . ? Cu4A F1A 2.254(2) . ? Cu1A Cu4A 3.2719(6) . ? Cu1A Cu2A 3.8169(7) . ? Cu1A Cu3A 4.1812(6) . ? Cu2A Cu3A 3.2863(6) . ? Cu2A Cu4A 4.1654(7) . ? Cu3A Cu4A 3.1899(6) . ? N1A C3A 1.356(5) . ? N1A N2A 1.362(4) . ? N2A C1A 1.343(5) . ? C1A C2A 1.377(6) . ? C2A C3A 1.403(5) . ? C3A C4A 1.463(5) . ? C4A C5A 1.378(6) . ? C4A C9A 1.401(5) . ? C5A C6A 1.393(6) . ? C6A C7A 1.376(7) . ? C7A F10A 1.365(5) . ? C7A C8A 1.367(7) . ? C8A C9A 1.372(6) . ? N3A C13A 1.341(5) . ? N3A N4A 1.351(4) . ? N4A C11A 1.338(5) . ? C11A C12A 1.387(6) . ? C12A C13A 1.399(5) . ? C13A C14A 1.466(5) . ? C14A C15A 1.396(5) . ? C14A C19A 1.399(5) . ? C15A C16A 1.394(5) . ? C16A C17A 1.378(6) . ? C17A F20A 1.375(4) . ? C17A C18A 1.381(6) . ? C18A C19A 1.387(6) . ? N5A N6A 1.354(4) . ? N5A C23A 1.354(5) . ? N6A C21A 1.334(5) . ? C21A C22A 1.384(5) . ? C22A C23A 1.396(5) . ? C23A C24A 1.474(5) . ? C24A C29A 1.386(5) . ? C24A C25A 1.386(6) . ? C25A C26A 1.378(7) . ? C26A C27A 1.388(7) . ? C27A C28A 1.356(7) . ? C27A F30A 1.371(5) . ? C28A C29A 1.389(6) . ? N7A C33A 1.368(5) . ? N7A N8A 1.378(4) . ? N8A C31A 1.339(5) . ? C31A C32A 1.379(6) . ? C32A C33A 1.398(6) . ? C33A C34C 1.485(7) . ? C33A C34A 1.486(7) . ? C34A C35A 1.3900 . ? C34A C39A 1.3900 . ? C35A C36A 1.3900 . ? C36A C37A 1.3900 . ? C37A F40A 1.346(9) . ? C37A C38A 1.3900 . ? C38A C39A 1.3900 . ? C34C C35C 1.3900 . ? C34C C39C 1.3900 . ? C35C C36C 1.3900 . ? C36C C37C 1.3900 . ? C37C F40C 1.344(8) . ? C37C C38C 1.3900 . ? C38C C39C 1.3900 . ? N9A C43A 1.348(5) . ? N9A N10A 1.358(4) . ? N10A C41A 1.344(5) . ? C41A C42A 1.382(6) . ? C42A C43A 1.386(6) . ? C43A C44C 1.452(7) . ? C43A C44A 1.482(7) . ? C44A C45A 1.3900 . ? C44A C49A 1.3900 . ? C45A C46A 1.3900 . ? C46A C47A 1.3900 . ? C47A F50A 1.344(8) . ? C47A C48A 1.3900 . ? C48A C49A 1.3900 . ? C44C C45C 1.3900 . ? C44C C49C 1.3900 . ? C45C C46C 1.3900 . ? C46C C47C 1.3900 . ? C47C F50C 1.339(8) . ? C47C C48C 1.3900 . ? C48C C49C 1.3900 . ? N11A N12A 1.330(5) . ? N11A C53A 1.349(5) . ? N12A C51A 1.328(5) . ? C51A C52A 1.358(6) . ? C52A C53A 1.391(6) . ? C53A C54A 1.467(6) . ? C54A C55A 1.383(7) . ? C54A C59A 1.394(7) . ? C55A C56A 1.378(7) . ? C56A C57A 1.359(9) . ? C57A F60A 1.351(6) . ? C57A C58A 1.361(9) . ? C58A C59A 1.394(8) . ? N13A N14A 1.349(9) . ? N13A C63A 1.362(9) . ? N14A C61A 1.329(9) . ? C61A C62A 1.387(9) . ? C62A C63A 1.383(9) . ? C63A C64A 1.471(9) . ? C64A C65A 1.3900 . ? C64A C69A 1.3900 . ? C65A C66A 1.3900 . ? C66A C67A 1.3900 . ? C67A F70A 1.331(8) . ? C67A C68A 1.3900 . ? C68A C69A 1.3900 . ? N13C N14C 1.353(9) . ? N13C C63C 1.360(9) . ? N14C C61C 1.330(9) . ? C61C C62C 1.396(9) . ? C62C C63C 1.382(9) . ? C63C C64C 1.470(9) . ? C64C C65C 1.3900 . ? C64C C69C 1.3900 . ? C65C C66C 1.3900 . ? C66C C67C 1.3900 . ? C67C F70C 1.335(8) . ? C67C C68C 1.3900 . ? C68C C69C 1.3900 . ? N15A C73A 1.349(5) . ? N15A N16A 1.350(4) . ? N16A C71A 1.331(5) . ? C71A C72A 1.390(6) . ? C72A C73A 1.391(5) . ? C73A C74C 1.446(7) . ? C73A C74A 1.489(7) . ? C74A C75A 1.3900 . ? C74A C79A 1.3900 . ? C75A C76A 1.3900 . ? C76A C77A 1.3900 . ? C77A F80A 1.328(8) . ? C77A C78A 1.3900 . ? C78A C79A 1.3900 . ? C74C C75C 1.3900 . ? C74C C79C 1.3900 . ? C75C C76C 1.3900 . ? C76C C77C 1.3900 . ? C77C F80C 1.333(8) . ? C77C C78C 1.3900 . ? C78C C79C 1.3900 . ? N17A C83A 1.352(5) . ? N17A N18A 1.353(4) . ? N18A C81A 1.321(5) . ? C81A C82A 1.376(6) . ? C82A C83A 1.387(5) . ? C83A C84A 1.465(5) . ? C84A C85A 1.387(6) . ? C84A C89A 1.402(5) . ? C85A C86A 1.373(6) . ? C86A C87A 1.389(6) . ? C87A C88A 1.359(6) . ? C87A F90A 1.361(5) . ? C88A C89A 1.387(6) . ? Cu1B N12B 1.825(18) . ? Cu1B F2B 1.971(2) . ? Cu1B N7B 1.988(3) . ? Cu1B N9B 1.993(3) . ? Cu1B N12D 2.111(15) . ? Cu1B F1B 2.267(2) . ? Cu2B F3B 1.936(2) . ? Cu2B N4B 1.948(3) . ? Cu2B N14B 1.95(2) . ? Cu2B N1B 1.996(3) . ? Cu2B N14D 2.09(2) . ? Cu2B F1B 2.269(2) . ? Cu3B N2B 1.974(3) . ? Cu3B N3B 1.981(3) . ? Cu3B N6B 1.984(3) . ? Cu3B N16B 2.018(3) . ? Cu3B F1B 2.324(2) . ? Cu4B N10B 1.975(3) . ? Cu4B N5B 1.989(3) . ? Cu4B N8B 2.016(3) . ? Cu4B N18B 2.023(3) . ? Cu4B F1B 2.226(2) . ? Cu1B Cu4B 3.2570(6) . ? Cu1B Cu2B 3.8104(7) . ? Cu1B Cu3B 4.2577(7) . ? Cu2B Cu3B 3.2836(6) . ? Cu2B Cu4B 4.1901(7) . ? Cu3B Cu4B 3.2199(6) . ? N1B C3B 1.348(5) . ? N1B N2B 1.360(4) . ? N2B C1B 1.332(5) . ? C1B C2B 1.390(6) . ? C2B C3B 1.399(6) . ? C3B C4B 1.463(5) . ? C4B C9B 1.386(6) . ? C4B C5B 1.389(6) . ? C5B C6B 1.396(6) . ? C6B C7B 1.376(7) . ? C7B F10B 1.362(5) . ? C7B C8B 1.374(7) . ? C8B C9B 1.384(6) . ? N3B C13B 1.352(5) . ? N3B N4B 1.365(4) . ? N4B C11B 1.353(5) . ? C11B C12B 1.376(6) . ? C12B C13B 1.396(6) . ? C13B C14B 1.460(6) . ? C14B C19B 1.396(6) . ? C14B C15B 1.403(6) . ? C15B C16B 1.382(6) . ? C16B C17B 1.367(7) . ? C17B C18B 1.362(7) . ? C17B F20B 1.373(5) . ? C18B C19B 1.381(6) . ? N5B C23B 1.349(5) . ? N5B N6B 1.357(4) . ? N6B C21B 1.341(5) . ? C21B C22B 1.377(6) . ? C22B C23B 1.391(6) . ? C23B C24B 1.483(6) . ? C24B C29B 1.394(6) . ? C24B C25B 1.396(6) . ? C25B C26B 1.373(7) . ? C26B C27B 1.351(8) . ? C27B F30B 1.373(5) . ? C27B C28B 1.379(7) . ? C28B C29B 1.389(7) . ? N7B C33B 1.351(5) . ? N7B N8B 1.357(4) . ? N8B C31B 1.345(5) . ? C31B C32B 1.379(6) . ? C32B C33B 1.400(6) . ? C33B C34B 1.475(6) . ? C34B C35B 1.390(7) . ? C34B C39B 1.390(7) . ? C35B C36B 1.395(7) . ? C36B C37B 1.354(9) . ? C37B C38B 1.366(11) . ? C37B F40B 1.370(7) . ? C38B C39B 1.388(9) . ? N9B C43B 1.351(5) . ? N9B N10B 1.358(4) . ? N10B C41B 1.340(5) . ? C41B C42B 1.380(6) . ? C42B C43B 1.398(6) . ? C43B C44D 1.462(7) . ? C43B C44B 1.483(7) . ? C44B C45B 1.3900 . ? C44B C49B 1.3900 . ? C45B C46B 1.3900 . ? C46B C47B 1.3900 . ? C47B F50B 1.347(8) . ? C47B C48B 1.3900 . ? C48B C49B 1.3900 . ? C44D C45D 1.3900 . ? C44D C49D 1.3900 . ? C45D C46D 1.3900 . ? C46D C47D 1.3900 . ? C47D F50D 1.342(9) . ? C47D C48D 1.3900 . ? C48D C49D 1.3900 . ? N11B N12B 1.344(9) . ? N11B C53B 1.348(8) . ? N12B C51B 1.333(9) . ? C51B C52B 1.386(9) . ? C52B C53B 1.378(9) . ? C53B C54B 1.463(7) . ? C54B C59B 1.368(10) . ? C54B C55B 1.399(11) . ? C55B C56B 1.366(14) . ? C56B C57B 1.391(14) . ? C57B F60B 1.332(7) . ? C57B C58B 1.371(10) . ? C58B C59B 1.380(10) . ? N11D N12D 1.346(9) . ? N11D C53D 1.347(8) . ? N12D C51D 1.338(9) . ? C51D C52D 1.387(9) . ? C52D C53D 1.378(8) . ? C53D C54D 1.467(7) . ? C54D C59D 1.382(9) . ? C54D C55D 1.396(10) . ? C55D C56D 1.392(10) . ? C56D C57D 1.356(11) . ? C57D C58D 1.342(10) . ? C57D F60D 1.351(7) . ? C58D C59D 1.405(10) . ? N13B N14B 1.341(9) . ? N13B C63B 1.348(9) . ? N14B C61B 1.335(9) . ? C61B C62B 1.386(9) . ? C62B C63B 1.378(9) . ? C63B C64B 1.471(9) . ? C64B C65B 1.3900 . ? C64B C69B 1.3900 . ? C65B C66B 1.3900 . ? C66B C67B 1.3900 . ? C67B F70B 1.341(8) . ? C67B C68B 1.3900 . ? C68B C69B 1.3900 . ? N13D N14D 1.343(9) . ? N13D C63D 1.349(9) . ? N14D C61D 1.335(9) . ? C61D C62D 1.389(9) . ? C62D C63D 1.381(9) . ? C63D C64D 1.472(9) . ? C64D C65D 1.3900 . ? C64D C69D 1.3900 . ? C65D C66D 1.3900 . ? C66D C67D 1.3900 . ? C67D F70D 1.339(9) . ? C67D C68D 1.3900 . ? C68D C69D 1.3900 . ? N15B C73B 1.340(5) . ? N15B N16B 1.350(5) . ? N16B C71B 1.325(5) . ? C71B C72B 1.387(6) . ? C72B C73B 1.375(6) . ? C73B C74B 1.462(8) . ? C73B C74D 1.463(7) . ? C74B C75B 1.3900 . ? C74B C79B 1.3900 . ? C75B C76B 1.3900 . ? C76B C77B 1.3900 . ? C77B F80B 1.330(9) . ? C77B C78B 1.3900 . ? C78B C79B 1.3900 . ? C74D C75D 1.3900 . ? C74D C79D 1.3900 . ? C75D C76D 1.3900 . ? C76D C77D 1.3900 . ? C77D F80D 1.332(8) . ? C77D C78D 1.3900 . ? C78D C79D 1.3900 . ? N17B C83B 1.338(5) . ? N17B N18B 1.359(4) . ? N18B C81B 1.333(5) . ? C81B C82B 1.393(6) . ? C82B C83B 1.381(6) . ? C83B C84B 1.478(5) . ? C84B C85B 1.385(6) . ? C84B C89B 1.396(5) . ? C85B C86B 1.389(6) . ? C86B C87B 1.369(6) . ? C87B C88B 1.362(6) . ? C87B F90B 1.372(5) . ? C88B C89B 1.378(6) . ? N1E C5E 1.342(9) . ? N1E N2E 1.359(10) . ? N2E C3E 1.323(10) . ? C3E C4E 1.368(9) . ? C4E C5E 1.378(9) . ? C5E C6E 1.479(8) . ? C6E C7E 1.3900 . ? C6E C11E 1.3900 . ? C7E C8E 1.3900 . ? C8E C9E 1.3900 . ? C9E F12E 1.3203 . ? C9E C10E 1.3900 . ? C10E C11E 1.3900 . ? N13E C17E 1.326(9) . ? N13E N14E 1.337(10) . ? N14E C15E 1.327(10) . ? C15E C16E 1.379(10) . ? C16E C17E 1.372(10) . ? C17E C18E 1.468(9) . ? C18E C19E 1.3900 . ? C18E C23E 1.3900 . ? C19E C20E 1.3900 . ? C20E C21E 1.3900 . ? C21E F24E 1.3045 . ? C21E C22E 1.3900 . ? C22E C23E 1.3900 . ? C1S Cl2S 1.746(6) . ? C1S Cl3S 1.794(7) . ? C4S Cl5S 1.737(16) . ? C4S Cl6S 1.808(15) . ? C7S Cl9S 1.787(19) . ? C7S Cl8S 1.796(19) . ? C10S Cl11S 1.771(16) . ? C10S Cl12S 1.816(16) . ? 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 F2A Cu1A N7A 98.28(10) . . ? F2A Cu1A N9A 173.72(11) . . ? N7A Cu1A N9A 88.00(13) . . ? F2A Cu1A N12A 85.50(11) . . ? N7A Cu1A N12A 163.87(14) . . ? N9A Cu1A N12A 88.39(13) . . ? F2A Cu1A F1A 84.26(8) . . ? N7A Cu1A F1A 88.73(10) . . ? N9A Cu1A F1A 96.18(11) . . ? N12A Cu1A F1A 107.28(11) . . ? F3A Cu2A N4A 172.72(12) . . ? F3A Cu2A N1A 96.48(11) . . ? N4A Cu2A N1A 90.00(13) . . ? F3A Cu2A N14C 86.2(9) . . ? N4A Cu2A N14C 88.8(9) . . ? N1A Cu2A N14C 160.1(7) . . ? F3A Cu2A N14A 89.3(9) . . ? N4A Cu2A N14A 86.2(9) . . ? N1A Cu2A N14A 154.6(7) . . ? F3A Cu2A F1A 83.83(9) . . ? N4A Cu2A F1A 92.98(10) . . ? N1A Cu2A F1A 89.19(11) . . ? N14C Cu2A F1A 110.7(7) . . ? N14A Cu2A F1A 116.1(7) . . ? N2A Cu3A N3A 89.58(13) . . ? N2A Cu3A N6A 89.22(13) . . ? N3A Cu3A N6A 160.91(13) . . ? N2A Cu3A N16A 179.21(13) . . ? N3A Cu3A N16A 89.92(12) . . ? N6A Cu3A N16A 91.45(12) . . ? N2A Cu3A F1A 85.07(11) . . ? N3A Cu3A F1A 92.15(10) . . ? N6A Cu3A F1A 106.72(10) . . ? N16A Cu3A F1A 94.33(10) . . ? N10A Cu4A N5A 160.48(13) . . ? N10A Cu4A N8A 91.91(13) . . ? N5A Cu4A N8A 87.01(13) . . ? N10A Cu4A N18A 88.74(13) . . ? N5A Cu4A N18A 91.01(12) . . ? N8A Cu4A N18A 175.88(13) . . ? N10A Cu4A F1A 90.07(11) . . ? N5A Cu4A F1A 109.18(10) . . ? N8A Cu4A F1A 84.25(10) . . ? N18A Cu4A F1A 99.82(11) . . ? Cu2A F1A Cu1A 116.13(9) . . ? Cu2A F1A Cu4A 135.62(9) . . ? Cu1A F1A Cu4A 93.10(8) . . ? Cu2A F1A Cu3A 92.76(8) . . ? Cu1A F1A Cu3A 133.68(9) . . ? Cu4A F1A Cu3A 89.06(7) . . ? C3A N1A N2A 107.9(3) . . ? C3A N1A Cu2A 135.4(3) . . ? N2A N1A Cu2A 116.7(2) . . ? C1A N2A N1A 108.2(3) . . ? C1A N2A Cu3A 130.1(3) . . ? N1A N2A Cu3A 120.6(2) . . ? N2A C1A C2A 110.3(3) . . ? C1A C2A C3A 104.6(3) . . ? N1A C3A C2A 109.0(3) . . ? N1A C3A C4A 122.5(3) . . ? C2A C3A C4A 128.4(4) . . ? C5A C4A C9A 117.6(4) . . ? C5A C4A C3A 122.5(4) . . ? C9A C4A C3A 119.9(4) . . ? C4A C5A C6A 121.5(4) . . ? C7A C6A C5A 117.9(4) . . ? F10A C7A C8A 118.9(4) . . ? F10A C7A C6A 118.2(4) . . ? C8A C7A C6A 122.9(4) . . ? C7A C8A C9A 117.9(4) . . ? C8A C9A C4A 122.2(4) . . ? C13A N3A N4A 108.9(3) . . ? C13A N3A Cu3A 129.7(2) . . ? N4A N3A Cu3A 120.5(2) . . ? C11A N4A N3A 108.0(3) . . ? C11A N4A Cu2A 134.2(3) . . ? N3A N4A Cu2A 117.8(2) . . ? N4A C11A C12A 109.9(3) . . ? C11A C12A C13A 104.3(3) . . ? N3A C13A C12A 108.8(3) . . ? N3A C13A C14A 120.8(3) . . ? C12A C13A C14A 130.4(3) . . ? C15A C14A C19A 119.0(3) . . ? C15A C14A C13A 121.0(3) . . ? C19A C14A C13A 120.0(3) . . ? C16A C15A C14A 120.7(4) . . ? C17A C16A C15A 117.9(4) . . ? F20A C17A C16A 118.3(4) . . ? F20A C17A C18A 118.0(4) . . ? C16A C17A C18A 123.7(4) . . ? C17A C18A C19A 117.3(4) . . ? C18A C19A C14A 121.5(4) . . ? N6A N5A C23A 108.5(3) . . ? N6A N5A Cu4A 115.9(2) . . ? C23A N5A Cu4A 135.2(3) . . ? C21A N6A N5A 108.3(3) . . ? C21A N6A Cu3A 132.9(3) . . ? N5A N6A Cu3A 118.7(2) . . ? N6A C21A C22A 109.9(3) . . ? C21A C22A C23A 104.9(3) . . ? N5A C23A C22A 108.4(3) . . ? N5A C23A C24A 122.8(3) . . ? C22A C23A C24A 128.7(3) . . ? C29A C24A C25A 118.0(4) . . ? C29A C24A C23A 119.5(4) . . ? C25A C24A C23A 122.5(4) . . ? C26A C25A C24A 121.2(4) . . ? C25A C26A C27A 118.4(5) . . ? C28A C27A F30A 120.0(4) . . ? C28A C27A C26A 122.5(4) . . ? F30A C27A C26A 117.5(5) . . ? C27A C28A C29A 117.9(4) . . ? C24A C29A C28A 122.0(4) . . ? C33A N7A N8A 108.0(3) . . ? C33A N7A Cu1A 139.2(3) . . ? N8A N7A Cu1A 112.6(2) . . ? C31A N8A N7A 107.8(3) . . ? C31A N8A Cu4A 128.0(3) . . ? N7A N8A Cu4A 124.2(2) . . ? N8A C31A C32A 110.4(4) . . ? C31A C32A C33A 105.5(4) . . ? N7A C33A C32A 108.2(3) . . ? N7A C33A C34C 130.3(7) . . ? C32A C33A C34C 121.4(7) . . ? N7A C33A C34A 115.9(7) . . ? C32A C33A C34A 135.8(7) . . ? C35A C34A C39A 120.0 . . ? C35A C34A C33A 106.1(10) . . ? C39A C34A C33A 133.6(11) . . ? C36A C35A C34A 120.0 . . ? C35A C36A C37A 120.0 . . ? F40A C37A C36A 127.3(18) . . ? F40A C37A C38A 112.6(18) . . ? C36A C37A C38A 120.0 . . ? C37A C38A C39A 120.0 . . ? C38A C39A C34A 120.0 . . ? C35C C34C C39C 120.0 . . ? C35C C34C C33A 126.0(10) . . ? C39C C34C C33A 114.0(10) . . ? C36C C35C C34C 120.0 . . ? C35C C36C C37C 120.0 . . ? F40C C37C C38C 124.1(16) . . ? F40C C37C C36C 115.5(16) . . ? C38C C37C C36C 120.0 . . ? C39C C38C C37C 120.0 . . ? C38C C39C C34C 120.0 . . ? C43A N9A N10A 108.4(3) . . ? C43A N9A Cu1A 134.7(3) . . ? N10A N9A Cu1A 114.6(2) . . ? C41A N10A N9A 107.9(3) . . ? C41A N10A Cu4A 131.0(3) . . ? N9A N10A Cu4A 119.8(2) . . ? N10A C41A C42A 109.6(4) . . ? C41A C42A C43A 105.1(4) . . ? N9A C43A C42A 108.9(3) . . ? N9A C43A C44C 121.8(8) . . ? C42A C43A C44C 129.3(8) . . ? N9A C43A C44A 120.9(8) . . ? C42A C43A C44A 130.1(9) . . ? C45A C44A C49A 120.0 . . ? C45A C44A C43A 126.5(11) . . ? C49A C44A C43A 113.4(11) . . ? C44A C45A C46A 120.0 . . ? C45A C46A C47A 120.0 . . ? F50A C47A C48A 123.1(17) . . ? F50A C47A C46A 116.9(17) . . ? C48A C47A C46A 120.0 . . ? C49A C48A C47A 120.0 . . ? C48A C49A C44A 120.0 . . ? C45C C44C C49C 120.0 . . ? C45C C44C C43A 114.1(11) . . ? C49C C44C C43A 125.9(11) . . ? C46C C45C C44C 120.0 . . ? C45C C46C C47C 120.0 . . ? F50C C47C C48C 118.8(16) . . ? F50C C47C C46C 121.2(16) . . ? C48C C47C C46C 120.0 . . ? C49C C48C C47C 120.0 . . ? C48C C49C C44C 120.0 . . ? N12A N11A C53A 111.3(3) . . ? C51A N12A N11A 105.9(3) . . ? C51A N12A Cu1A 128.4(3) . . ? N11A N12A Cu1A 121.5(2) . . ? N12A C51A C52A 111.4(4) . . ? C51A C52A C53A 105.2(4) . . ? N11A C53A C52A 106.1(4) . . ? N11A C53A C54A 122.0(4) . . ? C52A C53A C54A 131.8(4) . . ? C55A C54A C59A 118.4(5) . . ? C55A C54A C53A 122.1(4) . . ? C59A C54A C53A 119.3(5) . . ? C56A C55A C54A 121.5(5) . . ? C57A C56A C55A 118.6(6) . . ? F60A C57A C56A 119.3(6) . . ? F60A C57A C58A 118.3(6) . . ? C56A C57A C58A 122.4(5) . . ? C57A C58A C59A 119.1(6) . . ? C54A C59A C58A 120.0(6) . . ? N14A N13A C63A 102.0(15) . . ? C61A N14A N13A 114.9(16) . . ? C61A N14A Cu2A 128.1(13) . . ? N13A N14A Cu2A 115.9(16) . . ? N14A C61A C62A 104.7(15) . . ? C63A C62A C61A 104.9(15) . . ? N13A C63A C62A 111.2(16) . . ? N13A C63A C64A 118.2(17) . . ? C62A C63A C64A 129(2) . . ? C65A C64A C69A 120.0 . . ? C65A C64A C63A 115.0(14) . . ? C69A C64A C63A 125.0(14) . . ? C66A C65A C64A 120.0 . . ? C65A C66A C67A 120.0 . . ? F70A C67A C68A 116.4(18) . . ? F70A C67A C66A 123.4(18) . . ? C68A C67A C66A 120.0 . . ? C67A C68A C69A 120.0 . . ? C68A C69A C64A 120.0 . . ? N14C N13C C63C 121.6(15) . . ? C61C N14C N13C 98.0(15) . . ? C61C N14C Cu2A 130.4(15) . . ? N13C N14C Cu2A 129.8(17) . . ? N14C C61C C62C 112.8(15) . . ? C63C C62C C61C 108.7(14) . . ? N13C C63C C62C 97.7(12) . . ? N13C C63C C64C 128.9(16) . . ? C62C C63C C64C 133.3(18) . . ? C65C C64C C69C 120.0 . . ? C65C C64C C63C 122.2(14) . . ? C69C C64C C63C 117.8(14) . . ? C66C C65C C64C 120.0 . . ? C65C C66C C67C 120.0 . . ? F70C C67C C66C 115.7(17) . . ? F70C C67C C68C 124.1(17) . . ? C66C C67C C68C 120.0 . . ? C67C C68C C69C 120.0 . . ? C68C C69C C64C 120.0 . . ? C73A N15A N16A 112.2(3) . . ? C71A N16A N15A 105.3(3) . . ? C71A N16A Cu3A 129.7(3) . . ? N15A N16A Cu3A 122.8(2) . . ? N16A C71A C72A 111.1(3) . . ? C71A C72A C73A 105.3(3) . . ? N15A C73A C72A 106.0(3) . . ? N15A C73A C74C 127.3(10) . . ? C72A C73A C74C 126.6(10) . . ? N15A C73A C74A 119.6(9) . . ? C72A C73A C74A 134.3(9) . . ? C74C C73A C74A 8.1(19) . . ? C75A C74A C79A 120.0 . . ? C75A C74A C73A 113.7(14) . . ? C79A C74A C73A 126.3(14) . . ? C74A C75A C76A 120.0 . . ? C77A C76A C75A 120.0 . . ? F80A C77A C78A 118.2(19) . . ? F80A C77A C76A 121.8(19) . . ? C78A C77A C76A 120.0 . . ? C77A C78A C79A 120.0 . . ? C78A C79A C74A 120.0 . . ? C75C C74C C79C 120.0 . . ? C75C C74C C73A 124.4(16) . . ? C79C C74C C73A 115.5(16) . . ? C74C C75C C76C 120.0 . . ? C77C C76C C75C 120.0 . . ? F80C C77C C78C 122.1(18) . . ? F80C C77C C76C 117.8(18) . . ? C78C C77C C76C 120.0 . . ? C77C C78C C79C 120.0 . . ? C78C C79C C74C 120.0 . . ? C83A N17A N18A 111.9(3) . . ? C81A N18A N17A 105.2(3) . . ? C81A N18A Cu4A 130.3(3) . . ? N17A N18A Cu4A 123.4(2) . . ? N18A C81A C82A 111.5(4) . . ? C81A C82A C83A 105.9(3) . . ? N17A C83A C82A 105.5(3) . . ? N17A C83A C84A 124.4(3) . . ? C82A C83A C84A 130.1(3) . . ? C85A C84A C89A 118.3(4) . . ? C85A C84A C83A 122.7(3) . . ? C89A C84A C83A 119.0(4) . . ? C86A C85A C84A 121.4(4) . . ? C85A C86A C87A 118.5(4) . . ? C88A C87A F90A 118.8(4) . . ? C88A C87A C86A 122.4(4) . . ? F90A C87A C86A 118.8(4) . . ? C87A C88A C89A 118.4(4) . . ? C88A C89A C84A 121.0(4) . . ? N12B Cu1B F2B 85.6(10) . . ? N12B Cu1B N7B 161.7(7) . . ? F2B Cu1B N7B 98.03(11) . . ? N12B Cu1B N9B 89.0(10) . . ? F2B Cu1B N9B 174.16(12) . . ? N7B Cu1B N9B 87.79(13) . . ? F2B Cu1B N12D 85.4(8) . . ? N7B Cu1B N12D 163.0(5) . . ? N9B Cu1B N12D 89.2(8) . . ? N12B Cu1B F1B 110.9(7) . . ? F2B Cu1B F1B 82.67(9) . . ? N7B Cu1B F1B 87.40(11) . . ? N9B Cu1B F1B 97.16(10) . . ? N12D Cu1B F1B 109.6(5) . . ? F3B Cu2B N4B 172.12(12) . . ? F3B Cu2B N14B 81.3(4) . . ? N4B Cu2B N14B 93.1(4) . . ? F3B Cu2B N1B 96.35(11) . . ? N4B Cu2B N1B 90.91(14) . . ? N14B Cu2B N1B 157.4(6) . . ? F3B Cu2B N14D 91.9(4) . . ? N4B Cu2B N14D 82.9(4) . . ? N1B Cu2B N14D 153.6(6) . . ? F3B Cu2B F1B 83.28(9) . . ? N4B Cu2B F1B 93.89(11) . . ? N14B Cu2B F1B 113.4(6) . . ? N1B Cu2B F1B 88.43(11) . . ? N14D Cu2B F1B 117.5(6) . . ? N2B Cu3B N3B 90.18(13) . . ? N2B Cu3B N6B 89.51(13) . . ? N3B Cu3B N6B 161.27(13) . . ? N2B Cu3B N16B 178.09(13) . . ? N3B Cu3B N16B 88.91(13) . . ? N6B Cu3B N16B 91.89(13) . . ? N2B Cu3B F1B 84.49(10) . . ? N3B Cu3B F1B 93.68(11) . . ? N6B Cu3B F1B 104.93(11) . . ? N16B Cu3B F1B 93.89(11) . . ? N10B Cu4B N5B 158.35(13) . . ? N10B Cu4B N8B 91.29(13) . . ? N5B Cu4B N8B 87.67(13) . . ? N10B Cu4B N18B 87.58(13) . . ? N5B Cu4B N18B 92.59(13) . . ? N8B Cu4B N18B 177.60(14) . . ? N10B Cu4B F1B 92.46(11) . . ? N5B Cu4B F1B 108.91(11) . . ? N8B Cu4B F1B 83.93(10) . . ? N18B Cu4B F1B 98.24(11) . . ? Cu4B F1B Cu1B 92.92(8) . . ? Cu4B F1B Cu2B 137.55(10) . . ? Cu1B F1B Cu2B 114.32(9) . . ? Cu4B F1B Cu3B 90.07(8) . . ? Cu1B F1B Cu3B 136.11(9) . . ? Cu2B F1B Cu3B 91.28(8) . . ? C3B N1B N2B 108.2(3) . . ? C3B N1B Cu2B 134.7(3) . . ? N2B N1B Cu2B 117.0(2) . . ? C1B N2B N1B 108.5(3) . . ? C1B N2B Cu3B 130.4(3) . . ? N1B N2B Cu3B 120.4(2) . . ? N2B C1B C2B 109.8(4) . . ? C1B C2B C3B 104.5(4) . . ? N1B C3B C2B 108.9(3) . . ? N1B C3B C4B 122.4(3) . . ? C2B C3B C4B 128.7(4) . . ? C9B C4B C5B 118.3(4) . . ? C9B C4B C3B 120.1(4) . . ? C5B C4B C3B 121.6(4) . . ? C4B C5B C6B 121.2(4) . . ? C7B C6B C5B 117.7(5) . . ? F10B C7B C8B 118.4(5) . . ? F10B C7B C6B 118.4(5) . . ? C8B C7B C6B 123.2(4) . . ? C7B C8B C9B 117.6(4) . . ? C8B C9B C4B 121.9(4) . . ? C13B N3B N4B 108.6(3) . . ? C13B N3B Cu3B 131.0(3) . . ? N4B N3B Cu3B 119.2(2) . . ? C11B N4B N3B 107.4(3) . . ? C11B N4B Cu2B 133.8(3) . . ? N3B N4B Cu2B 118.8(2) . . ? N4B C11B C12B 110.1(4) . . ? C11B C12B C13B 105.0(4) . . ? N3B C13B C12B 108.9(4) . . ? N3B C13B C14B 120.6(3) . . ? C12B C13B C14B 130.5(4) . . ? C19B C14B C15B 117.8(4) . . ? C19B C14B C13B 120.7(4) . . ? C15B C14B C13B 121.5(4) . . ? C16B C15B C14B 121.4(4) . . ? C17B C16B C15B 117.6(4) . . ? C18B C17B C16B 123.8(4) . . ? C18B C17B F20B 118.5(5) . . ? C16B C17B F20B 117.7(4) . . ? C17B C18B C19B 118.2(5) . . ? C18B C19B C14B 121.2(4) . . ? C23B N5B N6B 108.2(3) . . ? C23B N5B Cu4B 135.8(3) . . ? N6B N5B Cu4B 115.9(2) . . ? C21B N6B N5B 108.2(3) . . ? C21B N6B Cu3B 131.7(3) . . ? N5B N6B Cu3B 119.8(2) . . ? N6B C21B C22B 109.6(4) . . ? C21B C22B C23B 105.2(3) . . ? N5B C23B C22B 108.8(4) . . ? N5B C23B C24B 123.0(4) . . ? C22B C23B C24B 128.1(4) . . ? C29B C24B C25B 117.5(4) . . ? C29B C24B C23B 122.3(4) . . ? C25B C24B C23B 120.2(4) . . ? C26B C25B C24B 121.9(5) . . ? C27B C26B C25B 118.3(4) . . ? C26B C27B F30B 119.8(5) . . ? C26B C27B C28B 123.4(4) . . ? F30B C27B C28B 116.8(5) . . ? C27B C28B C29B 117.5(5) . . ? C28B C29B C24B 121.3(5) . . ? C33B N7B N8B 108.6(3) . . ? C33B N7B Cu1B 137.5(3) . . ? N8B N7B Cu1B 113.6(2) . . ? C31B N8B N7B 108.4(3) . . ? C31B N8B Cu4B 128.3(3) . . ? N7B N8B Cu4B 123.1(2) . . ? N8B C31B C32B 109.3(4) . . ? C31B C32B C33B 105.5(4) . . ? N7B C33B C32B 108.2(4) . . ? N7B C33B C34B 124.0(4) . . ? C32B C33B C34B 127.8(4) . . ? C35B C34B C39B 118.4(5) . . ? C35B C34B C33B 122.8(4) . . ? C39B C34B C33B 118.8(5) . . ? C34B C35B C36B 120.4(5) . . ? C37B C36B C35B 118.8(6) . . ? C36B C37B C38B 123.1(6) . . ? C36B C37B F40B 118.3(7) . . ? C38B C37B F40B 118.6(6) . . ? C37B C38B C39B 118.0(6) . . ? C38B C39B C34B 121.3(7) . . ? C43B N9B N10B 108.8(3) . . ? C43B N9B Cu1B 134.8(3) . . ? N10B N9B Cu1B 114.6(2) . . ? C41B N10B N9B 107.8(3) . . ? C41B N10B Cu4B 131.2(3) . . ? N9B N10B Cu4B 120.3(2) . . ? N10B C41B C42B 110.1(4) . . ? C41B C42B C43B 105.0(4) . . ? N9B C43B C42B 108.4(3) . . ? N9B C43B C44D 125.0(7) . . ? C42B C43B C44D 125.9(7) . . ? N9B C43B C44B 117.9(7) . . ? C42B C43B C44B 133.5(8) . . ? C45B C44B C49B 120.0 . . ? C45B C44B C43B 115.1(11) . . ? C49B C44B C43B 123.4(12) . . ? C44B C45B C46B 120.0 . . ? C47B C46B C45B 120.0 . . ? F50B C47B C46B 122(2) . . ? F50B C47B C48B 118(2) . . ? C46B C47B C48B 120.0 . . ? C47B C48B C49B 120.0 . . ? C48B C49B C44B 120.0 . . ? C45D C44D C49D 120.0 . . ? C45D C44D C43B 124.2(11) . . ? C49D C44D C43B 114.6(11) . . ? C46D C45D C44D 120.0 . . ? C45D C46D C47D 120.0 . . ? F50D C47D C48D 119(2) . . ? F50D C47D C46D 120(2) . . ? C48D C47D C46D 120.0 . . ? C47D C48D C49D 120.0 . . ? C48D C49D C44D 120.0 . . ? N12B N11B C53B 115.9(11) . . ? C51B N12B N11B 98.8(15) . . ? C51B N12B Cu1B 133.5(11) . . ? N11B N12B Cu1B 125.3(13) . . ? N12B C51B C52B 117.4(16) . . ? C53B C52B C51B 101.5(12) . . ? N11B C53B C52B 106.3(8) . . ? N11B C53B C54B 121.9(7) . . ? C52B C53B C54B 131.6(8) . . ? C59B C54B C55B 118.4(7) . . ? C59B C54B C53B 121.2(7) . . ? C55B C54B C53B 120.3(7) . . ? C56B C55B C54B 119.6(9) . . ? C55B C56B C57B 119.9(9) . . ? F60B C57B C58B 119.6(7) . . ? F60B C57B C56B 120.6(8) . . ? C58B C57B C56B 118.3(8) . . ? C57B C58B C59B 119.6(8) . . ? C54B C59B C58B 121.5(7) . . ? N12D N11D C53D 109.6(10) . . ? C51D N12D N11D 109.3(13) . . ? C51D N12D Cu1B 123.6(9) . . ? N11D N12D Cu1B 126.6(10) . . ? N12D C51D C52D 106.5(12) . . ? C53D C52D C51D 108.3(10) . . ? N11D C53D C52D 106.3(8) . . ? N11D C53D C54D 122.5(7) . . ? C52D C53D C54D 131.0(8) . . ? C59D C54D C55D 118.6(6) . . ? C59D C54D C53D 123.0(6) . . ? C55D C54D C53D 118.2(6) . . ? C56D C55D C54D 120.1(7) . . ? C57D C56D C55D 118.5(7) . . ? C58D C57D F60D 119.4(8) . . ? C58D C57D C56D 124.0(6) . . ? F60D C57D C56D 116.5(7) . . ? C57D C58D C59D 117.6(7) . . ? C54D C59D C58D 121.0(6) . . ? N14B N13B C63B 113(2) . . ? C61B N14B N13B 104(2) . . ? C61B N14B Cu2B 129.8(17) . . ? N13B N14B Cu2B 124.3(14) . . ? N14B C61B C62B 111.4(15) . . ? C63B C62B C61B 105.4(12) . . ? N13B C63B C62B 105.8(14) . . ? N13B C63B C64B 125.6(18) . . ? C62B C63B C64B 128.6(16) . . ? C65B C64B C69B 120.0 . . ? C65B C64B C63B 117.8(15) . . ? C69B C64B C63B 122.2(15) . . ? C66B C65B C64B 120.0 . . ? C65B C66B C67B 120.0 . . ? F70B C67B C68B 114.0(13) . . ? F70B C67B C66B 125.9(13) . . ? C68B C67B C66B 120.0 . . ? C69B C68B C67B 120.0 . . ? C68B C69B C64B 120.0 . . ? N14D N13D C63D 110(2) . . ? C61D N14D N13D 107.4(19) . . ? C61D N14D Cu2B 127.9(15) . . ? N13D N14D Cu2B 124.7(11) . . ? N14D C61D C62D 109.6(13) . . ? C63D C62D C61D 105.4(9) . . ? N13D C63D C62D 107.6(15) . . ? N13D C63D C64D 122.2(17) . . ? C62D C63D C64D 130.2(15) . . ? C65D C64D C69D 120.0 . . ? C65D C64D C63D 126.4(15) . . ? C69D C64D C63D 113.6(15) . . ? C66D C65D C64D 120.0 . . ? C65D C66D C67D 120.0 . . ? F70D C67D C66D 116.6(19) . . ? F70D C67D C68D 123.4(19) . . ? C66D C67D C68D 120.0 . . ? C69D C68D C67D 120.0 . . ? C68D C69D C64D 120.0 . . ? C73B N15B N16B 112.1(3) . . ? C71B N16B N15B 105.3(3) . . ? C71B N16B Cu3B 132.0(3) . . ? N15B N16B Cu3B 120.6(2) . . ? N16B C71B C72B 110.5(4) . . ? C73B C72B C71B 106.0(4) . . ? N15B C73B C72B 106.0(4) . . ? N15B C73B C74B 121.0(12) . . ? C72B C73B C74B 132.1(12) . . ? N15B C73B C74D 122.8(9) . . ? C72B C73B C74D 131.1(9) . . ? C74B C73B C74D 10(2) . . ? C75B C74B C79B 120.0 . . ? C75B C74B C73B 122.8(17) . . ? C79B C74B C73B 117.1(17) . . ? C74B C75B C76B 120.0 . . ? C77B C76B C75B 120.0 . . ? F80B C77B C76B 122(3) . . ? F80B C77B C78B 118(3) . . ? C76B C77B C78B 120.0 . . ? C79B C78B C77B 120.0 . . ? C78B C79B C74B 120.0 . . ? C75D C74D C79D 120.0 . . ? C75D C74D C73B 117.9(12) . . ? C79D C74D C73B 122.1(12) . . ? C74D C75D C76D 120.0 . . ? C75D C76D C77D 120.0 . . ? F80D C77D C78D 119.3(18) . . ? F80D C77D C76D 120.7(18) . . ? C78D C77D C76D 120.0 . . ? C77D C78D C79D 120.0 . . ? C78D C79D C74D 120.0 . . ? C83B N17B N18B 111.4(3) . . ? C81B N18B N17B 105.6(3) . . ? C81B N18B Cu4B 129.4(3) . . ? N17B N18B Cu4B 123.0(2) . . ? N18B C81B C82B 110.5(4) . . ? C83B C82B C81B 105.4(3) . . ? N17B C83B C82B 107.1(3) . . ? N17B C83B C84B 124.1(3) . . ? C82B C83B C84B 128.8(3) . . ? C85B C84B C89B 118.0(4) . . ? C85B C84B C83B 122.1(3) . . ? C89B C84B C83B 119.8(4) . . ? C84B C85B C86B 121.3(4) . . ? C87B C86B C85B 117.9(4) . . ? C88B C87B C86B 123.2(4) . . ? C88B C87B F90B 118.5(4) . . ? C86B C87B F90B 118.3(4) . . ? C87B C88B C89B 118.2(4) . . ? C88B C89B C84B 121.4(4) . . ? C5E N1E N2E 109.4(12) . . ? C3E N2E N1E 104.5(13) . . ? N2E C3E C4E 112.9(13) . . ? C3E C4E C5E 102.5(11) . . ? N1E C5E C4E 109.0(10) . . ? N1E C5E C6E 128.6(10) . . ? C4E C5E C6E 121.3(10) . . ? C7E C6E C11E 120.0 . . ? C7E C6E C5E 119.7(6) . . ? C11E C6E C5E 120.0(6) . . ? C8E C7E C6E 120.0 . . ? C9E C8E C7E 120.0 . . ? F12E C9E C8E 119.9 . . ? F12E C9E C10E 119.7 . . ? C8E C9E C10E 120.0 . . ? C11E C10E C9E 120.0 . . ? C10E C11E C6E 120.0 . . ? C17E N13E N14E 100.7(12) . . ? C15E N14E N13E 113.4(18) . . ? N14E C15E C16E 107.3(18) . . ? C17E C16E C15E 101.6(15) . . ? N13E C17E C16E 115.2(12) . . ? N13E C17E C18E 128.1(13) . . ? C16E C17E C18E 115.1(12) . . ? C19E C18E C23E 120.0 . . ? C19E C18E C17E 116.7(8) . . ? C23E C18E C17E 123.1(8) . . ? C20E C19E C18E 120.0 . . ? C21E C20E C19E 120.0 . . ? F24E C21E C20E 136.2 . . ? F24E C21E C22E 103.7 . . ? C20E C21E C22E 120.0 . . ? C23E C22E C21E 120.0 . . ? C22E C23E C18E 120.0 . . ? Cl2S C1S Cl3S 108.9(3) . . ? Cl5S C4S Cl6S 116.9(10) . . ? Cl9S C7S Cl8S 110.1(14) . . ? Cl11S C10S Cl12S 102.6(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11A H11A F3A 0.88 1.98 2.752(4) 145.5 . N13A H13A F2A 0.88 1.81 2.66(2) 162.2 . N13C H13C F2A 0.88 1.91 2.749(19) 157.5 . N15A H15A F2A 0.88 1.93 2.693(4) 143.7 . N17A H17A F3A 0.88 1.78 2.647(4) 168.9 . N11B H11B F3B 0.88 2.05 2.787(8) 141.1 . N11D H11D F3B 0.88 1.82 2.656(9) 157.6 . N13B H13B F2B 0.88 1.93 2.73(2) 149.2 . N13D H13D F2B 0.88 1.90 2.73(2) 157.9 . N15B H15B F2B 0.88 1.90 2.689(4) 148.7 . N17B H17B F3B 0.88 1.78 2.644(4) 167.5 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.957 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.135 #=END data_c:\datasets\leeds\smcupy~1\smcuphf _database_code_depnum_ccdc_archive 'CCDC 632227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[5-{4-fluorophenyl}pyrazolido]-bis[5-{4-fluorophenyl}pyrazole]copper(II) ; _chemical_name_common ;Bis(5-(4-fluorophenyl)pyrazolido)-bis(5-(4- fluorophenyl)pyrazole)copper(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 Cu F4 N8' _chemical_formula_sum 'C36 H26 Cu F4 N8' _chemical_formula_weight 710.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 36.1535(6) _cell_length_b 7.69370(10) _cell_length_c 10.9951(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3058.33(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21870 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.562 _exptl_absorpt_correction_T_max 0.940 _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 ; 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_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 diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21870 _diffrn_reflns_av_R_equivalents 0.1084 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6837 _reflns_number_gt 5547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _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. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. The protonated and deprotonated N atoms of each hydrogen-bonded pair were distinguished in two ways. First, because appropriately positioned residual Fourier peaks were present in the vicinity of N3 and N27, but not N15 and N39. Second, because the Cu---N bonds to the protonated pyrazole N atoms N2 and N26 are 6 sus longer than those to the deprotonated pyrazolido ligand donors N14 and N38. The deepest residual Fourier hole of -1.0 e.\%A^-3^ is 0.9\%A from Cu1. ; _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^)+(0.0980P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.043(16) _refine_ls_number_reflns 6837 _refine_ls_number_parameters 442 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1481 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.255762(13) 0.19783(6) 0.50106(7) 0.02972(15) Uani 1 1 d . . . N2 N 0.29437(9) 0.3662(5) 0.4502(3) 0.0294(8) Uani 1 1 d . . . N3 N 0.33066(9) 0.3303(4) 0.4635(3) 0.0258(8) Uani 1 1 d . . . H3 H 0.3394 0.2363 0.4989 0.031 Uiso 1 1 calc R . . C4 C 0.35194(11) 0.4576(5) 0.4152(4) 0.0253(8) Uani 1 1 d . . . C5 C 0.32780(11) 0.5817(6) 0.3676(4) 0.0305(9) Uani 1 1 d . . . H5 H 0.3343 0.6868 0.3275 0.037 Uiso 1 1 calc R . . C6 C 0.29232(12) 0.5198(6) 0.3909(4) 0.0329(10) Uani 1 1 d . . . H6 H 0.2700 0.5769 0.3685 0.039 Uiso 1 1 calc R . . C7 C 0.39254(11) 0.4505(5) 0.4210(4) 0.0246(8) Uani 1 1 d . . . C8 C 0.41015(11) 0.3540(5) 0.5115(4) 0.0277(8) Uani 1 1 d . . . H8 H 0.3958 0.2948 0.5708 0.033 Uiso 1 1 calc R . . C9 C 0.44868(12) 0.3434(6) 0.5162(4) 0.0318(9) Uani 1 1 d . . . H9 H 0.4608 0.2763 0.5767 0.038 Uiso 1 1 calc R . . C10 C 0.46843(10) 0.4335(5) 0.4300(4) 0.0265(8) Uani 1 1 d . . . C11 C 0.45232(11) 0.5302(6) 0.3404(4) 0.0289(9) Uani 1 1 d . . . H11 H 0.4671 0.5903 0.2825 0.035 Uiso 1 1 calc R . . C12 C 0.41400(11) 0.5390(5) 0.3354(4) 0.0261(8) Uani 1 1 d . . . H12 H 0.4023 0.6055 0.2735 0.031 Uiso 1 1 calc R . . F13 F 0.50599(6) 0.4267(4) 0.4362(3) 0.0371(6) Uani 1 1 d . . . N14 N 0.28894(9) 0.0236(4) 0.5700(3) 0.0245(7) Uani 1 1 d . . . N15 N 0.32626(9) 0.0130(4) 0.5634(3) 0.0243(7) Uani 1 1 d . . . C16 C 0.33729(11) -0.1234(5) 0.6326(3) 0.0230(8) Uani 1 1 d . . . C17 C 0.30586(12) -0.2007(5) 0.6857(4) 0.0282(9) Uani 1 1 d . . . H17 H 0.3052 -0.2980 0.7389 0.034 Uiso 1 1 calc R . . C18 C 0.27653(12) -0.1062(6) 0.6445(4) 0.0290(9) Uani 1 1 d . . . H18 H 0.2514 -0.1273 0.6644 0.035 Uiso 1 1 calc R . . C19 C 0.37617(11) -0.1740(5) 0.6430(3) 0.0223(8) Uani 1 1 d . . . C20 C 0.40279(11) -0.1097(5) 0.5638(4) 0.0278(9) Uani 1 1 d . . . H20 H 0.3957 -0.0310 0.5014 0.033 Uiso 1 1 calc R . . C21 C 0.43978(12) -0.1588(6) 0.5743(4) 0.0275(8) Uani 1 1 d . . . H21 H 0.4578 -0.1155 0.5193 0.033 Uiso 1 1 calc R . . C22 C 0.44954(11) -0.2714(6) 0.6662(4) 0.0267(8) Uani 1 1 d . . . C23 C 0.42405(12) -0.3391(6) 0.7472(4) 0.0303(9) Uani 1 1 d . . . H23 H 0.4314 -0.4166 0.8099 0.036 Uiso 1 1 calc R . . C24 C 0.38760(12) -0.2903(5) 0.7341(4) 0.0274(9) Uani 1 1 d . . . H24 H 0.3697 -0.3367 0.7882 0.033 Uiso 1 1 calc R . . F25 F 0.48559(7) -0.3200(4) 0.6766(2) 0.0363(6) Uani 1 1 d . . . N26 N 0.21872(9) 0.3727(5) 0.5517(3) 0.0265(7) Uani 1 1 d . . . N27 N 0.18206(9) 0.3354(5) 0.5590(3) 0.0260(7) Uani 1 1 d . . . H27 H 0.1717 0.2415 0.5285 0.031 Uiso 1 1 calc R . . C28 C 0.16346(11) 0.4618(5) 0.6194(3) 0.0241(8) Uani 1 1 d . . . C29 C 0.18914(12) 0.5868(6) 0.6507(4) 0.0300(9) Uani 1 1 d . . . H29 H 0.1847 0.6922 0.6932 0.036 Uiso 1 1 calc R . . C30 C 0.22259(12) 0.5265(6) 0.6072(4) 0.0303(9) Uani 1 1 d . . . H30 H 0.2454 0.5865 0.6157 0.036 Uiso 1 1 calc R . . C31 C 0.12328(11) 0.4505(5) 0.6377(3) 0.0244(8) Uani 1 1 d . . . C32 C 0.10103(11) 0.3537(6) 0.5606(4) 0.0275(9) Uani 1 1 d . . . H32 H 0.1119 0.2934 0.4942 0.033 Uiso 1 1 calc R . . C33 C 0.06304(12) 0.3437(6) 0.5791(4) 0.0303(9) Uani 1 1 d . . . H33 H 0.0478 0.2762 0.5269 0.036 Uiso 1 1 calc R . . C34 C 0.04821(11) 0.4336(6) 0.6746(4) 0.0312(9) Uani 1 1 d . . . C35 C 0.06890(12) 0.5316(6) 0.7534(4) 0.0323(10) Uani 1 1 d . . . H35 H 0.0575 0.5918 0.8189 0.039 Uiso 1 1 calc R . . C36 C 0.10671(12) 0.5407(5) 0.7352(4) 0.0291(9) Uani 1 1 d . . . H36 H 0.1216 0.6080 0.7886 0.035 Uiso 1 1 calc R . . F37 F 0.01116(7) 0.4241(4) 0.6919(3) 0.0415(6) Uani 1 1 d . . . N38 N 0.22093(9) 0.0242(4) 0.4413(3) 0.0254(7) Uani 1 1 d . . . N39 N 0.18374(9) 0.0158(4) 0.4647(3) 0.0242(7) Uani 1 1 d . . . C40 C 0.17066(11) -0.1264(5) 0.4042(3) 0.0230(8) Uani 1 1 d . . . C41 C 0.19951(12) -0.2081(5) 0.3415(4) 0.0269(9) Uani 1 1 d . . . H41 H 0.1981 -0.3089 0.2918 0.032 Uiso 1 1 calc R . . C42 C 0.23036(12) -0.1103(6) 0.3677(4) 0.0278(9) Uani 1 1 d . . . H42 H 0.2546 -0.1335 0.3387 0.033 Uiso 1 1 calc R . . C43 C 0.13170(11) -0.1769(5) 0.4141(3) 0.0209(8) Uani 1 1 d . . . C44 C 0.10921(10) -0.1167(5) 0.5085(4) 0.0272(8) Uani 1 1 d . . . H44 H 0.1194 -0.0425 0.5689 0.033 Uiso 1 1 calc R . . C45 C 0.07224(11) -0.1636(5) 0.5154(4) 0.0269(8) Uani 1 1 d . . . H45 H 0.0569 -0.1208 0.5789 0.032 Uiso 1 1 calc R . . C46 C 0.05834(11) -0.2732(6) 0.4283(4) 0.0269(8) Uani 1 1 d . . . C47 C 0.07925(11) -0.3386(5) 0.3346(4) 0.0279(9) Uani 1 1 d . . . H47 H 0.0688 -0.4152 0.2762 0.033 Uiso 1 1 calc R . . C48 C 0.11611(12) -0.2896(5) 0.3277(4) 0.0251(8) Uani 1 1 d . . . H48 H 0.1311 -0.3330 0.2635 0.030 Uiso 1 1 calc R . . F49 F 0.02229(7) -0.3231(3) 0.4362(3) 0.0374(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0255(2) 0.0210(2) 0.0426(3) 0.0014(2) -0.0018(3) 0.00006(19) N2 0.0248(17) 0.0230(18) 0.0404(19) 0.0037(15) -0.0004(16) -0.0011(14) N3 0.0182(15) 0.0204(17) 0.0389(19) 0.0039(13) 0.0013(14) -0.0017(13) C4 0.029(2) 0.0197(19) 0.0278(18) 0.0023(15) 0.0037(17) -0.0040(16) C5 0.026(2) 0.024(2) 0.041(2) 0.0096(18) -0.0014(18) -0.0036(17) C6 0.030(2) 0.021(2) 0.047(2) 0.0058(19) 0.0000(19) -0.0005(17) C7 0.0275(19) 0.0181(19) 0.0282(18) -0.0059(15) 0.0034(16) -0.0031(15) C8 0.0276(19) 0.0247(19) 0.031(2) 0.0042(19) 0.001(2) -0.0025(15) C9 0.029(2) 0.033(2) 0.033(2) 0.001(2) -0.0034(19) 0.0036(16) C10 0.0189(18) 0.027(2) 0.034(2) -0.0053(17) 0.0001(16) -0.0009(16) C11 0.030(2) 0.025(2) 0.031(2) 0.0015(17) 0.0061(17) -0.0040(17) C12 0.029(2) 0.022(2) 0.0271(18) 0.0044(16) -0.0006(17) -0.0014(16) F13 0.0235(12) 0.0391(15) 0.0487(15) 0.0013(12) 0.0011(11) -0.0004(11) N14 0.0192(16) 0.0205(17) 0.0337(17) 0.0049(14) -0.0011(14) -0.0027(13) N15 0.0217(16) 0.0197(17) 0.0315(17) 0.0018(14) -0.0017(14) 0.0016(13) C16 0.027(2) 0.0173(19) 0.0253(18) 0.0001(15) -0.0018(16) -0.0001(16) C17 0.027(2) 0.025(2) 0.033(2) 0.0018(16) 0.0014(18) -0.0052(16) C18 0.024(2) 0.025(2) 0.038(2) -0.0015(17) 0.0006(17) -0.0012(17) C19 0.029(2) 0.0161(18) 0.0224(18) -0.0023(14) -0.0033(16) -0.0027(15) C20 0.030(2) 0.024(2) 0.030(2) 0.0007(18) 0.0026(18) 0.0029(17) C21 0.027(2) 0.025(2) 0.031(2) 0.0025(17) 0.0035(18) 0.0005(17) C22 0.0235(19) 0.024(2) 0.032(2) -0.0018(17) -0.0004(17) 0.0042(16) C23 0.033(2) 0.024(2) 0.033(2) 0.0041(17) -0.0029(18) 0.0053(18) C24 0.031(2) 0.022(2) 0.029(2) 0.0013(16) 0.0002(17) -0.0023(16) F25 0.0267(12) 0.0402(16) 0.0421(14) 0.0057(11) -0.0013(12) 0.0116(11) N26 0.0233(16) 0.0188(17) 0.0375(18) -0.0029(14) -0.0030(15) -0.0024(14) N27 0.0232(17) 0.0203(18) 0.0345(18) -0.0040(14) 0.0002(15) -0.0016(14) C28 0.0271(19) 0.022(2) 0.0233(18) -0.0003(15) -0.0012(16) 0.0058(16) C29 0.033(2) 0.019(2) 0.038(2) -0.0040(17) -0.0025(18) 0.0011(17) C30 0.026(2) 0.022(2) 0.042(2) -0.0023(18) -0.0045(18) -0.0018(17) C31 0.027(2) 0.020(2) 0.0261(18) 0.0006(16) 0.0017(16) 0.0046(16) C32 0.029(2) 0.027(2) 0.0268(19) -0.0004(17) -0.0017(17) 0.0022(17) C33 0.027(2) 0.032(2) 0.032(2) 0.0000(18) -0.0021(18) -0.0018(18) C34 0.027(2) 0.023(2) 0.043(2) 0.0085(19) 0.0045(18) 0.0034(17) C35 0.038(2) 0.026(2) 0.033(2) -0.0032(18) 0.0097(19) 0.0063(18) C36 0.036(2) 0.023(2) 0.029(2) -0.0048(17) -0.0004(17) 0.0042(18) F37 0.0258(12) 0.0444(16) 0.0542(16) 0.0061(13) 0.0081(12) 0.0006(12) N38 0.0214(16) 0.0208(17) 0.0341(17) 0.0003(15) -0.0022(14) 0.0005(13) N39 0.0194(15) 0.0217(17) 0.0316(17) 0.0013(13) -0.0022(13) -0.0017(13) C40 0.0256(19) 0.0188(19) 0.0246(18) 0.0011(15) -0.0022(16) -0.0010(15) C41 0.030(2) 0.020(2) 0.031(2) -0.0031(16) 0.0023(17) -0.0007(16) C42 0.024(2) 0.025(2) 0.035(2) -0.0006(16) 0.0041(17) 0.0028(17) C43 0.0219(19) 0.0152(17) 0.0256(18) 0.0010(14) -0.0031(16) -0.0009(15) C44 0.0313(19) 0.024(2) 0.0270(18) -0.0013(18) -0.002(2) -0.0008(15) C45 0.0266(19) 0.027(2) 0.028(2) 0.0022(17) 0.0030(18) 0.0048(15) C46 0.026(2) 0.027(2) 0.028(2) 0.0026(17) 0.0006(17) -0.0024(17) C47 0.031(2) 0.020(2) 0.032(2) -0.0008(16) -0.0029(18) -0.0038(17) C48 0.027(2) 0.022(2) 0.0261(19) 0.0001(16) 0.0018(17) 0.0015(16) F49 0.0254(12) 0.0401(15) 0.0468(14) -0.0007(12) 0.0029(12) -0.0104(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N38 1.950(3) . ? Cu1 N14 1.952(3) . ? Cu1 N26 1.978(4) . ? Cu1 N2 1.985(4) . ? N2 N3 1.348(5) . ? N2 C6 1.352(6) . ? N3 C4 1.354(5) . ? C4 C5 1.395(6) . ? C4 C7 1.470(5) . ? C5 C6 1.392(6) . ? C7 C8 1.396(6) . ? C7 C12 1.397(6) . ? C8 C9 1.396(6) . ? C9 C10 1.374(6) . ? C10 F13 1.361(4) . ? C10 C11 1.365(6) . ? C11 C12 1.388(6) . ? N14 N15 1.354(5) . ? N14 C18 1.367(6) . ? N15 C16 1.356(5) . ? C16 C17 1.409(6) . ? C16 C19 1.463(6) . ? C17 C18 1.363(6) . ? C19 C20 1.389(6) . ? C19 C24 1.405(6) . ? C20 C21 1.394(6) . ? C21 C22 1.377(6) . ? C22 F25 1.361(5) . ? C22 C23 1.383(6) . ? C23 C24 1.378(6) . ? N26 C30 1.339(5) . ? N26 N27 1.358(5) . ? N27 C28 1.356(5) . ? C28 C29 1.380(6) . ? C28 C31 1.469(6) . ? C29 C30 1.380(6) . ? C31 C32 1.386(6) . ? C31 C36 1.410(5) . ? C32 C33 1.391(6) . ? C33 C34 1.367(6) . ? C34 F37 1.355(5) . ? C34 C35 1.370(7) . ? C35 C36 1.383(6) . ? N38 C42 1.357(5) . ? N38 N39 1.370(4) . ? N39 C40 1.365(5) . ? C40 C41 1.400(6) . ? C40 C43 1.465(5) . ? C41 C42 1.376(6) . ? C43 C44 1.398(6) . ? C43 C48 1.404(5) . ? C44 C45 1.387(5) . ? C45 C46 1.372(6) . ? C46 F49 1.362(5) . ? C46 C47 1.374(6) . ? C47 C48 1.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N38 Cu1 N14 93.27(13) . . ? N38 Cu1 N26 97.10(13) . . ? N14 Cu1 N26 140.69(16) . . ? N38 Cu1 N2 143.76(16) . . ? N14 Cu1 N2 97.21(14) . . ? N26 Cu1 N2 96.41(14) . . ? N3 N2 C6 106.5(3) . . ? N3 N2 Cu1 121.3(3) . . ? C6 N2 Cu1 131.9(3) . . ? N2 N3 C4 111.3(3) . . ? N3 C4 C5 106.7(3) . . ? N3 C4 C7 121.6(3) . . ? C5 C4 C7 131.7(4) . . ? C6 C5 C4 105.9(4) . . ? N2 C6 C5 109.7(4) . . ? C8 C7 C12 119.1(4) . . ? C8 C7 C4 120.4(3) . . ? C12 C7 C4 120.5(4) . . ? C7 C8 C9 120.8(4) . . ? C10 C9 C8 117.6(4) . . ? F13 C10 C11 118.8(4) . . ? F13 C10 C9 117.7(4) . . ? C11 C10 C9 123.4(4) . . ? C10 C11 C12 118.7(4) . . ? C11 C12 C7 120.3(4) . . ? N15 N14 C18 108.4(3) . . ? N15 N14 Cu1 129.3(3) . . ? C18 N14 Cu1 122.2(3) . . ? N14 N15 C16 108.0(3) . . ? N15 C16 C17 108.8(4) . . ? N15 C16 C19 122.2(4) . . ? C17 C16 C19 129.1(4) . . ? C18 C17 C16 105.3(4) . . ? C17 C18 N14 109.5(4) . . ? C20 C19 C24 118.0(4) . . ? C20 C19 C16 121.5(4) . . ? C24 C19 C16 120.5(4) . . ? C19 C20 C21 121.1(4) . . ? C22 C21 C20 118.5(4) . . ? F25 C22 C21 118.7(4) . . ? F25 C22 C23 118.7(4) . . ? C21 C22 C23 122.6(4) . . ? C24 C23 C22 117.9(4) . . ? C23 C24 C19 122.0(4) . . ? C30 N26 N27 105.2(3) . . ? C30 N26 Cu1 131.2(3) . . ? N27 N26 Cu1 122.2(3) . . ? C28 N27 N26 111.2(3) . . ? N27 C28 C29 106.7(4) . . ? N27 C28 C31 121.0(4) . . ? C29 C28 C31 132.3(4) . . ? C28 C29 C30 105.6(4) . . ? N26 C30 C29 111.3(4) . . ? C32 C31 C36 118.8(4) . . ? C32 C31 C28 121.5(3) . . ? C36 C31 C28 119.7(4) . . ? C31 C32 C33 120.9(4) . . ? C34 C33 C32 118.2(4) . . ? F37 C34 C33 117.9(4) . . ? F37 C34 C35 118.7(4) . . ? C33 C34 C35 123.3(4) . . ? C34 C35 C36 118.4(4) . . ? C35 C36 C31 120.3(4) . . ? C42 N38 N39 108.8(3) . . ? C42 N38 Cu1 124.1(3) . . ? N39 N38 Cu1 127.1(3) . . ? C40 N39 N38 106.7(3) . . ? N39 C40 C41 110.0(3) . . ? N39 C40 C43 120.6(3) . . ? C41 C40 C43 129.3(4) . . ? C42 C41 C40 104.8(4) . . ? N38 C42 C41 109.8(4) . . ? C44 C43 C48 118.3(4) . . ? C44 C43 C40 121.8(3) . . ? C48 C43 C40 120.0(3) . . ? C45 C44 C43 121.0(4) . . ? C46 C45 C44 118.4(4) . . ? F49 C46 C45 118.7(4) . . ? F49 C46 C47 118.1(4) . . ? C45 C46 C47 123.2(4) . . ? C46 C47 C48 118.0(4) . . ? C47 C48 C43 121.2(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 N15 0.88 1.92 2.682(5) 144.2 . N27 H27 N39 0.88 1.92 2.669(5) 141.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.661 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.102