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 'S. Brooker' _publ_contact_author_address ; Chemistry Department University of Otago PO Box 56 Dunedin 9054 NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; Pyridazine-bridged copper(I) complexes of bis-bidentate ligands: tetranuclear [2 x 2] grid versus dinuclear side-by-side architectures as a function of ligand substituents ; loop_ _publ_author_name 'S. Brooker' 'Yanhua Lan.' 'Jason R. Price' # Attachment 'p_methyl_Cu_complex.cif' data_jp107cus _database_code_depnum_ccdc_archive 'CCDC 629020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C80 H72 Cu4 N16, 4(F6 P), 2(C3 H6 O)' _chemical_formula_sum 'C86 H84 Cu4 F24 N16 O2 P4' _chemical_formula_weight 2207.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6321(4) _cell_length_b 16.2001(4) _cell_length_c 22.2191(5) _cell_angle_alpha 94.0060(10) _cell_angle_beta 102.1290(10) _cell_angle_gamma 94.7260(10) _cell_volume 5111.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106393 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 20051 _reflns_number_gt 15002 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-H atoms ANIS. Two of the four PF6 anions are ?twirl? disordered with sof of 90:10 for one and 60:40 for the other. While the two acetones of solvation could be readily modelled, two diethylethers were substantially disordered and were removed with squeeze (Electron count /cell =150, 2 diethylethers in the asymmetric unit would account for 148 electrons/cell) ; _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^)+(0.0550P)^2^+2.1428P] 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 20051 _refine_ls_number_parameters 1264 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.16143(2) 0.306681(18) 0.361455(13) 0.01810(8) Uani 1 1 d . . . Cu2 Cu 1.06274(2) 0.365346(18) 0.201188(14) 0.01968(8) Uani 1 1 d . . . Cu3 Cu 0.95794(2) 0.147132(18) 0.300353(14) 0.01854(8) Uani 1 1 d . . . Cu4 Cu 0.84511(2) 0.208861(19) 0.145170(14) 0.01946(8) Uani 1 1 d . . . N1 N 1.19597(15) 0.26687(12) 0.28290(9) 0.0181(5) Uani 1 1 d . . . N2 N 1.15759(15) 0.28480(12) 0.22556(9) 0.0188(5) Uani 1 1 d . . . C2 C 1.18988(19) 0.25272(16) 0.17713(12) 0.0226(6) Uani 1 1 d . . . C3 C 1.2602(2) 0.19906(16) 0.18410(13) 0.0270(6) Uani 1 1 d . . . H3 H 1.2814 0.1768 0.1493 0.032 Uiso 1 1 calc R . . C4 C 1.29784(19) 0.17934(16) 0.24193(13) 0.0260(6) Uani 1 1 d . . . H4 H 1.3457 0.1427 0.2487 0.031 Uiso 1 1 calc R . . C5 C 1.26401(18) 0.21457(15) 0.29118(12) 0.0214(6) Uani 1 1 d . . . C6 C 1.29804(19) 0.19786(16) 0.35497(12) 0.0234(6) Uani 1 1 d . . . H6 H 1.3495 0.1657 0.3659 0.028 Uiso 1 1 calc R . . N3 N 1.25701(15) 0.22753(13) 0.39633(10) 0.0203(5) Uani 1 1 d . . . C8 C 1.28648(18) 0.21081(16) 0.45934(12) 0.0224(6) Uani 1 1 d . . . C9 C 1.3367(2) 0.14412(18) 0.47733(14) 0.0316(7) Uani 1 1 d . . . H9 H 1.3532 0.1072 0.4471 0.038 Uiso 1 1 calc R . . C10 C 1.3626(2) 0.1317(2) 0.53954(15) 0.0384(8) Uani 1 1 d . . . H10 H 1.3980 0.0866 0.5515 0.046 Uiso 1 1 calc R . . C11 C 1.3380(2) 0.1836(2) 0.58449(14) 0.0333(7) Uani 1 1 d . . . C12 C 1.2863(2) 0.24924(19) 0.56555(13) 0.0325(7) Uani 1 1 d . . . H12 H 1.2686 0.2855 0.5956 0.039 Uiso 1 1 calc R . . C13 C 1.26033(19) 0.26259(17) 0.50380(12) 0.0257(6) Uani 1 1 d . . . H13 H 1.2245 0.3073 0.4918 0.031 Uiso 1 1 calc R . . C14 C 1.3627(2) 0.1670(2) 0.65131(15) 0.0480(9) Uani 1 1 d . . . H14A H 1.3127 0.1292 0.6607 0.058 Uiso 1 1 calc R . . H14B H 1.3695 0.2195 0.6773 0.058 Uiso 1 1 calc R . . H14C H 1.4220 0.1415 0.6596 0.058 Uiso 1 1 calc R . . C16 C 1.1434(2) 0.27723(16) 0.11724(12) 0.0257(6) Uani 1 1 d . . . H16 H 1.1579 0.2542 0.0802 0.031 Uiso 1 1 calc R . . N4 N 1.08251(16) 0.33053(13) 0.11532(10) 0.0225(5) Uani 1 1 d . . . C18 C 1.0329(2) 0.35329(17) 0.05711(12) 0.0306(7) Uani 1 1 d . . . C19 C 1.0547(3) 0.3294(2) 0.00091(14) 0.0538(10) Uani 1 1 d . . . H19 H 1.1062 0.2977 -0.0003 0.065 Uiso 1 1 calc R . . C20 C 1.0007(4) 0.3521(2) -0.05347(15) 0.0666(13) Uani 1 1 d . . . H20 H 1.0145 0.3338 -0.0918 0.080 Uiso 1 1 calc R . . C21 C 0.9276(3) 0.4005(2) -0.05323(16) 0.0545(11) Uani 1 1 d . . . C22 C 0.9076(3) 0.4239(2) 0.00253(17) 0.0514(10) Uani 1 1 d . . . H22 H 0.8563 0.4558 0.0035 0.062 Uiso 1 1 calc R . . C23 C 0.9600(2) 0.40223(19) 0.05778(14) 0.0358(7) Uani 1 1 d . . . H23 H 0.9458 0.4210 0.0959 0.043 Uiso 1 1 calc R . . C24 C 0.8723(3) 0.4248(3) -0.11385(17) 0.0781(16) Uani 1 1 d . . . H24A H 0.9122 0.4636 -0.1316 0.094 Uiso 1 1 calc R . . H24B H 0.8175 0.4517 -0.1066 0.094 Uiso 1 1 calc R . . H24C H 0.8513 0.3750 -0.1427 0.094 Uiso 1 1 calc R . . N31 N 0.99216(15) 0.11575(12) 0.21987(9) 0.0193(5) Uani 1 1 d . . . N32 N 0.95202(15) 0.13840(12) 0.16440(9) 0.0192(5) Uani 1 1 d . . . C32 C 0.98429(19) 0.11299(16) 0.11446(12) 0.0224(6) Uani 1 1 d . . . C33 C 1.05722(19) 0.06159(16) 0.11782(12) 0.0250(6) Uani 1 1 d . . . H33 H 1.0802 0.0459 0.0822 0.030 Uiso 1 1 calc R . . C34 C 1.09432(19) 0.03476(16) 0.17382(12) 0.0259(6) Uani 1 1 d . . . H34 H 1.1422 -0.0019 0.1781 0.031 Uiso 1 1 calc R . . C35 C 1.05957(18) 0.06302(15) 0.22471(12) 0.0218(6) Uani 1 1 d . . . C36 C 1.09191(19) 0.03877(16) 0.28741(12) 0.0240(6) Uani 1 1 d . . . H36 H 1.1395 0.0021 0.2961 0.029 Uiso 1 1 calc R . . N33 N 1.05386(15) 0.06862(13) 0.33033(10) 0.0207(5) Uani 1 1 d . . . C46 C 0.93509(19) 0.14102(16) 0.05650(12) 0.0239(6) Uani 1 1 d . . . H46 H 0.9534 0.1270 0.0188 0.029 Uiso 1 1 calc R . . N34 N 0.86650(16) 0.18510(13) 0.05778(9) 0.0211(5) Uani 1 1 d . . . C38 C 1.08054(18) 0.04545(16) 0.39177(12) 0.0229(6) Uani 1 1 d . . . C39 C 1.07283(18) 0.10281(16) 0.43972(12) 0.0228(6) Uani 1 1 d . . . H39 H 1.0491 0.1545 0.4308 0.027 Uiso 1 1 calc R . . C40 C 1.09988(19) 0.08433(18) 0.50059(13) 0.0270(6) Uani 1 1 d . . . H40 H 1.0968 0.1245 0.5332 0.032 Uiso 1 1 calc R . . C41 C 1.13143(19) 0.00775(19) 0.51458(13) 0.0305(7) Uani 1 1 d . . . C42 C 1.1336(2) -0.05080(19) 0.46582(14) 0.0361(7) Uani 1 1 d . . . H42 H 1.1518 -0.1044 0.4747 0.043 Uiso 1 1 calc R . . C43 C 1.1100(2) -0.03282(18) 0.40508(14) 0.0325(7) Uani 1 1 d . . . H43 H 1.1136 -0.0730 0.3726 0.039 Uiso 1 1 calc R . . C44 C 1.1611(2) -0.0125(2) 0.58057(13) 0.0395(8) Uani 1 1 d . . . H44A H 1.1399 -0.0707 0.5838 0.047 Uiso 1 1 calc R . . H44B H 1.1328 0.0238 0.6072 0.047 Uiso 1 1 calc R . . H44C H 1.2297 -0.0037 0.5936 0.047 Uiso 1 1 calc R . . C48 C 0.8110(2) 0.20910(16) 0.00211(12) 0.0246(6) Uani 1 1 d . . . C49 C 0.8185(2) 0.17973(19) -0.05713(13) 0.0334(7) Uani 1 1 d . . . H49 H 0.8634 0.1421 -0.0623 0.040 Uiso 1 1 calc R . . C50 C 0.7604(2) 0.2057(2) -0.10816(13) 0.0394(8) Uani 1 1 d . . . H50 H 0.7657 0.1850 -0.1482 0.047 Uiso 1 1 calc R . . C51 C 0.6947(2) 0.26076(19) -0.10289(13) 0.0359(8) Uani 1 1 d . . . C52 C 0.6874(2) 0.28948(19) -0.04329(14) 0.0365(7) Uani 1 1 d . . . H52 H 0.6427 0.3272 -0.0382 0.044 Uiso 1 1 calc R . . C53 C 0.7450(2) 0.26336(18) 0.00826(13) 0.0302(7) Uani 1 1 d . . . H53 H 0.7389 0.2831 0.0484 0.036 Uiso 1 1 calc R . . C54 C 0.6343(2) 0.2893(2) -0.15926(15) 0.0455(9) Uani 1 1 d . . . H54A H 0.5754 0.3052 -0.1495 0.055 Uiso 1 1 calc R . . H54B H 0.6204 0.2441 -0.1925 0.055 Uiso 1 1 calc R . . H54C H 0.6675 0.3374 -0.1726 0.055 Uiso 1 1 calc R . . N61 N 1.02618(15) 0.31401(12) 0.36564(9) 0.0176(4) Uani 1 1 d . . . N62 N 0.95295(15) 0.25788(12) 0.34224(9) 0.0172(4) Uani 1 1 d . . . C62 C 0.86590(19) 0.27222(16) 0.34860(11) 0.0210(6) Uani 1 1 d . . . C63 C 0.84861(19) 0.34674(16) 0.37825(13) 0.0267(6) Uani 1 1 d . . . H63 H 0.7870 0.3561 0.3827 0.032 Uiso 1 1 calc R . . C64 C 0.9223(2) 0.40523(17) 0.40040(13) 0.0271(6) Uani 1 1 d . . . H64 H 0.9133 0.4570 0.4200 0.032 Uiso 1 1 calc R . . C65 C 1.01203(19) 0.38739(16) 0.39370(12) 0.0215(6) Uani 1 1 d . . . C66 C 1.09680(18) 0.44380(16) 0.41628(12) 0.0226(6) Uani 1 1 d . . . H66 H 1.0943 0.4959 0.4380 0.027 Uiso 1 1 calc R . . N63 N 1.17481(15) 0.42214(12) 0.40640(9) 0.0192(5) Uani 1 1 d . . . C68 C 1.26014(18) 0.47455(15) 0.43109(11) 0.0203(5) Uani 1 1 d . . . C69 C 1.2709(2) 0.53106(17) 0.48310(13) 0.0299(7) Uani 1 1 d . . . H69 H 1.2214 0.5344 0.5045 0.036 Uiso 1 1 calc R . . C70 C 1.3536(2) 0.58203(18) 0.50331(13) 0.0320(7) Uani 1 1 d . . . H70 H 1.3606 0.6198 0.5390 0.038 Uiso 1 1 calc R . . C71 C 1.42693(19) 0.57917(16) 0.47240(12) 0.0244(6) Uani 1 1 d . . . C72 C 1.41639(19) 0.51993(16) 0.42241(12) 0.0250(6) Uani 1 1 d . . . H72 H 1.4665 0.5153 0.4017 0.030 Uiso 1 1 calc R . . C73 C 1.33418(19) 0.46745(16) 0.40217(12) 0.0226(6) Uani 1 1 d . . . H73 H 1.3289 0.4267 0.3684 0.027 Uiso 1 1 calc R . . C74 C 1.5150(2) 0.63788(18) 0.49260(14) 0.0337(7) Uani 1 1 d . . . H74A H 1.5091 0.6869 0.4692 0.040 Uiso 1 1 calc R . . H74B H 1.5689 0.6098 0.4850 0.040 Uiso 1 1 calc R . . H74C H 1.5245 0.6551 0.5368 0.040 Uiso 1 1 calc R . . C76 C 0.79313(18) 0.20530(15) 0.32218(11) 0.0198(5) Uani 1 1 d . . . H76 H 0.7290 0.2109 0.3220 0.024 Uiso 1 1 calc R . . N64 N 0.81863(15) 0.13822(13) 0.29906(9) 0.0181(4) Uani 1 1 d . . . C78 C 0.75288(19) 0.06925(16) 0.27208(11) 0.0206(6) Uani 1 1 d . . . C79 C 0.6587(2) 0.06241(18) 0.27421(14) 0.0330(7) Uani 1 1 d . . . H79 H 0.6344 0.1058 0.2952 0.040 Uiso 1 1 calc R . . C80 C 0.6000(2) -0.00671(18) 0.24619(14) 0.0349(7) Uani 1 1 d . . . H80 H 0.5358 -0.0106 0.2487 0.042 Uiso 1 1 calc R . . C81 C 0.6327(2) -0.07060(17) 0.21442(12) 0.0296(7) Uani 1 1 d . . . C82 C 0.7271(2) -0.06333(18) 0.21220(14) 0.0352(7) Uani 1 1 d . . . H82 H 0.7512 -0.1063 0.1906 0.042 Uiso 1 1 calc R . . C83 C 0.7865(2) 0.00505(17) 0.24078(13) 0.0282(6) Uani 1 1 d . . . H83 H 0.8510 0.0084 0.2391 0.034 Uiso 1 1 calc R . . C84 C 0.5682(2) -0.14565(19) 0.18416(15) 0.0401(8) Uani 1 1 d . . . H84A H 0.5842 -0.1939 0.2071 0.048 Uiso 1 1 calc R . . H84B H 0.5753 -0.1566 0.1415 0.048 Uiso 1 1 calc R . . H84C H 0.5031 -0.1355 0.1841 0.048 Uiso 1 1 calc R . . N92 N 0.85472(15) 0.32210(12) 0.19170(9) 0.0191(5) Uani 1 1 d . . . N91 N 0.93188(15) 0.37550(12) 0.21264(9) 0.0181(5) Uani 1 1 d . . . C95 C 0.9238(2) 0.45039(16) 0.24085(12) 0.0230(6) Uani 1 1 d . . . C94 C 0.8380(2) 0.47396(17) 0.24962(14) 0.0337(7) Uani 1 1 d . . . H94 H 0.8339 0.5272 0.2691 0.040 Uiso 1 1 calc R . . C93 C 0.7601(2) 0.41931(17) 0.22974(14) 0.0318(7) Uani 1 1 d . . . H93 H 0.7003 0.4328 0.2353 0.038 Uiso 1 1 calc R . . C92 C 0.77127(19) 0.34236(16) 0.20081(12) 0.0225(6) Uani 1 1 d . . . C106 C 0.69305(19) 0.27894(17) 0.17795(12) 0.0249(6) Uani 1 1 d . . . H106 H 0.6311 0.2897 0.1805 0.030 Uiso 1 1 calc R . . N94 N 0.70855(15) 0.20809(13) 0.15416(9) 0.0210(5) Uani 1 1 d . . . C108 C 0.6314(2) 0.14606(17) 0.13176(13) 0.0268(6) Uani 1 1 d . . . C109 C 0.5423(3) 0.1539(3) 0.1415(3) 0.101(2) Uani 1 1 d . . . H109 H 0.5302 0.2028 0.1635 0.121 Uiso 1 1 calc R . . C110 C 0.4713(3) 0.0920(3) 0.1196(3) 0.103(2) Uani 1 1 d . . . H110 H 0.4107 0.0991 0.1271 0.124 Uiso 1 1 calc R . . C111 C 0.4838(2) 0.02052(19) 0.08773(15) 0.0369(7) Uani 1 1 d . . . C112 C 0.5727(2) 0.01236(18) 0.07983(14) 0.0334(7) Uani 1 1 d . . . H112 H 0.5847 -0.0373 0.0588 0.040 Uiso 1 1 calc R . . C113 C 0.6460(2) 0.07403(17) 0.10140(12) 0.0273(6) Uani 1 1 d . . . H113 H 0.7069 0.0660 0.0950 0.033 Uiso 1 1 calc R . . C114 C 0.4031(2) -0.0465(2) 0.06672(17) 0.0461(9) Uani 1 1 d . . . H11A H 0.3831 -0.0670 0.1029 0.055 Uiso 1 1 calc R . . H11B H 0.4233 -0.0925 0.0433 0.055 Uiso 1 1 calc R . . H11C H 0.3505 -0.0236 0.0404 0.055 Uiso 1 1 calc R . . C96 C 1.0104(2) 0.50448(16) 0.26058(12) 0.0246(6) Uani 1 1 d . . . H96 H 1.0112 0.5570 0.2827 0.030 Uiso 1 1 calc R . . N93 N 1.08615(15) 0.48045(12) 0.24775(9) 0.0200(5) Uani 1 1 d . . . C98 C 1.1727(2) 0.53169(16) 0.26685(11) 0.0235(6) Uani 1 1 d . . . C99 C 1.1824(2) 0.60887(17) 0.30144(14) 0.0343(7) Uani 1 1 d . . . H99 H 1.1295 0.6289 0.3141 0.041 Uiso 1 1 calc R . . C100 C 1.2679(2) 0.65562(19) 0.31703(15) 0.0396(8) Uani 1 1 d . . . H100 H 1.2731 0.7081 0.3400 0.048 Uiso 1 1 calc R . . C101 C 1.3466(2) 0.62819(18) 0.30008(13) 0.0343(7) Uani 1 1 d . . . C102 C 1.3375(2) 0.55094(18) 0.26603(13) 0.0316(7) Uani 1 1 d . . . H102 H 1.3908 0.5306 0.2542 0.038 Uiso 1 1 calc R . . C103 C 1.2508(2) 0.50375(16) 0.24941(12) 0.0255(6) Uani 1 1 d . . . H103 H 1.2452 0.4517 0.2258 0.031 Uiso 1 1 calc R . . C104 C 1.4402(2) 0.6795(2) 0.31925(16) 0.0467(9) Uani 1 1 d . . . H10A H 1.4788 0.6671 0.2893 0.056 Uiso 1 1 calc R . . H10B H 1.4723 0.6662 0.3602 0.056 Uiso 1 1 calc R . . H10C H 1.4305 0.7387 0.3207 0.056 Uiso 1 1 calc R . . P1 P 0.98750(8) 0.67224(6) 0.43220(5) 0.0507(3) Uani 1 1 d . . . F11 F 0.97619(16) 0.60388(13) 0.37456(9) 0.0622(6) Uani 1 1 d . . . F12 F 1.07734(19) 0.63116(14) 0.46700(11) 0.0800(8) Uani 1 1 d . . . F13 F 1.05461(17) 0.73160(15) 0.40246(12) 0.0761(7) Uani 1 1 d . . . F14 F 0.9980(2) 0.73697(14) 0.49096(12) 0.0884(9) Uani 1 1 d . . . F15 F 0.90043(17) 0.71408(17) 0.39801(13) 0.0853(8) Uani 1 1 d . . . F16 F 0.9222(2) 0.61014(15) 0.46144(11) 0.0947(10) Uani 1 1 d . . . P2 P 0.15867(6) 0.10333(5) 0.94880(4) 0.0411(2) Uani 1 1 d . . . F21 F 0.12774(14) 0.05342(13) 0.88223(9) 0.0558(6) Uani 1 1 d . . . F22 F 0.18837(17) 0.15291(12) 1.01646(9) 0.0641(6) Uani 1 1 d . . . F23 F 0.05207(17) 0.1084(2) 0.95006(13) 0.1040(11) Uani 1 1 d . . . F24 F 0.26478(17) 0.09750(19) 0.94856(13) 0.1010(11) Uani 1 1 d . . . F25 F 0.1630(2) 0.18736(14) 0.91850(12) 0.0905(9) Uani 1 1 d . . . F26 F 0.1545(3) 0.01908(13) 0.98036(12) 0.1084(11) Uani 1 1 d . . . P3 P 0.65223(6) 0.05554(5) 0.69149(4) 0.0356(2) Uani 1 1 d D . . F31 F 0.70119(14) -0.00316(13) 0.64919(10) 0.0603(6) Uani 1 1 d D A . F32 F 0.60341(14) 0.11197(13) 0.73356(10) 0.0594(6) Uani 1 1 d D A . F33 F 0.57794(18) -0.02345(14) 0.69145(15) 0.0664(6) Uani 0.90 1 d PD A 1 F34 F 0.58450(19) 0.08093(18) 0.63094(12) 0.0683(5) Uani 0.90 1 d PD A 1 F35 F 0.72720(19) 0.12914(15) 0.68890(15) 0.0664(6) Uani 0.90 1 d PD A 1 F36 F 0.7186(2) 0.02678(19) 0.75039(12) 0.0683(5) Uani 0.90 1 d PD A 1 F37 F 0.7554(9) 0.0842(12) 0.7416(7) 0.038(3) Uani 0.10 1 d PD A 2 F38 F 0.6319(16) -0.0017(12) 0.7465(10) 0.078(6) Uani 0.10 1 d PD A 2 F39 F 0.5529(8) 0.0331(12) 0.6583(7) 0.038(3) Uani 0.10 1 d PD A 2 F310 F 0.6788(16) 0.1267(12) 0.6550(12) 0.078(6) Uani 0.10 1 d PD A 2 P4 P 0.48827(5) 0.65370(5) 0.71035(4) 0.03238(19) Uani 1 1 d . . . F41 F 0.59715(12) 0.64022(11) 0.72896(10) 0.0485(5) Uani 1 1 d . B . F42 F 0.37891(13) 0.66777(13) 0.69286(10) 0.0538(5) Uani 1 1 d . B . F43 F 0.4749(5) 0.6312(3) 0.7770(3) 0.0621(11) Uani 0.60 1 d P B 1 F44 F 0.5069(3) 0.7466(2) 0.7317(2) 0.0537(9) Uani 0.60 1 d P B 1 F45 F 0.4652(3) 0.5537(2) 0.6887(2) 0.0537(9) Uani 0.60 1 d P B 1 F46 F 0.4989(3) 0.6683(3) 0.64327(18) 0.0621(11) Uani 0.60 1 d P B 1 F47 F 0.5141(4) 0.7227(5) 0.6646(4) 0.0728(19) Uani 0.40 1 d P B 2 F48 F 0.4684(5) 0.5862(5) 0.6590(4) 0.082(2) Uani 0.40 1 d P B 2 F49 F 0.5129(5) 0.7328(5) 0.7649(3) 0.082(2) Uani 0.40 1 d P B 2 F410 F 0.4668(7) 0.6006(5) 0.7618(5) 0.0728(19) Uani 0.40 1 d P B 2 O120 O 0.7074(2) 0.2005(2) 0.42984(13) 0.0766(9) Uani 1 1 d . . . C120 C 0.6672(3) 0.1796(2) 0.46766(17) 0.0484(9) Uani 1 1 d . . . C121 C 0.6971(3) 0.2132(3) 0.53296(17) 0.0605(11) Uani 1 1 d . . . H12A H 0.7584 0.2457 0.5394 0.073 Uiso 1 1 calc R . . H12B H 0.7018 0.1672 0.5595 0.073 Uiso 1 1 calc R . . H12C H 0.6508 0.2491 0.5433 0.073 Uiso 1 1 calc R . . C122 C 0.5834(4) 0.1174(4) 0.4504(3) 0.138(3) Uani 1 1 d . . . H12D H 0.5264 0.1454 0.4502 0.166 Uiso 1 1 calc R . . H12E H 0.5880 0.0757 0.4806 0.166 Uiso 1 1 calc R . . H12F H 0.5804 0.0900 0.4092 0.166 Uiso 1 1 calc R . . O130 O 0.9532(3) 0.66998(19) 0.21447(15) 0.0911(11) Uani 1 1 d . . . C130 C 0.9700(4) 0.7444(3) 0.2306(2) 0.0758(14) Uani 1 1 d . . . C131 C 1.0513(5) 0.7922(4) 0.2153(3) 0.136(3) Uani 1 1 d . . . H13A H 1.0803 0.7565 0.1888 0.163 Uiso 1 1 calc R . . H13B H 1.0974 0.8117 0.2535 0.163 Uiso 1 1 calc R . . H13C H 1.0301 0.8401 0.1936 0.163 Uiso 1 1 calc R . . C132 C 0.9131(5) 0.7894(5) 0.2639(3) 0.159(3) Uani 1 1 d . . . H13D H 0.8550 0.7546 0.2638 0.191 Uiso 1 1 calc R . . H13E H 0.8978 0.8402 0.2441 0.191 Uiso 1 1 calc R . . H13F H 0.9477 0.8041 0.3067 0.191 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01784(17) 0.01858(16) 0.01856(16) -0.00130(12) 0.00557(13) 0.00409(13) Cu2 0.02065(18) 0.01834(16) 0.01975(16) -0.00238(12) 0.00494(13) 0.00224(13) Cu3 0.01893(18) 0.01866(16) 0.01902(16) -0.00212(12) 0.00706(13) 0.00326(13) Cu4 0.02011(18) 0.02046(16) 0.01860(16) -0.00288(12) 0.00753(13) 0.00192(13) N1 0.0176(12) 0.0168(10) 0.0211(11) 0.0004(9) 0.0067(9) 0.0023(9) N2 0.0190(12) 0.0172(10) 0.0203(11) -0.0022(9) 0.0063(9) -0.0003(9) C2 0.0230(15) 0.0230(13) 0.0226(13) -0.0048(11) 0.0105(11) -0.0027(11) C3 0.0281(16) 0.0249(14) 0.0310(15) -0.0065(12) 0.0163(13) 0.0029(12) C4 0.0223(15) 0.0207(14) 0.0373(16) -0.0037(12) 0.0130(13) 0.0037(11) C5 0.0167(14) 0.0173(13) 0.0311(14) -0.0015(11) 0.0091(11) -0.0001(11) C6 0.0177(14) 0.0196(13) 0.0329(15) 0.0008(11) 0.0050(12) 0.0034(11) N3 0.0173(12) 0.0185(11) 0.0247(11) 0.0024(9) 0.0040(9) 0.0007(9) C8 0.0150(14) 0.0262(14) 0.0246(14) 0.0070(11) 0.0014(11) -0.0031(11) C9 0.0259(16) 0.0336(16) 0.0351(16) 0.0101(13) 0.0030(13) 0.0055(13) C10 0.0290(18) 0.0389(18) 0.0471(19) 0.0203(15) 0.0017(15) 0.0050(14) C11 0.0173(15) 0.0469(19) 0.0341(16) 0.0196(14) 0.0002(13) -0.0056(13) C12 0.0242(16) 0.0463(18) 0.0268(15) 0.0044(13) 0.0063(12) -0.0011(14) C13 0.0172(14) 0.0310(15) 0.0297(15) 0.0069(12) 0.0059(12) 0.0013(12) C14 0.035(2) 0.068(2) 0.0387(19) 0.0232(17) 0.0010(15) -0.0048(17) C16 0.0329(17) 0.0244(14) 0.0212(14) -0.0039(11) 0.0133(12) -0.0029(12) N4 0.0253(13) 0.0224(11) 0.0182(11) 0.0001(9) 0.0045(9) -0.0050(10) C18 0.0414(19) 0.0219(14) 0.0231(14) 0.0013(11) 0.0016(13) -0.0130(13) C19 0.096(3) 0.0400(19) 0.0233(16) -0.0009(14) 0.0092(18) 0.009(2) C20 0.125(4) 0.046(2) 0.0197(17) -0.0027(15) 0.002(2) -0.009(2) C21 0.072(3) 0.038(2) 0.0351(19) 0.0187(16) -0.0209(18) -0.0337(19) C22 0.038(2) 0.056(2) 0.053(2) 0.0335(18) -0.0085(17) -0.0155(17) C23 0.0283(18) 0.0428(18) 0.0340(17) 0.0157(14) 0.0024(14) -0.0084(15) C24 0.096(4) 0.065(3) 0.046(2) 0.032(2) -0.035(2) -0.043(2) N31 0.0204(12) 0.0174(11) 0.0209(11) -0.0011(9) 0.0077(9) 0.0003(9) N32 0.0208(12) 0.0183(11) 0.0193(11) -0.0023(9) 0.0087(9) -0.0002(9) C32 0.0255(15) 0.0200(13) 0.0226(13) -0.0065(11) 0.0112(11) -0.0014(11) C33 0.0252(15) 0.0262(14) 0.0260(14) -0.0057(11) 0.0140(12) 0.0023(12) C34 0.0224(15) 0.0242(14) 0.0321(15) -0.0065(12) 0.0101(12) 0.0047(12) C35 0.0183(14) 0.0190(13) 0.0284(14) -0.0010(11) 0.0072(11) 0.0011(11) C36 0.0216(15) 0.0232(14) 0.0292(14) 0.0025(11) 0.0091(12) 0.0051(11) N33 0.0177(12) 0.0193(11) 0.0247(11) -0.0007(9) 0.0050(9) 0.0007(9) C46 0.0295(16) 0.0244(14) 0.0195(13) -0.0049(11) 0.0132(12) -0.0010(12) N34 0.0240(13) 0.0189(11) 0.0202(11) -0.0007(9) 0.0078(9) -0.0046(9) C38 0.0163(14) 0.0268(14) 0.0263(14) 0.0047(11) 0.0053(11) 0.0023(11) C39 0.0180(14) 0.0231(14) 0.0275(14) 0.0034(11) 0.0053(11) 0.0014(11) C40 0.0208(15) 0.0350(16) 0.0244(14) 0.0025(12) 0.0055(12) -0.0036(12) C41 0.0161(15) 0.0467(18) 0.0304(15) 0.0152(13) 0.0055(12) 0.0033(13) C42 0.0325(18) 0.0368(17) 0.0439(18) 0.0149(14) 0.0110(14) 0.0163(14) C43 0.0340(18) 0.0322(16) 0.0348(16) 0.0043(13) 0.0112(14) 0.0134(14) C44 0.0318(18) 0.058(2) 0.0313(16) 0.0215(15) 0.0069(14) 0.0052(16) C48 0.0265(16) 0.0238(14) 0.0219(13) 0.0018(11) 0.0060(12) -0.0086(12) C49 0.0394(19) 0.0359(17) 0.0235(15) -0.0025(12) 0.0064(13) 0.0003(14) C50 0.046(2) 0.0456(19) 0.0221(15) -0.0014(13) 0.0042(14) -0.0121(16) C51 0.0340(18) 0.0386(18) 0.0286(16) 0.0107(13) -0.0022(13) -0.0172(15) C52 0.0300(18) 0.0376(17) 0.0418(18) 0.0144(14) 0.0055(14) 0.0003(14) C53 0.0335(18) 0.0337(16) 0.0245(14) 0.0039(12) 0.0105(13) -0.0018(13) C54 0.042(2) 0.045(2) 0.0415(19) 0.0167(15) -0.0070(16) -0.0153(16) N61 0.0179(12) 0.0201(11) 0.0146(10) 0.0005(8) 0.0033(9) 0.0029(9) N62 0.0176(12) 0.0178(11) 0.0163(10) -0.0013(8) 0.0048(9) 0.0012(9) C62 0.0209(14) 0.0238(14) 0.0194(13) 0.0026(11) 0.0053(11) 0.0048(11) C63 0.0173(14) 0.0277(14) 0.0344(15) -0.0087(12) 0.0064(12) 0.0052(12) C64 0.0247(16) 0.0254(14) 0.0313(15) -0.0092(12) 0.0086(12) 0.0072(12) C65 0.0216(15) 0.0216(13) 0.0206(13) -0.0028(11) 0.0038(11) 0.0036(11) C66 0.0203(15) 0.0213(13) 0.0252(14) -0.0037(11) 0.0041(11) 0.0034(11) N63 0.0200(12) 0.0188(11) 0.0181(10) 0.0011(8) 0.0029(9) 0.0009(9) C68 0.0201(14) 0.0188(13) 0.0206(13) 0.0017(10) 0.0018(11) 0.0008(11) C69 0.0250(16) 0.0324(16) 0.0316(15) -0.0102(12) 0.0099(13) -0.0012(13) C70 0.0292(17) 0.0330(16) 0.0291(15) -0.0108(13) 0.0036(13) -0.0056(13) C71 0.0217(15) 0.0220(14) 0.0264(14) 0.0063(11) -0.0020(11) -0.0010(11) C72 0.0208(15) 0.0300(15) 0.0255(14) 0.0070(12) 0.0061(12) 0.0032(12) C73 0.0278(16) 0.0189(13) 0.0224(13) 0.0020(10) 0.0081(12) 0.0032(11) C74 0.0282(17) 0.0290(16) 0.0407(17) 0.0067(13) 0.0020(14) -0.0046(13) C76 0.0185(14) 0.0239(13) 0.0176(12) -0.0002(10) 0.0063(10) 0.0021(11) N64 0.0186(12) 0.0239(11) 0.0130(10) 0.0037(8) 0.0054(9) 0.0017(9) C78 0.0235(15) 0.0236(13) 0.0143(12) 0.0034(10) 0.0046(11) -0.0022(11) C79 0.0287(17) 0.0331(16) 0.0391(17) -0.0072(13) 0.0180(14) -0.0051(13) C80 0.0313(18) 0.0366(17) 0.0381(17) 0.0010(14) 0.0158(14) -0.0084(14) C81 0.0377(18) 0.0290(15) 0.0186(13) 0.0046(11) 0.0020(12) -0.0081(13) C82 0.0383(19) 0.0294(16) 0.0355(17) -0.0083(13) 0.0071(14) 0.0010(14) C83 0.0254(16) 0.0264(15) 0.0319(15) -0.0021(12) 0.0060(12) 0.0018(12) C84 0.041(2) 0.0341(17) 0.0391(18) 0.0029(14) 0.0009(15) -0.0122(15) N92 0.0218(12) 0.0183(11) 0.0170(10) -0.0004(8) 0.0046(9) 0.0015(9) N91 0.0213(12) 0.0176(11) 0.0152(10) -0.0004(8) 0.0040(9) 0.0028(9) C95 0.0273(16) 0.0189(13) 0.0229(13) -0.0008(11) 0.0061(12) 0.0042(11) C94 0.0366(18) 0.0222(15) 0.0439(18) -0.0082(13) 0.0143(14) 0.0069(13) C93 0.0250(16) 0.0249(15) 0.0473(18) -0.0048(13) 0.0135(14) 0.0046(13) C92 0.0232(15) 0.0223(13) 0.0226(13) 0.0011(11) 0.0063(11) 0.0036(11) C106 0.0211(15) 0.0309(15) 0.0248(14) 0.0019(12) 0.0093(12) 0.0047(12) N94 0.0214(12) 0.0218(11) 0.0208(11) 0.0000(9) 0.0077(9) 0.0014(9) C108 0.0218(15) 0.0258(14) 0.0328(15) -0.0018(12) 0.0086(12) -0.0012(12) C109 0.034(2) 0.054(3) 0.211(6) -0.064(3) 0.048(3) -0.011(2) C110 0.027(2) 0.055(3) 0.224(7) -0.055(3) 0.045(3) -0.0125(19) C111 0.0285(18) 0.0356(17) 0.0432(18) 0.0055(14) 0.0032(14) -0.0066(14) C112 0.0339(18) 0.0273(15) 0.0385(17) -0.0038(13) 0.0125(14) -0.0063(13) C113 0.0265(16) 0.0272(15) 0.0299(15) 0.0015(12) 0.0118(12) -0.0003(12) C114 0.0332(19) 0.0431(19) 0.057(2) 0.0061(16) 0.0037(16) -0.0128(16) C96 0.0322(17) 0.0181(13) 0.0229(14) -0.0016(11) 0.0056(12) 0.0025(12) N93 0.0251(13) 0.0185(11) 0.0146(10) 0.0015(8) 0.0014(9) -0.0007(9) C98 0.0288(16) 0.0219(13) 0.0171(13) 0.0042(10) 0.0000(11) -0.0019(12) C99 0.0370(19) 0.0261(15) 0.0366(17) -0.0074(13) 0.0051(14) 0.0000(14) C100 0.045(2) 0.0278(16) 0.0396(18) -0.0048(14) 0.0000(15) -0.0049(15) C101 0.042(2) 0.0276(15) 0.0269(15) 0.0075(12) -0.0041(14) -0.0108(14) C102 0.0274(17) 0.0342(16) 0.0320(16) 0.0086(13) 0.0052(13) -0.0044(13) C103 0.0322(17) 0.0211(14) 0.0228(14) 0.0060(11) 0.0048(12) -0.0006(12) C104 0.042(2) 0.046(2) 0.0439(19) 0.0055(16) 0.0002(16) -0.0196(16) P1 0.0640(7) 0.0429(5) 0.0516(6) -0.0013(4) 0.0228(5) 0.0204(5) F11 0.0757(16) 0.0697(14) 0.0418(11) -0.0121(10) 0.0189(11) 0.0090(12) F12 0.107(2) 0.0644(15) 0.0640(15) -0.0147(12) -0.0011(14) 0.0474(14) F13 0.0595(16) 0.0717(16) 0.1031(19) 0.0130(14) 0.0306(14) 0.0045(13) F14 0.127(2) 0.0550(14) 0.0896(18) -0.0226(13) 0.0374(17) 0.0337(15) F15 0.0572(16) 0.1001(19) 0.111(2) 0.0165(16) 0.0343(15) 0.0351(14) F16 0.157(3) 0.0678(16) 0.0691(16) -0.0124(13) 0.0651(18) -0.0243(17) P2 0.0417(5) 0.0360(5) 0.0481(5) -0.0169(4) 0.0249(4) -0.0038(4) F21 0.0507(13) 0.0652(13) 0.0510(12) -0.0227(10) 0.0278(10) -0.0166(10) F22 0.0912(18) 0.0474(12) 0.0528(12) -0.0276(10) 0.0306(12) -0.0088(11) F23 0.0501(15) 0.154(3) 0.110(2) -0.059(2) 0.0539(15) -0.0129(16) F24 0.0432(14) 0.143(2) 0.105(2) -0.0691(19) 0.0162(14) 0.0067(15) F25 0.148(3) 0.0474(14) 0.0731(17) -0.0023(12) 0.0290(17) -0.0144(15) F26 0.204(4) 0.0342(13) 0.0711(17) -0.0115(12) 0.0108(19) -0.0160(16) P3 0.0249(4) 0.0298(4) 0.0543(5) 0.0016(4) 0.0129(4) 0.0073(3) F31 0.0382(12) 0.0594(13) 0.0798(15) -0.0253(11) 0.0135(11) 0.0093(10) F32 0.0474(13) 0.0565(13) 0.0791(15) -0.0119(11) 0.0246(11) 0.0208(10) F33 0.0517(13) 0.0421(10) 0.1087(17) -0.0068(11) 0.0346(11) -0.0085(9) F34 0.0584(13) 0.0873(15) 0.0602(11) 0.0121(10) 0.0039(9) 0.0320(11) F35 0.0517(13) 0.0421(10) 0.1087(17) -0.0068(11) 0.0346(11) -0.0085(9) F36 0.0584(13) 0.0873(15) 0.0602(11) 0.0121(10) 0.0039(9) 0.0320(11) F37 0.015(6) 0.068(10) 0.026(6) -0.021(6) 0.000(5) 0.018(7) F38 0.063(13) 0.072(12) 0.132(18) 0.071(12) 0.064(12) 0.034(10) F39 0.015(6) 0.068(10) 0.026(6) -0.021(6) 0.000(5) 0.018(7) F310 0.063(13) 0.072(12) 0.132(18) 0.071(12) 0.064(12) 0.034(10) P4 0.0239(4) 0.0390(4) 0.0350(4) -0.0069(3) 0.0116(3) 0.0031(3) F41 0.0233(10) 0.0410(10) 0.0825(14) -0.0053(10) 0.0175(10) 0.0041(8) F42 0.0248(10) 0.0681(14) 0.0691(14) 0.0132(11) 0.0065(9) 0.0109(9) F43 0.069(3) 0.086(3) 0.0441(18) 0.0157(18) 0.0312(17) 0.029(2) F44 0.0413(16) 0.0315(14) 0.083(3) -0.0154(15) 0.0084(18) 0.0017(11) F45 0.0413(16) 0.0315(14) 0.083(3) -0.0154(15) 0.0084(18) 0.0017(11) F46 0.069(3) 0.086(3) 0.0441(18) 0.0157(18) 0.0312(17) 0.029(2) F47 0.030(2) 0.090(5) 0.104(6) 0.050(4) 0.015(3) 0.000(3) F48 0.051(3) 0.088(5) 0.101(5) -0.063(4) 0.031(3) -0.014(3) F49 0.051(3) 0.088(5) 0.101(5) -0.063(4) 0.031(3) -0.014(3) F410 0.030(2) 0.090(5) 0.104(6) 0.050(4) 0.015(3) 0.000(3) O120 0.082(2) 0.102(2) 0.0527(17) 0.0121(16) 0.0301(16) 0.0052(18) C120 0.050(2) 0.055(2) 0.049(2) 0.0058(17) 0.0207(18) 0.0233(18) C121 0.071(3) 0.068(3) 0.050(2) 0.0089(19) 0.019(2) 0.031(2) C122 0.089(4) 0.148(6) 0.171(6) -0.072(5) 0.068(4) -0.054(4) O130 0.122(3) 0.056(2) 0.079(2) 0.0171(17) -0.018(2) 0.0046(19) C130 0.093(4) 0.064(3) 0.063(3) 0.013(2) -0.008(3) 0.021(3) C131 0.130(6) 0.091(4) 0.159(6) -0.026(4) 0.007(5) -0.054(4) C132 0.184(8) 0.186(8) 0.133(6) 0.037(5) 0.043(6) 0.127(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.996(2) . y Cu1 N61 2.013(2) . y Cu1 N63 2.032(2) . y Cu1 N3 2.044(2) . y Cu2 N2 2.001(2) . y Cu2 N91 2.002(2) . y Cu2 N93 2.035(2) . y Cu2 N4 2.037(2) . y Cu3 N62 1.9767(19) . y Cu3 N31 1.999(2) . y Cu3 N33 2.013(2) . y Cu3 N64 2.026(2) . y Cu4 N32 2.004(2) . y Cu4 N92 2.021(2) . y Cu4 N34 2.046(2) . y Cu4 N94 2.049(2) . y N1 N2 1.342(3) . ? N1 C5 1.351(3) . ? N2 C2 1.352(3) . ? C2 C3 1.392(4) . ? C2 C16 1.459(4) . ? C3 C4 1.358(4) . ? C3 H3 0.9500 . ? C4 C5 1.398(3) . ? C4 H4 0.9500 . ? C5 C6 1.452(4) . ? C6 N3 1.286(3) . ? C6 H6 0.9500 . ? N3 C8 1.428(3) . ? C8 C13 1.387(4) . ? C8 C9 1.391(4) . ? C9 C10 1.388(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C10 H10 0.9500 . ? C11 C12 1.393(4) . ? C11 C14 1.501(4) . ? C12 C13 1.382(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 N4 1.287(3) . ? C16 H16 0.9500 . ? N4 C18 1.433(3) . ? C18 C23 1.382(4) . ? C18 C19 1.390(4) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.378(6) . ? C20 H20 0.9500 . ? C21 C22 1.367(6) . ? C21 C24 1.515(5) . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N31 N32 1.339(3) . ? N31 C35 1.350(3) . ? N32 C32 1.346(3) . ? C32 C33 1.400(4) . ? C32 C46 1.459(4) . ? C33 C34 1.365(4) . ? C33 H33 0.9500 . ? C34 C35 1.398(3) . ? C34 H34 0.9500 . ? C35 C36 1.466(4) . ? C36 N33 1.287(3) . ? C36 H36 0.9500 . ? N33 C38 1.424(3) . ? C46 N34 1.283(3) . ? C46 H46 0.9500 . ? N34 C48 1.428(3) . ? C38 C39 1.393(4) . ? C38 C43 1.403(4) . ? C39 C40 1.388(4) . ? C39 H39 0.9500 . ? C40 C41 1.392(4) . ? C40 H40 0.9500 . ? C41 C42 1.396(4) . ? C41 C44 1.506(4) . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C48 C53 1.379(4) . ? C48 C49 1.398(4) . ? C49 C50 1.381(4) . ? C49 H49 0.9500 . ? C50 C51 1.381(5) . ? C50 H50 0.9500 . ? C51 C52 1.401(4) . ? C51 C54 1.499(4) . ? C52 C53 1.386(4) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N61 N62 1.336(3) . ? N61 C65 1.355(3) . ? N62 C62 1.348(3) . ? C62 C63 1.402(3) . ? C62 C76 1.453(4) . ? C63 C64 1.359(4) . ? C63 H63 0.9500 . ? C64 C65 1.403(4) . ? C64 H64 0.9500 . ? C65 C66 1.454(4) . ? C66 N63 1.279(3) . ? C66 H66 0.9500 . ? N63 C68 1.433(3) . ? C68 C73 1.379(4) . ? C68 C69 1.396(3) . ? C69 C70 1.379(4) . ? C69 H69 0.9500 . ? C70 C71 1.393(4) . ? C70 H70 0.9500 . ? C71 C72 1.390(4) . ? C71 C74 1.504(4) . ? C72 C73 1.387(4) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C76 N64 1.286(3) . ? C76 H76 0.9500 . ? N64 C78 1.421(3) . ? C78 C79 1.384(4) . ? C78 C83 1.391(4) . ? C79 C80 1.378(4) . ? C79 H79 0.9500 . ? C80 C81 1.386(4) . ? C80 H80 0.9500 . ? C81 C82 1.388(4) . ? C81 C84 1.500(4) . ? C82 C83 1.377(4) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? N92 C92 1.342(3) . ? N92 N91 1.342(3) . ? N91 C95 1.352(3) . ? C95 C94 1.390(4) . ? C95 C96 1.448(4) . ? C94 C93 1.358(4) . ? C94 H94 0.9500 . ? C93 C92 1.400(4) . ? C93 H93 0.9500 . ? C92 C106 1.454(4) . ? C106 N94 1.287(3) . ? C106 H106 0.9500 . ? N94 C108 1.428(3) . ? C108 C113 1.362(4) . ? C108 C109 1.379(5) . ? C109 C110 1.368(5) . ? C109 H109 0.9500 . ? C110 C111 1.360(5) . ? C110 H110 0.9500 . ? C111 C112 1.363(4) . ? C111 C114 1.510(4) . ? C112 C113 1.385(4) . ? C112 H112 0.9500 . ? C113 H113 0.9500 . ? C114 H11A 0.9800 . ? C114 H11B 0.9800 . ? C114 H11C 0.9800 . ? C96 N93 1.284(3) . ? C96 H96 0.9500 . ? N93 C98 1.423(3) . ? C98 C103 1.381(4) . ? C98 C99 1.402(4) . ? C99 C100 1.373(4) . ? C99 H99 0.9500 . ? C100 C101 1.382(5) . ? C100 H100 0.9500 . ? C101 C102 1.398(4) . ? C101 C104 1.506(4) . ? C102 C103 1.391(4) . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? C104 H10A 0.9800 . ? C104 H10B 0.9800 . ? C104 H10C 0.9800 . ? P1 F15 1.571(3) . ? P1 F14 1.589(2) . ? P1 F13 1.591(3) . ? P1 F16 1.594(3) . ? P1 F12 1.599(2) . ? P1 F11 1.605(2) . ? P2 F25 1.563(3) . ? P2 F24 1.564(2) . ? P2 F23 1.575(2) . ? P2 F26 1.580(3) . ? P2 F21 1.5930(19) . ? P2 F22 1.610(2) . ? P3 F39 1.488(11) . ? P3 F310 1.525(13) . ? P3 F35 1.565(3) . ? P3 F32 1.5774(19) . ? P3 F36 1.581(3) . ? P3 F34 1.596(3) . ? P3 F31 1.604(2) . ? P3 F33 1.609(2) . ? P3 F38 1.645(13) . ? P3 F37 1.686(11) . ? P4 F48 1.488(6) . ? P4 F44 1.530(4) . ? P4 F410 1.546(10) . ? P4 F46 1.563(4) . ? P4 F41 1.5968(19) . ? P4 F43 1.597(6) . ? P4 F42 1.6047(19) . ? P4 F47 1.636(6) . ? P4 F45 1.644(4) . ? P4 F49 1.663(6) . ? O120 C120 1.175(4) . ? C120 C121 1.475(5) . ? C120 C122 1.488(6) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? O130 C130 1.223(5) . ? C130 C132 1.434(7) . ? C130 C131 1.479(7) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N61 120.94(8) . . y N1 Cu1 N63 131.32(8) . . y N61 Cu1 N63 81.27(8) . . y N1 Cu1 N3 81.28(8) . . y N61 Cu1 N3 132.37(8) . . y N63 Cu1 N3 116.94(8) . . y N2 Cu2 N91 134.31(8) . . y N2 Cu2 N93 117.67(8) . . y N91 Cu2 N93 82.15(9) . . y N2 Cu2 N4 81.95(9) . . y N91 Cu2 N4 118.98(9) . . y N93 Cu2 N4 128.68(8) . . y N62 Cu3 N31 130.33(8) . . y N62 Cu3 N33 124.35(8) . . y N31 Cu3 N33 81.55(9) . . y N62 Cu3 N64 81.75(8) . . y N31 Cu3 N64 115.71(8) . . y N33 Cu3 N64 129.54(8) . . y N32 Cu4 N92 119.28(8) . . y N32 Cu4 N34 80.95(9) . . y N92 Cu4 N34 126.26(8) . . y N32 Cu4 N94 138.68(8) . . y N92 Cu4 N94 81.55(9) . . y N34 Cu4 N94 116.89(9) . . y N2 N1 C5 119.5(2) . . ? N2 N1 Cu1 127.15(16) . . ? C5 N1 Cu1 113.30(17) . . ? N1 N2 C2 119.5(2) . . ? N1 N2 Cu2 127.48(15) . . ? C2 N2 Cu2 112.68(17) . . ? N2 C2 C3 122.3(2) . . ? N2 C2 C16 114.6(2) . . ? C3 C2 C16 123.1(2) . . ? C4 C3 C2 118.2(2) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 118.0(3) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.3(2) . . ? N1 C5 C6 114.5(2) . . ? C4 C5 C6 123.2(2) . . ? N3 C6 C5 118.5(2) . . ? N3 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 N3 C8 120.5(2) . . ? C6 N3 Cu1 111.86(18) . . ? C8 N3 Cu1 127.35(17) . . ? C13 C8 C9 119.4(3) . . ? C13 C8 N3 117.4(2) . . ? C9 C8 N3 123.1(2) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 121.3(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 118.1(3) . . ? C10 C11 C14 120.7(3) . . ? C12 C11 C14 121.2(3) . . ? C13 C12 C11 121.2(3) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 120.1(3) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C16 C2 119.0(2) . . ? N4 C16 H16 120.5 . . ? C2 C16 H16 120.5 . . ? C16 N4 C18 120.3(2) . . ? C16 N4 Cu2 111.63(18) . . ? C18 N4 Cu2 127.90(19) . . ? C23 C18 C19 119.0(3) . . ? C23 C18 N4 117.4(3) . . ? C19 C18 N4 123.6(3) . . ? C20 C19 C18 119.6(4) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 121.7(4) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 117.8(3) . . ? C22 C21 C24 122.7(4) . . ? C20 C21 C24 119.5(4) . . ? C21 C22 C23 122.0(4) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C18 C23 C22 119.8(3) . . ? C18 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N32 N31 C35 120.0(2) . . ? N32 N31 Cu3 126.56(16) . . ? C35 N31 Cu3 113.33(17) . . ? N31 N32 C32 119.4(2) . . ? N31 N32 Cu4 127.09(15) . . ? C32 N32 Cu4 113.56(18) . . ? N32 C32 C33 122.5(2) . . ? N32 C32 C46 114.6(2) . . ? C33 C32 C46 122.9(2) . . ? C34 C33 C32 118.0(2) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 117.9(2) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? N31 C35 C34 122.1(2) . . ? N31 C35 C36 114.0(2) . . ? C34 C35 C36 123.9(2) . . ? N33 C36 C35 118.0(2) . . ? N33 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C36 N33 C38 120.5(2) . . ? C36 N33 Cu3 113.10(18) . . ? C38 N33 Cu3 126.39(16) . . ? N34 C46 C32 118.3(2) . . ? N34 C46 H46 120.9 . . ? C32 C46 H46 120.9 . . ? C46 N34 C48 121.0(2) . . ? C46 N34 Cu4 112.59(18) . . ? C48 N34 Cu4 126.35(17) . . ? C39 C38 C43 119.8(3) . . ? C39 C38 N33 117.4(2) . . ? C43 C38 N33 122.8(2) . . ? C40 C39 C38 119.9(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 120.9(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 118.4(3) . . ? C40 C41 C44 121.1(3) . . ? C42 C41 C44 120.5(3) . . ? C43 C42 C41 121.6(3) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C38 119.3(3) . . ? C42 C43 H43 120.4 . . ? C38 C43 H43 120.4 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C53 C48 C49 119.0(3) . . ? C53 C48 N34 116.9(2) . . ? C49 C48 N34 124.0(3) . . ? C50 C49 C48 119.6(3) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 122.2(3) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C50 C51 C52 117.7(3) . . ? C50 C51 C54 120.8(3) . . ? C52 C51 C54 121.5(3) . . ? C53 C52 C51 120.6(3) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C48 C53 C52 120.9(3) . . ? C48 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N62 N61 C65 119.6(2) . . ? N62 N61 Cu1 127.61(15) . . ? C65 N61 Cu1 112.75(17) . . ? N61 N62 C62 120.6(2) . . ? N61 N62 Cu3 126.17(16) . . ? C62 N62 Cu3 113.20(16) . . ? N62 C62 C63 121.5(2) . . ? N62 C62 C76 114.8(2) . . ? C63 C62 C76 123.6(2) . . ? C64 C63 C62 118.2(2) . . ? C64 C63 H63 120.9 . . ? C62 C63 H63 120.9 . . ? C63 C64 C65 118.5(2) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? N61 C65 C64 121.6(2) . . ? N61 C65 C66 114.4(2) . . ? C64 C65 C66 124.0(2) . . ? N63 C66 C65 118.9(2) . . ? N63 C66 H66 120.6 . . ? C65 C66 H66 120.6 . . ? C66 N63 C68 120.0(2) . . ? C66 N63 Cu1 112.62(18) . . ? C68 N63 Cu1 127.16(16) . . ? C73 C68 C69 119.5(2) . . ? C73 C68 N63 117.9(2) . . ? C69 C68 N63 122.6(2) . . ? C70 C69 C68 119.9(3) . . ? C70 C69 H69 120.1 . . ? C68 C69 H69 120.1 . . ? C69 C70 C71 121.3(3) . . ? C69 C70 H70 119.4 . . ? C71 C70 H70 119.4 . . ? C72 C71 C70 117.8(3) . . ? C72 C71 C74 121.0(3) . . ? C70 C71 C74 121.2(3) . . ? C73 C72 C71 121.4(3) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C68 C73 C72 119.9(2) . . ? C68 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N64 C76 C62 117.7(2) . . ? N64 C76 H76 121.2 . . ? C62 C76 H76 121.2 . . ? C76 N64 C78 122.0(2) . . ? C76 N64 Cu3 112.39(17) . . ? C78 N64 Cu3 125.46(16) . . ? C79 C78 C83 118.5(2) . . ? C79 C78 N64 124.7(2) . . ? C83 C78 N64 116.8(2) . . ? C80 C79 C78 120.6(3) . . ? C80 C79 H79 119.7 . . ? C78 C79 H79 119.7 . . ? C79 C80 C81 121.3(3) . . ? C79 C80 H80 119.4 . . ? C81 C80 H80 119.4 . . ? C80 C81 C82 117.9(3) . . ? C80 C81 C84 120.9(3) . . ? C82 C81 C84 121.2(3) . . ? C83 C82 C81 121.1(3) . . ? C83 C82 H82 119.4 . . ? C81 C82 H82 119.4 . . ? C82 C83 C78 120.6(3) . . ? C82 C83 H83 119.7 . . ? C78 C83 H83 119.7 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C92 N92 N91 119.8(2) . . ? C92 N92 Cu4 112.33(17) . . ? N91 N92 Cu4 127.86(16) . . ? N92 N91 C95 119.3(2) . . ? N92 N91 Cu2 128.53(15) . . ? C95 N91 Cu2 111.88(17) . . ? N91 C95 C94 122.2(3) . . ? N91 C95 C96 115.4(2) . . ? C94 C95 C96 122.5(2) . . ? C93 C94 C95 118.6(2) . . ? C93 C94 H94 120.7 . . ? C95 C94 H94 120.7 . . ? C94 C93 C92 117.6(3) . . ? C94 C93 H93 121.2 . . ? C92 C93 H93 121.2 . . ? N92 C92 C93 122.5(2) . . ? N92 C92 C106 115.2(2) . . ? C93 C92 C106 122.4(2) . . ? N94 C106 C92 119.4(2) . . ? N94 C106 H106 120.3 . . ? C92 C106 H106 120.3 . . ? C106 N94 C108 119.1(2) . . ? C106 N94 Cu4 111.10(18) . . ? C108 N94 Cu4 129.34(16) . . ? C113 C108 C109 117.6(3) . . ? C113 C108 N94 119.3(2) . . ? C109 C108 N94 123.1(3) . . ? C110 C109 C108 120.6(3) . . ? C110 C109 H109 119.7 . . ? C108 C109 H109 119.7 . . ? C111 C110 C109 122.7(4) . . ? C111 C110 H110 118.6 . . ? C109 C110 H110 118.6 . . ? C110 C111 C112 116.3(3) . . ? C110 C111 C114 120.0(3) . . ? C112 C111 C114 123.6(3) . . ? C111 C112 C113 122.3(3) . . ? C111 C112 H112 118.9 . . ? C113 C112 H112 118.9 . . ? C108 C113 C112 120.5(3) . . ? C108 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C111 C114 H11A 109.5 . . ? C111 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C111 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? N93 C96 C95 119.0(2) . . ? N93 C96 H96 120.5 . . ? C95 C96 H96 120.5 . . ? C96 N93 C98 120.6(2) . . ? C96 N93 Cu2 111.45(18) . . ? C98 N93 Cu2 127.98(17) . . ? C103 C98 C99 118.7(3) . . ? C103 C98 N93 117.7(2) . . ? C99 C98 N93 123.6(3) . . ? C100 C99 C98 120.2(3) . . ? C100 C99 H99 119.9 . . ? C98 C99 H99 119.9 . . ? C99 C100 C101 121.6(3) . . ? C99 C100 H100 119.2 . . ? C101 C100 H100 119.2 . . ? C100 C101 C102 118.3(3) . . ? C100 C101 C104 120.6(3) . . ? C102 C101 C104 121.0(3) . . ? C103 C102 C101 120.3(3) . . ? C103 C102 H102 119.8 . . ? C101 C102 H102 119.8 . . ? C98 C103 C102 120.8(3) . . ? C98 C103 H103 119.6 . . ? C102 C103 H103 119.6 . . ? C101 C104 H10A 109.5 . . ? C101 C104 H10B 109.5 . . ? H10A C104 H10B 109.5 . . ? C101 C104 H10C 109.5 . . ? H10A C104 H10C 109.5 . . ? H10B C104 H10C 109.5 . . ? F15 P1 F14 90.19(15) . . ? F15 P1 F13 89.75(14) . . ? F14 P1 F13 91.97(15) . . ? F15 P1 F16 91.66(17) . . ? F14 P1 F16 89.40(14) . . ? F13 P1 F16 178.03(15) . . ? F15 P1 F12 178.96(17) . . ? F14 P1 F12 89.38(13) . . ? F13 P1 F12 89.32(15) . . ? F16 P1 F12 89.28(17) . . ? F15 P1 F11 90.93(14) . . ? F14 P1 F11 177.69(15) . . ? F13 P1 F11 90.05(13) . . ? F16 P1 F11 88.55(13) . . ? F12 P1 F11 89.53(12) . . ? F25 P2 F24 89.66(18) . . ? F25 P2 F23 91.17(18) . . ? F24 P2 F23 179.0(2) . . ? F25 P2 F26 179.19(14) . . ? F24 P2 F26 90.45(19) . . ? F23 P2 F26 88.72(19) . . ? F25 P2 F21 90.46(13) . . ? F24 P2 F21 91.07(12) . . ? F23 P2 F21 89.42(12) . . ? F26 P2 F21 90.34(13) . . ? F25 P2 F22 90.18(13) . . ? F24 P2 F22 89.73(13) . . ? F23 P2 F22 89.77(13) . . ? F26 P2 F22 89.02(13) . . ? F21 P2 F22 178.98(12) . . ? F39 P3 F310 99.8(11) . . ? F39 P3 F35 133.3(8) . . ? F310 P3 F35 34.4(10) . . ? F39 P3 F32 81.4(5) . . ? F310 P3 F32 93.9(8) . . ? F35 P3 F32 91.35(13) . . ? F39 P3 F36 135.4(8) . . ? F310 P3 F36 124.6(10) . . ? F35 P3 F36 90.46(17) . . ? F32 P3 F36 91.02(13) . . ? F39 P3 F34 43.4(8) . . ? F310 P3 F34 56.8(10) . . ? F35 P3 F34 91.08(17) . . ? F32 P3 F34 90.52(13) . . ? F36 P3 F34 177.80(16) . . ? F39 P3 F31 98.3(5) . . ? F310 P3 F31 87.0(8) . . ? F35 P3 F31 89.50(13) . . ? F32 P3 F31 179.05(13) . . ? F36 P3 F31 88.57(13) . . ? F34 P3 F31 89.86(13) . . ? F39 P3 F33 47.2(8) . . ? F310 P3 F33 145.0(10) . . ? F35 P3 F33 176.60(14) . . ? F32 P3 F33 92.05(13) . . ? F36 P3 F33 89.64(17) . . ? F34 P3 F33 88.74(16) . . ? F31 P3 F33 87.10(12) . . ? F39 P3 F38 88.6(11) . . ? F310 P3 F38 164.5(13) . . ? F35 P3 F38 133.8(9) . . ? F32 P3 F38 74.4(7) . . ? F36 P3 F38 47.4(8) . . ? F34 P3 F38 131.7(9) . . ? F31 P3 F38 104.7(7) . . ? F33 P3 F38 47.7(9) . . ? F39 P3 F37 168.5(7) . . ? F310 P3 F37 86.3(11) . . ? F35 P3 F37 51.9(7) . . ? F32 P3 F37 88.5(5) . . ? F36 P3 F37 38.7(7) . . ? F34 P3 F37 143.0(7) . . ? F31 P3 F37 91.7(5) . . ? F33 P3 F37 128.3(7) . . ? F38 P3 F37 83.3(10) . . ? F48 P4 F44 149.2(4) . . ? F48 P4 F410 97.6(5) . . ? F44 P4 F410 112.5(4) . . ? F48 P4 F46 57.0(4) . . ? F44 P4 F46 92.8(2) . . ? F410 P4 F46 154.7(4) . . ? F48 P4 F41 93.3(3) . . ? F44 P4 F41 92.55(19) . . ? F410 P4 F41 91.1(4) . . ? F46 P4 F41 89.81(18) . . ? F48 P4 F43 118.4(4) . . ? F44 P4 F43 91.8(3) . . ? F410 P4 F43 20.8(4) . . ? F46 P4 F43 175.4(3) . . ? F41 P4 F43 90.5(3) . . ? F48 P4 F42 87.5(3) . . ? F44 P4 F42 86.96(19) . . ? F410 P4 F42 88.3(4) . . ? F46 P4 F42 91.06(18) . . ? F41 P4 F42 179.02(12) . . ? F43 P4 F42 88.7(3) . . ? F48 P4 F47 91.8(4) . . ? F44 P4 F47 58.1(3) . . ? F410 P4 F47 170.6(4) . . ? F46 P4 F47 34.8(3) . . ? F41 P4 F47 88.7(2) . . ? F43 P4 F47 149.8(4) . . ? F42 P4 F47 91.7(2) . . ? F48 P4 F45 32.1(4) . . ? F44 P4 F45 178.0(2) . . ? F410 P4 F45 66.0(3) . . ? F46 P4 F45 88.7(2) . . ? F41 P4 F45 88.82(17) . . ? F43 P4 F45 86.7(3) . . ? F42 P4 F45 91.64(17) . . ? F47 P4 F45 123.4(3) . . ? F48 P4 F49 176.7(4) . . ? F44 P4 F49 27.7(3) . . ? F410 P4 F49 85.7(4) . . ? F46 P4 F49 119.7(4) . . ? F41 P4 F49 86.2(3) . . ? F43 P4 F49 64.9(4) . . ? F42 P4 F49 93.0(3) . . ? F47 P4 F49 84.9(4) . . ? F45 P4 F49 151.1(4) . . ? O120 C120 C121 122.1(4) . . ? O120 C120 C122 120.1(4) . . ? C121 C120 C122 117.8(4) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C120 C122 H12D 109.5 . . ? C120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? O130 C130 C132 122.9(6) . . ? O130 C130 C131 120.1(5) . . ? C132 C130 C131 117.0(6) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.822 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.068 data_jrp114cus _database_code_depnum_ccdc_archive 'CCDC 629021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H40 Cl16 Cu4 N16' _chemical_formula_sum 'C72 H40 Cl16 Cu4 N16' _chemical_formula_weight 1950.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 20.4033(7) _cell_length_b 13.4597(4) _cell_length_c 21.0965(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.697(2) _cell_angle_gamma 90.00 _cell_volume 5781.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour red-black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 111556 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11361 _reflns_number_gt 7918 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. the anions and solvents were modelled tentatively as two hexaflourophosphate anions, two and half acetones and one diethyl ether for every asymmetric unit (R1 = 0.0657 before squeeze). However, due to substantial disorder the anions and solvent molecules were removed by squeeze. Electron count/cell =1111 and 2 PF6-, 21/2 acetones and a diethylether in the asymmetric unit would account for 1048 electrons/cell, R1 = 0.0519 after squeeze. ; _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^)+(0.0887P)^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_number_reflns 11361 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.301314(19) 0.45272(3) 0.138225(18) 0.02949(12) Uani 1 1 d . . . Cu2 Cu 0.36699(2) 0.44944(3) 0.305633(17) 0.02904(12) Uani 1 1 d . . . N1 N 0.32516(12) 0.33231(18) 0.19019(12) 0.0294(6) Uani 1 1 d . . . N2 N 0.34648(13) 0.33196(18) 0.25166(12) 0.0288(6) Uani 1 1 d . . . C2 C 0.36103(18) 0.2434(2) 0.28025(16) 0.0382(8) Uani 1 1 d . . . C3 C 0.3542(2) 0.1534(3) 0.2493(2) 0.0597(12) Uani 1 1 d . . . H3 H 0.3638 0.0926 0.2708 0.072 Uiso 1 1 calc R . . C4 C 0.3331(2) 0.1550(3) 0.18631(19) 0.0543(11) Uani 1 1 d . . . H4 H 0.3279 0.0952 0.1626 0.065 Uiso 1 1 calc R . . C5 C 0.31946(16) 0.2466(2) 0.15815(16) 0.0336(8) Uani 1 1 d . . . C6 C 0.29765(15) 0.2600(2) 0.09090(15) 0.0325(7) Uani 1 1 d . . . H6 H 0.2968 0.2050 0.0627 0.039 Uiso 1 1 calc R . . N3 N 0.28004(13) 0.34455(19) 0.07075(12) 0.0296(6) Uani 1 1 d . . . C8 C 0.25511(16) 0.3548(2) 0.00750(15) 0.0327(7) Uani 1 1 d . . . C9 C 0.26623(16) 0.4479(2) -0.02261(16) 0.0352(8) Uani 1 1 d . . . H9 H 0.2885 0.5004 -0.0001 0.042 Uiso 1 1 calc R . . C10 C 0.24365(19) 0.4595(3) -0.08528(17) 0.0424(9) Uani 1 1 d . . . Cl1 Cl 0.25781(5) 0.56718(8) -0.12422(5) 0.0524(3) Uani 1 1 d . . . C11 C 0.20786(19) 0.3834(3) -0.11862(18) 0.0503(10) Uani 1 1 d . . . H11 H 0.1928 0.3916 -0.1618 0.060 Uiso 1 1 calc R . . C12 C 0.19580(19) 0.2979(3) -0.08655(18) 0.0493(10) Uani 1 1 d . . . Cl2 Cl 0.14742(6) 0.20629(8) -0.12576(5) 0.0652(3) Uani 1 1 d . . . C13 C 0.21890(16) 0.2797(3) -0.02520(16) 0.0373(8) Uani 1 1 d . . . H13 H 0.2107 0.2180 -0.0053 0.045 Uiso 1 1 calc R . . C16 C 0.38574(18) 0.2541(2) 0.34752(17) 0.0409(9) Uani 1 1 d . . . H16 H 0.3963 0.1976 0.3731 0.049 Uiso 1 1 calc R . . N4 N 0.39238(13) 0.34258(19) 0.37004(12) 0.0336(6) Uani 1 1 d . . . C18 C 0.41710(17) 0.3550(3) 0.43406(16) 0.0389(8) Uani 1 1 d . . . C19 C 0.40154(17) 0.4438(2) 0.46417(16) 0.0366(8) Uani 1 1 d . . . H19 H 0.3756 0.4929 0.4420 0.044 Uiso 1 1 calc R . . C20 C 0.42425(18) 0.4592(3) 0.52631(17) 0.0427(9) Uani 1 1 d . . . Cl3 Cl 0.40526(5) 0.56754(7) 0.56373(5) 0.0509(3) Uani 1 1 d . . . C21 C 0.46409(19) 0.3902(3) 0.55836(17) 0.0463(9) Uani 1 1 d . . . H21 H 0.4793 0.4011 0.6013 0.056 Uiso 1 1 calc R . . C22 C 0.4817(2) 0.3041(3) 0.52655(19) 0.0530(10) Uani 1 1 d . . . Cl4 Cl 0.53307(7) 0.21992(10) 0.56583(5) 0.0806(4) Uani 1 1 d . . . C23 C 0.45796(19) 0.2856(3) 0.46568(17) 0.0447(9) Uani 1 1 d . . . H23 H 0.4692 0.2258 0.4450 0.054 Uiso 1 1 calc R . . N31 N 0.24600(13) 0.56972(18) 0.15797(12) 0.0279(6) Uani 1 1 d . . . N32 N 0.18520(13) 0.56733(17) 0.17665(11) 0.0267(6) Uani 1 1 d . . . C32 C 0.15268(17) 0.6552(2) 0.18338(15) 0.0335(8) Uani 1 1 d . . . C33 C 0.18057(18) 0.7464(2) 0.17430(17) 0.0400(8) Uani 1 1 d . . . H33 H 0.1567 0.8060 0.1801 0.048 Uiso 1 1 calc R . . C34 C 0.24430(18) 0.7488(2) 0.15651(17) 0.0415(8) Uani 1 1 d . . . H34 H 0.2663 0.8100 0.1509 0.050 Uiso 1 1 calc R . . C35 C 0.27528(16) 0.6592(2) 0.14715(15) 0.0319(7) Uani 1 1 d . . . C36 C 0.34155(17) 0.6499(2) 0.12608(18) 0.0411(9) Uani 1 1 d . . . H36 H 0.3659 0.7076 0.1168 0.049 Uiso 1 1 calc R . . N33 N 0.36686(14) 0.56361(19) 0.12005(13) 0.0336(6) Uani 1 1 d . . . C38 C 0.43211(18) 0.5535(3) 0.10012(16) 0.0398(8) Uani 1 1 d . . . C39 C 0.46686(17) 0.6317(3) 0.07345(16) 0.0438(9) Uani 1 1 d . . . H39 H 0.4469 0.6948 0.0661 0.053 Uiso 1 1 calc R . . C40 C 0.5296(2) 0.6148(4) 0.05849(19) 0.0625(13) Uani 1 1 d . . . Cl31 Cl 0.57317(6) 0.70973(12) 0.02518(6) 0.0839(4) Uani 1 1 d . . . C41 C 0.5608(2) 0.5244(5) 0.0672(2) 0.0693(15) Uani 1 1 d . . . H41 H 0.6049 0.5151 0.0564 0.083 Uiso 1 1 calc R . . C42 C 0.5256(2) 0.4480(4) 0.0922(2) 0.0610(13) Uani 1 1 d . . . Cl32 Cl 0.56230(6) 0.33252(11) 0.10285(7) 0.0944(5) Uani 1 1 d . . . C43 C 0.46183(19) 0.4604(3) 0.10934(19) 0.0494(10) Uani 1 1 d . . . H43 H 0.4387 0.4069 0.1270 0.059 Uiso 1 1 calc R . . C46 C 0.08568(17) 0.6432(2) 0.20201(15) 0.0327(7) Uani 1 1 d . . . H46 H 0.0579 0.6993 0.2058 0.039 Uiso 1 1 calc R . . N34 N 0.06491(13) 0.55513(18) 0.21328(11) 0.0283(6) Uani 1 1 d . . . C48 C -0.00102(17) 0.5414(2) 0.23171(15) 0.0326(7) Uani 1 1 d . . . C49 C -0.03660(17) 0.6160(3) 0.25752(15) 0.0367(8) Uani 1 1 d . . . H49 H -0.0180 0.6800 0.2648 0.044 Uiso 1 1 calc R . . C50 C -0.10098(18) 0.5955(3) 0.27283(17) 0.0457(9) Uani 1 1 d . . . Cl33 Cl -0.14754(5) 0.68736(9) 0.30513(5) 0.0640(3) Uani 1 1 d . . . C51 C -0.12986(19) 0.5038(3) 0.26223(17) 0.0491(10) Uani 1 1 d . . . H51 H -0.1741 0.4917 0.2716 0.059 Uiso 1 1 calc R . . C52 C -0.0910(2) 0.4284(3) 0.23693(17) 0.0443(9) Uani 1 1 d . . . Cl34 Cl -0.12597(6) 0.31262(8) 0.22523(6) 0.0675(3) Uani 1 1 d . . . C53 C -0.02810(17) 0.4456(3) 0.22279(16) 0.0374(8) Uani 1 1 d . . . H53 H -0.0024 0.3934 0.2070 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0347(2) 0.0229(2) 0.0310(2) -0.00230(15) 0.00252(17) 0.00421(16) Cu2 0.0374(2) 0.0212(2) 0.0285(2) -0.00071(15) 0.00214(17) -0.00118(16) N1 0.0264(14) 0.0266(13) 0.0345(15) -0.0024(11) -0.0026(12) 0.0016(11) N2 0.0340(15) 0.0225(13) 0.0293(15) 0.0010(11) -0.0017(12) -0.0016(11) C2 0.051(2) 0.0245(16) 0.0380(19) 0.0047(14) -0.0088(16) -0.0002(15) C3 0.087(3) 0.0259(18) 0.062(3) 0.0056(18) -0.024(2) 0.003(2) C4 0.074(3) 0.0262(18) 0.059(3) -0.0103(17) -0.024(2) 0.0086(18) C5 0.0310(18) 0.0300(17) 0.0396(19) -0.0027(14) -0.0002(15) -0.0008(14) C6 0.0273(17) 0.0340(18) 0.0361(19) -0.0090(14) 0.0023(14) 0.0032(14) N3 0.0266(14) 0.0340(15) 0.0285(14) -0.0075(11) 0.0038(12) 0.0010(12) C8 0.0315(18) 0.0340(17) 0.0325(18) -0.0106(14) 0.0019(15) 0.0057(14) C9 0.0301(18) 0.0424(19) 0.0333(19) -0.0049(15) 0.0050(15) 0.0107(15) C10 0.045(2) 0.050(2) 0.032(2) 0.0008(16) 0.0050(17) 0.0082(18) Cl1 0.0564(6) 0.0603(6) 0.0416(5) 0.0096(4) 0.0111(5) 0.0078(5) C11 0.040(2) 0.082(3) 0.029(2) -0.006(2) 0.0011(16) 0.000(2) C12 0.046(2) 0.062(3) 0.040(2) -0.0223(19) 0.0014(18) 0.0064(19) Cl2 0.0718(7) 0.0656(7) 0.0550(6) -0.0216(5) -0.0205(5) -0.0043(6) C13 0.0341(19) 0.0397(18) 0.0371(19) -0.0133(15) -0.0060(15) 0.0105(15) C16 0.050(2) 0.0264(17) 0.045(2) 0.0100(15) -0.0100(17) -0.0020(16) N4 0.0348(16) 0.0339(15) 0.0320(15) 0.0039(12) -0.0002(12) -0.0039(12) C18 0.036(2) 0.0408(19) 0.039(2) 0.0052(16) 0.0004(16) -0.0085(16) C19 0.039(2) 0.0356(18) 0.0353(19) 0.0042(15) 0.0038(16) -0.0081(15) C20 0.0316(19) 0.062(2) 0.036(2) -0.0013(17) 0.0103(16) -0.0135(17) Cl3 0.0571(6) 0.0523(6) 0.0438(5) -0.0104(4) 0.0078(5) -0.0109(5) C21 0.052(2) 0.053(2) 0.033(2) 0.0055(17) -0.0002(18) -0.0046(19) C22 0.052(3) 0.056(2) 0.049(2) 0.0139(19) -0.0120(19) -0.001(2) Cl4 0.0946(9) 0.0863(9) 0.0561(7) -0.0011(6) -0.0322(6) 0.0348(7) C23 0.049(2) 0.045(2) 0.040(2) 0.0059(16) 0.0051(18) 0.0084(18) N31 0.0324(15) 0.0237(13) 0.0276(14) -0.0030(10) 0.0010(12) 0.0020(11) N32 0.0357(16) 0.0234(13) 0.0210(13) -0.0020(10) 0.0010(11) 0.0020(11) C32 0.042(2) 0.0279(16) 0.0305(18) -0.0046(13) 0.0026(15) 0.0053(15) C33 0.048(2) 0.0241(16) 0.049(2) -0.0011(15) 0.0109(18) 0.0078(15) C34 0.044(2) 0.0288(18) 0.052(2) -0.0008(15) 0.0042(17) -0.0021(16) C35 0.0344(19) 0.0271(16) 0.0349(18) -0.0036(13) 0.0080(15) -0.0022(14) C36 0.037(2) 0.0284(17) 0.059(2) -0.0095(16) 0.0090(18) -0.0126(15) N33 0.0333(16) 0.0334(15) 0.0341(16) -0.0007(12) 0.0017(12) 0.0000(12) C38 0.037(2) 0.051(2) 0.0309(19) -0.0110(16) -0.0024(15) 0.0004(17) C39 0.030(2) 0.064(2) 0.037(2) -0.0066(18) 0.0042(16) -0.0053(18) C40 0.041(3) 0.110(4) 0.036(2) -0.007(2) 0.0014(19) -0.023(3) Cl31 0.0453(6) 0.1463(13) 0.0618(7) 0.0014(7) 0.0157(6) -0.0312(7) C41 0.035(2) 0.130(5) 0.043(3) -0.031(3) -0.002(2) 0.009(3) C42 0.039(2) 0.080(3) 0.061(3) -0.033(2) -0.015(2) 0.017(2) Cl32 0.0681(8) 0.1107(11) 0.0998(10) -0.0534(8) -0.0289(7) 0.0484(8) C43 0.034(2) 0.060(3) 0.053(2) -0.0139(19) -0.0064(18) 0.0117(18) C46 0.037(2) 0.0316(17) 0.0302(18) -0.0040(14) 0.0056(15) 0.0016(15) N34 0.0360(16) 0.0268(13) 0.0219(13) 0.0028(10) 0.0000(12) 0.0039(12) C48 0.0373(19) 0.0380(18) 0.0227(16) 0.0081(13) 0.0038(14) 0.0028(15) C49 0.036(2) 0.0425(19) 0.0317(19) 0.0027(15) 0.0052(15) 0.0048(16) C50 0.036(2) 0.063(3) 0.039(2) 0.0057(18) 0.0079(17) 0.0028(19) Cl33 0.0474(6) 0.0843(8) 0.0626(7) -0.0031(6) 0.0223(5) 0.0167(6) C51 0.038(2) 0.071(3) 0.039(2) 0.0150(19) 0.0099(18) -0.003(2) C52 0.057(3) 0.041(2) 0.034(2) 0.0081(15) -0.0042(18) -0.0139(18) Cl34 0.0675(7) 0.0609(7) 0.0727(8) 0.0162(5) -0.0055(6) -0.0288(6) C53 0.035(2) 0.043(2) 0.0338(19) 0.0099(15) -0.0017(15) 0.0009(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N31 1.997(2) . y Cu1 N1 1.999(3) . y Cu1 N33 2.056(3) . y Cu1 N3 2.063(2) . y Cu2 N32 1.960(2) 2 y Cu2 N2 1.977(2) . y Cu2 N4 2.023(3) . y Cu2 N34 2.046(3) 2 y N1 C5 1.339(4) . ? N1 N2 1.341(4) . ? N2 C2 1.360(4) . ? C2 C3 1.379(5) . ? C2 C16 1.482(5) . ? C3 C4 1.370(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.471(5) . ? C6 N3 1.259(4) . ? C6 H6 0.9500 . ? N3 C8 1.404(4) . ? C8 C13 1.407(4) . ? C8 C9 1.430(5) . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 C11 1.418(5) . ? C10 Cl1 1.700(4) . ? C11 C12 1.365(6) . ? C11 H11 0.9500 . ? C12 C13 1.371(5) . ? C12 Cl2 1.753(4) . ? C13 H13 0.9500 . ? C16 N4 1.286(4) . ? C16 H16 0.9500 . ? N4 C18 1.421(4) . ? C18 C23 1.393(5) . ? C18 C19 1.400(5) . ? C19 C20 1.378(5) . ? C19 H19 0.9500 . ? C20 C21 1.382(5) . ? C20 Cl3 1.715(4) . ? C21 C22 1.398(5) . ? C21 H21 0.9500 . ? C22 C23 1.366(5) . ? C22 Cl4 1.720(4) . ? C23 H23 0.9500 . ? N31 N32 1.326(4) . ? N31 C35 1.370(4) . ? N32 C32 1.367(4) . ? N32 Cu2 1.960(3) 2 ? C32 C33 1.372(5) . ? C32 C46 1.455(5) . ? C33 C34 1.377(5) . ? C33 H33 0.9500 . ? C34 C35 1.382(4) . ? C34 H34 0.9500 . ? C35 C36 1.456(5) . ? C36 N33 1.280(4) . ? C36 H36 0.9500 . ? N33 C38 1.428(4) . ? C38 C43 1.400(5) . ? C38 C39 1.407(5) . ? C39 C40 1.357(6) . ? C39 H39 0.9500 . ? C40 C41 1.381(7) . ? C40 Cl31 1.731(5) . ? C41 C42 1.378(7) . ? C41 H41 0.9500 . ? C42 C43 1.382(6) . ? C42 Cl32 1.734(5) . ? C43 H43 0.9500 . ? C46 N34 1.286(4) . ? C46 H46 0.9500 . ? N34 C48 1.436(4) . ? N34 Cu2 2.046(3) 2 ? C48 C49 1.372(5) . ? C48 C53 1.410(5) . ? C49 C50 1.400(5) . ? C49 H49 0.9500 . ? C50 C51 1.380(6) . ? C50 Cl33 1.726(4) . ? C51 C52 1.413(5) . ? C51 H51 0.9500 . ? C52 C53 1.355(5) . ? C52 Cl34 1.726(4) . ? C53 H53 0.9500 . ? 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 N31 Cu1 N1 130.22(10) . . y N31 Cu1 N33 81.35(11) . . y N1 Cu1 N33 123.53(11) . . y N31 Cu1 N3 127.15(11) . . y N1 Cu1 N3 80.74(11) . . y N33 Cu1 N3 119.61(10) . . y N32 Cu2 N2 131.28(11) 2 . y N32 Cu2 N4 124.48(11) 2 . y N2 Cu2 N4 81.59(11) . . y N32 Cu2 N34 81.86(11) 2 2 y N2 Cu2 N34 124.40(10) . 2 y N4 Cu2 N34 118.53(11) . 2 y C5 N1 N2 119.8(3) . . ? C5 N1 Cu1 114.3(2) . . ? N2 N1 Cu1 125.84(18) . . ? N1 N2 C2 118.7(2) . . ? N1 N2 Cu2 126.69(18) . . ? C2 N2 Cu2 114.4(2) . . ? N2 C2 C3 123.2(3) . . ? N2 C2 C16 113.0(3) . . ? C3 C2 C16 123.8(3) . . ? C4 C3 C2 117.4(3) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 118.1(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 113.1(3) . . ? C4 C5 C6 124.2(3) . . ? N3 C6 C5 119.9(3) . . ? N3 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 N3 C8 119.2(3) . . ? C6 N3 Cu1 111.2(2) . . ? C8 N3 Cu1 129.3(2) . . ? N3 C8 C13 122.8(3) . . ? N3 C8 C9 116.8(3) . . ? C13 C8 C9 120.4(3) . . ? C10 C9 C8 118.1(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 121.6(3) . . ? C9 C10 Cl1 120.1(3) . . ? C11 C10 Cl1 118.3(3) . . ? C12 C11 C10 117.8(3) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C13 123.8(4) . . ? C11 C12 Cl2 118.2(3) . . ? C13 C12 Cl2 118.0(3) . . ? C12 C13 C8 118.2(4) . . ? C12 C13 H13 120.9 . . ? C8 C13 H13 120.9 . . ? N4 C16 C2 117.7(3) . . ? N4 C16 H16 121.1 . . ? C2 C16 H16 121.1 . . ? C16 N4 C18 118.9(3) . . ? C16 N4 Cu2 113.2(2) . . ? C18 N4 Cu2 127.9(2) . . ? C23 C18 C19 120.1(3) . . ? C23 C18 N4 122.7(3) . . ? C19 C18 N4 117.1(3) . . ? C20 C19 C18 119.2(3) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 Cl3 119.6(3) . . ? C21 C20 Cl3 119.3(3) . . ? C20 C21 C22 118.9(4) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 121.1(4) . . ? C23 C22 Cl4 120.1(3) . . ? C21 C22 Cl4 118.8(3) . . ? C22 C23 C18 119.5(4) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? N32 N31 C35 119.8(2) . . ? N32 N31 Cu1 126.52(18) . . ? C35 N31 Cu1 113.6(2) . . ? N31 N32 C32 118.7(2) . . ? N31 N32 Cu2 127.33(18) . 2 ? C32 N32 Cu2 114.0(2) . 2 ? N32 C32 C33 123.4(3) . . ? N32 C32 C46 113.8(3) . . ? C33 C32 C46 122.8(3) . . ? C32 C33 C34 117.8(3) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C33 C34 C35 117.9(3) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? N31 C35 C34 122.3(3) . . ? N31 C35 C36 113.5(3) . . ? C34 C35 C36 124.1(3) . . ? N33 C36 C35 119.8(3) . . ? N33 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 N33 C38 120.4(3) . . ? C36 N33 Cu1 111.6(2) . . ? C38 N33 Cu1 128.0(2) . . ? C43 C38 C39 120.0(4) . . ? C43 C38 N33 116.6(3) . . ? C39 C38 N33 123.3(3) . . ? C40 C39 C38 118.3(4) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? C39 C40 C41 123.4(4) . . ? C39 C40 Cl31 119.2(4) . . ? C41 C40 Cl31 117.4(4) . . ? C42 C41 C40 117.5(4) . . ? C42 C41 H41 121.3 . . ? C40 C41 H41 121.3 . . ? C41 C42 C43 122.2(4) . . ? C41 C42 Cl32 119.1(4) . . ? C43 C42 Cl32 118.7(4) . . ? C42 C43 C38 118.5(4) . . ? C42 C43 H43 120.7 . . ? C38 C43 H43 120.7 . . ? N34 C46 C32 118.6(3) . . ? N34 C46 H46 120.7 . . ? C32 C46 H46 120.7 . . ? C46 N34 C48 119.6(3) . . ? C46 N34 Cu2 111.7(2) . 2 ? C48 N34 Cu2 128.5(2) . 2 ? C49 C48 C53 120.6(3) . . ? C49 C48 N34 122.8(3) . . ? C53 C48 N34 116.6(3) . . ? C48 C49 C50 118.4(3) . . ? C48 C49 H49 120.8 . . ? C50 C49 H49 120.8 . . ? C51 C50 C49 122.4(4) . . ? C51 C50 Cl33 117.7(3) . . ? C49 C50 Cl33 119.9(3) . . ? C50 C51 C52 117.3(3) . . ? C50 C51 H51 121.3 . . ? C52 C51 H51 121.3 . . ? C53 C52 C51 121.6(3) . . ? C53 C52 Cl34 120.7(3) . . ? C51 C52 Cl34 117.7(3) . . ? C52 C53 C48 119.6(3) . . ? C52 C53 H53 120.2 . . ? C48 C53 H53 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 Cu1 N1 C5 134.5(2) . . . . ? N33 Cu1 N1 C5 -116.6(2) . . . . ? N3 Cu1 N1 C5 2.9(2) . . . . ? N31 Cu1 N1 N2 -46.7(3) . . . . ? N33 Cu1 N1 N2 62.2(3) . . . . ? N3 Cu1 N1 N2 -178.3(3) . . . . ? C5 N1 N2 C2 -0.9(4) . . . . ? Cu1 N1 N2 C2 -179.7(2) . . . . ? C5 N1 N2 Cu2 173.5(2) . . . . ? Cu1 N1 N2 Cu2 -5.3(4) . . . . ? N32 Cu2 N2 N1 53.5(3) 2 . . . ? N4 Cu2 N2 N1 -177.4(3) . . . . ? N34 Cu2 N2 N1 -58.4(3) 2 . . . ? N32 Cu2 N2 C2 -132.0(2) 2 . . . ? N4 Cu2 N2 C2 -2.8(2) . . . . ? N34 Cu2 N2 C2 116.1(2) 2 . . . ? N1 N2 C2 C3 -0.8(5) . . . . ? Cu2 N2 C2 C3 -175.8(3) . . . . ? N1 N2 C2 C16 178.4(3) . . . . ? Cu2 N2 C2 C16 3.4(4) . . . . ? N2 C2 C3 C4 1.5(7) . . . . ? C16 C2 C3 C4 -177.6(4) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? N2 N1 C5 C4 1.8(5) . . . . ? Cu1 N1 C5 C4 -179.2(3) . . . . ? N2 N1 C5 C6 -178.1(3) . . . . ? Cu1 N1 C5 C6 0.9(3) . . . . ? C3 C4 C5 N1 -1.1(6) . . . . ? C3 C4 C5 C6 178.8(4) . . . . ? N1 C5 C6 N3 -7.3(4) . . . . ? C4 C5 C6 N3 172.8(3) . . . . ? C5 C6 N3 C8 -175.7(3) . . . . ? C5 C6 N3 Cu1 9.4(4) . . . . ? N31 Cu1 N3 C6 -140.9(2) . . . . ? N1 Cu1 N3 C6 -6.7(2) . . . . ? N33 Cu1 N3 C6 116.8(2) . . . . ? N31 Cu1 N3 C8 44.9(3) . . . . ? N1 Cu1 N3 C8 179.1(3) . . . . ? N33 Cu1 N3 C8 -57.5(3) . . . . ? C6 N3 C8 C13 32.4(5) . . . . ? Cu1 N3 C8 C13 -153.7(2) . . . . ? C6 N3 C8 C9 -149.6(3) . . . . ? Cu1 N3 C8 C9 24.2(4) . . . . ? N3 C8 C9 C10 178.5(3) . . . . ? C13 C8 C9 C10 -3.5(5) . . . . ? C8 C9 C10 C11 2.7(5) . . . . ? C8 C9 C10 Cl1 -177.9(2) . . . . ? C9 C10 C11 C12 0.5(6) . . . . ? Cl1 C10 C11 C12 -178.9(3) . . . . ? C10 C11 C12 C13 -3.2(6) . . . . ? C10 C11 C12 Cl2 176.3(3) . . . . ? C11 C12 C13 C8 2.5(6) . . . . ? Cl2 C12 C13 C8 -177.0(3) . . . . ? N3 C8 C13 C12 178.9(3) . . . . ? C9 C8 C13 C12 1.0(5) . . . . ? N2 C2 C16 N4 -2.0(5) . . . . ? C3 C2 C16 N4 177.1(4) . . . . ? C2 C16 N4 C18 -178.9(3) . . . . ? C2 C16 N4 Cu2 -0.3(4) . . . . ? N32 Cu2 N4 C16 136.7(2) 2 . . . ? N2 Cu2 N4 C16 1.7(3) . . . . ? N34 Cu2 N4 C16 -123.1(2) 2 . . . ? N32 Cu2 N4 C18 -44.9(3) 2 . . . ? N2 Cu2 N4 C18 -179.9(3) . . . . ? N34 Cu2 N4 C18 55.4(3) 2 . . . ? C16 N4 C18 C23 26.4(5) . . . . ? Cu2 N4 C18 C23 -151.9(3) . . . . ? C16 N4 C18 C19 -156.9(3) . . . . ? Cu2 N4 C18 C19 24.8(4) . . . . ? C23 C18 C19 C20 -3.4(5) . . . . ? N4 C18 C19 C20 179.8(3) . . . . ? C18 C19 C20 C21 2.6(5) . . . . ? C18 C19 C20 Cl3 -179.8(3) . . . . ? C19 C20 C21 C22 0.4(6) . . . . ? Cl3 C20 C21 C22 -177.2(3) . . . . ? C20 C21 C22 C23 -2.7(6) . . . . ? C20 C21 C22 Cl4 178.3(3) . . . . ? C21 C22 C23 C18 1.9(6) . . . . ? Cl4 C22 C23 C18 -179.1(3) . . . . ? C19 C18 C23 C22 1.2(5) . . . . ? N4 C18 C23 C22 177.8(3) . . . . ? N1 Cu1 N31 N32 -53.2(3) . . . . ? N33 Cu1 N31 N32 179.7(3) . . . . ? N3 Cu1 N31 N32 58.9(3) . . . . ? N1 Cu1 N31 C35 130.3(2) . . . . ? N33 Cu1 N31 C35 3.2(2) . . . . ? N3 Cu1 N31 C35 -117.6(2) . . . . ? C35 N31 N32 C32 1.3(4) . . . . ? Cu1 N31 N32 C32 -175.0(2) . . . . ? C35 N31 N32 Cu2 179.5(2) . . . 2 ? Cu1 N31 N32 Cu2 3.2(4) . . . 2 ? N31 N32 C32 C33 -2.7(5) . . . . ? Cu2 N32 C32 C33 178.9(3) 2 . . . ? N31 N32 C32 C46 178.1(3) . . . . ? Cu2 N32 C32 C46 -0.3(3) 2 . . . ? N32 C32 C33 C34 1.1(5) . . . . ? C46 C32 C33 C34 -179.8(3) . . . . ? C32 C33 C34 C35 1.9(5) . . . . ? N32 N31 C35 C34 1.7(5) . . . . ? Cu1 N31 C35 C34 178.4(3) . . . . ? N32 N31 C35 C36 -179.2(3) . . . . ? Cu1 N31 C35 C36 -2.4(4) . . . . ? C33 C34 C35 N31 -3.3(5) . . . . ? C33 C34 C35 C36 177.6(3) . . . . ? N31 C35 C36 N33 -0.7(5) . . . . ? C34 C35 C36 N33 178.4(3) . . . . ? C35 C36 N33 C38 -179.3(3) . . . . ? C35 C36 N33 Cu1 3.3(4) . . . . ? N31 Cu1 N33 C36 -3.5(2) . . . . ? N1 Cu1 N33 C36 -136.6(2) . . . . ? N3 Cu1 N33 C36 124.5(3) . . . . ? N31 Cu1 N33 C38 179.3(3) . . . . ? N1 Cu1 N33 C38 46.2(3) . . . . ? N3 Cu1 N33 C38 -52.6(3) . . . . ? C36 N33 C38 C43 165.0(3) . . . . ? Cu1 N33 C38 C43 -18.0(4) . . . . ? C36 N33 C38 C39 -13.9(5) . . . . ? Cu1 N33 C38 C39 163.1(3) . . . . ? C43 C38 C39 C40 -1.4(5) . . . . ? N33 C38 C39 C40 177.5(3) . . . . ? C38 C39 C40 C41 1.0(6) . . . . ? C38 C39 C40 Cl31 179.6(3) . . . . ? C39 C40 C41 C42 0.3(6) . . . . ? Cl31 C40 C41 C42 -178.4(3) . . . . ? C40 C41 C42 C43 -1.2(6) . . . . ? C40 C41 C42 Cl32 179.0(3) . . . . ? C41 C42 C43 C38 0.8(6) . . . . ? Cl32 C42 C43 C38 -179.4(3) . . . . ? C39 C38 C43 C42 0.5(5) . . . . ? N33 C38 C43 C42 -178.4(3) . . . . ? N32 C32 C46 N34 3.4(4) . . . . ? C33 C32 C46 N34 -175.8(3) . . . . ? C32 C46 N34 C48 -180.0(3) . . . . ? C32 C46 N34 Cu2 -4.6(4) . . . 2 ? C46 N34 C48 C49 -21.4(4) . . . . ? Cu2 N34 C48 C49 164.0(2) 2 . . . ? C46 N34 C48 C53 159.4(3) . . . . ? Cu2 N34 C48 C53 -15.2(4) 2 . . . ? C53 C48 C49 C50 -2.0(5) . . . . ? N34 C48 C49 C50 178.8(3) . . . . ? C48 C49 C50 C51 -0.8(5) . . . . ? C48 C49 C50 Cl33 -179.8(3) . . . . ? C49 C50 C51 C52 2.2(5) . . . . ? Cl33 C50 C51 C52 -178.8(3) . . . . ? C50 C51 C52 C53 -0.9(5) . . . . ? C50 C51 C52 Cl34 178.5(3) . . . . ? C51 C52 C53 C48 -1.8(5) . . . . ? Cl34 C52 C53 C48 178.9(3) . . . . ? C49 C48 C53 C52 3.3(5) . . . . ? N34 C48 C53 C52 -177.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.850 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.082 # Attachment 'mm_difluoro_Cu_complex.cif' data_jrp136 _database_code_depnum_ccdc_archive 'CCDC 629022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H88 Cu4 F40 N16 O8 P4' _chemical_formula_sum 'C96 H88 Cu4 F40 N16 O8 P4' _chemical_formula_weight 2731.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9140(18) _cell_length_b 15.2869(19) _cell_length_c 26.383(3) _cell_angle_alpha 96.460(7) _cell_angle_beta 97.077(7) _cell_angle_gamma 111.931(7) _cell_volume 5454.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombic prism' _exptl_crystal_colour 'dark red-brown' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8774 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50328 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 20.82 _reflns_number_total 11304 _reflns_number_gt 6648 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-H ANIS. A total of eight acetone of solvation are present. Due to a weak data set with a strong drop off in reflections, [R(?) > 1 at 1.00 - 0.95 \%A] SHEL was used. Due to problems with severe anisotropy, restraints to anisotropic parameters for C, N, O and F were used (ISOR, SIMU, DELU) and the aromatic rings were made FLAT. Although the data for this structure is poorly resolved it can be readily seen that the JG2, 3,5-difluoro substituted ligand forms a [2 x 2] grid in the solid state. ; _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^)+(0.2000P)^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_number_reflns 11304 _refine_ls_number_parameters 1529 _refine_ls_number_restraints 2140 _refine_ls_R_factor_all 0.2404 _refine_ls_R_factor_gt 0.1729 _refine_ls_wR_factor_ref 0.5069 _refine_ls_wR_factor_gt 0.4722 _refine_ls_goodness_of_fit_ref 1.923 _refine_ls_restrained_S_all 1.788 _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 0.6352(2) 0.0454(2) 0.26645(10) 0.0319(9) Uani 1 1 d . . . Cu2 Cu 0.7561(2) 0.1608(2) 0.16121(10) 0.0317(9) Uani 1 1 d . . . Cu3 Cu 0.8504(2) 0.2554(2) 0.33869(10) 0.0322(9) Uani 1 1 d . . . Cu4 Cu 0.9638(2) 0.3741(2) 0.23465(10) 0.0335(9) Uani 1 1 d . . . N1 N 0.7389(10) 0.0189(11) 0.2349(6) 0.030(3) Uani 1 1 d DU . . N2 N 0.7818(11) 0.0629(11) 0.1974(6) 0.030(3) Uani 1 1 d DU . . C2 C 0.8460(13) 0.0305(14) 0.1781(7) 0.032(3) Uani 1 1 d DU . . C3 C 0.8687(14) -0.0421(14) 0.1942(7) 0.033(3) Uani 1 1 d DU . . H3A H 0.9143 -0.0623 0.1794 0.040 Uiso 1 1 calc R . . C4 C 0.8222(13) -0.0861(14) 0.2335(7) 0.033(3) Uani 1 1 d DU . . H4A H 0.8344 -0.1368 0.2466 0.040 Uiso 1 1 calc R . . C5 C 0.7602(13) -0.0514(14) 0.2509(7) 0.031(3) Uani 1 1 d DU . . C6 C 0.7067(15) -0.0933(15) 0.2928(8) 0.029(3) Uani 1 1 d U . . H6A H 0.7148 -0.1444 0.3075 0.035 Uiso 1 1 calc R . . N3 N 0.6467(13) -0.0524(12) 0.3076(7) 0.031(3) Uani 1 1 d U . . C8 C 0.5932(11) -0.0890(15) 0.3475(7) 0.036(3) Uani 1 1 d DU . . C9 C 0.5792(11) -0.1805(15) 0.3621(7) 0.039(3) Uani 1 1 d DU . . H9A H 0.6017 -0.2231 0.3439 0.046 Uiso 1 1 calc R . . C10 C 0.5337(10) -0.2034(17) 0.4018(7) 0.044(3) Uani 1 1 d DU . . C11 C 0.4981(10) -0.1433(16) 0.4308(8) 0.043(3) Uani 1 1 d DU . . H11A H 0.4660 -0.1632 0.4589 0.051 Uiso 1 1 calc R . . C12 C 0.5107(9) -0.0568(16) 0.4174(7) 0.038(3) Uani 1 1 d DU . . C13 C 0.5593(10) -0.0291(16) 0.3749(7) 0.035(3) Uani 1 1 d DU . . H13A H 0.5684 0.0314 0.3654 0.042 Uiso 1 1 calc R . . F1 F 0.5202(10) -0.2869(10) 0.4156(5) 0.062(4) Uani 1 1 d DU . . F2 F 0.4805(8) 0.0022(9) 0.4418(4) 0.045(3) Uani 1 1 d DU . . C16 C 0.8894(16) 0.0783(15) 0.1352(8) 0.031(3) Uani 1 1 d U . . H16A H 0.9344 0.0608 0.1183 0.037 Uiso 1 1 calc R . . N4 N 0.8623(12) 0.1437(12) 0.1227(7) 0.028(3) Uani 1 1 d U . . C18 C 0.9016(15) 0.1927(10) 0.0807(7) 0.030(3) Uani 1 1 d DU . . C19 C 0.9869(15) 0.2038(10) 0.0703(7) 0.031(3) Uani 1 1 d DU . . H19A H 1.0273 0.1809 0.0909 0.037 Uiso 1 1 calc R . . C20 C 1.0196(16) 0.2471(9) 0.0309(7) 0.037(3) Uani 1 1 d DU . . C21 C 0.9610(16) 0.2826(10) -0.0010(7) 0.039(3) Uani 1 1 d DU . . H21A H 0.9831 0.3135 -0.0291 0.046 Uiso 1 1 calc R . . C22 C 0.8741(16) 0.2697(9) 0.0110(7) 0.037(3) Uani 1 1 d DU . . C23 C 0.8394(15) 0.2258(10) 0.0511(7) 0.033(3) Uani 1 1 d DU . . H23A H 0.7764 0.2179 0.0587 0.040 Uiso 1 1 calc R . . F3 F 0.8141(9) 0.3024(9) -0.0184(5) 0.050(3) Uani 1 1 d DU . . F4 F 1.1089(9) 0.2606(9) 0.0184(5) 0.051(3) Uani 1 1 d DU . . N31 N 0.9556(11) 0.2317(11) 0.3043(6) 0.030(3) Uani 1 1 d DU . . N32 N 0.9938(11) 0.2749(10) 0.2652(6) 0.028(3) Uani 1 1 d DU . . C32 C 1.0633(13) 0.2543(13) 0.2463(7) 0.030(3) Uani 1 1 d DU . . C33 C 1.0993(14) 0.1874(13) 0.2661(7) 0.031(3) Uani 1 1 d DU . . H33A H 1.1491 0.1726 0.2526 0.037 Uiso 1 1 calc R . . C34 C 1.0574(13) 0.1454(14) 0.3063(7) 0.033(3) Uani 1 1 d DU . . H34A H 1.0781 0.1007 0.3211 0.039 Uiso 1 1 calc R . . C35 C 0.9870(13) 0.1692(13) 0.3239(7) 0.030(3) Uani 1 1 d DU . . C36 C 0.9347(15) 0.1269(15) 0.3658(8) 0.029(3) Uani 1 1 d U . . H36A H 0.9510 0.0819 0.3828 0.034 Uiso 1 1 calc R . . N33 N 0.8684(12) 0.1533(12) 0.3776(7) 0.030(3) Uani 1 1 d U . . C38 C 0.8174(11) 0.1130(15) 0.4172(7) 0.029(3) Uani 1 1 d DU . . C39 C 0.8111(10) 0.0257(15) 0.4296(7) 0.032(3) Uani 1 1 d DU . . H39A H 0.8397 -0.0114 0.4114 0.039 Uiso 1 1 calc R . . C40 C 0.7616(10) -0.0063(16) 0.4698(7) 0.037(3) Uani 1 1 d DU . . C41 C 0.7218(10) 0.0438(16) 0.4953(7) 0.038(3) Uani 1 1 d DU . . H41A H 0.6888 0.0191 0.5224 0.046 Uiso 1 1 calc R . . C42 C 0.7261(9) 0.1261(16) 0.4849(7) 0.035(3) Uani 1 1 d DU . . C43 C 0.7763(10) 0.1650(16) 0.4436(7) 0.034(3) Uani 1 1 d DU . . H43A H 0.7801 0.2250 0.4354 0.041 Uiso 1 1 calc R . . F31 F 0.7556(9) -0.0924(9) 0.4817(5) 0.051(3) Uani 1 1 d DU . . F32 F 0.6872(8) 0.1812(9) 0.5093(5) 0.047(3) Uani 1 1 d DU . . C46 C 1.0981(16) 0.3001(15) 0.2047(8) 0.032(3) Uani 1 1 d U . . H46A H 1.1460 0.2874 0.1880 0.039 Uiso 1 1 calc R . . N34 N 1.0611(13) 0.3609(13) 0.1902(7) 0.035(3) Uani 1 1 d U . . C48 C 1.0955(17) 0.4163(12) 0.1510(8) 0.039(3) Uani 1 1 d DU . . C49 C 1.1901(17) 0.4367(11) 0.1397(7) 0.041(4) Uani 1 1 d DU . . H49A H 1.2356 0.4174 0.1589 0.049 Uiso 1 1 calc R . . C50 C 1.2130(17) 0.4848(10) 0.1006(7) 0.041(3) Uani 1 1 d DU . . C51 C 1.1488(16) 0.5159(10) 0.0704(8) 0.042(4) Uani 1 1 d DU . . H51A H 1.1661 0.5499 0.0427 0.051 Uiso 1 1 calc R . . C52 C 1.0592(17) 0.4913(10) 0.0854(8) 0.043(3) Uani 1 1 d DU . . C53 C 1.0307(18) 0.4455(11) 0.1223(8) 0.043(4) Uani 1 1 d DU . . H53A H 0.9667 0.4319 0.1298 0.052 Uiso 1 1 calc R . . F33 F 1.3052(10) 0.5073(9) 0.0875(5) 0.055(3) Uani 1 1 d DU . . F34 F 0.9960(9) 0.5210(8) 0.0564(5) 0.047(3) Uani 1 1 d DU . . N61 N 0.6398(13) 0.1762(13) 0.2880(6) 0.032(3) Uani 1 1 d DU . . N62 N 0.7187(13) 0.2516(13) 0.3113(6) 0.030(3) Uani 1 1 d DU . . C62 C 0.7082(16) 0.3363(16) 0.3231(7) 0.036(3) Uani 1 1 d DU . . C63 C 0.6191(16) 0.3462(17) 0.3117(7) 0.037(4) Uani 1 1 d DU . . H63A H 0.6144 0.4061 0.3204 0.045 Uiso 1 1 calc R . . C64 C 0.5398(16) 0.2678(15) 0.2878(7) 0.035(4) Uani 1 1 d DU . . H64A H 0.4768 0.2696 0.2790 0.042 Uiso 1 1 calc R . . C65 C 0.5555(16) 0.1852(16) 0.2771(6) 0.032(3) Uani 1 1 d DU . . C66 C 0.4734(16) 0.0908(16) 0.2529(8) 0.033(4) Uani 1 1 d U . . H66A H 0.4071 0.0850 0.2478 0.040 Uiso 1 1 calc R . . N63 N 0.4938(13) 0.0205(13) 0.2397(7) 0.035(3) Uani 1 1 d U . . C68 C 0.4168(15) -0.0720(17) 0.2222(9) 0.048(4) Uani 1 1 d DU . . C69 C 0.3334(17) -0.1001(18) 0.2471(9) 0.054(4) Uani 1 1 d DU . . H69A H 0.3271 -0.0596 0.2752 0.065 Uiso 1 1 calc R . . C70 C 0.2628(18) -0.1899(18) 0.2275(9) 0.059(4) Uani 1 1 d DU . . C71 C 0.2642(18) -0.2526(19) 0.1882(9) 0.059(4) Uani 1 1 d DU . . H71A H 0.2122 -0.3137 0.1769 0.071 Uiso 1 1 calc R . . C72 C 0.3479(18) -0.2217(18) 0.1649(9) 0.062(4) Uani 1 1 d DU . . C73 C 0.4220(19) -0.1328(18) 0.1822(9) 0.058(4) Uani 1 1 d DU . . H73A H 0.4778 -0.1136 0.1658 0.070 Uiso 1 1 calc R . . F61 F 0.1811(11) -0.2201(11) 0.2504(6) 0.072(4) Uani 1 1 d DU . . F62 F 0.3568(12) -0.2785(11) 0.1255(6) 0.078(4) Uani 1 1 d DU . . C76 C 0.7952(16) 0.4155(17) 0.3548(9) 0.037(4) Uani 1 1 d U . . H76 H 0.7969 0.4781 0.3639 0.045 Uiso 1 1 calc R . . N64 N 0.8726(13) 0.3922(13) 0.3699(7) 0.037(3) Uani 1 1 d U . . C78 C 0.9528(18) 0.4610(16) 0.4036(8) 0.045(3) Uani 1 1 d DU . . C79 C 0.9557(19) 0.5388(16) 0.4353(8) 0.051(4) Uani 1 1 d DU . . H79A H 0.8967 0.5493 0.4341 0.061 Uiso 1 1 calc R . . C80 C 1.0329(19) 0.5999(16) 0.4672(8) 0.053(4) Uani 1 1 d DU . . C81 C 1.1249(19) 0.5900(17) 0.4717(8) 0.055(4) Uani 1 1 d DU . . H81 H 1.1815 0.6347 0.4949 0.066 Uiso 1 1 calc R . . C82 C 1.128(2) 0.5121(17) 0.4404(8) 0.056(4) Uani 1 1 d DU . . C83 C 1.0464(18) 0.4528(17) 0.4089(8) 0.052(4) Uani 1 1 d DU . . H83A H 1.0500 0.3999 0.3879 0.062 Uiso 1 1 calc R . . F63 F 1.0296(11) 0.6752(10) 0.4974(5) 0.065(4) Uani 1 1 d DU . . F64 F 1.2103(11) 0.5028(11) 0.4443(6) 0.073(4) Uani 1 1 d DU . . N91 N 0.7570(13) 0.2929(13) 0.1819(6) 0.033(3) Uani 1 1 d DU . . N92 N 0.8308(13) 0.3687(13) 0.2102(6) 0.033(3) Uani 1 1 d DU . . C92 C 0.8209(16) 0.4512(16) 0.2186(7) 0.033(3) Uani 1 1 d DU . . C93 C 0.7359(16) 0.4615(16) 0.1989(7) 0.036(4) Uani 1 1 d DU . . H93A H 0.7318 0.5221 0.2059 0.043 Uiso 1 1 calc R . . C94 C 0.6596(17) 0.3877(16) 0.1703(7) 0.036(4) Uani 1 1 d DU . . H94A H 0.6005 0.3933 0.1564 0.044 Uiso 1 1 calc R . . C95 C 0.6727(16) 0.3006(16) 0.1620(7) 0.034(3) Uani 1 1 d DU . . C96 C 0.5982(17) 0.2121(16) 0.1306(9) 0.037(4) Uani 1 1 d U . . H96A H 0.5354 0.2097 0.1166 0.044 Uiso 1 1 calc R . . N93 N 0.6189(13) 0.1367(13) 0.1221(7) 0.036(3) Uani 1 1 d U . . C98 C 0.5484(17) 0.0535(16) 0.0942(8) 0.041(3) Uani 1 1 d DU . . C99 C 0.4472(18) 0.0254(16) 0.0904(7) 0.046(4) Uani 1 1 d DU . . H99A H 0.4222 0.0663 0.1082 0.055 Uiso 1 1 calc R . . C100 C 0.3862(19) -0.0568(17) 0.0627(7) 0.050(4) Uani 1 1 d DU . . C101 C 0.4166(19) -0.1219(18) 0.0351(7) 0.054(4) Uani 1 1 d DU . . H10A H 0.3720 -0.1814 0.0151 0.065 Uiso 1 1 calc R . . C102 C 0.514(2) -0.0919(18) 0.0400(7) 0.059(4) Uani 1 1 d DU . . C103 C 0.581(2) -0.0084(17) 0.0678(7) 0.052(4) Uani 1 1 d DU . . H10B H 0.6493 0.0075 0.0691 0.063 Uiso 1 1 calc R . . F91 F 0.2871(11) -0.0854(10) 0.0586(5) 0.066(4) Uani 1 1 d DU . . F92 F 0.5485(12) -0.1551(12) 0.0128(6) 0.086(5) Uani 1 1 d DU . . C106 C 0.9088(16) 0.5260(16) 0.2484(8) 0.034(4) Uani 1 1 d U . . H10C H 0.9113 0.5892 0.2556 0.041 Uiso 1 1 calc R . . N94 N 0.9829(14) 0.5090(13) 0.2650(7) 0.038(3) Uani 1 1 d U . . C108 C 1.069(2) 0.5780(16) 0.2965(9) 0.054(4) Uani 1 1 d DU . . C109 C 1.061(2) 0.6505(16) 0.3359(8) 0.060(4) Uani 1 1 d DU . . H10D H 1.0008 0.6546 0.3407 0.072 Uiso 1 1 calc R . . C110 C 1.149(2) 0.7105(17) 0.3645(9) 0.067(4) Uani 1 1 d DU . . C111 C 1.245(2) 0.7103(18) 0.3603(9) 0.068(4) Uani 1 1 d DU . . H11B H 1.3043 0.7544 0.3816 0.082 Uiso 1 1 calc R . . C112 C 1.240(2) 0.6445(18) 0.3251(9) 0.068(4) Uani 1 1 d DU . . C113 C 1.157(2) 0.5811(17) 0.2945(9) 0.062(4) Uani 1 1 d DU . . H11C H 1.1623 0.5349 0.2693 0.074 Uiso 1 1 calc R . . F93 F 1.1432(12) 0.7792(11) 0.4018(6) 0.078(4) Uani 1 1 d DU . . F94 F 1.3303(12) 0.6414(12) 0.3195(6) 0.087(4) Uani 1 1 d DU . . P1 P 0.7573(5) 0.6643(5) 0.3392(3) 0.0442(19) Uani 1 1 d . . . F11 F 0.7730(11) 0.7599(10) 0.3738(6) 0.069(5) Uani 1 1 d U . . F12 F 0.7424(11) 0.5633(10) 0.3046(5) 0.061(4) Uani 1 1 d U . . F13 F 0.7430(16) 0.7075(14) 0.2910(8) 0.113(7) Uani 1 1 d U . . F14 F 0.8688(17) 0.7006(16) 0.3371(9) 0.133(8) Uani 1 1 d U . . F15 F 0.7760(15) 0.6204(14) 0.3904(8) 0.106(6) Uani 1 1 d U . . F16 F 0.6493(15) 0.6228(15) 0.3427(8) 0.114(7) Uani 1 1 d U . . P2 P 1.3342(6) 1.1231(6) 0.3702(3) 0.062(2) Uani 1 1 d . . . F21 F 1.3710(11) 1.1384(11) 0.4304(6) 0.070(5) Uani 1 1 d U . . F22 F 1.2943(13) 1.1107(13) 0.3089(7) 0.091(6) Uani 1 1 d U . . F23 F 1.4373(12) 1.1232(12) 0.3583(6) 0.075(5) Uani 1 1 d U . . F24 F 1.3721(12) 1.2348(11) 0.3744(6) 0.079(5) Uani 1 1 d U . . F25 F 1.2300(12) 1.1200(13) 0.3832(7) 0.088(5) Uani 1 1 d U . . F26 F 1.2943(14) 1.0058(14) 0.3652(8) 0.103(6) Uani 1 1 d U . . P3 P 0.3536(6) 0.2538(6) 0.1533(3) 0.059(2) Uani 1 1 d . . . F311 F 0.4470(12) 0.2381(13) 0.1801(6) 0.085(5) Uani 1 1 d U . . F312 F 0.2625(13) 0.2666(13) 0.1244(7) 0.094(6) Uani 1 1 d U . . F313 F 0.3064(13) 0.1438(13) 0.1297(7) 0.099(6) Uani 1 1 d U . . F314 F 0.3052(12) 0.2397(12) 0.2042(6) 0.079(5) Uani 1 1 d U . . F315 F 0.4064(14) 0.3615(13) 0.1745(7) 0.099(6) Uani 1 1 d U . . F316 F 0.4073(12) 0.2677(12) 0.1022(6) 0.080(5) Uani 1 1 d U . . P4 P 0.9321(7) 0.7016(6) 0.1517(3) 0.066(2) Uani 1 1 d . . . F41 F 0.9172(11) 0.5922(10) 0.1517(6) 0.065(4) Uani 1 1 d U . . F42 F 0.9495(14) 0.8097(14) 0.1555(8) 0.102(6) Uani 1 1 d U . . F43 F 0.8997(12) 0.6786(12) 0.0901(6) 0.076(5) Uani 1 1 d U . . F44 F 1.0413(12) 0.7282(11) 0.1435(6) 0.078(5) Uani 1 1 d U . . F45 F 0.9719(15) 0.7218(14) 0.2146(8) 0.110(7) Uani 1 1 d U . . F46 F 0.8234(13) 0.6729(13) 0.1598(7) 0.091(6) Uani 1 1 d U . . O120 O 0.1209(13) 0.2711(13) 0.4229(7) 0.059(4) Uani 1 1 d U . . C120 C 0.160(2) 0.2595(19) 0.4627(11) 0.056(5) Uani 1 1 d U . . C121 C 0.092(2) 0.200(2) 0.4936(11) 0.066(6) Uani 1 1 d U . . H12A H 0.0242 0.1822 0.4766 0.099 Uiso 1 1 calc R . . H12B H 0.1031 0.2364 0.5284 0.099 Uiso 1 1 calc R . . H12C H 0.1047 0.1419 0.4963 0.099 Uiso 1 1 calc R . . C122 C 0.2656(19) 0.306(2) 0.4829(11) 0.063(6) Uani 1 1 d U . . H12D H 0.2977 0.3492 0.4600 0.095 Uiso 1 1 calc R . . H12E H 0.2931 0.2569 0.4846 0.095 Uiso 1 1 calc R . . H12F H 0.2766 0.3423 0.5177 0.095 Uiso 1 1 calc R . . O130 O 0.7473(15) 0.8996(15) 0.0842(9) 0.085(6) Uani 1 1 d U . . C130 C 0.753(2) 0.849(2) 0.0419(13) 0.074(6) Uani 1 1 d U . . C131 C 0.714(2) 0.750(2) 0.0339(13) 0.082(7) Uani 1 1 d U . . H13B H 0.6886 0.7280 0.0647 0.123 Uiso 1 1 calc R . . H13C H 0.7652 0.7270 0.0275 0.123 Uiso 1 1 calc R . . H13D H 0.6603 0.7252 0.0039 0.123 Uiso 1 1 calc R . . C132 C 0.798(2) 0.900(2) 0.0069(13) 0.082(7) Uani 1 1 d U . . H13E H 0.8563 0.9553 0.0250 0.123 Uiso 1 1 calc R . . H13F H 0.7523 0.9222 -0.0125 0.123 Uiso 1 1 calc R . . H13G H 0.8170 0.8594 -0.0172 0.123 Uiso 1 1 calc R . . O140 O 0.6873(17) 0.3916(17) 0.4362(9) 0.096(6) Uani 1 1 d U . . C140 C 0.620(3) 0.389(3) 0.4508(14) 0.084(6) Uani 1 1 d U . . C141 C 0.579(2) 0.337(2) 0.4873(13) 0.090(7) Uani 1 1 d U . . H14A H 0.6180 0.3012 0.4983 0.135 Uiso 1 1 calc R . . H14B H 0.5116 0.2930 0.4725 0.135 Uiso 1 1 calc R . . H14C H 0.5787 0.3813 0.5172 0.135 Uiso 1 1 calc R . . C142 C 0.571(2) 0.456(2) 0.4368(13) 0.088(7) Uani 1 1 d U . . H14D H 0.6090 0.4990 0.4156 0.132 Uiso 1 1 calc R . . H14E H 0.5669 0.4930 0.4686 0.132 Uiso 1 1 calc R . . H14F H 0.5041 0.4181 0.4172 0.132 Uiso 1 1 calc R . . O150 O 0.9373(14) 0.9390(14) 0.3405(8) 0.072(5) Uani 1 1 d U . . C150 C 1.003(2) 0.915(2) 0.3544(12) 0.066(5) Uani 1 1 d U . . C151 C 1.058(2) 0.889(2) 0.3121(11) 0.069(6) Uani 1 1 d U . . H15A H 1.0370 0.9060 0.2793 0.103 Uiso 1 1 calc R . . H15B H 1.0421 0.8198 0.3071 0.103 Uiso 1 1 calc R . . H15C H 1.1288 0.9238 0.3234 0.103 Uiso 1 1 calc R . . C152 C 1.031(2) 0.914(2) 0.4084(11) 0.072(6) Uani 1 1 d U . . H15D H 0.9727 0.8862 0.4237 0.108 Uiso 1 1 calc R . . H15E H 1.0700 0.9799 0.4266 0.108 Uiso 1 1 calc R . . H15F H 1.0713 0.8761 0.4117 0.108 Uiso 1 1 calc R . . O160 O 0.2727(15) 0.4294(14) 0.2615(8) 0.076(5) Uani 1 1 d U . . C160 C 0.322(2) 0.437(2) 0.3036(13) 0.069(6) Uani 1 1 d U . . C161 C 0.426(2) 0.445(2) 0.3046(12) 0.077(6) Uani 1 1 d U . . H16B H 0.4433 0.4542 0.2705 0.116 Uiso 1 1 calc R . . H16C H 0.4312 0.3863 0.3133 0.116 Uiso 1 1 calc R . . H16D H 0.4701 0.4998 0.3308 0.116 Uiso 1 1 calc R . . C162 C 0.282(2) 0.421(2) 0.3507(12) 0.078(7) Uani 1 1 d U . . H16E H 0.2123 0.4113 0.3438 0.117 Uiso 1 1 calc R . . H16F H 0.3177 0.4776 0.3778 0.117 Uiso 1 1 calc R . . H16G H 0.2880 0.3648 0.3623 0.117 Uiso 1 1 calc R . . O170 O 0.0817(13) 0.0684(14) 0.1565(7) 0.067(5) Uani 1 1 d U . . C170 C 0.109(2) 0.003(2) 0.1421(12) 0.066(5) Uani 1 1 d U . . C171 C 0.081(2) -0.047(2) 0.0882(11) 0.068(6) Uani 1 1 d U . . H17A H 0.0537 -0.0115 0.0667 0.102 Uiso 1 1 calc R . . H17B H 0.0324 -0.1117 0.0861 0.102 Uiso 1 1 calc R . . H17C H 0.1396 -0.0500 0.0758 0.102 Uiso 1 1 calc R . . C172 C 0.180(2) -0.024(2) 0.1773(12) 0.080(7) Uani 1 1 d U . . H17D H 0.2064 0.0226 0.2095 0.120 Uiso 1 1 calc R . . H17E H 0.2337 -0.0254 0.1598 0.120 Uiso 1 1 calc R . . H17F H 0.1446 -0.0880 0.1855 0.120 Uiso 1 1 calc R . . O180 O 0.6595(15) 0.3283(16) 0.0508(8) 0.082(5) Uani 1 1 d U . . C180 C 0.650(2) 0.396(2) 0.0378(12) 0.075(6) Uani 1 1 d U . . C181 C 0.730(2) 0.490(2) 0.0495(13) 0.082(7) Uani 1 1 d U . . H18A H 0.7680 0.4990 0.0841 0.123 Uiso 1 1 calc R . . H18B H 0.7025 0.5396 0.0488 0.123 Uiso 1 1 calc R . . H18C H 0.7726 0.4963 0.0237 0.123 Uiso 1 1 calc R . . C182 C 0.552(2) 0.392(2) 0.0109(13) 0.088(7) Uani 1 1 d U . . H18D H 0.5021 0.3277 0.0079 0.132 Uiso 1 1 calc R . . H18E H 0.5585 0.4086 -0.0238 0.132 Uiso 1 1 calc R . . H18F H 0.5336 0.4384 0.0312 0.132 Uiso 1 1 calc R . . O190 O 0.588(2) 0.764(2) 0.2030(11) 0.116(7) Uani 1 1 d U . . C190 C 0.544(3) 0.684(3) 0.2009(17) 0.117(8) Uani 1 1 d U . . C191 C 0.469(3) 0.630(3) 0.2256(16) 0.129(9) Uani 1 1 d U . . H19B H 0.4419 0.6722 0.2430 0.194 Uiso 1 1 calc R . . H19C H 0.4953 0.6001 0.2512 0.194 Uiso 1 1 calc R . . H19D H 0.4167 0.5802 0.1997 0.194 Uiso 1 1 calc R . . C192 C 0.568(3) 0.606(3) 0.1636(16) 0.126(9) Uani 1 1 d U . . H19E H 0.6357 0.6348 0.1581 0.189 Uiso 1 1 calc R . . H19F H 0.5229 0.5872 0.1302 0.189 Uiso 1 1 calc R . . H19G H 0.5586 0.5499 0.1800 0.189 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.051(2) 0.056(2) 0.0178(16) 0.0213(14) 0.0177(14) 0.0463(17) Cu2 0.050(2) 0.057(2) 0.0188(16) 0.0192(14) 0.0167(14) 0.0488(17) Cu3 0.050(2) 0.057(2) 0.0181(16) 0.0208(14) 0.0169(13) 0.0447(16) Cu4 0.052(2) 0.057(2) 0.0203(17) 0.0220(14) 0.0188(14) 0.0460(17) N1 0.033(6) 0.037(5) 0.024(5) 0.007(4) 0.008(4) 0.020(4) N2 0.034(6) 0.038(6) 0.025(5) 0.007(4) 0.007(4) 0.022(4) C2 0.035(5) 0.040(5) 0.030(5) 0.009(4) 0.008(4) 0.022(4) C3 0.036(6) 0.040(6) 0.032(6) 0.009(5) 0.009(5) 0.022(5) C4 0.037(6) 0.039(6) 0.031(6) 0.008(5) 0.007(5) 0.022(5) C5 0.036(5) 0.036(5) 0.026(5) 0.007(4) 0.010(4) 0.019(4) C6 0.035(6) 0.032(6) 0.026(6) 0.010(5) 0.009(5) 0.017(5) N3 0.037(6) 0.033(6) 0.027(5) 0.004(5) 0.011(4) 0.017(5) C8 0.041(5) 0.040(5) 0.032(5) 0.008(4) 0.013(4) 0.018(4) C9 0.046(6) 0.041(5) 0.036(6) 0.011(5) 0.014(5) 0.023(5) C10 0.049(6) 0.046(5) 0.044(6) 0.015(5) 0.016(5) 0.022(5) C11 0.047(6) 0.049(5) 0.037(6) 0.014(5) 0.015(5) 0.020(5) C12 0.042(6) 0.047(5) 0.034(6) 0.011(5) 0.014(5) 0.023(5) C13 0.040(6) 0.042(6) 0.032(6) 0.010(5) 0.013(5) 0.023(5) F1 0.079(7) 0.061(6) 0.063(7) 0.035(5) 0.028(6) 0.034(6) F2 0.055(6) 0.061(6) 0.032(6) 0.009(5) 0.023(5) 0.031(5) C16 0.034(6) 0.037(6) 0.031(6) 0.008(5) 0.009(5) 0.022(5) N4 0.028(6) 0.037(6) 0.028(5) 0.008(4) 0.008(4) 0.021(5) C18 0.030(5) 0.040(5) 0.028(5) 0.009(4) 0.008(4) 0.021(4) C19 0.033(5) 0.041(6) 0.029(6) 0.011(5) 0.010(5) 0.023(5) C20 0.042(5) 0.047(6) 0.031(6) 0.013(5) 0.013(5) 0.022(5) C21 0.045(5) 0.044(6) 0.031(6) 0.014(5) 0.010(5) 0.018(5) C22 0.042(5) 0.041(6) 0.035(6) 0.014(5) 0.005(5) 0.022(5) C23 0.033(6) 0.043(6) 0.032(6) 0.010(5) 0.006(5) 0.022(5) F3 0.055(6) 0.063(7) 0.045(6) 0.021(5) 0.009(5) 0.034(5) F4 0.059(6) 0.069(7) 0.045(6) 0.023(5) 0.030(5) 0.036(5) N31 0.031(5) 0.040(6) 0.023(5) 0.009(4) 0.003(4) 0.018(4) N32 0.029(5) 0.038(6) 0.023(5) 0.009(4) 0.005(4) 0.018(4) C32 0.031(5) 0.040(5) 0.026(5) 0.008(4) 0.005(4) 0.020(4) C33 0.033(6) 0.040(6) 0.027(6) 0.009(5) 0.009(5) 0.021(5) C34 0.036(6) 0.042(6) 0.027(6) 0.009(5) 0.008(5) 0.020(5) C35 0.032(5) 0.040(5) 0.023(5) 0.010(4) 0.007(4) 0.018(4) C36 0.034(6) 0.038(6) 0.024(6) 0.009(5) 0.010(5) 0.023(5) N33 0.033(5) 0.039(6) 0.027(5) 0.005(5) 0.011(4) 0.021(5) C38 0.029(5) 0.039(5) 0.028(5) 0.005(4) 0.012(4) 0.021(4) C39 0.033(6) 0.041(5) 0.030(6) 0.006(5) 0.011(5) 0.022(5) C40 0.040(6) 0.045(5) 0.033(6) 0.011(5) 0.011(5) 0.022(5) C41 0.038(6) 0.046(5) 0.032(6) 0.006(5) 0.015(5) 0.016(5) C42 0.037(6) 0.047(5) 0.029(6) 0.005(5) 0.017(5) 0.021(5) C43 0.038(6) 0.042(6) 0.030(6) 0.004(5) 0.016(5) 0.023(5) F31 0.060(7) 0.057(6) 0.051(7) 0.021(5) 0.020(5) 0.033(5) F32 0.046(6) 0.061(6) 0.049(6) 0.010(5) 0.025(5) 0.033(5) C46 0.032(6) 0.041(6) 0.029(6) 0.010(5) 0.007(5) 0.019(5) N34 0.038(6) 0.041(6) 0.030(6) 0.012(4) 0.007(5) 0.019(5) C48 0.043(5) 0.045(5) 0.033(5) 0.013(4) 0.010(4) 0.018(5) C49 0.044(5) 0.047(6) 0.035(6) 0.016(5) 0.010(5) 0.019(5) C50 0.045(5) 0.048(6) 0.039(6) 0.018(5) 0.013(5) 0.022(5) C51 0.048(5) 0.045(6) 0.040(6) 0.018(5) 0.010(5) 0.021(5) C52 0.047(5) 0.047(6) 0.038(6) 0.016(5) 0.008(5) 0.020(5) C53 0.048(6) 0.046(6) 0.035(6) 0.014(5) 0.007(5) 0.016(5) F33 0.052(6) 0.074(7) 0.051(7) 0.031(6) 0.023(5) 0.031(5) F34 0.054(6) 0.057(6) 0.044(6) 0.019(5) 0.010(5) 0.032(5) N61 0.035(5) 0.037(5) 0.033(6) 0.014(5) 0.004(5) 0.022(4) N62 0.032(5) 0.039(5) 0.028(6) 0.009(5) 0.011(5) 0.020(4) C62 0.038(5) 0.039(5) 0.036(6) 0.010(5) 0.006(5) 0.020(4) C63 0.038(5) 0.042(5) 0.038(6) 0.005(5) 0.008(5) 0.023(5) C64 0.034(5) 0.041(5) 0.038(6) 0.009(5) 0.002(5) 0.024(5) C65 0.034(5) 0.040(5) 0.033(6) 0.010(5) 0.004(5) 0.026(4) C66 0.034(6) 0.042(5) 0.034(6) 0.015(5) 0.004(5) 0.026(5) N63 0.041(6) 0.042(5) 0.035(6) 0.014(5) 0.005(5) 0.029(4) C68 0.051(5) 0.049(5) 0.048(6) 0.012(5) 0.005(5) 0.025(4) C69 0.055(6) 0.054(6) 0.055(6) 0.012(5) 0.008(5) 0.023(5) C70 0.059(6) 0.058(6) 0.059(6) 0.013(5) 0.011(5) 0.022(5) C71 0.062(6) 0.057(6) 0.058(6) 0.012(5) 0.010(5) 0.022(5) C72 0.065(6) 0.060(6) 0.057(6) 0.007(5) 0.013(5) 0.022(5) C73 0.059(6) 0.060(6) 0.054(6) 0.007(5) 0.011(5) 0.021(5) F61 0.068(7) 0.078(7) 0.073(7) 0.014(6) 0.028(6) 0.025(5) F62 0.084(8) 0.076(7) 0.069(7) 0.002(5) 0.019(6) 0.029(6) C76 0.042(5) 0.036(6) 0.037(6) 0.010(5) 0.007(5) 0.018(5) N64 0.041(5) 0.039(6) 0.039(6) 0.014(5) 0.011(5) 0.022(5) C78 0.048(5) 0.045(5) 0.046(6) 0.012(5) 0.005(5) 0.022(5) C79 0.051(6) 0.050(6) 0.051(6) 0.008(5) 0.006(5) 0.021(5) C80 0.053(6) 0.054(6) 0.052(6) 0.007(5) 0.005(5) 0.023(5) C81 0.052(6) 0.057(6) 0.054(7) 0.007(5) 0.004(5) 0.022(5) C82 0.051(5) 0.060(6) 0.056(6) 0.006(5) 0.004(5) 0.024(5) C83 0.049(5) 0.054(6) 0.052(6) 0.007(5) 0.005(5) 0.021(5) F63 0.068(7) 0.065(7) 0.061(7) 0.002(5) 0.007(6) 0.028(5) F64 0.055(6) 0.084(8) 0.076(8) -0.005(6) 0.003(6) 0.032(6) N91 0.035(5) 0.040(5) 0.033(6) 0.007(5) 0.010(5) 0.020(4) N92 0.038(5) 0.039(5) 0.028(6) 0.007(5) 0.010(5) 0.019(4) C92 0.040(5) 0.038(5) 0.029(6) 0.009(5) 0.014(5) 0.020(4) C93 0.041(6) 0.039(6) 0.035(6) 0.006(5) 0.012(5) 0.021(5) C94 0.039(6) 0.039(5) 0.038(6) 0.012(5) 0.008(5) 0.021(5) C95 0.036(5) 0.039(5) 0.035(6) 0.011(5) 0.010(5) 0.021(4) C96 0.036(6) 0.042(5) 0.040(6) 0.012(5) 0.006(5) 0.022(5) N93 0.036(5) 0.043(5) 0.040(6) 0.012(5) 0.011(5) 0.026(4) C98 0.042(5) 0.046(5) 0.042(6) 0.011(5) 0.007(5) 0.024(4) C99 0.046(5) 0.048(6) 0.047(7) 0.009(5) 0.002(5) 0.024(5) C100 0.049(5) 0.053(6) 0.048(6) 0.007(5) 0.004(5) 0.020(5) C101 0.055(5) 0.052(6) 0.054(7) 0.006(5) 0.005(6) 0.021(5) C102 0.057(6) 0.059(6) 0.058(7) 0.000(5) 0.010(6) 0.022(5) C103 0.049(6) 0.056(6) 0.052(7) 0.003(5) 0.008(5) 0.023(5) F91 0.054(6) 0.069(7) 0.072(7) 0.005(6) 0.002(6) 0.025(5) F92 0.080(7) 0.082(7) 0.095(8) -0.014(6) 0.015(6) 0.038(6) C106 0.043(5) 0.036(6) 0.033(6) 0.009(5) 0.013(5) 0.026(5) N94 0.050(5) 0.040(6) 0.041(6) 0.015(5) 0.009(5) 0.032(5) C108 0.058(5) 0.054(6) 0.052(6) 0.013(5) 0.007(5) 0.024(5) C109 0.065(6) 0.058(6) 0.055(6) 0.012(5) 0.009(5) 0.023(5) C110 0.069(6) 0.066(6) 0.062(6) 0.009(5) 0.010(5) 0.022(5) C111 0.066(6) 0.069(7) 0.065(7) 0.010(5) 0.007(6) 0.023(5) C112 0.063(5) 0.069(7) 0.066(7) 0.010(5) 0.006(5) 0.021(5) C113 0.060(5) 0.062(6) 0.060(7) 0.012(5) 0.006(5) 0.021(5) F93 0.084(7) 0.077(7) 0.071(7) 0.002(5) 0.015(6) 0.033(6) F94 0.074(6) 0.098(8) 0.085(8) 0.007(6) 0.010(6) 0.034(6) P1 0.051(5) 0.064(5) 0.041(4) 0.020(4) 0.020(4) 0.041(4) F11 0.085(8) 0.063(8) 0.068(8) 0.013(6) 0.011(6) 0.041(6) F12 0.076(8) 0.066(7) 0.045(7) 0.005(6) 0.026(6) 0.031(6) F13 0.141(10) 0.108(10) 0.093(10) 0.024(8) 0.017(8) 0.052(8) F14 0.125(11) 0.128(11) 0.148(11) 0.008(8) 0.029(8) 0.054(8) F15 0.128(10) 0.105(9) 0.097(10) 0.028(8) 0.010(8) 0.057(8) F16 0.104(10) 0.114(10) 0.124(10) 0.021(8) 0.032(8) 0.037(8) P2 0.064(6) 0.082(6) 0.055(5) 0.029(4) 0.017(4) 0.038(5) F21 0.075(8) 0.082(8) 0.068(8) 0.025(7) 0.014(6) 0.043(6) F22 0.090(9) 0.111(9) 0.080(9) 0.015(7) 0.007(7) 0.051(7) F23 0.079(8) 0.095(8) 0.067(8) 0.037(7) 0.030(7) 0.038(7) F24 0.088(8) 0.076(8) 0.077(8) 0.023(7) 0.010(7) 0.035(7) F25 0.086(9) 0.101(9) 0.086(9) 0.015(7) 0.012(7) 0.051(7) F26 0.100(9) 0.099(9) 0.106(10) 0.014(7) 0.021(8) 0.035(7) P3 0.072(6) 0.078(6) 0.050(5) 0.016(4) 0.016(4) 0.051(5) F311 0.084(8) 0.104(9) 0.069(8) 0.040(7) 0.000(7) 0.035(7) F312 0.093(9) 0.109(9) 0.100(9) 0.020(7) 0.011(7) 0.065(7) F313 0.098(9) 0.095(9) 0.103(10) 0.005(7) 0.010(7) 0.045(7) F314 0.078(8) 0.087(8) 0.071(8) 0.020(7) 0.023(7) 0.025(7) F315 0.106(9) 0.094(9) 0.089(9) 0.016(7) 0.036(7) 0.025(7) F316 0.085(8) 0.094(9) 0.074(8) 0.024(7) 0.012(7) 0.049(7) P4 0.105(7) 0.062(5) 0.059(6) 0.028(4) 0.045(5) 0.049(5) F41 0.077(8) 0.070(8) 0.061(8) 0.016(6) 0.025(6) 0.039(6) F42 0.102(9) 0.100(9) 0.119(10) 0.013(7) 0.035(8) 0.052(7) F43 0.082(8) 0.088(8) 0.077(9) 0.035(7) 0.012(7) 0.048(7) F44 0.088(8) 0.076(8) 0.072(8) 0.024(7) 0.029(7) 0.029(7) F45 0.123(10) 0.107(10) 0.094(10) 0.018(8) 0.022(8) 0.038(8) F46 0.092(9) 0.095(9) 0.100(9) 0.025(7) 0.041(7) 0.044(7) O120 0.061(7) 0.068(8) 0.056(7) 0.011(6) 0.012(6) 0.035(6) C120 0.059(7) 0.061(8) 0.054(8) 0.013(6) 0.010(6) 0.030(6) C121 0.070(9) 0.069(9) 0.058(9) 0.015(7) 0.013(7) 0.025(7) C122 0.064(7) 0.065(9) 0.059(9) 0.012(8) 0.007(6) 0.025(7) O130 0.091(9) 0.095(8) 0.080(8) 0.010(6) 0.015(7) 0.049(7) C130 0.077(9) 0.078(8) 0.076(8) 0.013(6) 0.015(7) 0.041(7) C131 0.081(10) 0.083(8) 0.084(10) 0.012(7) 0.019(8) 0.032(7) C132 0.086(10) 0.083(10) 0.083(9) 0.017(7) 0.018(8) 0.040(7) O140 0.087(8) 0.110(9) 0.087(9) 0.008(7) 0.024(7) 0.034(7) C140 0.078(8) 0.092(9) 0.082(9) 0.014(7) 0.019(7) 0.033(6) C141 0.086(10) 0.095(10) 0.087(10) 0.024(7) 0.014(7) 0.031(7) C142 0.090(10) 0.086(10) 0.087(11) 0.020(8) 0.016(8) 0.030(7) O150 0.069(8) 0.078(8) 0.071(8) 0.008(7) 0.016(6) 0.032(6) C150 0.069(8) 0.070(8) 0.064(8) 0.009(7) 0.015(6) 0.033(6) C151 0.070(9) 0.071(10) 0.068(9) 0.005(7) 0.014(7) 0.033(7) C152 0.078(10) 0.075(10) 0.071(8) 0.009(8) 0.016(7) 0.038(8) O160 0.078(8) 0.080(8) 0.072(7) 0.014(7) 0.007(6) 0.033(7) C160 0.071(8) 0.074(8) 0.069(8) 0.015(7) 0.012(6) 0.035(7) C161 0.071(8) 0.083(10) 0.076(10) 0.016(8) 0.011(7) 0.029(8) C162 0.079(9) 0.086(10) 0.073(8) 0.019(8) 0.015(7) 0.034(8) O170 0.070(8) 0.069(8) 0.061(8) 0.015(6) 0.009(6) 0.027(6) C170 0.067(8) 0.069(8) 0.062(8) 0.015(6) 0.013(6) 0.026(6) C171 0.066(9) 0.075(9) 0.065(8) 0.013(7) 0.016(7) 0.029(7) C172 0.085(10) 0.078(10) 0.077(9) 0.022(8) 0.006(7) 0.033(7) O180 0.091(9) 0.083(8) 0.074(9) 0.022(7) 0.012(7) 0.035(7) C180 0.077(8) 0.077(8) 0.072(9) 0.016(7) 0.014(7) 0.031(6) C181 0.084(9) 0.080(8) 0.084(10) 0.016(8) 0.012(8) 0.033(7) C182 0.085(9) 0.090(10) 0.089(11) 0.021(8) 0.010(7) 0.034(7) O190 0.117(10) 0.114(9) 0.121(10) 0.021(7) 0.009(8) 0.053(7) C190 0.116(10) 0.118(10) 0.121(10) 0.023(7) 0.017(7) 0.051(7) C191 0.130(11) 0.131(12) 0.127(12) 0.027(8) 0.024(8) 0.049(7) C192 0.125(12) 0.124(11) 0.130(12) 0.015(8) 0.016(8) 0.055(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.988(18) . y Cu1 N1 1.989(17) . y Cu1 N61 1.990(18) . y Cu1 N63 2.017(18) . y Cu2 N2 1.990(18) . y Cu2 N91 2.025(18) . y Cu2 N93 2.053(18) . y Cu2 N4 2.064(16) . y Cu3 N62 1.984(17) . y Cu3 N31 2.028(17) . y Cu3 N33 2.041(18) . y Cu3 N64 2.046(18) . y Cu4 N32 1.961(17) . y Cu4 N92 1.976(18) . y Cu4 N94 2.026(18) . y Cu4 N34 2.027(18) . y N1 C5 1.33(3) . ? N1 N2 1.35(2) . ? N2 C2 1.36(3) . ? C2 C3 1.37(3) . ? C2 C16 1.50(3) . ? C3 C4 1.41(3) . ? C3 H3A 0.9500 . ? C4 C5 1.33(3) . ? C4 H4A 0.9500 . ? C5 C6 1.50(3) . ? C6 N3 1.34(3) . ? C6 H6A 0.9500 . ? N3 C8 1.44(3) . ? C8 C13 1.38(3) . ? C8 C9 1.44(3) . ? C9 C10 1.33(3) . ? C9 H9A 0.9500 . ? C10 F1 1.32(3) . ? C10 C11 1.42(3) . ? C11 C12 1.36(3) . ? C11 H11A 0.9500 . ? C12 F2 1.29(2) . ? C12 C13 1.43(3) . ? C13 H13A 0.9500 . ? C16 N4 1.27(3) . ? C16 H16A 0.9500 . ? N4 C18 1.47(3) . ? C18 C19 1.29(3) . ? C18 C23 1.41(3) . ? C19 C20 1.34(3) . ? C19 H19A 0.9500 . ? C20 F4 1.36(2) . ? C20 C21 1.43(3) . ? C21 C22 1.32(3) . ? C21 H21A 0.9500 . ? C22 C23 1.37(3) . ? C22 F3 1.38(3) . ? C23 H23A 0.9500 . ? N31 C35 1.34(3) . ? N31 N32 1.36(2) . ? N32 C32 1.33(3) . ? C32 C46 1.42(3) . ? C32 C33 1.44(3) . ? C33 C34 1.39(3) . ? C33 H33A 0.9500 . ? C34 C35 1.35(3) . ? C34 H34A 0.9500 . ? C35 C36 1.50(3) . ? C36 N33 1.26(2) . ? C36 H36A 0.9500 . ? N33 C38 1.43(3) . ? C38 C43 1.36(3) . ? C38 C39 1.38(3) . ? C39 C40 1.40(3) . ? C39 H39A 0.9500 . ? C40 C41 1.31(3) . ? C40 F31 1.36(3) . ? C41 C42 1.30(3) . ? C41 H41A 0.9500 . ? C42 F32 1.34(2) . ? C42 C43 1.45(3) . ? C43 H43A 0.9500 . ? C46 N34 1.31(3) . ? C46 H46A 0.9500 . ? N34 C48 1.43(3) . ? C48 C53 1.39(3) . ? C48 C49 1.40(3) . ? C49 C50 1.34(3) . ? C49 H49A 0.9500 . ? C50 F33 1.39(3) . ? C50 C51 1.42(3) . ? C51 C52 1.37(3) . ? C51 H51A 0.9500 . ? C52 C53 1.28(3) . ? C52 F34 1.38(3) . ? C53 H53A 0.9500 . ? N61 C65 1.32(3) . ? N61 N62 1.32(2) . ? N62 C62 1.37(3) . ? C62 C63 1.39(3) . ? C62 C76 1.48(3) . ? C63 C64 1.35(3) . ? C63 H63A 0.9500 . ? C64 C65 1.37(3) . ? C64 H64A 0.9500 . ? C65 C66 1.51(3) . ? C66 N63 1.25(3) . ? C66 H66A 0.9500 . ? N63 C68 1.43(3) . ? C68 C73 1.35(3) . ? C68 C69 1.42(3) . ? C69 C70 1.37(3) . ? C69 H69A 0.9500 . ? C70 C71 1.34(4) . ? C70 F61 1.37(3) . ? C71 C72 1.40(4) . ? C71 H71A 0.9500 . ? C72 F62 1.33(3) . ? C72 C73 1.38(3) . ? C73 H73A 0.9500 . ? C76 N64 1.36(3) . ? C76 H76 0.9500 . ? N64 C78 1.38(3) . ? C78 C79 1.36(3) . ? C78 C83 1.44(3) . ? C79 C80 1.30(3) . ? C79 H79A 0.9500 . ? C80 F63 1.34(3) . ? C80 C81 1.43(4) . ? C81 C82 1.39(3) . ? C81 H81 0.9500 . ? C82 F64 1.28(3) . ? C82 C83 1.32(3) . ? C83 H83A 0.9500 . ? N91 N92 1.33(2) . ? N91 C95 1.35(3) . ? N92 C92 1.32(3) . ? C92 C93 1.38(3) . ? C92 C106 1.44(3) . ? C93 C94 1.33(3) . ? C93 H93A 0.9500 . ? C94 C95 1.41(3) . ? C94 H94A 0.9500 . ? C95 C96 1.47(3) . ? C96 N93 1.30(3) . ? C96 H96A 0.9500 . ? N93 C98 1.37(3) . ? C98 C103 1.38(3) . ? C98 C99 1.39(3) . ? C99 C100 1.31(3) . ? C99 H99A 0.9500 . ? C100 F91 1.36(3) . ? C100 C101 1.41(3) . ? C101 C102 1.34(3) . ? C101 H10A 0.9500 . ? C102 C103 1.35(3) . ? C102 F92 1.42(3) . ? C103 H10B 0.9500 . ? C106 N94 1.27(3) . ? C106 H10C 0.9500 . ? N94 C108 1.40(3) . ? C108 C113 1.30(3) . ? C108 C109 1.48(4) . ? C109 C110 1.35(3) . ? C109 H10D 0.9500 . ? C110 F93 1.39(3) . ? C110 C111 1.44(4) . ? C111 C112 1.27(4) . ? C111 H11B 0.9500 . ? C112 C113 1.35(3) . ? C112 F94 1.39(3) . ? C113 H11C 0.9500 . ? P1 F16 1.51(2) . ? P1 F13 1.52(2) . ? P1 F14 1.55(2) . ? P1 F11 1.554(16) . ? P1 F15 1.61(2) . ? P1 F12 1.626(15) . ? P2 F24 1.571(18) . ? P2 F21 1.576(17) . ? P2 F23 1.608(17) . ? P2 F25 1.616(19) . ? P2 F22 1.617(19) . ? P2 F26 1.65(2) . ? P3 F315 1.536(19) . ? P3 F312 1.563(18) . ? P3 F313 1.576(19) . ? P3 F311 1.594(18) . ? P3 F314 1.600(17) . ? P3 F316 1.644(18) . ? P4 F46 1.563(18) . ? P4 F42 1.56(2) . ? P4 F44 1.573(18) . ? P4 F43 1.598(18) . ? P4 F41 1.602(16) . ? P4 F45 1.65(2) . ? O120 C120 1.20(3) . ? C120 C122 1.46(4) . ? C120 C121 1.48(4) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? O130 C130 1.31(3) . ? C130 C132 1.35(4) . ? C130 C131 1.38(4) . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C132 H13G 0.9800 . ? O140 C140 1.11(3) . ? C140 C141 1.37(4) . ? C140 C142 1.52(4) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C142 H14D 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? O150 C150 1.19(3) . ? C150 C152 1.44(4) . ? C150 C151 1.57(4) . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C152 H15D 0.9800 . ? C152 H15E 0.9800 . ? C152 H15F 0.9800 . ? O160 C160 1.23(3) . ? C160 C162 1.45(4) . ? C160 C161 1.49(4) . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? C161 H16D 0.9800 . ? C162 H16E 0.9800 . ? C162 H16F 0.9800 . ? C162 H16G 0.9800 . ? O170 C170 1.26(3) . ? C170 C171 1.46(4) . ? C170 C172 1.52(4) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? O180 C180 1.18(3) . ? C180 C181 1.45(4) . ? C180 C182 1.52(4) . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? O190 C190 1.14(4) . ? C190 C191 1.41(5) . ? C190 C192 1.62(5) . ? C191 H19B 0.9800 . ? C191 H19C 0.9800 . ? C191 H19D 0.9800 . ? C192 H19E 0.9800 . ? C192 H19F 0.9800 . ? C192 H19G 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N1 81.6(7) . . y N3 Cu1 N61 131.5(6) . . y N1 Cu1 N61 123.9(7) . . y N3 Cu1 N63 111.8(7) . . y N1 Cu1 N63 133.7(7) . . y N61 Cu1 N63 81.1(7) . . y N2 Cu2 N91 136.6(6) . . y N2 Cu2 N93 121.8(7) . . y N91 Cu2 N93 81.6(7) . . y N2 Cu2 N4 80.6(7) . . y N91 Cu2 N4 120.4(6) . . y N93 Cu2 N4 121.4(7) . . y N62 Cu3 N31 133.1(6) . . y N62 Cu3 N33 122.3(7) . . y N31 Cu3 N33 79.9(7) . . y N62 Cu3 N64 81.8(7) . . y N31 Cu3 N64 119.4(7) . . y N33 Cu3 N64 126.9(7) . . y N32 Cu4 N92 125.7(7) . . y N32 Cu4 N94 132.1(7) . . y N92 Cu4 N94 80.6(8) . . y N32 Cu4 N34 81.2(7) . . y N92 Cu4 N34 127.0(7) . . y N94 Cu4 N34 116.7(7) . . y C5 N1 N2 120.4(17) . . ? C5 N1 Cu1 115.0(14) . . ? N2 N1 Cu1 124.4(14) . . ? N1 N2 C2 115.9(18) . . ? N1 N2 Cu2 129.6(13) . . ? C2 N2 Cu2 114.2(14) . . ? N2 C2 C3 124(2) . . ? N2 C2 C16 114.5(19) . . ? C3 C2 C16 121(2) . . ? C2 C3 C4 118(2) . . ? C2 C3 H3A 121.1 . . ? C4 C3 H3A 121.1 . . ? C5 C4 C3 115(2) . . ? C5 C4 H4A 122.4 . . ? C3 C4 H4A 122.4 . . ? N1 C5 C4 126(2) . . ? N1 C5 C6 114.3(19) . . ? C4 C5 C6 119(2) . . ? N3 C6 C5 114(2) . . ? N3 C6 H6A 122.9 . . ? C5 C6 H6A 122.9 . . ? C6 N3 C8 117.2(18) . . ? C6 N3 Cu1 114.4(14) . . ? C8 N3 Cu1 128.1(14) . . ? C13 C8 N3 117(2) . . ? C13 C8 C9 119(2) . . ? N3 C8 C9 124(2) . . ? C10 C9 C8 118(2) . . ? C10 C9 H9A 121.1 . . ? C8 C9 H9A 121.1 . . ? F1 C10 C9 119(2) . . ? F1 C10 C11 117(2) . . ? C9 C10 C11 124(2) . . ? C12 C11 C10 119(2) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? F2 C12 C11 123(2) . . ? F2 C12 C13 118(2) . . ? C11 C12 C13 119(2) . . ? C8 C13 C12 121(2) . . ? C8 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? N4 C16 C2 116(2) . . ? N4 C16 H16A 122.0 . . ? C2 C16 H16A 122.0 . . ? C16 N4 C18 118.7(18) . . ? C16 N4 Cu2 114.3(15) . . ? C18 N4 Cu2 126.8(13) . . ? C19 C18 C23 121(2) . . ? C19 C18 N4 123(2) . . ? C23 C18 N4 116.0(19) . . ? C18 C19 C20 121(2) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C19 C20 F4 123(2) . . ? C19 C20 C21 121(2) . . ? F4 C20 C21 115.5(19) . . ? C22 C21 C20 116(2) . . ? C22 C21 H21A 122.2 . . ? C20 C21 H21A 122.2 . . ? C21 C22 C23 124(2) . . ? C21 C22 F3 118(2) . . ? C23 C22 F3 117(2) . . ? C22 C23 C18 117(2) . . ? C22 C23 H23A 121.7 . . ? C18 C23 H23A 121.7 . . ? C35 N31 N32 121.0(17) . . ? C35 N31 Cu3 114.3(14) . . ? N32 N31 Cu3 124.8(13) . . ? C32 N32 N31 119.2(18) . . ? C32 N32 Cu4 113.8(14) . . ? N31 N32 Cu4 126.9(13) . . ? N32 C32 C46 116(2) . . ? N32 C32 C33 122(2) . . ? C46 C32 C33 122(2) . . ? C34 C33 C32 117(2) . . ? C34 C33 H33A 121.7 . . ? C32 C33 H33A 121.7 . . ? C35 C34 C33 119(2) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? N31 C35 C34 123(2) . . ? N31 C35 C36 113.5(19) . . ? C34 C35 C36 124(2) . . ? N33 C36 C35 117(2) . . ? N33 C36 H36A 121.3 . . ? C35 C36 H36A 121.3 . . ? C36 N33 C38 118.0(19) . . ? C36 N33 Cu3 114.7(15) . . ? C38 N33 Cu3 127.2(13) . . ? C43 C38 C39 120(2) . . ? C43 C38 N33 117(2) . . ? C39 C38 N33 122.3(18) . . ? C38 C39 C40 118(2) . . ? C38 C39 H39A 121.1 . . ? C40 C39 H39A 121.1 . . ? C41 C40 F31 121(2) . . ? C41 C40 C39 122(2) . . ? F31 C40 C39 118(2) . . ? C42 C41 C40 122(2) . . ? C42 C41 H41A 119.0 . . ? C40 C41 H41A 119.0 . . ? C41 C42 F32 125(2) . . ? C41 C42 C43 120(2) . . ? F32 C42 C43 115(2) . . ? C38 C43 C42 118(2) . . ? C38 C43 H43A 121.0 . . ? C42 C43 H43A 121.0 . . ? N34 C46 C32 117(2) . . ? N34 C46 H46A 121.6 . . ? C32 C46 H46A 121.6 . . ? C46 N34 C48 121.9(19) . . ? C46 N34 Cu4 111.7(15) . . ? C48 N34 Cu4 126.1(15) . . ? C53 C48 C49 120(2) . . ? C53 C48 N34 118(2) . . ? C49 C48 N34 122(2) . . ? C50 C49 C48 117(2) . . ? C50 C49 H49A 121.6 . . ? C48 C49 H49A 121.6 . . ? C49 C50 F33 120(2) . . ? C49 C50 C51 125(2) . . ? F33 C50 C51 116(2) . . ? C52 C51 C50 113(2) . . ? C52 C51 H51A 123.7 . . ? C50 C51 H51A 123.7 . . ? C53 C52 C51 127(3) . . ? C53 C52 F34 120(2) . . ? C51 C52 F34 113(2) . . ? C52 C53 C48 119(3) . . ? C52 C53 H53A 120.7 . . ? C48 C53 H53A 120.7 . . ? C65 N61 N62 119.3(19) . . ? C65 N61 Cu1 115.1(15) . . ? N62 N61 Cu1 125.6(13) . . ? N61 N62 C62 117.6(18) . . ? N61 N62 Cu3 127.6(14) . . ? C62 N62 Cu3 114.4(14) . . ? N62 C62 C63 123(2) . . ? N62 C62 C76 116(2) . . ? C63 C62 C76 121(2) . . ? C64 C63 C62 118(2) . . ? C64 C63 H63A 121.1 . . ? C62 C63 H63A 121.1 . . ? C63 C64 C65 116(2) . . ? C63 C64 H64A 122.1 . . ? C65 C64 H64A 122.1 . . ? N61 C65 C64 126(2) . . ? N61 C65 C66 111.6(19) . . ? C64 C65 C66 122(2) . . ? N63 C66 C65 119(2) . . ? N63 C66 H66A 120.5 . . ? C65 C66 H66A 120.5 . . ? C66 N63 C68 119.9(19) . . ? C66 N63 Cu1 112.3(16) . . ? C68 N63 Cu1 125.1(13) . . ? C73 C68 C69 120(2) . . ? C73 C68 N63 121(2) . . ? C69 C68 N63 119(2) . . ? C70 C69 C68 115(3) . . ? C70 C69 H69A 122.3 . . ? C68 C69 H69A 122.3 . . ? C71 C70 C69 127(3) . . ? C71 C70 F61 115(2) . . ? C69 C70 F61 117(2) . . ? C70 C71 C72 115(3) . . ? C70 C71 H71A 122.4 . . ? C72 C71 H71A 122.4 . . ? F62 C72 C73 119(2) . . ? F62 C72 C71 120(2) . . ? C73 C72 C71 121(3) . . ? C68 C73 C72 121(3) . . ? C68 C73 H73A 119.4 . . ? C72 C73 H73A 119.4 . . ? N64 C76 C62 115(2) . . ? N64 C76 H76 122.5 . . ? C62 C76 H76 122.5 . . ? C76 N64 C78 118(2) . . ? C76 N64 Cu3 113.0(15) . . ? C78 N64 Cu3 129.5(15) . . ? C79 C78 N64 128(2) . . ? C79 C78 C83 112(2) . . ? N64 C78 C83 120(2) . . ? C80 C79 C78 125(3) . . ? C80 C79 H79A 117.4 . . ? C78 C79 H79A 117.4 . . ? C79 C80 F63 121(2) . . ? C79 C80 C81 121(3) . . ? F63 C80 C81 117(2) . . ? C82 C81 C80 117(3) . . ? C82 C81 H81 121.5 . . ? C80 C81 H81 121.5 . . ? F64 C82 C83 125(3) . . ? F64 C82 C81 117(2) . . ? C83 C82 C81 118(3) . . ? C82 C83 C78 126(3) . . ? C82 C83 H83A 117.0 . . ? C78 C83 H83A 117.0 . . ? N92 N91 C95 120.0(19) . . ? N92 N91 Cu2 126.8(14) . . ? C95 N91 Cu2 113.2(15) . . ? C92 N92 N91 119.3(19) . . ? C92 N92 Cu4 115.2(15) . . ? N91 N92 Cu4 125.1(14) . . ? N92 C92 C93 122(2) . . ? N92 C92 C106 112(2) . . ? C93 C92 C106 126(2) . . ? C94 C93 C92 121(2) . . ? C94 C93 H93A 119.5 . . ? C92 C93 H93A 119.5 . . ? C93 C94 C95 115(2) . . ? C93 C94 H94A 122.3 . . ? C95 C94 H94A 122.3 . . ? N91 C95 C94 122(2) . . ? N91 C95 C96 114(2) . . ? C94 C95 C96 123(2) . . ? N93 C96 C95 119(2) . . ? N93 C96 H96A 120.3 . . ? C95 C96 H96A 120.3 . . ? C96 N93 C98 119.3(19) . . ? C96 N93 Cu2 111.3(15) . . ? C98 N93 Cu2 129.0(15) . . ? N93 C98 C103 117(2) . . ? N93 C98 C99 126(2) . . ? C103 C98 C99 117(2) . . ? C100 C99 C98 121(3) . . ? C100 C99 H99A 119.6 . . ? C98 C99 H99A 119.6 . . ? C99 C100 F91 122(2) . . ? C99 C100 C101 123(3) . . ? F91 C100 C101 115(2) . . ? C102 C101 C100 114(2) . . ? C102 C101 H10A 123.2 . . ? C100 C101 H10A 123.2 . . ? C101 C102 C103 126(3) . . ? C101 C102 F92 116(2) . . ? C103 C102 F92 119(2) . . ? C102 C103 C98 119(3) . . ? C102 C103 H10B 120.5 . . ? C98 C103 H10B 120.5 . . ? N94 C106 C92 121(2) . . ? N94 C106 H10C 119.5 . . ? C92 C106 H10C 119.5 . . ? C106 N94 C108 124(2) . . ? C106 N94 Cu4 110.4(16) . . ? C108 N94 Cu4 125.8(15) . . ? C113 C108 N94 124(3) . . ? C113 C108 C109 116(3) . . ? N94 C108 C109 120(2) . . ? C110 C109 C108 113(3) . . ? C110 C109 H10D 123.3 . . ? C108 C109 H10D 123.3 . . ? C109 C110 F93 114(3) . . ? C109 C110 C111 128(3) . . ? F93 C110 C111 118(3) . . ? C112 C111 C110 112(3) . . ? C112 C111 H11B 123.9 . . ? C110 C111 H11B 123.9 . . ? C111 C112 C113 125(3) . . ? C111 C112 F94 114(3) . . ? C113 C112 F94 121(3) . . ? C108 C113 C112 125(3) . . ? C108 C113 H11C 117.3 . . ? C112 C113 H11C 117.3 . . ? F16 P1 F13 94.9(12) . . ? F16 P1 F14 175.8(13) . . ? F13 P1 F14 88.6(13) . . ? F16 P1 F11 91.4(11) . . ? F13 P1 F11 89.7(10) . . ? F14 P1 F11 90.9(11) . . ? F16 P1 F15 86.8(11) . . ? F13 P1 F15 178.2(12) . . ? F14 P1 F15 89.7(12) . . ? F11 P1 F15 89.9(10) . . ? F16 P1 F12 89.0(10) . . ? F13 P1 F12 92.1(10) . . ? F14 P1 F12 88.6(10) . . ? F11 P1 F12 178.2(10) . . ? F15 P1 F12 88.3(9) . . ? F24 P2 F21 88.6(9) . . ? F24 P2 F23 91.8(10) . . ? F21 P2 F23 91.4(9) . . ? F24 P2 F25 89.8(10) . . ? F21 P2 F25 87.6(9) . . ? F23 P2 F25 178.1(10) . . ? F24 P2 F22 89.7(10) . . ? F21 P2 F22 177.6(11) . . ? F23 P2 F22 90.4(9) . . ? F25 P2 F22 90.6(10) . . ? F24 P2 F26 179.4(11) . . ? F21 P2 F26 91.9(10) . . ? F23 P2 F26 88.0(10) . . ? F25 P2 F26 90.4(10) . . ? F22 P2 F26 89.7(11) . . ? F315 P3 F312 92.4(11) . . ? F315 P3 F313 175.7(11) . . ? F312 P3 F313 90.0(11) . . ? F315 P3 F311 89.3(11) . . ? F312 P3 F311 177.1(11) . . ? F313 P3 F311 88.2(10) . . ? F315 P3 F314 89.6(10) . . ? F312 P3 F314 90.8(10) . . ? F313 P3 F314 93.9(10) . . ? F311 P3 F314 91.5(10) . . ? F315 P3 F316 90.4(10) . . ? F312 P3 F316 91.6(10) . . ? F313 P3 F316 86.0(10) . . ? F311 P3 F316 86.1(9) . . ? F314 P3 F316 177.6(10) . . ? F46 P4 F42 92.4(11) . . ? F46 P4 F44 178.8(10) . . ? F42 P4 F44 88.8(10) . . ? F46 P4 F43 91.9(10) . . ? F42 P4 F43 93.9(10) . . ? F44 P4 F43 88.0(9) . . ? F46 P4 F41 87.9(9) . . ? F42 P4 F41 176.4(11) . . ? F44 P4 F41 90.9(9) . . ? F43 P4 F41 89.7(9) . . ? F46 P4 F45 91.5(11) . . ? F42 P4 F45 88.6(11) . . ? F44 P4 F45 88.5(11) . . ? F43 P4 F45 175.7(11) . . ? F41 P4 F45 87.8(10) . . ? O120 C120 C122 124(3) . . ? O120 C120 C121 115(3) . . ? C122 C120 C121 120(3) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C120 C122 H12D 109.5 . . ? C120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? O130 C130 C132 116(3) . . ? O130 C130 C131 122(3) . . ? C132 C130 C131 123(3) . . ? C130 C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C131 H13D 109.5 . . ? H13B C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C132 H13G 109.5 . . ? H13E C132 H13G 109.5 . . ? H13F C132 H13G 109.5 . . ? O140 C140 C141 126(4) . . ? O140 C140 C142 121(4) . . ? C141 C140 C142 112(3) . . ? C140 C141 H14A 109.5 . . ? C140 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C140 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C140 C142 H14D 109.5 . . ? C140 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C140 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? O150 C150 C152 121(3) . . ? O150 C150 C151 118(3) . . ? C152 C150 C151 121(3) . . ? C150 C151 H15A 109.5 . . ? C150 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C150 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C150 C152 H15D 109.5 . . ? C150 C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? C150 C152 H15F 109.5 . . ? H15D C152 H15F 109.5 . . ? H15E C152 H15F 109.5 . . ? O160 C160 C162 123(3) . . ? O160 C160 C161 118(3) . . ? C162 C160 C161 118(3) . . ? C160 C161 H16B 109.5 . . ? C160 C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C160 C161 H16D 109.5 . . ? H16B C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C160 C162 H16E 109.5 . . ? C160 C162 H16F 109.5 . . ? H16E C162 H16F 109.5 . . ? C160 C162 H16G 109.5 . . ? H16E C162 H16G 109.5 . . ? H16F C162 H16G 109.5 . . ? O170 C170 C171 121(3) . . ? O170 C170 C172 123(3) . . ? C171 C170 C172 116(3) . . ? C170 C171 H17A 109.5 . . ? C170 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C172 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? O180 C180 C181 122(3) . . ? O180 C180 C182 122(3) . . ? C181 C180 C182 115(3) . . ? C180 C181 H18A 109.5 . . ? C180 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C180 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C180 C182 H18D 109.5 . . ? C180 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C180 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? O190 C190 C191 134(5) . . ? O190 C190 C192 120(4) . . ? C191 C190 C192 106(4) . . ? C190 C191 H19B 109.5 . . ? C190 C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C190 C191 H19D 109.5 . . ? H19B C191 H19D 109.5 . . ? H19C C191 H19D 109.5 . . ? C190 C192 H19E 109.5 . . ? C190 C192 H19F 109.5 . . ? H19E C192 H19F 109.5 . . ? C190 C192 H19G 109.5 . . ? H19E C192 H19G 109.5 . . ? H19F C192 H19G 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C5 5.3(8) . . . . ? N61 Cu1 N1 C5 140.3(8) . . . . ? N63 Cu1 N1 C5 -107.0(10) . . . . ? N3 Cu1 N1 N2 -179.0(9) . . . . ? N61 Cu1 N1 N2 -43.9(11) . . . . ? N63 Cu1 N1 N2 68.7(12) . . . . ? C5 N1 N2 C2 0.01(15) . . . . ? Cu1 N1 N2 C2 -175.5(10) . . . . ? C5 N1 N2 Cu2 173.8(10) . . . . ? Cu1 N1 N2 Cu2 -1.7(12) . . . . ? N91 Cu2 N2 N1 57.2(13) . . . . ? N93 Cu2 N2 N1 -56.8(12) . . . . ? N4 Cu2 N2 N1 -178.0(10) . . . . ? N91 Cu2 N2 C2 -129.0(9) . . . . ? N93 Cu2 N2 C2 117.0(9) . . . . ? N4 Cu2 N2 C2 -4.1(8) . . . . ? N1 N2 C2 C3 0.01(15) . . . . ? Cu2 N2 C2 C3 -174.7(9) . . . . ? N1 N2 C2 C16 177.8(14) . . . . ? Cu2 N2 C2 C16 3.1(12) . . . . ? N2 C2 C3 C4 0.0(3) . . . . ? C16 C2 C3 C4 -177.7(15) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? N2 N1 C5 C4 0.0(4) . . . . ? Cu1 N1 C5 C4 175.9(9) . . . . ? N2 N1 C5 C6 180.0(14) . . . . ? Cu1 N1 C5 C6 -4.1(12) . . . . ? C3 C4 C5 N1 0.0(5) . . . . ? C3 C4 C5 C6 180.0(14) . . . . ? N1 C5 C6 N3 -1(2) . . . . ? C4 C5 C6 N3 179.5(13) . . . . ? C5 C6 N3 C8 180.0(15) . . . . ? C5 C6 N3 Cu1 5(2) . . . . ? N1 Cu1 N3 C6 -5.5(14) . . . . ? N61 Cu1 N3 C6 -134.1(14) . . . . ? N63 Cu1 N3 C6 128.4(15) . . . . ? N1 Cu1 N3 C8 -180.0(16) . . . . ? N61 Cu1 N3 C8 51.5(19) . . . . ? N63 Cu1 N3 C8 -46.1(17) . . . . ? C6 N3 C8 C13 158.3(14) . . . . ? Cu1 N3 C8 C13 -27.3(18) . . . . ? C6 N3 C8 C9 -18(2) . . . . ? Cu1 N3 C8 C9 156.8(9) . . . . ? C13 C8 C9 C10 -0.02(14) . . . . ? N3 C8 C9 C10 175.8(14) . . . . ? C8 C9 C10 F1 179.98(15) . . . . ? C8 C9 C10 C11 -0.03(14) . . . . ? F1 C10 C11 C12 -179.9(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? C10 C11 C12 F2 180.0(3) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? N3 C8 C13 C12 -176.1(13) . . . . ? C9 C8 C13 C12 0.0(3) . . . . ? F2 C12 C13 C8 180.0(3) . . . . ? C11 C12 C13 C8 0.0(4) . . . . ? N2 C2 C16 N4 1(2) . . . . ? C3 C2 C16 N4 178.9(14) . . . . ? C2 C16 N4 C18 -179.6(15) . . . . ? C2 C16 N4 Cu2 -4(2) . . . . ? N2 Cu2 N4 C16 4.8(15) . . . . ? N91 Cu2 N4 C16 144.0(15) . . . . ? N93 Cu2 N4 C16 -116.8(16) . . . . ? N2 Cu2 N4 C18 179.5(15) . . . . ? N91 Cu2 N4 C18 -41.4(17) . . . . ? N93 Cu2 N4 C18 57.8(17) . . . . ? C16 N4 C18 C19 -29(2) . . . . ? Cu2 N4 C18 C19 156.2(8) . . . . ? C16 N4 C18 C23 149.2(15) . . . . ? Cu2 N4 C18 C23 -25.2(16) . . . . ? C23 C18 C19 C20 -0.07(16) . . . . ? N4 C18 C19 C20 178.5(13) . . . . ? C18 C19 C20 F4 179.96(17) . . . . ? C18 C19 C20 C21 0.02(16) . . . . ? C19 C20 C21 C22 -0.1(3) . . . . ? F4 C20 C21 C22 -180.0(3) . . . . ? C20 C21 C22 C23 0.1(5) . . . . ? C20 C21 C22 F3 -179.9(3) . . . . ? C21 C22 C23 C18 -0.2(5) . . . . ? F3 C22 C23 C18 179.9(3) . . . . ? C19 C18 C23 C22 0.1(3) . . . . ? N4 C18 C23 C22 -178.5(12) . . . . ? N62 Cu3 N31 C35 -128.2(9) . . . . ? N33 Cu3 N31 C35 -2.9(7) . . . . ? N64 Cu3 N31 C35 124.0(8) . . . . ? N62 Cu3 N31 N32 52.5(12) . . . . ? N33 Cu3 N31 N32 177.8(9) . . . . ? N64 Cu3 N31 N32 -55.2(10) . . . . ? C35 N31 N32 C32 0.00(16) . . . . ? Cu3 N31 N32 C32 179.2(9) . . . . ? C35 N31 N32 Cu4 -175.7(10) . . . . ? Cu3 N31 N32 Cu4 3.5(11) . . . . ? N92 Cu4 N32 C32 134.3(8) . . . . ? N94 Cu4 N32 C32 -113.6(10) . . . . ? N34 Cu4 N32 C32 4.6(8) . . . . ? N92 Cu4 N32 N31 -49.8(11) . . . . ? N94 Cu4 N32 N31 62.3(12) . . . . ? N34 Cu4 N32 N31 -179.5(9) . . . . ? N31 N32 C32 C46 178.5(15) . . . . ? Cu4 N32 C32 C46 -5.2(13) . . . . ? N31 N32 C32 C33 0.01(15) . . . . ? Cu4 N32 C32 C33 176.2(8) . . . . ? N32 C32 C33 C34 0.0(3) . . . . ? C46 C32 C33 C34 -178.5(16) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? N32 N31 C35 C34 0.0(4) . . . . ? Cu3 N31 C35 C34 -179.3(9) . . . . ? N32 N31 C35 C36 -178.5(14) . . . . ? Cu3 N31 C35 C36 2.3(12) . . . . ? C33 C34 C35 N31 0.0(5) . . . . ? C33 C34 C35 C36 178.3(15) . . . . ? N31 C35 C36 N33 0(2) . . . . ? C34 C35 C36 N33 -178.0(15) . . . . ? C35 C36 N33 C38 179.6(15) . . . . ? C35 C36 N33 Cu3 -3(2) . . . . ? N62 Cu3 N33 C36 138.4(15) . . . . ? N31 Cu3 N33 C36 3.2(15) . . . . ? N64 Cu3 N33 C36 -116.2(16) . . . . ? N62 Cu3 N33 C38 -44.4(17) . . . . ? N31 Cu3 N33 C38 -179.6(16) . . . . ? N64 Cu3 N33 C38 61.0(18) . . . . ? C36 N33 C38 C43 154.9(15) . . . . ? Cu3 N33 C38 C43 -22.3(17) . . . . ? C36 N33 C38 C39 -24(2) . . . . ? Cu3 N33 C38 C39 159.1(8) . . . . ? C43 C38 C39 C40 -0.03(14) . . . . ? N33 C38 C39 C40 178.6(13) . . . . ? C38 C39 C40 C41 -0.01(15) . . . . ? C38 C39 C40 F31 179.97(14) . . . . ? F31 C40 C41 C42 -180.0(3) . . . . ? C39 C40 C41 C42 0.0(3) . . . . ? C40 C41 C42 F32 180.0(3) . . . . ? C40 C41 C42 C43 0.0(4) . . . . ? C39 C38 C43 C42 0.1(3) . . . . ? N33 C38 C43 C42 -178.6(13) . . . . ? C41 C42 C43 C38 -0.1(4) . . . . ? F32 C42 C43 C38 180.0(2) . . . . ? N32 C32 C46 N34 2(2) . . . . ? C33 C32 C46 N34 -179.0(14) . . . . ? C32 C46 N34 C48 175.7(16) . . . . ? C32 C46 N34 Cu4 1(2) . . . . ? N32 Cu4 N34 C46 -3.3(15) . . . . ? N92 Cu4 N34 C46 -131.8(15) . . . . ? N94 Cu4 N34 C46 129.7(15) . . . . ? N32 Cu4 N34 C48 -177.2(16) . . . . ? N92 Cu4 N34 C48 54.3(19) . . . . ? N94 Cu4 N34 C48 -44.3(18) . . . . ? C46 N34 C48 C53 152.7(16) . . . . ? Cu4 N34 C48 C53 -33.9(18) . . . . ? C46 N34 C48 C49 -24(2) . . . . ? Cu4 N34 C48 C49 149.3(9) . . . . ? C53 C48 C49 C50 -0.03(14) . . . . ? N34 C48 C49 C50 176.7(14) . . . . ? C48 C49 C50 F33 179.99(14) . . . . ? C48 C49 C50 C51 -0.01(15) . . . . ? C49 C50 C51 C52 0.0(3) . . . . ? F33 C50 C51 C52 -180.0(2) . . . . ? C50 C51 C52 C53 0.0(4) . . . . ? C50 C51 C52 F34 -180.0(2) . . . . ? C51 C52 C53 C48 0.0(5) . . . . ? F34 C52 C53 C48 179.9(2) . . . . ? C49 C48 C53 C52 0.0(3) . . . . ? N34 C48 C53 C52 -176.8(14) . . . . ? N3 Cu1 N61 C65 -109.7(10) . . . . ? N1 Cu1 N61 C65 139.1(8) . . . . ? N63 Cu1 N61 C65 1.6(8) . . . . ? N3 Cu1 N61 N62 70.5(12) . . . . ? N1 Cu1 N61 N62 -40.6(11) . . . . ? N63 Cu1 N61 N62 -178.2(10) . . . . ? C65 N61 N62 C62 0.02(16) . . . . ? Cu1 N61 N62 C62 179.7(10) . . . . ? C65 N61 N62 Cu3 172.9(10) . . . . ? Cu1 N61 N62 Cu3 -7.3(12) . . . . ? N31 Cu3 N62 N61 66.8(12) . . . . ? N33 Cu3 N62 N61 -41.3(12) . . . . ? N64 Cu3 N62 N61 -170.1(10) . . . . ? N31 Cu3 N62 C62 -120.1(9) . . . . ? N33 Cu3 N62 C62 131.9(8) . . . . ? N64 Cu3 N62 C62 3.0(8) . . . . ? N61 N62 C62 C63 -0.03(15) . . . . ? Cu3 N62 C62 C63 -173.9(9) . . . . ? N61 N62 C62 C76 172.8(15) . . . . ? Cu3 N62 C62 C76 -1.1(14) . . . . ? N62 C62 C63 C64 0.1(3) . . . . ? C76 C62 C63 C64 -172.4(16) . . . . ? C62 C63 C64 C65 -0.1(4) . . . . ? N62 N61 C65 C64 -0.1(4) . . . . ? Cu1 N61 C65 C64 -179.8(9) . . . . ? N62 N61 C65 C66 -177.3(14) . . . . ? Cu1 N61 C65 C66 3.0(12) . . . . ? C63 C64 C65 N61 0.1(5) . . . . ? C63 C64 C65 C66 177.1(15) . . . . ? N61 C65 C66 N63 -9(2) . . . . ? C64 C65 C66 N63 173.3(16) . . . . ? C65 C66 N63 C68 172.9(17) . . . . ? C65 C66 N63 Cu1 11(2) . . . . ? N3 Cu1 N63 C66 124.6(16) . . . . ? N1 Cu1 N63 C66 -135.9(16) . . . . ? N61 Cu1 N63 C66 -6.7(16) . . . . ? N3 Cu1 N63 C68 -36.7(19) . . . . ? N1 Cu1 N63 C68 63(2) . . . . ? N61 Cu1 N63 C68 -168.0(18) . . . . ? C66 N63 C68 C73 140.7(17) . . . . ? Cu1 N63 C68 C73 -59.3(18) . . . . ? C66 N63 C68 C69 -39(2) . . . . ? Cu1 N63 C68 C69 121.1(12) . . . . ? C73 C68 C69 C70 -0.04(14) . . . . ? N63 C68 C69 C70 179.6(15) . . . . ? C68 C69 C70 C71 -0.04(15) . . . . ? C68 C69 C70 F61 179.97(13) . . . . ? C69 C70 C71 C72 0.1(3) . . . . ? F61 C70 C71 C72 -179.9(2) . . . . ? C70 C71 C72 F62 180.0(2) . . . . ? C70 C71 C72 C73 0.0(4) . . . . ? C69 C68 C73 C72 0.1(3) . . . . ? N63 C68 C73 C72 -179.6(15) . . . . ? F62 C72 C73 C68 180.0(2) . . . . ? C71 C72 C73 C68 0.0(4) . . . . ? N62 C62 C76 N64 -3(2) . . . . ? C63 C62 C76 N64 170.2(14) . . . . ? C62 C76 N64 C78 -174.3(16) . . . . ? C62 C76 N64 Cu3 5(2) . . . . ? N62 Cu3 N64 C76 -4.5(15) . . . . ? N31 Cu3 N64 C76 130.9(15) . . . . ? N33 Cu3 N64 C76 -129.1(15) . . . . ? N62 Cu3 N64 C78 174.8(18) . . . . ? N31 Cu3 N64 C78 -49.8(19) . . . . ? N33 Cu3 N64 C78 50(2) . . . . ? C76 N64 C78 C79 21(2) . . . . ? Cu3 N64 C78 C79 -158.8(9) . . . . ? C76 N64 C78 C83 -161.5(15) . . . . ? Cu3 N64 C78 C83 19(2) . . . . ? N64 C78 C79 C80 178.1(17) . . . . ? C83 C78 C79 C80 0.01(15) . . . . ? C78 C79 C80 F63 -179.98(17) . . . . ? C78 C79 C80 C81 0.05(16) . . . . ? C79 C80 C81 C82 -0.1(4) . . . . ? F63 C80 C81 C82 179.9(3) . . . . ? C80 C81 C82 F64 -180.0(3) . . . . ? C80 C81 C82 C83 0.1(5) . . . . ? F64 C82 C83 C78 -180.0(3) . . . . ? C81 C82 C83 C78 0.0(5) . . . . ? C79 C78 C83 C82 0.0(4) . . . . ? N64 C78 C83 C82 -178.3(16) . . . . ? N2 Cu2 N91 N92 55.0(12) . . . . ? N93 Cu2 N91 N92 -176.8(10) . . . . ? N4 Cu2 N91 N92 -55.2(11) . . . . ? N2 Cu2 N91 C95 -127.6(9) . . . . ? N93 Cu2 N91 C95 0.7(8) . . . . ? N4 Cu2 N91 C95 122.2(8) . . . . ? C95 N91 N92 C92 0.02(16) . . . . ? Cu2 N91 N92 C92 177.3(10) . . . . ? C95 N91 N92 Cu4 -171.9(10) . . . . ? Cu2 N91 N92 Cu4 5.3(12) . . . . ? N32 Cu4 N92 C92 143.3(8) . . . . ? N94 Cu4 N92 C92 7.5(8) . . . . ? N34 Cu4 N92 C92 -109.0(10) . . . . ? N32 Cu4 N92 N91 -44.5(11) . . . . ? N94 Cu4 N92 N91 179.8(10) . . . . ? N34 Cu4 N92 N91 63.3(12) . . . . ? N91 N92 C92 C93 0.01(16) . . . . ? Cu4 N92 C92 C93 172.7(9) . . . . ? N91 N92 C92 C106 -178.0(14) . . . . ? Cu4 N92 C92 C106 -5.2(13) . . . . ? N92 C92 C93 C94 0.0(4) . . . . ? C106 C92 C93 C94 177.7(16) . . . . ? C92 C93 C94 C95 0.0(4) . . . . ? N92 N91 C95 C94 0.0(4) . . . . ? Cu2 N91 C95 C94 -177.7(9) . . . . ? N92 N91 C95 C96 178.6(14) . . . . ? Cu2 N91 C95 C96 1.0(13) . . . . ? C93 C94 C95 N91 0.0(5) . . . . ? C93 C94 C95 C96 -178.5(16) . . . . ? N91 C95 C96 N93 -3(2) . . . . ? C94 C95 C96 N93 175.3(15) . . . . ? C95 C96 N93 C98 177.9(17) . . . . ? C95 C96 N93 Cu2 4(2) . . . . ? N2 Cu2 N93 C96 138.2(15) . . . . ? N91 Cu2 N93 C96 -2.4(15) . . . . ? N4 Cu2 N93 C96 -123.0(15) . . . . ? N2 Cu2 N93 C98 -35(2) . . . . ? N91 Cu2 N93 C98 -175.9(18) . . . . ? N4 Cu2 N93 C98 63.5(19) . . . . ? C96 N93 C98 C103 153.0(16) . . . . ? Cu2 N93 C98 C103 -33.9(19) . . . . ? C96 N93 C98 C99 -28(2) . . . . ? Cu2 N93 C98 C99 145.5(11) . . . . ? N93 C98 C99 C100 -179.5(16) . . . . ? C103 C98 C99 C100 0.00(15) . . . . ? C98 C99 C100 F91 179.98(16) . . . . ? C98 C99 C100 C101 -0.01(16) . . . . ? C99 C100 C101 C102 0.1(3) . . . . ? F91 C100 C101 C102 -179.9(3) . . . . ? C100 C101 C102 C103 -0.1(5) . . . . ? C100 C101 C102 F92 -180.0(2) . . . . ? C101 C102 C103 C98 0.1(5) . . . . ? F92 C102 C103 C98 179.9(3) . . . . ? N93 C98 C103 C102 179.5(15) . . . . ? C99 C98 C103 C102 0.0(3) . . . . ? N92 C92 C106 N94 -2(2) . . . . ? C93 C92 C106 N94 179.6(16) . . . . ? C92 C106 N94 C108 -176.4(18) . . . . ? C92 C106 N94 Cu4 8(3) . . . . ? N32 Cu4 N94 C106 -138.6(15) . . . . ? N92 Cu4 N94 C106 -8.4(15) . . . . ? N34 Cu4 N94 C106 118.4(16) . . . . ? N32 Cu4 N94 C108 46(2) . . . . ? N92 Cu4 N94 C108 176.6(18) . . . . ? N34 Cu4 N94 C108 -56.6(19) . . . . ? C106 N94 C108 C113 -146.0(18) . . . . ? Cu4 N94 C108 C113 28(2) . . . . ? C106 N94 C108 C109 36(3) . . . . ? Cu4 N94 C108 C109 -149.6(10) . . . . ? C113 C108 C109 C110 0.02(13) . . . . ? N94 C108 C109 C110 178.1(16) . . . . ? C108 C109 C110 F93 -179.99(12) . . . . ? C108 C109 C110 C111 0.01(14) . . . . ? C109 C110 C111 C112 0.0(3) . . . . ? F93 C110 C111 C112 180.0(2) . . . . ? C110 C111 C112 C113 0.0(4) . . . . ? C110 C111 C112 F94 180.0(2) . . . . ? N94 C108 C113 C112 -178.0(17) . . . . ? C109 C108 C113 C112 0.0(3) . . . . ? C111 C112 C113 C108 0.0(5) . . . . ? F94 C112 C113 C108 -180.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.432 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.278 # Attachment 'mm_difluoro_free_ligand.cif' data_jrp129 _database_code_depnum_ccdc_archive 'CCDC 629023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H10 F4 N4' _chemical_formula_sum 'C18 H10 F4 N4' _chemical_formula_weight 358.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.706(2) _cell_length_b 5.5894(8) _cell_length_c 22.376(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.667(9) _cell_angle_gamma 90.00 _cell_volume 1550.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'DCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29353 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.27 _reflns_number_total 3119 _reflns_number_gt 2777 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non H ANIS. All H fixed to ride at -1.2 ; _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^)+(0.0445P)^2^+0.6924P] 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 3119 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 N1 N 0.71089(8) 0.20548(18) 0.47848(5) 0.0229(2) Uani 1 1 d . . . N2 N 0.63554(8) 0.17472(18) 0.51155(5) 0.0218(2) Uani 1 1 d . . . C2 C 0.61113(9) 0.3576(2) 0.54491(5) 0.0173(2) Uani 1 1 d . . . C3 C 0.65824(9) 0.5853(2) 0.54562(5) 0.0197(2) Uani 1 1 d . . . H3 H 0.6379 0.7125 0.5689 0.024 Uiso 1 1 calc R . . C4 C 0.73455(9) 0.6171(2) 0.51154(5) 0.0195(2) Uani 1 1 d . . . H4 H 0.7687 0.7673 0.5099 0.023 Uiso 1 1 calc R . . C5 C 0.76005(9) 0.4186(2) 0.47914(5) 0.0179(2) Uani 1 1 d . . . C6 C 0.84365(10) 0.4252(2) 0.44267(6) 0.0212(3) Uani 1 1 d . . . H6 H 0.8594 0.2841 0.4226 0.025 Uiso 1 1 calc R . . N3 N 0.89505(8) 0.61685(19) 0.43765(5) 0.0209(2) Uani 1 1 d . . . C8 C 0.97250(9) 0.6201(2) 0.40041(5) 0.0193(2) Uani 1 1 d . . . C9 C 0.97879(9) 0.4460(2) 0.35601(5) 0.0218(3) Uani 1 1 d . . . H9 H 0.9304 0.3142 0.3492 0.026 Uiso 1 1 calc R . . C10 C 1.05715(10) 0.4720(2) 0.32260(5) 0.0226(3) Uani 1 1 d . . . C11 C 1.12979(9) 0.6595(2) 0.32973(6) 0.0233(3) Uani 1 1 d . . . H11 H 1.1834 0.6714 0.3062 0.028 Uiso 1 1 calc R . . C12 C 1.11971(10) 0.8285(2) 0.37315(6) 0.0222(3) Uani 1 1 d . . . C13 C 1.04320(9) 0.8151(2) 0.40872(5) 0.0209(3) Uani 1 1 d . . . H13 H 1.0389 0.9356 0.4380 0.025 Uiso 1 1 calc R . . C16 C 0.53190(9) 0.2991(2) 0.58207(5) 0.0189(2) Uani 1 1 d . . . H16 H 0.5042 0.1411 0.5818 0.023 Uiso 1 1 calc R . . N4 N 0.50065(8) 0.46046(18) 0.61450(4) 0.0187(2) Uani 1 1 d . . . C18 C 0.42676(9) 0.4039(2) 0.65171(5) 0.0180(2) Uani 1 1 d . . . C19 C 0.35833(9) 0.2034(2) 0.64334(5) 0.0199(3) Uani 1 1 d . . . H19 H 0.3591 0.0913 0.6115 0.024 Uiso 1 1 calc R . . C20 C 0.28996(10) 0.1752(2) 0.68298(6) 0.0220(3) Uani 1 1 d . . . C21 C 0.28468(10) 0.3307(2) 0.73044(6) 0.0239(3) Uani 1 1 d . . . H21 H 0.2370 0.3051 0.7571 0.029 Uiso 1 1 calc R . . C22 C 0.35315(9) 0.5255(2) 0.73649(6) 0.0228(3) Uani 1 1 d . . . C23 C 0.42335(9) 0.5679(2) 0.69849(5) 0.0207(3) Uani 1 1 d . . . H23 H 0.4684 0.7054 0.7040 0.025 Uiso 1 1 calc R . . F1 F 1.06254(6) 0.30481(15) 0.27922(4) 0.0330(2) Uani 1 1 d . . . F2 F 1.18837(6) 1.01762(14) 0.38111(4) 0.0314(2) Uani 1 1 d . . . F3 F 0.22202(6) -0.01634(14) 0.67489(4) 0.0320(2) Uani 1 1 d . . . F4 F 0.35064(6) 0.68454(16) 0.78218(4) 0.0347(2) 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 N1 0.0266(5) 0.0186(5) 0.0274(5) -0.0020(4) 0.0145(4) -0.0016(4) N2 0.0246(5) 0.0183(5) 0.0259(5) -0.0017(4) 0.0127(4) -0.0019(4) C2 0.0175(5) 0.0172(6) 0.0174(5) 0.0010(4) 0.0042(4) 0.0009(4) C3 0.0227(6) 0.0164(6) 0.0213(6) -0.0020(4) 0.0079(5) 0.0009(5) C4 0.0212(6) 0.0158(6) 0.0226(6) -0.0003(5) 0.0067(4) -0.0018(5) C5 0.0188(5) 0.0175(6) 0.0184(5) 0.0012(4) 0.0058(4) 0.0008(4) C6 0.0233(6) 0.0195(6) 0.0229(6) -0.0009(5) 0.0097(5) 0.0016(5) N3 0.0192(5) 0.0225(5) 0.0229(5) -0.0001(4) 0.0086(4) -0.0002(4) C8 0.0171(5) 0.0202(6) 0.0212(6) 0.0030(5) 0.0054(4) 0.0015(5) C9 0.0196(6) 0.0227(6) 0.0240(6) -0.0014(5) 0.0070(5) -0.0034(5) C10 0.0215(6) 0.0261(6) 0.0208(6) -0.0028(5) 0.0060(5) 0.0006(5) C11 0.0179(6) 0.0315(7) 0.0222(6) 0.0033(5) 0.0080(5) -0.0004(5) C12 0.0187(6) 0.0220(6) 0.0250(6) 0.0038(5) 0.0026(5) -0.0045(5) C13 0.0221(6) 0.0196(6) 0.0215(6) 0.0003(5) 0.0060(5) 0.0006(5) C16 0.0192(5) 0.0172(6) 0.0214(6) 0.0011(4) 0.0069(4) -0.0014(4) N4 0.0186(5) 0.0201(5) 0.0185(5) 0.0005(4) 0.0063(4) -0.0008(4) C18 0.0168(5) 0.0194(6) 0.0185(5) 0.0020(4) 0.0051(4) 0.0017(4) C19 0.0208(6) 0.0188(6) 0.0211(6) -0.0017(5) 0.0063(4) 0.0000(5) C20 0.0181(6) 0.0208(6) 0.0275(6) 0.0020(5) 0.0056(5) -0.0032(5) C21 0.0188(6) 0.0317(7) 0.0237(6) 0.0020(5) 0.0103(5) 0.0011(5) C22 0.0200(6) 0.0280(7) 0.0212(6) -0.0064(5) 0.0064(5) 0.0024(5) C23 0.0177(5) 0.0206(6) 0.0241(6) -0.0034(5) 0.0054(4) -0.0017(5) F1 0.0321(4) 0.0395(5) 0.0322(4) -0.0145(4) 0.0173(3) -0.0073(3) F2 0.0290(4) 0.0297(4) 0.0377(4) -0.0016(3) 0.0117(3) -0.0134(3) F3 0.0303(4) 0.0277(4) 0.0422(5) -0.0031(3) 0.0169(3) -0.0125(3) F4 0.0302(4) 0.0447(5) 0.0338(4) -0.0200(4) 0.0172(3) -0.0062(4) _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 N1 N2 1.3432(14) . ? N1 C5 1.3435(16) . ? N2 C2 1.3415(15) . ? C2 C3 1.4049(17) . ? C2 C16 1.4762(16) . ? C3 C4 1.3702(16) . ? C3 H3 0.9500 . ? C4 C5 1.4014(16) . ? C4 H4 0.9500 . ? C5 C6 1.4752(16) . ? C6 N3 1.2724(16) . ? C6 H6 0.9500 . ? N3 C8 1.4221(15) . ? C8 C13 1.3989(17) . ? C8 C9 1.4054(17) . ? C9 C10 1.3776(16) . ? C9 H9 0.9500 . ? C10 F1 1.3598(14) . ? C10 C11 1.3824(18) . ? C11 C12 1.3809(18) . ? C11 H11 0.9500 . ? C12 F2 1.3574(14) . ? C12 C13 1.3868(17) . ? C13 H13 0.9500 . ? C16 N4 1.2744(16) . ? C16 H16 0.9500 . ? N4 C18 1.4203(14) . ? C18 C23 1.3991(16) . ? C18 C19 1.4055(17) . ? C19 C20 1.3799(17) . ? C19 H19 0.9500 . ? C20 F3 1.3623(14) . ? C20 C21 1.3853(18) . ? C21 C22 1.3818(18) . ? C21 H21 0.9500 . ? C22 F4 1.3603(14) . ? C22 C23 1.3811(16) . ? C23 H23 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 N1 C5 119.55(10) . . ? C2 N2 N1 119.26(10) . . ? N2 C2 C3 123.13(10) . . ? N2 C2 C16 114.47(10) . . ? C3 C2 C16 122.39(10) . . ? C4 C3 C2 117.57(11) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 117.21(11) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? N1 C5 C4 123.22(10) . . ? N1 C5 C6 113.92(10) . . ? C4 C5 C6 122.86(11) . . ? N3 C6 C5 121.05(11) . . ? N3 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 N3 C8 119.79(10) . . ? C13 C8 C9 119.94(11) . . ? C13 C8 N3 116.02(10) . . ? C9 C8 N3 124.01(11) . . ? C10 C9 C8 118.07(11) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? F1 C10 C9 118.06(11) . . ? F1 C10 C11 117.81(10) . . ? C9 C10 C11 124.13(12) . . ? C12 C11 C10 115.92(11) . . ? C12 C11 H11 122.0 . . ? C10 C11 H11 122.0 . . ? F2 C12 C11 117.97(11) . . ? F2 C12 C13 118.54(11) . . ? C11 C12 C13 123.49(11) . . ? C12 C13 C8 118.44(11) . . ? C12 C13 H13 120.8 . . ? C8 C13 H13 120.8 . . ? N4 C16 C2 120.01(11) . . ? N4 C16 H16 120.0 . . ? C2 C16 H16 120.0 . . ? C16 N4 C18 120.32(10) . . ? C23 C18 C19 120.15(10) . . ? C23 C18 N4 115.20(10) . . ? C19 C18 N4 124.64(10) . . ? C20 C19 C18 117.63(11) . . ? C20 C19 H19 121.2 . . ? C18 C19 H19 121.2 . . ? F3 C20 C19 118.32(11) . . ? F3 C20 C21 117.33(11) . . ? C19 C20 C21 124.35(11) . . ? C22 C21 C20 115.74(11) . . ? C22 C21 H21 122.1 . . ? C20 C21 H21 122.1 . . ? F4 C22 C23 118.40(11) . . ? F4 C22 C21 118.06(10) . . ? C23 C22 C21 123.54(11) . . ? C22 C23 C18 118.59(11) . . ? C22 C23 H23 120.7 . . ? C18 C23 H23 120.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 C2 -0.30(17) . . . . ? N1 N2 C2 C3 2.15(18) . . . . ? N1 N2 C2 C16 -176.66(10) . . . . ? N2 C2 C3 C4 -1.67(18) . . . . ? C16 C2 C3 C4 177.05(11) . . . . ? C2 C3 C4 C5 -0.57(17) . . . . ? N2 N1 C5 C4 -2.01(18) . . . . ? N2 N1 C5 C6 177.93(10) . . . . ? C3 C4 C5 N1 2.42(18) . . . . ? C3 C4 C5 C6 -177.52(11) . . . . ? N1 C5 C6 N3 178.09(11) . . . . ? C4 C5 C6 N3 -1.96(18) . . . . ? C5 C6 N3 C8 -177.77(10) . . . . ? C6 N3 C8 C13 -165.08(11) . . . . ? C6 N3 C8 C9 16.83(18) . . . . ? C13 C8 C9 C10 1.29(17) . . . . ? N3 C8 C9 C10 179.32(11) . . . . ? C8 C9 C10 F1 -179.36(11) . . . . ? C8 C9 C10 C11 -0.37(19) . . . . ? F1 C10 C11 C12 178.38(11) . . . . ? C9 C10 C11 C12 -0.62(19) . . . . ? C10 C11 C12 F2 -179.08(10) . . . . ? C10 C11 C12 C13 0.72(18) . . . . ? F2 C12 C13 C8 179.97(10) . . . . ? C11 C12 C13 C8 0.17(18) . . . . ? C9 C8 C13 C12 -1.20(17) . . . . ? N3 C8 C13 C12 -179.38(10) . . . . ? N2 C2 C16 N4 -178.34(11) . . . . ? C3 C2 C16 N4 2.84(17) . . . . ? C2 C16 N4 C18 -178.22(10) . . . . ? C16 N4 C18 C23 161.19(11) . . . . ? C16 N4 C18 C19 -20.26(17) . . . . ? C23 C18 C19 C20 -0.66(17) . . . . ? N4 C18 C19 C20 -179.15(11) . . . . ? C18 C19 C20 F3 179.05(10) . . . . ? C18 C19 C20 C21 -0.22(19) . . . . ? F3 C20 C21 C22 -178.72(11) . . . . ? C19 C20 C21 C22 0.56(19) . . . . ? C20 C21 C22 F4 179.61(11) . . . . ? C20 C21 C22 C23 -0.02(19) . . . . ? F4 C22 C23 C18 179.54(11) . . . . ? C21 C22 C23 C18 -0.83(19) . . . . ? C19 C18 C23 C22 1.16(17) . . . . ? N4 C18 C23 C22 179.79(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.268 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.039 # Attachment 'o_biphenyl_Cu_complex.cif' data_jrp115cu _database_code_depnum_ccdc_archive 'CCDC 629024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H80 Cu2 F12 N8 P2' _chemical_formula_sum 'C96 H80 Cu2 F12 N8 P2' _chemical_formula_weight 1762.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall "C 2c 2'" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.5144(5) _cell_length_b 27.3551(12) _cell_length_c 22.2181(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8213.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74864 _diffrn_reflns_av_R_equivalents 0.1478 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.99 _reflns_number_total 8076 _reflns_number_gt 4717 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. First benzene C51-C53 is full occupancy but lies across a 2-fold axis such that there are only three atoms in the asymmetric unit of this ring. Second benzene C61-C64 is again full occupancy and lies across a 2-fold axis but in this case the axis runs through two of the atoms so there are four atoms (including the two half-occupancy atoms C61 & C64 that lie on the axis) in the asymmetric unit of this ring. Third benzene is disordered over two half occupancy, overlapping, sites (C71-6 and C81-6). Fourth benzene is disordered over two half occupancy, overlapping, sites (C91-6 and C101-6). Helical structure hence can be in a chiral space group like this. ; _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^)+(0.0275P)^2^+11.4372P] 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 0.000(15) _refine_ls_number_reflns 8076 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.27688(4) 0.43841(2) 0.46082(3) 0.03705(17) Uani 1 1 d . . . N1 N 0.1600(3) 0.47672(13) 0.4926(2) 0.0370(11) Uani 1 1 d . . . C2 C 0.0737(3) 0.45211(17) 0.4875(2) 0.0258(12) Uani 1 1 d . . . C3 C -0.0169(3) 0.47558(16) 0.4947(2) 0.0338(13) Uani 1 1 d . . . H3 H -0.0772 0.4578 0.4922 0.041 Uiso 1 1 calc R . . C6 C 0.0846(3) 0.39989(17) 0.4763(2) 0.0344(13) Uani 1 1 d . . . H6 H 0.0282 0.3793 0.4730 0.041 Uiso 1 1 calc R . . N2 N 0.1719(3) 0.38253(12) 0.47097(17) 0.0283(9) Uani 1 1 d . . . C8 C 0.1878(3) 0.33172(17) 0.4620(3) 0.0374(12) Uani 1 1 d . . . C9 C 0.1275(5) 0.30504(19) 0.4229(3) 0.0610(19) Uani 1 1 d . . . H9 H 0.0728 0.3204 0.4038 0.073 Uiso 1 1 calc R . . C10 C 0.1475(6) 0.2565(2) 0.4121(3) 0.088(3) Uani 1 1 d . . . H10 H 0.1073 0.2385 0.3849 0.106 Uiso 1 1 calc R . . C11 C 0.2255(6) 0.2342(2) 0.4405(3) 0.089(2) Uani 1 1 d . . . H11 H 0.2382 0.2005 0.4337 0.106 Uiso 1 1 calc R . . C12 C 0.2862(5) 0.26068(18) 0.4792(3) 0.0619(18) Uani 1 1 d . . . H12 H 0.3397 0.2447 0.4987 0.074 Uiso 1 1 calc R . . C13 C 0.2699(4) 0.31006(16) 0.4899(2) 0.0386(12) Uani 1 1 d . . . C14 C 0.3378(3) 0.33824(16) 0.5296(2) 0.0325(12) Uani 1 1 d . . . C15 C 0.4396(4) 0.3332(2) 0.5210(2) 0.0460(15) Uani 1 1 d . . . H15 H 0.4637 0.3114 0.4911 0.055 Uiso 1 1 calc R . . C16 C 0.5052(4) 0.3595(2) 0.5554(3) 0.0557(18) Uani 1 1 d . . . H16 H 0.5742 0.3558 0.5488 0.067 Uiso 1 1 calc R . . C17 C 0.4730(4) 0.3909(2) 0.5989(3) 0.0578(18) Uani 1 1 d . . . H17 H 0.5190 0.4095 0.6217 0.069 Uiso 1 1 calc R . . C18 C 0.3723(4) 0.3953(2) 0.6092(3) 0.0640(18) Uani 1 1 d . . . H18 H 0.3488 0.4160 0.6405 0.077 Uiso 1 1 calc R . . C19 C 0.3055(3) 0.3693(2) 0.5738(2) 0.0477(15) Uani 1 1 d . . . H19 H 0.2365 0.3732 0.5803 0.057 Uiso 1 1 calc R . . N31 N 0.4015(3) 0.4810(2) 0.4808(2) 0.089(2) Uani 1 1 d . . . C32 C 0.4845(3) 0.46326(17) 0.4609(2) 0.0295(11) Uani 1 1 d . . . C33 C 0.5735(3) 0.48169(17) 0.4793(2) 0.0398(15) Uani 1 1 d . . . H33 H 0.6339 0.4693 0.4635 0.048 Uiso 1 1 calc R . . C36 C 0.4709(3) 0.42502(17) 0.4161(2) 0.0309(12) Uani 1 1 d . . . H36 H 0.5260 0.4103 0.3967 0.037 Uiso 1 1 calc R . . N32 N 0.3821(3) 0.41170(13) 0.40368(18) 0.0315(10) Uani 1 1 d . . . C38 C 0.3617(4) 0.37654(18) 0.3584(2) 0.0412(14) Uani 1 1 d . . . C39 C 0.4218(4) 0.33533(19) 0.3520(3) 0.0514(16) Uani 1 1 d . . . H39 H 0.4777 0.3308 0.3772 0.062 Uiso 1 1 calc R . . C40 C 0.3983(5) 0.3008(2) 0.3078(3) 0.077(2) Uani 1 1 d . . . H40 H 0.4383 0.2725 0.3030 0.093 Uiso 1 1 calc R . . C41 C 0.3163(5) 0.3080(3) 0.2708(4) 0.094(3) Uani 1 1 d . . . H41 H 0.3010 0.2849 0.2402 0.113 Uiso 1 1 calc R . . C42 C 0.2580(4) 0.3482(2) 0.2786(3) 0.074(2) Uani 1 1 d . . . H42 H 0.2019 0.3522 0.2534 0.088 Uiso 1 1 calc R . . C43 C 0.2775(4) 0.38371(19) 0.3222(2) 0.0484(15) Uani 1 1 d . . . C44 C 0.2101(4) 0.42611(19) 0.3292(2) 0.0396(13) Uani 1 1 d . . . C45 C 0.1079(4) 0.4191(2) 0.3250(2) 0.0452(15) Uani 1 1 d . . . H45 H 0.0827 0.3873 0.3174 0.054 Uiso 1 1 calc R . . C46 C 0.0424(4) 0.4578(2) 0.3318(2) 0.0436(15) Uani 1 1 d . . . H46 H -0.0266 0.4525 0.3271 0.052 Uiso 1 1 calc R . . C47 C 0.0767(4) 0.5039(2) 0.3454(2) 0.0466(15) Uani 1 1 d . . . H47 H 0.0317 0.5300 0.3519 0.056 Uiso 1 1 calc R . . C48 C 0.1781(4) 0.5116(2) 0.3494(2) 0.0465(15) Uani 1 1 d . . . H48 H 0.2024 0.5434 0.3582 0.056 Uiso 1 1 calc R . . C49 C 0.2445(3) 0.47359(19) 0.3407(2) 0.0408(14) Uani 1 1 d . . . H49 H 0.3136 0.4797 0.3426 0.049 Uiso 1 1 calc R . . P1 P 0.78024(10) 0.37160(5) 0.41697(6) 0.0375(3) Uani 1 1 d . . . F11 F 0.7800(3) 0.31872(11) 0.39304(17) 0.0822(11) Uani 1 1 d . . . F12 F 0.8773(2) 0.38322(13) 0.38015(18) 0.0786(12) Uani 1 1 d . . . F13 F 0.8468(2) 0.35521(13) 0.47247(16) 0.0706(10) Uani 1 1 d . . . F14 F 0.6832(2) 0.36091(13) 0.45542(16) 0.0722(11) Uani 1 1 d . . . F15 F 0.7128(3) 0.38984(15) 0.36400(16) 0.0941(13) Uani 1 1 d . . . F16 F 0.7814(2) 0.42548(11) 0.4421(2) 0.1087(17) Uani 1 1 d . . . C51 C 0.5408(4) 0.5627(3) 0.7334(2) 0.0598(17) Uani 1 1 d . . . H51 H 0.5693 0.5930 0.7216 0.072 Uiso 1 1 calc R . . C52 C 0.5842(5) 0.5204(4) 0.7158(3) 0.080(2) Uani 1 1 d . . . H52 H 0.6423 0.5209 0.6918 0.096 Uiso 1 1 calc R . . C53 C 0.5433(6) 0.4771(3) 0.7330(3) 0.101(3) Uani 1 1 d . . . H53 H 0.5736 0.4471 0.7219 0.121 Uiso 1 1 calc R . . C61 C 0.5000 0.2095(4) 0.7500 0.102(5) Uani 1 2 d S . . H61 H 0.5000 0.1748 0.7500 0.123 Uiso 1 2 calc SR . . C62 C 0.4459(5) 0.2348(4) 0.7086(4) 0.092(3) Uani 1 1 d . . . H62 H 0.4076 0.2176 0.6797 0.110 Uiso 1 1 calc R . . C63 C 0.4467(5) 0.2833(4) 0.7086(3) 0.085(3) Uani 1 1 d . . . H63 H 0.4095 0.3007 0.6793 0.101 Uiso 1 1 calc R . . C64 C 0.5000 0.3082(4) 0.7500 0.085(4) Uani 1 2 d S . . H64 H 0.5000 0.3429 0.7500 0.103 Uiso 1 2 calc SR . . C71 C 0.7480(9) 0.4055(3) 0.6016(4) 0.048(5) Uani 0.50 1 d PG A 1 H71 H 0.7251 0.3847 0.5704 0.058 Uiso 0.50 1 calc PR A 1 C72 C 0.7495(9) 0.3890(3) 0.6608(5) 0.069(6) Uani 0.50 1 d PG A 1 H72 H 0.7276 0.3569 0.6700 0.083 Uiso 0.50 1 calc PR A 1 C73 C 0.7831(9) 0.4195(4) 0.7065(3) 0.060(4) Uani 0.50 1 d PG A 1 H73 H 0.7842 0.4082 0.7469 0.073 Uiso 0.50 1 calc PR A 1 C74 C 0.8152(9) 0.4665(3) 0.6930(3) 0.048(4) Uani 0.50 1 d PG A 1 H74 H 0.8382 0.4873 0.7242 0.058 Uiso 0.50 1 calc PR A 1 C75 C 0.8137(7) 0.4830(2) 0.6338(4) 0.042(3) Uani 0.50 1 d PG A 1 H75 H 0.8356 0.5152 0.6246 0.051 Uiso 0.50 1 calc PR A 1 C76 C 0.7801(6) 0.4525(3) 0.5882(3) 0.037(2) Uani 0.50 1 d PG A 1 H76 H 0.7791 0.4638 0.5477 0.044 Uiso 0.50 1 calc PR A 1 C81 C 0.7183(7) 0.3739(3) 0.6533(4) 0.050(4) Uani 0.50 1 d PG B 2 H81 H 0.6791 0.3484 0.6368 0.060 Uiso 0.50 1 calc PR B 2 C82 C 0.7514(5) 0.3709(3) 0.7124(4) 0.051(3) Uani 0.50 1 d PG B 2 H82 H 0.7349 0.3433 0.7363 0.061 Uiso 0.50 1 calc PR B 2 C83 C 0.8088(6) 0.4082(3) 0.7365(3) 0.050(4) Uani 0.50 1 d PG B 2 H83 H 0.8315 0.4062 0.7769 0.060 Uiso 0.50 1 calc PR B 2 C84 C 0.8330(7) 0.4486(3) 0.7014(4) 0.043(4) Uani 0.50 1 d PG B 2 H84 H 0.8722 0.4742 0.7179 0.051 Uiso 0.50 1 calc PR B 2 C85 C 0.7999(7) 0.4516(3) 0.6423(4) 0.057(4) Uani 0.50 1 d PG B 2 H85 H 0.8164 0.4792 0.6184 0.068 Uiso 0.50 1 calc PR B 2 C86 C 0.7425(7) 0.4143(4) 0.6182(4) 0.045(5) Uani 0.50 1 d PG B 2 H86 H 0.7199 0.4163 0.5779 0.054 Uiso 0.50 1 calc PR B 2 C91 C 0.0732(14) 0.2810(6) 0.5860(8) 0.060(6) Uani 0.50 1 d PG C 1 H91 H 0.0761 0.2578 0.5542 0.072 Uiso 0.50 1 calc PR C 1 C92 C 0.1419(12) 0.2791(7) 0.6324(9) 0.060(8) Uani 0.50 1 d PG C 1 H92 H 0.1917 0.2546 0.6324 0.072 Uiso 0.50 1 calc PR C 1 C93 C 0.1377(8) 0.3130(8) 0.6790(6) 0.069(7) Uani 0.50 1 d PG C 1 H93 H 0.1847 0.3117 0.7107 0.083 Uiso 0.50 1 calc PR C 1 C94 C 0.0648(9) 0.3488(6) 0.6790(5) 0.090(7) Uani 0.50 1 d PG C 1 H94 H 0.0619 0.3720 0.7108 0.109 Uiso 0.50 1 calc PR C 1 C95 C -0.0040(8) 0.3507(5) 0.6325(6) 0.098(9) Uani 0.50 1 d PG C 1 H95 H -0.0538 0.3752 0.6325 0.118 Uiso 0.50 1 calc PR C 1 C96 C 0.0002(10) 0.3168(6) 0.5860(6) 0.071(7) Uani 0.50 1 d PG C 1 H96 H -0.0467 0.3181 0.5542 0.085 Uiso 0.50 1 calc PR C 1 C101 C 0.0192(9) 0.3400(4) 0.6606(6) 0.048(4) Uani 0.50 1 d PG D 2 H101 H -0.0054 0.3648 0.6865 0.058 Uiso 0.50 1 calc PR D 2 C102 C -0.0179(6) 0.3355(4) 0.6025(6) 0.054(6) Uani 0.50 1 d PG D 2 H102 H -0.0679 0.3572 0.5887 0.065 Uiso 0.50 1 calc PR D 2 C103 C 0.0181(8) 0.2992(5) 0.5646(5) 0.049(5) Uani 0.50 1 d PG D 2 H103 H -0.0073 0.2960 0.5249 0.058 Uiso 0.50 1 calc PR D 2 C104 C 0.0913(11) 0.2674(6) 0.5848(6) 0.059(6) Uani 0.50 1 d PG D 2 H104 H 0.1159 0.2426 0.5589 0.071 Uiso 0.50 1 calc PR D 2 C105 C 0.1284(11) 0.2720(6) 0.6429(7) 0.058(7) Uani 0.50 1 d PG D 2 H105 H 0.1784 0.2503 0.6567 0.069 Uiso 0.50 1 calc PR D 2 C106 C 0.0924(10) 0.3083(6) 0.6808(5) 0.061(6) Uani 0.50 1 d PG D 2 H106 H 0.1178 0.3114 0.7204 0.073 Uiso 0.50 1 calc PR D 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 0.0207(3) 0.0488(4) 0.0417(4) -0.0169(3) 0.0099(3) -0.0063(3) N1 0.029(2) 0.026(2) 0.055(3) 0.001(2) -0.006(2) -0.0027(17) C2 0.017(2) 0.036(3) 0.025(3) 0.011(2) -0.006(2) -0.0066(19) C3 0.012(2) 0.049(3) 0.040(3) 0.008(3) 0.001(2) -0.0033(19) C6 0.026(3) 0.040(3) 0.038(4) 0.005(3) -0.014(2) -0.009(2) N2 0.035(2) 0.024(2) 0.026(3) -0.0021(19) -0.0035(18) -0.0017(16) C8 0.042(3) 0.032(3) 0.038(3) -0.006(3) -0.001(3) -0.009(2) C9 0.085(5) 0.027(4) 0.071(5) -0.005(3) -0.035(4) -0.010(3) C10 0.135(7) 0.021(4) 0.108(6) -0.011(4) -0.053(5) -0.012(4) C11 0.115(6) 0.030(3) 0.121(7) -0.009(4) -0.032(6) -0.001(4) C12 0.072(4) 0.029(3) 0.085(5) -0.004(3) -0.012(4) 0.010(3) C13 0.039(3) 0.030(3) 0.048(3) -0.002(2) 0.002(3) -0.003(3) C14 0.027(3) 0.037(3) 0.033(3) 0.007(3) 0.006(2) -0.002(2) C15 0.031(3) 0.065(4) 0.042(4) 0.001(3) 0.011(3) 0.016(3) C16 0.019(3) 0.085(5) 0.063(5) 0.025(4) 0.000(3) 0.007(3) C17 0.030(3) 0.065(4) 0.078(5) 0.001(4) -0.020(3) 0.001(3) C18 0.045(4) 0.079(4) 0.069(5) -0.030(4) -0.023(3) 0.020(3) C19 0.024(3) 0.067(4) 0.052(4) -0.015(3) -0.001(3) 0.011(3) N31 0.019(2) 0.151(6) 0.097(5) -0.101(4) 0.004(2) 0.003(3) C32 0.019(2) 0.051(3) 0.018(3) -0.003(3) 0.005(2) 0.003(2) C33 0.019(3) 0.044(4) 0.055(4) -0.009(3) 0.012(2) -0.001(2) C36 0.023(3) 0.043(3) 0.027(3) 0.000(3) 0.006(2) 0.004(2) N32 0.029(2) 0.033(3) 0.033(3) -0.006(2) 0.0090(19) -0.0027(17) C38 0.041(3) 0.032(3) 0.051(4) -0.017(3) 0.015(3) -0.008(3) C39 0.049(3) 0.049(4) 0.056(4) -0.017(3) 0.019(3) 0.000(3) C40 0.066(5) 0.066(5) 0.100(6) -0.044(4) 0.028(4) -0.004(4) C41 0.067(5) 0.103(6) 0.111(7) -0.084(5) 0.020(5) -0.012(4) C42 0.046(4) 0.102(5) 0.073(5) -0.061(4) 0.006(3) -0.012(3) C43 0.032(3) 0.064(4) 0.049(4) -0.031(3) 0.010(3) -0.010(3) C44 0.032(3) 0.066(4) 0.020(3) -0.010(2) 0.009(2) -0.011(3) C45 0.040(3) 0.062(4) 0.034(4) -0.006(3) -0.001(3) -0.016(3) C46 0.028(3) 0.073(4) 0.030(3) 0.008(3) -0.006(2) -0.009(3) C47 0.035(3) 0.059(4) 0.046(4) -0.004(3) -0.001(3) -0.009(3) C48 0.043(3) 0.057(4) 0.040(4) -0.012(3) -0.003(3) -0.008(3) C49 0.027(3) 0.062(4) 0.033(3) -0.016(3) 0.003(2) -0.003(2) P1 0.0224(6) 0.0429(8) 0.0474(9) -0.0017(7) -0.0014(7) -0.0047(7) F11 0.082(2) 0.057(2) 0.108(3) -0.036(2) 0.016(3) -0.017(2) F12 0.0379(19) 0.097(3) 0.101(3) 0.037(2) 0.0193(19) -0.0121(18) F13 0.0370(18) 0.118(3) 0.056(2) 0.012(2) -0.0154(17) 0.0015(17) F14 0.0318(17) 0.126(3) 0.059(2) -0.002(2) 0.0121(17) -0.0104(16) F15 0.057(2) 0.142(3) 0.084(3) 0.053(3) -0.023(2) -0.007(2) F16 0.0421(18) 0.053(2) 0.231(5) -0.054(3) -0.027(3) 0.0084(18) C51 0.056(4) 0.089(5) 0.035(4) 0.011(4) -0.010(3) -0.005(4) C52 0.065(5) 0.135(7) 0.039(4) 0.002(5) -0.003(3) 0.034(5) C53 0.152(10) 0.094(6) 0.056(7) -0.017(5) -0.056(6) 0.050(6) C61 0.101(11) 0.041(7) 0.165(16) 0.000 0.095(10) 0.000 C62 0.055(5) 0.141(9) 0.079(7) -0.045(7) 0.029(4) -0.039(6) C63 0.053(5) 0.134(8) 0.067(6) 0.041(6) 0.004(4) 0.006(5) C64 0.079(8) 0.044(6) 0.134(12) 0.000 0.039(8) 0.000 C71 0.056(11) 0.057(10) 0.031(8) -0.013(7) 0.005(6) -0.004(7) C72 0.082(15) 0.060(11) 0.067(13) -0.010(10) -0.007(9) -0.005(9) C73 0.082(11) 0.054(10) 0.044(10) 0.021(8) 0.001(9) -0.004(9) C74 0.045(9) 0.054(10) 0.045(10) -0.006(8) -0.001(7) 0.009(7) C75 0.031(6) 0.046(8) 0.051(9) -0.001(7) -0.014(5) 0.001(6) C76 0.025(5) 0.044(7) 0.041(7) -0.005(6) -0.013(6) 0.008(5) C81 0.034(8) 0.061(9) 0.055(10) -0.009(8) -0.002(7) 0.010(8) C82 0.028(7) 0.054(8) 0.070(10) -0.007(7) 0.007(6) 0.005(5) C83 0.045(8) 0.050(9) 0.056(11) -0.013(8) 0.003(7) 0.003(6) C84 0.031(8) 0.060(11) 0.037(9) -0.009(7) 0.004(6) -0.004(8) C85 0.036(8) 0.070(11) 0.064(10) -0.023(9) 0.008(7) -0.001(7) C86 0.032(9) 0.075(12) 0.027(9) -0.015(8) -0.020(6) 0.013(8) C91 0.080(17) 0.049(10) 0.052(14) 0.007(9) -0.008(11) -0.021(10) C92 0.074(14) 0.040(11) 0.066(14) 0.023(11) 0.037(12) 0.031(10) C93 0.054(12) 0.089(15) 0.065(13) 0.034(11) 0.024(9) 0.032(11) C94 0.029(9) 0.108(17) 0.134(17) -0.050(12) 0.003(10) 0.011(10) C95 0.097(14) 0.18(2) 0.022(12) -0.012(13) -0.006(11) 0.071(13) C96 0.024(9) 0.113(19) 0.075(14) 0.000(12) 0.013(9) 0.036(10) C101 0.047(11) 0.028(8) 0.069(12) 0.014(8) 0.026(9) 0.004(7) C102 0.024(8) 0.078(13) 0.060(14) 0.022(11) 0.032(8) 0.014(8) C103 0.017(8) 0.060(12) 0.069(12) 0.028(9) -0.016(8) 0.008(7) C104 0.018(7) 0.095(16) 0.064(15) 0.019(11) -0.009(8) -0.004(9) C105 0.043(9) 0.099(18) 0.030(10) 0.010(12) -0.010(8) 0.014(10) C106 0.065(13) 0.094(14) 0.023(9) -0.010(9) 0.020(7) 0.025(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 Cu1 N1 2.023(4) . y Cu1 N32 2.041(4) . y Cu1 N31 2.096(4) . y Cu1 N2 2.098(3) . y N1 N1 1.315(7) 4_566 ? N1 C2 1.351(5) . ? C2 C3 1.393(6) . ? C2 C6 1.457(6) . ? C3 C3 1.357(9) 4_566 ? C3 H3 0.9500 . ? C6 N2 1.278(5) . ? C6 H6 0.9500 . ? N2 C8 1.421(5) . ? C8 C9 1.397(7) . ? C8 C13 1.403(6) . ? C9 C10 1.375(7) . ? C9 H9 0.9500 . ? C10 C11 1.373(9) . ? C10 H10 0.9500 . ? C11 C12 1.391(8) . ? C11 H11 0.9500 . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 C14 1.488(6) . ? C14 C19 1.369(7) . ? C14 C15 1.395(6) . ? C15 C16 1.375(7) . ? C15 H15 0.9500 . ? C16 C17 1.363(8) . ? C16 H16 0.9500 . ? C17 C18 1.386(7) . ? C17 H17 0.9500 . ? C18 C19 1.393(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? N31 C32 1.301(5) . ? N31 N31 1.342(9) 4_566 ? C32 C33 1.367(6) . ? C32 C36 1.455(6) . ? C33 C33 1.361(9) 4_566 ? C33 H33 0.9500 . ? C36 N32 1.285(5) . ? C36 H36 0.9500 . ? N32 C38 1.419(6) . ? C38 C39 1.396(7) . ? C38 C43 1.407(7) . ? C39 C40 1.398(8) . ? C39 H39 0.9500 . ? C40 C41 1.394(9) . ? C40 H40 0.9500 . ? C41 C42 1.364(8) . ? C41 H41 0.9500 . ? C42 C43 1.396(7) . ? C42 H42 0.9500 . ? C43 C44 1.483(7) . ? C44 C45 1.397(7) . ? C44 C49 1.403(7) . ? C45 C46 1.388(7) . ? C45 H45 0.9500 . ? C46 C47 1.377(7) . ? C46 H46 0.9500 . ? C47 C48 1.390(6) . ? C47 H47 0.9500 . ? C48 C49 1.387(7) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? P1 F11 1.541(3) . ? P1 F15 1.570(4) . ? P1 F16 1.576(3) . ? P1 F12 1.578(3) . ? P1 F13 1.590(3) . ? P1 F14 1.593(3) . ? C51 C51 1.327(10) 3_656 ? C51 C52 1.355(9) . ? C51 H51 0.9500 . ? C52 C53 1.362(10) . ? C52 H52 0.9500 . ? C53 C53 1.392(16) 3_656 ? C53 H53 0.9500 . ? C61 C62 1.362(10) 3_656 ? C61 C62 1.362(10) . ? C61 H61 0.9500 . ? C62 C63 1.328(10) . ? C62 H62 0.9500 . ? C63 C64 1.352(9) . ? C63 H63 0.9500 . ? C64 C63 1.352(9) 3_656 ? C64 H64 0.9500 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C71 H71 0.9500 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C81 H81 0.9500 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 C86 1.3900 . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 H91 0.9500 . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C101 H101 0.9500 . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 C104 1.3900 . ? C103 H103 0.9500 . ? C104 C105 1.3900 . ? C104 H104 0.9500 . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N32 161.15(16) . . y N1 Cu1 N31 105.36(14) . . y N32 Cu1 N31 76.80(15) . . y N1 Cu1 N2 79.16(15) . . y N32 Cu1 N2 106.08(15) . . y N31 Cu1 N2 157.8(2) . . y N1 N1 C2 120.2(3) 4_566 . ? N1 N1 Cu1 126.08(15) 4_566 . ? C2 N1 Cu1 112.7(3) . . ? N1 C2 C3 121.3(4) . . ? N1 C2 C6 114.6(4) . . ? C3 C2 C6 124.0(4) . . ? C3 C3 C2 118.3(3) 4_566 . ? C3 C3 H3 120.9 4_566 . ? C2 C3 H3 120.9 . . ? N2 C6 C2 118.2(4) . . ? N2 C6 H6 120.9 . . ? C2 C6 H6 120.9 . . ? C6 N2 C8 121.1(4) . . ? C6 N2 Cu1 111.3(3) . . ? C8 N2 Cu1 126.5(3) . . ? C9 C8 C13 121.1(5) . . ? C9 C8 N2 120.7(5) . . ? C13 C8 N2 118.1(4) . . ? C10 C9 C8 119.9(6) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.4(6) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 121.3(6) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 117.4(5) . . ? C12 C13 C14 120.5(5) . . ? C8 C13 C14 122.1(4) . . ? C19 C14 C15 118.3(5) . . ? C19 C14 C13 123.3(4) . . ? C15 C14 C13 118.4(5) . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 121.2(5) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 119.8(6) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C14 C19 C18 121.0(5) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C32 N31 N31 120.4(3) . 4_566 ? C32 N31 Cu1 114.4(4) . . ? N31 N31 Cu1 124.38(18) 4_566 . ? N31 C32 C33 121.3(5) . . ? N31 C32 C36 113.1(4) . . ? C33 C32 C36 125.5(4) . . ? C33 C33 C32 118.3(3) 4_566 . ? C33 C33 H33 120.9 4_566 . ? C32 C33 H33 120.9 . . ? N32 C36 C32 118.0(4) . . ? N32 C36 H36 121.0 . . ? C32 C36 H36 121.0 . . ? C36 N32 C38 121.8(4) . . ? C36 N32 Cu1 114.5(3) . . ? C38 N32 Cu1 123.3(3) . . ? C39 C38 C43 121.6(5) . . ? C39 C38 N32 120.4(5) . . ? C43 C38 N32 117.9(4) . . ? C38 C39 C40 119.0(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C41 C40 C39 120.0(6) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 119.8(6) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 122.7(6) . . ? C41 C42 H42 118.6 . . ? C43 C42 H42 118.6 . . ? C42 C43 C38 116.8(5) . . ? C42 C43 C44 120.1(5) . . ? C38 C43 C44 123.0(4) . . ? C45 C44 C49 117.8(5) . . ? C45 C44 C43 119.5(5) . . ? C49 C44 C43 122.7(4) . . ? C46 C45 C44 121.2(5) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C47 C46 C45 120.5(5) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 119.1(5) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C49 C48 C47 121.0(5) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 C44 120.4(4) . . ? C48 C49 H49 119.8 . . ? C44 C49 H49 119.8 . . ? F11 P1 F15 92.2(2) . . ? F11 P1 F16 179.3(2) . . ? F15 P1 F16 88.5(2) . . ? F11 P1 F12 90.7(2) . . ? F15 P1 F12 91.7(2) . . ? F16 P1 F12 89.3(2) . . ? F11 P1 F13 90.2(2) . . ? F15 P1 F13 177.3(2) . . ? F16 P1 F13 89.0(2) . . ? F12 P1 F13 89.36(19) . . ? F11 P1 F14 90.7(2) . . ? F15 P1 F14 89.0(2) . . ? F16 P1 F14 89.4(2) . . ? F12 P1 F14 178.5(2) . . ? F13 P1 F14 89.89(18) . . ? C51 C51 C52 121.3(4) 3_656 . ? C51 C51 H51 119.3 3_656 . ? C52 C51 H51 119.3 . . ? C51 C52 C53 119.1(7) . . ? C51 C52 H52 120.4 . . ? C53 C52 H52 120.4 . . ? C52 C53 C53 119.6(5) . 3_656 ? C52 C53 H53 120.2 . . ? C53 C53 H53 120.2 3_656 . ? C62 C61 C62 119.1(12) 3_656 . ? C62 C61 H61 120.4 3_656 . ? C62 C61 H61 120.4 . . ? C63 C62 C61 120.2(9) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C62 C63 C64 120.5(8) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C63 119.5(10) . 3_656 ? C63 C64 H64 120.2 . . ? C63 C64 H64 120.2 3_656 . ? C72 C71 C76 120.0 . . ? C72 C71 H71 120.0 . . ? C76 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? C82 C81 C86 120.0 . . ? C82 C81 H81 120.0 . . ? C86 C81 H81 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C81 120.0 . . ? C85 C86 H86 120.0 . . ? C81 C86 H86 120.0 . . ? C92 C91 C96 120.0 . . ? C92 C91 H91 120.0 . . ? C96 C91 H91 120.0 . . ? C93 C92 C91 120.0 . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C92 C93 C94 120.0 . . ? C92 C93 H93 120.0 . . ? C94 C93 H93 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C102 C101 C106 120.0 . . ? C102 C101 H101 120.0 . . ? C106 C101 H101 120.0 . . ? C101 C102 C103 120.0 . . ? C101 C102 H102 120.0 . . ? C103 C102 H102 120.0 . . ? C104 C103 C102 120.0 . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C106 C105 C104 120.0 . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C105 C106 C101 120.0 . . ? C105 C106 H106 120.0 . . ? C101 C106 H106 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N32 Cu1 N1 N1 -77.8(7) . . . 4_566 ? N31 Cu1 N1 N1 16.3(6) . . . 4_566 ? N2 Cu1 N1 N1 174.0(6) . . . 4_566 ? N32 Cu1 N1 C2 90.9(5) . . . . ? N31 Cu1 N1 C2 -175.0(4) . . . . ? N2 Cu1 N1 C2 -17.3(3) . . . . ? N1 N1 C2 C3 3.2(8) 4_566 . . . ? Cu1 N1 C2 C3 -166.2(4) . . . . ? N1 N1 C2 C6 -174.7(5) 4_566 . . . ? Cu1 N1 C2 C6 15.9(5) . . . . ? N1 C2 C3 C3 1.9(9) . . . 4_566 ? C6 C2 C3 C3 179.5(5) . . . 4_566 ? N1 C2 C6 N2 -1.6(6) . . . . ? C3 C2 C6 N2 -179.4(5) . . . . ? C2 C6 N2 C8 177.9(4) . . . . ? C2 C6 N2 Cu1 -12.9(5) . . . . ? N1 Cu1 N2 C6 16.4(3) . . . . ? N32 Cu1 N2 C6 -145.0(3) . . . . ? N31 Cu1 N2 C6 120.6(4) . . . . ? N1 Cu1 N2 C8 -175.2(4) . . . . ? N32 Cu1 N2 C8 23.5(4) . . . . ? N31 Cu1 N2 C8 -71.0(6) . . . . ? C6 N2 C8 C9 41.5(7) . . . . ? Cu1 N2 C8 C9 -125.8(5) . . . . ? C6 N2 C8 C13 -143.1(5) . . . . ? Cu1 N2 C8 C13 49.6(6) . . . . ? C13 C8 C9 C10 1.0(9) . . . . ? N2 C8 C9 C10 176.3(6) . . . . ? C8 C9 C10 C11 1.1(11) . . . . ? C9 C10 C11 C12 -1.5(12) . . . . ? C10 C11 C12 C13 -0.3(11) . . . . ? C11 C12 C13 C8 2.3(8) . . . . ? C11 C12 C13 C14 -177.6(5) . . . . ? C9 C8 C13 C12 -2.7(8) . . . . ? N2 C8 C13 C12 -178.1(5) . . . . ? C9 C8 C13 C14 177.2(5) . . . . ? N2 C8 C13 C14 1.9(7) . . . . ? C12 C13 C14 C19 -133.8(6) . . . . ? C8 C13 C14 C19 46.3(7) . . . . ? C12 C13 C14 C15 47.0(7) . . . . ? C8 C13 C14 C15 -132.9(5) . . . . ? C19 C14 C15 C16 -1.1(8) . . . . ? C13 C14 C15 C16 178.1(5) . . . . ? C14 C15 C16 C17 0.3(8) . . . . ? C15 C16 C17 C18 1.5(9) . . . . ? C16 C17 C18 C19 -2.6(9) . . . . ? C15 C14 C19 C18 0.0(8) . . . . ? C13 C14 C19 C18 -179.2(5) . . . . ? C17 C18 C19 C14 1.8(9) . . . . ? N1 Cu1 N31 C32 -176.7(5) . . . . ? N32 Cu1 N31 C32 -16.0(5) . . . . ? N2 Cu1 N31 C32 84.3(6) . . . . ? N1 Cu1 N31 N31 14.2(9) . . . 4_566 ? N32 Cu1 N31 N31 174.9(9) . . . 4_566 ? N2 Cu1 N31 N31 -84.9(9) . . . 4_566 ? N31 N31 C32 C33 1.6(12) 4_566 . . . ? Cu1 N31 C32 C33 -168.0(4) . . . . ? N31 N31 C32 C36 -175.3(8) 4_566 . . . ? Cu1 N31 C32 C36 15.1(6) . . . . ? N31 C32 C33 C33 2.1(9) . . . 4_566 ? C36 C32 C33 C33 178.6(6) . . . 4_566 ? N31 C32 C36 N32 -3.2(7) . . . . ? C33 C32 C36 N32 -179.9(5) . . . . ? C32 C36 N32 C38 176.6(4) . . . . ? C32 C36 N32 Cu1 -10.7(5) . . . . ? N1 Cu1 N32 C36 112.9(5) . . . . ? N31 Cu1 N32 C36 14.0(4) . . . . ? N2 Cu1 N32 C36 -143.3(3) . . . . ? N1 Cu1 N32 C38 -74.6(6) . . . . ? N31 Cu1 N32 C38 -173.5(4) . . . . ? N2 Cu1 N32 C38 29.3(4) . . . . ? C36 N32 C38 C39 40.3(7) . . . . ? Cu1 N32 C38 C39 -131.7(4) . . . . ? C36 N32 C38 C43 -142.1(5) . . . . ? Cu1 N32 C38 C43 45.9(6) . . . . ? C43 C38 C39 C40 1.1(8) . . . . ? N32 C38 C39 C40 178.5(5) . . . . ? C38 C39 C40 C41 0.3(9) . . . . ? C39 C40 C41 C42 -1.3(11) . . . . ? C40 C41 C42 C43 0.9(11) . . . . ? C41 C42 C43 C38 0.4(10) . . . . ? C41 C42 C43 C44 -178.7(6) . . . . ? C39 C38 C43 C42 -1.4(8) . . . . ? N32 C38 C43 C42 -178.9(5) . . . . ? C39 C38 C43 C44 177.7(5) . . . . ? N32 C38 C43 C44 0.2(7) . . . . ? C42 C43 C44 C45 40.2(7) . . . . ? C38 C43 C44 C45 -138.9(5) . . . . ? C42 C43 C44 C49 -140.5(6) . . . . ? C38 C43 C44 C49 40.4(8) . . . . ? C49 C44 C45 C46 0.2(8) . . . . ? C43 C44 C45 C46 179.5(5) . . . . ? C44 C45 C46 C47 -2.7(8) . . . . ? C45 C46 C47 C48 3.0(8) . . . . ? C46 C47 C48 C49 -0.9(8) . . . . ? C47 C48 C49 C44 -1.6(8) . . . . ? C45 C44 C49 C48 1.9(7) . . . . ? C43 C44 C49 C48 -177.4(5) . . . . ? C51 C51 C52 C53 -0.4(11) 3_656 . . . ? C51 C52 C53 C53 1.6(13) . . . 3_656 ? C62 C61 C62 C63 0.4(5) 3_656 . . . ? C61 C62 C63 C64 -0.8(10) . . . . ? C62 C63 C64 C63 0.4(5) . . . 3_656 ? C76 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? C86 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C86 0.0 . . . . ? C84 C85 C86 C81 0.0 . . . . ? C82 C81 C86 C85 0.0 . . . . ? C96 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C92 C91 C96 C95 0.0 . . . . ? C106 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C101 0.0 . . . . ? C102 C101 C106 C105 0.0 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.783 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.071 data_g6 _database_code_depnum_ccdc_archive 'CCDC 629025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 N4' _chemical_formula_weight 370.49 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5883(2) _cell_length_b 9.9822(2) _cell_length_c 24.5153(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.4910(10) _cell_angle_gamma 90.00 _cell_volume 2078.66(8) _cell_formula_units_Z 4 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.144 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Bruker SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17964 _diffrn_reflns_av_R_equivalents 0.1501 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.43 _reflns_number_total 3802 _reflns_number_gt 2057 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-H ANIS. All H's calc and ride. No disorder. No solvent. ; _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^)+(0.0812P)^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_number_reflns 3802 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1512 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 N1 N 0.2861(4) 0.4535(3) 0.00084(13) 0.0483(10) Uani 1 1 d . . . N2 N 0.1885(4) 0.5095(3) 0.03285(13) 0.0481(10) Uani 1 1 d . . . C2 C 0.1486(4) 0.4407(3) 0.07567(13) 0.0297(8) Uani 1 1 d . . . C3 C 0.2007(4) 0.3095(3) 0.08788(13) 0.0279(8) Uani 1 1 d . . . H3 H 0.1693 0.2618 0.1180 0.033 Uiso 1 1 calc R . . C4 C 0.2976(4) 0.2526(3) 0.05521(14) 0.0292(9) Uani 1 1 d . . . H4 H 0.3354 0.1637 0.0617 0.035 Uiso 1 1 calc R . . C5 C 0.3399(4) 0.3285(3) 0.01182(14) 0.0297(9) Uani 1 1 d . . . C6 C 0.4503(4) 0.2801(3) -0.02421(14) 0.0340(9) Uani 1 1 d . . . H6 H 0.4730 0.3355 -0.0536 0.041 Uiso 1 1 calc R . . N3 N 0.5156(4) 0.1672(3) -0.01721(12) 0.0309(7) Uani 1 1 d . . . C8 C 0.6273(4) 0.1300(3) -0.05243(13) 0.0258(8) Uani 1 1 d . . . C9 C 0.5773(4) 0.0828(3) -0.10689(13) 0.0278(8) Uani 1 1 d . . . C10 C 0.6924(4) 0.0479(3) -0.13851(14) 0.0276(8) Uani 1 1 d . . . H10 H 0.6606 0.0162 -0.1750 0.033 Uiso 1 1 calc R . . C11 C 0.8530(4) 0.0575(3) -0.11887(13) 0.0263(8) Uani 1 1 d . . . C12 C 0.8980(4) 0.1016(3) -0.06427(13) 0.0264(8) Uani 1 1 d . . . H12 H 1.0067 0.1077 -0.0500 0.032 Uiso 1 1 calc R . . C13 C 0.7876(4) 0.1363(3) -0.03074(14) 0.0274(8) Uani 1 1 d . . . C31 C 0.4047(4) 0.0667(3) -0.12803(15) 0.0379(10) Uani 1 1 d . . . H31A H 0.3577 0.1549 -0.1370 0.045 Uiso 1 1 calc R . . H31B H 0.3524 0.0241 -0.0996 0.045 Uiso 1 1 calc R . . H31C H 0.3916 0.0106 -0.1612 0.045 Uiso 1 1 calc R . . C32 C 0.9765(4) 0.0222(3) -0.15477(14) 0.0337(9) Uani 1 1 d . . . H32A H 1.0191 -0.0670 -0.1448 0.040 Uiso 1 1 calc R . . H32B H 1.0617 0.0884 -0.1491 0.040 Uiso 1 1 calc R . . H32C H 0.9285 0.0224 -0.1936 0.040 Uiso 1 1 calc R . . C33 C 0.8375(5) 0.1838(3) 0.02808(13) 0.0323(9) Uani 1 1 d . . . H33A H 0.9453 0.1539 0.0410 0.039 Uiso 1 1 calc R . . H33B H 0.7663 0.1464 0.0519 0.039 Uiso 1 1 calc R . . H33C H 0.8331 0.2819 0.0293 0.039 Uiso 1 1 calc R . . C16 C 0.0434(4) 0.5141(3) 0.10751(14) 0.0331(9) Uani 1 1 d . . . H16 H 0.0103 0.6018 0.0962 0.040 Uiso 1 1 calc R . . N4 N -0.0040(3) 0.4643(3) 0.14919(11) 0.0287(7) Uani 1 1 d . . . C18 C -0.1054(4) 0.5438(3) 0.17764(13) 0.0265(8) Uani 1 1 d . . . C19 C -0.0412(4) 0.6458(3) 0.21477(14) 0.0295(9) Uani 1 1 d . . . C20 C -0.1448(4) 0.7186(3) 0.24217(13) 0.0286(9) Uani 1 1 d . . . H20 H -0.1036 0.7887 0.2663 0.034 Uiso 1 1 calc R . . C21 C -0.3051(5) 0.6933(3) 0.23570(14) 0.0300(9) Uani 1 1 d . . . C22 C -0.3630(4) 0.5895(3) 0.19935(13) 0.0287(8) Uani 1 1 d . . . H22 H -0.4725 0.5702 0.1942 0.034 Uiso 1 1 calc R . . C23 C -0.2660(4) 0.5147(3) 0.17089(13) 0.0274(8) Uani 1 1 d . . . C41 C 0.1330(4) 0.6715(3) 0.22510(15) 0.0366(10) Uani 1 1 d . . . H41A H 0.1570 0.7361 0.2553 0.044 Uiso 1 1 calc R . . H41B H 0.1668 0.7079 0.1916 0.044 Uiso 1 1 calc R . . H41C H 0.1888 0.5874 0.2351 0.044 Uiso 1 1 calc R . . C42 C -0.4145(5) 0.7737(3) 0.26597(15) 0.0367(9) Uani 1 1 d . . . H42A H -0.4472 0.7189 0.2955 0.044 Uiso 1 1 calc R . . H42B H -0.5074 0.8004 0.2401 0.044 Uiso 1 1 calc R . . H42C H -0.3597 0.8538 0.2820 0.044 Uiso 1 1 calc R . . C43 C -0.3326(4) 0.4028(3) 0.13199(14) 0.0334(9) Uani 1 1 d . . . H43A H -0.3197 0.4263 0.0941 0.040 Uiso 1 1 calc R . . H43B H -0.4447 0.3909 0.1343 0.040 Uiso 1 1 calc R . . H43C H -0.2761 0.3193 0.1425 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.078(3) 0.0227(17) 0.050(2) 0.0135(15) 0.0317(19) 0.0187(17) N2 0.078(3) 0.0280(18) 0.046(2) 0.0135(15) 0.0316(19) 0.0210(17) C2 0.044(2) 0.0173(18) 0.0287(19) 0.0029(15) 0.0086(17) 0.0004(16) C3 0.041(2) 0.0163(18) 0.0250(18) 0.0041(14) 0.0017(17) -0.0006(16) C4 0.042(2) 0.0134(17) 0.0317(19) -0.0018(15) 0.0045(17) 0.0000(15) C5 0.042(2) 0.0145(17) 0.032(2) 0.0014(15) 0.0036(18) 0.0039(15) C6 0.052(3) 0.0199(19) 0.031(2) 0.0026(16) 0.0083(18) 0.0006(18) N3 0.042(2) 0.0151(15) 0.0348(17) 0.0025(13) 0.0040(15) 0.0032(13) C8 0.038(2) 0.0101(16) 0.0313(19) 0.0046(14) 0.0103(17) 0.0037(15) C9 0.039(2) 0.0131(17) 0.0309(19) 0.0066(15) 0.0049(17) 0.0001(15) C10 0.041(2) 0.0154(17) 0.0258(18) 0.0028(15) 0.0016(17) -0.0010(15) C11 0.041(2) 0.0087(16) 0.0291(19) -0.0019(14) 0.0068(17) 0.0013(15) C12 0.035(2) 0.0142(17) 0.0286(19) 0.0026(14) -0.0012(16) -0.0020(15) C13 0.041(2) 0.0063(16) 0.035(2) 0.0023(14) 0.0062(18) 0.0027(15) C31 0.047(3) 0.027(2) 0.038(2) 0.0006(17) 0.0016(19) -0.0030(18) C32 0.050(3) 0.0209(18) 0.0293(19) 0.0019(16) 0.0014(18) -0.0009(17) C33 0.052(3) 0.0154(17) 0.0290(19) -0.0008(15) 0.0035(18) 0.0017(16) C16 0.050(3) 0.0165(18) 0.033(2) 0.0055(16) 0.0060(18) 0.0039(16) N4 0.0399(19) 0.0201(15) 0.0260(15) 0.0010(13) 0.0040(14) 0.0032(13) C18 0.041(2) 0.0163(17) 0.0234(18) 0.0038(15) 0.0075(16) 0.0063(16) C19 0.040(2) 0.0200(19) 0.0274(19) 0.0064(15) 0.0021(17) 0.0021(16) C20 0.046(3) 0.0146(17) 0.0256(19) -0.0005(14) 0.0057(17) 0.0004(16) C21 0.048(3) 0.0163(18) 0.0268(19) 0.0060(15) 0.0082(17) 0.0075(16) C22 0.038(2) 0.0224(19) 0.0259(19) 0.0054(15) 0.0052(16) -0.0014(16) C23 0.043(2) 0.0137(17) 0.0253(18) 0.0046(14) 0.0055(17) 0.0038(16) C41 0.048(3) 0.0228(19) 0.037(2) -0.0027(17) -0.0001(19) 0.0001(17) C42 0.053(3) 0.0236(19) 0.034(2) -0.0023(16) 0.0072(18) 0.0075(18) C43 0.048(3) 0.0231(19) 0.0283(19) -0.0025(16) 0.0037(18) -0.0040(17) _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 N1 C5 1.344(4) . ? N1 N2 1.351(4) . ? N2 C2 1.340(4) . ? C2 C3 1.402(4) . ? C2 C16 1.473(5) . ? C3 C4 1.362(4) . ? C3 H3 0.9500 . ? C4 C5 1.397(4) . ? C4 H4 0.9500 . ? C5 C6 1.470(5) . ? C6 N3 1.259(4) . ? C6 H6 0.9500 . ? N3 C8 1.431(4) . ? C8 C13 1.402(5) . ? C8 C9 1.421(4) . ? C9 C10 1.387(5) . ? C9 C31 1.505(5) . ? C10 C11 1.396(5) . ? C10 H10 0.9500 . ? C11 C12 1.408(4) . ? C11 C32 1.516(5) . ? C12 C13 1.387(4) . ? C12 H12 0.9500 . ? C13 C33 1.518(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C16 N4 1.257(4) . ? C16 H16 0.9500 . ? N4 C18 1.433(4) . ? C18 C23 1.395(5) . ? C18 C19 1.422(5) . ? C19 C20 1.396(4) . ? C19 C41 1.502(5) . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.409(5) . ? C21 C42 1.510(5) . ? C22 C23 1.382(4) . ? C22 H22 0.9500 . ? C23 C43 1.524(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N1 N2 119.5(3) . . ? C2 N2 N1 119.7(3) . . ? N2 C2 C3 122.4(3) . . ? N2 C2 C16 114.1(3) . . ? C3 C2 C16 123.5(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 118.2(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 122.9(3) . . ? N3 C6 C5 121.7(3) . . ? N3 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 N3 C8 118.3(3) . . ? C13 C8 C9 121.0(3) . . ? C13 C8 N3 117.9(3) . . ? C9 C8 N3 121.1(3) . . ? C10 C9 C8 117.8(3) . . ? C10 C9 C31 121.8(3) . . ? C8 C9 C31 120.3(3) . . ? C9 C10 C11 122.6(3) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 117.9(3) . . ? C10 C11 C32 121.6(3) . . ? C12 C11 C32 120.5(3) . . ? C13 C12 C11 121.8(3) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C8 118.8(3) . . ? C12 C13 C33 121.3(3) . . ? C8 C13 C33 119.9(3) . . ? C9 C31 H31A 109.5 . . ? C9 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C9 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C11 C32 H32A 109.5 . . ? C11 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C11 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C16 C2 122.2(3) . . ? N4 C16 H16 118.9 . . ? C2 C16 H16 118.9 . . ? C16 N4 C18 118.0(3) . . ? C23 C18 C19 120.6(3) . . ? C23 C18 N4 119.2(3) . . ? C19 C18 N4 120.1(3) . . ? C20 C19 C18 117.8(3) . . ? C20 C19 C41 121.3(3) . . ? C18 C19 C41 120.9(3) . . ? C21 C20 C19 122.9(3) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C20 C21 C22 117.3(3) . . ? C20 C21 C42 121.8(3) . . ? C22 C21 C42 121.0(3) . . ? C23 C22 C21 122.3(3) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C18 119.1(3) . . ? C22 C23 C43 120.9(3) . . ? C18 C23 C43 120.0(3) . . ? C19 C41 H41A 109.5 . . ? C19 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C19 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C21 C42 H42A 109.5 . . ? C21 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C21 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C23 C43 H43A 109.5 . . ? C23 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C23 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 C2 1.2(6) . . . . ? N1 N2 C2 C3 -2.1(6) . . . . ? N1 N2 C2 C16 179.2(3) . . . . ? N2 C2 C3 C4 1.3(5) . . . . ? C16 C2 C3 C4 179.9(3) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? N2 N1 C5 C4 0.5(6) . . . . ? N2 N1 C5 C6 -177.6(3) . . . . ? C3 C4 C5 N1 -1.3(5) . . . . ? C3 C4 C5 C6 176.7(3) . . . . ? N1 C5 C6 N3 176.8(4) . . . . ? C4 C5 C6 N3 -1.3(6) . . . . ? C5 C6 N3 C8 -177.1(3) . . . . ? C6 N3 C8 C13 103.5(4) . . . . ? C6 N3 C8 C9 -79.1(4) . . . . ? C13 C8 C9 C10 -2.3(4) . . . . ? N3 C8 C9 C10 -179.6(3) . . . . ? C13 C8 C9 C31 175.3(3) . . . . ? N3 C8 C9 C31 -2.0(4) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C31 C9 C10 C11 -177.6(3) . . . . ? C9 C10 C11 C12 1.5(5) . . . . ? C9 C10 C11 C32 -178.3(3) . . . . ? C10 C11 C12 C13 -0.8(5) . . . . ? C32 C11 C12 C13 179.1(3) . . . . ? C11 C12 C13 C8 -1.5(5) . . . . ? C11 C12 C13 C33 -179.9(3) . . . . ? C9 C8 C13 C12 3.0(5) . . . . ? N3 C8 C13 C12 -179.6(3) . . . . ? C9 C8 C13 C33 -178.5(3) . . . . ? N3 C8 C13 C33 -1.1(4) . . . . ? N2 C2 C16 N4 -179.4(3) . . . . ? C3 C2 C16 N4 1.9(6) . . . . ? C2 C16 N4 C18 179.7(3) . . . . ? C16 N4 C18 C23 104.2(4) . . . . ? C16 N4 C18 C19 -79.4(4) . . . . ? C23 C18 C19 C20 -2.6(4) . . . . ? N4 C18 C19 C20 -178.8(3) . . . . ? C23 C18 C19 C41 175.9(3) . . . . ? N4 C18 C19 C41 -0.4(4) . . . . ? C18 C19 C20 C21 1.7(5) . . . . ? C41 C19 C20 C21 -176.8(3) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C19 C20 C21 C42 179.9(3) . . . . ? C20 C21 C22 C23 -0.1(5) . . . . ? C42 C21 C22 C23 179.7(3) . . . . ? C21 C22 C23 C18 -0.9(5) . . . . ? C21 C22 C23 C43 179.9(3) . . . . ? C19 C18 C23 C22 2.2(4) . . . . ? N4 C18 C23 C22 178.5(3) . . . . ? C19 C18 C23 C43 -178.5(3) . . . . ? N4 C18 C23 C43 -2.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.240 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.059 # Attachment 'op_dimethyl_Cu_complex_1.cif' data_jrp140 _database_code_depnum_ccdc_archive 'CCDC 629026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109 H110.30 Cu4 F24 N16 O0.65 P4' _chemical_formula_weight 2478.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 45.818(6) _cell_length_b 16.454(2) _cell_length_c 30.973(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.412(8) _cell_angle_gamma 90.00 _cell_volume 22889(6) _cell_formula_units_Z 8 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10188 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SCALE (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96561 _diffrn_reflns_av_R_equivalents 0.1817 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 19.78 _reflns_number_total 10308 _reflns_number_gt 6248 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-H ANIS with the exception of the disordered carbon atoms which were left isotropic. There are 3 full occupancy PF6 anions, plus one half a PF6 anion across a 2-fold axis, (P4 F41 F42 F43 F44) and a half occupancy PF6 anion (P5 F51 F52 F53 F54 F55 F56, made SAME as P1 F11 F12 F13 F14 F15 F16) completing the charge balance for the four Cu(I) cations. One of the Ph-Me2 groups on one of the four independent ligand strands is disordered over two sites (C108 C109 C110 C111 C112 C113 C114 C115 : C118 C119 C120 C121 C122 C123 C124 C125) with an occupancy of 65:35 and partial occupancy water O170 of solvation was acosiated with the first part (65% occ). All of the Ph-Me2 groups were made similar by DFIX on the similar C-C bond distances. There are three full occupancy benzene molecules of solvation and one half occupancy benzene (C161 C162 C163 C164 C165 C166) all of which were restrained with AFIX 66. H atoms inserted at calculated positions and ride on attached atoms, except with the H on the water (O170 H171 H172) which were found, HIMP?ed to 0.85\%A and then fixed xyz, ? riding on O(1.2x). Due to severe anisotropy (thin plate) restraints to anisotropic parameters were used (ISOR, SIMU, DELU) ; _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^)+(0.1180P)^2^+879.1896P] 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 10308 _refine_ls_number_parameters 1534 _refine_ls_number_restraints 2704 _refine_ls_R_factor_all 0.1557 _refine_ls_R_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.2805 _refine_ls_wR_factor_gt 0.2246 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 0.996 _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 0.14639(3) 1.01273(10) 0.85975(6) 0.0280(5) Uani 1 1 d U . . Cu2 Cu 0.12847(3) 1.17775(11) 0.93687(6) 0.0294(5) Uani 1 1 d U . . Cu3 Cu 0.12835(3) 0.83357(11) 0.92798(6) 0.0302(5) Uani 1 1 d U . . Cu4 Cu 0.12272(3) 0.99663(10) 1.01550(6) 0.0286(5) Uani 1 1 d U A . N1 N 0.1741(2) 1.0677(6) 0.9086(3) 0.023(2) Uani 1 1 d U . . N2 N 0.1683(2) 1.1251(6) 0.9357(3) 0.021(2) Uani 1 1 d U . . N3 N 0.1853(2) 0.9538(6) 0.8523(4) 0.025(2) Uani 1 1 d U . . N4 N 0.1541(2) 1.2422(7) 0.9882(4) 0.031(2) Uani 1 1 d U . . N31 N 0.1615(2) 0.8886(7) 0.9719(4) 0.028(2) Uani 1 1 d U . . N32 N 0.1600(2) 0.9461(7) 1.0018(4) 0.026(2) Uani 1 1 d U . . N33 N 0.1642(2) 0.7728(7) 0.9110(4) 0.029(2) Uani 1 1 d U . . N34 N 0.1531(2) 1.0558(7) 1.0630(4) 0.028(2) Uani 1 1 d U . . N61 N 0.1063(2) 0.9648(7) 0.8604(4) 0.025(2) Uani 1 1 d U . . N62 N 0.0999(2) 0.9042(7) 0.8850(4) 0.027(2) Uani 1 1 d U . . N63 N 0.1218(2) 1.0865(7) 0.8124(4) 0.027(2) Uani 1 1 d U . . N64 N 0.0887(3) 0.7773(7) 0.9341(4) 0.032(2) Uani 1 1 d U . . N91 N 0.0922(2) 1.1089(7) 0.9436(4) 0.025(2) Uani 1 1 d U . . N92 N 0.0902(2) 1.0487(7) 0.9711(4) 0.025(2) Uani 1 1 d U A . N93 N 0.0982(2) 1.2322(7) 0.8866(4) 0.030(2) Uani 1 1 d U A . N94 N 0.0874(3) 0.9259(7) 1.0265(4) 0.031(2) Uani 1 1 d U . . C2 C 0.1904(3) 1.1569(8) 0.9664(4) 0.025(2) Uani 1 1 d U . . C3 C 0.2200(3) 1.1310(8) 0.9719(4) 0.027(3) Uani 1 1 d U . . H3A H 0.2351 1.1522 0.9946 0.032 Uiso 1 1 calc R . . C4 C 0.2262(3) 1.0742(8) 0.9433(4) 0.026(3) Uani 1 1 d U . . H4A H 0.2460 1.0556 0.9451 0.032 Uiso 1 1 calc R . . C5 C 0.2030(3) 1.0427(8) 0.9109(4) 0.024(2) Uani 1 1 d U . . C6 C 0.2076(3) 0.9836(8) 0.8805(4) 0.025(3) Uani 1 1 d U . . H6A H 0.2272 0.9650 0.8805 0.030 Uiso 1 1 calc R . . C8 C 0.1919(3) 0.8912(8) 0.8237(4) 0.027(2) Uani 1 1 d DU . . C9 C 0.1768(3) 0.8851(8) 0.7801(4) 0.031(3) Uani 1 1 d DU . . C10 C 0.1852(3) 0.8265(8) 0.7540(5) 0.034(3) Uani 1 1 d DU . . H10A H 0.1746 0.8221 0.7244 0.040 Uiso 1 1 calc R . . C11 C 0.2087(3) 0.7724(8) 0.7685(4) 0.037(3) Uani 1 1 d DU . . C12 C 0.2229(3) 0.7773(8) 0.8123(4) 0.035(3) Uani 1 1 d DU . . H12A H 0.2383 0.7401 0.8236 0.042 Uiso 1 1 calc R . . C13 C 0.2148(3) 0.8353(8) 0.8391(5) 0.031(3) Uani 1 1 d DU . . H13A H 0.2249 0.8379 0.8690 0.037 Uiso 1 1 calc R . . C14 C 0.2185(4) 0.7108(9) 0.7383(5) 0.049(4) Uani 1 1 d DU . . H14A H 0.2376 0.6872 0.7527 0.059 Uiso 1 1 calc R . . H14B H 0.2208 0.7374 0.7109 0.059 Uiso 1 1 calc R . . H14C H 0.2036 0.6676 0.7317 0.059 Uiso 1 1 calc R . . C15 C 0.1512(3) 0.9423(8) 0.7617(5) 0.033(3) Uani 1 1 d DU . . H15A H 0.1427 0.9270 0.7312 0.040 Uiso 1 1 calc R . . H15B H 0.1587 0.9982 0.7624 0.040 Uiso 1 1 calc R . . H15C H 0.1359 0.9384 0.7796 0.040 Uiso 1 1 calc R . . C16 C 0.1815(3) 1.2200(8) 0.9942(4) 0.027(3) Uani 1 1 d U . . H16A H 0.1959 1.2447 1.0167 0.032 Uiso 1 1 calc R . . C18 C 0.1486(3) 1.3114(9) 1.0138(5) 0.041(3) Uani 1 1 d DU . . C19 C 0.1233(3) 1.3167(9) 1.0318(5) 0.048(3) Uani 1 1 d DU . . C20 C 0.1197(4) 1.3841(9) 1.0583(5) 0.050(3) Uani 1 1 d DU . . H20A H 0.1028 1.3874 1.0719 0.060 Uiso 1 1 calc R . . C21 C 0.1409(3) 1.4462(9) 1.0647(5) 0.055(3) Uani 1 1 d DU . . C22 C 0.1650(4) 1.4442(10) 1.0444(5) 0.055(3) Uani 1 1 d DU . . H22A H 0.1787 1.4882 1.0470 0.067 Uiso 1 1 calc R . . C23 C 0.1687(4) 1.3769(9) 1.0205(5) 0.051(3) Uani 1 1 d DU . . H23A H 0.1858 1.3740 1.0075 0.061 Uiso 1 1 calc R . . C24 C 0.1366(4) 1.5175(10) 1.0949(6) 0.070(5) Uani 1 1 d DU . . H24A H 0.1535 1.5196 1.1200 0.084 Uiso 1 1 calc R . . H24B H 0.1181 1.5100 1.1057 0.084 Uiso 1 1 calc R . . H24C H 0.1356 1.5685 1.0783 0.084 Uiso 1 1 calc R . . C25 C 0.1010(3) 1.2509(9) 1.0243(5) 0.051(4) Uani 1 1 d DU . . H25A H 0.1110 1.1986 1.0320 0.061 Uiso 1 1 calc R . . H25B H 0.0911 1.2504 0.9932 0.061 Uiso 1 1 calc R . . H25C H 0.0862 1.2600 1.0427 0.061 Uiso 1 1 calc R . . C32 C 0.1847(3) 0.9727(8) 1.0298(4) 0.027(2) Uani 1 1 d U . . C33 C 0.2127(3) 0.9415(8) 1.0259(5) 0.030(3) Uani 1 1 d U . . H33A H 0.2303 0.9603 1.0450 0.036 Uiso 1 1 calc R . . C34 C 0.2146(3) 0.8853(8) 0.9953(4) 0.029(3) Uani 1 1 d U . . H34A H 0.2335 0.8649 0.9924 0.035 Uiso 1 1 calc R . . C35 C 0.1890(3) 0.8567(8) 0.9680(4) 0.028(2) Uani 1 1 d U . . C36 C 0.1888(3) 0.7963(8) 0.9355(4) 0.030(3) Uani 1 1 d U . . H36A H 0.2071 0.7727 0.9317 0.036 Uiso 1 1 calc R . . C38 C 0.1666(3) 0.7072(8) 0.8813(4) 0.030(2) Uani 1 1 d DU . . C39 C 0.1492(3) 0.7067(8) 0.8388(4) 0.032(3) Uani 1 1 d DU . . C40 C 0.1548(3) 0.6462(8) 0.8104(5) 0.034(3) Uani 1 1 d DU . . H40A H 0.1444 0.6478 0.7807 0.041 Uiso 1 1 calc R . . C41 C 0.1747(3) 0.5833(8) 0.8234(4) 0.034(3) Uani 1 1 d DU . . C42 C 0.1895(3) 0.5823(9) 0.8668(4) 0.036(3) Uani 1 1 d DU . . H42A H 0.2025 0.5384 0.8770 0.044 Uiso 1 1 calc R . . C43 C 0.1860(3) 0.6419(8) 0.8953(5) 0.032(3) Uani 1 1 d DU . . H43A H 0.1966 0.6397 0.9249 0.038 Uiso 1 1 calc R . . C44 C 0.1806(4) 0.5195(9) 0.7907(5) 0.047(4) Uani 1 1 d DU . . H44A H 0.1664 0.5261 0.7629 0.057 Uiso 1 1 calc R . . H44B H 0.1784 0.4652 0.8027 0.057 Uiso 1 1 calc R . . H44C H 0.2009 0.5260 0.7856 0.057 Uiso 1 1 calc R . . C45 C 0.1265(3) 0.7711(8) 0.8229(5) 0.038(4) Uani 1 1 d DU . . H45A H 0.1210 0.7690 0.7907 0.045 Uiso 1 1 calc R . . H45B H 0.1349 0.8246 0.8321 0.045 Uiso 1 1 calc R . . H45C H 0.1088 0.7617 0.8356 0.045 Uiso 1 1 calc R . . C46 C 0.1800(3) 1.0315(8) 1.0608(4) 0.027(3) Uani 1 1 d U . . H46A H 0.1966 1.0538 1.0805 0.032 Uiso 1 1 calc R . . C48 C 0.1507(3) 1.1177(8) 1.0932(4) 0.032(2) Uani 1 1 d DU . . C49 C 0.1266(3) 1.1180(8) 1.1153(4) 0.034(3) Uani 1 1 d DU . . C50 C 0.1233(3) 1.1827(8) 1.1423(5) 0.038(3) Uani 1 1 d DU . . H50A H 0.1073 1.1816 1.1576 0.045 Uiso 1 1 calc R . . C51 C 0.1423(3) 1.2494(8) 1.1481(5) 0.040(3) Uani 1 1 d DU . . C52 C 0.1665(3) 1.2475(9) 1.1265(4) 0.038(3) Uani 1 1 d DU . . H52A H 0.1801 1.2916 1.1301 0.046 Uiso 1 1 calc R . . C53 C 0.1708(3) 1.1830(8) 1.1000(4) 0.034(3) Uani 1 1 d DU . . H53A H 0.1876 1.1828 1.0863 0.041 Uiso 1 1 calc R . . C54 C 0.1369(4) 1.3202(9) 1.1762(5) 0.055(4) Uani 1 1 d DU . . H54A H 0.1335 1.3002 1.2046 0.066 Uiso 1 1 calc R . . H54B H 0.1194 1.3505 1.1612 0.066 Uiso 1 1 calc R . . H54C H 0.1543 1.3560 1.1811 0.066 Uiso 1 1 calc R . . C55 C 0.1051(3) 1.0480(8) 1.1104(5) 0.040(4) Uani 1 1 d DU . . H55A H 0.0939 1.0497 1.1343 0.048 Uiso 1 1 calc R . . H55B H 0.1161 0.9967 1.1118 0.048 Uiso 1 1 calc R . . H55C H 0.0913 1.0520 1.0820 0.048 Uiso 1 1 calc R . . C62 C 0.0710(3) 0.8784(9) 0.8813(5) 0.030(2) Uani 1 1 d U . . C63 C 0.0476(3) 0.9152(9) 0.8515(5) 0.035(3) Uani 1 1 d U . . H63A H 0.0277 0.8966 0.8489 0.042 Uiso 1 1 calc R . . C64 C 0.0540(3) 0.9778(9) 0.8264(5) 0.035(3) Uani 1 1 d U . . H64A H 0.0388 1.0038 0.8058 0.042 Uiso 1 1 calc R . . C65 C 0.0841(3) 1.0036(8) 0.8318(4) 0.026(2) Uani 1 1 d U . . C66 C 0.0936(3) 1.0678(8) 0.8052(4) 0.029(3) Uani 1 1 d U . . H66A H 0.0796 1.0953 0.7833 0.034 Uiso 1 1 calc R . . C68 C 0.1331(3) 1.1458(8) 0.7867(4) 0.027(2) Uani 1 1 d DU . . C69 C 0.1244(3) 1.1541(8) 0.7416(4) 0.033(3) Uani 1 1 d DU . . C70 C 0.1396(3) 1.2111(8) 0.7217(5) 0.037(3) Uani 1 1 d DU . . H70A H 0.1350 1.2150 0.6904 0.044 Uiso 1 1 calc R . . C71 C 0.1611(3) 1.2630(8) 0.7444(4) 0.037(3) Uani 1 1 d DU . . C72 C 0.1686(3) 1.2542(8) 0.7891(4) 0.034(3) Uani 1 1 d DU . . H72A H 0.1835 1.2884 0.8056 0.041 Uiso 1 1 calc R . . C73 C 0.1552(3) 1.1969(8) 0.8100(5) 0.030(3) Uani 1 1 d DU . . H73A H 0.1609 1.1914 0.8411 0.036 Uiso 1 1 calc R . . C74 C 0.1765(4) 1.3235(10) 0.7193(5) 0.055(4) Uani 1 1 d DU . . H74A H 0.1819 1.3721 0.7374 0.066 Uiso 1 1 calc R . . H74B H 0.1630 1.3388 0.6919 0.066 Uiso 1 1 calc R . . H74C H 0.1945 1.2987 0.7125 0.066 Uiso 1 1 calc R . . C75 C 0.1018(3) 1.0999(9) 0.7131(5) 0.044(4) Uani 1 1 d DU . . H75A H 0.1032 1.0449 0.7255 0.052 Uiso 1 1 calc R . . H75B H 0.1058 1.0982 0.6832 0.052 Uiso 1 1 calc R . . H75C H 0.0817 1.1215 0.7122 0.052 Uiso 1 1 calc R . . C76 C 0.0667(3) 0.8104(9) 0.9074(5) 0.032(3) Uani 1 1 d U . . H76A H 0.0473 0.7887 0.9052 0.039 Uiso 1 1 calc R . . C78 C 0.0808(3) 0.7139(8) 0.9619(5) 0.033(2) Uani 1 1 d DU . . C79 C 0.0975(3) 0.6426(8) 0.9705(5) 0.036(3) Uani 1 1 d DU . . C80 C 0.0868(3) 0.5828(9) 0.9941(5) 0.039(3) Uani 1 1 d DU . . H80A H 0.0969 0.5322 0.9980 0.047 Uiso 1 1 calc R . . C81 C 0.0618(3) 0.5930(8) 1.0126(5) 0.044(3) Uani 1 1 d DU . . C82 C 0.0469(3) 0.6667(8) 1.0060(5) 0.039(3) Uani 1 1 d DU . . H82A H 0.0302 0.6760 1.0194 0.047 Uiso 1 1 calc R . . C83 C 0.0557(3) 0.7254(9) 0.9808(5) 0.036(3) Uani 1 1 d DU . . H83A H 0.0447 0.7748 0.9758 0.044 Uiso 1 1 calc R . . C84 C 0.0510(4) 0.5246(9) 1.0381(5) 0.055(4) Uani 1 1 d DU . . H84A H 0.0385 0.5468 1.0575 0.066 Uiso 1 1 calc R . . H84B H 0.0682 0.4966 1.0558 0.066 Uiso 1 1 calc R . . H84C H 0.0394 0.4860 1.0174 0.066 Uiso 1 1 calc R . . C85 C 0.1249(3) 0.6280(9) 0.9505(5) 0.040(4) Uani 1 1 d DU . . H85A H 0.1410 0.6646 0.9643 0.047 Uiso 1 1 calc R . . H85B H 0.1200 0.6386 0.9188 0.047 Uiso 1 1 calc R . . H85C H 0.1315 0.5715 0.9556 0.047 Uiso 1 1 calc R . . C92 C 0.0634(3) 1.0127(8) 0.9707(5) 0.030(2) Uani 1 1 d U . . C93 C 0.0380(3) 1.0382(9) 0.9419(5) 0.034(3) Uani 1 1 d U A . H93A H 0.0195 1.0116 0.9416 0.041 Uiso 1 1 calc R . . C94 C 0.0394(3) 1.1004(9) 0.9145(5) 0.034(3) Uani 1 1 d U . . H94A H 0.0222 1.1194 0.8949 0.041 Uiso 1 1 calc R A . C95 C 0.0679(3) 1.1372(8) 0.9156(5) 0.028(2) Uani 1 1 d U A . C96 C 0.0719(3) 1.2026(8) 0.8871(4) 0.027(3) Uani 1 1 d U . . H96A H 0.0550 1.2250 0.8680 0.033 Uiso 1 1 calc R A . C98 C 0.0997(3) 1.2922(8) 0.8544(4) 0.033(2) Uani 1 1 d DU . . C99 C 0.1184(3) 1.3604(8) 0.8629(4) 0.036(3) Uani 1 1 d DU A . C100 C 0.1171(3) 1.4176(9) 0.8304(4) 0.041(3) Uani 1 1 d DU . . H10B H 0.1289 1.4651 0.8368 0.049 Uiso 1 1 calc R A . C101 C 0.0996(3) 1.4103(9) 0.7890(5) 0.048(3) Uani 1 1 d DU A . C102 C 0.0824(3) 1.3413(8) 0.7806(5) 0.043(3) Uani 1 1 d DU . . H10C H 0.0703 1.3340 0.7522 0.051 Uiso 1 1 calc R A . C103 C 0.0821(3) 1.2828(9) 0.8120(4) 0.039(3) Uani 1 1 d DU A . H10D H 0.0701 1.2358 0.8051 0.046 Uiso 1 1 calc R . . C104 C 0.1004(4) 1.4732(10) 0.7542(5) 0.068(5) Uani 1 1 d DU . . H10E H 0.1068 1.5254 0.7682 0.082 Uiso 1 1 calc R A . H10F H 0.0805 1.4791 0.7358 0.082 Uiso 1 1 calc R . . H10G H 0.1144 1.4563 0.7357 0.082 Uiso 1 1 calc R . . C105 C 0.1371(3) 1.3735(10) 0.9076(4) 0.045(4) Uani 1 1 d DU . . H10H H 0.1476 1.4254 0.9081 0.054 Uiso 1 1 calc R A . H10I H 0.1516 1.3292 0.9144 0.054 Uiso 1 1 calc R . . H10J H 0.1243 1.3744 0.9295 0.054 Uiso 1 1 calc R . . C106 C 0.0632(3) 0.9485(8) 1.0011(5) 0.031(3) Uani 1 1 d U A . H10K H 0.0450 0.9221 1.0027 0.038 Uiso 1 1 calc R . . C108 C 0.0833(5) 0.8671(16) 1.0592(10) 0.033(3) Uani 0.65 1 d PDU A 1 C109 C 0.0601(5) 0.8727(15) 1.0821(7) 0.034(3) Uani 0.65 1 d PDU A 1 H10L H 0.0461 0.9157 1.0753 0.041 Uiso 0.65 1 calc PR A 1 C110 C 0.0569(5) 0.8180(11) 1.1141(7) 0.033(3) Uani 0.65 1 d PDU A 1 H11A H 0.0413 0.8254 1.1300 0.040 Uiso 0.65 1 calc PR A 1 C111 C 0.0759(5) 0.7516(12) 1.1240(8) 0.035(3) Uani 0.65 1 d PDU A 1 C112 C 0.0990(5) 0.7472(15) 1.1013(8) 0.035(3) Uani 0.65 1 d PDU A 1 H11B H 0.1119 0.7013 1.1060 0.042 Uiso 0.65 1 calc PR A 1 C113 C 0.1041(5) 0.8052(12) 1.0726(7) 0.034(3) Uani 0.65 1 d PDU A 1 C114 C 0.0715(5) 0.6875(13) 1.1567(7) 0.043(5) Uani 0.65 1 d PDU A 1 H11C H 0.0648 0.6369 1.1411 0.051 Uiso 0.65 1 calc PR A 1 H11D H 0.0564 0.7058 1.1730 0.051 Uiso 0.65 1 calc PR A 1 H11E H 0.0903 0.6779 1.1774 0.051 Uiso 0.65 1 calc PR A 1 C115 C 0.1302(5) 0.7949(14) 1.0491(8) 0.035(4) Uani 0.65 1 d PU A 1 H11F H 0.1230 0.8003 1.0172 0.042 Uiso 0.65 1 calc PR A 1 H11G H 0.1390 0.7411 1.0557 0.042 Uiso 0.65 1 calc PR A 1 H11H H 0.1451 0.8368 1.0592 0.042 Uiso 0.65 1 calc PR A 1 O170 O 0.0177(8) 0.983(2) 1.1514(11) 0.167(12) Uani 0.65 1 d PU B 1 H171 H 0.0097 0.9452 1.1642 0.200 Uiso 0.65 1 d P C 1 H172 H 0.0259 1.0236 1.1640 0.200 Uiso 0.65 1 d P D 1 C118 C 0.0913(10) 0.862(3) 1.0579(18) 0.033(3) Uani 0.35 1 d PDU A 2 C119 C 0.0706(9) 0.846(2) 1.0844(13) 0.035(3) Uani 0.35 1 d PDU A 2 C120 C 0.0758(9) 0.781(2) 1.1132(14) 0.035(3) Uani 0.35 1 d PDU A 2 H120 H 0.0628 0.7722 1.1332 0.042 Uiso 0.35 1 calc PR A 2 C121 C 0.0996(9) 0.728(2) 1.1139(14) 0.036(3) Uani 0.35 1 d PDU A 2 C122 C 0.1187(8) 0.736(2) 1.0848(12) 0.036(3) Uani 0.35 1 d PDU A 2 H122 H 0.1335 0.6972 1.0821 0.043 Uiso 0.35 1 calc PR A 2 C123 C 0.1147(10) 0.806(2) 1.0604(15) 0.034(4) Uani 0.35 1 d PDU A 2 H123 H 0.1292 0.8170 1.0432 0.041 Uiso 0.35 1 calc PR A 2 C124 C 0.1003(10) 0.657(2) 1.1457(13) 0.044(6) Uani 0.35 1 d PDU A 2 H12B H 0.1193 0.6572 1.1667 0.052 Uiso 0.35 1 calc PR A 2 H12C H 0.0980 0.6060 1.1293 0.052 Uiso 0.35 1 calc PR A 2 H12D H 0.0839 0.6631 1.1617 0.052 Uiso 0.35 1 calc PR A 2 C125 C 0.0488(9) 0.912(2) 1.0869(15) 0.039(6) Uani 0.35 1 d PDU A 2 H12E H 0.0547 0.9613 1.0727 0.047 Uiso 0.35 1 calc PR A 2 H12F H 0.0485 0.9242 1.1178 0.047 Uiso 0.35 1 calc PR A 2 H12G H 0.0289 0.8953 1.0718 0.047 Uiso 0.35 1 calc PR A 2 P1 P 0.26833(8) 1.1762(2) 1.09374(13) 0.0339(10) Uani 1 1 d DU . . F11 F 0.24304(16) 1.2377(5) 1.0689(3) 0.045(2) Uani 1 1 d DU . . F12 F 0.29276(18) 1.1146(5) 1.1174(3) 0.052(2) Uani 1 1 d DU . . F13 F 0.28113(17) 1.1700(5) 1.0495(2) 0.042(2) Uani 1 1 d DU . . F14 F 0.28983(16) 1.2519(5) 1.1092(3) 0.039(2) Uani 1 1 d DU . . F15 F 0.25513(19) 1.1834(5) 1.1368(3) 0.051(2) Uani 1 1 d DU . . F16 F 0.24675(17) 1.1025(5) 1.0772(3) 0.046(2) Uani 1 1 d DU . . P2 P 0.21089(9) 0.6745(3) 1.05374(16) 0.0493(12) Uani 1 1 d U . . F21 F 0.1916(2) 0.7559(6) 1.0470(3) 0.066(3) Uani 1 1 d U . . F22 F 0.2311(2) 0.5944(6) 1.0616(3) 0.065(3) Uani 1 1 d U . . F23 F 0.2051(2) 0.6670(6) 1.1019(3) 0.070(3) Uani 1 1 d U . . F24 F 0.2395(2) 0.7291(6) 1.0714(3) 0.075(3) Uani 1 1 d U . . F25 F 0.2175(2) 0.6849(6) 1.0054(3) 0.076(3) Uani 1 1 d U . . F26 F 0.1821(2) 0.6226(7) 1.0360(4) 0.089(3) Uani 1 1 d U . . P3 P 0.02279(11) 1.1491(3) 1.0484(2) 0.0691(14) Uani 1 1 d U . . F31 F -0.0057(2) 1.1415(6) 1.0707(3) 0.073(3) Uani 1 1 d U . . F32 F 0.0504(2) 1.1516(7) 1.0244(4) 0.084(3) Uani 1 1 d U . . F33 F 0.0235(3) 1.0531(7) 1.0434(4) 0.102(3) Uani 1 1 d U . . F34 F 0.0004(2) 1.1527(7) 1.0014(4) 0.091(3) Uani 1 1 d U . . F35 F 0.0211(2) 1.2445(6) 1.0483(4) 0.085(3) Uani 1 1 d U . . F36 F 0.0444(3) 1.1529(8) 1.0931(4) 0.104(3) Uani 1 1 d U . . P4 P 0.0000 0.8352(5) 1.2500 0.081(2) Uani 1 2 d SU . . F41 F -0.0167(2) 0.8366(7) 1.1993(4) 0.092(3) Uani 1 1 d U . . F42 F -0.0316(3) 0.8368(9) 1.2643(5) 0.121(4) Uani 1 1 d U . . F43 F 0.0000 0.7414(10) 1.2500 0.105(4) Uani 1 2 d SU . . F44 F 0.0000 0.9311(11) 1.2500 0.118(5) Uani 1 2 d SU . . P5 P 0.0522(3) 1.1375(7) 1.2267(4) 0.090(3) Uani 0.50 1 d PDU . . F51 F 0.0658(5) 1.2239(11) 1.2199(7) 0.110(5) Uani 0.50 1 d PDU . . F52 F 0.0382(5) 1.0501(11) 1.2308(8) 0.120(5) Uani 0.50 1 d PDU . . F53 F 0.0806(4) 1.1125(13) 1.2593(7) 0.096(5) Uani 0.50 1 d PDU . . F54 F 0.0351(5) 1.1714(14) 1.2630(7) 0.120(5) Uani 0.50 1 d PDU . . F55 F 0.0244(4) 1.1567(15) 1.1901(7) 0.122(5) Uani 0.50 1 d PDU . . F56 F 0.0686(5) 1.0983(14) 1.1928(7) 0.120(5) Uani 0.50 1 d PDU . . C131 C 0.27949(18) 1.0409(6) 0.8538(3) 0.043(3) Uani 1 1 d GU . . H13B H 0.2966 1.0335 0.8763 0.051 Uiso 1 1 calc R . . C132 C 0.2617(2) 1.1092(5) 0.8541(3) 0.043(3) Uani 1 1 d GU . . H13C H 0.2667 1.1485 0.8769 0.051 Uiso 1 1 calc R . . C133 C 0.2366(2) 1.1201(5) 0.8212(3) 0.044(3) Uani 1 1 d GU . . H13D H 0.2244 1.1668 0.8214 0.053 Uiso 1 1 calc R . . C134 C 0.22929(18) 1.0626(6) 0.7879(3) 0.048(3) Uani 1 1 d GU . . H13E H 0.2121 1.0700 0.7653 0.058 Uiso 1 1 calc R . . C135 C 0.2471(2) 0.9943(6) 0.7876(3) 0.048(3) Uani 1 1 d GU . . H13F H 0.2421 0.9550 0.7648 0.057 Uiso 1 1 calc R . . C136 C 0.2722(2) 0.9834(5) 0.8205(3) 0.047(3) Uani 1 1 d GU . . H13G H 0.2843 0.9367 0.8203 0.056 Uiso 1 1 calc R . . C141 C 0.2696(2) 0.5892(7) 0.8577(4) 0.060(3) Uani 1 1 d GU . . H14D H 0.2536 0.6155 0.8675 0.072 Uiso 1 1 calc R . . C142 C 0.2661(2) 0.5105(7) 0.8412(4) 0.064(3) Uani 1 1 d GU . . H14E H 0.2477 0.4829 0.8397 0.076 Uiso 1 1 calc R . . C143 C 0.2895(3) 0.4721(5) 0.8270(4) 0.070(4) Uani 1 1 d GU . . H14F H 0.2871 0.4183 0.8157 0.083 Uiso 1 1 calc R . . C144 C 0.3164(2) 0.5124(7) 0.8292(4) 0.067(4) Uani 1 1 d GU . . H14G H 0.3324 0.4862 0.8194 0.081 Uiso 1 1 calc R . . C145 C 0.3199(2) 0.5911(7) 0.8456(4) 0.066(3) Uani 1 1 d GU . . H14H H 0.3383 0.6187 0.8472 0.080 Uiso 1 1 calc R . . C146 C 0.2965(3) 0.6296(5) 0.8599(4) 0.062(3) Uani 1 1 d GU . . H14I H 0.2989 0.6834 0.8712 0.075 Uiso 1 1 calc R . . C151 C 0.0305(3) 1.3289(8) 0.9470(4) 0.087(4) Uani 1 1 d GU . . H15D H 0.0293 1.3060 0.9748 0.104 Uiso 1 1 calc R . . C152 C 0.0531(3) 1.3835(9) 0.9437(4) 0.096(4) Uani 1 1 d GU . . H15E H 0.0673 1.3980 0.9692 0.115 Uiso 1 1 calc R . . C153 C 0.0548(3) 1.4170(8) 0.9031(5) 0.100(4) Uani 1 1 d GU . . H153 H 0.0702 1.4544 0.9008 0.120 Uiso 1 1 calc R . . C154 C 0.0339(4) 1.3959(9) 0.8658(4) 0.098(4) Uani 1 1 d GU . . H15F H 0.0351 1.4188 0.8380 0.118 Uiso 1 1 calc R . . C155 C 0.0113(3) 1.3413(9) 0.8691(4) 0.101(4) Uani 1 1 d GU . . H15G H -0.0030 1.3269 0.8436 0.121 Uiso 1 1 calc R . . C156 C 0.0096(3) 1.3078(8) 0.9097(5) 0.091(4) Uani 1 1 d GU . . H15H H -0.0058 1.2705 0.9120 0.109 Uiso 1 1 calc R . . C161 C -0.0492(10) 1.328(3) 1.1835(12) 0.149(10) Uani 0.50 1 d PGU . . H16B H -0.0605 1.3169 1.2054 0.179 Uiso 0.50 1 calc PR . . C162 C -0.0223(10) 1.288(2) 1.1846(12) 0.149(10) Uani 0.50 1 d PGU . . H16C H -0.0152 1.2499 1.2072 0.178 Uiso 0.50 1 calc PR . . C163 C -0.0056(7) 1.304(2) 1.1526(15) 0.149(10) Uani 0.50 1 d PGU . . H16D H 0.0127 1.2773 1.1533 0.179 Uiso 0.50 1 calc PR . . C164 C -0.0159(9) 1.361(3) 1.1195(12) 0.149(10) Uani 0.50 1 d PGU . . H16E H -0.0046 1.3717 1.0976 0.178 Uiso 0.50 1 calc PR . . C165 C -0.0428(10) 1.400(2) 1.1184(12) 0.148(10) Uani 0.50 1 d PGU . . H16F H -0.0498 1.4387 1.0958 0.178 Uiso 0.50 1 calc PR . . C166 C -0.0594(7) 1.384(2) 1.1504(15) 0.149(10) Uani 0.50 1 d PGU . . H16G H -0.0778 1.4113 1.1497 0.179 Uiso 0.50 1 calc PR . . 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 0.0052(9) 0.0369(11) 0.0409(10) -0.0005(8) 0.0019(7) 0.0009(8) Cu2 0.0033(9) 0.0398(11) 0.0444(11) -0.0012(9) 0.0029(8) 0.0004(8) Cu3 0.0056(9) 0.0387(11) 0.0460(11) -0.0019(9) 0.0048(8) 0.0028(8) Cu4 0.0051(9) 0.0373(11) 0.0426(11) -0.0010(9) 0.0026(8) 0.0018(8) N1 0.010(4) 0.026(5) 0.034(5) 0.000(4) 0.009(4) -0.002(4) N2 0.008(4) 0.025(5) 0.030(5) 0.003(4) 0.007(4) -0.004(4) N3 0.011(5) 0.031(5) 0.035(5) 0.002(4) 0.010(4) 0.001(4) N4 0.013(4) 0.043(5) 0.035(5) 0.003(4) 0.001(4) 0.007(4) N31 0.014(4) 0.035(5) 0.036(5) 0.000(4) 0.006(4) 0.004(4) N32 0.013(4) 0.033(5) 0.032(5) 0.000(4) 0.004(4) -0.003(4) N33 0.013(5) 0.038(5) 0.038(5) 0.000(4) 0.009(4) 0.002(4) N34 0.018(5) 0.030(5) 0.037(5) 0.004(4) 0.006(4) 0.003(4) N61 0.009(4) 0.030(5) 0.035(5) -0.002(4) -0.001(4) 0.003(4) N62 0.010(4) 0.035(5) 0.034(5) -0.002(4) 0.004(4) 0.004(4) N63 0.015(4) 0.031(5) 0.034(5) -0.002(4) 0.000(4) 0.002(4) N64 0.021(5) 0.037(5) 0.040(5) -0.002(4) 0.008(4) 0.004(4) N91 0.009(4) 0.030(5) 0.038(5) -0.001(4) 0.007(4) 0.003(4) N92 0.011(4) 0.027(5) 0.038(5) -0.003(4) 0.005(4) 0.001(4) N93 0.015(5) 0.032(5) 0.041(5) 0.000(4) 0.005(4) -0.002(4) N94 0.024(4) 0.029(4) 0.039(4) -0.002(3) 0.006(4) -0.003(4) C2 0.014(4) 0.030(5) 0.031(5) 0.002(4) 0.002(4) -0.004(4) C3 0.012(4) 0.034(5) 0.034(5) 0.002(4) 0.003(4) -0.007(4) C4 0.009(5) 0.036(5) 0.035(5) 0.005(4) 0.007(4) -0.002(4) C5 0.011(4) 0.031(5) 0.032(5) 0.005(4) 0.005(4) 0.002(4) C6 0.012(5) 0.032(5) 0.033(5) 0.005(4) 0.007(4) 0.002(4) C8 0.014(5) 0.031(5) 0.037(4) 0.001(4) 0.011(4) 0.000(4) C9 0.018(5) 0.037(5) 0.040(5) -0.002(4) 0.010(4) 0.001(4) C10 0.023(5) 0.034(5) 0.042(5) -0.004(4) 0.003(4) 0.002(4) C11 0.023(5) 0.043(5) 0.045(5) -0.003(5) 0.008(5) 0.007(4) C12 0.017(5) 0.042(5) 0.047(5) -0.001(5) 0.008(4) 0.006(4) C13 0.014(5) 0.036(5) 0.043(5) 0.000(4) 0.007(4) 0.001(4) C14 0.043(7) 0.050(7) 0.054(7) -0.007(6) 0.007(6) 0.016(6) C15 0.015(6) 0.042(7) 0.045(7) -0.002(6) 0.010(5) 0.003(5) C16 0.011(5) 0.036(5) 0.032(5) 0.003(4) 0.004(4) -0.004(4) C18 0.033(5) 0.050(5) 0.040(5) 0.000(4) 0.005(4) 0.010(4) C19 0.040(5) 0.057(5) 0.046(5) 0.000(5) 0.006(4) 0.012(4) C20 0.042(6) 0.060(5) 0.048(6) 0.000(5) 0.007(5) 0.015(5) C21 0.048(6) 0.062(5) 0.052(6) 0.001(5) 0.006(5) 0.007(5) C22 0.051(6) 0.058(6) 0.054(6) -0.003(5) 0.003(5) 0.003(5) C23 0.048(6) 0.051(5) 0.049(6) -0.003(5) -0.002(5) 0.008(5) C24 0.062(8) 0.076(7) 0.072(8) -0.008(6) 0.012(6) 0.005(7) C25 0.040(7) 0.062(7) 0.056(8) -0.001(6) 0.018(6) 0.012(5) C32 0.014(4) 0.032(5) 0.035(5) 0.004(4) 0.005(4) 0.000(4) C33 0.011(4) 0.038(5) 0.040(5) 0.002(4) 0.004(4) -0.001(4) C34 0.012(5) 0.038(5) 0.037(5) 0.006(4) 0.004(4) 0.006(4) C35 0.015(4) 0.034(5) 0.036(5) 0.006(4) 0.003(4) 0.004(4) C36 0.015(5) 0.040(5) 0.036(5) 0.002(4) 0.009(4) 0.005(4) C38 0.018(5) 0.035(5) 0.039(4) 0.003(4) 0.011(4) -0.001(4) C39 0.021(5) 0.037(5) 0.040(5) -0.002(4) 0.012(4) -0.002(4) C40 0.022(5) 0.040(5) 0.042(5) -0.003(4) 0.012(5) -0.003(4) C41 0.022(5) 0.036(5) 0.048(5) -0.005(4) 0.014(5) -0.002(4) C42 0.024(5) 0.035(5) 0.051(5) -0.001(4) 0.012(5) 0.001(5) C43 0.020(5) 0.037(5) 0.040(5) 0.001(4) 0.010(4) -0.001(4) C44 0.042(7) 0.048(7) 0.052(7) -0.005(6) 0.006(6) 0.010(6) C45 0.027(7) 0.043(7) 0.044(7) 0.000(6) 0.007(5) 0.003(5) C46 0.015(5) 0.031(5) 0.036(5) 0.004(4) 0.007(4) -0.002(4) C48 0.025(5) 0.034(5) 0.035(5) 0.000(4) 0.002(4) 0.003(4) C49 0.024(5) 0.038(5) 0.038(5) 0.001(4) 0.003(4) 0.005(4) C50 0.031(5) 0.039(5) 0.042(5) 0.001(4) 0.006(5) 0.008(4) C51 0.035(5) 0.042(5) 0.043(5) -0.001(4) 0.006(4) 0.004(4) C52 0.031(5) 0.039(5) 0.043(6) 0.001(4) 0.001(4) 0.000(5) C53 0.024(5) 0.039(5) 0.038(5) 0.000(4) 0.002(4) -0.001(4) C54 0.054(8) 0.052(7) 0.057(7) -0.012(6) 0.007(6) 0.004(6) C55 0.029(7) 0.045(6) 0.048(7) -0.007(6) 0.014(6) 0.001(5) C62 0.014(4) 0.037(5) 0.041(5) 0.001(4) 0.007(4) 0.001(4) C63 0.015(5) 0.043(5) 0.046(5) 0.003(4) 0.002(4) -0.001(4) C64 0.016(4) 0.041(5) 0.045(5) 0.002(4) 0.000(4) 0.003(4) C65 0.013(4) 0.028(5) 0.035(5) -0.005(4) -0.004(4) 0.000(4) C66 0.016(5) 0.031(5) 0.035(5) -0.001(4) -0.005(4) 0.003(4) C68 0.017(5) 0.028(5) 0.035(4) 0.001(4) 0.002(4) 0.008(4) C69 0.028(5) 0.034(5) 0.037(5) -0.001(4) 0.002(4) 0.006(4) C70 0.034(5) 0.040(5) 0.036(5) 0.001(4) 0.006(4) 0.009(4) C71 0.034(5) 0.038(5) 0.042(5) 0.005(5) 0.012(5) 0.003(4) C72 0.025(5) 0.037(5) 0.041(5) -0.001(5) 0.006(5) 0.001(4) C73 0.021(5) 0.031(5) 0.037(5) 0.002(4) 0.001(4) 0.002(4) C74 0.052(8) 0.058(7) 0.056(7) 0.011(6) 0.015(6) -0.003(6) C75 0.037(7) 0.047(7) 0.043(7) 0.001(6) -0.001(6) 0.001(5) C76 0.017(5) 0.039(5) 0.042(5) 0.001(4) 0.009(4) 0.006(4) C78 0.023(5) 0.036(5) 0.041(5) -0.002(4) 0.010(4) 0.003(4) C79 0.026(5) 0.039(5) 0.047(5) 0.001(4) 0.014(4) 0.006(4) C80 0.032(5) 0.042(5) 0.045(6) 0.002(5) 0.009(4) 0.004(5) C81 0.036(5) 0.047(5) 0.049(5) 0.005(5) 0.012(4) 0.002(5) C82 0.026(5) 0.045(5) 0.049(6) 0.000(5) 0.011(5) 0.002(4) C83 0.025(5) 0.040(5) 0.045(6) -0.002(5) 0.009(4) 0.005(4) C84 0.043(7) 0.060(7) 0.063(8) 0.017(6) 0.017(6) 0.000(6) C85 0.025(6) 0.043(7) 0.054(7) 0.002(6) 0.016(5) 0.009(5) C92 0.016(4) 0.031(5) 0.042(5) 0.001(4) 0.007(4) -0.002(4) C93 0.017(5) 0.039(5) 0.048(5) 0.003(4) 0.007(4) -0.001(4) C94 0.015(5) 0.040(5) 0.045(5) 0.004(4) 0.000(5) -0.005(4) C95 0.011(4) 0.033(5) 0.041(5) 0.000(4) 0.003(4) -0.001(4) C96 0.012(5) 0.029(5) 0.040(5) -0.004(4) 0.002(4) -0.002(4) C98 0.021(5) 0.039(5) 0.043(5) 0.000(4) 0.015(4) 0.002(4) C99 0.023(5) 0.042(5) 0.045(5) 0.004(4) 0.012(4) -0.004(4) C100 0.029(6) 0.041(5) 0.051(5) 0.004(4) 0.005(5) -0.006(5) C101 0.040(6) 0.049(5) 0.051(5) 0.005(5) 0.005(5) -0.004(5) C102 0.036(6) 0.047(5) 0.043(5) -0.001(4) 0.005(5) -0.001(5) C103 0.031(5) 0.042(5) 0.044(5) -0.002(4) 0.008(5) -0.002(5) C104 0.070(8) 0.064(8) 0.067(7) 0.015(6) 0.003(7) -0.008(7) C105 0.039(7) 0.046(7) 0.049(6) 0.002(6) 0.006(5) -0.006(6) C106 0.020(5) 0.030(5) 0.042(5) -0.002(4) 0.002(4) -0.005(4) C108 0.030(5) 0.031(5) 0.038(5) -0.001(4) 0.005(4) -0.001(4) C109 0.031(5) 0.033(5) 0.039(5) -0.001(5) 0.007(4) 0.002(5) C110 0.028(5) 0.034(5) 0.036(5) -0.003(4) 0.005(4) -0.002(4) C111 0.031(5) 0.035(5) 0.037(5) 0.002(4) 0.004(4) -0.002(4) C112 0.031(5) 0.035(5) 0.038(5) 0.001(4) 0.005(4) 0.001(4) C113 0.030(5) 0.033(5) 0.038(5) 0.000(4) 0.005(4) -0.001(4) C114 0.044(8) 0.039(7) 0.046(8) 0.006(6) 0.009(6) -0.003(7) C115 0.028(7) 0.035(7) 0.040(7) 0.000(6) 0.004(6) 0.000(6) O170 0.162(15) 0.170(15) 0.171(15) 0.000(9) 0.039(10) 0.013(10) C118 0.030(5) 0.032(5) 0.037(5) -0.001(4) 0.005(4) -0.001(4) C119 0.032(5) 0.035(5) 0.038(5) -0.001(4) 0.005(4) -0.001(4) C120 0.032(5) 0.036(5) 0.037(5) -0.001(4) 0.005(4) -0.002(4) C121 0.033(5) 0.036(5) 0.037(5) 0.000(5) 0.006(5) -0.001(5) C122 0.033(5) 0.035(5) 0.038(5) -0.001(5) 0.005(4) 0.001(5) C123 0.033(6) 0.033(5) 0.036(6) -0.001(5) 0.006(5) 0.000(5) C124 0.043(9) 0.044(8) 0.043(9) 0.005(7) 0.006(7) 0.002(7) C125 0.035(9) 0.040(8) 0.042(9) 0.001(8) 0.008(7) 0.002(7) P1 0.017(2) 0.040(2) 0.044(2) 0.001(2) 0.0052(18) -0.0038(18) F11 0.015(4) 0.058(5) 0.058(5) 0.002(4) -0.005(4) 0.007(4) F12 0.034(4) 0.049(5) 0.068(5) 0.012(4) 0.000(4) 0.004(4) F13 0.027(4) 0.053(5) 0.047(4) -0.005(4) 0.012(3) -0.009(4) F14 0.017(4) 0.043(4) 0.053(5) 0.002(4) -0.004(3) -0.007(3) F15 0.045(5) 0.061(5) 0.049(4) -0.003(4) 0.017(4) -0.015(4) F16 0.028(4) 0.051(4) 0.062(5) -0.009(4) 0.014(4) -0.021(4) P2 0.021(2) 0.059(3) 0.066(3) 0.012(2) 0.004(2) 0.010(2) F21 0.051(5) 0.067(5) 0.081(6) 0.011(4) 0.017(4) 0.022(4) F22 0.046(5) 0.069(5) 0.082(6) 0.013(4) 0.017(4) 0.029(4) F23 0.063(6) 0.076(6) 0.078(5) 0.017(4) 0.031(4) 0.019(5) F24 0.043(5) 0.081(5) 0.095(6) 0.015(5) 0.001(4) -0.014(4) F25 0.071(6) 0.096(6) 0.063(4) 0.010(4) 0.015(4) 0.039(5) F26 0.046(5) 0.087(6) 0.126(6) -0.010(5) -0.005(5) -0.004(4) P3 0.032(3) 0.073(3) 0.106(4) 0.001(3) 0.024(2) 0.001(3) F31 0.048(5) 0.079(6) 0.101(6) 0.010(5) 0.033(4) 0.006(4) F32 0.048(5) 0.101(6) 0.111(6) -0.024(5) 0.035(5) -0.002(5) F33 0.089(6) 0.081(5) 0.150(7) 0.000(5) 0.054(6) 0.011(5) F34 0.059(5) 0.118(6) 0.097(5) -0.005(5) 0.017(4) 0.003(5) F35 0.064(6) 0.076(5) 0.123(7) -0.003(5) 0.037(5) 0.000(4) F36 0.072(6) 0.142(7) 0.099(5) 0.000(5) 0.020(4) 0.024(6) P4 0.042(4) 0.071(4) 0.114(5) 0.000 -0.026(4) 0.000 F41 0.064(6) 0.090(6) 0.105(5) -0.009(5) -0.023(5) -0.010(5) F42 0.078(6) 0.143(7) 0.136(7) -0.019(6) 0.008(6) 0.013(5) F43 0.094(8) 0.080(5) 0.132(8) 0.000 0.001(7) 0.000 F44 0.121(8) 0.086(5) 0.126(8) 0.000 -0.031(7) 0.000 P5 0.076(5) 0.107(6) 0.087(5) 0.013(5) 0.018(4) -0.004(5) F51 0.113(9) 0.105(7) 0.107(9) 0.011(7) 0.009(7) -0.001(6) F52 0.115(9) 0.120(7) 0.122(9) -0.004(7) 0.016(7) -0.024(7) F53 0.073(7) 0.095(8) 0.119(8) 0.018(7) 0.017(6) 0.000(6) F54 0.115(9) 0.130(9) 0.119(8) 0.006(7) 0.033(7) 0.028(7) F55 0.099(7) 0.144(9) 0.117(8) 0.005(7) 0.005(6) 0.000(7) F56 0.120(9) 0.120(9) 0.126(8) -0.002(7) 0.038(7) 0.010(7) C131 0.032(5) 0.052(6) 0.047(5) 0.002(5) 0.013(5) -0.004(5) C132 0.036(6) 0.045(5) 0.050(6) 0.002(5) 0.014(5) -0.008(5) C133 0.035(5) 0.049(6) 0.052(6) 0.006(5) 0.018(5) -0.004(5) C134 0.038(6) 0.058(6) 0.050(6) 0.005(5) 0.011(5) -0.007(5) C135 0.044(6) 0.051(6) 0.049(5) -0.002(5) 0.014(5) -0.009(5) C136 0.038(5) 0.053(6) 0.054(6) 0.000(5) 0.019(5) 0.001(5) C141 0.056(6) 0.064(6) 0.058(6) 0.013(5) 0.011(5) 0.009(5) C142 0.060(6) 0.067(6) 0.061(6) 0.013(5) 0.004(5) -0.001(5) C143 0.075(6) 0.071(6) 0.059(6) 0.003(5) 0.003(5) 0.010(5) C144 0.067(6) 0.080(6) 0.057(6) 0.011(5) 0.017(5) 0.020(5) C145 0.058(6) 0.078(6) 0.063(6) 0.019(5) 0.011(5) 0.000(5) C146 0.064(6) 0.060(6) 0.060(6) 0.010(5) 0.006(5) 0.003(5) C151 0.077(7) 0.089(7) 0.100(6) -0.005(6) 0.031(5) 0.009(5) C152 0.089(7) 0.095(7) 0.109(6) -0.003(6) 0.031(6) 0.007(5) C153 0.095(7) 0.098(7) 0.113(7) 0.002(6) 0.034(6) 0.014(6) C154 0.095(7) 0.097(7) 0.107(6) 0.004(6) 0.031(6) 0.024(6) C155 0.092(7) 0.103(7) 0.108(6) 0.002(6) 0.020(6) 0.023(5) C156 0.080(7) 0.096(7) 0.101(7) -0.004(6) 0.027(6) 0.016(6) C161 0.150(12) 0.147(12) 0.148(12) -0.003(6) 0.025(6) -0.004(7) C162 0.148(12) 0.149(12) 0.148(12) -0.002(6) 0.026(6) -0.004(6) C163 0.150(12) 0.149(12) 0.147(12) 0.000(6) 0.024(6) -0.005(6) C164 0.151(12) 0.146(12) 0.146(12) -0.003(6) 0.024(6) -0.002(7) C165 0.150(12) 0.146(12) 0.147(12) -0.004(6) 0.025(6) -0.004(6) C166 0.151(12) 0.146(12) 0.148(12) -0.004(6) 0.025(6) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.988(11) . y Cu1 N61 2.004(11) . y Cu1 N63 2.058(11) . y Cu1 N3 2.081(10) . y Cu2 N2 2.029(10) . y Cu2 N91 2.056(11) . y Cu2 N4 2.071(11) . y Cu2 N93 2.074(11) . y Cu3 N62 2.033(11) . y Cu3 N31 2.040(11) . y Cu3 N33 2.076(11) . y Cu3 N64 2.079(11) . y Cu4 N92 2.009(11) . y Cu4 N32 2.018(11) . y Cu4 N34 2.058(11) . y Cu4 N94 2.076(11) . y N1 N2 1.323(14) . ? N1 C5 1.376(16) . ? N2 C2 1.351(16) . ? N3 C6 1.302(16) . ? N3 C8 1.431(16) . ? N4 C16 1.287(16) . ? N4 C18 1.440(18) . ? N31 N32 1.335(14) . ? N31 C35 1.391(17) . ? N32 C32 1.357(17) . ? N33 C36 1.290(16) . ? N33 C38 1.436(17) . ? N34 C46 1.310(16) . ? N34 C48 1.402(17) . ? N61 N62 1.323(15) . ? N61 C65 1.369(16) . ? N62 C62 1.374(17) . ? N63 C66 1.305(16) . ? N63 C68 1.420(17) . ? N64 C76 1.291(17) . ? N64 C78 1.443(17) . ? N91 N92 1.320(14) . ? N91 C95 1.350(16) . ? N92 C92 1.361(17) . ? N93 C96 1.302(16) . ? N93 C98 1.415(17) . ? N94 C106 1.282(16) . ? N94 C118 1.42(4) . ? N94 C108 1.44(3) . ? C2 C3 1.401(18) . ? C2 C16 1.457(19) . ? C3 C4 1.354(18) . ? C3 H3A 0.9500 . ? C4 C5 1.408(18) . ? C4 H4A 0.9500 . ? C5 C6 1.398(18) . ? C6 H6A 0.9500 . ? C8 C9 1.393(14) . ? C8 C13 1.407(14) . ? C9 C10 1.363(14) . ? C9 C15 1.522(15) . ? C10 C11 1.400(15) . ? C10 H10A 0.9500 . ? C11 C12 1.383(15) . ? C11 C14 1.509(15) . ? C12 C13 1.364(15) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9500 . ? C18 C19 1.384(15) . ? C18 C23 1.407(16) . ? C19 C20 1.409(16) . ? C19 C25 1.473(16) . ? C20 C21 1.396(16) . ? C20 H20A 0.9500 . ? C21 C22 1.377(16) . ? C21 C24 1.538(16) . ? C22 C23 1.361(16) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C32 C33 1.409(19) . ? C32 C46 1.410(19) . ? C33 C34 1.339(18) . ? C33 H33A 0.9500 . ? C34 C35 1.387(19) . ? C34 H34A 0.9500 . ? C35 C36 1.413(19) . ? C36 H36A 0.9500 . ? C38 C39 1.398(15) . ? C38 C43 1.407(15) . ? C39 C40 1.384(15) . ? C39 C45 1.497(15) . ? C40 C41 1.386(15) . ? C40 H40A 0.9500 . ? C41 C42 1.382(15) . ? C41 C44 1.519(15) . ? C42 C43 1.349(15) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9500 . ? C48 C53 1.404(15) . ? C48 C49 1.411(15) . ? C49 C50 1.380(15) . ? C49 C55 1.504(15) . ? C50 C51 1.389(15) . ? C50 H50A 0.9500 . ? C51 C52 1.404(15) . ? C51 C54 1.502(15) . ? C52 C53 1.379(15) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C62 C63 1.405(19) . ? C62 C76 1.416(19) . ? C63 C64 1.356(19) . ? C63 H63A 0.9500 . ? C64 C65 1.418(19) . ? C64 H64A 0.9500 . ? C65 C66 1.458(19) . ? C66 H66A 0.9500 . ? C68 C69 1.384(14) . ? C68 C73 1.402(15) . ? C69 C70 1.382(15) . ? C69 C75 1.512(15) . ? C70 C71 1.385(15) . ? C70 H70A 0.9500 . ? C71 C72 1.367(15) . ? C71 C74 1.520(15) . ? C72 C73 1.358(15) . ? C72 H72A 0.9500 . ? C73 H73A 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9500 . ? C78 C79 1.396(15) . ? C78 C83 1.406(15) . ? C79 C80 1.374(15) . ? C79 C85 1.527(15) . ? C80 C81 1.387(15) . ? C80 H80A 0.9500 . ? C81 C82 1.387(15) . ? C81 C84 1.512(16) . ? C82 C83 1.354(15) . ? C82 H82A 0.9500 . ? C83 H83A 0.9500 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C92 C93 1.385(19) . ? C92 C106 1.418(19) . ? C93 C94 1.340(19) . ? C93 H93A 0.9500 . ? C94 C95 1.433(19) . ? C94 H94A 0.9500 . ? C95 C96 1.426(19) . ? C96 H96A 0.9500 . ? C98 C103 1.404(15) . ? C98 C99 1.406(15) . ? C99 C100 1.370(15) . ? C99 C105 1.493(15) . ? C100 C101 1.375(15) . ? C100 H10B 0.9500 . ? C101 C102 1.379(15) . ? C101 C104 1.501(16) . ? C102 C103 1.370(15) . ? C102 H10C 0.9500 . ? C103 H10D 0.9500 . ? C104 H10E 0.9800 . ? C104 H10F 0.9800 . ? C104 H10G 0.9800 . ? C105 H10H 0.9800 . ? C105 H10I 0.9800 . ? C105 H10J 0.9800 . ? C106 H10K 0.9500 . ? C108 C109 1.397(19) . ? C108 C113 1.400(19) . ? C109 C110 1.368(19) . ? C109 H10L 0.9500 . ? C110 C111 1.394(19) . ? C110 H11A 0.9500 . ? C111 C112 1.383(19) . ? C111 C114 1.506(18) . ? C112 C113 1.356(18) . ? C112 H11B 0.9500 . ? C113 C115 1.52(3) . ? C114 H11C 0.9800 . ? C114 H11D 0.9800 . ? C114 H11E 0.9800 . ? C115 H11F 0.9800 . ? C115 H11G 0.9800 . ? C115 H11H 0.9800 . ? O170 H171 0.8579 . ? O170 H172 0.8275 . ? C118 C119 1.40(2) . ? C118 C123 1.41(2) . ? C119 C120 1.38(2) . ? C119 C125 1.50(2) . ? C120 C121 1.39(2) . ? C120 H120 0.9500 . ? C121 C122 1.38(2) . ? C121 C124 1.52(2) . ? C122 C123 1.36(2) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? C124 H12D 0.9800 . ? C125 H12E 0.9800 . ? C125 H12F 0.9800 . ? C125 H12G 0.9800 . ? P1 F15 1.573(9) . ? P1 F12 1.578(9) . ? P1 F16 1.584(8) . ? P1 F13 1.596(8) . ? P1 F14 1.602(8) . ? P1 F11 1.615(8) . ? P2 F23 1.570(10) . ? P2 F26 1.577(11) . ? P2 F24 1.593(11) . ? P2 F25 1.594(11) . ? P2 F21 1.595(10) . ? P2 F22 1.602(10) . ? P3 F36 1.536(13) . ? P3 F35 1.572(12) . ? P3 F33 1.589(13) . ? P3 F32 1.590(11) . ? P3 F31 1.599(11) . ? P3 F34 1.606(12) . ? P4 F43 1.543(18) . ? P4 F44 1.579(19) . ? P4 F42 1.595(14) 2_557 ? P4 F42 1.595(14) . ? P4 F41 1.604(11) 2_557 ? P4 F41 1.604(11) . ? P5 F53 1.538(16) . ? P5 F56 1.548(16) . ? P5 F55 1.561(16) . ? P5 F51 1.584(16) . ? P5 F52 1.589(16) . ? P5 F54 1.593(16) . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C131 H13B 0.9500 . ? C132 C133 1.3900 . ? C132 H13C 0.9500 . ? C133 C134 1.3900 . ? C133 H13D 0.9500 . ? C134 C135 1.3900 . ? C134 H13E 0.9500 . ? C135 C136 1.3900 . ? C135 H13F 0.9500 . ? C136 H13G 0.9500 . ? C141 C142 1.3900 . ? C141 C146 1.3900 . ? C141 H14D 0.9500 . ? C142 C143 1.3900 . ? C142 H14E 0.9500 . ? C143 C144 1.3900 . ? C143 H14F 0.9500 . ? C144 C145 1.3900 . ? C144 H14G 0.9500 . ? C145 C146 1.3900 . ? C145 H14H 0.9500 . ? C146 H14I 0.9500 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C151 H15D 0.9500 . ? C152 C153 1.3900 . ? C152 H15E 0.9500 . ? C153 C154 1.3900 . ? C153 H153 0.9500 . ? C154 C155 1.3900 . ? C154 H15F 0.9500 . ? C155 C156 1.3900 . ? C155 H15G 0.9500 . ? C156 H15H 0.9500 . ? C161 C162 1.3900 . ? C161 C166 1.3900 . ? C161 H16B 0.9500 . ? C162 C163 1.3900 . ? C162 H16C 0.9500 . ? C163 C164 1.3900 . ? C163 H16D 0.9500 . ? C164 C165 1.3900 . ? C164 H16E 0.9500 . ? C165 C166 1.3900 . ? C165 H16F 0.9500 . ? C166 H16G 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N61 128.2(4) . . y N1 Cu1 N63 116.8(4) . . y N61 Cu1 N63 82.3(4) . . y N1 Cu1 N3 82.3(4) . . y N61 Cu1 N3 128.7(4) . . y N63 Cu1 N3 123.7(4) . . y N2 Cu2 N91 121.0(4) . . y N2 Cu2 N4 81.8(4) . . y N91 Cu2 N4 123.5(4) . . y N2 Cu2 N93 130.0(4) . . y N91 Cu2 N93 83.0(4) . . y N4 Cu2 N93 123.3(4) . . y N62 Cu3 N31 118.7(4) . . y N62 Cu3 N33 123.1(4) . . y N31 Cu3 N33 82.0(4) . . y N62 Cu3 N64 81.7(5) . . y N31 Cu3 N64 133.3(4) . . y N33 Cu3 N64 123.8(4) . . y N92 Cu4 N32 125.1(4) . . y N92 Cu4 N34 126.3(4) . . y N32 Cu4 N34 82.2(4) . . y N92 Cu4 N94 81.7(5) . . y N32 Cu4 N94 121.6(4) . . y N34 Cu4 N94 125.9(4) . . y N2 N1 C5 119.3(11) . . ? N2 N1 Cu1 129.1(8) . . ? C5 N1 Cu1 111.5(9) . . ? N1 N2 C2 120.6(11) . . ? N1 N2 Cu2 127.5(8) . . ? C2 N2 Cu2 111.9(9) . . ? C6 N3 C8 117.0(11) . . ? C6 N3 Cu1 109.0(9) . . ? C8 N3 Cu1 134.0(8) . . ? C16 N4 C18 114.7(12) . . ? C16 N4 Cu2 110.8(9) . . ? C18 N4 Cu2 133.9(9) . . ? N32 N31 C35 120.1(11) . . ? N32 N31 Cu3 130.0(8) . . ? C35 N31 Cu3 109.9(9) . . ? N31 N32 C32 121.4(11) . . ? N31 N32 Cu4 126.9(8) . . ? C32 N32 Cu4 111.5(9) . . ? C36 N33 C38 115.5(11) . . ? C36 N33 Cu3 110.6(9) . . ? C38 N33 Cu3 133.6(9) . . ? C46 N34 C48 117.0(11) . . ? C46 N34 Cu4 109.3(9) . . ? C48 N34 Cu4 133.6(9) . . ? N62 N61 C65 120.3(11) . . ? N62 N61 Cu1 127.6(8) . . ? C65 N61 Cu1 112.1(9) . . ? N61 N62 C62 120.2(11) . . ? N61 N62 Cu3 128.5(8) . . ? C62 N62 Cu3 111.2(9) . . ? C66 N63 C68 121.7(11) . . ? C66 N63 Cu1 111.6(9) . . ? C68 N63 Cu1 126.5(8) . . ? C76 N64 C78 115.5(12) . . ? C76 N64 Cu3 109.9(10) . . ? C78 N64 Cu3 134.6(9) . . ? N92 N91 C95 121.3(11) . . ? N92 N91 Cu2 129.6(8) . . ? C95 N91 Cu2 109.0(9) . . ? N91 N92 C92 119.8(11) . . ? N91 N92 Cu4 128.8(8) . . ? C92 N92 Cu4 111.4(9) . . ? C96 N93 C98 116.3(11) . . ? C96 N93 Cu2 108.2(9) . . ? C98 N93 Cu2 135.4(9) . . ? C106 N94 C118 128(2) . . ? C106 N94 C108 114.2(14) . . ? C118 N94 C108 15.4(17) . . ? C106 N94 Cu4 110.2(10) . . ? C118 N94 Cu4 122(2) . . ? C108 N94 Cu4 135.0(13) . . ? N2 C2 C3 122.6(13) . . ? N2 C2 C16 115.7(12) . . ? C3 C2 C16 121.6(12) . . ? C4 C3 C2 116.9(13) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? C3 C4 C5 119.7(13) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 C6 116.4(12) . . ? N1 C5 C4 120.6(12) . . ? C6 C5 C4 122.9(12) . . ? N3 C6 C5 120.7(12) . . ? N3 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C9 C8 C13 118.5(12) . . ? C9 C8 N3 121.8(11) . . ? C13 C8 N3 119.6(11) . . ? C10 C9 C8 118.8(12) . . ? C10 C9 C15 120.2(12) . . ? C8 C9 C15 121.1(11) . . ? C9 C10 C11 123.2(13) . . ? C9 C10 H10A 118.4 . . ? C11 C10 H10A 118.4 . . ? C12 C11 C10 117.4(12) . . ? C12 C11 C14 120.4(12) . . ? C10 C11 C14 122.2(12) . . ? C13 C12 C11 120.4(13) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C8 121.6(13) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C2 119.7(12) . . ? N4 C16 H16A 120.1 . . ? C2 C16 H16A 120.1 . . ? C19 C18 C23 118.1(14) . . ? C19 C18 N4 121.6(13) . . ? C23 C18 N4 120.3(13) . . ? C18 C19 C20 119.2(14) . . ? C18 C19 C25 119.9(13) . . ? C20 C19 C25 120.9(13) . . ? C21 C20 C19 120.0(14) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C22 C21 C20 121.2(15) . . ? C22 C21 C24 120.4(15) . . ? C20 C21 C24 118.4(14) . . ? C23 C22 C21 117.8(16) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C22 C23 C18 123.6(16) . . ? C22 C23 H23A 118.2 . . ? C18 C23 H23A 118.2 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N32 C32 C33 119.2(13) . . ? N32 C32 C46 115.8(12) . . ? C33 C32 C46 125.0(13) . . ? C34 C33 C32 119.9(13) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.2(13) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 N31 119.3(13) . . ? C34 C35 C36 123.9(13) . . ? N31 C35 C36 116.9(12) . . ? N33 C36 C35 120.6(13) . . ? N33 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? C39 C38 C43 119.5(12) . . ? C39 C38 N33 120.3(11) . . ? C43 C38 N33 120.2(11) . . ? C40 C39 C38 117.4(12) . . ? C40 C39 C45 120.2(12) . . ? C38 C39 C45 122.3(12) . . ? C39 C40 C41 123.1(13) . . ? C39 C40 H40A 118.4 . . ? C41 C40 H40A 118.4 . . ? C42 C41 C40 117.3(12) . . ? C42 C41 C44 121.5(12) . . ? C40 C41 C44 121.2(12) . . ? C43 C42 C41 122.0(14) . . ? C43 C42 H42A 119.0 . . ? C41 C42 H42A 119.0 . . ? C42 C43 C38 120.2(13) . . ? C42 C43 H43A 119.9 . . ? C38 C43 H43A 119.9 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N34 C46 C32 121.1(13) . . ? N34 C46 H46A 119.4 . . ? C32 C46 H46A 119.4 . . ? N34 C48 C53 121.5(12) . . ? N34 C48 C49 120.0(11) . . ? C53 C48 C49 118.5(12) . . ? C50 C49 C48 119.2(12) . . ? C50 C49 C55 120.3(12) . . ? C48 C49 C55 120.6(12) . . ? C49 C50 C51 123.2(13) . . ? C49 C50 H50A 118.4 . . ? C51 C50 H50A 118.4 . . ? C50 C51 C52 116.9(13) . . ? C50 C51 C54 121.1(13) . . ? C52 C51 C54 121.9(13) . . ? C53 C52 C51 121.4(13) . . ? C53 C52 H52A 119.3 . . ? C51 C52 H52A 119.3 . . ? C52 C53 C48 120.8(13) . . ? C52 C53 H53A 119.6 . . ? C48 C53 H53A 119.6 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 H55A 109.5 . . ? C49 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C49 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N62 C62 C63 121.2(13) . . ? N62 C62 C76 115.8(12) . . ? C63 C62 C76 122.8(13) . . ? C64 C63 C62 118.7(14) . . ? C64 C63 H63A 120.6 . . ? C62 C63 H63A 120.6 . . ? C63 C64 C65 118.4(13) . . ? C63 C64 H64A 120.8 . . ? C65 C64 H64A 120.8 . . ? N61 C65 C64 121.0(13) . . ? N61 C65 C66 115.9(12) . . ? C64 C65 C66 122.9(12) . . ? N63 C66 C65 118.1(12) . . ? N63 C66 H66A 121.0 . . ? C65 C66 H66A 121.0 . . ? C69 C68 C73 119.7(12) . . ? C69 C68 N63 124.8(12) . . ? C73 C68 N63 115.5(11) . . ? C70 C69 C68 116.7(12) . . ? C70 C69 C75 119.2(12) . . ? C68 C69 C75 123.9(12) . . ? C69 C70 C71 124.1(13) . . ? C69 C70 H70A 118.0 . . ? C71 C70 H70A 118.0 . . ? C72 C71 C70 117.5(12) . . ? C72 C71 C74 122.5(13) . . ? C70 C71 C74 120.0(12) . . ? C73 C72 C71 120.7(13) . . ? C73 C72 H72A 119.7 . . ? C71 C72 H72A 119.7 . . ? C72 C73 C68 121.3(13) . . ? C72 C73 H73A 119.4 . . ? C68 C73 H73A 119.4 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C69 C75 H75A 109.5 . . ? C69 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C69 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N64 C76 C62 121.3(14) . . ? N64 C76 H76A 119.4 . . ? C62 C76 H76A 119.4 . . ? C79 C78 C83 119.7(13) . . ? C79 C78 N64 122.0(11) . . ? C83 C78 N64 118.3(11) . . ? C80 C79 C78 117.7(12) . . ? C80 C79 C85 120.9(12) . . ? C78 C79 C85 121.1(12) . . ? C79 C80 C81 122.9(13) . . ? C79 C80 H80A 118.5 . . ? C81 C80 H80A 118.5 . . ? C80 C81 C82 117.9(13) . . ? C80 C81 C84 120.4(13) . . ? C82 C81 C84 121.7(13) . . ? C83 C82 C81 121.0(13) . . ? C83 C82 H82A 119.5 . . ? C81 C82 H82A 119.5 . . ? C82 C83 C78 120.4(13) . . ? C82 C83 H83A 119.8 . . ? C78 C83 H83A 119.8 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C79 C85 H85A 109.5 . . ? C79 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C79 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N92 C92 C93 121.2(13) . . ? N92 C92 C106 116.4(12) . . ? C93 C92 C106 122.4(13) . . ? C94 C93 C92 119.8(14) . . ? C94 C93 H93A 120.1 . . ? C92 C93 H93A 120.1 . . ? C93 C94 C95 117.9(13) . . ? C93 C94 H94A 121.1 . . ? C95 C94 H94A 121.1 . . ? N91 C95 C96 117.9(12) . . ? N91 C95 C94 120.0(13) . . ? C96 C95 C94 122.1(13) . . ? N93 C96 C95 121.4(13) . . ? N93 C96 H96A 119.3 . . ? C95 C96 H96A 119.3 . . ? C103 C98 C99 118.5(13) . . ? C103 C98 N93 118.9(12) . . ? C99 C98 N93 122.6(12) . . ? C100 C99 C98 118.4(12) . . ? C100 C99 C105 121.0(12) . . ? C98 C99 C105 120.3(12) . . ? C99 C100 C101 123.8(14) . . ? C99 C100 H10B 118.1 . . ? C101 C100 H10B 118.1 . . ? C100 C101 C102 117.0(13) . . ? C100 C101 C104 121.2(13) . . ? C102 C101 C104 121.8(13) . . ? C103 C102 C101 121.9(14) . . ? C103 C102 H10C 119.0 . . ? C101 C102 H10C 119.0 . . ? C102 C103 C98 120.2(14) . . ? C102 C103 H10D 119.9 . . ? C98 C103 H10D 119.9 . . ? C101 C104 H10E 109.5 . . ? C101 C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? C101 C104 H10G 109.5 . . ? H10E C104 H10G 109.5 . . ? H10F C104 H10G 109.5 . . ? C99 C105 H10H 109.5 . . ? C99 C105 H10I 109.5 . . ? H10H C105 H10I 109.5 . . ? C99 C105 H10J 109.5 . . ? H10H C105 H10J 109.5 . . ? H10I C105 H10J 109.5 . . ? N94 C106 C92 120.2(13) . . ? N94 C106 H10K 119.9 . . ? C92 C106 H10K 119.9 . . ? C109 C108 C113 116(2) . . ? C109 C108 N94 122.1(17) . . ? C113 C108 N94 121.5(17) . . ? C110 C109 C108 122(2) . . ? C110 C109 H10L 119.1 . . ? C108 C109 H10L 119.1 . . ? C109 C110 C111 121(2) . . ? C109 C110 H11A 119.3 . . ? C111 C110 H11A 119.3 . . ? C112 C111 C110 116.0(18) . . ? C112 C111 C114 121.6(18) . . ? C110 C111 C114 122.3(18) . . ? C113 C112 C111 123(2) . . ? C113 C112 H11B 118.5 . . ? C111 C112 H11B 118.5 . . ? C112 C113 C108 121(2) . . ? C112 C113 C115 119.2(18) . . ? C108 C113 C115 119.3(18) . . ? H171 O170 H172 124.2 . . ? C119 C118 C123 116(4) . . ? C119 C118 N94 123(3) . . ? C123 C118 N94 121(3) . . ? C120 C119 C118 119(3) . . ? C120 C119 C125 124(3) . . ? C118 C119 C125 115(3) . . ? C119 C120 C121 122(3) . . ? C119 C120 H120 119.0 . . ? C121 C120 H120 119.0 . . ? C122 C121 C120 121(3) . . ? C122 C121 C124 125(3) . . ? C120 C121 C124 114(3) . . ? C123 C122 C121 115(4) . . ? C123 C122 H122 122.7 . . ? C121 C122 H122 122.7 . . ? C122 C123 C118 127(4) . . ? C122 C123 H123 116.5 . . ? C118 C123 H123 116.5 . . ? C121 C124 H12B 109.5 . . ? C121 C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C121 C124 H12D 109.5 . . ? H12B C124 H12D 109.5 . . ? H12C C124 H12D 109.5 . . ? C119 C125 H12E 109.5 . . ? C119 C125 H12F 109.5 . . ? H12E C125 H12F 109.5 . . ? C119 C125 H12G 109.5 . . ? H12E C125 H12G 109.5 . . ? H12F C125 H12G 109.5 . . ? F15 P1 F12 90.7(5) . . ? F15 P1 F16 90.7(5) . . ? F12 P1 F16 90.0(5) . . ? F15 P1 F13 178.7(5) . . ? F12 P1 F13 90.6(5) . . ? F16 P1 F13 89.1(4) . . ? F15 P1 F14 90.2(5) . . ? F12 P1 F14 91.3(4) . . ? F16 P1 F14 178.4(5) . . ? F13 P1 F14 89.9(4) . . ? F15 P1 F11 89.8(5) . . ? F12 P1 F11 178.9(5) . . ? F16 P1 F11 89.0(5) . . ? F13 P1 F11 89.0(4) . . ? F14 P1 F11 89.7(4) . . ? F23 P2 F26 90.0(6) . . ? F23 P2 F24 90.0(6) . . ? F26 P2 F24 178.5(6) . . ? F23 P2 F25 178.0(7) . . ? F26 P2 F25 91.9(7) . . ? F24 P2 F25 88.1(6) . . ? F23 P2 F21 89.9(5) . . ? F26 P2 F21 90.3(6) . . ? F24 P2 F21 88.2(6) . . ? F25 P2 F21 89.4(5) . . ? F23 P2 F22 89.5(5) . . ? F26 P2 F22 91.5(6) . . ? F24 P2 F22 90.0(6) . . ? F25 P2 F22 91.1(5) . . ? F21 P2 F22 178.0(7) . . ? F36 P3 F35 89.1(7) . . ? F36 P3 F33 96.1(8) . . ? F35 P3 F33 174.4(8) . . ? F36 P3 F32 89.4(7) . . ? F35 P3 F32 90.9(6) . . ? F33 P3 F32 87.0(6) . . ? F36 P3 F31 92.9(7) . . ? F35 P3 F31 92.1(6) . . ? F33 P3 F31 89.8(6) . . ? F32 P3 F31 176.3(7) . . ? F36 P3 F34 175.6(8) . . ? F35 P3 F34 86.6(7) . . ? F33 P3 F34 88.2(7) . . ? F32 P3 F34 89.9(7) . . ? F31 P3 F34 88.0(6) . . ? F43 P4 F44 180.000(17) . . ? F43 P4 F42 91.0(6) . 2_557 ? F44 P4 F42 89.0(6) . 2_557 ? F43 P4 F42 91.0(6) . . ? F44 P4 F42 89.0(6) . . ? F42 P4 F42 178.1(12) 2_557 . ? F43 P4 F41 90.8(5) . 2_557 ? F44 P4 F41 89.2(5) . 2_557 ? F42 P4 F41 89.3(7) 2_557 2_557 ? F42 P4 F41 90.7(6) . 2_557 ? F43 P4 F41 90.8(5) . . ? F44 P4 F41 89.2(5) . . ? F42 P4 F41 90.7(6) 2_557 . ? F42 P4 F41 89.3(7) . . ? F41 P4 F41 178.3(10) 2_557 . ? F53 P5 F56 82.6(12) . . ? F53 P5 F55 174.1(15) . . ? F56 P5 F55 91.7(13) . . ? F53 P5 F51 91.3(12) . . ? F56 P5 F51 91.5(13) . . ? F55 P5 F51 90.5(12) . . ? F53 P5 F52 90.4(12) . . ? F56 P5 F52 86.3(13) . . ? F55 P5 F52 87.6(13) . . ? F51 P5 F52 177.0(14) . . ? F53 P5 F54 95.7(12) . . ? F56 P5 F54 175.9(14) . . ? F55 P5 F54 89.9(13) . . ? F51 P5 F54 92.4(13) . . ? F52 P5 F54 89.9(13) . . ? C132 C131 C136 120.0 . . ? C132 C131 H13B 120.0 . . ? C136 C131 H13B 120.0 . . ? C133 C132 C131 120.0 . . ? C133 C132 H13C 120.0 . . ? C131 C132 H13C 120.0 . . ? C134 C133 C132 120.0 . . ? C134 C133 H13D 120.0 . . ? C132 C133 H13D 120.0 . . ? C133 C134 C135 120.0 . . ? C133 C134 H13E 120.0 . . ? C135 C134 H13E 120.0 . . ? C136 C135 C134 120.0 . . ? C136 C135 H13F 120.0 . . ? C134 C135 H13F 120.0 . . ? C135 C136 C131 120.0 . . ? C135 C136 H13G 120.0 . . ? C131 C136 H13G 120.0 . . ? C142 C141 C146 120.0 . . ? C142 C141 H14D 120.0 . . ? C146 C141 H14D 120.0 . . ? C141 C142 C143 120.0 . . ? C141 C142 H14E 120.0 . . ? C143 C142 H14E 120.0 . . ? C142 C143 C144 120.0 . . ? C142 C143 H14F 120.0 . . ? C144 C143 H14F 120.0 . . ? C145 C144 C143 120.0 . . ? C145 C144 H14G 120.0 . . ? C143 C144 H14G 120.0 . . ? C144 C145 C146 120.0 . . ? C144 C145 H14H 120.0 . . ? C146 C145 H14H 120.0 . . ? C145 C146 C141 120.0 . . ? C145 C146 H14I 120.0 . . ? C141 C146 H14I 120.0 . . ? C152 C151 C156 120.0 . . ? C152 C151 H15D 120.0 . . ? C156 C151 H15D 120.0 . . ? C153 C152 C151 120.0 . . ? C153 C152 H15E 120.0 . . ? C151 C152 H15E 120.0 . . ? C152 C153 C154 120.0 . . ? C152 C153 H153 120.0 . . ? C154 C153 H153 120.0 . . ? C155 C154 C153 120.0 . . ? C155 C154 H15F 120.0 . . ? C153 C154 H15F 120.0 . . ? C154 C155 C156 120.0 . . ? C154 C155 H15G 120.0 . . ? C156 C155 H15G 120.0 . . ? C155 C156 C151 120.0 . . ? C155 C156 H15H 120.0 . . ? C151 C156 H15H 120.0 . . ? C162 C161 C166 120.0 . . ? C162 C161 H16B 120.0 . . ? C166 C161 H16B 120.0 . . ? C163 C162 C161 120.0 . . ? C163 C162 H16C 120.0 . . ? C161 C162 H16C 120.0 . . ? C162 C163 C164 120.0 . . ? C162 C163 H16D 120.0 . . ? C164 C163 H16D 120.0 . . ? C163 C164 C165 120.0 . . ? C163 C164 H16E 120.0 . . ? C165 C164 H16E 120.0 . . ? C166 C165 C164 120.0 . . ? C166 C165 H16F 120.0 . . ? C164 C165 H16F 120.0 . . ? C165 C166 C161 120.0 . . ? C165 C166 H16G 120.0 . . ? C161 C166 H16G 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N61 Cu1 N1 N2 -47.3(12) . . . . ? N63 Cu1 N1 N2 54.6(11) . . . . ? N3 Cu1 N1 N2 178.6(11) . . . . ? N61 Cu1 N1 C5 136.6(8) . . . . ? N63 Cu1 N1 C5 -121.5(9) . . . . ? N3 Cu1 N1 C5 2.5(9) . . . . ? C5 N1 N2 C2 -2.3(17) . . . . ? Cu1 N1 N2 C2 -178.2(9) . . . . ? C5 N1 N2 Cu2 176.0(9) . . . . ? Cu1 N1 N2 Cu2 0.1(15) . . . . ? N91 Cu2 N2 N1 56.4(11) . . . . ? N4 Cu2 N2 N1 -179.3(10) . . . . ? N93 Cu2 N2 N1 -52.3(12) . . . . ? N91 Cu2 N2 C2 -125.2(9) . . . . ? N4 Cu2 N2 C2 -0.9(9) . . . . ? N93 Cu2 N2 C2 126.1(9) . . . . ? N1 Cu1 N3 C6 -3.0(9) . . . . ? N61 Cu1 N3 C6 -136.7(8) . . . . ? N63 Cu1 N3 C6 114.1(9) . . . . ? N1 Cu1 N3 C8 177.6(12) . . . . ? N61 Cu1 N3 C8 43.9(13) . . . . ? N63 Cu1 N3 C8 -65.2(13) . . . . ? N2 Cu2 N4 C16 0.7(9) . . . . ? N91 Cu2 N4 C16 122.6(9) . . . . ? N93 Cu2 N4 C16 -132.3(9) . . . . ? N2 Cu2 N4 C18 171.2(13) . . . . ? N91 Cu2 N4 C18 -66.8(14) . . . . ? N93 Cu2 N4 C18 38.3(14) . . . . ? N62 Cu3 N31 N32 56.1(12) . . . . ? N33 Cu3 N31 N32 179.6(11) . . . . ? N64 Cu3 N31 N32 -50.6(13) . . . . ? N62 Cu3 N31 C35 -124.6(9) . . . . ? N33 Cu3 N31 C35 -1.1(9) . . . . ? N64 Cu3 N31 C35 128.7(9) . . . . ? C35 N31 N32 C32 -2.3(18) . . . . ? Cu3 N31 N32 C32 176.9(9) . . . . ? C35 N31 N32 Cu4 -176.5(9) . . . . ? Cu3 N31 N32 Cu4 2.7(16) . . . . ? N92 Cu4 N32 N31 -54.1(12) . . . . ? N34 Cu4 N32 N31 176.5(11) . . . . ? N94 Cu4 N32 N31 48.9(12) . . . . ? N92 Cu4 N32 C32 131.2(9) . . . . ? N34 Cu4 N32 C32 1.8(9) . . . . ? N94 Cu4 N32 C32 -125.8(9) . . . . ? N62 Cu3 N33 C36 120.4(9) . . . . ? N31 Cu3 N33 C36 1.2(9) . . . . ? N64 Cu3 N33 C36 -136.4(9) . . . . ? N62 Cu3 N33 C38 -66.3(13) . . . . ? N31 Cu3 N33 C38 174.6(12) . . . . ? N64 Cu3 N33 C38 36.9(13) . . . . ? N92 Cu4 N34 C46 -128.9(9) . . . . ? N32 Cu4 N34 C46 -0.6(9) . . . . ? N94 Cu4 N34 C46 122.9(9) . . . . ? N92 Cu4 N34 C48 45.9(14) . . . . ? N32 Cu4 N34 C48 174.2(12) . . . . ? N94 Cu4 N34 C48 -62.2(13) . . . . ? N1 Cu1 N61 N62 -62.0(12) . . . . ? N63 Cu1 N61 N62 179.9(11) . . . . ? N3 Cu1 N61 N62 52.3(12) . . . . ? N1 Cu1 N61 C65 116.9(9) . . . . ? N63 Cu1 N61 C65 -1.3(9) . . . . ? N3 Cu1 N61 C65 -128.8(9) . . . . ? C65 N61 N62 C62 1.3(18) . . . . ? Cu1 N61 N62 C62 -179.8(9) . . . . ? C65 N61 N62 Cu3 177.2(9) . . . . ? Cu1 N61 N62 Cu3 -4.0(16) . . . . ? N31 Cu3 N62 N61 46.9(12) . . . . ? N33 Cu3 N62 N61 -52.7(12) . . . . ? N64 Cu3 N62 N61 -177.9(11) . . . . ? N31 Cu3 N62 C62 -136.9(9) . . . . ? N33 Cu3 N62 C62 123.5(9) . . . . ? N64 Cu3 N62 C62 -1.7(9) . . . . ? N1 Cu1 N63 C66 -129.9(9) . . . . ? N61 Cu1 N63 C66 -0.8(9) . . . . ? N3 Cu1 N63 C66 131.1(9) . . . . ? N1 Cu1 N63 C68 55.8(11) . . . . ? N61 Cu1 N63 C68 -175.1(11) . . . . ? N3 Cu1 N63 C68 -43.1(12) . . . . ? N62 Cu3 N64 C76 3.0(9) . . . . ? N31 Cu3 N64 C76 124.8(9) . . . . ? N33 Cu3 N64 C76 -121.5(9) . . . . ? N62 Cu3 N64 C78 -174.1(13) . . . . ? N31 Cu3 N64 C78 -52.3(14) . . . . ? N33 Cu3 N64 C78 61.4(13) . . . . ? N2 Cu2 N91 N92 45.6(12) . . . . ? N4 Cu2 N91 N92 -55.8(12) . . . . ? N93 Cu2 N91 N92 178.6(11) . . . . ? N2 Cu2 N91 C95 -137.6(8) . . . . ? N4 Cu2 N91 C95 121.0(9) . . . . ? N93 Cu2 N91 C95 -4.6(9) . . . . ? C95 N91 N92 C92 1.7(18) . . . . ? Cu2 N91 N92 C92 178.1(9) . . . . ? C95 N91 N92 Cu4 -179.8(9) . . . . ? Cu2 N91 N92 Cu4 -3.4(16) . . . . ? N32 Cu4 N92 N91 -56.2(12) . . . . ? N34 Cu4 N92 N91 51.9(12) . . . . ? N94 Cu4 N92 N91 -179.2(11) . . . . ? N32 Cu4 N92 C92 122.4(9) . . . . ? N34 Cu4 N92 C92 -129.6(9) . . . . ? N94 Cu4 N92 C92 -0.6(9) . . . . ? N2 Cu2 N93 C96 131.0(9) . . . . ? N91 Cu2 N93 C96 5.9(9) . . . . ? N4 Cu2 N93 C96 -119.9(9) . . . . ? N2 Cu2 N93 C98 -50.6(14) . . . . ? N91 Cu2 N93 C98 -175.7(13) . . . . ? N4 Cu2 N93 C98 58.5(14) . . . . ? N92 Cu4 N94 C106 -0.2(9) . . . . ? N32 Cu4 N94 C106 -126.5(9) . . . . ? N34 Cu4 N94 C106 129.1(9) . . . . ? N92 Cu4 N94 C118 179(3) . . . . ? N32 Cu4 N94 C118 53(3) . . . . ? N34 Cu4 N94 C118 -51(3) . . . . ? N92 Cu4 N94 C108 -169.9(19) . . . . ? N32 Cu4 N94 C108 63.8(19) . . . . ? N34 Cu4 N94 C108 -41(2) . . . . ? N1 N2 C2 C3 -1.0(19) . . . . ? Cu2 N2 C2 C3 -179.5(10) . . . . ? N1 N2 C2 C16 179.6(11) . . . . ? Cu2 N2 C2 C16 1.1(14) . . . . ? N2 C2 C3 C4 3(2) . . . . ? C16 C2 C3 C4 -177.6(12) . . . . ? C2 C3 C4 C5 -1.7(19) . . . . ? N2 N1 C5 C6 -178.2(11) . . . . ? Cu1 N1 C5 C6 -1.7(14) . . . . ? N2 N1 C5 C4 3.5(18) . . . . ? Cu1 N1 C5 C4 -179.9(10) . . . . ? C3 C4 C5 N1 -1(2) . . . . ? C3 C4 C5 C6 -179.6(13) . . . . ? C8 N3 C6 C5 -177.4(11) . . . . ? Cu1 N3 C6 C5 3.1(15) . . . . ? N1 C5 C6 N3 -1.1(19) . . . . ? C4 C5 C6 N3 177.1(12) . . . . ? C6 N3 C8 C9 -143.8(13) . . . . ? Cu1 N3 C8 C9 35.5(19) . . . . ? C6 N3 C8 C13 34.2(17) . . . . ? Cu1 N3 C8 C13 -146.5(10) . . . . ? C13 C8 C9 C10 -1(2) . . . . ? N3 C8 C9 C10 176.7(12) . . . . ? C13 C8 C9 C15 178.4(12) . . . . ? N3 C8 C9 C15 -4(2) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C15 C9 C10 C11 179.3(13) . . . . ? C9 C10 C11 C12 3(2) . . . . ? C9 C10 C11 C14 -176.9(14) . . . . ? C10 C11 C12 C13 -3(2) . . . . ? C14 C11 C12 C13 177.2(14) . . . . ? C11 C12 C13 C8 0(2) . . . . ? C9 C8 C13 C12 2(2) . . . . ? N3 C8 C13 C12 -176.5(12) . . . . ? C18 N4 C16 C2 -172.8(12) . . . . ? Cu2 N4 C16 C2 -0.3(15) . . . . ? N2 C2 C16 N4 -0.5(19) . . . . ? C3 C2 C16 N4 -180.0(13) . . . . ? C16 N4 C18 C19 -142.3(14) . . . . ? Cu2 N4 C18 C19 47(2) . . . . ? C16 N4 C18 C23 39.1(19) . . . . ? Cu2 N4 C18 C23 -131.3(13) . . . . ? C23 C18 C19 C20 -4(2) . . . . ? N4 C18 C19 C20 177.1(13) . . . . ? C23 C18 C19 C25 177.8(14) . . . . ? N4 C18 C19 C25 -1(2) . . . . ? C18 C19 C20 C21 3(2) . . . . ? C25 C19 C20 C21 -179.4(15) . . . . ? C19 C20 C21 C22 2(3) . . . . ? C19 C20 C21 C24 -178.3(15) . . . . ? C20 C21 C22 C23 -5(2) . . . . ? C24 C21 C22 C23 175.6(15) . . . . ? C21 C22 C23 C18 3(2) . . . . ? C19 C18 C23 C22 2(2) . . . . ? N4 C18 C23 C22 -179.7(14) . . . . ? N31 N32 C32 C33 2.8(19) . . . . ? Cu4 N32 C32 C33 177.8(10) . . . . ? N31 N32 C32 C46 -177.7(11) . . . . ? Cu4 N32 C32 C46 -2.7(15) . . . . ? N32 C32 C33 C34 -1(2) . . . . ? C46 C32 C33 C34 179.5(13) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 N31 2(2) . . . . ? C33 C34 C35 C36 -178.6(13) . . . . ? N32 N31 C35 C34 0.1(19) . . . . ? Cu3 N31 C35 C34 -179.3(10) . . . . ? N32 N31 C35 C36 -179.7(11) . . . . ? Cu3 N31 C35 C36 0.9(15) . . . . ? C38 N33 C36 C35 -175.8(12) . . . . ? Cu3 N33 C36 C35 -1.1(16) . . . . ? C34 C35 C36 N33 -179.6(13) . . . . ? N31 C35 C36 N33 0(2) . . . . ? C36 N33 C38 C39 -141.4(13) . . . . ? Cu3 N33 C38 C39 45.5(18) . . . . ? C36 N33 C38 C43 40.3(18) . . . . ? Cu3 N33 C38 C43 -132.8(12) . . . . ? C43 C38 C39 C40 -8(2) . . . . ? N33 C38 C39 C40 173.7(12) . . . . ? C43 C38 C39 C45 175.4(13) . . . . ? N33 C38 C39 C45 -3(2) . . . . ? C38 C39 C40 C41 6(2) . . . . ? C45 C39 C40 C41 -177.8(13) . . . . ? C39 C40 C41 C42 0(2) . . . . ? C39 C40 C41 C44 -178.4(14) . . . . ? C40 C41 C42 C43 -3(2) . . . . ? C44 C41 C42 C43 175.2(14) . . . . ? C41 C42 C43 C38 1(2) . . . . ? C39 C38 C43 C42 5(2) . . . . ? N33 C38 C43 C42 -176.5(13) . . . . ? C48 N34 C46 C32 -176.5(12) . . . . ? Cu4 N34 C46 C32 -0.7(15) . . . . ? N32 C32 C46 N34 2.4(19) . . . . ? C33 C32 C46 N34 -178.2(13) . . . . ? C46 N34 C48 C53 38.9(18) . . . . ? Cu4 N34 C48 C53 -135.6(12) . . . . ? C46 N34 C48 C49 -145.2(13) . . . . ? Cu4 N34 C48 C49 40.3(19) . . . . ? N34 C48 C49 C50 -174.9(13) . . . . ? C53 C48 C49 C50 1(2) . . . . ? N34 C48 C49 C55 6(2) . . . . ? C53 C48 C49 C55 -177.7(13) . . . . ? C48 C49 C50 C51 1(2) . . . . ? C55 C49 C50 C51 -179.7(14) . . . . ? C49 C50 C51 C52 -3(2) . . . . ? C49 C50 C51 C54 177.2(14) . . . . ? C50 C51 C52 C53 1(2) . . . . ? C54 C51 C52 C53 -178.6(14) . . . . ? C51 C52 C53 C48 1(2) . . . . ? N34 C48 C53 C52 173.4(13) . . . . ? C49 C48 C53 C52 -3(2) . . . . ? N61 N62 C62 C63 0(2) . . . . ? Cu3 N62 C62 C63 -176.2(11) . . . . ? N61 N62 C62 C76 176.8(12) . . . . ? Cu3 N62 C62 C76 0.3(15) . . . . ? N62 C62 C63 C64 -1(2) . . . . ? C76 C62 C63 C64 -177.0(14) . . . . ? C62 C63 C64 C65 0(2) . . . . ? N62 N61 C65 C64 -2.5(19) . . . . ? Cu1 N61 C65 C64 178.5(10) . . . . ? N62 N61 C65 C66 -178.0(11) . . . . ? Cu1 N61 C65 C66 3.0(14) . . . . ? C63 C64 C65 N61 2(2) . . . . ? C63 C64 C65 C66 177.2(13) . . . . ? C68 N63 C66 C65 177.2(11) . . . . ? Cu1 N63 C66 C65 2.7(15) . . . . ? N61 C65 C66 N63 -3.9(18) . . . . ? C64 C65 C66 N63 -179.3(13) . . . . ? C66 N63 C68 C69 -41(2) . . . . ? Cu1 N63 C68 C69 132.7(12) . . . . ? C66 N63 C68 C73 140.6(13) . . . . ? Cu1 N63 C68 C73 -45.7(16) . . . . ? C73 C68 C69 C70 3(2) . . . . ? N63 C68 C69 C70 -175.0(12) . . . . ? C73 C68 C69 C75 177.3(13) . . . . ? N63 C68 C69 C75 -1(2) . . . . ? C68 C69 C70 C71 -5(2) . . . . ? C75 C69 C70 C71 -179.0(14) . . . . ? C69 C70 C71 C72 3(2) . . . . ? C69 C70 C71 C74 179.9(14) . . . . ? C70 C71 C72 C73 -1(2) . . . . ? C74 C71 C72 C73 -177.1(14) . . . . ? C71 C72 C73 C68 0(2) . . . . ? C69 C68 C73 C72 -1(2) . . . . ? N63 C68 C73 C72 177.5(12) . . . . ? C78 N64 C76 C62 173.9(12) . . . . ? Cu3 N64 C76 C62 -3.8(16) . . . . ? N62 C62 C76 N64 3(2) . . . . ? C63 C62 C76 N64 179.0(13) . . . . ? C76 N64 C78 C79 138.9(14) . . . . ? Cu3 N64 C78 C79 -44(2) . . . . ? C76 N64 C78 C83 -41.4(18) . . . . ? Cu3 N64 C78 C83 135.6(12) . . . . ? C83 C78 C79 C80 6(2) . . . . ? N64 C78 C79 C80 -174.4(13) . . . . ? C83 C78 C79 C85 180.0(13) . . . . ? N64 C78 C79 C85 0(2) . . . . ? C78 C79 C80 C81 -5(2) . . . . ? C85 C79 C80 C81 -179.5(14) . . . . ? C79 C80 C81 C82 1(2) . . . . ? C79 C80 C81 C84 179.6(15) . . . . ? C80 C81 C82 C83 3(2) . . . . ? C84 C81 C82 C83 -175.7(15) . . . . ? C81 C82 C83 C78 -2(2) . . . . ? C79 C78 C83 C82 -2(2) . . . . ? N64 C78 C83 C82 178.0(13) . . . . ? N91 N92 C92 C93 0(2) . . . . ? Cu4 N92 C92 C93 -178.9(11) . . . . ? N91 N92 C92 C106 180.0(11) . . . . ? Cu4 N92 C92 C106 1.2(15) . . . . ? N92 C92 C93 C94 -1(2) . . . . ? C106 C92 C93 C94 178.5(13) . . . . ? C92 C93 C94 C95 1(2) . . . . ? N92 N91 C95 C96 179.8(11) . . . . ? Cu2 N91 C95 C96 2.7(15) . . . . ? N92 N91 C95 C94 -1.8(19) . . . . ? Cu2 N91 C95 C94 -178.8(11) . . . . ? C93 C94 C95 N91 0(2) . . . . ? C93 C94 C95 C96 178.6(13) . . . . ? C98 N93 C96 C95 174.9(12) . . . . ? Cu2 N93 C96 C95 -6.4(16) . . . . ? N91 C95 C96 N93 3(2) . . . . ? C94 C95 C96 N93 -175.7(13) . . . . ? C96 N93 C98 C103 -39.8(18) . . . . ? Cu2 N93 C98 C103 141.9(12) . . . . ? C96 N93 C98 C99 141.3(14) . . . . ? Cu2 N93 C98 C99 -37(2) . . . . ? C103 C98 C99 C100 5(2) . . . . ? N93 C98 C99 C100 -176.4(13) . . . . ? C103 C98 C99 C105 179.2(14) . . . . ? N93 C98 C99 C105 -2(2) . . . . ? C98 C99 C100 C101 -4(2) . . . . ? C105 C99 C100 C101 -178.0(15) . . . . ? C99 C100 C101 C102 1(2) . . . . ? C99 C100 C101 C104 -176.9(16) . . . . ? C100 C101 C102 C103 1(2) . . . . ? C104 C101 C102 C103 178.5(16) . . . . ? C101 C102 C103 C98 0(2) . . . . ? C99 C98 C103 C102 -3(2) . . . . ? N93 C98 C103 C102 177.8(13) . . . . ? C118 N94 C106 C92 -178(3) . . . . ? C108 N94 C106 C92 173.0(17) . . . . ? Cu4 N94 C106 C92 1.0(16) . . . . ? N92 C92 C106 N94 -2(2) . . . . ? C93 C92 C106 N94 178.6(13) . . . . ? C106 N94 C108 C109 -41(3) . . . . ? C118 N94 C108 C109 165(16) . . . . ? Cu4 N94 C108 C109 128(2) . . . . ? C106 N94 C108 C113 145(2) . . . . ? C118 N94 C108 C113 -9(12) . . . . ? Cu4 N94 C108 C113 -46(4) . . . . ? C113 C108 C109 C110 -4(4) . . . . ? N94 C108 C109 C110 -178(2) . . . . ? C108 C109 C110 C111 -3(4) . . . . ? C109 C110 C111 C112 3(4) . . . . ? C109 C110 C111 C114 -175(2) . . . . ? C110 C111 C112 C113 3(4) . . . . ? C114 C111 C112 C113 -178(3) . . . . ? C111 C112 C113 C108 -10(4) . . . . ? C111 C112 C113 C115 180(2) . . . . ? C109 C108 C113 C112 10(4) . . . . ? N94 C108 C113 C112 -176(3) . . . . ? C109 C108 C113 C115 180(2) . . . . ? N94 C108 C113 C115 -6(4) . . . . ? C106 N94 C118 C119 -39(7) . . . . ? C108 N94 C118 C119 -8(10) . . . . ? Cu4 N94 C118 C119 142(4) . . . . ? C106 N94 C118 C123 133(4) . . . . ? C108 N94 C118 C123 164(19) . . . . ? Cu4 N94 C118 C123 -46(6) . . . . ? C123 C118 C119 C120 5(8) . . . . ? N94 C118 C119 C120 178(5) . . . . ? C123 C118 C119 C125 171(5) . . . . ? N94 C118 C119 C125 -16(7) . . . . ? C118 C119 C120 C121 -6(8) . . . . ? C125 C119 C120 C121 -170(5) . . . . ? C119 C120 C121 C122 -1(8) . . . . ? C119 C120 C121 C124 -176(4) . . . . ? C120 C121 C122 C123 8(7) . . . . ? C124 C121 C122 C123 -178(5) . . . . ? C121 C122 C123 C118 -8(7) . . . . ? C119 C118 C123 C122 2(8) . . . . ? N94 C118 C123 C122 -171(5) . . . . ? C136 C131 C132 C133 0.0 . . . . ? C131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C136 0.0 . . . . ? C134 C135 C136 C131 0.0 . . . . ? C132 C131 C136 C135 0.0 . . . . ? C146 C141 C142 C143 0.0 . . . . ? C141 C142 C143 C144 0.0 . . . . ? C142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 C146 0.0 . . . . ? C144 C145 C146 C141 0.0 . . . . ? C142 C141 C146 C145 0.0 . . . . ? C156 C151 C152 C153 0.0 . . . . ? C151 C152 C153 C154 0.0 . . . . ? C152 C153 C154 C155 0.0 . . . . ? C153 C154 C155 C156 0.0 . . . . ? C154 C155 C156 C151 0.0 . . . . ? C152 C151 C156 C155 0.0 . . . . ? C166 C161 C162 C163 0.0 . . . . ? C161 C162 C163 C164 0.0 . . . . ? C162 C163 C164 C165 0.0 . . . . ? C163 C164 C165 C166 0.0 . . . . ? C164 C165 C166 C161 0.0 . . . . ? C162 C161 C166 C165 0.0 . . . . ? 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 O170 H171 F41 0.86 2.52 3.38(4) 176.9 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 19.78 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.269 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.136