Electronic Supplementary Material for Chemical Communications This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof William Tolman' _publ_contact_author_address ; Department of Chemistry University of Minnesota 139 Smith Hall 207 Pleasant St. SE Minneapolis MN 55455 USA ; _publ_contact_author_email TOLMAN@CHEM.UMN.EDU _publ_section_title ; Reactivity of a 1:1 Copper-Oxygen Complex: Isolation of a Cu(II)-o-Iminosemiquinonato Species ; loop_ _publ_author_name 'William Tolman' 'Nermeen W. Aboelella' 'Elizabeth A. Lewis' 'Anne M. Reynolds' data_02198 _database_code_depnum_ccdc_archive 'CCDC 258882' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02198 _chemical_compound_source 'Elizabeth A. Lewis' _chemical_melting_point ? _chemical_formula_moiety 'C44 H52 Cu N4 O, C F3 O3 S, C4 H8 O' _chemical_formula_sum 'C49 H60 Cu F3 N4 O5 S' _chemical_formula_weight 937.61 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 29.967(3) _cell_length_b 13.6607(12) _cell_length_c 23.462(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.711(2) _cell_angle_gamma 90.00 _cell_volume 9593.9(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2505 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842308 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23905 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.06 _reflns_number_total 8490 _reflns_number_gt 4467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All hydrogen atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters, except for H1, located on N4, which was located from the E-map and refined. A highly disordered THF molecule, which could not be modeled, was removed using program PLATON, function SQUEEZE. It determined that there were 319 electrons in a volume of 1230.9 per unit cell. This corresponds to eight THF molecules, the expected number. Due to the removal of solvent, various fields in Table 1 are incorrect (e.g. F(100), density). The entire molecule is unique. The triflate anion is disordered over two positions (90:10). EADP and SAME restraints were placed on the triflate molecule to aid in modeling the disorder and refinement. ; _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^)+(0.0350P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8490 _refine_ls_number_parameters 562 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.152753(14) 0.00591(4) 0.124598(18) 0.03663(14) Uani 1 1 d . . . N1 N 0.09361(9) -0.0124(2) 0.15386(11) 0.0350(7) Uani 1 1 d . . . N2 N 0.13077(9) 0.1090(2) 0.07562(12) 0.0379(8) Uani 1 1 d . . . N3 N 0.18861(9) -0.1137(2) 0.13420(12) 0.0340(8) Uani 1 1 d . . . N4 N 0.18668(11) -0.1835(2) 0.09195(13) 0.0362(8) Uani 1 1 d . . . O1 O 0.20581(7) 0.0904(2) 0.13122(10) 0.0415(7) Uani 1 1 d . . . C1 C 0.01129(11) -0.0181(3) 0.14701(17) 0.0570(13) Uani 1 1 d . . . H1A H -0.0030 -0.0698 0.1236 0.085 Uiso 1 1 calc R . . H1B H -0.0075 0.0406 0.1454 0.085 Uiso 1 1 calc R . . H1C H 0.0151 -0.0406 0.1866 0.085 Uiso 1 1 calc R . . C2 C 0.05617(11) 0.0055(3) 0.12458(15) 0.0405(9) Uani 1 1 d . . . C3 C 0.05594(12) 0.0500(3) 0.06859(15) 0.0411(10) Uani 1 1 d . . . H3 H 0.0294 0.0429 0.0451 0.049 Uiso 1 1 calc R . . C4 C 0.08934(12) 0.0999(3) 0.04676(16) 0.0395(10) Uani 1 1 d . . . C5 C 0.08688(13) 0.1341(4) -0.01403(15) 0.0583(13) Uani 1 1 d . . . H5A H 0.0997 0.0841 -0.0383 0.088 Uiso 1 1 calc R . . H5B H 0.1037 0.1952 -0.0171 0.088 Uiso 1 1 calc R . . H5C H 0.0556 0.1452 -0.0264 0.088 Uiso 1 1 calc R . . C6 C 0.09306(11) -0.0479(3) 0.21153(15) 0.0391(10) Uani 1 1 d . . . C7 C 0.09150(11) -0.1483(3) 0.22265(16) 0.0434(11) Uani 1 1 d . . . C8 C 0.09305(12) -0.1770(4) 0.27953(17) 0.0548(12) Uani 1 1 d . . . H8 H 0.0919 -0.2447 0.2886 0.066 Uiso 1 1 calc R . . C9 C 0.09631(13) -0.1090(4) 0.32323(18) 0.0646(15) Uani 1 1 d . . . H9 H 0.0970 -0.1304 0.3618 0.078 Uiso 1 1 calc R . . C10 C 0.09853(12) -0.0094(4) 0.31099(17) 0.0579(12) Uani 1 1 d . . . H10 H 0.1010 0.0367 0.3413 0.070 Uiso 1 1 calc R . . C11 C 0.09712(12) 0.0229(3) 0.25526(16) 0.0466(11) Uani 1 1 d . . . C12 C 0.08756(13) -0.2257(3) 0.17668(17) 0.0475(11) Uani 1 1 d . . . H12 H 0.0906 -0.1925 0.1391 0.057 Uiso 1 1 calc R . . C13 C 0.04201(14) -0.2760(4) 0.1753(2) 0.0752(15) Uani 1 1 d . . . H13A H 0.0409 -0.3266 0.1457 0.113 Uiso 1 1 calc R . . H13B H 0.0185 -0.2275 0.1669 0.113 Uiso 1 1 calc R . . H13C H 0.0374 -0.3062 0.2125 0.113 Uiso 1 1 calc R . . C14 C 0.12414(14) -0.3023(3) 0.18308(17) 0.0602(13) Uani 1 1 d . . . H14A H 0.1223 -0.3465 0.1502 0.090 Uiso 1 1 calc R . . H14B H 0.1204 -0.3398 0.2181 0.090 Uiso 1 1 calc R . . H14C H 0.1534 -0.2699 0.1851 0.090 Uiso 1 1 calc R . . C15 C 0.09872(14) 0.1323(3) 0.24295(17) 0.0561(12) Uani 1 1 d . . . H15 H 0.0942 0.1415 0.2008 0.067 Uiso 1 1 calc R . . C16 C 0.14218(17) 0.1790(4) 0.2613(3) 0.110(2) Uani 1 1 d . . . H16A H 0.1414 0.2485 0.2510 0.165 Uiso 1 1 calc R . . H16B H 0.1665 0.1466 0.2421 0.165 Uiso 1 1 calc R . . H16C H 0.1471 0.1724 0.3027 0.165 Uiso 1 1 calc R . . C17 C 0.06179(18) 0.1861(4) 0.2713(3) 0.119(2) Uani 1 1 d . . . H17A H 0.0636 0.2561 0.2625 0.179 Uiso 1 1 calc R . . H17B H 0.0650 0.1766 0.3127 0.179 Uiso 1 1 calc R . . H17C H 0.0328 0.1606 0.2571 0.179 Uiso 1 1 calc R . . C18 C 0.15372(13) 0.1929(3) 0.08396(15) 0.0422(10) Uani 1 1 d . . . C19 C 0.14084(14) 0.2940(3) 0.07312(16) 0.0489(11) Uani 1 1 d . . . C20 C 0.17512(15) 0.3582(3) 0.07032(18) 0.0619(13) Uani 1 1 d . . . H20 H 0.1685 0.4243 0.0606 0.074 Uiso 1 1 calc R . . C21 C 0.22147(15) 0.3307(4) 0.08149(19) 0.0658(14) Uani 1 1 d . . . H21 H 0.2438 0.3789 0.0764 0.079 Uiso 1 1 calc R . . C22 C 0.23471(13) 0.2403(3) 0.09882(17) 0.0486(11) Uani 1 1 d . . . C23 C 0.19967(13) 0.1729(3) 0.10590(16) 0.0425(10) Uani 1 1 d . . . C24 C 0.09313(14) 0.3292(3) 0.07091(19) 0.0576(12) Uani 1 1 d . . . H24 H 0.0736 0.2715 0.0617 0.069 Uiso 1 1 calc R . . C25 C 0.08273(18) 0.4060(4) 0.0268(3) 0.121(2) Uani 1 1 d . . . H25A H 0.0508 0.4214 0.0261 0.181 Uiso 1 1 calc R . . H25B H 0.0906 0.3818 -0.0108 0.181 Uiso 1 1 calc R . . H25C H 0.1000 0.4652 0.0361 0.181 Uiso 1 1 calc R . . C26 C 0.08122(17) 0.3667(5) 0.1288(2) 0.119(2) Uani 1 1 d . . . H26A H 0.0503 0.3901 0.1269 0.178 Uiso 1 1 calc R . . H26B H 0.1012 0.4208 0.1402 0.178 Uiso 1 1 calc R . . H26C H 0.0844 0.3138 0.1569 0.178 Uiso 1 1 calc R . . C27 C 0.28184(13) 0.2106(3) 0.11648(19) 0.0565(12) Uani 1 1 d . . . H27 H 0.2854 0.1406 0.1050 0.068 Uiso 1 1 calc R . . C28 C 0.31613(14) 0.2694(4) 0.0856(2) 0.0857(18) Uani 1 1 d . . . H28A H 0.3456 0.2388 0.0913 0.129 Uiso 1 1 calc R . . H28B H 0.3172 0.3363 0.1007 0.129 Uiso 1 1 calc R . . H28C H 0.3077 0.2712 0.0447 0.129 Uiso 1 1 calc R . . C29 C 0.28947(14) 0.2149(4) 0.1803(2) 0.0722(14) Uani 1 1 d . . . H29A H 0.3204 0.1965 0.1907 0.108 Uiso 1 1 calc R . . H29B H 0.2691 0.1694 0.1982 0.108 Uiso 1 1 calc R . . H29C H 0.2839 0.2816 0.1936 0.108 Uiso 1 1 calc R . . C30 C 0.22704(12) -0.1345(3) 0.16504(15) 0.0359(9) Uani 1 1 d . . . C31 C 0.24740(12) -0.2162(3) 0.14181(15) 0.0395(10) Uani 1 1 d . . . H31 H 0.2744 -0.2463 0.1557 0.047 Uiso 1 1 calc R . . C32 C 0.22109(12) -0.2453(3) 0.09477(15) 0.0359(9) Uani 1 1 d . . . C33 C 0.24273(12) -0.0780(3) 0.21503(15) 0.0397(10) Uani 1 1 d . . . C34 C 0.21380(14) -0.0419(3) 0.25385(17) 0.0524(12) Uani 1 1 d . . . H34 H 0.1825 -0.0508 0.2477 0.063 Uiso 1 1 calc R . . C35 C 0.23066(15) 0.0076(4) 0.30211(17) 0.0618(12) Uani 1 1 d . . . H35 H 0.2108 0.0340 0.3284 0.074 Uiso 1 1 calc R . . C36 C 0.27602(15) 0.0184(3) 0.31176(18) 0.0615(13) Uani 1 1 d . . . H36 H 0.2874 0.0523 0.3447 0.074 Uiso 1 1 calc R . . C37 C 0.30434(15) -0.0193(4) 0.27427(19) 0.0676(14) Uani 1 1 d . . . H37 H 0.3357 -0.0130 0.2812 0.081 Uiso 1 1 calc R . . C38 C 0.28781(13) -0.0667(3) 0.22610(18) 0.0540(12) Uani 1 1 d . . . H38 H 0.3080 -0.0922 0.1999 0.065 Uiso 1 1 calc R . . C39 C 0.22766(13) -0.3245(3) 0.05452(15) 0.0386(10) Uani 1 1 d . . . C40 C 0.26882(14) -0.3693(3) 0.05258(16) 0.0450(10) Uani 1 1 d . . . H40 H 0.2926 -0.3482 0.0779 0.054 Uiso 1 1 calc R . . C41 C 0.27627(16) -0.4444(3) 0.01462(19) 0.0561(12) Uani 1 1 d . . . H41 H 0.3046 -0.4757 0.0144 0.067 Uiso 1 1 calc R . . C42 C 0.24250(19) -0.4725(3) -0.0223(2) 0.0666(14) Uani 1 1 d . . . H42 H 0.2475 -0.5231 -0.0490 0.080 Uiso 1 1 calc R . . C43 C 0.20087(17) -0.4287(4) -0.02168(19) 0.0683(14) Uani 1 1 d . . . H43 H 0.1775 -0.4491 -0.0477 0.082 Uiso 1 1 calc R . . C44 C 0.19369(14) -0.3550(3) 0.01720(17) 0.0532(12) Uani 1 1 d . . . H44 H 0.1651 -0.3252 0.0182 0.064 Uiso 1 1 calc R . . S1 S 0.09074(5) -0.16647(11) -0.03251(6) 0.0610(5) Uani 0.904(3) 1 d PD A 1 O2 O 0.11618(12) -0.2226(4) -0.07064(15) 0.0954(15) Uani 0.904(3) 1 d PD A 1 O3 O 0.11470(12) -0.1407(3) 0.02045(19) 0.0640(14) Uani 0.904(3) 1 d PD A 1 O4 O 0.0645(3) -0.0885(4) -0.0580(3) 0.0845(11) Uani 0.904(3) 1 d PD A 1 C50 C 0.0483(2) -0.2510(5) -0.0083(3) 0.0862(19) Uani 0.904(3) 1 d PD A 1 F1 F 0.02372(15) -0.2068(4) 0.0299(3) 0.124(2) Uani 0.904(3) 1 d PD A 1 F2 F 0.02190(14) -0.2792(4) -0.0514(2) 0.147(2) Uani 0.904(3) 1 d PD A 1 F3 F 0.06721(17) -0.3276(3) 0.0166(2) 0.1376(19) Uani 0.904(3) 1 d PD A 1 S1' S 0.0657(5) -0.1694(11) -0.0068(6) 0.0610(5) Uani 0.096(3) 1 d PD A 2 O2' O 0.0268(12) -0.167(4) 0.026(2) 0.0954(15) Uani 0.096(3) 1 d PD A 2 O3' O 0.1073(12) -0.175(3) 0.027(2) 0.0640(14) Uani 0.096(3) 1 d PD A 2 O4' O 0.066(3) -0.098(4) -0.052(2) 0.0845(11) Uani 0.096(3) 1 d PD A 2 C50' C 0.0654(11) -0.285(2) -0.0459(14) 0.0862(19) Uani 0.096(3) 1 d PD A 2 F1' F 0.0989(11) -0.284(3) -0.0805(15) 0.124(2) Uani 0.096(3) 1 d PD A 2 F2' F 0.0295(12) -0.298(4) -0.078(2) 0.147(2) Uani 0.096(3) 1 d PD A 2 F3' F 0.0762(18) -0.357(2) -0.0116(19) 0.1376(19) Uani 0.096(3) 1 d PD A 2 H1 H 0.1657(10) -0.181(2) 0.0653(13) 0.023(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0363(2) 0.0369(3) 0.0370(3) 0.0010(3) 0.00448(17) 0.0038(3) N1 0.0374(16) 0.035(2) 0.0325(16) -0.0023(16) 0.0002(13) 0.0053(16) N2 0.0392(18) 0.042(2) 0.0328(18) 0.0024(16) 0.0079(14) 0.0015(17) N3 0.0394(18) 0.033(2) 0.0293(18) -0.0023(15) 0.0022(14) 0.0057(16) N4 0.040(2) 0.037(2) 0.0316(19) -0.0010(16) -0.0007(16) 0.0035(17) O1 0.0366(14) 0.0399(19) 0.0482(17) -0.0006(14) 0.0037(12) 0.0022(13) C1 0.034(2) 0.074(4) 0.064(3) 0.017(3) 0.0007(18) 0.003(2) C2 0.039(2) 0.042(3) 0.041(2) 0.001(2) 0.0046(17) 0.004(2) C3 0.038(2) 0.050(3) 0.036(2) 0.001(2) -0.0009(17) 0.007(2) C4 0.043(2) 0.036(3) 0.040(2) 0.0040(19) 0.0024(19) 0.008(2) C5 0.056(3) 0.078(4) 0.041(3) 0.015(2) -0.003(2) -0.004(3) C6 0.034(2) 0.049(3) 0.034(2) 0.005(2) 0.0035(17) 0.003(2) C7 0.035(2) 0.063(3) 0.032(2) 0.010(2) 0.0011(18) 0.002(2) C8 0.049(3) 0.068(4) 0.047(3) 0.015(3) 0.009(2) 0.005(2) C9 0.051(3) 0.108(5) 0.035(3) 0.015(3) 0.009(2) 0.021(3) C10 0.051(2) 0.083(4) 0.040(3) -0.006(3) 0.0069(19) 0.017(3) C11 0.046(2) 0.057(3) 0.037(2) -0.004(2) 0.0053(18) 0.006(2) C12 0.053(3) 0.039(3) 0.050(3) 0.009(2) -0.002(2) -0.004(2) C13 0.071(3) 0.060(4) 0.093(4) 0.007(3) -0.012(3) -0.014(3) C14 0.077(3) 0.042(3) 0.061(3) 0.014(2) 0.006(2) 0.003(3) C15 0.072(3) 0.056(3) 0.040(3) -0.007(2) 0.002(2) 0.008(3) C16 0.073(4) 0.061(4) 0.196(7) -0.010(4) 0.001(4) -0.009(3) C17 0.100(4) 0.077(5) 0.184(7) 0.003(4) 0.039(4) 0.026(4) C18 0.045(2) 0.044(3) 0.039(2) 0.005(2) 0.0102(18) 0.006(2) C19 0.057(3) 0.039(3) 0.051(3) 0.009(2) 0.007(2) -0.001(2) C20 0.079(3) 0.036(3) 0.071(3) 0.017(2) 0.001(3) 0.003(3) C21 0.064(3) 0.062(4) 0.071(3) 0.012(3) 0.004(2) -0.020(3) C22 0.047(3) 0.044(3) 0.056(3) -0.001(2) 0.008(2) -0.008(2) C23 0.053(3) 0.033(3) 0.042(2) 0.000(2) 0.011(2) 0.005(2) C24 0.060(3) 0.037(3) 0.076(3) 0.013(2) 0.001(2) 0.015(2) C25 0.097(4) 0.090(5) 0.175(6) 0.076(5) 0.016(4) 0.031(4) C26 0.088(4) 0.159(7) 0.111(5) -0.034(5) 0.023(3) 0.040(4) C27 0.050(3) 0.055(3) 0.065(3) -0.007(2) 0.006(2) -0.010(2) C28 0.055(3) 0.122(5) 0.081(4) 0.000(3) 0.015(3) -0.026(3) C29 0.063(3) 0.069(4) 0.085(4) 0.004(3) -0.003(3) -0.007(3) C30 0.039(2) 0.038(3) 0.031(2) 0.0055(19) 0.0022(17) 0.004(2) C31 0.041(2) 0.038(3) 0.040(2) 0.002(2) 0.0015(19) 0.009(2) C32 0.042(2) 0.035(3) 0.032(2) 0.0029(19) 0.0074(18) 0.004(2) C33 0.049(2) 0.036(3) 0.034(2) 0.0012(19) -0.0039(18) 0.007(2) C34 0.053(3) 0.057(3) 0.046(3) -0.012(2) -0.005(2) 0.005(2) C35 0.078(3) 0.062(3) 0.045(3) -0.015(3) 0.001(2) 0.006(3) C36 0.070(3) 0.056(4) 0.056(3) -0.006(2) -0.024(2) 0.000(3) C37 0.057(3) 0.077(4) 0.067(3) -0.016(3) -0.016(2) 0.002(3) C38 0.044(3) 0.060(3) 0.058(3) -0.009(2) -0.003(2) 0.006(2) C39 0.054(2) 0.035(3) 0.028(2) 0.0042(19) 0.0101(19) -0.001(2) C40 0.063(3) 0.037(3) 0.036(2) 0.006(2) 0.014(2) 0.006(2) C41 0.070(3) 0.042(3) 0.059(3) 0.008(2) 0.028(3) 0.006(3) C42 0.100(4) 0.037(3) 0.067(3) -0.015(2) 0.043(3) -0.010(3) C43 0.084(4) 0.062(4) 0.060(3) -0.014(3) 0.011(3) -0.027(3) C44 0.065(3) 0.043(3) 0.052(3) -0.014(2) 0.006(2) 0.000(2) S1 0.0564(9) 0.0753(11) 0.0500(9) 0.0000(8) -0.0115(8) 0.0038(8) O2 0.082(3) 0.138(4) 0.066(3) -0.033(3) -0.002(2) 0.019(3) O3 0.058(2) 0.078(4) 0.054(2) -0.006(2) -0.0247(19) 0.009(2) O4 0.094(2) 0.085(3) 0.070(3) 0.022(2) -0.037(2) 0.017(2) C50 0.084(5) 0.052(5) 0.122(6) 0.001(4) -0.003(4) 0.004(4) F1 0.079(2) 0.149(5) 0.147(4) 0.022(4) 0.034(2) 0.015(3) F2 0.095(3) 0.126(4) 0.217(6) -0.059(4) -0.042(3) -0.024(3) F3 0.131(4) 0.071(3) 0.212(5) 0.048(3) 0.023(3) 0.011(3) S1' 0.0564(9) 0.0753(11) 0.0500(9) 0.0000(8) -0.0115(8) 0.0038(8) O2' 0.082(3) 0.138(4) 0.066(3) -0.033(3) -0.002(2) 0.019(3) O3' 0.058(2) 0.078(4) 0.054(2) -0.006(2) -0.0247(19) 0.009(2) O4' 0.094(2) 0.085(3) 0.070(3) 0.022(2) -0.037(2) 0.017(2) C50' 0.084(5) 0.052(5) 0.122(6) 0.001(4) -0.003(4) 0.004(4) F1' 0.079(2) 0.149(5) 0.147(4) 0.022(4) 0.034(2) 0.015(3) F2' 0.095(3) 0.126(4) 0.217(6) -0.059(4) -0.042(3) -0.024(3) F3' 0.131(4) 0.071(3) 0.212(5) 0.048(3) 0.023(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.915(3) . ? Cu1 N1 1.947(3) . ? Cu1 N3 1.963(3) . ? Cu1 O1 1.965(2) . ? N1 C2 1.310(4) . ? N1 C6 1.438(4) . ? N2 C18 1.346(5) . ? N2 C4 1.391(4) . ? N3 C30 1.361(4) . ? N3 N4 1.375(4) . ? N4 C32 1.332(4) . ? O1 C23 1.284(4) . ? C1 C2 1.502(5) . ? C2 C3 1.447(5) . ? C3 C4 1.333(5) . ? C4 C5 1.499(5) . ? C6 C7 1.397(5) . ? C6 C11 1.411(5) . ? C7 C8 1.390(5) . ? C7 C12 1.511(5) . ? C8 C9 1.383(6) . ? C9 C10 1.394(6) . ? C10 C11 1.379(5) . ? C11 C15 1.523(6) . ? C12 C14 1.517(5) . ? C12 C13 1.527(5) . ? C15 C16 1.495(6) . ? C15 C17 1.509(6) . ? C18 C19 1.453(5) . ? C18 C23 1.473(5) . ? C19 C20 1.355(5) . ? C19 C24 1.507(5) . ? C20 C21 1.451(6) . ? C21 C22 1.355(6) . ? C22 C23 1.412(5) . ? C22 C27 1.508(5) . ? C24 C25 1.498(6) . ? C24 C26 1.511(6) . ? C27 C29 1.506(5) . ? C27 C28 1.516(5) . ? C30 C31 1.395(5) . ? C30 C33 1.463(5) . ? C31 C32 1.384(5) . ? C32 C39 1.455(5) . ? C33 C38 1.372(5) . ? C33 C34 1.378(5) . ? C34 C35 1.393(5) . ? C35 C36 1.375(5) . ? C36 C37 1.353(6) . ? C37 C38 1.374(5) . ? C39 C44 1.376(5) . ? C39 C40 1.380(5) . ? C40 C41 1.384(5) . ? C41 C42 1.356(6) . ? C42 C43 1.384(6) . ? C43 C44 1.382(6) . ? S1 O2 1.426(4) . ? S1 O4 1.437(6) . ? S1 O3 1.449(4) . ? S1 C50 1.828(7) . ? C50 F2 1.311(7) . ? C50 F3 1.314(7) . ? C50 F1 1.331(7) . ? S1' O2' 1.422(18) . ? S1' O4' 1.446(19) . ? S1' O3' 1.449(18) . ? S1' C50' 1.824(18) . ? C50' F2' 1.295(19) . ? C50' F3' 1.306(19) . ? C50' F1' 1.320(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 90.74(12) . . ? N2 Cu1 N3 148.45(12) . . ? N1 Cu1 N3 110.80(12) . . ? N2 Cu1 O1 82.51(12) . . ? N1 Cu1 O1 142.60(11) . . ? N3 Cu1 O1 92.48(12) . . ? C2 N1 C6 120.5(3) . . ? C2 N1 Cu1 124.2(2) . . ? C6 N1 Cu1 115.2(2) . . ? C18 N2 C4 125.8(3) . . ? C18 N2 Cu1 112.3(2) . . ? C4 N2 Cu1 120.0(3) . . ? C30 N3 N4 104.1(3) . . ? C30 N3 Cu1 132.8(3) . . ? N4 N3 Cu1 119.4(2) . . ? C32 N4 N3 113.4(3) . . ? C23 O1 Cu1 112.4(2) . . ? N1 C2 C3 121.4(3) . . ? N1 C2 C1 122.3(3) . . ? C3 C2 C1 116.2(3) . . ? C4 C3 C2 126.3(3) . . ? C3 C4 N2 121.8(3) . . ? C3 C4 C5 121.4(3) . . ? N2 C4 C5 116.0(3) . . ? C7 C6 C11 122.7(4) . . ? C7 C6 N1 120.6(4) . . ? C11 C6 N1 116.6(4) . . ? C8 C7 C6 117.2(4) . . ? C8 C7 C12 119.0(4) . . ? C6 C7 C12 123.8(3) . . ? C9 C8 C7 121.3(5) . . ? C8 C9 C10 120.4(4) . . ? C11 C10 C9 120.5(4) . . ? C10 C11 C6 117.9(4) . . ? C10 C11 C15 119.6(4) . . ? C6 C11 C15 122.5(4) . . ? C7 C12 C14 112.3(3) . . ? C7 C12 C13 111.7(3) . . ? C14 C12 C13 109.4(3) . . ? C16 C15 C17 108.2(4) . . ? C16 C15 C11 113.5(4) . . ? C17 C15 C11 111.4(4) . . ? N2 C18 C19 130.8(4) . . ? N2 C18 C23 110.9(4) . . ? C19 C18 C23 118.3(4) . . ? C20 C19 C18 115.4(4) . . ? C20 C19 C24 120.8(4) . . ? C18 C19 C24 123.6(4) . . ? C19 C20 C21 123.0(4) . . ? C22 C21 C20 123.7(4) . . ? C21 C22 C23 114.9(4) . . ? C21 C22 C27 125.8(4) . . ? C23 C22 C27 119.0(4) . . ? O1 C23 C22 122.4(4) . . ? O1 C23 C18 115.8(4) . . ? C22 C23 C18 121.8(4) . . ? C25 C24 C19 114.4(4) . . ? C25 C24 C26 109.5(5) . . ? C19 C24 C26 110.0(4) . . ? C29 C27 C22 111.0(3) . . ? C29 C27 C28 112.4(4) . . ? C22 C27 C28 111.9(4) . . ? N3 C30 C31 109.5(3) . . ? N3 C30 C33 123.2(3) . . ? C31 C30 C33 127.3(3) . . ? C32 C31 C30 107.3(3) . . ? N4 C32 C31 105.6(3) . . ? N4 C32 C39 124.5(3) . . ? C31 C32 C39 129.9(4) . . ? C38 C33 C34 118.6(4) . . ? C38 C33 C30 119.1(4) . . ? C34 C33 C30 122.0(3) . . ? C33 C34 C35 119.7(4) . . ? C36 C35 C34 120.2(4) . . ? C37 C36 C35 119.8(4) . . ? C36 C37 C38 120.1(4) . . ? C33 C38 C37 121.5(4) . . ? C44 C39 C40 118.7(4) . . ? C44 C39 C32 121.3(4) . . ? C40 C39 C32 120.0(4) . . ? C39 C40 C41 121.5(4) . . ? C42 C41 C40 118.9(4) . . ? C41 C42 C43 121.1(4) . . ? C44 C43 C42 119.3(4) . . ? C39 C44 C43 120.5(4) . . ? O2 S1 O4 115.8(4) . . ? O2 S1 O3 114.2(3) . . ? O4 S1 O3 114.5(4) . . ? O2 S1 C50 104.8(3) . . ? O4 S1 C50 102.9(4) . . ? O3 S1 C50 102.2(3) . . ? F2 C50 F3 109.9(6) . . ? F2 C50 F1 108.6(6) . . ? F3 C50 F1 107.6(6) . . ? F2 C50 S1 110.5(5) . . ? F3 C50 S1 110.5(5) . . ? F1 C50 S1 109.7(5) . . ? O2' S1' O4' 114(3) . . ? O2' S1' O3' 114(2) . . ? O4' S1' O3' 114(3) . . ? O2' S1' C50' 108(2) . . ? O4' S1' C50' 102(2) . . ? O3' S1' C50' 102.5(19) . . ? F2' C50' F3' 115(3) . . ? F2' C50' F1' 106(3) . . ? F3' C50' F1' 102(2) . . ? F2' C50' S1' 113(2) . . ? F3' C50' S1' 111(2) . . ? F1' C50' S1' 108(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 N2 Cu1 N1 C2 29.4(3) . . . . ? N3 Cu1 N1 C2 -127.1(3) . . . . ? O1 Cu1 N1 C2 108.0(3) . . . . ? N2 Cu1 N1 C6 -150.6(3) . . . . ? N3 Cu1 N1 C6 52.9(3) . . . . ? O1 Cu1 N1 C6 -72.0(3) . . . . ? N1 Cu1 N2 C18 124.3(3) . . . . ? N3 Cu1 N2 C18 -101.3(3) . . . . ? O1 Cu1 N2 C18 -18.8(2) . . . . ? N1 Cu1 N2 C4 -41.1(3) . . . . ? N3 Cu1 N2 C4 93.3(3) . . . . ? O1 Cu1 N2 C4 175.8(3) . . . . ? N2 Cu1 N3 C30 113.3(3) . . . . ? N1 Cu1 N3 C30 -116.5(3) . . . . ? O1 Cu1 N3 C30 33.6(3) . . . . ? N2 Cu1 N3 N4 -41.4(4) . . . . ? N1 Cu1 N3 N4 88.8(3) . . . . ? O1 Cu1 N3 N4 -121.1(2) . . . . ? C30 N3 N4 C32 0.0(4) . . . . ? Cu1 N3 N4 C32 161.1(2) . . . . ? N2 Cu1 O1 C23 5.8(2) . . . . ? N1 Cu1 O1 C23 -75.6(3) . . . . ? N3 Cu1 O1 C23 154.5(3) . . . . ? C6 N1 C2 C3 174.0(4) . . . . ? Cu1 N1 C2 C3 -6.0(5) . . . . ? C6 N1 C2 C1 -5.6(6) . . . . ? Cu1 N1 C2 C1 174.4(3) . . . . ? N1 C2 C3 C4 -18.6(7) . . . . ? C1 C2 C3 C4 161.0(4) . . . . ? C2 C3 C4 N2 4.6(6) . . . . ? C2 C3 C4 C5 173.8(4) . . . . ? C18 N2 C4 C3 -131.8(4) . . . . ? Cu1 N2 C4 C3 31.5(5) . . . . ? C18 N2 C4 C5 58.5(5) . . . . ? Cu1 N2 C4 C5 -138.3(3) . . . . ? C2 N1 C6 C7 89.0(5) . . . . ? Cu1 N1 C6 C7 -91.0(4) . . . . ? C2 N1 C6 C11 -95.1(4) . . . . ? Cu1 N1 C6 C11 84.9(3) . . . . ? C11 C6 C7 C8 1.5(5) . . . . ? N1 C6 C7 C8 177.2(3) . . . . ? C11 C6 C7 C12 -179.4(3) . . . . ? N1 C6 C7 C12 -3.7(5) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C12 C7 C8 C9 -179.5(4) . . . . ? C7 C8 C9 C10 -0.6(6) . . . . ? C8 C9 C10 C11 0.6(6) . . . . ? C9 C10 C11 C6 0.5(6) . . . . ? C9 C10 C11 C15 178.8(4) . . . . ? C7 C6 C11 C10 -1.5(5) . . . . ? N1 C6 C11 C10 -177.4(3) . . . . ? C7 C6 C11 C15 -179.9(4) . . . . ? N1 C6 C11 C15 4.3(5) . . . . ? C8 C7 C12 C14 -54.8(5) . . . . ? C6 C7 C12 C14 126.1(4) . . . . ? C8 C7 C12 C13 68.6(4) . . . . ? C6 C7 C12 C13 -110.4(4) . . . . ? C10 C11 C15 C16 66.3(5) . . . . ? C6 C11 C15 C16 -115.4(5) . . . . ? C10 C11 C15 C17 -56.1(5) . . . . ? C6 C11 C15 C17 122.2(4) . . . . ? C4 N2 C18 C19 8.9(6) . . . . ? Cu1 N2 C18 C19 -155.5(3) . . . . ? C4 N2 C18 C23 -168.8(3) . . . . ? Cu1 N2 C18 C23 26.9(4) . . . . ? N2 C18 C19 C20 -161.3(4) . . . . ? C23 C18 C19 C20 16.2(5) . . . . ? N2 C18 C19 C24 24.7(7) . . . . ? C23 C18 C19 C24 -157.8(4) . . . . ? C18 C19 C20 C21 -4.5(6) . . . . ? C24 C19 C20 C21 169.6(4) . . . . ? C19 C20 C21 C22 -3.9(7) . . . . ? C20 C21 C22 C23 -0.5(7) . . . . ? C20 C21 C22 C27 -173.7(4) . . . . ? Cu1 O1 C23 C22 -171.9(3) . . . . ? Cu1 O1 C23 C18 7.5(4) . . . . ? C21 C22 C23 O1 -167.7(4) . . . . ? C27 C22 C23 O1 6.0(6) . . . . ? C21 C22 C23 C18 13.0(6) . . . . ? C27 C22 C23 C18 -173.3(4) . . . . ? N2 C18 C23 O1 -22.9(5) . . . . ? C19 C18 C23 O1 159.1(3) . . . . ? N2 C18 C23 C22 156.4(4) . . . . ? C19 C18 C23 C22 -21.6(6) . . . . ? C20 C19 C24 C25 43.6(6) . . . . ? C18 C19 C24 C25 -142.7(5) . . . . ? C20 C19 C24 C26 -80.0(5) . . . . ? C18 C19 C24 C26 93.6(5) . . . . ? C21 C22 C27 C29 96.2(5) . . . . ? C23 C22 C27 C29 -76.8(5) . . . . ? C21 C22 C27 C28 -30.3(6) . . . . ? C23 C22 C27 C28 156.8(4) . . . . ? N4 N3 C30 C31 -0.6(4) . . . . ? Cu1 N3 C30 C31 -158.0(3) . . . . ? N4 N3 C30 C33 -180.0(3) . . . . ? Cu1 N3 C30 C33 22.6(5) . . . . ? N3 C30 C31 C32 1.0(4) . . . . ? C33 C30 C31 C32 -179.7(4) . . . . ? N3 N4 C32 C31 0.6(4) . . . . ? N3 N4 C32 C39 -178.6(3) . . . . ? C30 C31 C32 N4 -1.0(4) . . . . ? C30 C31 C32 C39 178.1(4) . . . . ? N3 C30 C33 C38 -146.8(4) . . . . ? C31 C30 C33 C38 34.0(6) . . . . ? N3 C30 C33 C34 38.3(6) . . . . ? C31 C30 C33 C34 -140.9(4) . . . . ? C38 C33 C34 C35 2.1(6) . . . . ? C30 C33 C34 C35 177.0(4) . . . . ? C33 C34 C35 C36 -1.6(7) . . . . ? C34 C35 C36 C37 0.0(7) . . . . ? C35 C36 C37 C38 1.2(8) . . . . ? C34 C33 C38 C37 -1.0(7) . . . . ? C30 C33 C38 C37 -176.1(4) . . . . ? C36 C37 C38 C33 -0.7(7) . . . . ? N4 C32 C39 C44 -14.3(6) . . . . ? C31 C32 C39 C44 166.7(4) . . . . ? N4 C32 C39 C40 164.5(3) . . . . ? C31 C32 C39 C40 -14.5(6) . . . . ? C44 C39 C40 C41 -0.8(6) . . . . ? C32 C39 C40 C41 -179.6(3) . . . . ? C39 C40 C41 C42 1.6(6) . . . . ? C40 C41 C42 C43 -1.2(7) . . . . ? C41 C42 C43 C44 0.1(7) . . . . ? C40 C39 C44 C43 -0.4(6) . . . . ? C32 C39 C44 C43 178.4(4) . . . . ? C42 C43 C44 C39 0.8(7) . . . . ? O2 S1 C50 F2 -63.1(5) . . . . ? O4 S1 C50 F2 58.4(6) . . . . ? O3 S1 C50 F2 177.4(5) . . . . ? O2 S1 C50 F3 58.7(6) . . . . ? O4 S1 C50 F3 -179.8(6) . . . . ? O3 S1 C50 F3 -60.8(6) . . . . ? O2 S1 C50 F1 177.2(5) . . . . ? O4 S1 C50 F1 -61.3(6) . . . . ? O3 S1 C50 F1 57.7(5) . . . . ? O2' S1' C50' F2' 56(4) . . . . ? O4' S1' C50' F2' -64(4) . . . . ? O3' S1' C50' F2' 177(4) . . . . ? O2' S1' C50' F3' -75(4) . . . . ? O4' S1' C50' F3' 165(4) . . . . ? O3' S1' C50' F3' 46(3) . . . . ? O2' S1' C50' F1' 174(3) . . . . ? O4' S1' C50' F1' 53(4) . . . . ? O3' S1' C50' F1' -65(3) . . . . ? 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 N4 H1 O3 0.87(3) 1.89(3) 2.733(5) 162(3) . N4 H1 O3' 0.87(3) 1.93(4) 2.76(2) 161(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.306 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.063 #===END data_04248 _database_code_depnum_ccdc_archive 'CCDC 258883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(Me2LiPr2)Cu(PMePh2)' ; _chemical_name_common (Me2LiPr2)Cu(PMePh2) _chemical_compound_source 'Anne M. Reynolds' _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 Cu N2 P' _chemical_formula_sum 'C42 H54 Cu N2 P' _chemical_formula_weight 681.38 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6105(10) _cell_length_b 21.0202(12) _cell_length_c 15.9832(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.837(2) _cell_angle_gamma 90.00 _cell_volume 3864(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4008 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.04 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859901 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37565 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6828 _reflns_number_gt 5456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'Sir 97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0289P)^2^+3.1924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6828 _refine_ls_number_parameters 435 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.039 _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 0.78703(3) 0.256949(13) 0.389491(18) 0.02643(9) Uani 1 1 d . A . N1 N 0.72060(17) 0.21588(9) 0.48237(12) 0.0271(5) Uani 1 1 d . . . N2 N 0.83589(17) 0.33611(9) 0.44609(12) 0.0260(5) Uani 1 1 d . . . P1 P 0.78524(6) 0.21502(3) 0.26607(4) 0.02972(17) Uani 1 1 d . . . C1 C 0.6790(3) 0.20858(14) 0.62962(16) 0.0425(7) Uani 1 1 d . . . H1A H 0.6070 0.1872 0.6057 0.064 Uiso 1 1 calc R . . H1B H 0.6616 0.2407 0.6706 0.064 Uiso 1 1 calc R . . H1C H 0.7334 0.1772 0.6580 0.064 Uiso 1 1 calc R . . C2 C 0.7334(2) 0.24056(12) 0.55942(15) 0.0308(6) Uani 1 1 d . . . C3 C 0.7939(2) 0.29769(12) 0.58091(15) 0.0311(6) Uani 1 1 d . . . H3 H 0.8087 0.3065 0.6397 0.037 Uiso 1 1 calc R . . C4 C 0.8354(2) 0.34338(12) 0.52887(16) 0.0286(6) Uani 1 1 d . . . C5 C 0.8785(3) 0.40506(13) 0.57149(17) 0.0415(7) Uani 1 1 d . . . H5A H 0.9613 0.4105 0.5669 0.062 Uiso 1 1 calc R . . H5B H 0.8677 0.4037 0.6312 0.062 Uiso 1 1 calc R . . H5C H 0.8345 0.4408 0.5439 0.062 Uiso 1 1 calc R . . C6 C 0.6456(2) 0.16239(12) 0.46172(15) 0.0291(6) Uani 1 1 d . . . C7 C 0.6850(2) 0.10032(13) 0.47862(18) 0.0381(7) Uani 1 1 d . . . C8 C 0.6112(3) 0.04978(14) 0.4522(2) 0.0479(8) Uani 1 1 d . . . H8 H 0.6370 0.0074 0.4637 0.057 Uiso 1 1 calc R . . C9 C 0.5010(3) 0.06041(15) 0.40960(18) 0.0466(8) Uani 1 1 d . . . H9 H 0.4514 0.0255 0.3924 0.056 Uiso 1 1 calc R . . C10 C 0.4638(2) 0.12145(15) 0.39236(18) 0.0413(7) Uani 1 1 d . . . H10 H 0.3880 0.1283 0.3630 0.050 Uiso 1 1 calc R . . C11 C 0.5342(2) 0.17354(13) 0.41674(16) 0.0318(6) Uani 1 1 d . . . C12 C 0.8110(3) 0.04152(17) 0.5965(2) 0.0775(12) Uani 1 1 d . . . H12A H 0.8919 0.0344 0.6213 0.116 Uiso 1 1 calc R . . H12B H 0.7751 0.0008 0.5780 0.116 Uiso 1 1 calc R . . H12C H 0.7681 0.0608 0.6388 0.116 Uiso 1 1 calc R . . C13 C 0.8077(3) 0.08616(14) 0.5206(2) 0.0565(9) Uani 1 1 d . . . H13 H 0.8443 0.1273 0.5412 0.068 Uiso 1 1 calc R . . C14 C 0.8791(3) 0.05866(18) 0.4552(3) 0.0788(13) Uani 1 1 d . . . H14A H 0.9584 0.0499 0.4823 0.118 Uiso 1 1 calc R . . H14B H 0.8815 0.0894 0.4094 0.118 Uiso 1 1 calc R . . H14C H 0.8431 0.0191 0.4322 0.118 Uiso 1 1 calc R . . C15 C 0.4442(3) 0.27251(17) 0.4673(2) 0.0672(11) Uani 1 1 d . . . H15A H 0.4195 0.3158 0.4509 0.101 Uiso 1 1 calc R . . H15B H 0.5040 0.2741 0.5169 0.101 Uiso 1 1 calc R . . H15C H 0.3773 0.2482 0.4811 0.101 Uiso 1 1 calc R . . C16 C 0.4933(2) 0.24074(14) 0.39511(18) 0.0418(7) Uani 1 1 d . . . H16 H 0.5637 0.2657 0.3856 0.050 Uiso 1 1 calc R . . C17 C 0.4071(3) 0.24641(17) 0.31414(19) 0.0604(9) Uani 1 1 d . . . H17A H 0.3858 0.2912 0.3042 0.091 Uiso 1 1 calc R . . H17B H 0.3372 0.2216 0.3199 0.091 Uiso 1 1 calc R . . H17C H 0.4430 0.2301 0.2664 0.091 Uiso 1 1 calc R . . C18 C 0.8640(2) 0.38903(11) 0.39565(15) 0.0283(6) Uani 1 1 d . . . C19 C 0.9799(2) 0.40209(12) 0.38561(16) 0.0313(6) Uani 1 1 d . . . C20 C 1.0020(3) 0.45126(13) 0.33177(17) 0.0406(7) Uani 1 1 d . . . H20 H 1.0801 0.4602 0.3240 0.049 Uiso 1 1 calc R . . C21 C 0.9133(3) 0.48740(13) 0.28942(18) 0.0465(8) Uani 1 1 d . . . H21 H 0.9302 0.5210 0.2532 0.056 Uiso 1 1 calc R . . C22 C 0.8004(3) 0.47426(13) 0.3003(2) 0.0480(8) Uani 1 1 d . . . H22 H 0.7397 0.4995 0.2714 0.058 Uiso 1 1 calc R . . C23 C 0.7722(2) 0.42532(12) 0.35203(18) 0.0373(7) Uani 1 1 d . . . C24 C 1.1739(3) 0.40331(16) 0.4801(2) 0.0560(9) Uani 1 1 d . . . H24A H 1.2354 0.3756 0.5080 0.084 Uiso 1 1 calc R . . H24B H 1.1399 0.4278 0.5228 0.084 Uiso 1 1 calc R . . H24C H 1.2070 0.4326 0.4419 0.084 Uiso 1 1 calc R . . C25 C 1.0796(2) 0.36273(13) 0.42941(18) 0.0391(7) Uani 1 1 d . . . H25 H 1.0475 0.3333 0.4696 0.047 Uiso 1 1 calc R . . C26 C 1.1326(3) 0.32219(16) 0.3651(2) 0.0618(10) Uani 1 1 d . . . H26A H 1.1960 0.2964 0.3943 0.093 Uiso 1 1 calc R . . H26B H 1.1631 0.3500 0.3240 0.093 Uiso 1 1 calc R . . H26C H 1.0729 0.2942 0.3357 0.093 Uiso 1 1 calc R . . C27 C 0.6005(3) 0.4582(2) 0.4225(3) 0.0921(14) Uani 1 1 d . . . H27A H 0.5194 0.4479 0.4274 0.138 Uiso 1 1 calc R . . H27B H 0.6051 0.5016 0.4009 0.138 Uiso 1 1 calc R . . H27C H 0.6475 0.4550 0.4781 0.138 Uiso 1 1 calc R . . C28 C 0.6462(3) 0.41199(15) 0.3623(2) 0.0529(9) Uani 1 1 d . . . H28 H 0.6431 0.3685 0.3871 0.063 Uiso 1 1 calc R . . C29 C 0.5670(3) 0.4119(2) 0.2783(3) 0.0952(15) Uani 1 1 d . . . H29A H 0.4870 0.4030 0.2880 0.143 Uiso 1 1 calc R . . H29B H 0.5927 0.3790 0.2415 0.143 Uiso 1 1 calc R . . H29C H 0.5701 0.4536 0.2513 0.143 Uiso 1 1 calc R . . C30 C 0.764(2) 0.2745(14) 0.178(2) 0.028(2) Uani 0.50 1 d PD A 1 C31 C 0.8466(11) 0.3218(9) 0.1743(12) 0.040(2) Uani 0.50 1 d PD A 1 H31A H 0.9148 0.3232 0.2145 0.048 Uiso 0.50 1 calc PR A 1 C32 C 0.8279(11) 0.3669(8) 0.1109(12) 0.060(3) Uani 0.50 1 d PD A 1 H32A H 0.8841 0.3993 0.1075 0.072 Uiso 0.50 1 calc PR A 1 C33 C 0.7287(11) 0.3654(7) 0.0524(10) 0.065(3) Uani 0.50 1 d PD A 1 H33A H 0.7162 0.3977 0.0105 0.078 Uiso 0.50 1 calc PR A 1 C34 C 0.6480(10) 0.3179(7) 0.0541(9) 0.058(3) Uani 0.50 1 d PD A 1 H34A H 0.5818 0.3157 0.0122 0.070 Uiso 0.50 1 calc PR A 1 C35 C 0.6652(13) 0.2727(7) 0.1187(11) 0.043(2) Uani 0.50 1 d PD A 1 H35A H 0.6086 0.2405 0.1221 0.051 Uiso 0.50 1 calc PR A 1 C30' C 0.739(2) 0.2643(14) 0.176(2) 0.028(2) Uani 0.50 1 d PD A 2 C31' C 0.8077(11) 0.3171(9) 0.1654(12) 0.040(2) Uani 0.50 1 d PD A 2 H31B H 0.8773 0.3231 0.2032 0.048 Uiso 0.50 1 calc PR A 2 C32' C 0.7785(11) 0.3614(8) 0.1018(12) 0.060(3) Uani 0.50 1 d PD A 2 H32B H 0.8280 0.3964 0.0947 0.072 Uiso 0.50 1 calc PR A 2 C33' C 0.6751(11) 0.3530(6) 0.0492(9) 0.065(3) Uani 0.50 1 d PD A 2 H33B H 0.6541 0.3819 0.0040 0.078 Uiso 0.50 1 calc PR A 2 C34' C 0.6021(10) 0.3034(7) 0.0614(9) 0.058(3) Uani 0.50 1 d PD A 2 H34B H 0.5280 0.3007 0.0280 0.070 Uiso 0.50 1 calc PR A 2 C35' C 0.6354(13) 0.2573(7) 0.1220(12) 0.043(2) Uani 0.50 1 d PD A 2 H35B H 0.5876 0.2212 0.1267 0.051 Uiso 0.50 1 calc PR A 2 C36 C 0.9213(2) 0.17720(12) 0.24841(15) 0.0292(6) Uani 1 1 d D A . C37 C 1.0071(2) 0.16737(14) 0.31611(18) 0.0443(7) Uani 1 1 d D . . H37 H 0.9968 0.1833 0.3702 0.053 Uiso 1 1 calc R A . C38 C 1.1078(3) 0.13458(17) 0.3060(2) 0.0583(9) Uani 1 1 d D A . H38 H 1.1659 0.1283 0.3531 0.070 Uiso 1 1 calc R . . C39 C 1.1240(3) 0.11139(16) 0.2291(2) 0.0581(9) Uani 1 1 d D . . H39 H 1.1925 0.0882 0.2227 0.070 Uiso 1 1 calc R A . C40 C 1.0411(3) 0.12156(16) 0.1607(2) 0.0554(9) Uani 1 1 d D A . H40 H 1.0530 0.1062 0.1067 0.066 Uiso 1 1 calc R . . C41 C 0.9400(3) 0.15415(14) 0.17007(17) 0.0428(7) Uani 1 1 d D . . H41 H 0.8829 0.1608 0.1224 0.051 Uiso 1 1 calc R A . C42 C 0.6833(2) 0.14928(14) 0.24131(18) 0.0433(7) Uani 1 1 d . A . H42A H 0.6951 0.1176 0.2866 0.065 Uiso 1 1 calc R . . H42B H 0.6966 0.1296 0.1879 0.065 Uiso 1 1 calc R . . H42C H 0.6034 0.1654 0.2361 0.065 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 0.02997(17) 0.02421(17) 0.02461(16) -0.00276(13) 0.00200(12) -0.00135(14) N1 0.0272(11) 0.0271(11) 0.0257(11) 0.0021(9) -0.0007(9) -0.0012(9) N2 0.0288(12) 0.0234(11) 0.0251(11) -0.0003(9) 0.0009(9) -0.0002(9) P1 0.0337(4) 0.0281(4) 0.0268(4) -0.0048(3) 0.0021(3) -0.0028(3) C1 0.0484(18) 0.0500(18) 0.0283(15) 0.0022(13) 0.0027(13) -0.0114(14) C2 0.0305(14) 0.0350(15) 0.0256(13) 0.0042(11) -0.0007(11) 0.0015(12) C3 0.0355(15) 0.0359(15) 0.0202(13) -0.0027(11) -0.0020(11) -0.0012(12) C4 0.0270(14) 0.0294(14) 0.0282(14) -0.0049(11) -0.0013(11) 0.0014(11) C5 0.0575(19) 0.0342(16) 0.0319(15) -0.0100(12) 0.0029(14) -0.0067(14) C6 0.0306(15) 0.0312(14) 0.0259(14) -0.0017(11) 0.0057(11) -0.0058(11) C7 0.0363(16) 0.0318(16) 0.0442(17) 0.0032(13) -0.0017(13) -0.0067(12) C8 0.052(2) 0.0338(16) 0.058(2) -0.0019(14) 0.0064(16) -0.0099(14) C9 0.0438(19) 0.051(2) 0.0455(18) -0.0109(15) 0.0067(15) -0.0224(15) C10 0.0290(16) 0.057(2) 0.0374(16) -0.0050(14) 0.0047(13) -0.0091(14) C11 0.0264(14) 0.0434(16) 0.0261(14) -0.0038(12) 0.0059(11) -0.0030(12) C12 0.082(3) 0.058(2) 0.082(3) 0.016(2) -0.026(2) 0.004(2) C13 0.0444(19) 0.0303(17) 0.089(3) 0.0087(17) -0.0117(18) -0.0021(14) C14 0.042(2) 0.066(3) 0.127(4) 0.033(2) 0.007(2) 0.0090(18) C15 0.072(2) 0.072(2) 0.051(2) -0.0163(18) -0.0159(18) 0.030(2) C16 0.0264(14) 0.0485(18) 0.0491(17) -0.0020(14) 0.0002(12) 0.0024(13) C17 0.055(2) 0.080(3) 0.0439(18) 0.0049(18) 0.0012(15) 0.0227(19) C18 0.0385(16) 0.0198(13) 0.0259(13) -0.0038(10) 0.0016(11) 0.0001(11) C19 0.0387(16) 0.0246(14) 0.0305(14) -0.0015(11) 0.0045(12) 0.0004(12) C20 0.0481(18) 0.0319(16) 0.0436(17) 0.0006(13) 0.0126(14) -0.0053(13) C21 0.070(2) 0.0296(16) 0.0399(17) 0.0095(13) 0.0059(16) 0.0000(15) C22 0.055(2) 0.0301(16) 0.0539(19) 0.0060(14) -0.0093(16) 0.0048(14) C23 0.0434(17) 0.0234(14) 0.0427(16) -0.0012(12) -0.0027(13) 0.0018(12) C24 0.052(2) 0.056(2) 0.055(2) -0.0012(17) -0.0097(16) 0.0010(16) C25 0.0333(16) 0.0349(16) 0.0494(18) 0.0062(13) 0.0067(13) -0.0013(12) C26 0.049(2) 0.052(2) 0.082(3) -0.0173(19) 0.0017(18) 0.0129(16) C27 0.057(3) 0.135(4) 0.088(3) -0.014(3) 0.023(2) -0.001(3) C28 0.0391(18) 0.0348(17) 0.080(2) 0.0137(16) -0.0101(17) 0.0047(14) C29 0.048(2) 0.133(4) 0.096(3) -0.035(3) -0.021(2) 0.001(2) C30 0.033(9) 0.021(7) 0.029(2) -0.007(5) -0.002(5) -0.007(4) C31 0.037(8) 0.040(3) 0.035(4) 0.004(3) -0.019(5) -0.014(5) C32 0.081(10) 0.037(3) 0.055(4) 0.010(3) -0.013(7) -0.013(6) C33 0.103(11) 0.040(5) 0.040(2) 0.000(4) -0.031(7) 0.003(6) C34 0.061(8) 0.065(7) 0.042(3) -0.001(4) -0.014(6) 0.008(5) C35 0.047(7) 0.034(6) 0.043(2) -0.006(4) -0.013(4) -0.011(3) C30' 0.033(9) 0.021(7) 0.029(2) -0.007(5) -0.002(5) -0.007(4) C31' 0.037(8) 0.040(3) 0.035(4) 0.004(3) -0.019(5) -0.014(5) C32' 0.081(10) 0.037(3) 0.055(4) 0.010(3) -0.013(7) -0.013(6) C33' 0.103(11) 0.040(5) 0.040(2) 0.000(4) -0.031(7) 0.003(6) C34' 0.061(8) 0.065(7) 0.042(3) -0.001(4) -0.014(6) 0.008(5) C35' 0.047(7) 0.034(6) 0.043(2) -0.006(4) -0.013(4) -0.011(3) C36 0.0340(15) 0.0276(14) 0.0264(14) 0.0032(11) 0.0058(12) -0.0052(11) C37 0.0426(18) 0.058(2) 0.0332(16) 0.0030(14) 0.0069(14) 0.0000(15) C38 0.045(2) 0.080(3) 0.050(2) 0.0193(18) 0.0065(16) 0.0096(18) C39 0.043(2) 0.059(2) 0.077(3) 0.0153(19) 0.0250(19) 0.0133(16) C40 0.056(2) 0.058(2) 0.057(2) -0.0126(17) 0.0264(18) 0.0020(17) C41 0.0439(18) 0.0525(19) 0.0323(16) -0.0049(13) 0.0063(13) 0.0004(15) C42 0.0381(17) 0.0462(18) 0.0460(18) -0.0191(14) 0.0069(14) -0.0108(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.941(2) . ? Cu1 N1 1.964(2) . ? Cu1 P1 2.1581(9) . ? N1 C2 1.326(3) . ? N1 C6 1.433(3) . ? N2 C4 1.333(3) . ? N2 C18 1.437(3) . ? P1 C30' 1.796(16) . ? P1 C36 1.825(3) . ? P1 C42 1.828(3) . ? P1 C30 1.871(16) . ? C1 C2 1.517(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.410(3) . ? C3 C4 1.399(4) . ? C3 H3 0.9500 . ? C4 C5 1.518(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.397(4) . ? C6 C11 1.411(4) . ? C7 C8 1.394(4) . ? C7 C13 1.519(4) . ? C8 C9 1.383(4) . ? C8 H8 0.9500 . ? C9 C10 1.370(4) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C16 1.515(4) . ? C12 C13 1.530(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.532(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.511(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.529(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.404(4) . ? C18 C23 1.414(4) . ? C19 C20 1.391(4) . ? C19 C25 1.514(4) . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 C22 1.374(4) . ? C21 H21 0.9500 . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 C28 1.520(4) . ? C24 C25 1.531(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.528(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.514(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.520(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.385(10) . ? C30 C35 1.391(10) . ? C31 C32 1.383(10) . ? C31 H31A 0.9500 . ? C32 C33 1.381(9) . ? C32 H32A 0.9500 . ? C33 C34 1.372(10) . ? C33 H33A 0.9500 . ? C34 C35 1.396(10) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C30' C31' 1.388(10) . ? C30' C35' 1.391(10) . ? C31' C32' 1.385(10) . ? C31' H31B 0.9500 . ? C32' C33' 1.380(10) . ? C32' H32B 0.9500 . ? C33' C34' 1.374(10) . ? C33' H33B 0.9500 . ? C34' C35' 1.388(10) . ? C34' H34B 0.9500 . ? C35' H35B 0.9500 . ? C36 C37 1.383(4) . ? C36 C41 1.387(3) . ? C37 C38 1.385(4) . ? C37 H37 0.9500 . ? C38 C39 1.359(4) . ? C38 H38 0.9500 . ? C39 C40 1.371(4) . ? C39 H39 0.9500 . ? C40 C41 1.385(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 N2 Cu1 N1 98.31(8) . . ? N2 Cu1 P1 137.88(6) . . ? N1 Cu1 P1 123.76(6) . . ? C2 N1 C6 120.6(2) . . ? C2 N1 Cu1 121.62(17) . . ? C6 N1 Cu1 117.38(15) . . ? C4 N2 C18 120.0(2) . . ? C4 N2 Cu1 121.35(16) . . ? C18 N2 Cu1 118.44(15) . . ? C30' P1 C36 107.2(14) . . ? C30' P1 C42 98.6(5) . . ? C36 P1 C42 100.72(13) . . ? C30' P1 C30 11.0(8) . . ? C36 P1 C30 101.6(13) . . ? C42 P1 C30 109.2(5) . . ? C30' P1 Cu1 117.6(14) . . ? C36 P1 Cu1 114.76(8) . . ? C42 P1 Cu1 115.59(10) . . ? C30 P1 Cu1 113.4(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.3(2) . . ? N1 C2 C1 120.6(2) . . ? C3 C2 C1 116.2(2) . . ? C4 C3 C2 129.8(2) . . ? C4 C3 H3 115.1 . . ? C2 C3 H3 115.1 . . ? N2 C4 C3 124.1(2) . . ? N2 C4 C5 119.8(2) . . ? C3 C4 C5 116.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.5(2) . . ? C7 C6 N1 121.0(2) . . ? C11 C6 N1 118.2(2) . . ? C8 C7 C6 118.8(3) . . ? C8 C7 C13 119.0(3) . . ? C6 C7 C13 122.1(2) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.6(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.4(3) . . ? C10 C11 C16 121.1(2) . . ? C6 C11 C16 120.5(2) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 C12 113.0(3) . . ? C7 C13 C14 109.6(3) . . ? C12 C13 C14 110.6(3) . . ? C7 C13 H13 107.8 . . ? C12 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C15 C16 C11 112.1(3) . . ? C15 C16 C17 109.9(2) . . ? C11 C16 C17 114.5(2) . . ? C15 C16 H16 106.6 . . ? C11 C16 H16 106.6 . . ? C17 C16 H16 106.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.5(2) . . ? C19 C18 N2 120.6(2) . . ? C23 C18 N2 118.8(2) . . ? C20 C19 C18 118.5(2) . . ? C20 C19 C25 119.9(2) . . ? C18 C19 C25 121.6(2) . . ? C21 C20 C19 121.6(3) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 122.1(3) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C18 118.1(3) . . ? C22 C23 C28 120.6(3) . . ? C18 C23 C28 121.2(2) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 C26 110.3(2) . . ? C19 C25 C24 112.8(2) . . ? C26 C25 C24 110.0(2) . . ? C19 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? C24 C25 H25 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C27 C28 C29 109.9(3) . . ? C27 C28 C23 112.1(3) . . ? C29 C28 C23 112.4(3) . . ? C27 C28 H28 107.4 . . ? C29 C28 H28 107.4 . . ? C23 C28 H28 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.0(10) . . ? C31 C30 P1 119.6(10) . . ? C35 C30 P1 120.3(10) . . ? C32 C31 C30 119.0(9) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C33 C32 C31 120.9(9) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 120.8(10) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 118.7(9) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C30 C35 C34 120.6(9) . . ? C30 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C31' C30' C35' 118.1(10) . . ? C31' C30' P1 116.5(10) . . ? C35' C30' P1 125.0(10) . . ? C32' C31' C30' 122.6(9) . . ? C32' C31' H31B 118.7 . . ? C30' C31' H31B 118.7 . . ? C33' C32' C31' 117.8(9) . . ? C33' C32' H32B 121.1 . . ? C31' C32' H32B 121.1 . . ? C34' C33' C32' 120.9(10) . . ? C34' C33' H33B 119.6 . . ? C32' C33' H33B 119.6 . . ? C33' C34' C35' 120.7(9) . . ? C33' C34' H34B 119.7 . . ? C35' C34' H34B 119.7 . . ? C34' C35' C30' 119.6(9) . . ? C34' C35' H35B 120.2 . . ? C30' C35' H35B 120.2 . . ? C37 C36 C41 118.0(3) . . ? C37 C36 P1 119.4(2) . . ? C41 C36 P1 122.5(2) . . ? C36 C37 C38 120.8(3) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 120.5(3) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 119.7(3) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C41 120.3(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C36 120.6(3) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? P1 C42 H42A 109.5 . . ? P1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 N2 Cu1 N1 C2 -8.9(2) . . . . ? P1 Cu1 N1 C2 173.46(16) . . . . ? N2 Cu1 N1 C6 163.67(17) . . . . ? P1 Cu1 N1 C6 -14.0(2) . . . . ? N1 Cu1 N2 C4 10.6(2) . . . . ? P1 Cu1 N2 C4 -172.31(14) . . . . ? N1 Cu1 N2 C18 -164.41(17) . . . . ? P1 Cu1 N2 C18 12.7(2) . . . . ? N2 Cu1 P1 C30' -44.0(8) . . . . ? N1 Cu1 P1 C30' 132.6(8) . . . . ? N2 Cu1 P1 C36 83.48(13) . . . . ? N1 Cu1 P1 C36 -99.94(11) . . . . ? N2 Cu1 P1 C42 -159.91(14) . . . . ? N1 Cu1 P1 C42 16.67(14) . . . . ? N2 Cu1 P1 C30 -32.7(8) . . . . ? N1 Cu1 P1 C30 143.9(8) . . . . ? C6 N1 C2 C3 -171.7(2) . . . . ? Cu1 N1 C2 C3 0.6(3) . . . . ? C6 N1 C2 C1 6.4(4) . . . . ? Cu1 N1 C2 C1 178.72(19) . . . . ? N1 C2 C3 C4 10.5(4) . . . . ? C1 C2 C3 C4 -167.7(3) . . . . ? C18 N2 C4 C3 170.7(2) . . . . ? Cu1 N2 C4 C3 -4.2(3) . . . . ? C18 N2 C4 C5 -7.4(3) . . . . ? Cu1 N2 C4 C5 177.66(18) . . . . ? C2 C3 C4 N2 -8.5(4) . . . . ? C2 C3 C4 C5 169.8(3) . . . . ? C2 N1 C6 C7 -84.7(3) . . . . ? Cu1 N1 C6 C7 102.7(2) . . . . ? C2 N1 C6 C11 101.1(3) . . . . ? Cu1 N1 C6 C11 -71.5(3) . . . . ? C11 C6 C7 C8 -1.7(4) . . . . ? N1 C6 C7 C8 -175.7(2) . . . . ? C11 C6 C7 C13 175.0(3) . . . . ? N1 C6 C7 C13 0.9(4) . . . . ? C6 C7 C8 C9 0.4(4) . . . . ? C13 C7 C8 C9 -176.4(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C6 -1.3(4) . . . . ? C9 C10 C11 C16 178.2(3) . . . . ? C7 C6 C11 C10 2.1(4) . . . . ? N1 C6 C11 C10 176.3(2) . . . . ? C7 C6 C11 C16 -177.4(2) . . . . ? N1 C6 C11 C16 -3.1(4) . . . . ? C8 C7 C13 C12 -54.4(4) . . . . ? C6 C7 C13 C12 129.0(3) . . . . ? C8 C7 C13 C14 69.5(4) . . . . ? C6 C7 C13 C14 -107.2(3) . . . . ? C10 C11 C16 C15 97.2(3) . . . . ? C6 C11 C16 C15 -83.3(3) . . . . ? C10 C11 C16 C17 -29.0(4) . . . . ? C6 C11 C16 C17 150.5(3) . . . . ? C4 N2 C18 C19 87.7(3) . . . . ? Cu1 N2 C18 C19 -97.2(2) . . . . ? C4 N2 C18 C23 -96.2(3) . . . . ? Cu1 N2 C18 C23 78.9(3) . . . . ? C23 C18 C19 C20 -0.2(4) . . . . ? N2 C18 C19 C20 175.9(2) . . . . ? C23 C18 C19 C25 -178.1(2) . . . . ? N2 C18 C19 C25 -2.1(4) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? C25 C19 C20 C21 178.7(3) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C20 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C18 1.1(4) . . . . ? C21 C22 C23 C28 -179.8(3) . . . . ? C19 C18 C23 C22 -0.7(4) . . . . ? N2 C18 C23 C22 -176.8(2) . . . . ? C19 C18 C23 C28 -179.8(3) . . . . ? N2 C18 C23 C28 4.0(4) . . . . ? C20 C19 C25 C26 -68.4(3) . . . . ? C18 C19 C25 C26 109.5(3) . . . . ? C20 C19 C25 C24 55.0(3) . . . . ? C18 C19 C25 C24 -127.1(3) . . . . ? C22 C23 C28 C27 -78.7(4) . . . . ? C18 C23 C28 C27 100.4(3) . . . . ? C22 C23 C28 C29 45.6(4) . . . . ? C18 C23 C28 C29 -135.2(3) . . . . ? C30' P1 C30 C31 177(19) . . . . ? C36 P1 C30 C31 -61(4) . . . . ? C42 P1 C30 C31 -167(3) . . . . ? Cu1 P1 C30 C31 62(4) . . . . ? C30' P1 C30 C35 -1(12) . . . . ? C36 P1 C30 C35 121(3) . . . . ? C42 P1 C30 C35 15(4) . . . . ? Cu1 P1 C30 C35 -115(3) . . . . ? C35 C30 C31 C32 0(6) . . . . ? P1 C30 C31 C32 -178(2) . . . . ? C30 C31 C32 C33 0(4) . . . . ? C31 C32 C33 C34 -2(4) . . . . ? C32 C33 C34 C35 3(3) . . . . ? C31 C30 C35 C34 1(6) . . . . ? P1 C30 C35 C34 179(2) . . . . ? C33 C34 C35 C30 -2(4) . . . . ? C36 P1 C30' C31' -68(3) . . . . ? C42 P1 C30' C31' -172(3) . . . . ? C30 P1 C30' C31' -7(12) . . . . ? Cu1 P1 C30' C31' 63(4) . . . . ? C36 P1 C30' C35' 119(4) . . . . ? C42 P1 C30' C35' 15(4) . . . . ? C30 P1 C30' C35' 180(19) . . . . ? Cu1 P1 C30' C35' -110(4) . . . . ? C35' C30' C31' C32' -2(6) . . . . ? P1 C30' C31' C32' -176(2) . . . . ? C30' C31' C32' C33' 2(4) . . . . ? C31' C32' C33' C34' 2(3) . . . . ? C32' C33' C34' C35' -6(3) . . . . ? C33' C34' C35' C30' 6(4) . . . . ? C31' C30' C35' C34' -2(5) . . . . ? P1 C30' C35' C34' 171(2) . . . . ? C30' P1 C36 C37 143.9(8) . . . . ? C42 P1 C36 C37 -113.5(2) . . . . ? C30 P1 C36 C37 134.1(8) . . . . ? Cu1 P1 C36 C37 11.3(2) . . . . ? C30' P1 C36 C41 -40.1(8) . . . . ? C42 P1 C36 C41 62.5(2) . . . . ? C30 P1 C36 C41 -49.9(8) . . . . ? Cu1 P1 C36 C41 -172.7(2) . . . . ? C41 C36 C37 C38 -1.0(4) . . . . ? P1 C36 C37 C38 175.2(2) . . . . ? C36 C37 C38 C39 0.0(5) . . . . ? C37 C38 C39 C40 1.2(5) . . . . ? C38 C39 C40 C41 -1.4(5) . . . . ? C39 C40 C41 C36 0.3(5) . . . . ? C37 C36 C41 C40 0.8(4) . . . . ? P1 C36 C41 C40 -175.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.336 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.048 #===END data_04249 _database_code_depnum_ccdc_archive 'CCDC 258884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Me2LiPr2CuPPh3 ; _chemical_name_common Me2LiPr2CuPPh3 _chemical_compound_source 'Anne M. Reynolds' _chemical_melting_point ? _chemical_formula_moiety 'C47 H56 Cu N2 P' _chemical_formula_sum 'C47 H56 Cu N2 P' _chemical_formula_weight 743.45 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.439(2) _cell_length_b 15.9011(15) _cell_length_c 24.217(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.850(2) _cell_angle_gamma 90.00 _cell_volume 8377.2(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3854 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.94 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.920818 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79358 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.06 _reflns_number_total 14812 _reflns_number_gt 10455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+5.3186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14812 _refine_ls_number_parameters 923 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.868667(13) 0.232396(18) 0.852293(12) 0.02019(8) Uani 1 1 d . . . Cu2 Cu 0.371365(13) 0.227216(18) 0.856832(12) 0.02028(8) Uani 1 1 d . . . N1 N 0.89986(9) 0.24116(12) 0.78745(8) 0.0213(4) Uani 1 1 d . . . N2 N 0.92230(9) 0.31831(12) 0.90551(8) 0.0226(5) Uani 1 1 d . . . N3 N 0.39101(9) 0.23980(12) 0.78478(8) 0.0206(4) Uani 1 1 d . . . N4 N 0.43107(9) 0.31004(13) 0.90645(8) 0.0227(5) Uani 1 1 d . . . P1 P 0.79634(3) 0.15929(4) 0.86608(3) 0.02159(15) Uani 1 1 d . . . P2 P 0.30138(3) 0.15367(4) 0.87443(3) 0.02201(15) Uani 1 1 d . . . C1 C 0.96065(13) 0.30779(17) 0.73497(11) 0.0341(7) Uani 1 1 d . . . H1A H 0.9877 0.2600 0.7367 0.051 Uiso 1 1 calc R . . H1B H 0.9834 0.3604 0.7380 0.051 Uiso 1 1 calc R . . H1C H 0.9253 0.3066 0.6972 0.051 Uiso 1 1 calc R . . C2 C 0.93823(11) 0.30202(16) 0.78655(10) 0.0233(6) Uani 1 1 d . . . C3 C 0.96223(11) 0.36261(15) 0.83144(10) 0.0245(6) Uani 1 1 d . . . H3 H 0.9841 0.4073 0.8222 0.029 Uiso 1 1 calc R . . C4 C 0.95856(11) 0.36687(15) 0.88818(11) 0.0251(6) Uani 1 1 d . . . C5 C 1.00186(13) 0.42944(18) 0.93048(12) 0.0387(7) Uani 1 1 d . . . H5A H 0.9822 0.4538 0.9561 0.058 Uiso 1 1 calc R . . H5B H 1.0115 0.4743 0.9076 0.058 Uiso 1 1 calc R . . H5C H 1.0398 0.4007 0.9551 0.058 Uiso 1 1 calc R . . C6 C 0.88901(11) 0.17481(15) 0.74463(10) 0.0227(6) Uani 1 1 d . . . C7 C 0.92788(12) 0.10453(17) 0.75932(11) 0.0297(6) Uani 1 1 d . . . C8 C 0.91717(12) 0.03964(17) 0.71785(12) 0.0336(7) Uani 1 1 d . . . H8 H 0.9440 -0.0075 0.7269 0.040 Uiso 1 1 calc R . . C9 C 0.86855(13) 0.04272(18) 0.66407(12) 0.0349(7) Uani 1 1 d . . . H9 H 0.8620 -0.0018 0.6362 0.042 Uiso 1 1 calc R . . C10 C 0.82962(13) 0.11045(18) 0.65102(11) 0.0357(7) Uani 1 1 d . . . H10 H 0.7956 0.1114 0.6142 0.043 Uiso 1 1 calc R . . C11 C 0.83820(12) 0.17789(16) 0.69000(11) 0.0296(6) Uani 1 1 d . . . C12 C 1.04290(15) 0.0986(3) 0.8120(2) 0.0913(16) Uani 1 1 d . . . H12A H 1.0760 0.0941 0.8512 0.137 Uiso 1 1 calc R . . H12B H 1.0472 0.1514 0.7931 0.137 Uiso 1 1 calc R . . H12C H 1.0452 0.0511 0.7872 0.137 Uiso 1 1 calc R . . C13 C 0.98080(14) 0.0974(2) 0.81925(14) 0.0501(9) Uani 1 1 d . . . H13 H 0.9790 0.1469 0.8440 0.060 Uiso 1 1 calc R . . C14 C 0.97637(16) 0.0179(3) 0.85226(15) 0.0740(12) Uani 1 1 d . . . H14A H 1.0108 0.0160 0.8907 0.111 Uiso 1 1 calc R . . H14B H 0.9779 -0.0314 0.8286 0.111 Uiso 1 1 calc R . . H14C H 0.9375 0.0180 0.8588 0.111 Uiso 1 1 calc R . . C15 C 0.78874(18) 0.2932(3) 0.61576(18) 0.0870(14) Uani 1 1 d . . . H15A H 0.7599 0.3404 0.6077 0.131 Uiso 1 1 calc R . . H15B H 0.7738 0.2524 0.5832 0.131 Uiso 1 1 calc R . . H15C H 0.8292 0.3141 0.6190 0.131 Uiso 1 1 calc R . . C16 C 0.79396(14) 0.25090(18) 0.67395(13) 0.0455(8) Uani 1 1 d . . . H16 H 0.8097 0.2937 0.7064 0.055 Uiso 1 1 calc R . . C17 C 0.73040(15) 0.2242(2) 0.67006(15) 0.0601(10) Uani 1 1 d . . . H17A H 0.7029 0.2730 0.6601 0.090 Uiso 1 1 calc R . . H17B H 0.7330 0.2011 0.7085 0.090 Uiso 1 1 calc R . . H17C H 0.7143 0.1812 0.6392 0.090 Uiso 1 1 calc R . . C18 C 0.92685(11) 0.32467(16) 0.96627(10) 0.0254(6) Uani 1 1 d . . . C19 C 0.97248(12) 0.27902(17) 1.01102(11) 0.0311(6) Uani 1 1 d . . . C20 C 0.97492(14) 0.28609(19) 1.06915(12) 0.0404(7) Uani 1 1 d . . . H20 H 1.0053 0.2554 1.0998 0.048 Uiso 1 1 calc R . . C21 C 0.93472(14) 0.33604(19) 1.08342(12) 0.0424(8) Uani 1 1 d . . . H21 H 0.9380 0.3408 1.1236 0.051 Uiso 1 1 calc R . . C22 C 0.88944(13) 0.37939(18) 1.03906(11) 0.0363(7) Uani 1 1 d . . . H22 H 0.8613 0.4132 1.0490 0.044 Uiso 1 1 calc R . . C23 C 0.88427(12) 0.37443(16) 0.97992(11) 0.0278(6) Uani 1 1 d . . . C24 C 0.99695(16) 0.1293(2) 0.99728(18) 0.0693(11) Uani 1 1 d . . . H24A H 1.0256 0.0925 0.9878 0.104 Uiso 1 1 calc R . . H24B H 0.9554 0.1219 0.9674 0.104 Uiso 1 1 calc R . . H24C H 0.9972 0.1148 1.0367 0.104 Uiso 1 1 calc R . . C25 C 1.01671(13) 0.22043(19) 0.99724(12) 0.0384(7) Uani 1 1 d . . . H25 H 1.0151 0.2340 0.9564 0.046 Uiso 1 1 calc R . . C26 C 1.08338(14) 0.2317(2) 1.04068(15) 0.0615(10) Uani 1 1 d . . . H26A H 1.1102 0.1933 1.0297 0.092 Uiso 1 1 calc R . . H26B H 1.0861 0.2191 1.0812 0.092 Uiso 1 1 calc R . . H26C H 1.0964 0.2898 1.0388 0.092 Uiso 1 1 calc R . . C27 C 0.77341(14) 0.4234(2) 0.94306(14) 0.0523(9) Uani 1 1 d . . . H27A H 0.7419 0.4531 0.9104 0.078 Uiso 1 1 calc R . . H27B H 0.7803 0.4528 0.9806 0.078 Uiso 1 1 calc R . . H27C H 0.7596 0.3658 0.9455 0.078 Uiso 1 1 calc R . . C28 C 0.83308(12) 0.42097(17) 0.93170(12) 0.0344(7) Uani 1 1 d . . . H28 H 0.8245 0.3895 0.8937 0.041 Uiso 1 1 calc R . . C29 C 0.85207(16) 0.5095(2) 0.92226(16) 0.0638(10) Uani 1 1 d . . . H29A H 0.8180 0.5371 0.8906 0.096 Uiso 1 1 calc R . . H29B H 0.8880 0.5069 0.9108 0.096 Uiso 1 1 calc R . . H29C H 0.8624 0.5417 0.9592 0.096 Uiso 1 1 calc R . . C30 C 0.81831(11) 0.11011(17) 0.93955(11) 0.0265(6) Uani 1 1 d . . . C31 C 0.83516(13) 0.1620(2) 0.98935(12) 0.0402(7) Uani 1 1 d . . . H31 H 0.8343 0.2214 0.9845 0.048 Uiso 1 1 calc R . . C32 C 0.85305(14) 0.1281(2) 1.04576(13) 0.0518(9) Uani 1 1 d . . . H32 H 0.8639 0.1643 1.0793 0.062 Uiso 1 1 calc R . . C33 C 0.85520(14) 0.0426(3) 1.05363(14) 0.0549(10) Uani 1 1 d . . . H33 H 0.8672 0.0195 1.0925 0.066 Uiso 1 1 calc R . . C34 C 0.84001(15) -0.0092(2) 1.00510(15) 0.0539(9) Uani 1 1 d . . . H34 H 0.8423 -0.0684 1.0106 0.065 Uiso 1 1 calc R . . C35 C 0.82113(13) 0.02395(18) 0.94754(13) 0.0388(7) Uani 1 1 d . . . H35 H 0.8103 -0.0126 0.9142 0.047 Uiso 1 1 calc R . . C36 C 0.72808(11) 0.22163(15) 0.85916(11) 0.0263(6) Uani 1 1 d . . . C37 C 0.70540(13) 0.27517(18) 0.81082(12) 0.0382(7) Uani 1 1 d . . . H37 H 0.7284 0.2838 0.7862 0.046 Uiso 1 1 calc R . . C38 C 0.64999(14) 0.3164(2) 0.79764(15) 0.0534(9) Uani 1 1 d . . . H38 H 0.6348 0.3521 0.7639 0.064 Uiso 1 1 calc R . . C39 C 0.61707(14) 0.3053(2) 0.83354(17) 0.0567(9) Uani 1 1 d . . . H39 H 0.5790 0.3336 0.8247 0.068 Uiso 1 1 calc R . . C40 C 0.63894(15) 0.2542(2) 0.88166(17) 0.0549(9) Uani 1 1 d . . . H40 H 0.6161 0.2471 0.9066 0.066 Uiso 1 1 calc R . . C41 C 0.69442(13) 0.21205(18) 0.89486(14) 0.0422(7) Uani 1 1 d . . . H41 H 0.7092 0.1764 0.9287 0.051 Uiso 1 1 calc R . . C42 C 0.75911(11) 0.07294(16) 0.81517(11) 0.0252(6) Uani 1 1 d . . . C43 C 0.70241(13) 0.04184(19) 0.81086(14) 0.0455(8) Uani 1 1 d . . . H43 H 0.6830 0.0645 0.8357 0.055 Uiso 1 1 calc R . . C44 C 0.67376(14) -0.0211(2) 0.77153(14) 0.0496(8) Uani 1 1 d . . . H44 H 0.6351 -0.0419 0.7698 0.059 Uiso 1 1 calc R . . C45 C 0.70063(14) -0.05407(18) 0.73475(13) 0.0437(8) Uani 1 1 d . . . H45A H 0.6806 -0.0971 0.7071 0.052 Uiso 1 1 calc R . . C46 C 0.75672(15) -0.02400(19) 0.73860(13) 0.0475(8) Uani 1 1 d . . . H46A H 0.7756 -0.0466 0.7133 0.057 Uiso 1 1 calc R . . C47 C 0.78658(13) 0.03916(17) 0.77883(12) 0.0345(7) Uani 1 1 d . . . H47A H 0.8257 0.0588 0.7812 0.041 Uiso 1 1 calc R . . C48 C 0.44001(12) 0.30999(17) 0.72270(11) 0.0315(6) Uani 1 1 d . . . H48A H 0.4741 0.2729 0.7246 0.047 Uiso 1 1 calc R . . H48B H 0.4510 0.3684 0.7184 0.047 Uiso 1 1 calc R . . H48C H 0.4032 0.2944 0.6884 0.047 Uiso 1 1 calc R . . C49 C 0.42711(10) 0.30094(15) 0.77958(10) 0.0216(5) Uani 1 1 d . . . C50 C 0.45696(10) 0.35874(15) 0.82446(10) 0.0227(5) Uani 1 1 d . . . H50A H 0.4763 0.4041 0.8127 0.027 Uiso 1 1 calc R . . C51 C 0.46271(11) 0.36008(15) 0.88430(11) 0.0246(6) Uani 1 1 d . . . C52 C 0.50982(12) 0.42159(18) 0.92398(12) 0.0369(7) Uani 1 1 d . . . H52A H 0.4976 0.4392 0.9568 0.055 Uiso 1 1 calc R . . H52B H 0.5121 0.4710 0.9007 0.055 Uiso 1 1 calc R . . H52C H 0.5502 0.3943 0.9401 0.055 Uiso 1 1 calc R . . C53 C 0.37334(11) 0.17543(15) 0.73980(10) 0.0223(5) Uani 1 1 d . . . C54 C 0.41472(11) 0.10969(17) 0.74355(11) 0.0275(6) Uani 1 1 d . . . C55 C 0.39659(13) 0.04694(17) 0.70027(11) 0.0327(6) Uani 1 1 d . . . H55A H 0.4238 0.0016 0.7026 0.039 Uiso 1 1 calc R . . C56 C 0.34034(13) 0.04904(17) 0.65433(11) 0.0340(7) Uani 1 1 d . . . H56A H 0.3293 0.0062 0.6249 0.041 Uiso 1 1 calc R . . C57 C 0.30009(13) 0.11359(17) 0.65111(11) 0.0329(7) Uani 1 1 d . . . H57A H 0.2614 0.1148 0.6190 0.039 Uiso 1 1 calc R . . C58 C 0.31462(11) 0.17729(16) 0.69388(10) 0.0258(6) Uani 1 1 d . . . C59 C 0.52964(14) 0.0876(2) 0.77332(16) 0.0608(10) Uani 1 1 d . . . H59A H 0.5683 0.0846 0.8079 0.091 Uiso 1 1 calc R . . H59B H 0.5318 0.1334 0.7471 0.091 Uiso 1 1 calc R . . H59C H 0.5227 0.0342 0.7516 0.091 Uiso 1 1 calc R . . C60 C 0.47679(13) 0.10394(19) 0.79417(12) 0.0408(7) Uani 1 1 d . . . H60 H 0.4847 0.1590 0.8157 0.049 Uiso 1 1 calc R . . C61 C 0.47556(16) 0.0358(3) 0.83828(16) 0.0818(14) Uani 1 1 d . . . H61A H 0.5157 0.0330 0.8709 0.123 Uiso 1 1 calc R . . H61B H 0.4663 -0.0187 0.8179 0.123 Uiso 1 1 calc R . . H61C H 0.4439 0.0494 0.8542 0.123 Uiso 1 1 calc R . . C62 C 0.26309(13) 0.31004(19) 0.64165(14) 0.0468(8) Uani 1 1 d . . . H62A H 0.2330 0.3532 0.6410 0.070 Uiso 1 1 calc R . . H62B H 0.2497 0.2817 0.6030 0.070 Uiso 1 1 calc R . . H62C H 0.3032 0.3365 0.6499 0.070 Uiso 1 1 calc R . . C63 C 0.26840(12) 0.24577(17) 0.69024(11) 0.0325(6) Uani 1 1 d . . . H63 H 0.2835 0.2763 0.7291 0.039 Uiso 1 1 calc R . . C64 C 0.20479(12) 0.21048(19) 0.68105(12) 0.0409(7) Uani 1 1 d . . . H64A H 0.1767 0.2569 0.6794 0.061 Uiso 1 1 calc R . . H64B H 0.2078 0.1731 0.7142 0.061 Uiso 1 1 calc R . . H64C H 0.1891 0.1788 0.6437 0.061 Uiso 1 1 calc R . . C65 C 0.44384(11) 0.31386(16) 0.96934(10) 0.0260(6) Uani 1 1 d . . . C66 C 0.49367(12) 0.26860(17) 1.00919(11) 0.0330(6) Uani 1 1 d . . . C67 C 0.50368(14) 0.2727(2) 1.06972(12) 0.0446(8) Uani 1 1 d . . . H67A H 0.5371 0.2425 1.0974 0.054 Uiso 1 1 calc R . . C68 C 0.46621(15) 0.3194(2) 1.08986(12) 0.0475(8) Uani 1 1 d . . . H68A H 0.4745 0.3228 1.1313 0.057 Uiso 1 1 calc R . . C69 C 0.41668(14) 0.36134(18) 1.05011(12) 0.0391(7) Uani 1 1 d . . . H69A H 0.3903 0.3921 1.0645 0.047 Uiso 1 1 calc R . . C70 C 0.40413(12) 0.35992(16) 0.98940(11) 0.0284(6) Uani 1 1 d . . . C71 C 0.51975(18) 0.1198(2) 0.99336(19) 0.0781(12) Uani 1 1 d . . . H71A H 0.5462 0.0847 0.9796 0.117 Uiso 1 1 calc R . . H71B H 0.4766 0.1090 0.9688 0.117 Uiso 1 1 calc R . . H71C H 0.5271 0.1064 1.0349 0.117 Uiso 1 1 calc R . . C72 C 0.53438(13) 0.2122(2) 0.98834(12) 0.0416(8) Uani 1 1 d . . . H72 H 0.5254 0.2249 0.9455 0.050 Uiso 1 1 calc R . . C73 C 0.60255(14) 0.2281(2) 1.02298(15) 0.0618(10) Uani 1 1 d . . . H73A H 0.6269 0.1909 1.0080 0.093 Uiso 1 1 calc R . . H73B H 0.6123 0.2166 1.0653 0.093 Uiso 1 1 calc R . . H73C H 0.6123 0.2868 1.0179 0.093 Uiso 1 1 calc R . . C74 C 0.36486(15) 0.49163(19) 0.92834(14) 0.0515(9) Uani 1 1 d . . . H74A H 0.3277 0.5181 0.9001 0.077 Uiso 1 1 calc R . . H74B H 0.3953 0.4852 0.9098 0.077 Uiso 1 1 calc R . . H74C H 0.3819 0.5270 0.9639 0.077 Uiso 1 1 calc R . . C75 C 0.34869(12) 0.40523(18) 0.94597(12) 0.0362(7) Uani 1 1 d . . . H75 H 0.3330 0.3704 0.9089 0.043 Uiso 1 1 calc R . . C76 C 0.29616(14) 0.4134(2) 0.96863(15) 0.0580(10) Uani 1 1 d . . . H76A H 0.2614 0.4423 0.9387 0.087 Uiso 1 1 calc R . . H76B H 0.3102 0.4458 1.0057 0.087 Uiso 1 1 calc R . . H76C H 0.2832 0.3573 0.9760 0.087 Uiso 1 1 calc R . . C77 C 0.32449(11) 0.09354(16) 0.94387(11) 0.0269(6) Uani 1 1 d . . . C78 C 0.36690(12) 0.12886(18) 0.99489(11) 0.0356(7) Uani 1 1 d . . . H78 H 0.3854 0.1813 0.9928 0.043 Uiso 1 1 calc R . . C79 C 0.38246(14) 0.0878(2) 1.04929(12) 0.0440(8) Uani 1 1 d . . . H79 H 0.4118 0.1122 1.0841 0.053 Uiso 1 1 calc R . . C80 C 0.35562(14) 0.0124(2) 1.05277(13) 0.0454(8) Uani 1 1 d . . . H80 H 0.3659 -0.0152 1.0900 0.055 Uiso 1 1 calc R . . C81 C 0.31381(14) -0.02316(19) 1.00227(13) 0.0437(8) Uani 1 1 d . . . H81 H 0.2953 -0.0755 1.0047 0.052 Uiso 1 1 calc R . . C82 C 0.29833(13) 0.01673(17) 0.94778(12) 0.0350(7) Uani 1 1 d . . . H82 H 0.2697 -0.0086 0.9130 0.042 Uiso 1 1 calc R . . C83 C 0.23787(11) 0.21750(16) 0.87847(11) 0.0266(6) Uani 1 1 d . . . C84 C 0.21495(13) 0.20964(18) 0.92326(13) 0.0413(7) Uani 1 1 d . . . H84 H 0.2342 0.1725 0.9556 0.050 Uiso 1 1 calc R . . C85 C 0.16376(16) 0.2560(2) 0.92109(16) 0.0585(10) Uani 1 1 d . . . H85 H 0.1487 0.2509 0.9523 0.070 Uiso 1 1 calc R . . C86 C 0.13493(14) 0.3090(2) 0.87422(16) 0.0535(9) Uani 1 1 d . . . H86 H 0.0994 0.3395 0.8725 0.064 Uiso 1 1 calc R . . C87 C 0.15776(13) 0.31779(19) 0.82970(14) 0.0444(8) Uani 1 1 d . . . H87 H 0.1381 0.3546 0.7972 0.053 Uiso 1 1 calc R . . C88 C 0.20895(12) 0.27330(16) 0.83226(12) 0.0333(6) Uani 1 1 d . . . H88 H 0.2249 0.2808 0.8018 0.040 Uiso 1 1 calc R . . C89 C 0.25946(11) 0.07523(15) 0.81858(10) 0.0254(6) Uani 1 1 d . . . C90 C 0.29097(13) 0.02980(17) 0.79001(12) 0.0333(6) Uani 1 1 d . . . H90 H 0.3336 0.0396 0.7998 0.040 Uiso 1 1 calc R . . C91 C 0.26094(15) -0.02972(18) 0.74732(13) 0.0424(8) Uani 1 1 d . . . H91 H 0.2831 -0.0605 0.7281 0.051 Uiso 1 1 calc R . . C92 C 0.19897(14) -0.04453(18) 0.73253(12) 0.0422(8) Uani 1 1 d . . . H92 H 0.1783 -0.0853 0.7032 0.051 Uiso 1 1 calc R . . C93 C 0.16741(14) 0.00011(19) 0.76050(13) 0.0435(8) Uani 1 1 d . . . H93 H 0.1248 -0.0101 0.7504 0.052 Uiso 1 1 calc R . . C94 C 0.19677(12) 0.05957(17) 0.80301(12) 0.0350(7) Uani 1 1 d . . . H94 H 0.1742 0.0901 0.8218 0.042 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 0.02057(16) 0.02110(17) 0.01964(16) -0.00041(13) 0.00834(12) -0.00149(13) Cu2 0.02010(16) 0.02171(17) 0.01811(15) -0.00057(13) 0.00603(12) -0.00203(13) N1 0.0219(11) 0.0228(12) 0.0200(10) 0.0007(9) 0.0088(9) 0.0000(9) N2 0.0238(11) 0.0235(12) 0.0191(11) -0.0013(9) 0.0063(9) -0.0012(9) N3 0.0211(11) 0.0200(11) 0.0185(10) -0.0008(9) 0.0048(8) -0.0017(9) N4 0.0211(11) 0.0253(12) 0.0196(11) -0.0037(9) 0.0052(9) -0.0002(9) P1 0.0224(3) 0.0220(4) 0.0223(3) -0.0003(3) 0.0105(3) -0.0015(3) P2 0.0235(3) 0.0218(4) 0.0211(3) 0.0011(3) 0.0087(3) -0.0019(3) C1 0.0409(17) 0.0341(16) 0.0333(15) -0.0002(12) 0.0206(13) -0.0092(13) C2 0.0219(13) 0.0236(14) 0.0248(13) 0.0049(11) 0.0091(11) 0.0022(11) C3 0.0253(14) 0.0215(14) 0.0279(14) 0.0023(11) 0.0113(11) -0.0044(11) C4 0.0247(14) 0.0215(14) 0.0265(14) -0.0017(11) 0.0064(11) 0.0006(11) C5 0.0419(17) 0.0373(17) 0.0350(16) -0.0082(13) 0.0119(13) -0.0163(14) C6 0.0252(13) 0.0258(14) 0.0206(13) -0.0033(11) 0.0124(11) -0.0074(11) C7 0.0262(14) 0.0328(16) 0.0317(15) -0.0055(12) 0.0128(12) 0.0014(12) C8 0.0321(15) 0.0290(16) 0.0446(17) -0.0087(13) 0.0200(14) 0.0006(12) C9 0.0439(18) 0.0328(17) 0.0361(16) -0.0114(13) 0.0242(14) -0.0112(14) C10 0.0447(18) 0.0365(17) 0.0220(14) -0.0036(12) 0.0077(12) -0.0126(14) C11 0.0359(16) 0.0272(15) 0.0245(14) 0.0007(11) 0.0097(12) -0.0056(12) C12 0.033(2) 0.086(3) 0.126(4) 0.052(3) -0.004(2) -0.009(2) C13 0.0423(18) 0.043(2) 0.0494(19) -0.0146(16) -0.0007(15) 0.0195(15) C14 0.049(2) 0.125(4) 0.043(2) 0.025(2) 0.0121(17) 0.010(2) C15 0.073(3) 0.082(3) 0.098(3) 0.059(3) 0.022(2) 0.017(2) C16 0.0495(19) 0.0309(17) 0.0343(16) -0.0029(13) -0.0097(14) 0.0044(14) C17 0.060(2) 0.064(2) 0.056(2) 0.0067(18) 0.0213(18) 0.0269(19) C18 0.0281(14) 0.0256(15) 0.0218(13) -0.0023(11) 0.0086(11) -0.0029(11) C19 0.0316(15) 0.0343(16) 0.0245(14) -0.0013(12) 0.0071(12) 0.0028(12) C20 0.0468(18) 0.0461(19) 0.0229(14) 0.0021(13) 0.0067(13) 0.0094(15) C21 0.058(2) 0.0479(19) 0.0215(14) -0.0024(13) 0.0148(14) 0.0021(16) C22 0.0462(18) 0.0360(17) 0.0313(15) -0.0064(13) 0.0198(14) 0.0041(14) C23 0.0324(15) 0.0254(15) 0.0245(14) -0.0033(11) 0.0091(12) 0.0002(12) C24 0.053(2) 0.051(2) 0.104(3) -0.018(2) 0.031(2) 0.0080(18) C25 0.0381(17) 0.0469(19) 0.0284(15) 0.0032(13) 0.0104(13) 0.0118(14) C26 0.0366(19) 0.081(3) 0.060(2) -0.006(2) 0.0108(16) 0.0072(18) C27 0.0431(19) 0.054(2) 0.057(2) -0.0076(17) 0.0148(16) 0.0134(16) C28 0.0365(16) 0.0340(16) 0.0298(15) -0.0049(12) 0.0089(13) 0.0075(13) C29 0.058(2) 0.047(2) 0.071(2) 0.0220(18) 0.0064(19) 0.0066(18) C30 0.0232(14) 0.0323(16) 0.0276(14) 0.0063(12) 0.0135(11) 0.0001(11) C31 0.0492(18) 0.0439(18) 0.0288(15) -0.0003(14) 0.0161(14) -0.0109(15) C32 0.0450(19) 0.082(3) 0.0254(16) 0.0059(16) 0.0095(14) -0.0118(18) C33 0.0394(19) 0.087(3) 0.0373(19) 0.0304(19) 0.0134(15) 0.0132(18) C34 0.054(2) 0.051(2) 0.066(2) 0.0328(19) 0.0327(18) 0.0234(17) C35 0.0443(18) 0.0358(18) 0.0426(17) 0.0104(14) 0.0234(14) 0.0086(14) C36 0.0256(14) 0.0218(14) 0.0340(14) -0.0021(12) 0.0140(12) -0.0030(11) C37 0.0379(17) 0.0398(18) 0.0370(16) 0.0065(14) 0.0141(13) 0.0081(14) C38 0.0436(19) 0.049(2) 0.059(2) 0.0096(17) 0.0095(17) 0.0147(16) C39 0.0326(18) 0.043(2) 0.093(3) -0.0018(19) 0.0221(19) 0.0076(15) C40 0.047(2) 0.051(2) 0.084(3) 0.0025(19) 0.0446(19) 0.0063(17) C41 0.0443(18) 0.0392(18) 0.0540(19) 0.0108(15) 0.0307(16) 0.0065(14) C42 0.0259(14) 0.0243(14) 0.0255(13) 0.0004(11) 0.0097(11) -0.0030(11) C43 0.0378(18) 0.0443(19) 0.062(2) -0.0224(16) 0.0279(16) -0.0117(15) C44 0.0347(17) 0.047(2) 0.068(2) -0.0198(17) 0.0198(16) -0.0181(15) C45 0.059(2) 0.0321(17) 0.0382(17) -0.0090(14) 0.0157(15) -0.0143(15) C46 0.069(2) 0.0412(19) 0.0478(19) -0.0181(15) 0.0400(17) -0.0179(17) C47 0.0407(17) 0.0307(16) 0.0421(17) -0.0071(13) 0.0271(14) -0.0090(13) C48 0.0346(15) 0.0373(16) 0.0248(14) -0.0022(12) 0.0136(12) -0.0113(13) C49 0.0173(12) 0.0249(14) 0.0214(13) 0.0036(11) 0.0060(10) 0.0031(11) C50 0.0202(13) 0.0206(14) 0.0267(13) 0.0023(11) 0.0081(11) -0.0026(10) C51 0.0198(13) 0.0216(14) 0.0285(14) -0.0008(11) 0.0045(11) 0.0009(11) C52 0.0347(16) 0.0369(17) 0.0358(16) -0.0104(13) 0.0092(13) -0.0146(13) C53 0.0271(14) 0.0240(14) 0.0166(12) 0.0008(10) 0.0091(10) -0.0049(11) C54 0.0292(14) 0.0298(15) 0.0257(14) -0.0025(12) 0.0128(11) -0.0026(12) C55 0.0384(16) 0.0282(16) 0.0345(16) -0.0046(12) 0.0169(13) -0.0019(13) C56 0.0456(18) 0.0325(17) 0.0279(15) -0.0121(12) 0.0183(13) -0.0149(14) C57 0.0353(16) 0.0383(17) 0.0197(13) -0.0025(12) 0.0041(12) -0.0143(14) C58 0.0298(14) 0.0275(15) 0.0195(13) 0.0034(11) 0.0084(11) -0.0067(12) C59 0.0356(18) 0.070(3) 0.075(2) -0.009(2) 0.0178(17) 0.0016(17) C60 0.0341(16) 0.0413(18) 0.0393(17) -0.0141(14) 0.0050(13) 0.0100(14) C61 0.043(2) 0.140(4) 0.055(2) 0.042(3) 0.0096(18) 0.024(2) C62 0.0371(17) 0.0395(18) 0.057(2) 0.0147(15) 0.0101(15) -0.0018(14) C63 0.0301(15) 0.0339(16) 0.0255(14) -0.0006(12) 0.0012(12) -0.0009(12) C64 0.0316(16) 0.054(2) 0.0322(16) 0.0098(14) 0.0064(13) 0.0017(14) C65 0.0250(14) 0.0283(15) 0.0217(13) -0.0062(11) 0.0050(11) -0.0054(11) C66 0.0328(15) 0.0366(17) 0.0235(14) -0.0031(12) 0.0034(12) -0.0004(13) C67 0.0488(19) 0.051(2) 0.0225(15) -0.0008(14) 0.0003(13) 0.0050(16) C68 0.065(2) 0.053(2) 0.0209(15) -0.0032(14) 0.0123(15) 0.0028(17) C69 0.0499(19) 0.0416(18) 0.0291(16) -0.0083(13) 0.0186(14) 0.0002(15) C70 0.0308(15) 0.0263(15) 0.0263(14) -0.0055(11) 0.0087(12) -0.0038(12) C71 0.070(3) 0.058(3) 0.114(3) -0.027(2) 0.044(3) 0.010(2) C72 0.0320(16) 0.056(2) 0.0296(15) -0.0025(14) 0.0028(13) 0.0123(14) C73 0.0358(18) 0.083(3) 0.053(2) -0.0065(19) -0.0001(16) 0.0127(18) C74 0.052(2) 0.0403(19) 0.050(2) 0.0012(15) 0.0041(16) 0.0108(16) C75 0.0335(16) 0.0373(17) 0.0347(16) -0.0111(13) 0.0090(13) 0.0061(13) C76 0.0421(19) 0.077(3) 0.056(2) -0.0105(19) 0.0201(17) 0.0147(18) C77 0.0297(14) 0.0265(15) 0.0265(14) 0.0051(11) 0.0129(12) 0.0053(12) C78 0.0386(17) 0.0369(17) 0.0283(15) 0.0046(13) 0.0089(13) -0.0023(13) C79 0.0417(18) 0.057(2) 0.0290(16) 0.0082(14) 0.0085(14) 0.0047(16) C80 0.0420(18) 0.058(2) 0.0392(18) 0.0267(16) 0.0189(15) 0.0150(16) C81 0.0424(18) 0.0399(18) 0.0510(19) 0.0227(15) 0.0199(16) 0.0040(14) C82 0.0367(16) 0.0316(16) 0.0371(16) 0.0069(13) 0.0141(13) 0.0009(13) C83 0.0253(14) 0.0227(14) 0.0334(14) -0.0002(11) 0.0128(12) -0.0025(11) C84 0.0456(18) 0.0417(18) 0.0465(18) 0.0118(14) 0.0286(15) 0.0092(14) C85 0.062(2) 0.062(2) 0.077(2) 0.014(2) 0.054(2) 0.0156(19) C86 0.0367(18) 0.046(2) 0.086(3) 0.0107(19) 0.0324(18) 0.0139(15) C87 0.0374(17) 0.0369(18) 0.055(2) 0.0100(15) 0.0125(15) 0.0110(14) C88 0.0358(16) 0.0276(16) 0.0369(16) 0.0038(13) 0.0138(13) 0.0027(13) C89 0.0287(14) 0.0236(14) 0.0227(13) 0.0008(11) 0.0080(11) -0.0054(11) C90 0.0386(16) 0.0291(16) 0.0360(16) -0.0006(12) 0.0184(13) -0.0081(13) C91 0.064(2) 0.0297(17) 0.0433(18) -0.0061(14) 0.0315(16) -0.0096(15) C92 0.057(2) 0.0349(18) 0.0296(16) -0.0047(13) 0.0105(15) -0.0199(15) C93 0.0359(17) 0.0421(19) 0.0451(18) -0.0014(15) 0.0063(14) -0.0136(14) C94 0.0318(16) 0.0331(16) 0.0395(16) -0.0032(13) 0.0126(13) -0.0063(13) _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 1.9683(19) . ? Cu1 N2 1.975(2) . ? Cu1 P1 2.1813(7) . ? Cu2 N4 1.971(2) . ? Cu2 N3 1.9734(19) . ? Cu2 P2 2.1819(7) . ? N1 C2 1.327(3) . ? N1 C6 1.434(3) . ? N2 C4 1.327(3) . ? N2 C18 1.439(3) . ? N3 C49 1.325(3) . ? N3 C53 1.439(3) . ? N4 C51 1.329(3) . ? N4 C65 1.440(3) . ? P1 C30 1.833(2) . ? P1 C42 1.835(3) . ? P1 C36 1.836(3) . ? P2 C77 1.832(2) . ? P2 C89 1.833(2) . ? P2 C83 1.834(3) . ? C1 C2 1.528(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.404(3) . ? C3 C4 1.410(3) . ? C3 H3 0.9500 . ? C4 C5 1.515(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.401(4) . ? C6 C11 1.414(3) . ? C7 C8 1.396(4) . ? C7 C13 1.522(4) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.370(4) . ? C9 H9 0.9500 . ? C10 C11 1.393(4) . ? C10 H10 0.9500 . ? C11 C16 1.508(4) . ? C12 C13 1.530(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.519(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.525(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.518(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.406(3) . ? C18 C19 1.408(3) . ? C19 C20 1.392(4) . ? C19 C25 1.520(4) . ? C20 C21 1.371(4) . ? C20 H20 0.9500 . ? C21 C22 1.381(4) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 C28 1.519(3) . ? C24 C25 1.521(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.535(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.523(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.519(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.382(4) . ? C30 C31 1.392(4) . ? C31 C32 1.381(4) . ? C31 H31 0.9500 . ? C32 C33 1.371(5) . ? C32 H32 0.9500 . ? C33 C34 1.370(5) . ? C33 H33 0.9500 . ? C34 C35 1.399(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.379(4) . ? C36 C37 1.384(4) . ? C37 C38 1.382(4) . ? C37 H37 0.9500 . ? C38 C39 1.372(5) . ? C38 H38 0.9500 . ? C39 C40 1.356(5) . ? C39 H39 0.9500 . ? C40 C41 1.390(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.378(3) . ? C42 C43 1.385(4) . ? C43 C44 1.372(4) . ? C43 H43 0.9500 . ? C44 C45 1.372(4) . ? C44 H44 0.9500 . ? C45 C46 1.369(4) . ? C45 H45A 0.9500 . ? C46 C47 1.393(4) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 C49 1.523(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.396(3) . ? C50 C51 1.405(3) . ? C50 H50A 0.9500 . ? C51 C52 1.520(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.406(3) . ? C53 C58 1.412(3) . ? C54 C55 1.394(3) . ? C54 C60 1.517(4) . ? C55 C56 1.373(4) . ? C55 H55A 0.9500 . ? C56 C57 1.377(4) . ? C56 H56A 0.9500 . ? C57 C58 1.397(3) . ? C57 H57A 0.9500 . ? C58 C63 1.515(4) . ? C59 C60 1.524(4) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.529(5) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.528(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.530(4) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.405(4) . ? C65 C70 1.406(3) . ? C66 C67 1.397(4) . ? C66 C72 1.526(4) . ? C67 C68 1.371(4) . ? C67 H67A 0.9500 . ? C68 C69 1.373(4) . ? C68 H68A 0.9500 . ? C69 C70 1.388(3) . ? C69 H69A 0.9500 . ? C70 C75 1.515(4) . ? C71 C72 1.524(5) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.524(4) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.528(4) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.529(4) . ? C75 H75 1.0000 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.384(4) . ? C77 C82 1.386(4) . ? C78 C79 1.391(4) . ? C78 H78 0.9500 . ? C79 C80 1.372(4) . ? C79 H79 0.9500 . ? C80 C81 1.372(4) . ? C80 H80 0.9500 . ? C81 C82 1.385(4) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.384(4) . ? C83 C88 1.391(3) . ? C84 C85 1.393(4) . ? C84 H84 0.9500 . ? C85 C86 1.373(4) . ? C85 H85 0.9500 . ? C86 C87 1.378(4) . ? C86 H86 0.9500 . ? C87 C88 1.374(4) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.388(4) . ? C89 C94 1.397(3) . ? C90 C91 1.385(4) . ? C90 H90 0.9500 . ? C91 C92 1.381(4) . ? C91 H91 0.9500 . ? C92 C93 1.372(4) . ? C92 H92 0.9500 . ? C93 C94 1.378(4) . ? C93 H93 0.9500 . ? C94 H94 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 N2 97.84(8) . . ? N1 Cu1 P1 134.46(6) . . ? N2 Cu1 P1 127.65(6) . . ? N4 Cu2 N3 97.18(8) . . ? N4 Cu2 P2 130.83(6) . . ? N3 Cu2 P2 131.82(6) . . ? C2 N1 C6 117.62(19) . . ? C2 N1 Cu1 121.32(16) . . ? C6 N1 Cu1 120.42(15) . . ? C4 N2 C18 118.1(2) . . ? C4 N2 Cu1 121.54(16) . . ? C18 N2 Cu1 120.19(16) . . ? C49 N3 C53 117.64(19) . . ? C49 N3 Cu2 121.72(16) . . ? C53 N3 Cu2 120.08(15) . . ? C51 N4 C65 118.3(2) . . ? C51 N4 Cu2 122.00(16) . . ? C65 N4 Cu2 119.60(16) . . ? C30 P1 C42 102.97(12) . . ? C30 P1 C36 103.85(11) . . ? C42 P1 C36 99.35(11) . . ? C30 P1 Cu1 114.98(8) . . ? C42 P1 Cu1 119.89(8) . . ? C36 P1 Cu1 113.50(8) . . ? C77 P2 C89 102.49(12) . . ? C77 P2 C83 102.03(11) . . ? C89 P2 C83 101.13(12) . . ? C77 P2 Cu2 118.17(9) . . ? C89 P2 Cu2 117.13(8) . . ? C83 P2 Cu2 113.45(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.5(2) . . ? N1 C2 C1 119.9(2) . . ? C3 C2 C1 115.5(2) . . ? C2 C3 C4 129.4(2) . . ? C2 C3 H3 115.3 . . ? C4 C3 H3 115.3 . . ? N2 C4 C3 124.0(2) . . ? N2 C4 C5 121.0(2) . . ? C3 C4 C5 115.0(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.5(2) . . ? C7 C6 N1 118.7(2) . . ? C11 C6 N1 120.8(2) . . ? C8 C7 C6 118.7(2) . . ? C8 C7 C13 119.7(2) . . ? C6 C7 C13 121.6(2) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 122.2(3) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C6 117.8(2) . . ? C10 C11 C16 120.4(2) . . ? C6 C11 C16 121.8(2) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C7 111.9(3) . . ? C14 C13 C12 109.0(3) . . ? C7 C13 C12 111.3(3) . . ? C14 C13 H13 108.2 . . ? C7 C13 H13 108.2 . . ? C12 C13 H13 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 C17 111.4(3) . . ? C11 C16 C15 112.9(3) . . ? C17 C16 C15 109.1(3) . . ? C11 C16 H16 107.7 . . ? C17 C16 H16 107.7 . . ? C15 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.8(2) . . ? C23 C18 N2 119.4(2) . . ? C19 C18 N2 119.8(2) . . ? C20 C19 C18 118.1(2) . . ? C20 C19 C25 119.8(2) . . ? C18 C19 C25 122.1(2) . . ? C21 C20 C19 121.9(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.4(2) . . ? C22 C23 C28 120.3(2) . . ? C18 C23 C28 121.3(2) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 C24 110.5(2) . . ? C19 C25 C26 112.4(2) . . ? C24 C25 C26 110.1(3) . . ? C19 C25 H25 107.9 . . ? C24 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 C29 112.0(2) . . ? C23 C28 C27 112.9(2) . . ? C29 C28 C27 110.1(3) . . ? C23 C28 H28 107.2 . . ? C29 C28 H28 107.2 . . ? C27 C28 H28 107.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 118.9(2) . . ? C35 C30 P1 122.7(2) . . ? C31 C30 P1 118.3(2) . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C30 C35 C34 119.6(3) . . ? C30 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C41 C36 C37 118.0(2) . . ? C41 C36 P1 124.5(2) . . ? C37 C36 P1 117.17(19) . . ? C38 C37 C36 121.3(3) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C39 C38 C37 119.7(3) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C40 C39 C38 120.0(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.6(3) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C36 C41 C40 120.5(3) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C47 C42 C43 118.4(2) . . ? C47 C42 P1 120.16(19) . . ? C43 C42 P1 121.4(2) . . ? C44 C43 C42 121.4(3) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 118.9(3) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C45 C46 C47 121.3(3) . . ? C45 C46 H46A 119.4 . . ? C47 C46 H46A 119.4 . . ? C42 C47 C46 119.7(3) . . ? C42 C47 H47A 120.2 . . ? C46 C47 H47A 120.2 . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N3 C49 C50 124.2(2) . . ? N3 C49 C48 120.3(2) . . ? C50 C49 C48 115.5(2) . . ? C49 C50 C51 129.9(2) . . ? C49 C50 H50A 115.1 . . ? C51 C50 H50A 115.1 . . ? N4 C51 C50 123.6(2) . . ? N4 C51 C52 120.9(2) . . ? C50 C51 C52 115.5(2) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C58 120.9(2) . . ? C54 C53 N3 118.9(2) . . ? C58 C53 N3 120.2(2) . . ? C55 C54 C53 118.3(2) . . ? C55 C54 C60 119.8(2) . . ? C53 C54 C60 121.9(2) . . ? C56 C55 C54 121.6(3) . . ? C56 C55 H55A 119.2 . . ? C54 C55 H55A 119.2 . . ? C55 C56 C57 119.7(2) . . ? C55 C56 H56A 120.2 . . ? C57 C56 H56A 120.2 . . ? C56 C57 C58 121.7(2) . . ? C56 C57 H57A 119.1 . . ? C58 C57 H57A 119.1 . . ? C57 C58 C53 117.8(2) . . ? C57 C58 C63 120.4(2) . . ? C53 C58 C63 121.8(2) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C54 C60 C59 113.3(2) . . ? C54 C60 C61 110.2(3) . . ? C59 C60 C61 109.8(3) . . ? C54 C60 H60 107.8 . . ? C59 C60 H60 107.8 . . ? C61 C60 H60 107.8 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C63 C62 112.1(2) . . ? C58 C63 C64 112.5(2) . . ? C62 C63 C64 109.7(2) . . ? C58 C63 H63 107.4 . . ? C62 C63 H63 107.4 . . ? C64 C63 H63 107.4 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C70 121.2(2) . . ? C66 C65 N4 119.8(2) . . ? C70 C65 N4 118.9(2) . . ? C67 C66 C65 118.0(3) . . ? C67 C66 C72 119.5(2) . . ? C65 C66 C72 122.4(2) . . ? C68 C67 C66 121.2(3) . . ? C68 C67 H67A 119.4 . . ? C66 C67 H67A 119.4 . . ? C67 C68 C69 120.0(3) . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C68 C69 C70 121.7(3) . . ? C68 C69 H69A 119.2 . . ? C70 C69 H69A 119.2 . . ? C69 C70 C65 117.9(2) . . ? C69 C70 C75 121.1(2) . . ? C65 C70 C75 121.0(2) . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C71 C72 C73 109.6(3) . . ? C71 C72 C66 110.7(3) . . ? C73 C72 C66 112.2(2) . . ? C71 C72 H72 108.1 . . ? C73 C72 H72 108.1 . . ? C66 C72 H72 108.1 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C75 C74 H74A 109.5 . . ? C75 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C75 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C70 C75 C74 112.6(2) . . ? C70 C75 C76 112.8(2) . . ? C74 C75 C76 109.9(3) . . ? C70 C75 H75 107.0 . . ? C74 C75 H75 107.0 . . ? C76 C75 H75 107.0 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C82 119.1(2) . . ? C78 C77 P2 118.4(2) . . ? C82 C77 P2 122.4(2) . . ? C77 C78 C79 120.2(3) . . ? C77 C78 H78 119.9 . . ? C79 C78 H78 119.9 . . ? C80 C79 C78 120.2(3) . . ? C80 C79 H79 119.9 . . ? C78 C79 H79 119.9 . . ? C79 C80 C81 119.8(3) . . ? C79 C80 H80 120.1 . . ? C81 C80 H80 120.1 . . ? C80 C81 C82 120.5(3) . . ? C80 C81 H81 119.8 . . ? C82 C81 H81 119.8 . . ? C81 C82 C77 120.2(3) . . ? C81 C82 H82 119.9 . . ? C77 C82 H82 119.9 . . ? C84 C83 C88 118.2(2) . . ? C84 C83 P2 123.5(2) . . ? C88 C83 P2 118.19(19) . . ? C83 C84 C85 120.2(3) . . ? C83 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C86 C85 C84 120.5(3) . . ? C86 C85 H85 119.7 . . ? C84 C85 H85 119.7 . . ? C85 C86 C87 119.6(3) . . ? C85 C86 H86 120.2 . . ? C87 C86 H86 120.2 . . ? C88 C87 C86 120.0(3) . . ? C88 C87 H87 120.0 . . ? C86 C87 H87 120.0 . . ? C87 C88 C83 121.4(3) . . ? C87 C88 H88 119.3 . . ? C83 C88 H88 119.3 . . ? C90 C89 C94 118.3(2) . . ? C90 C89 P2 118.91(19) . . ? C94 C89 P2 122.8(2) . . ? C91 C90 C89 120.7(3) . . ? C91 C90 H90 119.6 . . ? C89 C90 H90 119.6 . . ? C92 C91 C90 120.2(3) . . ? C92 C91 H91 119.9 . . ? C90 C91 H91 119.9 . . ? C93 C92 C91 119.5(3) . . ? C93 C92 H92 120.3 . . ? C91 C92 H92 120.3 . . ? C92 C93 C94 120.8(3) . . ? C92 C93 H93 119.6 . . ? C94 C93 H93 119.6 . . ? C93 C94 C89 120.4(3) . . ? C93 C94 H94 119.8 . . ? C89 C94 H94 119.8 . . ? 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 N2 Cu1 N1 C2 -9.16(19) . . . . ? P1 Cu1 N1 C2 168.38(15) . . . . ? N2 Cu1 N1 C6 161.46(17) . . . . ? P1 Cu1 N1 C6 -21.0(2) . . . . ? N1 Cu1 N2 C4 7.6(2) . . . . ? P1 Cu1 N2 C4 -170.18(16) . . . . ? N1 Cu1 N2 C18 -166.95(17) . . . . ? P1 Cu1 N2 C18 15.3(2) . . . . ? N4 Cu2 N3 C49 -9.89(19) . . . . ? P2 Cu2 N3 C49 165.68(15) . . . . ? N4 Cu2 N3 C53 161.31(17) . . . . ? P2 Cu2 N3 C53 -23.1(2) . . . . ? N3 Cu2 N4 C51 8.3(2) . . . . ? P2 Cu2 N4 C51 -167.35(15) . . . . ? N3 Cu2 N4 C65 -168.08(18) . . . . ? P2 Cu2 N4 C65 16.3(2) . . . . ? N1 Cu1 P1 C30 134.71(12) . . . . ? N2 Cu1 P1 C30 -48.37(12) . . . . ? N1 Cu1 P1 C42 11.11(13) . . . . ? N2 Cu1 P1 C42 -171.97(11) . . . . ? N1 Cu1 P1 C36 -105.91(12) . . . . ? N2 Cu1 P1 C36 71.01(12) . . . . ? N4 Cu2 P2 C77 -51.01(13) . . . . ? N3 Cu2 P2 C77 134.81(12) . . . . ? N4 Cu2 P2 C89 -174.37(12) . . . . ? N3 Cu2 P2 C89 11.45(13) . . . . ? N4 Cu2 P2 C83 68.33(12) . . . . ? N3 Cu2 P2 C83 -105.85(12) . . . . ? C6 N1 C2 C3 -168.0(2) . . . . ? Cu1 N1 C2 C3 2.9(3) . . . . ? C6 N1 C2 C1 10.2(3) . . . . ? Cu1 N1 C2 C1 -178.95(17) . . . . ? N1 C2 C3 C4 9.1(4) . . . . ? C1 C2 C3 C4 -169.2(2) . . . . ? C18 N2 C4 C3 175.0(2) . . . . ? Cu1 N2 C4 C3 0.3(3) . . . . ? C18 N2 C4 C5 -2.2(3) . . . . ? Cu1 N2 C4 C5 -176.84(18) . . . . ? C2 C3 C4 N2 -10.9(4) . . . . ? C2 C3 C4 C5 166.4(3) . . . . ? C2 N1 C6 C7 88.7(3) . . . . ? Cu1 N1 C6 C7 -82.2(2) . . . . ? C2 N1 C6 C11 -94.7(3) . . . . ? Cu1 N1 C6 C11 94.4(2) . . . . ? C11 C6 C7 C8 3.0(4) . . . . ? N1 C6 C7 C8 179.6(2) . . . . ? C11 C6 C7 C13 -176.6(3) . . . . ? N1 C6 C7 C13 0.0(4) . . . . ? C6 C7 C8 C9 -1.8(4) . . . . ? C13 C7 C8 C9 177.8(3) . . . . ? C7 C8 C9 C10 -0.4(4) . . . . ? C8 C9 C10 C11 1.4(4) . . . . ? C9 C10 C11 C6 -0.2(4) . . . . ? C9 C10 C11 C16 -179.6(3) . . . . ? C7 C6 C11 C10 -2.1(4) . . . . ? N1 C6 C11 C10 -178.6(2) . . . . ? C7 C6 C11 C16 177.4(3) . . . . ? N1 C6 C11 C16 0.9(4) . . . . ? C8 C7 C13 C14 -56.1(4) . . . . ? C6 C7 C13 C14 123.5(3) . . . . ? C8 C7 C13 C12 66.1(4) . . . . ? C6 C7 C13 C12 -114.4(3) . . . . ? C10 C11 C16 C17 65.5(4) . . . . ? C6 C11 C16 C17 -114.0(3) . . . . ? C10 C11 C16 C15 -57.7(4) . . . . ? C6 C11 C16 C15 122.9(3) . . . . ? C4 N2 C18 C23 98.3(3) . . . . ? Cu1 N2 C18 C23 -87.0(3) . . . . ? C4 N2 C18 C19 -83.8(3) . . . . ? Cu1 N2 C18 C19 90.9(3) . . . . ? C23 C18 C19 C20 -1.4(4) . . . . ? N2 C18 C19 C20 -179.3(2) . . . . ? C23 C18 C19 C25 176.1(2) . . . . ? N2 C18 C19 C25 -1.8(4) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C25 C19 C20 C21 -177.9(3) . . . . ? C19 C20 C21 C22 1.5(5) . . . . ? C20 C21 C22 C23 -1.0(5) . . . . ? C21 C22 C23 C18 -0.7(4) . . . . ? C21 C22 C23 C28 178.5(3) . . . . ? C19 C18 C23 C22 1.8(4) . . . . ? N2 C18 C23 C22 179.8(2) . . . . ? C19 C18 C23 C28 -177.3(2) . . . . ? N2 C18 C23 C28 0.6(4) . . . . ? C20 C19 C25 C24 75.7(3) . . . . ? C18 C19 C25 C24 -101.7(3) . . . . ? C20 C19 C25 C26 -47.7(4) . . . . ? C18 C19 C25 C26 134.9(3) . . . . ? C22 C23 C28 C29 89.6(3) . . . . ? C18 C23 C28 C29 -91.3(3) . . . . ? C22 C23 C28 C27 -35.4(4) . . . . ? C18 C23 C28 C27 143.7(3) . . . . ? C42 P1 C30 C35 17.2(2) . . . . ? C36 P1 C30 C35 120.4(2) . . . . ? Cu1 P1 C30 C35 -115.0(2) . . . . ? C42 P1 C30 C31 -165.4(2) . . . . ? C36 P1 C30 C31 -62.2(2) . . . . ? Cu1 P1 C30 C31 62.4(2) . . . . ? C35 C30 C31 C32 -1.5(4) . . . . ? P1 C30 C31 C32 -178.9(2) . . . . ? C30 C31 C32 C33 0.8(5) . . . . ? C31 C32 C33 C34 0.6(5) . . . . ? C32 C33 C34 C35 -1.3(5) . . . . ? C31 C30 C35 C34 0.8(4) . . . . ? P1 C30 C35 C34 178.1(2) . . . . ? C33 C34 C35 C30 0.6(5) . . . . ? C30 P1 C36 C41 -15.5(3) . . . . ? C42 P1 C36 C41 90.5(3) . . . . ? Cu1 P1 C36 C41 -141.0(2) . . . . ? C30 P1 C36 C37 171.8(2) . . . . ? C42 P1 C36 C37 -82.2(2) . . . . ? Cu1 P1 C36 C37 46.3(2) . . . . ? C41 C36 C37 C38 -1.6(4) . . . . ? P1 C36 C37 C38 171.6(2) . . . . ? C36 C37 C38 C39 1.1(5) . . . . ? C37 C38 C39 C40 -0.1(5) . . . . ? C38 C39 C40 C41 -0.5(5) . . . . ? C37 C36 C41 C40 1.0(4) . . . . ? P1 C36 C41 C40 -171.6(2) . . . . ? C39 C40 C41 C36 0.0(5) . . . . ? C30 P1 C42 C47 -111.7(2) . . . . ? C36 P1 C42 C47 141.6(2) . . . . ? Cu1 P1 C42 C47 17.5(3) . . . . ? C30 P1 C42 C43 70.3(3) . . . . ? C36 P1 C42 C43 -36.4(3) . . . . ? Cu1 P1 C42 C43 -160.5(2) . . . . ? C47 C42 C43 C44 0.0(5) . . . . ? P1 C42 C43 C44 178.1(2) . . . . ? C42 C43 C44 C45 -0.8(5) . . . . ? C43 C44 C45 C46 0.9(5) . . . . ? C44 C45 C46 C47 -0.2(5) . . . . ? C43 C42 C47 C46 0.8(4) . . . . ? P1 C42 C47 C46 -177.3(2) . . . . ? C45 C46 C47 C42 -0.7(5) . . . . ? C53 N3 C49 C50 -167.9(2) . . . . ? Cu2 N3 C49 C50 3.5(3) . . . . ? C53 N3 C49 C48 10.1(3) . . . . ? Cu2 N3 C49 C48 -178.50(17) . . . . ? N3 C49 C50 C51 9.0(4) . . . . ? C48 C49 C50 C51 -169.1(2) . . . . ? C65 N4 C51 C50 176.2(2) . . . . ? Cu2 N4 C51 C50 -0.2(3) . . . . ? C65 N4 C51 C52 -1.8(3) . . . . ? Cu2 N4 C51 C52 -178.18(18) . . . . ? C49 C50 C51 N4 -10.9(4) . . . . ? C49 C50 C51 C52 167.2(2) . . . . ? C49 N3 C53 C54 81.0(3) . . . . ? Cu2 N3 C53 C54 -90.6(2) . . . . ? C49 N3 C53 C58 -101.0(3) . . . . ? Cu2 N3 C53 C58 87.4(2) . . . . ? C58 C53 C54 C55 0.9(4) . . . . ? N3 C53 C54 C55 178.9(2) . . . . ? C58 C53 C54 C60 -176.9(2) . . . . ? N3 C53 C54 C60 1.1(4) . . . . ? C53 C54 C55 C56 1.0(4) . . . . ? C60 C54 C55 C56 178.8(3) . . . . ? C54 C55 C56 C57 -1.2(4) . . . . ? C55 C56 C57 C58 -0.6(4) . . . . ? C56 C57 C58 C53 2.4(4) . . . . ? C56 C57 C58 C63 -177.8(2) . . . . ? C54 C53 C58 C57 -2.5(4) . . . . ? N3 C53 C58 C57 179.5(2) . . . . ? C54 C53 C58 C63 177.7(2) . . . . ? N3 C53 C58 C63 -0.3(3) . . . . ? C55 C54 C60 C59 50.2(4) . . . . ? C53 C54 C60 C59 -132.1(3) . . . . ? C55 C54 C60 C61 -73.4(3) . . . . ? C53 C54 C60 C61 104.4(3) . . . . ? C57 C58 C63 C62 -75.2(3) . . . . ? C53 C58 C63 C62 104.6(3) . . . . ? C57 C58 C63 C64 49.0(3) . . . . ? C53 C58 C63 C64 -131.2(2) . . . . ? C51 N4 C65 C66 -82.6(3) . . . . ? Cu2 N4 C65 C66 93.9(3) . . . . ? C51 N4 C65 C70 100.4(3) . . . . ? Cu2 N4 C65 C70 -83.1(3) . . . . ? C70 C65 C66 C67 -1.8(4) . . . . ? N4 C65 C66 C67 -178.7(2) . . . . ? C70 C65 C66 C72 174.8(3) . . . . ? N4 C65 C66 C72 -2.1(4) . . . . ? C65 C66 C67 C68 -0.1(5) . . . . ? C72 C66 C67 C68 -176.8(3) . . . . ? C66 C67 C68 C69 1.9(5) . . . . ? C67 C68 C69 C70 -1.9(5) . . . . ? C68 C69 C70 C65 0.1(4) . . . . ? C68 C69 C70 C75 179.0(3) . . . . ? C66 C65 C70 C69 1.8(4) . . . . ? N4 C65 C70 C69 178.8(2) . . . . ? C66 C65 C70 C75 -177.1(2) . . . . ? N4 C65 C70 C75 -0.1(4) . . . . ? C67 C66 C72 C71 71.5(4) . . . . ? C65 C66 C72 C71 -105.1(3) . . . . ? C67 C66 C72 C73 -51.3(4) . . . . ? C65 C66 C72 C73 132.1(3) . . . . ? C69 C70 C75 C74 97.7(3) . . . . ? C65 C70 C75 C74 -83.4(3) . . . . ? C69 C70 C75 C76 -27.4(4) . . . . ? C65 C70 C75 C76 151.4(3) . . . . ? C89 P2 C77 C78 168.5(2) . . . . ? C83 P2 C77 C78 -87.1(2) . . . . ? Cu2 P2 C77 C78 38.1(2) . . . . ? C89 P2 C77 C82 -15.6(2) . . . . ? C83 P2 C77 C82 88.9(2) . . . . ? Cu2 P2 C77 C82 -145.97(19) . . . . ? C82 C77 C78 C79 -0.5(4) . . . . ? P2 C77 C78 C79 175.6(2) . . . . ? C77 C78 C79 C80 -0.4(4) . . . . ? C78 C79 C80 C81 0.8(5) . . . . ? C79 C80 C81 C82 -0.2(5) . . . . ? C80 C81 C82 C77 -0.7(4) . . . . ? C78 C77 C82 C81 1.1(4) . . . . ? P2 C77 C82 C81 -174.9(2) . . . . ? C77 P2 C83 C84 -4.8(3) . . . . ? C89 P2 C83 C84 100.8(2) . . . . ? Cu2 P2 C83 C84 -133.0(2) . . . . ? C77 P2 C83 C88 179.1(2) . . . . ? C89 P2 C83 C88 -75.4(2) . . . . ? Cu2 P2 C83 C88 50.9(2) . . . . ? C88 C83 C84 C85 0.8(4) . . . . ? P2 C83 C84 C85 -175.4(3) . . . . ? C83 C84 C85 C86 0.9(5) . . . . ? C84 C85 C86 C87 -1.5(6) . . . . ? C85 C86 C87 C88 0.3(5) . . . . ? C86 C87 C88 C83 1.5(5) . . . . ? C84 C83 C88 C87 -2.0(4) . . . . ? P2 C83 C88 C87 174.3(2) . . . . ? C77 P2 C89 C90 -93.4(2) . . . . ? C83 P2 C89 C90 161.4(2) . . . . ? Cu2 P2 C89 C90 37.6(2) . . . . ? C77 P2 C89 C94 87.2(2) . . . . ? C83 P2 C89 C94 -18.0(2) . . . . ? Cu2 P2 C89 C94 -141.78(19) . . . . ? C94 C89 C90 C91 -0.2(4) . . . . ? P2 C89 C90 C91 -179.7(2) . . . . ? C89 C90 C91 C92 0.1(4) . . . . ? C90 C91 C92 C93 -0.1(4) . . . . ? C91 C92 C93 C94 0.1(4) . . . . ? C92 C93 C94 C89 -0.3(4) . . . . ? C90 C89 C94 C93 0.3(4) . . . . ? P2 C89 C94 C93 179.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.445 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.049 #===END