# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jfnmm120521 _database_code_depnum_ccdc_archive 'CCDC 905746' #TrackingRef 'web_deposit_cif_file_0_Nierengarten_1354039004.jfnmm120521bis.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H70 Cu N2 O7 P2, B F4' _chemical_formula_sum 'C66 H70 B Cu F4 N2 O7 P2' _chemical_formula_weight 1215.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6380(5) _cell_length_b 14.9398(5) _cell_length_c 15.6669(6) _cell_angle_alpha 78.7330(10) _cell_angle_beta 72.8980(10) _cell_angle_gamma 83.9640(10) _cell_volume 2988.29(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 29.54 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8676 _exptl_absorpt_correction_T_max 0.9088 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47180 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.09 _reflns_number_total 17435 _reflns_number_gt 10675 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distance between B1 and F3 in the BF4 anion was restrained to 1.36 Ang according to the International Tables for Crystallography. DFIX 1.36 0.02 B1 F3 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17435 _refine_ls_number_parameters 634 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.1250 _refine_ls_wR_factor_ref 0.4038 _refine_ls_wR_factor_gt 0.3530 _refine_ls_goodness_of_fit_ref 1.484 _refine_ls_restrained_S_all 1.484 _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 C1 C 0.7353(5) 0.7195(4) 0.9406(4) 0.0374(12) Uani 1 1 d . . . C2 C 0.7683(5) 0.6793(5) 1.0170(4) 0.0514(16) Uani 1 1 d . . . H2 H 0.7477 0.7068 1.0697 0.062 Uiso 1 1 calc R . . C3 C 0.8279(6) 0.6033(6) 1.0162(4) 0.060(2) Uani 1 1 d . . . H3 H 0.8507 0.5777 1.0680 0.072 Uiso 1 1 calc R . . C4 C 0.8579(5) 0.5601(5) 0.9393(4) 0.0478(16) Uani 1 1 d . . . C5 C 0.9168(5) 0.4744(6) 0.9359(5) 0.064(2) Uani 1 1 d . . . H5 H 0.9336 0.4421 0.9887 0.077 Uiso 1 1 calc R . . C6 C 0.9485(5) 0.4394(4) 0.8581(5) 0.0546(18) Uani 1 1 d . . . H6 H 0.9898 0.3841 0.8560 0.065 Uiso 1 1 calc R . . C7 C 0.9205(4) 0.4849(4) 0.7802(4) 0.0412(13) Uani 1 1 d . . . C8 C 0.9510(5) 0.4494(4) 0.6986(5) 0.0430(14) Uani 1 1 d . . . H8 H 0.9936 0.3950 0.6942 0.052 Uiso 1 1 calc R . . C9 C 0.9189(4) 0.4943(4) 0.6260(4) 0.0376(12) Uani 1 1 d . . . H9 H 0.9419 0.4727 0.5699 0.045 Uiso 1 1 calc R . . C10 C 0.8514(4) 0.5728(3) 0.6342(4) 0.0313(10) Uani 1 1 d . . . C11 C 0.8568(4) 0.5652(3) 0.7820(3) 0.0300(10) Uani 1 1 d . . . C12 C 0.8256(4) 0.6044(4) 0.8638(4) 0.0324(11) Uani 1 1 d . . . C13 C 0.6612(6) 0.7990(4) 0.9456(4) 0.0509(17) Uani 1 1 d . . . H13A H 0.6497 0.8210 0.8853 0.061 Uiso 1 1 calc R . . H13B H 0.6903 0.8491 0.9620 0.061 Uiso 1 1 calc R . . C14 C 0.5593(6) 0.7755(6) 1.0150(5) 0.0584(19) Uani 1 1 d . . . H14A H 0.5712 0.7510 1.0748 0.070 Uiso 1 1 calc R . . H14B H 0.5286 0.7274 0.9971 0.070 Uiso 1 1 calc R . . C15 C 0.4848(9) 0.8592(9) 1.0228(9) 0.1068(12) Uani 1 1 d . . . H15A H 0.5148 0.9065 1.0424 0.128 Uiso 1 1 calc R . . H15B H 0.4749 0.8848 0.9625 0.128 Uiso 1 1 calc R . . C16 C 0.3248(10) 0.9165(9) 1.0872(9) 0.1068(12) Uani 1 1 d . . . H16A H 0.3589 0.9687 1.0946 0.128 Uiso 1 1 calc R . . H16B H 0.2681 0.9009 1.1431 0.128 Uiso 1 1 calc R . . C17 C 0.2776(10) 0.9480(9) 1.0058(9) 0.1068(12) Uani 1 1 d . . . H17A H 0.2367 1.0065 1.0115 0.128 Uiso 1 1 calc R . . H17B H 0.3322 0.9559 0.9474 0.128 Uiso 1 1 calc R . . C18 C 0.1361(10) 0.9003(9) 0.9648(9) 0.1068(12) Uani 1 1 d . . . H18A H 0.0927 0.9513 0.9907 0.128 Uiso 1 1 calc R . . H18B H 0.1713 0.9241 0.9007 0.128 Uiso 1 1 calc R . . C19 C 0.0750(10) 0.8356(9) 0.9670(9) 0.1068(12) Uani 1 1 d . . . H19A H 0.0165 0.8655 0.9450 0.128 Uiso 1 1 calc R . . H19B H 0.0466 0.8067 1.0310 0.128 Uiso 1 1 calc R . . C20 C 0.1219(10) 0.7641(9) 0.8290(8) 0.1068(12) Uani 1 1 d . . . H20A H 0.1396 0.8276 0.8002 0.128 Uiso 1 1 calc R . . H20B H 0.0487 0.7600 0.8328 0.128 Uiso 1 1 calc R . . C21 C 0.1842(10) 0.7023(9) 0.7590(9) 0.1068(12) Uani 1 1 d . . . H21A H 0.1867 0.7341 0.6967 0.128 Uiso 1 1 calc R . . H21B H 0.2555 0.6915 0.7634 0.128 Uiso 1 1 calc R . . C22 C 0.1362(10) 0.6136(9) 0.7764(9) 0.1068(12) Uani 1 1 d . . . H22A H 0.1274 0.5845 0.8405 0.128 Uiso 1 1 calc R . . H22B H 0.0674 0.6240 0.7660 0.128 Uiso 1 1 calc R . . C23 C 0.1993(10) 0.5534(9) 0.7175(9) 0.1068(12) Uani 1 1 d . . . H23A H 0.1635 0.4967 0.7254 0.128 Uiso 1 1 calc R . . H23B H 0.2125 0.5838 0.6533 0.128 Uiso 1 1 calc R . . C24 C 0.3443(10) 0.4581(9) 0.6959(9) 0.1068(12) Uani 1 1 d . . . H24A H 0.3692 0.4786 0.6296 0.128 Uiso 1 1 calc R . . H24B H 0.2983 0.4074 0.7076 0.128 Uiso 1 1 calc R . . C25 C 0.4375(10) 0.4243(9) 0.7351(9) 0.1068(12) Uani 1 1 d . . . H25A H 0.4730 0.4787 0.7355 0.128 Uiso 1 1 calc R . . H25B H 0.4101 0.3946 0.7990 0.128 Uiso 1 1 calc R . . C26 C 0.5824(10) 0.3327(9) 0.7316(9) 0.1068(12) Uani 1 1 d . . . H26A H 0.6156 0.2789 0.7041 0.128 Uiso 1 1 calc R . . H26B H 0.5515 0.3107 0.7971 0.128 Uiso 1 1 calc R . . C27 C 0.6654(6) 0.3981(7) 0.7214(6) 0.071(2) Uani 1 1 d . . . H27A H 0.6336 0.4515 0.7501 0.085 Uiso 1 1 calc R . . H27B H 0.7156 0.3668 0.7534 0.085 Uiso 1 1 calc R . . C28 C 0.6786(6) 0.5062(5) 0.5770(6) 0.0591(19) Uani 1 1 d . . . H28A H 0.6336 0.5457 0.6182 0.071 Uiso 1 1 calc R . . H28B H 0.6371 0.4857 0.5428 0.071 Uiso 1 1 calc R . . C29 C 0.7654(5) 0.5591(4) 0.5126(4) 0.0436(14) Uani 1 1 d . . . H29A H 0.7403 0.5981 0.4638 0.052 Uiso 1 1 calc R . . H29B H 0.8195 0.5157 0.4843 0.052 Uiso 1 1 calc R . . C30 C 0.8124(5) 0.6189(3) 0.5561(4) 0.0363(12) Uani 1 1 d . . . H30A H 0.8702 0.6496 0.5088 0.044 Uiso 1 1 calc R . . H30B H 0.7603 0.6671 0.5770 0.044 Uiso 1 1 calc R . . C31 C 0.5194(4) 0.8846(4) 0.7386(3) 0.0307(10) Uani 1 1 d . . . C32 C 0.4229(4) 0.9096(4) 0.7220(4) 0.0398(13) Uani 1 1 d . . . H32 H 0.3883 0.8661 0.7063 0.048 Uiso 1 1 calc R . . C33 C 0.3787(5) 0.9950(5) 0.7282(4) 0.0515(17) Uani 1 1 d . . . H33 H 0.3127 1.0098 0.7190 0.062 Uiso 1 1 calc R . . C34 C 0.4299(5) 1.0609(4) 0.7478(4) 0.0443(14) Uani 1 1 d . . . H34 H 0.3994 1.1207 0.7512 0.053 Uiso 1 1 calc R . . C35 C 0.5257(5) 1.0384(4) 0.7625(4) 0.0399(13) Uani 1 1 d . . . H35 H 0.5614 1.0828 0.7759 0.048 Uiso 1 1 calc R . . C36 C 0.5692(4) 0.9500(3) 0.7574(3) 0.0308(10) Uani 1 1 d . . . H36 H 0.6349 0.9350 0.7672 0.037 Uiso 1 1 calc R . . C37 C 0.4889(4) 0.6938(4) 0.8235(4) 0.0385(12) Uani 1 1 d . . . C38 C 0.5240(8) 0.6030(4) 0.8397(5) 0.069(3) Uani 1 1 d . . . H38 H 0.5890 0.5842 0.8033 0.082 Uiso 1 1 calc R . . C39 C 0.4674(10) 0.5395(6) 0.9070(5) 0.093(4) Uani 1 1 d . . . H39 H 0.4924 0.4777 0.9163 0.112 Uiso 1 1 calc R . . C40 C 0.3736(9) 0.5670(8) 0.9609(7) 0.091(3) Uani 1 1 d . . . H40 H 0.3324 0.5240 1.0067 0.109 Uiso 1 1 calc R . . C41 C 0.3406(6) 0.6575(11) 0.9473(7) 0.106(5) Uani 1 1 d . . . H41 H 0.2779 0.6773 0.9862 0.127 Uiso 1 1 calc R . . C42 C 0.3973(5) 0.7205(6) 0.8777(5) 0.060(2) Uani 1 1 d . . . H42 H 0.3720 0.7823 0.8680 0.071 Uiso 1 1 calc R . . C43 C 0.5545(4) 0.7483(3) 0.6282(4) 0.0301(10) Uani 1 1 d . . . C44 C 0.4733(5) 0.6978(4) 0.6266(4) 0.0407(13) Uani 1 1 d . . . H44 H 0.4270 0.6716 0.6820 0.049 Uiso 1 1 calc R . . C45 C 0.4607(6) 0.6864(4) 0.5455(5) 0.0466(15) Uani 1 1 d . . . H45 H 0.4056 0.6526 0.5452 0.056 Uiso 1 1 calc R . . C46 C 0.5280(6) 0.7240(4) 0.4640(5) 0.0490(16) Uani 1 1 d . . . H46 H 0.5189 0.7157 0.4083 0.059 Uiso 1 1 calc R . . C47 C 0.6094(5) 0.7742(4) 0.4635(4) 0.0398(13) Uani 1 1 d . . . H47 H 0.6561 0.7995 0.4079 0.048 Uiso 1 1 calc R . . C48 C 0.6205(4) 0.7863(3) 0.5447(3) 0.0297(10) Uani 1 1 d . . . C49 C 0.7082(4) 0.9172(3) 0.5463(3) 0.0294(10) Uani 1 1 d . . . C50 C 0.6462(4) 0.9819(4) 0.5096(4) 0.0345(11) Uani 1 1 d . . . H50 H 0.5970 0.9640 0.4850 0.041 Uiso 1 1 calc R . . C51 C 0.6557(5) 1.0740(4) 0.5085(4) 0.0410(13) Uani 1 1 d . . . H51 H 0.6132 1.1193 0.4830 0.049 Uiso 1 1 calc R . . C52 C 0.7281(5) 1.0993(4) 0.5451(4) 0.0396(13) Uani 1 1 d . . . H52 H 0.7345 1.1621 0.5446 0.048 Uiso 1 1 calc R . . C53 C 0.7910(4) 1.0339(3) 0.5821(4) 0.0343(11) Uani 1 1 d . . . H53 H 0.8406 1.0521 0.6061 0.041 Uiso 1 1 calc R . . C54 C 0.7814(4) 0.9415(3) 0.5843(3) 0.0257(9) Uani 1 1 d . . . C55 C 0.9466(4) 0.8035(3) 0.5495(3) 0.0279(10) Uani 1 1 d . . . C56 C 1.0194(4) 0.7365(3) 0.5714(4) 0.0370(12) Uani 1 1 d . . . H56 H 1.0180 0.7157 0.6330 0.044 Uiso 1 1 calc R . . C57 C 1.0933(5) 0.7004(4) 0.5038(5) 0.0440(14) Uani 1 1 d . . . H57 H 1.1429 0.6556 0.5193 0.053 Uiso 1 1 calc R . . C58 C 1.0956(5) 0.7286(4) 0.4148(5) 0.0503(16) Uani 1 1 d . . . H58 H 1.1469 0.7036 0.3688 0.060 Uiso 1 1 calc R . . C59 C 1.0239(5) 0.7929(4) 0.3918(4) 0.0408(13) Uani 1 1 d . . . H59 H 1.0253 0.8119 0.3300 0.049 Uiso 1 1 calc R . . C60 C 0.9494(4) 0.8303(3) 0.4588(3) 0.0336(11) Uani 1 1 d . . . H60 H 0.8998 0.8747 0.4424 0.040 Uiso 1 1 calc R . . C61 C 0.9262(4) 0.9067(3) 0.6892(3) 0.0305(10) Uani 1 1 d . . . C62 C 1.0284(5) 0.9265(4) 0.6479(4) 0.0446(14) Uani 1 1 d . . . H62 H 1.0623 0.9085 0.5912 0.053 Uiso 1 1 calc R . . C63 C 1.0815(6) 0.9716(5) 0.6871(5) 0.0545(18) Uani 1 1 d . . . H63 H 1.1520 0.9821 0.6582 0.065 Uiso 1 1 calc R . . C64 C 1.0348(7) 1.0015(5) 0.7671(6) 0.063(2) Uani 1 1 d . . . H64 H 1.0715 1.0327 0.7943 0.075 Uiso 1 1 calc R . . C65 C 0.9338(7) 0.9850(5) 0.8063(6) 0.062(2) Uani 1 1 d . . . H65 H 0.8994 1.0085 0.8602 0.075 Uiso 1 1 calc R . . C66 C 0.8789(6) 0.9362(6) 0.7721(5) 0.0585(19) Uani 1 1 d . . . H66 H 0.8099 0.9225 0.8041 0.070 Uiso 1 1 calc R . . N1 N 0.7653(3) 0.6833(3) 0.8630(3) 0.0297(9) Uani 1 1 d . . . N2 N 0.8219(3) 0.6086(3) 0.7098(3) 0.0263(8) Uani 1 1 d . . . O1 O 0.7079(3) 0.8254(2) 0.5462(2) 0.0302(7) Uani 1 1 d . . . O2 O 0.3978(5) 0.8399(6) 1.0792(5) 0.0949(9) Uani 1 1 d . . . O3 O 0.2112(5) 0.8733(6) 1.0115(5) 0.0949(9) Uani 1 1 d . . . O4 O 0.1258(5) 0.7558(6) 0.9090(5) 0.0949(9) Uani 1 1 d . . . O5 O 0.2884(5) 0.5332(6) 0.7389(5) 0.0949(9) Uani 1 1 d . . . O6 O 0.5055(5) 0.3680(6) 0.6937(5) 0.0949(9) Uani 1 1 d . . . O7 O 0.7176(5) 0.4287(6) 0.6289(5) 0.0949(9) Uani 1 1 d . . . B1 B 0.8323(11) 0.7819(11) 0.2170(14) 0.152(9) Uani 1 1 d D . . F1 F 0.8508(7) 0.8539(7) 0.1349(6) 0.1496(16) Uani 1 1 d . . . F2 F 0.7379(7) 0.7602(7) 0.2104(6) 0.1496(16) Uani 1 1 d . . . F3 F 0.9387(7) 0.7766(6) 0.1971(6) 0.1496(16) Uani 1 1 d D . . F4 F 0.8025(7) 0.8405(6) 0.2793(6) 0.1496(16) Uani 1 1 d . . . P1 P 0.57776(10) 0.76805(8) 0.73296(8) 0.0272(3) Uani 1 1 d . . . P2 P 0.84996(9) 0.84764(8) 0.64170(8) 0.0241(3) Uani 1 1 d . . . Cu1 Cu 0.74495(4) 0.73724(4) 0.73510(4) 0.0258(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.037(3) 0.032(3) -0.005(2) -0.006(2) 0.000(2) C2 0.043(3) 0.077(5) 0.030(3) -0.002(3) -0.010(3) 0.005(3) C3 0.048(4) 0.086(5) 0.038(3) 0.005(3) -0.020(3) 0.017(4) C4 0.032(3) 0.059(4) 0.039(3) 0.010(3) -0.007(2) 0.012(3) C5 0.044(4) 0.073(5) 0.053(4) 0.022(3) -0.012(3) 0.024(4) C6 0.042(3) 0.041(3) 0.068(4) 0.011(3) -0.016(3) 0.019(3) C7 0.027(3) 0.034(3) 0.054(3) 0.006(2) -0.010(2) 0.007(2) C8 0.033(3) 0.025(2) 0.067(4) -0.009(2) -0.011(3) 0.010(2) C9 0.033(3) 0.025(2) 0.052(3) -0.010(2) -0.009(2) 0.007(2) C10 0.026(2) 0.019(2) 0.044(3) -0.0008(18) -0.005(2) -0.0014(18) C11 0.020(2) 0.026(2) 0.039(3) 0.0028(19) -0.007(2) -0.0001(18) C12 0.019(2) 0.035(3) 0.036(3) 0.007(2) -0.0054(19) -0.001(2) C13 0.078(5) 0.041(3) 0.029(3) -0.008(2) -0.011(3) 0.012(3) C14 0.051(4) 0.073(5) 0.047(4) -0.007(3) -0.016(3) 0.020(4) C15 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C16 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C17 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C18 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C19 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C20 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C21 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C22 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C23 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C24 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C25 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C26 0.096(3) 0.126(3) 0.108(2) -0.043(2) -0.042(2) 0.035(2) C27 0.052(4) 0.101(7) 0.066(5) -0.034(5) -0.008(4) -0.011(5) C28 0.045(4) 0.040(3) 0.092(6) -0.016(3) -0.018(4) 0.006(3) C29 0.048(4) 0.029(3) 0.056(4) -0.015(2) -0.016(3) 0.006(3) C30 0.046(3) 0.021(2) 0.042(3) -0.0090(19) -0.013(2) 0.007(2) C31 0.026(2) 0.033(2) 0.028(2) -0.0042(19) -0.0048(19) 0.008(2) C32 0.032(3) 0.047(3) 0.047(3) -0.016(2) -0.021(2) 0.010(2) C33 0.040(3) 0.062(4) 0.053(4) -0.016(3) -0.019(3) 0.028(3) C34 0.049(4) 0.035(3) 0.045(3) -0.009(2) -0.013(3) 0.014(3) C35 0.052(4) 0.034(3) 0.031(3) -0.005(2) -0.011(2) 0.008(3) C36 0.032(3) 0.030(2) 0.028(2) -0.0039(18) -0.009(2) 0.006(2) C37 0.031(3) 0.049(3) 0.033(3) -0.003(2) -0.006(2) -0.007(2) C38 0.098(7) 0.034(3) 0.051(4) -0.007(3) 0.018(4) -0.013(4) C39 0.151(11) 0.062(5) 0.050(4) -0.007(4) 0.016(5) -0.064(6) C40 0.096(8) 0.105(8) 0.071(6) 0.025(5) -0.026(6) -0.066(7) C41 0.030(4) 0.200(14) 0.068(6) 0.015(7) 0.001(4) -0.032(6) C42 0.027(3) 0.081(5) 0.053(4) 0.013(3) -0.001(3) 0.003(3) C43 0.025(2) 0.028(2) 0.039(3) -0.0047(19) -0.013(2) 0.0021(19) C44 0.040(3) 0.040(3) 0.048(3) -0.007(2) -0.020(3) -0.005(2) C45 0.055(4) 0.029(3) 0.068(4) -0.013(3) -0.032(3) -0.006(3) C46 0.063(4) 0.041(3) 0.060(4) -0.026(3) -0.039(3) 0.014(3) C47 0.044(3) 0.039(3) 0.038(3) -0.008(2) -0.016(3) 0.009(3) C48 0.030(2) 0.022(2) 0.036(2) -0.0042(18) -0.011(2) 0.0058(19) C49 0.025(2) 0.028(2) 0.028(2) 0.0011(17) 0.0003(19) 0.0006(19) C50 0.032(3) 0.031(2) 0.035(3) 0.000(2) -0.009(2) 0.006(2) C51 0.040(3) 0.026(2) 0.049(3) 0.003(2) -0.011(3) 0.010(2) C52 0.035(3) 0.023(2) 0.052(3) 0.001(2) -0.005(2) 0.004(2) C53 0.034(3) 0.024(2) 0.039(3) -0.0014(19) -0.006(2) 0.003(2) C54 0.022(2) 0.021(2) 0.029(2) -0.0002(16) -0.0040(18) 0.0028(17) C55 0.024(2) 0.019(2) 0.037(2) -0.0041(17) -0.0044(19) -0.0002(18) C56 0.033(3) 0.026(2) 0.047(3) -0.001(2) -0.009(2) 0.005(2) C57 0.030(3) 0.026(2) 0.066(4) -0.009(2) -0.004(3) 0.011(2) C58 0.036(3) 0.039(3) 0.070(4) -0.026(3) 0.005(3) 0.002(3) C59 0.041(3) 0.035(3) 0.042(3) -0.012(2) -0.001(2) 0.001(2) C60 0.036(3) 0.029(2) 0.031(2) -0.0057(19) -0.005(2) 0.005(2) C61 0.033(3) 0.026(2) 0.034(2) -0.0030(18) -0.014(2) 0.002(2) C62 0.051(4) 0.047(3) 0.038(3) 0.004(2) -0.015(3) -0.023(3) C63 0.053(4) 0.059(4) 0.056(4) 0.012(3) -0.025(3) -0.034(3) C64 0.084(6) 0.037(3) 0.094(6) -0.014(3) -0.065(5) 0.003(3) C65 0.066(5) 0.061(4) 0.077(5) -0.039(4) -0.033(4) 0.015(4) C66 0.044(4) 0.081(5) 0.062(4) -0.046(4) -0.017(3) 0.018(4) N1 0.026(2) 0.030(2) 0.030(2) -0.0003(16) -0.0065(17) -0.0015(17) N2 0.0223(19) 0.0179(17) 0.035(2) -0.0003(15) -0.0046(16) -0.0030(15) O1 0.0298(18) 0.0259(16) 0.0346(18) -0.0042(13) -0.0119(15) 0.0059(14) O2 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) O3 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) O4 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) O5 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) O6 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) O7 0.0590(16) 0.135(3) 0.093(2) -0.0365(18) -0.0222(15) 0.0167(17) B1 0.095(11) 0.107(11) 0.196(17) -0.074(12) 0.094(11) -0.050(9) F1 0.137(4) 0.143(3) 0.158(4) -0.052(3) -0.012(3) 0.008(3) F2 0.137(4) 0.143(3) 0.158(4) -0.052(3) -0.012(3) 0.008(3) F3 0.137(4) 0.143(3) 0.158(4) -0.052(3) -0.012(3) 0.008(3) F4 0.137(4) 0.143(3) 0.158(4) -0.052(3) -0.012(3) 0.008(3) P1 0.0228(6) 0.0275(6) 0.0303(6) -0.0044(5) -0.0074(5) 0.0016(5) P2 0.0225(6) 0.0198(5) 0.0282(6) -0.0019(4) -0.0062(5) 0.0009(4) Cu1 0.0250(3) 0.0209(3) 0.0290(3) -0.0008(2) -0.0073(2) 0.0022(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.362(7) . ? C1 C2 1.406(8) . ? C1 C13 1.476(8) . ? C2 C3 1.324(10) . ? C2 H2 0.9500 . ? C3 C4 1.414(10) . ? C3 H3 0.9500 . ? C4 C12 1.404(7) . ? C4 C5 1.440(9) . ? C5 C6 1.355(11) . ? C5 H5 0.9500 . ? C6 C7 1.412(8) . ? C6 H6 0.9500 . ? C7 C11 1.405(7) . ? C7 C8 1.411(9) . ? C8 C9 1.367(8) . ? C8 H8 0.9500 . ? C9 C10 1.415(7) . ? C9 H9 0.9500 . ? C10 N2 1.332(7) . ? C10 C30 1.494(7) . ? C11 N2 1.375(6) . ? C11 C12 1.444(8) . ? C12 N1 1.365(6) . ? C13 C14 1.517(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O2 1.275(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.436(12) . ? C16 C17 1.565(15) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O3 1.483(15) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.330(17) . ? C18 O3 1.408(13) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O4 1.614(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O4 1.252(12) . ? C20 C21 1.568(15) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.481(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.448(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O5 1.343(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O5 1.450(13) . ? C24 C25 1.566(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O6 1.297(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O6 1.364(12) . ? C26 C27 1.526(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O7 1.421(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O7 1.429(10) . ? C28 C29 1.492(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.513(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.369(8) . ? C31 C32 1.414(7) . ? C31 P1 1.844(5) . ? C32 C33 1.361(8) . ? C32 H32 0.9500 . ? C33 C34 1.392(10) . ? C33 H33 0.9500 . ? C34 C35 1.388(9) . ? C34 H34 0.9500 . ? C35 C36 1.397(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.358(9) . ? C37 C38 1.391(9) . ? C37 P1 1.835(6) . ? C38 C39 1.376(10) . ? C38 H38 0.9500 . ? C39 C40 1.380(16) . ? C39 H39 0.9500 . ? C40 C41 1.376(17) . ? C40 H40 0.9500 . ? C41 C42 1.388(13) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.403(7) . ? C43 C44 1.412(8) . ? C43 P1 1.843(5) . ? C44 C45 1.376(8) . ? C44 H44 0.9500 . ? C45 C46 1.388(10) . ? C45 H45 0.9500 . ? C46 C47 1.401(9) . ? C46 H46 0.9500 . ? C47 C48 1.372(7) . ? C47 H47 0.9500 . ? C48 O1 1.390(6) . ? C49 C50 1.370(7) . ? C49 O1 1.373(6) . ? C49 C54 1.412(7) . ? C50 C51 1.392(8) . ? C50 H50 0.9500 . ? C51 C52 1.393(9) . ? C51 H51 0.9500 . ? C52 C53 1.386(7) . ? C52 H52 0.9500 . ? C53 C54 1.393(7) . ? C53 H53 0.9500 . ? C54 P2 1.836(5) . ? C55 C60 1.390(7) . ? C55 C56 1.401(7) . ? C55 P2 1.824(5) . ? C56 C57 1.381(8) . ? C56 H56 0.9500 . ? C57 C58 1.368(10) . ? C57 H57 0.9500 . ? C58 C59 1.372(9) . ? C58 H58 0.9500 . ? C59 C60 1.389(7) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.390(8) . ? C61 C66 1.402(8) . ? C61 P2 1.822(5) . ? C62 C63 1.371(9) . ? C62 H62 0.9500 . ? C63 C64 1.366(11) . ? C63 H63 0.9500 . ? C64 C65 1.360(12) . ? C64 H64 0.9500 . ? C65 C66 1.373(10) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? N1 Cu1 2.095(4) . ? N2 Cu1 2.140(4) . ? B1 F4 1.382(16) . ? B1 F3 1.388(14) . ? B1 F2 1.398(19) . ? B1 F1 1.48(2) . ? P1 Cu1 2.2869(14) . ? P2 Cu1 2.2879(13) . ? 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 C1 C2 121.5(5) . . ? N1 C1 C13 118.6(5) . . ? C2 C1 C13 119.8(5) . . ? C3 C2 C1 120.6(6) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.7(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C12 C4 C3 116.5(6) . . ? C12 C4 C5 119.9(6) . . ? C3 C4 C5 123.6(6) . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.2(6) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C11 C7 C8 117.2(5) . . ? C11 C7 C6 121.2(6) . . ? C8 C7 C6 121.5(5) . . ? C9 C8 C7 119.4(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.1(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 122.0(5) . . ? N2 C10 C30 118.0(4) . . ? C9 C10 C30 119.9(5) . . ? N2 C11 C7 123.4(5) . . ? N2 C11 C12 117.9(4) . . ? C7 C11 C12 118.7(5) . . ? N1 C12 C4 123.6(5) . . ? N1 C12 C11 117.4(4) . . ? C4 C12 C11 119.1(5) . . ? C1 C13 C14 111.7(5) . . ? C1 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C1 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C15 111.3(8) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O2 C15 C14 112.0(11) . . ? O2 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? O2 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O2 C16 C17 115.5(9) . . ? O2 C16 H16A 108.4 . . ? C17 C16 H16A 108.4 . . ? O2 C16 H16B 108.4 . . ? C17 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? O3 C17 C16 104.6(10) . . ? O3 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O3 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C19 C18 O3 115.9(12) . . ? C19 C18 H18A 108.3 . . ? O3 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? O3 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C18 C19 O4 116.9(11) . . ? C18 C19 H19A 108.1 . . ? O4 C19 H19A 108.1 . . ? C18 C19 H19B 108.1 . . ? O4 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? O4 C20 C21 125.3(10) . . ? O4 C20 H20A 106.0 . . ? C21 C20 H20A 106.0 . . ? O4 C20 H20B 106.0 . . ? C21 C20 H20B 106.0 . . ? H20A C20 H20B 106.3 . . ? C22 C21 C20 110.8(11) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 110.7(12) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? O5 C23 C22 108.5(10) . . ? O5 C23 H23A 110.0 . . ? C22 C23 H23A 110.0 . . ? O5 C23 H23B 110.0 . . ? C22 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O5 C24 C25 109.3(9) . . ? O5 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? O5 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? O6 C25 C24 117.3(10) . . ? O6 C25 H25A 108.0 . . ? C24 C25 H25A 108.0 . . ? O6 C25 H25B 108.0 . . ? C24 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? O6 C26 C27 115.6(11) . . ? O6 C26 H26A 108.4 . . ? C27 C26 H26A 108.4 . . ? O6 C26 H26B 108.4 . . ? C27 C26 H26B 108.4 . . ? H26A C26 H26B 107.4 . . ? O7 C27 C26 111.8(8) . . ? O7 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? O7 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? O7 C28 C29 110.0(6) . . ? O7 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? O7 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 114.0(6) . . ? C28 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C10 C30 C29 116.9(4) . . ? C10 C30 H30A 108.1 . . ? C29 C30 H30A 108.1 . . ? C10 C30 H30B 108.1 . . ? C29 C30 H30B 108.1 . . ? H30A C30 H30B 107.3 . . ? C36 C31 C32 117.9(5) . . ? C36 C31 P1 120.9(4) . . ? C32 C31 P1 121.2(4) . . ? C33 C32 C31 121.2(6) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 120.3(6) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 119.4(6) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 121.6(5) . . ? C31 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C42 C37 C38 118.6(6) . . ? C42 C37 P1 126.3(5) . . ? C38 C37 P1 115.1(5) . . ? C39 C38 C37 121.9(8) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 119.1(9) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C41 C40 C39 119.1(8) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 121.2(9) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C37 C42 C41 120.0(8) . . ? C37 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C48 C43 C44 117.7(5) . . ? C48 C43 P1 118.3(4) . . ? C44 C43 P1 124.0(4) . . ? C45 C44 C43 120.5(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 120.4(6) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 120.3(6) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 118.9(6) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 O1 119.5(5) . . ? C47 C48 C43 122.2(5) . . ? O1 C48 C43 117.6(4) . . ? C50 C49 O1 123.7(5) . . ? C50 C49 C54 121.6(5) . . ? O1 C49 C54 114.7(4) . . ? C49 C50 C51 119.7(5) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C50 C51 C52 119.5(5) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C53 C52 C51 120.8(5) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 120.1(5) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C53 C54 C49 118.2(4) . . ? C53 C54 P2 124.6(4) . . ? C49 C54 P2 117.0(3) . . ? C60 C55 C56 118.2(5) . . ? C60 C55 P2 123.4(4) . . ? C56 C55 P2 118.4(4) . . ? C57 C56 C55 120.4(5) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C58 C57 C56 120.5(5) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 120.2(5) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C60 120.1(6) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C55 120.6(5) . . ? C59 C60 H60 119.7 . . ? C55 C60 H60 119.7 . . ? C62 C61 C66 117.2(6) . . ? C62 C61 P2 124.4(4) . . ? C66 C61 P2 118.5(5) . . ? C63 C62 C61 121.6(6) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C64 C63 C62 121.2(7) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C65 C64 C63 117.5(6) . . ? C65 C64 H64 121.2 . . ? C63 C64 H64 121.2 . . ? C64 C65 C66 123.4(7) . . ? C64 C65 H65 118.3 . . ? C66 C65 H65 118.3 . . ? C65 C66 C61 119.1(7) . . ? C65 C66 H66 120.5 . . ? C61 C66 H66 120.5 . . ? C1 N1 C12 117.1(4) . . ? C1 N1 Cu1 129.6(4) . . ? C12 N1 Cu1 113.1(3) . . ? C10 N2 C11 117.8(4) . . ? C10 N2 Cu1 130.6(3) . . ? C11 N2 Cu1 110.9(3) . . ? C49 O1 C48 121.1(4) . . ? C15 O2 C16 113.7(11) . . ? C18 O3 C17 113.4(9) . . ? C20 O4 C19 119.6(9) . . ? C23 O5 C24 110.2(8) . . ? C25 O6 C26 117.6(9) . . ? C27 O7 C28 121.0(7) . . ? F4 B1 F3 103.3(13) . . ? F4 B1 F2 102.0(9) . . ? F3 B1 F2 154.6(14) . . ? F4 B1 F1 96.3(11) . . ? F3 B1 F1 83.7(8) . . ? F2 B1 F1 94.3(16) . . ? C37 P1 C43 103.9(3) . . ? C37 P1 C31 104.9(3) . . ? C43 P1 C31 100.6(2) . . ? C37 P1 Cu1 112.54(19) . . ? C43 P1 Cu1 113.14(17) . . ? C31 P1 Cu1 119.93(18) . . ? C61 P2 C55 102.8(2) . . ? C61 P2 C54 103.3(2) . . ? C55 P2 C54 104.3(2) . . ? C61 P2 Cu1 119.00(17) . . ? C55 P2 Cu1 112.42(16) . . ? C54 P2 Cu1 113.44(16) . . ? N1 Cu1 N2 79.78(16) . . ? N1 Cu1 P1 114.99(12) . . ? N2 Cu1 P1 120.98(12) . . ? N1 Cu1 P2 119.17(13) . . ? N2 Cu1 P2 106.52(11) . . ? P1 Cu1 P2 111.98(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 N1 C1 C2 C3 -1.6(10) . . . . ? C13 C1 C2 C3 174.2(7) . . . . ? C1 C2 C3 C4 -1.3(12) . . . . ? C2 C3 C4 C12 3.2(11) . . . . ? C2 C3 C4 C5 -175.8(8) . . . . ? C12 C4 C5 C6 5.2(11) . . . . ? C3 C4 C5 C6 -175.8(7) . . . . ? C4 C5 C6 C7 -2.6(12) . . . . ? C5 C6 C7 C11 -2.0(10) . . . . ? C5 C6 C7 C8 -179.0(7) . . . . ? C11 C7 C8 C9 0.6(9) . . . . ? C6 C7 C8 C9 177.7(6) . . . . ? C7 C8 C9 C10 -3.2(9) . . . . ? C8 C9 C10 N2 4.0(8) . . . . ? C8 C9 C10 C30 -177.0(5) . . . . ? C8 C7 C11 N2 1.6(8) . . . . ? C6 C7 C11 N2 -175.5(5) . . . . ? C8 C7 C11 C12 -178.8(5) . . . . ? C6 C7 C11 C12 4.0(8) . . . . ? C3 C4 C12 N1 -2.4(9) . . . . ? C5 C4 C12 N1 176.6(6) . . . . ? C3 C4 C12 C11 177.9(6) . . . . ? C5 C4 C12 C11 -3.1(9) . . . . ? N2 C11 C12 N1 -1.5(7) . . . . ? C7 C11 C12 N1 178.9(5) . . . . ? N2 C11 C12 C4 178.2(5) . . . . ? C7 C11 C12 C4 -1.4(8) . . . . ? N1 C1 C13 C14 113.6(6) . . . . ? C2 C1 C13 C14 -62.4(8) . . . . ? C1 C13 C14 C15 177.4(7) . . . . ? C13 C14 C15 O2 178.2(8) . . . . ? O2 C16 C17 O3 69.3(13) . . . . ? O3 C18 C19 O4 -71.0(15) . . . . ? O4 C20 C21 C22 78.4(17) . . . . ? C20 C21 C22 C23 -174.4(10) . . . . ? C21 C22 C23 O5 65.1(14) . . . . ? O5 C24 C25 O6 -168.8(11) . . . . ? O6 C26 C27 O7 -61.4(12) . . . . ? O7 C28 C29 C30 -78.2(7) . . . . ? N2 C10 C30 C29 -129.9(5) . . . . ? C9 C10 C30 C29 51.1(7) . . . . ? C28 C29 C30 C10 56.2(7) . . . . ? C36 C31 C32 C33 -2.7(9) . . . . ? P1 C31 C32 C33 178.5(5) . . . . ? C31 C32 C33 C34 2.4(10) . . . . ? C32 C33 C34 C35 -0.9(10) . . . . ? C33 C34 C35 C36 -0.1(9) . . . . ? C32 C31 C36 C35 1.6(8) . . . . ? P1 C31 C36 C35 -179.6(4) . . . . ? C34 C35 C36 C31 -0.3(8) . . . . ? C42 C37 C38 C39 2.0(13) . . . . ? P1 C37 C38 C39 178.2(8) . . . . ? C37 C38 C39 C40 -1.0(15) . . . . ? C38 C39 C40 C41 -1.7(16) . . . . ? C39 C40 C41 C42 3.3(16) . . . . ? C38 C37 C42 C41 -0.3(12) . . . . ? P1 C37 C42 C41 -176.1(7) . . . . ? C40 C41 C42 C37 -2.3(15) . . . . ? C48 C43 C44 C45 0.4(8) . . . . ? P1 C43 C44 C45 179.7(4) . . . . ? C43 C44 C45 C46 0.3(9) . . . . ? C44 C45 C46 C47 -0.2(9) . . . . ? C45 C46 C47 C48 -0.7(8) . . . . ? C46 C47 C48 O1 171.6(5) . . . . ? C46 C47 C48 C43 1.5(8) . . . . ? C44 C43 C48 C47 -1.4(7) . . . . ? P1 C43 C48 C47 179.3(4) . . . . ? C44 C43 C48 O1 -171.7(4) . . . . ? P1 C43 C48 O1 9.1(6) . . . . ? O1 C49 C50 C51 -176.5(5) . . . . ? C54 C49 C50 C51 0.7(8) . . . . ? C49 C50 C51 C52 -0.1(9) . . . . ? C50 C51 C52 C53 0.2(9) . . . . ? C51 C52 C53 C54 -0.8(9) . . . . ? C52 C53 C54 C49 1.3(8) . . . . ? C52 C53 C54 P2 -173.3(4) . . . . ? C50 C49 C54 C53 -1.2(7) . . . . ? O1 C49 C54 C53 176.2(4) . . . . ? C50 C49 C54 P2 173.8(4) . . . . ? O1 C49 C54 P2 -8.8(6) . . . . ? C60 C55 C56 C57 1.8(8) . . . . ? P2 C55 C56 C57 179.2(5) . . . . ? C55 C56 C57 C58 -0.9(9) . . . . ? C56 C57 C58 C59 -0.3(10) . . . . ? C57 C58 C59 C60 0.6(10) . . . . ? C58 C59 C60 C55 0.3(9) . . . . ? C56 C55 C60 C59 -1.5(8) . . . . ? P2 C55 C60 C59 -178.8(4) . . . . ? C66 C61 C62 C63 1.2(9) . . . . ? P2 C61 C62 C63 179.7(5) . . . . ? C61 C62 C63 C64 -2.3(10) . . . . ? C62 C63 C64 C65 0.0(11) . . . . ? C63 C64 C65 C66 3.5(12) . . . . ? C64 C65 C66 C61 -4.6(12) . . . . ? C62 C61 C66 C65 2.1(10) . . . . ? P2 C61 C66 C65 -176.5(6) . . . . ? C2 C1 N1 C12 2.4(8) . . . . ? C13 C1 N1 C12 -173.5(5) . . . . ? C2 C1 N1 Cu1 -170.9(5) . . . . ? C13 C1 N1 Cu1 13.2(8) . . . . ? C4 C12 N1 C1 -0.3(8) . . . . ? C11 C12 N1 C1 179.4(5) . . . . ? C4 C12 N1 Cu1 174.0(5) . . . . ? C11 C12 N1 Cu1 -6.2(6) . . . . ? C9 C10 N2 C11 -1.8(7) . . . . ? C30 C10 N2 C11 179.2(4) . . . . ? C9 C10 N2 Cu1 167.4(4) . . . . ? C30 C10 N2 Cu1 -11.6(7) . . . . ? C7 C11 N2 C10 -1.0(7) . . . . ? C12 C11 N2 C10 179.5(4) . . . . ? C7 C11 N2 Cu1 -172.2(4) . . . . ? C12 C11 N2 Cu1 8.2(5) . . . . ? C50 C49 O1 C48 -27.5(7) . . . . ? C54 C49 O1 C48 155.1(4) . . . . ? C47 C48 O1 C49 95.6(6) . . . . ? C43 C48 O1 C49 -93.9(5) . . . . ? C14 C15 O2 C16 -178.9(8) . . . . ? C17 C16 O2 C15 74.1(14) . . . . ? C19 C18 O3 C17 179.3(11) . . . . ? C16 C17 O3 C18 159.9(9) . . . . ? C21 C20 O4 C19 168.1(12) . . . . ? C18 C19 O4 C20 -92.3(14) . . . . ? C22 C23 O5 C24 167.5(11) . . . . ? C25 C24 O5 C23 -170.0(12) . . . . ? C24 C25 O6 C26 -174.9(12) . . . . ? C27 C26 O6 C25 -74.3(15) . . . . ? C26 C27 O7 C28 86.4(11) . . . . ? C29 C28 O7 C27 143.8(7) . . . . ? C42 C37 P1 C43 -101.4(6) . . . . ? C38 C37 P1 C43 82.7(6) . . . . ? C42 C37 P1 C31 3.8(7) . . . . ? C38 C37 P1 C31 -172.1(6) . . . . ? C42 C37 P1 Cu1 135.8(6) . . . . ? C38 C37 P1 Cu1 -40.1(6) . . . . ? C48 C43 P1 C37 -171.8(4) . . . . ? C44 C43 P1 C37 9.0(5) . . . . ? C48 C43 P1 C31 79.8(4) . . . . ? C44 C43 P1 C31 -99.4(5) . . . . ? C48 C43 P1 Cu1 -49.4(4) . . . . ? C44 C43 P1 Cu1 131.4(4) . . . . ? C36 C31 P1 C37 118.0(4) . . . . ? C32 C31 P1 C37 -63.2(5) . . . . ? C36 C31 P1 C43 -134.4(4) . . . . ? C32 C31 P1 C43 44.4(5) . . . . ? C36 C31 P1 Cu1 -9.7(5) . . . . ? C32 C31 P1 Cu1 169.1(4) . . . . ? C62 C61 P2 C55 12.3(5) . . . . ? C66 C61 P2 C55 -169.2(5) . . . . ? C62 C61 P2 C54 -96.1(5) . . . . ? C66 C61 P2 C54 82.5(5) . . . . ? C62 C61 P2 Cu1 137.2(4) . . . . ? C66 C61 P2 Cu1 -44.3(5) . . . . ? C60 C55 P2 C61 -116.7(5) . . . . ? C56 C55 P2 C61 66.0(4) . . . . ? C60 C55 P2 C54 -9.1(5) . . . . ? C56 C55 P2 C54 173.5(4) . . . . ? C60 C55 P2 Cu1 114.2(4) . . . . ? C56 C55 P2 Cu1 -63.1(4) . . . . ? C53 C54 P2 C61 -0.2(5) . . . . ? C49 C54 P2 C61 -174.9(4) . . . . ? C53 C54 P2 C55 -107.3(5) . . . . ? C49 C54 P2 C55 78.0(4) . . . . ? C53 C54 P2 Cu1 130.0(4) . . . . ? C49 C54 P2 Cu1 -44.7(4) . . . . ? C1 N1 Cu1 N2 -178.5(5) . . . . ? C12 N1 Cu1 N2 8.0(3) . . . . ? C1 N1 Cu1 P1 -59.0(5) . . . . ? C12 N1 Cu1 P1 127.6(3) . . . . ? C1 N1 Cu1 P2 78.2(5) . . . . ? C12 N1 Cu1 P2 -95.3(3) . . . . ? C10 N2 Cu1 N1 -178.5(5) . . . . ? C11 N2 Cu1 N1 -8.6(3) . . . . ? C10 N2 Cu1 P1 68.4(5) . . . . ? C11 N2 Cu1 P1 -121.7(3) . . . . ? C10 N2 Cu1 P2 -60.9(5) . . . . ? C11 N2 Cu1 P2 109.0(3) . . . . ? C37 P1 Cu1 N1 -28.2(3) . . . . ? C43 P1 Cu1 N1 -145.7(2) . . . . ? C31 P1 Cu1 N1 95.8(2) . . . . ? C37 P1 Cu1 N2 64.7(2) . . . . ? C43 P1 Cu1 N2 -52.7(2) . . . . ? C31 P1 Cu1 N2 -171.2(2) . . . . ? C37 P1 Cu1 P2 -168.4(2) . . . . ? C43 P1 Cu1 P2 74.17(18) . . . . ? C31 P1 Cu1 P2 -44.36(19) . . . . ? C61 P2 Cu1 N1 -15.3(2) . . . . ? C55 P2 Cu1 N1 104.8(2) . . . . ? C54 P2 Cu1 N1 -137.1(2) . . . . ? C61 P2 Cu1 N2 -102.6(2) . . . . ? C55 P2 Cu1 N2 17.5(2) . . . . ? C54 P2 Cu1 N2 135.6(2) . . . . ? C61 P2 Cu1 P1 123.06(19) . . . . ? C55 P2 Cu1 P1 -116.83(18) . . . . ? C54 P2 Cu1 P1 1.26(18) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.826 _refine_diff_density_min -1.996 _refine_diff_density_rms 0.196 data_jfnmm120628 _database_code_depnum_ccdc_archive 'CCDC 905751' #TrackingRef 'web_deposit_cif_file_0_Nierengarten_1354039201.jfnmm120628bis.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 Cu N2 O6 P2, B F4, C2 H5 O0.5' _chemical_formula_sum 'C58 H71 B Cu F4 N2 O6.50 P2' _chemical_formula_weight 1112.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7950(7) _cell_length_b 13.2034(7) _cell_length_c 19.7058(11) _cell_angle_alpha 106.6420(10) _cell_angle_beta 106.2010(10) _cell_angle_gamma 91.4020(10) _cell_volume 2805.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9156 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.94 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7840 _exptl_absorpt_correction_T_max 0.9272 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36543 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.09 _reflns_number_total 13533 _reflns_number_gt 8630 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distance between C21 and C22 was restrained to 1.54 Ang according to the International Tables for Crystallography. DFIX 1.54 0.02 C21 C22 ; _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^)+(0.1853P)^2^+0.1020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13533 _refine_ls_number_parameters 553 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2942 _refine_ls_wR_factor_gt 0.2677 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 C1 C 0.2874(4) 0.2975(4) 0.4061(2) 0.0310(9) Uani 1 1 d . . . C2 C 0.2166(5) 0.3646(4) 0.4438(3) 0.0425(12) Uani 1 1 d . . . H2 H 0.2352 0.4396 0.4586 0.051 Uiso 1 1 calc R . . C3 C 0.1247(5) 0.3241(4) 0.4586(3) 0.0463(13) Uani 1 1 d . . . H3 H 0.0793 0.3704 0.4841 0.056 Uiso 1 1 calc R . . C4 C 0.0948(4) 0.2132(4) 0.4368(3) 0.0363(11) Uani 1 1 d . . . C5 C 0.0003(4) 0.1625(5) 0.4521(3) 0.0451(13) Uani 1 1 d . . . H5 H -0.0465 0.2050 0.4787 0.054 Uiso 1 1 calc R . . C6 C -0.0235(4) 0.0572(5) 0.4300(3) 0.0454(13) Uani 1 1 d . . . H6 H -0.0872 0.0260 0.4408 0.054 Uiso 1 1 calc R . . C7 C 0.0457(4) -0.0105(4) 0.3901(3) 0.0347(10) Uani 1 1 d . . . C8 C 0.0252(4) -0.1213(4) 0.3663(3) 0.0428(12) Uani 1 1 d . . . H8 H -0.0347 -0.1564 0.3779 0.051 Uiso 1 1 calc R . . C9 C 0.0928(4) -0.1795(4) 0.3258(3) 0.0415(11) Uani 1 1 d . . . H9 H 0.0780 -0.2549 0.3085 0.050 Uiso 1 1 calc R . . C10 C 0.1827(4) -0.1284(4) 0.3099(3) 0.0322(10) Uani 1 1 d . . . C11 C 0.1383(4) 0.0364(4) 0.3733(2) 0.0271(9) Uani 1 1 d . . . C12 C 0.1651(4) 0.1505(4) 0.3978(2) 0.0271(9) Uani 1 1 d . . . C13 C 0.3940(4) 0.3395(4) 0.3911(3) 0.0347(10) Uani 1 1 d . . . H13A H 0.3990 0.2926 0.3430 0.042 Uiso 1 1 calc R . . H13B H 0.4658 0.3344 0.4300 0.042 Uiso 1 1 calc R . . C14 C 0.3970(5) 0.4526(4) 0.3883(3) 0.0423(12) Uani 1 1 d . . . H14A H 0.3960 0.5007 0.4369 0.051 Uiso 1 1 calc R . . H14B H 0.3246 0.4591 0.3504 0.051 Uiso 1 1 calc R . . C15 C 0.5050(5) 0.4877(4) 0.3702(3) 0.0474(13) Uani 1 1 d . . . H15A H 0.5038 0.5627 0.3703 0.057 Uiso 1 1 calc R . . H15B H 0.5782 0.4827 0.4082 0.057 Uiso 1 1 calc R . . C16 C 0.5968(6) 0.4615(5) 0.2765(4) 0.0554(15) Uani 1 1 d . . . H16A H 0.6752 0.4656 0.3130 0.066 Uiso 1 1 calc R . . H16B H 0.5842 0.5338 0.2727 0.066 Uiso 1 1 calc R . . C17 C 0.5939(6) 0.3874(6) 0.2023(4) 0.071(2) Uani 1 1 d . . . H17A H 0.5102 0.3637 0.1718 0.086 Uiso 1 1 calc R . . H17B H 0.6317 0.4260 0.1766 0.086 Uiso 1 1 calc R . . C18 C 0.7680(10) 0.3035(9) 0.1980(6) 0.1205(11) Uani 1 1 d . . . H18A H 0.8062 0.3779 0.2200 0.145 Uiso 1 1 calc R . . H18B H 0.7596 0.2815 0.1442 0.145 Uiso 1 1 calc R . . C19 C 0.8442(10) 0.2331(9) 0.2334(7) 0.1205(11) Uani 1 1 d . . . H19A H 0.9259 0.2451 0.2309 0.145 Uiso 1 1 calc R . . H19B H 0.8477 0.2523 0.2864 0.145 Uiso 1 1 calc R . . C20 C 0.8874(10) 0.0591(9) 0.2174(7) 0.1205(11) Uani 1 1 d . . . H20A H 0.9084 0.0696 0.2714 0.145 Uiso 1 1 calc R . . H20B H 0.9600 0.0806 0.2068 0.145 Uiso 1 1 calc R . . C21 C 0.8521(10) -0.0524(9) 0.1788(6) 0.1205(11) Uani 1 1 d D . . H21A H 0.7868 -0.0772 0.1947 0.145 Uiso 1 1 calc R . . H21B H 0.9200 -0.0927 0.1925 0.145 Uiso 1 1 calc R . . C22 C 0.8126(10) -0.0746(10) 0.0983(6) 0.1205(11) Uani 1 1 d D . . H22A H 0.8688 -0.0332 0.0845 0.145 Uiso 1 1 calc R . . H22B H 0.8170 -0.1510 0.0750 0.145 Uiso 1 1 calc R . . C23 C 0.6929(10) -0.0505(10) 0.0673(7) 0.1205(11) Uani 1 1 d . . . H23A H 0.6623 -0.0071 0.1069 0.145 Uiso 1 1 calc R . . H23B H 0.6916 -0.0114 0.0311 0.145 Uiso 1 1 calc R . . C24 C 0.5059(10) -0.1548(9) 0.0062(7) 0.1205(11) Uani 1 1 d . . . H24A H 0.4819 -0.1404 -0.0421 0.145 Uiso 1 1 calc R . . H24B H 0.4755 -0.1024 0.0421 0.145 Uiso 1 1 calc R . . C25 C 0.4595(11) -0.2738(9) -0.0022(6) 0.1205(11) Uani 1 1 d . . . H25A H 0.3767 -0.2926 -0.0352 0.145 Uiso 1 1 calc R . . H25B H 0.5097 -0.3243 -0.0242 0.145 Uiso 1 1 calc R . . C26 C 0.4229(11) -0.3827(9) 0.0608(6) 0.1205(11) Uani 1 1 d . . . H26A H 0.4673 -0.4341 0.0339 0.145 Uiso 1 1 calc R . . H26B H 0.3376 -0.3977 0.0320 0.145 Uiso 1 1 calc R . . C27 C 0.4398(10) -0.3922(10) 0.1357(6) 0.1205(11) Uani 1 1 d . . . H27A H 0.5175 -0.3538 0.1692 0.145 Uiso 1 1 calc R . . H27B H 0.4400 -0.4680 0.1335 0.145 Uiso 1 1 calc R . . C28 C 0.3594(7) -0.3501(6) 0.2334(5) 0.076(2) Uani 1 1 d . . . H28A H 0.4386 -0.3126 0.2649 0.091 Uiso 1 1 calc R . . H28B H 0.3583 -0.4252 0.2333 0.091 Uiso 1 1 calc R . . C29 C 0.2685(6) -0.3011(4) 0.2647(4) 0.0534(14) Uani 1 1 d . . . H29A H 0.2871 -0.3030 0.3165 0.064 Uiso 1 1 calc R . . H29B H 0.1912 -0.3446 0.2364 0.064 Uiso 1 1 calc R . . C30 C 0.2557(5) -0.1887(4) 0.2646(4) 0.0478(13) Uani 1 1 d . . . H30A H 0.3362 -0.1493 0.2826 0.057 Uiso 1 1 calc R . . H30B H 0.2203 -0.1893 0.2126 0.057 Uiso 1 1 calc R . . C31 C 0.2387(4) 0.2095(4) 0.1758(3) 0.0360(10) Uani 1 1 d . . . C32 C 0.2636(5) 0.2414(5) 0.1181(3) 0.0540(15) Uani 1 1 d . . . H32 H 0.3077 0.2008 0.0884 0.065 Uiso 1 1 calc R . . C33 C 0.2209(6) 0.3346(6) 0.1064(5) 0.073(2) Uani 1 1 d . . . H33 H 0.2382 0.3577 0.0686 0.088 Uiso 1 1 calc R . . C34 C 0.1565(7) 0.3929(6) 0.1461(5) 0.082(2) Uani 1 1 d . . . H34 H 0.1285 0.4556 0.1360 0.098 Uiso 1 1 calc R . . C35 C 0.1315(6) 0.3612(5) 0.2015(4) 0.0665(19) Uani 1 1 d . . . H35 H 0.0861 0.4018 0.2302 0.080 Uiso 1 1 calc R . . C36 C 0.1731(5) 0.2692(4) 0.2153(3) 0.0483(13) Uani 1 1 d . . . H36 H 0.1551 0.2476 0.2535 0.058 Uiso 1 1 calc R . . C37 C 0.2218(5) -0.0167(5) 0.1151(3) 0.0548(7) Uani 1 1 d . . . C40 C 0.0962(5) -0.1836(5) -0.0063(3) 0.0548(7) Uani 1 1 d . . . H40 H 0.0574 -0.2396 -0.0503 0.066 Uiso 1 1 calc R A 1 C38 C 0.1046(10) -0.0023(9) 0.0677(6) 0.0548(7) Uani 0.55 1 d P B 1 H38 H 0.0726 0.0638 0.0785 0.066 Uiso 0.55 1 calc PR B 1 C39 C 0.0446(10) -0.0861(8) 0.0085(6) 0.0548(7) Uani 0.55 1 d P B 1 H39 H -0.0308 -0.0798 -0.0226 0.066 Uiso 0.55 1 calc PR B 1 C41 C 0.1925(10) -0.1988(9) 0.0374(6) 0.0548(7) Uani 0.55 1 d P B 1 H41 H 0.2207 -0.2667 0.0278 0.066 Uiso 0.55 1 calc PR B 1 C42 C 0.2558(10) -0.1154(9) 0.0989(6) 0.0548(7) Uani 0.55 1 d P B 1 H42 H 0.3264 -0.1285 0.1311 0.066 Uiso 0.55 1 calc PR B 1 C38B C 0.2563(12) -0.0306(10) 0.0508(7) 0.0548(7) Uani 0.45 1 d P B 2 H38B H 0.3181 0.0159 0.0497 0.066 Uiso 0.45 1 calc PR B 2 C39B C 0.1957(12) -0.1166(10) -0.0128(7) 0.0548(7) Uani 0.45 1 d P B 2 H39B H 0.2169 -0.1314 -0.0574 0.066 Uiso 0.45 1 calc PR B 2 C41B C 0.0799(12) -0.1679(11) 0.0530(7) 0.0548(7) Uani 0.45 1 d P B 2 H41B H 0.0242 -0.2166 0.0577 0.066 Uiso 0.45 1 calc PR B 2 C42B C 0.1373(12) -0.0824(10) 0.1159(7) 0.0548(7) Uani 0.45 1 d P B 2 H42B H 0.1146 -0.0718 0.1598 0.066 Uiso 0.45 1 calc PR B 2 C43 C 0.4511(4) 0.1072(4) 0.1966(3) 0.0347(10) Uani 1 1 d . . . H43A H 0.4517 0.0880 0.1443 0.042 Uiso 1 1 calc R B . H43B H 0.4843 0.1828 0.2208 0.042 Uiso 1 1 calc R . . C44 C 0.5318(4) 0.0377(4) 0.2359(2) 0.0318(10) Uani 1 1 d . B . H44A H 0.6157 0.0580 0.2406 0.038 Uiso 1 1 calc R . . H44B H 0.5104 -0.0380 0.2056 0.038 Uiso 1 1 calc R . . C45 C 0.6264(4) 0.1658(4) 0.3914(2) 0.0284(9) Uani 1 1 d . B . C46 C 0.6549(5) 0.1826(4) 0.4670(3) 0.0425(12) Uani 1 1 d . . . H46 H 0.6204 0.1344 0.4854 0.051 Uiso 1 1 calc R . . C47 C 0.7343(5) 0.2700(5) 0.5166(3) 0.0505(14) Uani 1 1 d . . . H47 H 0.7537 0.2803 0.5684 0.061 Uiso 1 1 calc R . . C48 C 0.7841(5) 0.3406(4) 0.4915(3) 0.0514(15) Uani 1 1 d . . . H48 H 0.8374 0.4003 0.5253 0.062 Uiso 1 1 calc R . . C49 C 0.7555(5) 0.3237(4) 0.4157(4) 0.0514(14) Uani 1 1 d . . . H49 H 0.7900 0.3718 0.3973 0.062 Uiso 1 1 calc R . . C50 C 0.6772(4) 0.2373(4) 0.3667(3) 0.0391(11) Uani 1 1 d . . . H50 H 0.6581 0.2272 0.3149 0.047 Uiso 1 1 calc R . . C51 C 0.5782(4) -0.0593(4) 0.3541(3) 0.0366(11) Uani 1 1 d . B . C52 C 0.6576(4) -0.1156(4) 0.3224(4) 0.0512(15) Uani 1 1 d . . . H52 H 0.6810 -0.0956 0.2852 0.061 Uiso 1 1 calc R . . C53 C 0.7031(5) -0.2004(5) 0.3442(5) 0.067(2) Uani 1 1 d . . . H53 H 0.7571 -0.2384 0.3216 0.081 Uiso 1 1 calc R . . C54 C 0.6712(6) -0.2307(5) 0.3980(5) 0.072(2) Uani 1 1 d . . . H54 H 0.7044 -0.2882 0.4134 0.086 Uiso 1 1 calc R . . C55 C 0.5907(7) -0.1769(5) 0.4296(4) 0.070(2) Uani 1 1 d . . . H55 H 0.5675 -0.1981 0.4664 0.084 Uiso 1 1 calc R . . C56 C 0.5432(6) -0.0912(5) 0.4075(3) 0.0508(14) Uani 1 1 d . . . H56 H 0.4872 -0.0548 0.4290 0.061 Uiso 1 1 calc R . . N1 N 0.2579(3) 0.1918(3) 0.38251(18) 0.0247(7) Uani 1 1 d . . . N2 N 0.2052(3) -0.0214(3) 0.33305(19) 0.0270(7) Uani 1 1 d . . . O1 O 0.5049(3) 0.4226(3) 0.3002(2) 0.0465(9) Uani 1 1 d . . . O2 O 0.6532(6) 0.2975(5) 0.2086(4) 0.1009(9) Uani 1 1 d . . . O3 O 0.8024(6) 0.1266(5) 0.1996(4) 0.1009(9) Uani 1 1 d . . . O4 O 0.6235(6) -0.1525(5) 0.0314(4) 0.1009(9) Uani 1 1 d . . . O5 O 0.4649(6) -0.2802(5) 0.0695(4) 0.1009(9) Uani 1 1 d . . . O6 O 0.3422(6) -0.3465(5) 0.1655(4) 0.1009(9) Uani 1 1 d . . . B1 B 0.0547(6) 0.4309(6) 0.6610(4) 0.0514(16) Uani 1 1 d . . . F1 F 0.0682(4) 0.5087(3) 0.6303(3) 0.0995(16) Uani 1 1 d . . . F2 F -0.0533(4) 0.4340(3) 0.6769(3) 0.0896(14) Uani 1 1 d . . . F3 F 0.0468(4) 0.3335(3) 0.6097(2) 0.0758(11) Uani 1 1 d . . . F4 F 0.1488(5) 0.4347(5) 0.7211(3) 0.128(2) Uani 1 1 d . . . P1 P 0.29709(9) 0.09229(9) 0.19847(6) 0.0268(3) Uani 1 1 d . B . P2 P 0.51574(9) 0.05441(9) 0.32911(6) 0.0267(3) Uani 1 1 d . . . Cu1 Cu 0.32257(4) 0.07552(4) 0.31301(3) 0.02620(18) Uani 1 1 d . B . 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 C1 0.036(2) 0.029(2) 0.025(2) 0.0036(18) 0.0085(18) 0.0109(18) C2 0.058(3) 0.029(2) 0.045(3) 0.007(2) 0.025(2) 0.018(2) C3 0.043(3) 0.050(3) 0.049(3) 0.007(3) 0.025(2) 0.023(2) C4 0.036(2) 0.047(3) 0.031(2) 0.014(2) 0.0154(19) 0.019(2) C5 0.040(3) 0.060(4) 0.045(3) 0.018(3) 0.024(2) 0.020(2) C6 0.029(2) 0.074(4) 0.051(3) 0.032(3) 0.025(2) 0.014(2) C7 0.026(2) 0.052(3) 0.032(2) 0.018(2) 0.0128(18) 0.007(2) C8 0.030(2) 0.054(3) 0.058(3) 0.032(3) 0.018(2) 0.001(2) C9 0.040(3) 0.039(3) 0.053(3) 0.022(2) 0.018(2) -0.001(2) C10 0.031(2) 0.031(2) 0.037(2) 0.0113(19) 0.0133(19) 0.0014(18) C11 0.0251(19) 0.038(2) 0.023(2) 0.0148(18) 0.0079(16) 0.0052(17) C12 0.027(2) 0.036(2) 0.021(2) 0.0112(18) 0.0077(16) 0.0114(17) C13 0.036(2) 0.025(2) 0.043(3) 0.007(2) 0.014(2) 0.0064(18) C14 0.044(3) 0.030(2) 0.051(3) 0.013(2) 0.011(2) 0.004(2) C15 0.048(3) 0.030(3) 0.060(4) 0.014(2) 0.012(3) -0.003(2) C16 0.058(3) 0.048(3) 0.068(4) 0.026(3) 0.023(3) -0.008(3) C17 0.068(4) 0.091(5) 0.083(5) 0.052(4) 0.037(4) 0.016(4) C18 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C19 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C20 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C21 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C22 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C23 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C24 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C25 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C26 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C27 0.123(3) 0.123(3) 0.120(3) 0.032(2) 0.046(2) 0.036(2) C28 0.086(5) 0.051(4) 0.120(7) 0.037(4) 0.063(5) 0.016(3) C29 0.061(3) 0.037(3) 0.069(4) 0.016(3) 0.030(3) 0.012(3) C30 0.054(3) 0.031(3) 0.074(4) 0.019(3) 0.039(3) 0.006(2) C31 0.033(2) 0.033(2) 0.036(2) 0.011(2) -0.0003(19) -0.0033(19) C32 0.049(3) 0.061(4) 0.059(4) 0.038(3) 0.009(3) 0.001(3) C33 0.065(4) 0.067(5) 0.090(5) 0.051(4) 0.000(4) -0.001(4) C34 0.078(5) 0.044(4) 0.099(6) 0.024(4) -0.012(4) 0.009(3) C35 0.063(4) 0.051(4) 0.067(4) 0.008(3) -0.001(3) 0.020(3) C36 0.042(3) 0.045(3) 0.045(3) 0.008(2) -0.002(2) 0.013(2) C37 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C40 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C38 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C39 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C41 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C42 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C38B 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C39B 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C41B 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C42B 0.0565(17) 0.0477(16) 0.0454(16) 0.0030(14) 0.0045(13) -0.0054(13) C43 0.033(2) 0.046(3) 0.033(2) 0.018(2) 0.0171(19) -0.001(2) C44 0.029(2) 0.038(2) 0.032(2) 0.009(2) 0.0174(18) 0.0039(18) C45 0.0252(19) 0.032(2) 0.032(2) 0.0116(19) 0.0105(17) 0.0130(17) C46 0.051(3) 0.044(3) 0.034(3) 0.009(2) 0.017(2) 0.009(2) C47 0.056(3) 0.053(3) 0.031(3) 0.001(2) 0.008(2) 0.019(3) C48 0.037(3) 0.030(3) 0.066(4) -0.001(3) -0.001(3) 0.011(2) C49 0.040(3) 0.036(3) 0.069(4) 0.017(3) 0.002(3) 0.003(2) C50 0.035(2) 0.036(3) 0.042(3) 0.012(2) 0.005(2) 0.000(2) C51 0.028(2) 0.028(2) 0.052(3) 0.017(2) 0.004(2) 0.0031(18) C52 0.034(3) 0.036(3) 0.095(5) 0.027(3) 0.030(3) 0.011(2) C53 0.032(3) 0.044(3) 0.123(6) 0.032(4) 0.013(3) 0.013(2) C54 0.052(4) 0.043(3) 0.102(6) 0.039(4) -0.024(4) 0.000(3) C55 0.099(5) 0.049(4) 0.058(4) 0.035(3) -0.002(4) 0.000(4) C56 0.070(4) 0.048(3) 0.038(3) 0.025(3) 0.008(3) 0.011(3) N1 0.0260(16) 0.0281(18) 0.0214(17) 0.0064(14) 0.0102(13) 0.0076(14) N2 0.0265(17) 0.0312(19) 0.0261(18) 0.0113(15) 0.0094(14) 0.0024(14) O1 0.048(2) 0.040(2) 0.049(2) 0.0117(17) 0.0146(17) -0.0082(16) O2 0.114(2) 0.0873(19) 0.117(2) 0.0317(17) 0.0577(18) 0.0171(16) O3 0.114(2) 0.0873(19) 0.117(2) 0.0317(17) 0.0577(18) 0.0171(16) O4 0.114(2) 0.0873(19) 0.117(2) 0.0317(17) 0.0577(18) 0.0171(16) O5 0.114(2) 0.0873(19) 0.117(2) 0.0317(17) 0.0577(18) 0.0171(16) O6 0.114(2) 0.0873(19) 0.117(2) 0.0317(17) 0.0577(18) 0.0171(16) B1 0.048(3) 0.049(4) 0.053(4) 0.017(3) 0.009(3) -0.016(3) F1 0.106(3) 0.071(3) 0.145(4) 0.067(3) 0.039(3) -0.005(2) F2 0.097(3) 0.067(3) 0.120(4) 0.011(3) 0.075(3) 0.008(2) F3 0.091(3) 0.059(2) 0.090(3) 0.023(2) 0.047(2) 0.016(2) F4 0.124(4) 0.134(5) 0.096(4) 0.052(4) -0.025(3) -0.047(4) P1 0.0255(5) 0.0297(6) 0.0251(6) 0.0086(4) 0.0077(4) 0.0000(4) P2 0.0263(5) 0.0302(6) 0.0298(6) 0.0141(5) 0.0126(4) 0.0063(4) Cu1 0.0278(3) 0.0262(3) 0.0292(3) 0.0085(2) 0.0156(2) 0.0039(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.341(6) . ? C1 C2 1.429(6) . ? C1 C13 1.497(6) . ? C2 C3 1.335(8) . ? C2 H2 0.9500 . ? C3 C4 1.408(8) . ? C3 H3 0.9500 . ? C4 C12 1.410(6) . ? C4 C5 1.432(7) . ? C5 C6 1.329(8) . ? C5 H5 0.9500 . ? C6 C7 1.440(7) . ? C6 H6 0.9500 . ? C7 C8 1.396(7) . ? C7 C11 1.404(6) . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.396(6) . ? C9 H9 0.9500 . ? C10 N2 1.349(6) . ? C10 C30 1.492(7) . ? C11 N2 1.365(5) . ? C11 C12 1.442(6) . ? C12 N1 1.355(5) . ? C13 C14 1.509(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O1 1.400(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O1 1.432(6) . ? C16 C17 1.499(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O2 1.410(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O2 1.431(12) . ? C18 C19 1.490(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O3 1.381(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O3 1.396(11) . ? C20 C21 1.440(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.461(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.457(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O4 1.435(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O4 1.333(12) . ? C24 C25 1.598(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O5 1.423(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O5 1.377(12) . ? C26 C27 1.474(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O6 1.499(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O6 1.311(10) . ? C28 C29 1.456(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.497(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.356(7) . ? C31 C32 1.419(7) . ? C31 P1 1.830(5) . ? C32 C33 1.396(9) . ? C32 H32 0.9500 . ? C33 C34 1.340(12) . ? C33 H33 0.9500 . ? C34 C35 1.375(11) . ? C34 H34 0.9500 . ? C35 C36 1.390(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42B 1.312(15) . ? C37 C42 1.348(13) . ? C37 C38B 1.401(15) . ? C37 C38 1.488(12) . ? C37 P1 1.825(6) . ? C40 C41B 1.196(15) . ? C40 C41 1.279(12) . ? C40 C39 1.428(13) . ? C40 C39B 1.509(15) . ? C40 H40 0.9500 . ? C38 C39 1.359(14) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C41 C42 1.389(14) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C38B C39B 1.419(17) . ? C38B H38B 0.9500 . ? C39B H39B 0.9500 . ? C41B C42B 1.400(17) . ? C41B H41B 0.9500 . ? C42B H42B 0.9500 . ? C43 C44 1.545(7) . ? C43 P1 1.835(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 P2 1.850(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.374(7) . ? C45 C46 1.382(7) . ? C45 P2 1.831(5) . ? C46 C47 1.397(8) . ? C46 H46 0.9500 . ? C47 C48 1.364(9) . ? C47 H47 0.9500 . ? C48 C49 1.385(9) . ? C48 H48 0.9500 . ? C49 C50 1.380(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.383(7) . ? C51 C56 1.394(7) . ? C51 P2 1.820(5) . ? C52 C53 1.379(8) . ? C52 H52 0.9500 . ? C53 C54 1.373(11) . ? C53 H53 0.9500 . ? C54 C55 1.379(11) . ? C54 H54 0.9500 . ? C55 C56 1.401(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N1 Cu1 2.062(3) . ? N2 Cu1 2.054(3) . ? B1 F1 1.360(8) . ? B1 F4 1.366(9) . ? B1 F3 1.371(8) . ? B1 F2 1.393(8) . ? P1 Cu1 2.2683(12) . ? P2 Cu1 2.2468(11) . ? 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 C1 C2 119.1(4) . . ? N1 C1 C13 117.8(4) . . ? C2 C1 C13 123.1(4) . . ? C3 C2 C1 121.4(5) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 116.1(4) . . ? C3 C4 C5 124.4(4) . . ? C12 C4 C5 119.6(5) . . ? C6 C5 C4 121.5(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C11 117.5(4) . . ? C8 C7 C6 123.5(4) . . ? C11 C7 C6 119.0(5) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.5(5) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N2 C10 C9 121.2(4) . . ? N2 C10 C30 116.8(4) . . ? C9 C10 C30 122.0(4) . . ? N2 C11 C7 122.9(4) . . ? N2 C11 C12 117.1(4) . . ? C7 C11 C12 120.0(4) . . ? N1 C12 C4 123.4(4) . . ? N1 C12 C11 117.8(4) . . ? C4 C12 C11 118.8(4) . . ? C1 C13 C14 116.3(4) . . ? C1 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? C1 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 113.1(4) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O1 C15 C14 109.4(4) . . ? O1 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? O1 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? O1 C16 C17 108.8(5) . . ? O1 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? O1 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O2 C17 C16 112.2(6) . . ? O2 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? O2 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? O2 C18 C19 110.4(10) . . ? O2 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? O2 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? O3 C19 C18 112.5(10) . . ? O3 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? O3 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? O3 C20 C21 115.4(10) . . ? O3 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? O3 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 112.2(11) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 115.5(10) . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22B 108.4 . . ? C21 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? O4 C23 C22 104.6(9) . . ? O4 C23 H23A 110.8 . . ? C22 C23 H23A 110.8 . . ? O4 C23 H23B 110.8 . . ? C22 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? O4 C24 C25 102.8(9) . . ? O4 C24 H24A 111.2 . . ? C25 C24 H24A 111.2 . . ? O4 C24 H24B 111.2 . . ? C25 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? O5 C25 C24 108.3(9) . . ? O5 C25 H25A 110.0 . . ? C24 C25 H25A 110.0 . . ? O5 C25 H25B 110.0 . . ? C24 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O5 C26 C27 107.2(10) . . ? O5 C26 H26A 110.3 . . ? C27 C26 H26A 110.3 . . ? O5 C26 H26B 110.3 . . ? C27 C26 H26B 110.3 . . ? H26A C26 H26B 108.5 . . ? C26 C27 O6 110.2(9) . . ? C26 C27 H27A 109.6 . . ? O6 C27 H27A 109.6 . . ? C26 C27 H27B 109.6 . . ? O6 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O6 C28 C29 111.4(7) . . ? O6 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? O6 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 115.1(5) . . ? C28 C29 H29A 108.5 . . ? C30 C29 H29A 108.5 . . ? C28 C29 H29B 108.5 . . ? C30 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C10 C30 C29 116.7(4) . . ? C10 C30 H30A 108.1 . . ? C29 C30 H30A 108.1 . . ? C10 C30 H30B 108.1 . . ? C29 C30 H30B 108.1 . . ? H30A C30 H30B 107.3 . . ? C36 C31 C32 118.7(5) . . ? C36 C31 P1 120.4(4) . . ? C32 C31 P1 120.8(4) . . ? C33 C32 C31 117.5(6) . . ? C33 C32 H32 121.2 . . ? C31 C32 H32 121.2 . . ? C34 C33 C32 123.0(7) . . ? C34 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 C34 C35 119.3(7) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 119.5(7) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 121.9(6) . . ? C31 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C42B C37 C42 72.3(8) . . ? C42B C37 C38B 120.4(9) . . ? C42 C37 C38B 74.4(8) . . ? C42B C37 C38 69.4(8) . . ? C42 C37 C38 116.7(7) . . ? C38B C37 C38 84.1(8) . . ? C42B C37 P1 120.1(7) . . ? C42 C37 P1 124.4(6) . . ? C38B C37 P1 119.5(7) . . ? C38 C37 P1 118.2(6) . . ? C41B C40 C41 73.7(9) . . ? C41B C40 C39 73.0(9) . . ? C41 C40 C39 122.6(8) . . ? C41B C40 C39B 118.8(9) . . ? C41 C40 C39B 73.0(8) . . ? C39 C40 C39B 84.1(8) . . ? C41B C40 H40 126.7 . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C39B C40 H40 114.2 . . ? C39 C38 C37 118.2(10) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C38 C39 C40 119.2(10) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C40 C41 C42 119.6(11) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C37 C42 C41 123.2(10) . . ? C37 C42 H42 118.4 . . ? C41 C42 H42 118.4 . . ? C37 C38B C39B 117.7(12) . . ? C37 C38B H38B 121.2 . . ? C39B C38B H38B 121.2 . . ? C38B C39B C40 117.1(12) . . ? C38B C39B H39B 121.4 . . ? C40 C39B H39B 121.4 . . ? C40 C41B C42B 124.5(13) . . ? C40 C41B H41B 117.8 . . ? C42B C41B H41B 117.8 . . ? C37 C42B C41B 121.1(13) . . ? C37 C42B H42B 119.5 . . ? C41B C42B H42B 119.5 . . ? C44 C43 P1 113.3(3) . . ? C44 C43 H43A 108.9 . . ? P1 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? P1 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 P2 110.9(3) . . ? C43 C44 H44A 109.5 . . ? P2 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? P2 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C50 C45 C46 118.3(4) . . ? C50 C45 P2 122.9(3) . . ? C46 C45 P2 118.6(4) . . ? C45 C46 C47 120.4(5) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 120.8(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 118.8(5) . . ? C47 C48 H48 120.6 . . ? C49 C48 H48 120.6 . . ? C50 C49 C48 120.4(6) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C45 C50 C49 121.3(5) . . ? C45 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C52 C51 C56 118.7(5) . . ? C52 C51 P2 123.3(4) . . ? C56 C51 P2 118.0(4) . . ? C53 C52 C51 120.8(6) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C54 C53 C52 120.9(6) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 119.5(5) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.1(7) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C51 C56 C55 120.1(6) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C1 N1 C12 119.5(3) . . ? C1 N1 Cu1 129.0(3) . . ? C12 N1 Cu1 111.1(3) . . ? C10 N2 C11 118.4(4) . . ? C10 N2 Cu1 130.1(3) . . ? C11 N2 Cu1 111.5(3) . . ? C15 O1 C16 111.3(4) . . ? C17 O2 C18 112.9(7) . . ? C19 O3 C20 113.1(8) . . ? C24 O4 C23 117.9(8) . . ? C26 O5 C25 107.3(8) . . ? C28 O6 C27 110.7(7) . . ? F1 B1 F4 112.9(5) . . ? F1 B1 F3 109.2(6) . . ? F4 B1 F3 106.6(6) . . ? F1 B1 F2 109.5(6) . . ? F4 B1 F2 112.7(6) . . ? F3 B1 F2 105.6(5) . . ? C37 P1 C31 103.1(3) . . ? C37 P1 C43 105.0(3) . . ? C31 P1 C43 102.6(2) . . ? C37 P1 Cu1 120.9(2) . . ? C31 P1 Cu1 120.90(17) . . ? C43 P1 Cu1 101.70(15) . . ? C51 P2 C45 102.7(2) . . ? C51 P2 C44 104.3(2) . . ? C45 P2 C44 105.0(2) . . ? C51 P2 Cu1 121.54(15) . . ? C45 P2 Cu1 118.27(13) . . ? C44 P2 Cu1 103.20(15) . . ? N2 Cu1 N1 81.85(14) . . ? N2 Cu1 P2 124.17(10) . . ? N1 Cu1 P2 124.97(10) . . ? N2 Cu1 P1 121.75(10) . . ? N1 Cu1 P1 114.86(10) . . ? P2 Cu1 P1 92.42(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.7(7) . . . . ? C13 C1 C2 C3 -177.5(5) . . . . ? C1 C2 C3 C4 -0.4(8) . . . . ? C2 C3 C4 C12 -1.4(8) . . . . ? C2 C3 C4 C5 178.0(5) . . . . ? C3 C4 C5 C6 -179.9(5) . . . . ? C12 C4 C5 C6 -0.5(8) . . . . ? C4 C5 C6 C7 0.5(8) . . . . ? C5 C6 C7 C8 179.4(5) . . . . ? C5 C6 C7 C11 -1.2(7) . . . . ? C11 C7 C8 C9 -2.1(7) . . . . ? C6 C7 C8 C9 177.3(5) . . . . ? C7 C8 C9 C10 1.4(8) . . . . ? C8 C9 C10 N2 -0.6(8) . . . . ? C8 C9 C10 C30 -178.5(5) . . . . ? C8 C7 C11 N2 2.2(7) . . . . ? C6 C7 C11 N2 -177.3(4) . . . . ? C8 C7 C11 C12 -178.7(4) . . . . ? C6 C7 C11 C12 1.7(6) . . . . ? C3 C4 C12 N1 1.2(7) . . . . ? C5 C4 C12 N1 -178.3(4) . . . . ? C3 C4 C12 C11 -179.5(4) . . . . ? C5 C4 C12 C11 1.0(6) . . . . ? N2 C11 C12 N1 -3.2(6) . . . . ? C7 C11 C12 N1 177.7(4) . . . . ? N2 C11 C12 C4 177.4(4) . . . . ? C7 C11 C12 C4 -1.7(6) . . . . ? N1 C1 C13 C14 155.6(4) . . . . ? C2 C1 C13 C14 -24.2(7) . . . . ? C1 C13 C14 C15 -177.9(4) . . . . ? C13 C14 C15 O1 60.9(6) . . . . ? O1 C16 C17 O2 -81.7(7) . . . . ? O2 C18 C19 O3 65.8(12) . . . . ? O3 C20 C21 C22 54.8(14) . . . . ? C20 C21 C22 C23 -78.0(14) . . . . ? C21 C22 C23 O4 -106.6(12) . . . . ? O4 C24 C25 O5 78.0(10) . . . . ? O5 C26 C27 O6 80.5(11) . . . . ? O6 C28 C29 C30 -55.9(9) . . . . ? N2 C10 C30 C29 155.9(5) . . . . ? C9 C10 C30 C29 -26.1(8) . . . . ? C28 C29 C30 C10 -167.6(6) . . . . ? C36 C31 C32 C33 1.4(8) . . . . ? P1 C31 C32 C33 -176.9(4) . . . . ? C31 C32 C33 C34 -1.2(10) . . . . ? C32 C33 C34 C35 0.6(11) . . . . ? C33 C34 C35 C36 -0.1(11) . . . . ? C32 C31 C36 C35 -1.0(8) . . . . ? P1 C31 C36 C35 177.3(4) . . . . ? C34 C35 C36 C31 0.4(9) . . . . ? C42B C37 C38 C39 -61.4(12) . . . . ? C42 C37 C38 C39 -5.0(14) . . . . ? C38B C37 C38 C39 64.2(11) . . . . ? P1 C37 C38 C39 -175.4(8) . . . . ? C37 C38 C39 C40 -0.6(15) . . . . ? C41B C40 C39 C38 63.0(12) . . . . ? C41 C40 C39 C38 5.9(15) . . . . ? C39B C40 C39 C38 -59.6(11) . . . . ? C41B C40 C41 C42 -61.9(12) . . . . ? C39 C40 C41 C42 -5.2(16) . . . . ? C39B C40 C41 C42 66.0(11) . . . . ? C42B C37 C42 C41 61.0(12) . . . . ? C38B C37 C42 C41 -68.9(12) . . . . ? C38 C37 C42 C41 6.0(15) . . . . ? P1 C37 C42 C41 175.8(8) . . . . ? C40 C41 C42 C37 -1.1(17) . . . . ? C42B C37 C38B C39B 0.7(17) . . . . ? C42 C37 C38B C39B 58.7(12) . . . . ? C38 C37 C38B C39B -61.1(12) . . . . ? P1 C37 C38B C39B 179.8(9) . . . . ? C37 C38B C39B C40 2.1(17) . . . . ? C41B C40 C39B C38B -6.6(17) . . . . ? C41 C40 C39B C38B -66.5(12) . . . . ? C39 C40 C39B C38B 60.2(12) . . . . ? C41 C40 C41B C42B 67.8(14) . . . . ? C39 C40 C41B C42B -64.8(14) . . . . ? C39B C40 C41B C42B 8.3(19) . . . . ? C42 C37 C42B C41B -58.7(13) . . . . ? C38B C37 C42B C41B 0.3(18) . . . . ? C38 C37 C42B C41B 69.8(13) . . . . ? P1 C37 C42B C41B -178.8(10) . . . . ? C40 C41B C42B C37 -5(2) . . . . ? P1 C43 C44 P2 -49.6(4) . . . . ? C50 C45 C46 C47 -0.5(7) . . . . ? P2 C45 C46 C47 -176.7(4) . . . . ? C45 C46 C47 C48 0.6(8) . . . . ? C46 C47 C48 C49 -0.6(8) . . . . ? C47 C48 C49 C50 0.5(8) . . . . ? C46 C45 C50 C49 0.4(7) . . . . ? P2 C45 C50 C49 176.4(4) . . . . ? C48 C49 C50 C45 -0.4(8) . . . . ? C56 C51 C52 C53 -1.2(8) . . . . ? P2 C51 C52 C53 179.3(5) . . . . ? C51 C52 C53 C54 -0.4(10) . . . . ? C52 C53 C54 C55 1.4(10) . . . . ? C53 C54 C55 C56 -0.9(10) . . . . ? C52 C51 C56 C55 1.7(8) . . . . ? P2 C51 C56 C55 -178.7(5) . . . . ? C54 C55 C56 C51 -0.7(10) . . . . ? C2 C1 N1 C12 -2.9(6) . . . . ? C13 C1 N1 C12 177.3(4) . . . . ? C2 C1 N1 Cu1 169.2(3) . . . . ? C13 C1 N1 Cu1 -10.6(6) . . . . ? C4 C12 N1 C1 1.0(6) . . . . ? C11 C12 N1 C1 -178.3(4) . . . . ? C4 C12 N1 Cu1 -172.4(3) . . . . ? C11 C12 N1 Cu1 8.2(4) . . . . ? C9 C10 N2 C11 0.6(7) . . . . ? C30 C10 N2 C11 178.6(4) . . . . ? C9 C10 N2 Cu1 -175.7(3) . . . . ? C30 C10 N2 Cu1 2.4(6) . . . . ? C7 C11 N2 C10 -1.4(6) . . . . ? C12 C11 N2 C10 179.5(4) . . . . ? C7 C11 N2 Cu1 175.5(3) . . . . ? C12 C11 N2 Cu1 -3.6(4) . . . . ? C14 C15 O1 C16 172.3(5) . . . . ? C17 C16 O1 C15 178.7(5) . . . . ? C16 C17 O2 C18 -103.4(8) . . . . ? C19 C18 O2 C17 157.6(8) . . . . ? C18 C19 O3 C20 163.2(9) . . . . ? C21 C20 O3 C19 -174.9(10) . . . . ? C25 C24 O4 C23 -160.7(9) . . . . ? C22 C23 O4 C24 171.2(9) . . . . ? C27 C26 O5 C25 174.4(8) . . . . ? C24 C25 O5 C26 179.1(9) . . . . ? C29 C28 O6 C27 177.1(7) . . . . ? C26 C27 O6 C28 -177.1(8) . . . . ? C42B C37 P1 C31 -107.4(9) . . . . ? C42 C37 P1 C31 164.2(8) . . . . ? C38B C37 P1 C31 73.5(8) . . . . ? C38 C37 P1 C31 -26.1(7) . . . . ? C42B C37 P1 C43 145.4(8) . . . . ? C42 C37 P1 C43 57.1(8) . . . . ? C38B C37 P1 C43 -33.6(8) . . . . ? C38 C37 P1 C43 -133.3(6) . . . . ? C42B C37 P1 Cu1 31.5(9) . . . . ? C42 C37 P1 Cu1 -56.8(8) . . . . ? C38B C37 P1 Cu1 -147.5(7) . . . . ? C38 C37 P1 Cu1 112.8(6) . . . . ? C36 C31 P1 C37 116.4(4) . . . . ? C32 C31 P1 C37 -65.3(5) . . . . ? C36 C31 P1 C43 -134.7(4) . . . . ? C32 C31 P1 C43 43.6(5) . . . . ? C36 C31 P1 Cu1 -22.6(5) . . . . ? C32 C31 P1 Cu1 155.7(4) . . . . ? C44 C43 P1 C37 -89.5(4) . . . . ? C44 C43 P1 C31 163.0(3) . . . . ? C44 C43 P1 Cu1 37.3(4) . . . . ? C52 C51 P2 C45 -87.6(5) . . . . ? C56 C51 P2 C45 92.9(4) . . . . ? C52 C51 P2 C44 21.8(5) . . . . ? C56 C51 P2 C44 -157.8(4) . . . . ? C52 C51 P2 Cu1 137.4(4) . . . . ? C56 C51 P2 Cu1 -42.2(5) . . . . ? C50 C45 P2 C51 127.2(4) . . . . ? C46 C45 P2 C51 -56.8(4) . . . . ? C50 C45 P2 C44 18.4(4) . . . . ? C46 C45 P2 C44 -165.6(4) . . . . ? C50 C45 P2 Cu1 -96.0(4) . . . . ? C46 C45 P2 Cu1 80.0(4) . . . . ? C43 C44 P2 C51 163.1(3) . . . . ? C43 C44 P2 C45 -89.2(3) . . . . ? C43 C44 P2 Cu1 35.3(3) . . . . ? C10 N2 Cu1 N1 -177.4(4) . . . . ? C11 N2 Cu1 N1 6.1(3) . . . . ? C10 N2 Cu1 P2 -50.4(4) . . . . ? C11 N2 Cu1 P2 133.2(2) . . . . ? C10 N2 Cu1 P1 68.3(4) . . . . ? C11 N2 Cu1 P1 -108.1(3) . . . . ? C1 N1 Cu1 N2 179.6(4) . . . . ? C12 N1 Cu1 N2 -7.7(3) . . . . ? C1 N1 Cu1 P2 53.3(4) . . . . ? C12 N1 Cu1 P2 -134.1(2) . . . . ? C1 N1 Cu1 P1 -59.1(4) . . . . ? C12 N1 Cu1 P1 113.6(3) . . . . ? C51 P2 Cu1 N2 5.3(2) . . . . ? C45 P2 Cu1 N2 -123.2(2) . . . . ? C44 P2 Cu1 N2 121.5(2) . . . . ? C51 P2 Cu1 N1 110.7(2) . . . . ? C45 P2 Cu1 N1 -17.8(2) . . . . ? C44 P2 Cu1 N1 -133.1(2) . . . . ? C51 P2 Cu1 P1 -126.4(2) . . . . ? C45 P2 Cu1 P1 105.13(17) . . . . ? C44 P2 Cu1 P1 -10.22(16) . . . . ? C37 P1 Cu1 N2 -29.3(3) . . . . ? C31 P1 Cu1 N2 102.5(2) . . . . ? C43 P1 Cu1 N2 -144.9(2) . . . . ? C37 P1 Cu1 N1 -125.2(3) . . . . ? C31 P1 Cu1 N1 6.6(2) . . . . ? C43 P1 Cu1 N1 119.2(2) . . . . ? C37 P1 Cu1 P2 104.1(2) . . . . ? C31 P1 Cu1 P2 -124.11(17) . . . . ? C43 P1 Cu1 P2 -11.49(17) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.879 _refine_diff_density_min -2.162 _refine_diff_density_rms 0.126 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 1.000 265.6 46.6 _platon_squeeze_details ; The residual electron density was assigned to half a molecule of the diethylether solvent [48/2= 24 e per asymmetric unit; half a molecule of C4H10O1 would give 21 e]. ;