# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Wang, Xiu-Jian' _publ_contact_author_name 'Wang, Xiu-Jian' _publ_contact_author_email wang1_xj@yahoo.com.cn _publ_section_title ; Synthesis, Structural Characterization and Luminescent Properties of A Series of Cu(I) Complexes Based on Polyphosphine Ligands ; # Attachment '- 1a.CIF' data_1a _database_code_depnum_ccdc_archive 'CCDC 815811' #TrackingRef '- 1a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H37 B Cu F4 N3 P2' _chemical_formula_weight 820.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.715(3) _cell_length_b 12.682(4) _cell_length_c 13.797(3) _cell_angle_alpha 87.688(2) _cell_angle_beta 73.678(2) _cell_angle_gamma 88.855(3) _cell_volume 1965.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3421 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 53.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 17.22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10733 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6829 _reflns_number_gt 5550 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0542P)^2^+0.6239P] 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 6829 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.68935(3) 0.76047(3) 0.31176(3) 0.03636(15) Uani 1 1 d . . . P1 P 0.74433(8) 0.59107(7) 0.28818(6) 0.0365(2) Uani 1 1 d . . . P2 P 0.76537(7) 0.84370(6) 0.16105(6) 0.0342(2) Uani 1 1 d . . . N1 N 0.8713(2) 0.6497(2) 0.09469(18) 0.0365(6) Uani 1 1 d . . . N2 N 0.5274(2) 0.7927(2) 0.41302(19) 0.0388(6) Uani 1 1 d . . . N3 N 0.7490(2) 0.8181(2) 0.42750(19) 0.0404(6) Uani 1 1 d . . . C1 C 0.8503(3) 0.5984(3) 0.0136(2) 0.0388(7) Uani 1 1 d . . . C2 C 0.8415(4) 0.6547(3) -0.0737(3) 0.0509(9) Uani 1 1 d . . . H2A H 0.8486 0.7278 -0.0780 0.061 Uiso 1 1 calc R . . C3 C 0.8223(4) 0.6015(4) -0.1536(3) 0.0677(12) Uani 1 1 d . . . H3A H 0.8182 0.6399 -0.2114 0.081 Uiso 1 1 calc R . . C4 C 0.8091(4) 0.4941(4) -0.1501(3) 0.0690(13) Uani 1 1 d . . . H4A H 0.7955 0.4599 -0.2042 0.083 Uiso 1 1 calc R . . C5 C 0.8164(4) 0.4387(4) -0.0651(3) 0.0650(12) Uani 1 1 d . . . H5A H 0.8075 0.3658 -0.0611 0.078 Uiso 1 1 calc R . . C6 C 0.8371(4) 0.4896(3) 0.0156(3) 0.0516(9) Uani 1 1 d . . . H6A H 0.8422 0.4498 0.0724 0.062 Uiso 1 1 calc R . . C7 C 0.8844(3) 0.5907(3) 0.1834(2) 0.0383(7) Uani 1 1 d . . . H7A H 0.9474 0.6215 0.2057 0.046 Uiso 1 1 calc R . . H7B H 0.9071 0.5185 0.1658 0.046 Uiso 1 1 calc R . . C8 C 0.7839(4) 0.5191(3) 0.3911(2) 0.0472(9) Uani 1 1 d . . . C9 C 0.7093(5) 0.5326(4) 0.4891(3) 0.0752(14) Uani 1 1 d . . . H9A H 0.6426 0.5764 0.4989 0.090 Uiso 1 1 calc R . . C10 C 0.7346(7) 0.4811(5) 0.5710(3) 0.0958(19) Uani 1 1 d . . . H10A H 0.6827 0.4869 0.6354 0.115 Uiso 1 1 calc R . . C11 C 0.8370(7) 0.4211(5) 0.5567(4) 0.093(2) Uani 1 1 d . . . H11A H 0.8557 0.3890 0.6122 0.111 Uiso 1 1 calc R . . C12 C 0.9106(5) 0.4084(4) 0.4625(4) 0.0855(16) Uani 1 1 d . . . H12A H 0.9791 0.3673 0.4541 0.103 Uiso 1 1 calc R . . C13 C 0.8849(4) 0.4558(3) 0.3789(3) 0.0649(11) Uani 1 1 d . . . H13A H 0.9352 0.4453 0.3146 0.078 Uiso 1 1 calc R . . C14 C 0.6427(3) 0.5052(3) 0.2492(2) 0.0379(7) Uani 1 1 d . . . C15 C 0.6283(4) 0.3991(3) 0.2758(4) 0.0654(12) Uani 1 1 d . . . H15A H 0.6695 0.3677 0.3181 0.079 Uiso 1 1 calc R . . C16 C 0.5540(5) 0.3404(4) 0.2403(4) 0.0835(15) Uani 1 1 d . . . H16A H 0.5465 0.2687 0.2575 0.100 Uiso 1 1 calc R . . C17 C 0.4899(5) 0.3846(4) 0.1795(4) 0.0791(14) Uani 1 1 d . . . H17A H 0.4384 0.3437 0.1567 0.095 Uiso 1 1 calc R . . C18 C 0.5029(4) 0.4904(3) 0.1527(3) 0.0628(11) Uani 1 1 d . . . H18A H 0.4607 0.5216 0.1110 0.075 Uiso 1 1 calc R . . C19 C 0.5781(3) 0.5492(3) 0.1879(3) 0.0511(9) Uani 1 1 d . . . H19A H 0.5861 0.6207 0.1700 0.061 Uiso 1 1 calc R . . C20 C 0.8958(3) 0.7625(3) 0.0915(2) 0.0374(7) Uani 1 1 d . . . H20A H 0.9210 0.7878 0.0215 0.045 Uiso 1 1 calc R . . H20B H 0.9612 0.7728 0.1204 0.045 Uiso 1 1 calc R . . C21 C 0.8312(3) 0.9741(3) 0.1614(2) 0.0415(8) Uani 1 1 d . . . C22 C 0.7860(4) 1.0661(3) 0.1276(3) 0.0570(10) Uani 1 1 d . . . H22A H 0.7270 1.0624 0.0947 0.068 Uiso 1 1 calc R . . C23 C 0.8289(5) 1.1637(4) 0.1428(4) 0.0789(15) Uani 1 1 d . . . H23A H 0.7976 1.2248 0.1203 0.095 Uiso 1 1 calc R . . C24 C 0.9158(5) 1.1715(4) 0.1901(4) 0.0835(17) Uani 1 1 d . . . H24A H 0.9429 1.2373 0.2007 0.100 Uiso 1 1 calc R . . C25 C 0.9628(4) 1.0810(4) 0.2219(4) 0.0722(13) Uani 1 1 d . . . H25A H 1.0232 1.0856 0.2532 0.087 Uiso 1 1 calc R . . C26 C 0.9211(4) 0.9818(3) 0.2078(3) 0.0558(10) Uani 1 1 d . . . H26A H 0.9538 0.9211 0.2296 0.067 Uiso 1 1 calc R . . C27 C 0.6768(3) 0.8617(3) 0.0719(2) 0.0396(7) Uani 1 1 d . . . C28 C 0.5602(3) 0.8298(3) 0.0988(3) 0.0459(8) Uani 1 1 d . . . H28A H 0.5257 0.8031 0.1640 0.055 Uiso 1 1 calc R . . C29 C 0.4933(4) 0.8365(3) 0.0308(3) 0.0601(10) Uani 1 1 d . . . H29A H 0.4146 0.8145 0.0499 0.072 Uiso 1 1 calc R . . C30 C 0.5444(4) 0.8764(4) -0.0658(3) 0.0661(12) Uani 1 1 d . . . H30A H 0.5010 0.8789 -0.1129 0.079 Uiso 1 1 calc R . . C31 C 0.6583(4) 0.9120(4) -0.0926(3) 0.0617(11) Uani 1 1 d . . . H31A H 0.6911 0.9416 -0.1570 0.074 Uiso 1 1 calc R . . C32 C 0.7253(3) 0.9045(3) -0.0252(3) 0.0501(9) Uani 1 1 d . . . H32A H 0.8034 0.9282 -0.0445 0.060 Uiso 1 1 calc R . . C33 C 0.8587(4) 0.8267(3) 0.4356(3) 0.0555(10) Uani 1 1 d . . . H33A H 0.9213 0.7974 0.3865 0.067 Uiso 1 1 calc R . . C34 C 0.8842(4) 0.8782(4) 0.5153(3) 0.0690(12) Uani 1 1 d . . . H34A H 0.9622 0.8829 0.5185 0.083 Uiso 1 1 calc R . . C35 C 0.7943(5) 0.9207(4) 0.5871(3) 0.0679(12) Uani 1 1 d . . . H35A H 0.8106 0.9566 0.6390 0.082 Uiso 1 1 calc R . . C36 C 0.6771(4) 0.9112(3) 0.5842(2) 0.0502(9) Uani 1 1 d . . . C37 C 0.5774(5) 0.9544(3) 0.6554(3) 0.0611(12) Uani 1 1 d . . . H37A H 0.5893 0.9927 0.7077 0.073 Uiso 1 1 calc R . . C38 C 0.4667(5) 0.9417(3) 0.6494(3) 0.0605(12) Uani 1 1 d . . . H38A H 0.4036 0.9713 0.6977 0.073 Uiso 1 1 calc R . . C39 C 0.4423(3) 0.8831(3) 0.5696(3) 0.0487(9) Uani 1 1 d . . . C40 C 0.3293(4) 0.8642(3) 0.5603(3) 0.0649(12) Uani 1 1 d . . . H40A H 0.2626 0.8885 0.6087 0.078 Uiso 1 1 calc R . . C41 C 0.3162(4) 0.8112(4) 0.4819(4) 0.0658(12) Uani 1 1 d . . . H41A H 0.2406 0.7974 0.4764 0.079 Uiso 1 1 calc R . . C42 C 0.4173(3) 0.7768(3) 0.4083(3) 0.0531(9) Uani 1 1 d . . . H42A H 0.4069 0.7412 0.3538 0.064 Uiso 1 1 calc R . . C43 C 0.6574(3) 0.8582(2) 0.5013(2) 0.0381(7) Uani 1 1 d . . . C44 C 0.5400(3) 0.8442(2) 0.4942(2) 0.0373(7) Uani 1 1 d . . . B1 B 0.1819(5) 0.8075(4) 0.2340(5) 0.0692(14) Uani 1 1 d . . . F1 F 0.1660(5) 0.8876(4) 0.2869(5) 0.230(3) Uani 1 1 d . . . F2 F 0.1883(4) 0.8376(4) 0.1317(3) 0.1303(14) Uani 1 1 d . . . F3 F 0.2808(3) 0.7497(3) 0.2342(3) 0.1031(10) Uani 1 1 d . . . F4 F 0.0856(2) 0.7436(2) 0.2567(2) 0.0867(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0408(3) 0.0378(3) 0.0279(2) -0.00782(16) -0.00429(17) -0.00236(17) P1 0.0440(5) 0.0357(5) 0.0292(4) -0.0039(3) -0.0090(4) -0.0006(4) P2 0.0353(5) 0.0355(5) 0.0300(4) -0.0021(3) -0.0060(3) -0.0031(3) N1 0.0424(16) 0.0375(15) 0.0289(13) -0.0082(11) -0.0082(12) 0.0011(12) N2 0.0375(15) 0.0391(15) 0.0367(14) -0.0011(12) -0.0049(12) -0.0053(12) N3 0.0405(16) 0.0468(17) 0.0326(14) -0.0068(12) -0.0072(12) -0.0051(13) C1 0.0282(16) 0.051(2) 0.0336(17) -0.0113(14) -0.0023(13) 0.0022(14) C2 0.056(2) 0.059(2) 0.0413(19) -0.0088(17) -0.0183(17) 0.0024(18) C3 0.075(3) 0.092(4) 0.042(2) -0.014(2) -0.025(2) 0.011(3) C4 0.066(3) 0.092(4) 0.058(3) -0.036(2) -0.028(2) 0.008(2) C5 0.063(3) 0.066(3) 0.065(3) -0.031(2) -0.012(2) -0.002(2) C6 0.059(2) 0.049(2) 0.0428(19) -0.0129(16) -0.0058(17) -0.0008(18) C7 0.0374(18) 0.0425(19) 0.0347(17) -0.0048(14) -0.0095(14) 0.0042(14) C8 0.068(3) 0.042(2) 0.0346(18) 0.0023(15) -0.0190(17) -0.0110(17) C9 0.103(4) 0.075(3) 0.042(2) 0.005(2) -0.013(2) -0.001(3) C10 0.158(6) 0.088(4) 0.039(2) 0.011(2) -0.025(3) -0.019(4) C11 0.152(6) 0.080(4) 0.066(3) 0.030(3) -0.064(4) -0.037(4) C12 0.101(4) 0.073(3) 0.101(4) 0.029(3) -0.063(4) -0.013(3) C13 0.074(3) 0.066(3) 0.062(3) 0.011(2) -0.033(2) -0.002(2) C14 0.0364(18) 0.0361(18) 0.0399(17) -0.0059(14) -0.0077(14) 0.0009(14) C15 0.079(3) 0.041(2) 0.089(3) 0.008(2) -0.045(3) -0.009(2) C16 0.096(4) 0.042(2) 0.128(4) 0.002(3) -0.056(4) -0.016(2) C17 0.078(3) 0.066(3) 0.109(4) -0.018(3) -0.050(3) -0.012(2) C18 0.059(3) 0.062(3) 0.077(3) -0.002(2) -0.034(2) 0.000(2) C19 0.054(2) 0.045(2) 0.058(2) 0.0015(17) -0.0216(19) -0.0043(17) C20 0.0339(17) 0.0431(19) 0.0313(16) -0.0038(13) -0.0020(13) -0.0031(14) C21 0.0407(19) 0.0389(19) 0.0363(17) -0.0042(14) 0.0041(14) -0.0080(14) C22 0.060(3) 0.043(2) 0.060(2) 0.0012(18) -0.0036(19) -0.0002(18) C23 0.083(4) 0.042(2) 0.088(3) 0.003(2) 0.013(3) -0.009(2) C24 0.078(4) 0.059(3) 0.089(4) -0.022(3) 0.022(3) -0.033(3) C25 0.055(3) 0.074(3) 0.079(3) -0.022(3) -0.002(2) -0.025(2) C26 0.050(2) 0.055(2) 0.059(2) -0.0139(18) -0.0080(19) -0.0067(18) C27 0.0399(19) 0.0419(19) 0.0368(17) -0.0014(14) -0.0106(14) 0.0022(14) C28 0.045(2) 0.045(2) 0.0466(19) 0.0019(16) -0.0111(16) -0.0009(16) C29 0.048(2) 0.062(3) 0.074(3) -0.003(2) -0.024(2) -0.0044(19) C30 0.067(3) 0.080(3) 0.061(3) 0.000(2) -0.034(2) 0.004(2) C31 0.064(3) 0.080(3) 0.041(2) 0.0044(19) -0.0165(19) 0.008(2) C32 0.044(2) 0.061(2) 0.0429(19) 0.0044(17) -0.0087(16) 0.0011(17) C33 0.048(2) 0.072(3) 0.049(2) -0.0105(19) -0.0170(18) -0.0007(19) C34 0.060(3) 0.090(3) 0.068(3) -0.015(2) -0.034(2) -0.010(2) C35 0.096(4) 0.069(3) 0.053(2) -0.016(2) -0.042(3) -0.010(2) C36 0.081(3) 0.042(2) 0.0298(17) -0.0038(14) -0.0188(18) 0.0030(18) C37 0.099(4) 0.052(2) 0.0298(19) -0.0089(16) -0.015(2) 0.010(2) C38 0.094(4) 0.047(2) 0.0250(17) -0.0045(15) 0.0069(19) 0.022(2) C39 0.054(2) 0.041(2) 0.0376(19) 0.0081(15) 0.0071(16) 0.0085(17) C40 0.055(3) 0.061(3) 0.058(3) 0.008(2) 0.014(2) 0.010(2) C41 0.037(2) 0.067(3) 0.085(3) 0.005(2) -0.005(2) -0.0083(19) C42 0.038(2) 0.056(2) 0.062(2) -0.0007(18) -0.0092(18) -0.0096(17) C43 0.054(2) 0.0305(17) 0.0290(16) -0.0015(13) -0.0092(15) -0.0032(14) C44 0.047(2) 0.0296(16) 0.0282(15) 0.0022(12) 0.0011(14) 0.0014(14) B1 0.063(3) 0.062(3) 0.089(4) 0.004(3) -0.032(3) -0.008(3) F1 0.217(6) 0.163(4) 0.373(8) -0.183(5) -0.166(6) 0.032(4) F2 0.116(3) 0.161(4) 0.114(3) 0.036(3) -0.038(2) 0.004(3) F3 0.0535(17) 0.151(3) 0.107(2) 0.020(2) -0.0293(16) 0.0022(17) F4 0.0592(16) 0.091(2) 0.108(2) -0.0201(16) -0.0178(15) -0.0085(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 2.060(3) . ? Cu1 N3 2.077(3) . ? Cu1 P1 2.2404(11) . ? Cu1 P2 2.2474(10) . ? P1 C8 1.821(4) . ? P1 C14 1.831(3) . ? P1 C7 1.858(3) . ? P2 C27 1.823(3) . ? P2 C21 1.839(3) . ? P2 C20 1.873(3) . ? N1 C1 1.398(4) . ? N1 C7 1.452(4) . ? N1 C20 1.461(4) . ? N2 C42 1.330(5) . ? N2 C44 1.363(4) . ? N3 C33 1.328(5) . ? N3 C43 1.361(4) . ? C1 C6 1.390(5) . ? C1 C2 1.404(5) . ? C2 C3 1.389(5) . ? C2 H2A 0.9300 . ? C3 C4 1.371(6) . ? C3 H3A 0.9300 . ? C4 C5 1.366(7) . ? C4 H4A 0.9300 . ? C5 C6 1.390(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.391(6) . ? C8 C9 1.403(6) . ? C9 C10 1.383(7) . ? C9 H9A 0.9300 . ? C10 C11 1.378(9) . ? C10 H10A 0.9300 . ? C11 C12 1.357(8) . ? C11 H11A 0.9300 . ? C12 C13 1.383(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C19 1.380(5) . ? C14 C15 1.381(5) . ? C15 C16 1.359(6) . ? C15 H15A 0.9300 . ? C16 C17 1.371(7) . ? C16 H16A 0.9300 . ? C17 C18 1.378(6) . ? C17 H17A 0.9300 . ? C18 C19 1.365(5) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.385(5) . ? C21 C22 1.389(5) . ? C22 C23 1.391(6) . ? C22 H22A 0.9300 . ? C23 C24 1.362(8) . ? C23 H23A 0.9300 . ? C24 C25 1.373(8) . ? C24 H24A 0.9300 . ? C25 C26 1.398(6) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.377(5) . ? C27 C32 1.392(5) . ? C28 C29 1.380(5) . ? C28 H28A 0.9300 . ? C29 C30 1.377(6) . ? C29 H29A 0.9300 . ? C30 C31 1.363(6) . ? C30 H30A 0.9300 . ? C31 C32 1.374(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.406(5) . ? C33 H33A 0.9300 . ? C34 C35 1.347(7) . ? C34 H34A 0.9300 . ? C35 C36 1.393(6) . ? C35 H35A 0.9300 . ? C36 C37 1.415(6) . ? C36 C43 1.425(4) . ? C37 C38 1.335(6) . ? C37 H37A 0.9300 . ? C38 C39 1.448(6) . ? C38 H38A 0.9300 . ? C39 C40 1.392(6) . ? C39 C44 1.409(5) . ? C40 C41 1.343(6) . ? C40 H40A 0.9300 . ? C41 C42 1.401(6) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.421(5) . ? B1 F1 1.255(7) . ? B1 F4 1.359(6) . ? B1 F3 1.359(6) . ? B1 F2 1.429(7) . ? 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 N3 80.95(11) . . ? N2 Cu1 P1 118.03(8) . . ? N3 Cu1 P1 109.91(8) . . ? N2 Cu1 P2 125.85(8) . . ? N3 Cu1 P2 114.03(8) . . ? P1 Cu1 P2 105.36(3) . . ? C8 P1 C14 105.61(16) . . ? C8 P1 C7 103.68(17) . . ? C14 P1 C7 105.49(15) . . ? C8 P1 Cu1 117.28(12) . . ? C14 P1 Cu1 116.94(11) . . ? C7 P1 Cu1 106.46(11) . . ? C27 P2 C21 103.96(16) . . ? C27 P2 C20 103.86(15) . . ? C21 P2 C20 102.82(15) . . ? C27 P2 Cu1 120.56(11) . . ? C21 P2 Cu1 117.04(11) . . ? C20 P2 Cu1 106.50(11) . . ? C1 N1 C7 121.1(3) . . ? C1 N1 C20 123.1(3) . . ? C7 N1 C20 115.4(2) . . ? C42 N2 C44 117.3(3) . . ? C42 N2 Cu1 130.7(2) . . ? C44 N2 Cu1 111.8(2) . . ? C33 N3 C43 118.4(3) . . ? C33 N3 Cu1 130.3(2) . . ? C43 N3 Cu1 111.2(2) . . ? C6 C1 N1 121.8(3) . . ? C6 C1 C2 116.9(3) . . ? N1 C1 C2 121.3(3) . . ? C3 C2 C1 120.0(4) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 122.2(4) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C5 C4 C3 118.1(4) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 121.7(4) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? N1 C7 P1 111.6(2) . . ? N1 C7 H7A 109.3 . . ? P1 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? P1 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C13 C8 C9 118.7(4) . . ? C13 C8 P1 124.2(3) . . ? C9 C8 P1 117.1(3) . . ? C10 C9 C8 120.2(5) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 119.7(5) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C12 C13 C8 120.0(5) . . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? C19 C14 C15 118.1(3) . . ? C19 C14 P1 117.7(3) . . ? C15 C14 P1 124.2(3) . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C19 C18 C17 119.4(4) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C14 121.7(4) . . ? C18 C19 H19A 119.1 . . ? C14 C19 H19A 119.1 . . ? N1 C20 P2 113.8(2) . . ? N1 C20 H20A 108.8 . . ? P2 C20 H20A 108.8 . . ? N1 C20 H20B 108.8 . . ? P2 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C26 C21 C22 118.7(4) . . ? C26 C21 P2 118.0(3) . . ? C22 C21 P2 122.9(3) . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C24 C23 C22 121.2(5) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C25 119.1(4) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C24 C25 C26 120.8(5) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C21 C26 C25 120.0(4) . . ? C21 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C32 118.3(3) . . ? C28 C27 P2 120.1(3) . . ? C32 C27 P2 121.6(3) . . ? C27 C28 C29 121.3(3) . . ? C27 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C30 C29 C28 119.3(4) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C30 C31 C32 120.5(4) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 C27 120.3(4) . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? N3 C33 C34 122.7(4) . . ? N3 C33 H33A 118.6 . . ? C34 C33 H33A 118.6 . . ? C35 C34 C33 119.2(4) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 120.6(3) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C37 124.4(4) . . ? C35 C36 C43 117.4(4) . . ? C37 C36 C43 118.1(4) . . ? C38 C37 C36 121.8(4) . . ? C38 C37 H37A 119.1 . . ? C36 C37 H37A 119.1 . . ? C37 C38 C39 121.8(4) . . ? C37 C38 H38A 119.1 . . ? C39 C38 H38A 119.1 . . ? C40 C39 C44 117.2(4) . . ? C40 C39 C38 124.9(4) . . ? C44 C39 C38 117.9(4) . . ? C41 C40 C39 120.4(4) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C40 C41 C42 119.4(4) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? N2 C42 C41 122.9(4) . . ? N2 C42 H42A 118.6 . . ? C41 C42 H42A 118.6 . . ? N3 C43 C44 117.8(3) . . ? N3 C43 C36 121.7(3) . . ? C44 C43 C36 120.5(3) . . ? N2 C44 C39 122.7(3) . . ? N2 C44 C43 117.5(3) . . ? C39 C44 C43 119.8(3) . . ? F1 B1 F4 112.9(6) . . ? F1 B1 F3 114.9(5) . . ? F4 B1 F3 109.7(4) . . ? F1 B1 F2 110.0(6) . . ? F4 B1 F2 100.1(4) . . ? F3 B1 F2 108.2(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 P1 C8 -70.67(17) . . . . ? N3 Cu1 P1 C8 19.52(17) . . . . ? P2 Cu1 P1 C8 142.79(15) . . . . ? N2 Cu1 P1 C14 56.31(15) . . . . ? N3 Cu1 P1 C14 146.50(14) . . . . ? P2 Cu1 P1 C14 -90.23(12) . . . . ? N2 Cu1 P1 C7 173.86(13) . . . . ? N3 Cu1 P1 C7 -95.95(14) . . . . ? P2 Cu1 P1 C7 27.32(11) . . . . ? N2 Cu1 P2 C27 -49.98(16) . . . . ? N3 Cu1 P2 C27 -146.28(16) . . . . ? P1 Cu1 P2 C27 93.12(13) . . . . ? N2 Cu1 P2 C21 78.04(17) . . . . ? N3 Cu1 P2 C21 -18.26(16) . . . . ? P1 Cu1 P2 C21 -138.86(14) . . . . ? N2 Cu1 P2 C20 -167.69(14) . . . . ? N3 Cu1 P2 C20 96.01(14) . . . . ? P1 Cu1 P2 C20 -24.59(11) . . . . ? N3 Cu1 N2 C42 -177.0(3) . . . . ? P1 Cu1 N2 C42 -69.2(3) . . . . ? P2 Cu1 N2 C42 69.8(3) . . . . ? N3 Cu1 N2 C44 7.1(2) . . . . ? P1 Cu1 N2 C44 114.9(2) . . . . ? P2 Cu1 N2 C44 -106.1(2) . . . . ? N2 Cu1 N3 C33 177.1(4) . . . . ? P1 Cu1 N3 C33 60.5(3) . . . . ? P2 Cu1 N3 C33 -57.6(4) . . . . ? N2 Cu1 N3 C43 -7.5(2) . . . . ? P1 Cu1 N3 C43 -124.1(2) . . . . ? P2 Cu1 N3 C43 117.9(2) . . . . ? C7 N1 C1 C6 2.2(5) . . . . ? C20 N1 C1 C6 174.5(3) . . . . ? C7 N1 C1 C2 -177.8(3) . . . . ? C20 N1 C1 C2 -5.5(5) . . . . ? C6 C1 C2 C3 -0.9(5) . . . . ? N1 C1 C2 C3 179.1(4) . . . . ? C1 C2 C3 C4 1.2(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 C1 0.4(7) . . . . ? N1 C1 C6 C5 -179.9(4) . . . . ? C2 C1 C6 C5 0.2(6) . . . . ? C1 N1 C7 P1 -99.0(3) . . . . ? C20 N1 C7 P1 88.1(3) . . . . ? C8 P1 C7 N1 -177.4(2) . . . . ? C14 P1 C7 N1 71.8(3) . . . . ? Cu1 P1 C7 N1 -53.1(2) . . . . ? C14 P1 C8 C13 94.6(4) . . . . ? C7 P1 C8 C13 -16.1(4) . . . . ? Cu1 P1 C8 C13 -133.1(3) . . . . ? C14 P1 C8 C9 -88.1(3) . . . . ? C7 P1 C8 C9 161.2(3) . . . . ? Cu1 P1 C8 C9 44.2(4) . . . . ? C13 C8 C9 C10 -1.9(7) . . . . ? P1 C8 C9 C10 -179.4(4) . . . . ? C8 C9 C10 C11 3.6(8) . . . . ? C9 C10 C11 C12 -2.9(9) . . . . ? C10 C11 C12 C13 0.4(8) . . . . ? C11 C12 C13 C8 1.3(7) . . . . ? C9 C8 C13 C12 -0.5(6) . . . . ? P1 C8 C13 C12 176.7(3) . . . . ? C8 P1 C14 C19 165.9(3) . . . . ? C7 P1 C14 C19 -84.7(3) . . . . ? Cu1 P1 C14 C19 33.4(3) . . . . ? C8 P1 C14 C15 -15.4(4) . . . . ? C7 P1 C14 C15 94.0(4) . . . . ? Cu1 P1 C14 C15 -147.9(3) . . . . ? C19 C14 C15 C16 1.2(7) . . . . ? P1 C14 C15 C16 -177.5(4) . . . . ? C14 C15 C16 C17 -1.4(9) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? C16 C17 C18 C19 -0.6(8) . . . . ? C17 C18 C19 C14 0.5(7) . . . . ? C15 C14 C19 C18 -0.8(6) . . . . ? P1 C14 C19 C18 178.0(3) . . . . ? C1 N1 C20 P2 102.5(3) . . . . ? C7 N1 C20 P2 -84.8(3) . . . . ? C27 P2 C20 N1 -81.2(2) . . . . ? C21 P2 C20 N1 170.7(2) . . . . ? Cu1 P2 C20 N1 47.0(2) . . . . ? C27 P2 C21 C26 -168.3(3) . . . . ? C20 P2 C21 C26 -60.3(3) . . . . ? Cu1 P2 C21 C26 56.0(3) . . . . ? C27 P2 C21 C22 19.1(3) . . . . ? C20 P2 C21 C22 127.1(3) . . . . ? Cu1 P2 C21 C22 -116.6(3) . . . . ? C26 C21 C22 C23 -1.7(6) . . . . ? P2 C21 C22 C23 170.9(3) . . . . ? C21 C22 C23 C24 0.5(7) . . . . ? C22 C23 C24 C25 0.9(7) . . . . ? C23 C24 C25 C26 -1.1(7) . . . . ? C22 C21 C26 C25 1.5(6) . . . . ? P2 C21 C26 C25 -171.5(3) . . . . ? C24 C25 C26 C21 -0.1(6) . . . . ? C21 P2 C27 C28 -129.9(3) . . . . ? C20 P2 C27 C28 122.8(3) . . . . ? Cu1 P2 C27 C28 3.8(3) . . . . ? C21 P2 C27 C32 52.1(3) . . . . ? C20 P2 C27 C32 -55.2(3) . . . . ? Cu1 P2 C27 C32 -174.2(2) . . . . ? C32 C27 C28 C29 2.0(5) . . . . ? P2 C27 C28 C29 -176.0(3) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C28 C29 C30 C31 -2.3(7) . . . . ? C29 C30 C31 C32 2.8(7) . . . . ? C30 C31 C32 C27 -0.9(6) . . . . ? C28 C27 C32 C31 -1.5(5) . . . . ? P2 C27 C32 C31 176.5(3) . . . . ? C43 N3 C33 C34 -2.1(6) . . . . ? Cu1 N3 C33 C34 173.1(3) . . . . ? N3 C33 C34 C35 0.2(7) . . . . ? C33 C34 C35 C36 1.8(7) . . . . ? C34 C35 C36 C37 -179.1(4) . . . . ? C34 C35 C36 C43 -1.9(6) . . . . ? C35 C36 C37 C38 -179.2(4) . . . . ? C43 C36 C37 C38 3.6(6) . . . . ? C36 C37 C38 C39 -0.1(6) . . . . ? C37 C38 C39 C40 178.1(4) . . . . ? C37 C38 C39 C44 -3.5(5) . . . . ? C44 C39 C40 C41 -0.1(6) . . . . ? C38 C39 C40 C41 178.2(4) . . . . ? C39 C40 C41 C42 -1.3(6) . . . . ? C44 N2 C42 C41 0.6(5) . . . . ? Cu1 N2 C42 C41 -175.1(3) . . . . ? C40 C41 C42 N2 1.1(6) . . . . ? C33 N3 C43 C44 -177.1(3) . . . . ? Cu1 N3 C43 C44 6.8(3) . . . . ? C33 N3 C43 C36 1.9(5) . . . . ? Cu1 N3 C43 C36 -174.1(3) . . . . ? C35 C36 C43 N3 0.0(5) . . . . ? C37 C36 C43 N3 177.4(3) . . . . ? C35 C36 C43 C44 179.1(3) . . . . ? C37 C36 C43 C44 -3.6(5) . . . . ? C42 N2 C44 C39 -2.1(5) . . . . ? Cu1 N2 C44 C39 174.4(2) . . . . ? C42 N2 C44 C43 177.8(3) . . . . ? Cu1 N2 C44 C43 -5.7(3) . . . . ? C40 C39 C44 N2 1.9(5) . . . . ? C38 C39 C44 N2 -176.6(3) . . . . ? C40 C39 C44 C43 -178.1(3) . . . . ? C38 C39 C44 C43 3.5(5) . . . . ? N3 C43 C44 N2 -0.8(4) . . . . ? C36 C43 C44 N2 -179.9(3) . . . . ? N3 C43 C44 C39 179.1(3) . . . . ? C36 C43 C44 C39 0.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.110 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.070 # Attachment '- 1b.CIF' data_1b _database_code_depnum_ccdc_archive 'CCDC 815812' #TrackingRef '- 1b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H41 B Cu F4 N3 O0 P2' _chemical_formula_weight 848.11 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' 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.871(3) _cell_length_b 14.472(3) _cell_length_c 19.411(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.221(3) _cell_angle_gamma 90.00 _cell_volume 4123.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2634 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 53.25 _exptl_crystal_description block _exptl_crystal_colour yelloq _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 17.22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23204 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7261 _reflns_number_gt 5633 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0982P)^2^+0.8982P] 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 7261 _refine_ls_number_parameters 523 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 0.85718(2) 0.41800(3) 0.171502(18) 0.04237(16) Uani 1 1 d . . . P1 P 0.80388(5) 0.31268(6) 0.09088(4) 0.0429(2) Uani 1 1 d . . . P2 P 0.82779(5) 0.54804(6) 0.10957(4) 0.0410(2) Uani 1 1 d . . . N1 N 0.76064(19) 0.44826(19) -0.01366(13) 0.0485(6) Uani 1 1 d . . . N2 N 0.8213(2) 0.41522(18) 0.27051(15) 0.0516(7) Uani 1 1 d . . . N3 N 0.98521(19) 0.40824(19) 0.22829(15) 0.0508(7) Uani 1 1 d . . . C1 C 0.7172(2) 0.4654(2) -0.08424(16) 0.0493(8) Uani 1 1 d . . . C2 C 0.6669(3) 0.5458(3) -0.0994(2) 0.0645(10) Uani 1 1 d . . . H2A H 0.6620 0.5873 -0.0636 0.077 Uiso 1 1 calc R . . C3 C 0.6243(3) 0.5656(3) -0.1660(2) 0.0782(13) Uani 1 1 d . . . H3A H 0.5920 0.6205 -0.1750 0.094 Uiso 1 1 calc R . . C4 C 0.6294(3) 0.5047(4) -0.2184(2) 0.0848(13) Uani 1 1 d . . . H4A H 0.5991 0.5168 -0.2632 0.102 Uiso 1 1 calc R . . C5 C 0.6786(4) 0.4265(3) -0.2054(2) 0.0807(13) Uani 1 1 d . . . H5A H 0.6825 0.3857 -0.2418 0.097 Uiso 1 1 calc R . . C6 C 0.7236(3) 0.4052(3) -0.13889(19) 0.0635(10) Uani 1 1 d . . . H6A H 0.7576 0.3513 -0.1311 0.076 Uiso 1 1 calc R . . C7 C 0.7988(2) 0.3563(2) 0.00032(16) 0.0514(8) Uani 1 1 d . . . H7A H 0.8601 0.3561 -0.0108 0.062 Uiso 1 1 calc R . . H7B H 0.7630 0.3132 -0.0311 0.062 Uiso 1 1 calc R . . C8 C 0.8661(2) 0.2057(2) 0.08337(17) 0.0465(7) Uani 1 1 d . . . C9 C 0.9473(3) 0.1914(3) 0.1269(2) 0.0617(9) Uani 1 1 d . . . H9A H 0.9692 0.2361 0.1597 0.074 Uiso 1 1 calc R . . C10 C 0.9972(3) 0.1107(3) 0.1223(3) 0.0771(12) Uani 1 1 d . . . H10A H 1.0526 0.1015 0.1514 0.092 Uiso 1 1 calc R . . C11 C 0.9632(3) 0.0452(3) 0.0740(3) 0.0784(13) Uani 1 1 d . . . H11A H 0.9963 -0.0086 0.0704 0.094 Uiso 1 1 calc R . . C12 C 0.8820(3) 0.0570(3) 0.0312(2) 0.0717(12) Uani 1 1 d . . . H12A H 0.8595 0.0111 -0.0005 0.086 Uiso 1 1 calc R . . C13 C 0.8334(3) 0.1380(2) 0.0351(2) 0.0585(9) Uani 1 1 d . . . H13A H 0.7785 0.1470 0.0054 0.070 Uiso 1 1 calc R . . C14 C 0.6894(2) 0.2687(2) 0.09345(18) 0.0490(8) Uani 1 1 d . . . C15 C 0.6805(3) 0.1976(3) 0.1384(2) 0.0668(10) Uani 1 1 d . . . H15A H 0.7323 0.1696 0.1627 0.080 Uiso 1 1 calc R . . C16 C 0.5944(3) 0.1665(3) 0.1481(3) 0.0852(14) Uani 1 1 d . . . H16A H 0.5889 0.1188 0.1792 0.102 Uiso 1 1 calc R . . C17 C 0.5182(3) 0.2072(4) 0.1114(3) 0.0911(16) Uani 1 1 d . . . H17A H 0.4606 0.1874 0.1177 0.109 Uiso 1 1 calc R . . C18 C 0.5271(3) 0.2763(4) 0.0659(3) 0.0884(15) Uani 1 1 d . . . H18A H 0.4750 0.3033 0.0410 0.106 Uiso 1 1 calc R . . C19 C 0.6117(3) 0.3077(3) 0.0555(2) 0.0667(10) Uani 1 1 d . . . H19A H 0.6164 0.3545 0.0234 0.080 Uiso 1 1 calc R . . C20 C 0.8206(2) 0.5238(2) 0.01516(15) 0.0492(8) Uani 1 1 d . . . H20A H 0.8004 0.5798 -0.0103 0.059 Uiso 1 1 calc R . . H20B H 0.8815 0.5104 0.0061 0.059 Uiso 1 1 calc R . . C21 C 0.7196(2) 0.6002(2) 0.12060(17) 0.0463(8) Uani 1 1 d . . . C22 C 0.6383(3) 0.5686(3) 0.0846(2) 0.0660(10) Uani 1 1 d . . . H22A H 0.6380 0.5277 0.0476 0.079 Uiso 1 1 calc R . . C23 C 0.5562(3) 0.5976(4) 0.1035(3) 0.0797(13) Uani 1 1 d . . . H23A H 0.5013 0.5765 0.0787 0.096 Uiso 1 1 calc R . . C24 C 0.5558(3) 0.6575(3) 0.1590(3) 0.0795(13) Uani 1 1 d . . . H24A H 0.5010 0.6764 0.1716 0.095 Uiso 1 1 calc R . . C25 C 0.6360(3) 0.6885(3) 0.1949(2) 0.0719(11) Uani 1 1 d . . . H25A H 0.6360 0.7281 0.2326 0.086 Uiso 1 1 calc R . . C26 C 0.7182(3) 0.6613(2) 0.1755(2) 0.0594(9) Uani 1 1 d . . . H26A H 0.7727 0.6843 0.1996 0.071 Uiso 1 1 calc R . . C27 C 0.9097(2) 0.6431(2) 0.11802(17) 0.0465(7) Uani 1 1 d . . . C28 C 0.9072(3) 0.7122(3) 0.0682(2) 0.0650(10) Uani 1 1 d . . . H28A H 0.8596 0.7140 0.0307 0.078 Uiso 1 1 calc R . . C29 C 0.9749(3) 0.7784(3) 0.0737(3) 0.0785(12) Uani 1 1 d . . . H29A H 0.9739 0.8230 0.0391 0.094 Uiso 1 1 calc R . . C30 C 1.0426(3) 0.7786(3) 0.1294(3) 0.0817(13) Uani 1 1 d . . . H30A H 1.0870 0.8244 0.1334 0.098 Uiso 1 1 calc R . . C31 C 1.0465(3) 0.7126(3) 0.1796(3) 0.0765(12) Uani 1 1 d . . . H31A H 1.0933 0.7133 0.2177 0.092 Uiso 1 1 calc R . . C32 C 0.9803(3) 0.6438(3) 0.1738(2) 0.0617(9) Uani 1 1 d . . . H32A H 0.9835 0.5981 0.2077 0.074 Uiso 1 1 calc R . . C33 C 0.7390(3) 0.4154(3) 0.2901(2) 0.0715(13) Uani 1 1 d . . . C34 C 0.7292(5) 0.4100(4) 0.3605(3) 0.111(2) Uani 1 1 d . . . H34A H 0.6713 0.4079 0.3727 0.133 Uiso 1 1 calc R . . C35 C 0.8029(6) 0.4080(4) 0.4105(3) 0.113(2) Uani 1 1 d . . . H35A H 0.7959 0.4062 0.4572 0.135 Uiso 1 1 calc R . . C36 C 0.8902(5) 0.4085(3) 0.3922(2) 0.0905(16) Uani 1 1 d . . . C37 C 0.9700(7) 0.4056(5) 0.4409(3) 0.133(3) Uani 1 1 d . . . H37A H 0.9659 0.4046 0.4882 0.159 Uiso 1 1 calc R . . C38 C 1.0507(6) 0.4041(5) 0.4218(3) 0.128(3) Uani 1 1 d . . . H38A H 1.1021 0.4015 0.4561 0.154 Uiso 1 1 calc R . . C39 C 1.0625(4) 0.4066(4) 0.3484(3) 0.0963(17) Uani 1 1 d . . . C40 C 1.1432(5) 0.4041(5) 0.3247(4) 0.126(3) Uani 1 1 d . . . H40A H 1.1970 0.4034 0.3566 0.151 Uiso 1 1 calc R . . C41 C 1.1475(3) 0.4028(4) 0.2559(4) 0.1093(19) Uani 1 1 d . . . H41A H 1.2036 0.3997 0.2406 0.131 Uiso 1 1 calc R . . C42 C 1.0657(3) 0.4060(3) 0.2070(2) 0.0697(11) Uani 1 1 d . . . C43 C 0.8955(3) 0.4113(2) 0.32045(19) 0.0619(10) Uani 1 1 d . . . C44 C 0.9827(3) 0.4086(2) 0.29823(19) 0.0615(10) Uani 1 1 d . . . C45 C 0.6562(3) 0.4191(3) 0.2351(3) 0.0892(16) Uani 1 1 d . . . H45A H 0.6745 0.4234 0.1900 0.134 Uiso 1 1 calc R . . H45B H 0.6203 0.4722 0.2427 0.134 Uiso 1 1 calc R . . H45C H 0.6207 0.3641 0.2374 0.134 Uiso 1 1 calc R . . C46 C 1.0671(3) 0.4100(3) 0.1304(3) 0.0862(15) Uani 1 1 d . . . H46A H 1.0058 0.4127 0.1057 0.129 Uiso 1 1 calc R . . H46B H 1.0967 0.3558 0.1163 0.129 Uiso 1 1 calc R . . H46C H 1.0999 0.4640 0.1198 0.129 Uiso 1 1 calc R . . B1 B 0.7466(5) 0.8249(5) -0.1055(6) 0.121(3) Uani 1 1 d U . . F1 F 0.8032(6) 0.7824(5) -0.1287(5) 0.315(5) Uani 1 1 d U A . F2 F 0.7190(9) 0.8991(6) -0.0950(6) 0.346(5) Uani 1 1 d U A . F3 F 0.6882(4) 0.8260(6) -0.1660(2) 0.125(3) Uani 0.50 1 d PU A 1 F3' F 0.8037(6) 0.8867(10) -0.0758(8) 0.243(7) Uani 0.50 1 d PU A 2 F4 F 0.7113(4) 0.7713(4) -0.0592(2) 0.1794(19) Uani 1 1 d U A . 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 0.0449(3) 0.0464(3) 0.0371(2) 0.00261(15) 0.01078(17) 0.00005(16) P1 0.0434(4) 0.0409(5) 0.0453(5) -0.0005(3) 0.0097(3) 0.0018(3) P2 0.0462(5) 0.0400(4) 0.0377(4) 0.0006(3) 0.0095(3) -0.0017(3) N1 0.0618(17) 0.0427(15) 0.0399(14) -0.0012(12) 0.0047(12) 0.0022(13) N2 0.074(2) 0.0428(16) 0.0433(16) 0.0039(12) 0.0267(15) 0.0024(13) N3 0.0500(16) 0.0490(17) 0.0523(17) 0.0056(12) 0.0049(13) -0.0044(12) C1 0.0512(19) 0.057(2) 0.0397(17) -0.0015(15) 0.0060(14) -0.0045(16) C2 0.072(3) 0.064(2) 0.056(2) 0.0013(18) 0.0054(19) 0.012(2) C3 0.083(3) 0.082(3) 0.064(3) 0.010(2) -0.004(2) 0.014(2) C4 0.095(3) 0.091(3) 0.059(3) 0.007(2) -0.014(2) -0.006(3) C5 0.104(4) 0.085(3) 0.047(2) -0.012(2) -0.006(2) -0.005(3) C6 0.076(3) 0.063(2) 0.049(2) -0.0102(17) 0.0063(19) 0.0037(19) C7 0.061(2) 0.051(2) 0.0434(18) -0.0049(15) 0.0111(15) 0.0028(16) C8 0.0460(18) 0.0419(18) 0.0546(19) 0.0015(15) 0.0177(15) 0.0004(14) C9 0.060(2) 0.055(2) 0.069(2) 0.0068(18) 0.0088(18) 0.0112(18) C10 0.073(3) 0.075(3) 0.085(3) 0.017(3) 0.016(2) 0.029(2) C11 0.085(3) 0.059(3) 0.101(3) 0.018(3) 0.043(3) 0.026(2) C12 0.088(3) 0.048(2) 0.088(3) -0.013(2) 0.042(3) -0.007(2) C13 0.057(2) 0.052(2) 0.070(2) -0.0061(18) 0.0193(18) -0.0017(17) C14 0.0450(18) 0.0471(19) 0.056(2) -0.0087(15) 0.0129(15) 0.0005(15) C15 0.062(2) 0.066(3) 0.077(3) 0.005(2) 0.026(2) -0.0017(19) C16 0.075(3) 0.080(3) 0.110(4) -0.008(3) 0.044(3) -0.018(2) C17 0.062(3) 0.094(4) 0.126(4) -0.034(3) 0.043(3) -0.020(3) C18 0.047(2) 0.092(4) 0.124(4) -0.019(3) 0.008(2) 0.008(2) C19 0.054(2) 0.066(3) 0.079(3) -0.007(2) 0.0059(19) 0.0026(19) C20 0.062(2) 0.0483(19) 0.0376(17) 0.0014(14) 0.0098(15) -0.0028(16) C21 0.054(2) 0.0399(17) 0.0469(18) 0.0065(14) 0.0127(15) 0.0037(14) C22 0.055(2) 0.076(3) 0.066(2) -0.0079(19) 0.0079(19) 0.0018(19) C23 0.048(2) 0.099(4) 0.090(3) 0.006(3) 0.006(2) 0.005(2) C24 0.065(3) 0.064(3) 0.118(4) 0.014(3) 0.038(3) 0.021(2) C25 0.078(3) 0.054(2) 0.091(3) -0.005(2) 0.037(2) 0.010(2) C26 0.061(2) 0.048(2) 0.072(2) -0.0065(17) 0.0189(19) 0.0002(17) C27 0.0511(18) 0.0433(18) 0.0470(18) -0.0020(14) 0.0143(15) -0.0010(14) C28 0.085(3) 0.046(2) 0.064(2) 0.0041(17) 0.011(2) -0.0089(19) C29 0.102(3) 0.054(2) 0.084(3) 0.007(2) 0.028(3) -0.022(2) C30 0.076(3) 0.060(3) 0.114(4) -0.013(3) 0.031(3) -0.024(2) C31 0.057(2) 0.069(3) 0.099(3) -0.014(3) 0.000(2) -0.014(2) C32 0.065(2) 0.056(2) 0.062(2) -0.0022(18) 0.0060(19) -0.0076(18) C33 0.101(3) 0.052(2) 0.076(3) 0.0048(18) 0.056(3) 0.011(2) C34 0.169(6) 0.094(4) 0.094(4) 0.012(3) 0.094(4) 0.021(4) C35 0.189(7) 0.103(4) 0.063(3) 0.006(3) 0.071(4) 0.024(4) C36 0.158(5) 0.074(3) 0.040(2) 0.0028(19) 0.017(3) 0.018(3) C37 0.222(9) 0.116(5) 0.054(3) -0.001(3) 0.001(5) 0.044(6) C38 0.170(7) 0.134(5) 0.058(4) -0.011(3) -0.049(4) 0.031(5) C39 0.097(4) 0.094(4) 0.083(4) -0.007(3) -0.031(3) 0.016(3) C40 0.107(5) 0.141(6) 0.107(5) -0.008(4) -0.051(4) -0.006(4) C41 0.054(3) 0.126(5) 0.140(6) 0.006(4) -0.009(3) -0.008(3) C42 0.048(2) 0.070(3) 0.089(3) 0.013(2) 0.007(2) -0.0038(18) C43 0.104(3) 0.042(2) 0.042(2) 0.0009(14) 0.021(2) 0.0062(19) C44 0.083(3) 0.048(2) 0.046(2) -0.0020(15) -0.0106(19) -0.0002(18) C45 0.079(3) 0.078(3) 0.125(4) 0.006(3) 0.059(3) 0.008(2) C46 0.060(3) 0.104(4) 0.105(4) 0.020(3) 0.043(3) -0.001(2) B1 0.092(5) 0.086(4) 0.206(9) 0.007(5) 0.092(6) 0.013(4) F1 0.298(9) 0.221(7) 0.487(13) -0.047(8) 0.251(10) 0.004(6) F2 0.482(15) 0.177(7) 0.373(12) 0.050(7) 0.051(12) 0.079(9) F3 0.103(4) 0.220(8) 0.040(3) 0.010(3) -0.023(3) -0.074(5) F3' 0.119(6) 0.281(12) 0.335(13) -0.232(11) 0.054(8) -0.114(8) F4 0.189(4) 0.219(5) 0.127(3) 0.023(3) 0.016(3) -0.041(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.046(3) . ? Cu1 N2 2.076(3) . ? Cu1 P1 2.2368(9) . ? Cu1 P2 2.2382(9) . ? P1 C8 1.821(3) . ? P1 C14 1.826(3) . ? P1 C7 1.857(3) . ? P2 C21 1.821(3) . ? P2 C27 1.828(3) . ? P2 C20 1.852(3) . ? N1 C1 1.439(4) . ? N1 C7 1.456(4) . ? N1 C20 1.464(4) . ? N2 C33 1.338(5) . ? N2 C43 1.348(5) . ? N3 C42 1.327(5) . ? N3 C44 1.364(5) . ? C1 C6 1.387(5) . ? C1 C2 1.389(5) . ? C2 C3 1.375(5) . ? C2 H2A 0.9300 . ? C3 C4 1.358(6) . ? C3 H3A 0.9300 . ? C4 C5 1.349(6) . ? C4 H4A 0.9300 . ? C5 C6 1.389(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.374(5) . ? C8 C13 1.389(5) . ? C9 C10 1.394(5) . ? C9 H9A 0.9300 . ? C10 C11 1.372(7) . ? C10 H10A 0.9300 . ? C11 C12 1.362(6) . ? C11 H11A 0.9300 . ? C12 C13 1.386(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.369(5) . ? C14 C19 1.387(5) . ? C15 C16 1.398(6) . ? C15 H15A 0.9300 . ? C16 C17 1.371(7) . ? C16 H16A 0.9300 . ? C17 C18 1.355(7) . ? C17 H17A 0.9300 . ? C18 C19 1.382(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.374(5) . ? C21 C26 1.388(5) . ? C22 C23 1.395(6) . ? C22 H22A 0.9300 . ? C23 C24 1.382(7) . ? C23 H23A 0.9300 . ? C24 C25 1.357(6) . ? C24 H24A 0.9300 . ? C25 C26 1.392(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C32 1.382(5) . ? C27 C28 1.389(5) . ? C28 C29 1.381(5) . ? C28 H28A 0.9300 . ? C29 C30 1.355(6) . ? C29 H29A 0.9300 . ? C30 C31 1.360(6) . ? C30 H30A 0.9300 . ? C31 C32 1.391(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.398(7) . ? C33 C45 1.496(7) . ? C34 C35 1.342(9) . ? C34 H34A 0.9300 . ? C35 C36 1.400(9) . ? C35 H35A 0.9300 . ? C36 C37 1.394(9) . ? C36 C43 1.408(6) . ? C37 C38 1.311(11) . ? C37 H37A 0.9300 . ? C38 C39 1.464(9) . ? C38 H38A 0.9300 . ? C39 C40 1.353(9) . ? C39 C44 1.410(6) . ? C40 C41 1.347(9) . ? C40 H40A 0.9300 . ? C41 C42 1.419(7) . ? C41 H41A 0.9300 . ? C42 C46 1.492(6) . ? C43 C44 1.432(6) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? B1 F2 1.179(10) . ? B1 F1 1.188(8) . ? B1 F3' 1.301(11) . ? B1 F3 1.344(11) . ? B1 F4 1.355(8) . ? F2 F3' 1.267(14) . ? F2 F3 1.740(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 81.68(12) . . ? N3 Cu1 P1 121.65(8) . . ? N2 Cu1 P1 121.30(8) . . ? N3 Cu1 P2 115.61(8) . . ? N2 Cu1 P2 117.16(8) . . ? P1 Cu1 P2 100.39(4) . . ? C8 P1 C14 101.21(15) . . ? C8 P1 C7 99.04(15) . . ? C14 P1 C7 104.31(16) . . ? C8 P1 Cu1 120.49(12) . . ? C14 P1 Cu1 116.47(10) . . ? C7 P1 Cu1 112.77(12) . . ? C21 P2 C27 105.49(15) . . ? C21 P2 C20 106.42(16) . . ? C27 P2 C20 99.39(15) . . ? C21 P2 Cu1 112.67(10) . . ? C27 P2 Cu1 120.96(12) . . ? C20 P2 Cu1 110.36(11) . . ? C1 N1 C7 115.9(3) . . ? C1 N1 C20 112.8(3) . . ? C7 N1 C20 114.7(3) . . ? C33 N2 C43 118.4(3) . . ? C33 N2 Cu1 130.2(3) . . ? C43 N2 Cu1 111.3(2) . . ? C42 N3 C44 118.7(3) . . ? C42 N3 Cu1 129.9(3) . . ? C44 N3 Cu1 111.4(2) . . ? C6 C1 C2 117.6(3) . . ? C6 C1 N1 123.0(3) . . ? C2 C1 N1 119.3(3) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 119.4(4) . . ? C1 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? N1 C7 P1 116.3(2) . . ? N1 C7 H7A 108.2 . . ? P1 C7 H7A 108.2 . . ? N1 C7 H7B 108.2 . . ? P1 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C13 119.1(3) . . ? C9 C8 P1 119.2(3) . . ? C13 C8 P1 121.7(3) . . ? C8 C9 C10 120.8(4) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 118.7(4) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C12 C11 C10 121.6(4) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C12 C13 C8 120.3(4) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? C15 C14 C19 119.1(3) . . ? C15 C14 P1 117.7(3) . . ? C19 C14 P1 123.0(3) . . ? C14 C15 C16 120.8(4) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C18 C17 C16 119.8(4) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 121.6(5) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C18 C19 C14 119.2(4) . . ? C18 C19 H19A 120.4 . . ? C14 C19 H19A 120.4 . . ? N1 C20 P2 117.0(2) . . ? N1 C20 H20A 108.0 . . ? P2 C20 H20A 108.0 . . ? N1 C20 H20B 108.0 . . ? P2 C20 H20B 108.0 . . ? H20A C20 H20B 107.3 . . ? C22 C21 C26 118.8(3) . . ? C22 C21 P2 121.7(3) . . ? C26 C21 P2 118.5(3) . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C21 C26 C25 120.7(4) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C32 C27 C28 118.2(3) . . ? C32 C27 P2 119.2(3) . . ? C28 C27 P2 122.5(3) . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 120.7(4) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C27 C32 C31 120.5(4) . . ? C27 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? N2 C33 C34 121.4(5) . . ? N2 C33 C45 118.8(4) . . ? C34 C33 C45 119.8(5) . . ? C35 C34 C33 120.5(6) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 120.0(5) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C37 C36 C35 123.5(5) . . ? C37 C36 C43 119.7(6) . . ? C35 C36 C43 116.8(5) . . ? C38 C37 C36 121.8(6) . . ? C38 C37 H37A 119.1 . . ? C36 C37 H37A 119.1 . . ? C37 C38 C39 122.2(6) . . ? C37 C38 H38A 118.9 . . ? C39 C38 H38A 118.9 . . ? C40 C39 C44 117.3(5) . . ? C40 C39 C38 125.6(6) . . ? C44 C39 C38 117.0(6) . . ? C41 C40 C39 121.6(5) . . ? C41 C40 H40A 119.2 . . ? C39 C40 H40A 119.2 . . ? C40 C41 C42 119.4(6) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? N3 C42 C41 120.8(5) . . ? N3 C42 C46 117.9(4) . . ? C41 C42 C46 121.3(4) . . ? N2 C43 C36 123.0(4) . . ? N2 C43 C44 117.5(3) . . ? C36 C43 C44 119.6(5) . . ? N3 C44 C39 122.2(5) . . ? N3 C44 C43 118.1(3) . . ? C39 C44 C43 119.7(4) . . ? C33 C45 H45A 109.5 . . ? C33 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C33 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F2 B1 F1 145.6(10) . . ? F2 B1 F3' 61.2(9) . . ? F1 B1 F3' 94.1(8) . . ? F2 B1 F3 86.9(9) . . ? F1 B1 F3 94.2(9) . . ? F3' B1 F3 131.5(11) . . ? F2 B1 F4 103.0(8) . . ? F1 B1 F4 109.1(8) . . ? F3' B1 F4 113.2(11) . . ? F3 B1 F4 108.7(6) . . ? B1 F2 F3' 64.2(8) . . ? B1 F2 F3 50.5(8) . . ? F3' F2 F3 105.6(9) . . ? B1 F3 F2 42.6(4) . . ? F2 F3' B1 54.6(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.011 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.061 # Attachment '- 2a.CIF' data_2a _database_code_depnum_ccdc_archive 'CCDC 815813' #TrackingRef '- 2a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H68 B2 Cu2 F8 N6 O0 P4' _chemical_formula_weight 1562.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4138(3) _cell_length_b 18.5980(7) _cell_length_c 22.5631(8) _cell_angle_alpha 72.718(3) _cell_angle_beta 89.843(3) _cell_angle_gamma 85.223(3) _cell_volume 3757.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8036 _cell_measurement_theta_min 2.7169 _cell_measurement_theta_max 62.5124 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 2.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5749 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19086 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 62.60 _reflns_number_total 11681 _reflns_number_gt 8267 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0650P)^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 11681 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.68009(4) -0.01701(2) 0.194554(18) 0.02912(11) Uani 1 1 d . . . Cu2 Cu -0.14187(4) 0.49699(2) 0.319413(17) 0.02793(11) Uani 1 1 d . . . P1 P 0.44427(7) -0.00992(4) 0.21072(3) 0.02861(16) Uani 1 1 d . . . P2 P 0.74048(7) 0.09091(4) 0.20713(3) 0.02715(15) Uani 1 1 d . . . P3 P 0.09287(7) 0.48808(4) 0.30548(3) 0.02663(15) Uani 1 1 d . . . P4 P -0.20469(7) 0.38631(4) 0.31431(3) 0.02613(15) Uani 1 1 d . . . N1 N 0.4582(2) 0.13307(12) 0.22454(10) 0.0268(5) Uani 1 1 d . . . N2 N 0.0768(2) 0.34288(12) 0.29636(10) 0.0274(5) Uani 1 1 d . . . N3 N 0.8067(2) -0.11627(13) 0.23365(11) 0.0319(5) Uani 1 1 d . . . N4 N 0.7172(2) -0.04842(12) 0.11554(10) 0.0271(5) Uani 1 1 d . . . N5 N -0.2017(2) 0.54966(13) 0.38384(11) 0.0328(5) Uani 1 1 d . . . N6 N -0.2602(3) 0.58774(14) 0.26120(12) 0.0381(6) Uani 1 1 d . . . C1 C 0.3651(3) 0.18746(15) 0.24287(12) 0.0253(5) Uani 1 1 d . . . C2 C 0.2697(3) 0.16136(15) 0.28952(13) 0.0294(6) Uani 1 1 d . . . H2A H 0.2706 0.1097 0.3091 0.035 Uiso 1 1 calc R . . C3 C 0.1726(3) 0.21062(15) 0.30780(13) 0.0285(6) Uani 1 1 d . . . H3A H 0.1095 0.1920 0.3393 0.034 Uiso 1 1 calc R . . C4 C 0.1701(3) 0.28790(15) 0.27872(12) 0.0262(5) Uani 1 1 d . . . C5 C 0.2663(3) 0.31426(15) 0.23187(13) 0.0297(6) Uani 1 1 d . . . H5A H 0.2656 0.3659 0.2123 0.036 Uiso 1 1 calc R . . C6 C 0.3627(3) 0.26499(15) 0.21394(13) 0.0289(6) Uani 1 1 d . . . H6A H 0.4262 0.2836 0.1825 0.035 Uiso 1 1 calc R . . C7 C 0.3779(3) 0.09074(15) 0.19236(13) 0.0294(6) Uani 1 1 d . . . H7A H 0.3828 0.1142 0.1479 0.035 Uiso 1 1 calc R . . H7B H 0.2786 0.0941 0.2036 0.035 Uiso 1 1 calc R . . C8 C 0.3897(3) -0.05040(16) 0.29055(14) 0.0348(6) Uani 1 1 d . . . C9 C 0.4723(4) -0.03962(19) 0.33752(15) 0.0458(8) Uani 1 1 d . . . H9A H 0.5535 -0.0136 0.3276 0.055 Uiso 1 1 calc R . . C10 C 0.4354(4) -0.0671(2) 0.39872(17) 0.0592(9) Uani 1 1 d . . . H10A H 0.4903 -0.0582 0.4296 0.071 Uiso 1 1 calc R . . C11 C 0.3175(4) -0.1077(2) 0.41451(16) 0.0545(9) Uani 1 1 d . . . H11A H 0.2924 -0.1258 0.4559 0.065 Uiso 1 1 calc R . . C12 C 0.2373(4) -0.1211(2) 0.36848(16) 0.0508(9) Uani 1 1 d . . . H12A H 0.1598 -0.1499 0.3790 0.061 Uiso 1 1 calc R . . C13 C 0.2716(3) -0.09202(18) 0.30682(15) 0.0422(7) Uani 1 1 d . . . H13A H 0.2155 -0.1003 0.2760 0.051 Uiso 1 1 calc R . . C14 C 0.3212(3) -0.04099(16) 0.16284(13) 0.0318(6) Uani 1 1 d . . . C15 C 0.3712(3) -0.09724(16) 0.13699(14) 0.0353(6) Uani 1 1 d . . . H15A H 0.4646 -0.1186 0.1454 0.042 Uiso 1 1 calc R . . C16 C 0.2841(3) -0.12223(17) 0.09878(15) 0.0428(7) Uani 1 1 d . . . H16A H 0.3185 -0.1604 0.0823 0.051 Uiso 1 1 calc R . . C17 C 0.1464(4) -0.08988(19) 0.08573(17) 0.0473(8) Uani 1 1 d . . . H17A H 0.0877 -0.1064 0.0603 0.057 Uiso 1 1 calc R . . C18 C 0.0944(3) -0.03300(19) 0.11011(16) 0.0457(8) Uani 1 1 d . . . H18A H 0.0018 -0.0109 0.1004 0.055 Uiso 1 1 calc R . . C19 C 0.1801(3) -0.00911(17) 0.14880(15) 0.0392(7) Uani 1 1 d . . . H19A H 0.1442 0.0284 0.1657 0.047 Uiso 1 1 calc R . . C20 C 0.5857(3) 0.16242(15) 0.19169(13) 0.0272(6) Uani 1 1 d . . . H20A H 0.6103 0.2055 0.2043 0.033 Uiso 1 1 calc R . . H20B H 0.5645 0.1799 0.1474 0.033 Uiso 1 1 calc R . . C21 C 0.8036(3) 0.08623(16) 0.28455(13) 0.0312(6) Uani 1 1 d . . . C22 C 0.7404(3) 0.12864(17) 0.32030(14) 0.0374(7) Uani 1 1 d . . . H22A H 0.6607 0.1619 0.3046 0.045 Uiso 1 1 calc R . . C23 C 0.7942(4) 0.12234(19) 0.37907(15) 0.0454(8) Uani 1 1 d . . . H23A H 0.7511 0.1516 0.4023 0.055 Uiso 1 1 calc R . . C24 C 0.9113(4) 0.0728(2) 0.40290(15) 0.0488(8) Uani 1 1 d . . . H24A H 0.9471 0.0682 0.4424 0.059 Uiso 1 1 calc R . . C25 C 0.9757(4) 0.0298(2) 0.36816(17) 0.0538(9) Uani 1 1 d . . . H25A H 1.0552 -0.0035 0.3842 0.065 Uiso 1 1 calc R . . C26 C 0.9226(3) 0.03601(18) 0.30965(16) 0.0437(7) Uani 1 1 d . . . H26A H 0.9662 0.0066 0.2867 0.052 Uiso 1 1 calc R . . C27 C 0.8647(3) 0.14658(15) 0.15395(13) 0.0295(6) Uani 1 1 d . . . C28 C 0.9764(3) 0.18020(16) 0.17279(14) 0.0345(6) Uani 1 1 d . . . H28A H 0.9943 0.1722 0.2149 0.041 Uiso 1 1 calc R . . C29 C 1.0610(3) 0.22551(18) 0.12904(15) 0.0408(7) Uani 1 1 d . . . H29A H 1.1355 0.2475 0.1420 0.049 Uiso 1 1 calc R . . C30 C 1.0354(3) 0.23806(19) 0.06681(16) 0.0450(8) Uani 1 1 d . . . H30A H 1.0929 0.2680 0.0377 0.054 Uiso 1 1 calc R . . C31 C 0.9229(4) 0.2057(2) 0.04733(15) 0.0495(8) Uani 1 1 d . . . H31A H 0.9034 0.2151 0.0052 0.059 Uiso 1 1 calc R . . C32 C 0.8405(3) 0.15958(19) 0.09081(14) 0.0403(7) Uani 1 1 d . . . H32A H 0.7675 0.1368 0.0776 0.048 Uiso 1 1 calc R . . C33 C 0.1577(3) 0.38709(15) 0.32699(13) 0.0290(6) Uani 1 1 d . . . H33A H 0.2572 0.3828 0.3162 0.035 Uiso 1 1 calc R . . H33B H 0.1521 0.3655 0.3716 0.035 Uiso 1 1 calc R . . C34 C 0.2141(3) 0.52215(15) 0.35211(13) 0.0296(6) Uani 1 1 d . . . C35 C 0.1614(3) 0.57910(15) 0.37691(13) 0.0325(6) Uani 1 1 d . . . H35A H 0.0679 0.6001 0.3678 0.039 Uiso 1 1 calc R . . C36 C 0.2469(3) 0.60499(17) 0.41510(15) 0.0407(7) Uani 1 1 d . . . H36A H 0.2115 0.6439 0.4305 0.049 Uiso 1 1 calc R . . C37 C 0.3842(3) 0.57275(18) 0.42993(15) 0.0423(7) Uani 1 1 d . . . H37A H 0.4409 0.5893 0.4561 0.051 Uiso 1 1 calc R . . C38 C 0.4383(3) 0.51577(18) 0.40605(15) 0.0423(7) Uani 1 1 d . . . H38A H 0.5311 0.4942 0.4162 0.051 Uiso 1 1 calc R . . C39 C 0.3542(3) 0.49088(17) 0.36700(14) 0.0355(6) Uani 1 1 d . . . H39A H 0.3914 0.4531 0.3506 0.043 Uiso 1 1 calc R . . C40 C 0.1446(3) 0.52842(16) 0.22508(13) 0.0325(6) Uani 1 1 d . . . C41 C 0.2472(3) 0.57977(17) 0.20696(15) 0.0385(7) Uani 1 1 d . . . H41A H 0.3002 0.5918 0.2369 0.046 Uiso 1 1 calc R . . C42 C 0.2711(4) 0.6133(2) 0.14434(16) 0.0493(8) Uani 1 1 d . . . H42A H 0.3388 0.6483 0.1326 0.059 Uiso 1 1 calc R . . C43 C 0.1954(4) 0.5951(2) 0.09968(16) 0.0532(9) Uani 1 1 d . . . H43A H 0.2117 0.6176 0.0579 0.064 Uiso 1 1 calc R . . C44 C 0.0962(4) 0.5437(2) 0.11684(16) 0.0568(9) Uani 1 1 d . . . H44A H 0.0465 0.5306 0.0865 0.068 Uiso 1 1 calc R . . C45 C 0.0685(4) 0.5107(2) 0.17902(15) 0.0462(8) Uani 1 1 d . . . H45A H -0.0009 0.4767 0.1900 0.055 Uiso 1 1 calc R . . C46 C -0.0511(3) 0.31446(15) 0.32925(13) 0.0293(6) Uani 1 1 d . . . H46A H -0.0295 0.2968 0.3735 0.035 Uiso 1 1 calc R . . H46B H -0.0768 0.2716 0.3167 0.035 Uiso 1 1 calc R . . C47 C -0.2747(3) 0.39070(15) 0.23788(13) 0.0293(6) Uani 1 1 d . . . C48 C -0.2084(3) 0.35189(17) 0.19973(13) 0.0354(6) Uani 1 1 d . . . H48A H -0.1243 0.3214 0.2131 0.042 Uiso 1 1 calc R . . C49 C -0.2680(4) 0.35868(19) 0.14169(15) 0.0437(7) Uani 1 1 d . . . H49A H -0.2238 0.3322 0.1166 0.052 Uiso 1 1 calc R . . C50 C -0.3916(4) 0.40416(19) 0.12111(15) 0.0457(8) Uani 1 1 d . . . H50A H -0.4305 0.4087 0.0822 0.055 Uiso 1 1 calc R . . C51 C -0.4583(3) 0.44333(18) 0.15864(15) 0.0416(7) Uani 1 1 d . . . H51A H -0.5424 0.4738 0.1449 0.050 Uiso 1 1 calc R . . C52 C -0.4000(3) 0.43716(17) 0.21632(14) 0.0355(6) Uani 1 1 d . . . H52A H -0.4445 0.4641 0.2410 0.043 Uiso 1 1 calc R . . C53 C -0.3309(3) 0.33368(15) 0.36834(13) 0.0279(6) Uani 1 1 d . . . C54 C -0.3112(3) 0.32641(17) 0.43104(13) 0.0356(6) Uani 1 1 d . . . H54A H -0.2392 0.3505 0.4435 0.043 Uiso 1 1 calc R . . C55 C -0.3974(4) 0.28392(18) 0.47491(15) 0.0428(7) Uani 1 1 d . . . H55A H -0.3821 0.2788 0.5167 0.051 Uiso 1 1 calc R . . C56 C -0.5069(3) 0.24876(17) 0.45688(15) 0.0397(7) Uani 1 1 d . . . H56A H -0.5655 0.2204 0.4865 0.048 Uiso 1 1 calc R . . C57 C -0.5282(3) 0.25627(17) 0.39477(15) 0.0387(7) Uani 1 1 d . . . H57A H -0.6020 0.2332 0.3824 0.046 Uiso 1 1 calc R . . C58 C -0.4405(3) 0.29790(16) 0.35080(14) 0.0319(6) Uani 1 1 d . . . H58A H -0.4548 0.3020 0.3091 0.038 Uiso 1 1 calc R . . C59 C 0.8559(3) -0.14821(18) 0.29147(14) 0.0394(7) Uani 1 1 d . . . H59A H 0.8318 -0.1243 0.3214 0.047 Uiso 1 1 calc R . . C60 C 0.9426(3) -0.21655(19) 0.30921(15) 0.0438(7) Uani 1 1 d . . . H60A H 0.9768 -0.2366 0.3499 0.053 Uiso 1 1 calc R . . C61 C 0.9765(3) -0.25339(19) 0.26643(15) 0.0440(7) Uani 1 1 d . . . H61A H 1.0348 -0.2984 0.2778 0.053 Uiso 1 1 calc R . . C62 C 0.9232(3) -0.22323(16) 0.20527(14) 0.0349(6) Uani 1 1 d . . . C63 C 0.9454(3) -0.25983(17) 0.15850(15) 0.0403(7) Uani 1 1 d . . . H63A H 1.0020 -0.3054 0.1677 0.048 Uiso 1 1 calc R . . C64 C 0.8865(3) -0.23015(16) 0.10116(14) 0.0382(7) Uani 1 1 d . . . H64A H 0.8974 -0.2570 0.0724 0.046 Uiso 1 1 calc R . . C65 C 0.8073(3) -0.15761(16) 0.08419(13) 0.0322(6) Uani 1 1 d . . . C66 C 0.7507(3) -0.12187(18) 0.02437(14) 0.0380(7) Uani 1 1 d . . . H66A H 0.7599 -0.1460 -0.0062 0.046 Uiso 1 1 calc R . . C67 C 0.6823(3) -0.05148(18) 0.01146(13) 0.0367(7) Uani 1 1 d . . . H67A H 0.6445 -0.0272 -0.0282 0.044 Uiso 1 1 calc R . . C68 C 0.6689(3) -0.01587(16) 0.05776(13) 0.0317(6) Uani 1 1 d . . . H68A H 0.6242 0.0329 0.0477 0.038 Uiso 1 1 calc R . . C69 C 0.7865(3) -0.11860(15) 0.12877(12) 0.0271(6) Uani 1 1 d . . . C70 C 0.8399(3) -0.15310(15) 0.19107(13) 0.0290(6) Uani 1 1 d . . . C71 C -0.1652(3) 0.5326(2) 0.44304(15) 0.0428(7) Uani 1 1 d . . . H71A H -0.1152 0.4862 0.4621 0.051 Uiso 1 1 calc R . . C72 C -0.1994(4) 0.5821(3) 0.47851(18) 0.0589(10) Uani 1 1 d . . . H72A H -0.1705 0.5692 0.5200 0.071 Uiso 1 1 calc R . . C73 C -0.2759(4) 0.6496(2) 0.4509(2) 0.0647(12) Uani 1 1 d . . . H73A H -0.2977 0.6833 0.4735 0.078 Uiso 1 1 calc R . . C74 C -0.3213(4) 0.66834(19) 0.3894(2) 0.0559(10) Uani 1 1 d . . . C75 C -0.4107(4) 0.7370(2) 0.3564(3) 0.0738(15) Uani 1 1 d . . . H75A H -0.4395 0.7723 0.3769 0.089 Uiso 1 1 calc R . . C76 C -0.4517(5) 0.7495(2) 0.2965(3) 0.0774(14) Uani 1 1 d . . . H76A H -0.5124 0.7922 0.2773 0.093 Uiso 1 1 calc R . . C77 C -0.4064(4) 0.7008(2) 0.2625(2) 0.0617(11) Uani 1 1 d . . . C78 C -0.4373(4) 0.7116(2) 0.1984(2) 0.0675(12) Uani 1 1 d . . . H78A H -0.4995 0.7525 0.1769 0.081 Uiso 1 1 calc R . . C79 C -0.3791(4) 0.6643(2) 0.1679(2) 0.0680(12) Uani 1 1 d . . . H79A H -0.3986 0.6730 0.1259 0.082 Uiso 1 1 calc R . . C80 C -0.2909(4) 0.6034(2) 0.20057(17) 0.0528(9) Uani 1 1 d . . . H80A H -0.2499 0.5711 0.1795 0.063 Uiso 1 1 calc R . . C81 C -0.3155(3) 0.63473(17) 0.29215(17) 0.0428(8) Uani 1 1 d . . . C82 C -0.2785(3) 0.61752(17) 0.35673(17) 0.0402(7) Uani 1 1 d . . . F1 F 0.5721(3) 0.25478(16) -0.04125(12) 0.0872(8) Uani 1 1 d . . . F2 F 0.5428(4) 0.28683(16) 0.04507(15) 0.1090(11) Uani 1 1 d . . . F3 F 0.3520(3) 0.27410(15) -0.01041(14) 0.0813(7) Uani 1 1 d . . . F4 F 0.4988(3) 0.17014(12) 0.04229(10) 0.0647(6) Uani 1 1 d . . . B1 B 0.4897(4) 0.2481(2) 0.00908(17) 0.0463(9) Uani 1 1 d . . . F5 F 0.1280(3) 0.2582(2) 0.46478(11) 0.1055(11) Uani 1 1 d . . . F6 F -0.0345(3) 0.1765(2) 0.49607(15) 0.1005(9) Uani 1 1 d . . . F7 F 0.1490(4) 0.18363(17) 0.56063(12) 0.0929(8) Uani 1 1 d . . . F8 F -0.0342(3) 0.27077(18) 0.53652(14) 0.0927(9) Uani 1 1 d . . . B2 B 0.0507(5) 0.2234(3) 0.51292(18) 0.0538(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0248(2) 0.0318(2) 0.0345(2) -0.01664(17) 0.00075(16) 0.00192(16) Cu2 0.0239(2) 0.0293(2) 0.0329(2) -0.01403(17) -0.00208(16) 0.00221(16) P1 0.0236(3) 0.0296(4) 0.0361(4) -0.0158(3) 0.0024(3) -0.0001(3) P2 0.0200(3) 0.0321(4) 0.0342(4) -0.0180(3) 0.0008(3) 0.0006(3) P3 0.0215(3) 0.0282(3) 0.0329(4) -0.0139(3) -0.0014(3) 0.0009(3) P4 0.0197(3) 0.0304(3) 0.0326(4) -0.0167(3) 0.0001(3) 0.0006(3) N1 0.0197(10) 0.0297(11) 0.0354(12) -0.0170(10) 0.0023(9) -0.0009(9) N2 0.0186(10) 0.0287(11) 0.0389(13) -0.0168(10) 0.0015(9) 0.0001(9) N3 0.0271(11) 0.0364(13) 0.0329(13) -0.0115(10) -0.0011(10) -0.0012(10) N4 0.0208(10) 0.0291(12) 0.0314(12) -0.0102(10) -0.0027(9) 0.0018(9) N5 0.0234(11) 0.0351(13) 0.0439(15) -0.0183(11) 0.0021(10) -0.0008(10) N6 0.0297(12) 0.0351(13) 0.0453(15) -0.0053(11) -0.0098(11) -0.0031(11) C1 0.0193(12) 0.0290(14) 0.0308(14) -0.0148(11) -0.0025(10) 0.0019(11) C2 0.0257(13) 0.0280(13) 0.0351(15) -0.0111(11) -0.0001(11) 0.0007(11) C3 0.0216(13) 0.0325(14) 0.0329(14) -0.0123(12) 0.0017(11) -0.0006(11) C4 0.0177(12) 0.0318(14) 0.0335(14) -0.0170(12) -0.0030(11) 0.0006(11) C5 0.0245(13) 0.0278(14) 0.0379(15) -0.0117(12) 0.0027(11) -0.0010(11) C6 0.0221(13) 0.0332(15) 0.0325(14) -0.0123(12) 0.0023(11) 0.0000(11) C7 0.0241(13) 0.0314(14) 0.0369(15) -0.0173(12) -0.0007(11) -0.0005(11) C8 0.0345(15) 0.0291(14) 0.0413(16) -0.0128(12) 0.0039(13) 0.0028(12) C9 0.0447(18) 0.0491(18) 0.0409(18) -0.0086(15) -0.0036(14) -0.0073(15) C10 0.068(2) 0.067(2) 0.0393(19) -0.0114(17) -0.0052(17) -0.004(2) C11 0.057(2) 0.056(2) 0.0407(19) -0.0033(16) 0.0086(17) 0.0100(18) C12 0.0457(19) 0.0476(19) 0.052(2) -0.0044(16) 0.0160(16) -0.0024(16) C13 0.0340(16) 0.0450(18) 0.0486(18) -0.0157(15) 0.0073(14) -0.0027(14) C14 0.0272(14) 0.0328(14) 0.0383(15) -0.0146(12) 0.0040(12) -0.0047(12) C15 0.0325(15) 0.0313(15) 0.0449(17) -0.0154(13) 0.0019(13) -0.0035(12) C16 0.0462(19) 0.0362(16) 0.0520(19) -0.0214(15) -0.0007(15) -0.0070(14) C17 0.0415(18) 0.0481(19) 0.059(2) -0.0239(16) -0.0037(15) -0.0135(15) C18 0.0286(15) 0.0499(19) 0.064(2) -0.0239(16) -0.0040(14) -0.0063(14) C19 0.0284(15) 0.0407(16) 0.0548(19) -0.0233(15) 0.0042(13) -0.0051(13) C20 0.0204(12) 0.0305(14) 0.0326(14) -0.0132(11) -0.0002(11) 0.0017(11) C21 0.0266(14) 0.0339(15) 0.0362(15) -0.0152(12) -0.0009(12) -0.0028(12) C22 0.0371(16) 0.0411(16) 0.0369(16) -0.0180(13) -0.0018(13) 0.0049(13) C23 0.0511(19) 0.0518(19) 0.0368(17) -0.0204(15) -0.0023(15) 0.0032(16) C24 0.059(2) 0.0514(19) 0.0371(17) -0.0159(15) -0.0125(15) 0.0006(17) C25 0.054(2) 0.054(2) 0.053(2) -0.0199(17) -0.0241(17) 0.0140(17) C26 0.0406(17) 0.0429(17) 0.0509(19) -0.0226(15) -0.0072(14) 0.0098(14) C27 0.0217(13) 0.0333(14) 0.0382(15) -0.0189(12) 0.0017(11) 0.0015(11) C28 0.0261(14) 0.0402(16) 0.0423(16) -0.0204(13) -0.0021(12) -0.0017(12) C29 0.0267(14) 0.0451(17) 0.058(2) -0.0249(15) 0.0014(14) -0.0067(13) C30 0.0364(16) 0.0513(19) 0.054(2) -0.0241(16) 0.0153(15) -0.0131(15) C31 0.0521(19) 0.067(2) 0.0391(17) -0.0269(16) 0.0106(15) -0.0198(17) C32 0.0351(15) 0.0555(19) 0.0411(17) -0.0278(15) 0.0056(13) -0.0154(14) C33 0.0227(13) 0.0327(14) 0.0364(15) -0.0180(12) -0.0024(11) -0.0015(11) C34 0.0247(13) 0.0310(14) 0.0357(15) -0.0137(12) 0.0002(11) -0.0032(11) C35 0.0298(14) 0.0300(14) 0.0396(16) -0.0138(12) -0.0034(12) -0.0003(12) C36 0.0453(18) 0.0363(16) 0.0467(18) -0.0213(14) -0.0023(14) -0.0056(14) C37 0.0395(17) 0.0481(18) 0.0455(18) -0.0215(15) -0.0058(14) -0.0115(15) C38 0.0278(15) 0.0470(18) 0.0544(19) -0.0183(15) -0.0075(14) -0.0041(14) C39 0.0272(14) 0.0371(15) 0.0464(17) -0.0190(13) 0.0013(12) -0.0027(12) C40 0.0311(14) 0.0304(14) 0.0348(15) -0.0101(12) 0.0000(12) 0.0057(12) C41 0.0287(14) 0.0425(16) 0.0433(17) -0.0116(14) 0.0022(13) -0.0015(13) C42 0.0381(17) 0.0503(19) 0.051(2) -0.0025(16) 0.0095(15) -0.0017(15) C43 0.050(2) 0.064(2) 0.0362(18) -0.0034(16) 0.0055(15) 0.0066(18) C44 0.065(2) 0.070(2) 0.0347(18) -0.0149(17) -0.0039(16) -0.006(2) C45 0.0472(18) 0.056(2) 0.0370(17) -0.0148(15) -0.0038(14) -0.0093(16) C46 0.0221(13) 0.0345(14) 0.0353(15) -0.0169(12) 0.0004(11) -0.0023(11) C47 0.0244(13) 0.0311(14) 0.0354(15) -0.0144(12) -0.0005(11) -0.0022(11) C48 0.0344(15) 0.0382(16) 0.0367(16) -0.0173(13) -0.0007(12) 0.0020(13) C49 0.0489(19) 0.0509(18) 0.0381(17) -0.0237(15) 0.0036(14) -0.0048(16) C50 0.053(2) 0.0482(18) 0.0373(17) -0.0136(14) -0.0112(15) -0.0075(16) C51 0.0408(17) 0.0399(16) 0.0429(18) -0.0114(14) -0.0146(14) 0.0005(14) C52 0.0304(15) 0.0366(15) 0.0423(17) -0.0174(13) -0.0041(12) 0.0018(13) C53 0.0221(13) 0.0274(13) 0.0370(15) -0.0158(11) -0.0021(11) 0.0044(11) C54 0.0334(15) 0.0416(16) 0.0384(16) -0.0210(13) 0.0020(13) -0.0074(13) C55 0.0513(19) 0.0453(17) 0.0374(16) -0.0197(14) 0.0057(14) -0.0083(15) C56 0.0359(16) 0.0359(16) 0.0474(18) -0.0133(14) 0.0114(14) -0.0011(13) C57 0.0269(14) 0.0363(16) 0.0541(19) -0.0152(14) -0.0033(13) -0.0025(13) C58 0.0247(13) 0.0345(15) 0.0380(15) -0.0144(12) -0.0024(12) 0.0013(12) C59 0.0407(17) 0.0457(18) 0.0307(16) -0.0095(13) -0.0022(13) -0.0054(14) C60 0.0436(17) 0.0459(18) 0.0339(16) -0.0014(14) -0.0102(13) 0.0026(15) C61 0.0410(17) 0.0398(17) 0.0435(18) -0.0033(14) -0.0063(14) 0.0065(14) C62 0.0285(14) 0.0326(15) 0.0400(17) -0.0062(13) 0.0001(12) 0.0003(12) C63 0.0384(16) 0.0313(15) 0.0509(19) -0.0141(14) 0.0061(14) 0.0064(13) C64 0.0420(17) 0.0317(15) 0.0440(18) -0.0179(13) 0.0040(14) 0.0032(13) C65 0.0314(14) 0.0342(15) 0.0334(15) -0.0141(12) 0.0022(12) -0.0010(12) C66 0.0388(16) 0.0458(18) 0.0348(16) -0.0204(14) 0.0012(13) -0.0041(14) C67 0.0354(15) 0.0468(18) 0.0280(15) -0.0117(13) -0.0048(12) -0.0031(14) C68 0.0271(14) 0.0332(15) 0.0328(15) -0.0086(12) -0.0068(11) 0.0039(12) C69 0.0206(12) 0.0283(14) 0.0337(15) -0.0117(11) 0.0006(11) -0.0009(11) C70 0.0235(13) 0.0315(14) 0.0321(15) -0.0096(12) 0.0003(11) -0.0023(12) C71 0.0377(16) 0.058(2) 0.0392(18) -0.0237(15) 0.0053(14) -0.0103(15) C72 0.054(2) 0.085(3) 0.054(2) -0.041(2) 0.0199(18) -0.024(2) C73 0.059(2) 0.065(3) 0.096(3) -0.058(2) 0.038(2) -0.025(2) C74 0.049(2) 0.0403(19) 0.089(3) -0.0352(19) 0.031(2) -0.0112(16) C75 0.055(2) 0.034(2) 0.143(5) -0.042(2) 0.044(3) -0.0046(18) C76 0.055(2) 0.045(2) 0.120(4) -0.009(3) 0.007(3) 0.0041(19) C77 0.0359(18) 0.0340(18) 0.105(3) -0.0062(19) 0.004(2) 0.0024(15) C78 0.049(2) 0.045(2) 0.081(3) 0.023(2) -0.026(2) -0.0027(18) C79 0.053(2) 0.062(3) 0.070(3) 0.009(2) -0.020(2) -0.006(2) C80 0.0425(18) 0.054(2) 0.049(2) 0.0071(16) -0.0162(15) -0.0129(16) C81 0.0238(14) 0.0307(15) 0.066(2) -0.0020(15) -0.0027(14) -0.0023(12) C82 0.0228(14) 0.0310(16) 0.071(2) -0.0217(15) 0.0121(14) -0.0046(13) F1 0.0953(19) 0.0851(17) 0.0657(15) -0.0038(13) 0.0270(14) 0.0112(15) F2 0.156(3) 0.0754(17) 0.107(2) -0.0453(16) -0.065(2) -0.0049(18) F3 0.0525(13) 0.0850(17) 0.106(2) -0.0301(15) -0.0035(13) 0.0002(12) F4 0.0791(15) 0.0562(12) 0.0548(12) -0.0074(10) -0.0178(11) -0.0161(11) B1 0.044(2) 0.062(2) 0.0357(19) -0.0171(18) -0.0010(16) -0.0118(19) F5 0.0877(18) 0.168(3) 0.0468(13) 0.0009(16) -0.0024(13) -0.055(2) F6 0.0945(19) 0.131(2) 0.111(2) -0.081(2) 0.0152(17) -0.0451(18) F7 0.120(2) 0.0955(19) 0.0595(15) -0.0233(14) -0.0252(15) 0.0161(17) F8 0.0802(17) 0.112(2) 0.102(2) -0.0643(18) -0.0219(15) 0.0173(16) B2 0.055(2) 0.076(3) 0.036(2) -0.023(2) 0.0021(18) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 2.055(2) . ? Cu1 N3 2.068(2) . ? Cu1 P2 2.2273(8) . ? Cu1 P1 2.2482(7) . ? Cu2 N5 2.034(2) . ? Cu2 N6 2.047(2) . ? Cu2 P4 2.2235(8) . ? Cu2 P3 2.2306(7) . ? P1 C8 1.825(3) . ? P1 C14 1.825(3) . ? P1 C7 1.847(3) . ? P2 C21 1.822(3) . ? P2 C27 1.826(3) . ? P2 C20 1.849(3) . ? P3 C34 1.826(3) . ? P3 C40 1.827(3) . ? P3 C33 1.845(3) . ? P4 C47 1.825(3) . ? P4 C53 1.826(3) . ? P4 C46 1.845(3) . ? N1 C1 1.436(3) . ? N1 C20 1.467(3) . ? N1 C7 1.469(3) . ? N2 C4 1.437(3) . ? N2 C46 1.465(3) . ? N2 C33 1.476(3) . ? N3 C59 1.329(4) . ? N3 C70 1.358(4) . ? N4 C68 1.327(4) . ? N4 C69 1.359(4) . ? N5 C71 1.317(4) . ? N5 C82 1.372(4) . ? N6 C80 1.338(5) . ? N6 C81 1.344(4) . ? C1 C2 1.384(4) . ? C1 C6 1.393(4) . ? C2 C3 1.388(4) . ? C2 H2A 0.9300 . ? C3 C4 1.390(4) . ? C3 H3A 0.9300 . ? C4 C5 1.392(4) . ? C5 C6 1.381(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.388(5) . ? C8 C13 1.393(4) . ? C9 C10 1.377(5) . ? C9 H9A 0.9300 . ? C10 C11 1.381(6) . ? C10 H10A 0.9300 . ? C11 C12 1.379(6) . ? C11 H11A 0.9300 . ? C12 C13 1.383(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.391(4) . ? C14 C19 1.405(4) . ? C15 C16 1.392(4) . ? C15 H15A 0.9300 . ? C16 C17 1.377(5) . ? C16 H16A 0.9300 . ? C17 C18 1.385(5) . ? C17 H17A 0.9300 . ? C18 C19 1.380(5) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.387(4) . ? C21 C26 1.401(4) . ? C22 C23 1.389(5) . ? C22 H22A 0.9300 . ? C23 C24 1.376(5) . ? C23 H23A 0.9300 . ? C24 C25 1.382(5) . ? C24 H24A 0.9300 . ? C25 C26 1.382(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C32 1.388(4) . ? C27 C28 1.396(4) . ? C28 C29 1.390(4) . ? C28 H28A 0.9300 . ? C29 C30 1.372(5) . ? C29 H29A 0.9300 . ? C30 C31 1.394(5) . ? C30 H30A 0.9300 . ? C31 C32 1.380(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.394(4) . ? C34 C39 1.396(4) . ? C35 C36 1.392(4) . ? C35 H35A 0.9300 . ? C36 C37 1.377(5) . ? C36 H36A 0.9300 . ? C37 C38 1.386(5) . ? C37 H37A 0.9300 . ? C38 C39 1.387(4) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.390(4) . ? C40 C45 1.396(4) . ? C41 C42 1.391(5) . ? C41 H41A 0.9300 . ? C42 C43 1.374(6) . ? C42 H42A 0.9300 . ? C43 C44 1.364(6) . ? C43 H43A 0.9300 . ? C44 C45 1.388(5) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.394(4) . ? C47 C52 1.399(4) . ? C48 C49 1.393(4) . ? C48 H48A 0.9300 . ? C49 C50 1.375(5) . ? C49 H49A 0.9300 . ? C50 C51 1.389(5) . ? C50 H50A 0.9300 . ? C51 C52 1.383(4) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? C53 C58 1.392(4) . ? C53 C54 1.392(4) . ? C54 C55 1.378(4) . ? C54 H54A 0.9300 . ? C55 C56 1.389(5) . ? C55 H55A 0.9300 . ? C56 C57 1.380(5) . ? C56 H56A 0.9300 . ? C57 C58 1.383(4) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 C60 1.403(5) . ? C59 H59A 0.9300 . ? C60 C61 1.363(5) . ? C60 H60A 0.9300 . ? C61 C62 1.403(5) . ? C61 H61A 0.9300 . ? C62 C70 1.415(4) . ? C62 C63 1.422(4) . ? C63 C64 1.347(5) . ? C63 H63A 0.9300 . ? C64 C65 1.432(4) . ? C64 H64A 0.9300 . ? C65 C66 1.400(4) . ? C65 C69 1.409(4) . ? C66 C67 1.359(4) . ? C66 H66A 0.9300 . ? C67 C68 1.394(4) . ? C67 H67A 0.9300 . ? C68 H68A 0.9300 . ? C69 C70 1.433(4) . ? C71 C72 1.407(5) . ? C71 H71A 0.9300 . ? C72 C73 1.368(6) . ? C72 H72A 0.9300 . ? C73 C74 1.385(6) . ? C73 H73A 0.9300 . ? C74 C82 1.396(5) . ? C74 C75 1.468(6) . ? C75 C76 1.354(7) . ? C75 H75A 0.9300 . ? C76 C77 1.393(7) . ? C76 H76A 0.9300 . ? C77 C78 1.426(7) . ? C77 C81 1.424(5) . ? C78 C79 1.350(7) . ? C78 H78A 0.9300 . ? C79 C80 1.366(5) . ? C79 H79A 0.9300 . ? C80 H80A 0.9300 . ? C81 C82 1.433(5) . ? F1 B1 1.354(5) . ? F2 B1 1.356(5) . ? F3 B1 1.371(5) . ? F4 B1 1.416(5) . ? F5 B2 1.336(5) . ? F6 B2 1.364(5) . ? F7 B2 1.407(5) . ? F8 B2 1.363(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N3 81.47(9) . . ? N4 Cu1 P2 124.06(7) . . ? N3 Cu1 P2 119.84(7) . . ? N4 Cu1 P1 109.12(6) . . ? N3 Cu1 P1 120.82(7) . . ? P2 Cu1 P1 101.89(3) . . ? N5 Cu2 N6 82.48(10) . . ? N5 Cu2 P4 127.08(7) . . ? N6 Cu2 P4 113.41(7) . . ? N5 Cu2 P3 113.76(7) . . ? N6 Cu2 P3 117.39(7) . . ? P4 Cu2 P3 102.85(3) . . ? C8 P1 C14 105.49(13) . . ? C8 P1 C7 103.44(12) . . ? C14 P1 C7 100.04(13) . . ? C8 P1 Cu1 116.18(10) . . ? C14 P1 Cu1 120.72(9) . . ? C7 P1 Cu1 108.49(9) . . ? C21 P2 C27 105.29(13) . . ? C21 P2 C20 104.12(12) . . ? C27 P2 C20 98.20(12) . . ? C21 P2 Cu1 116.20(9) . . ? C27 P2 Cu1 119.74(9) . . ? C20 P2 Cu1 110.83(9) . . ? C34 P3 C40 105.50(13) . . ? C34 P3 C33 100.63(12) . . ? C40 P3 C33 105.69(12) . . ? C34 P3 Cu2 120.74(9) . . ? C40 P3 Cu2 114.06(9) . . ? C33 P3 Cu2 108.52(9) . . ? C47 P4 C53 104.23(12) . . ? C47 P4 C46 105.07(12) . . ? C53 P4 C46 99.62(12) . . ? C47 P4 Cu2 112.98(9) . . ? C53 P4 Cu2 121.41(8) . . ? C46 P4 Cu2 111.65(9) . . ? C1 N1 C20 115.2(2) . . ? C1 N1 C7 110.96(19) . . ? C20 N1 C7 113.4(2) . . ? C4 N2 C46 115.6(2) . . ? C4 N2 C33 110.90(19) . . ? C46 N2 C33 114.1(2) . . ? C59 N3 C70 117.7(3) . . ? C59 N3 Cu1 131.0(2) . . ? C70 N3 Cu1 111.25(18) . . ? C68 N4 C69 117.7(2) . . ? C68 N4 Cu1 130.14(18) . . ? C69 N4 Cu1 111.55(17) . . ? C71 N5 C82 118.2(3) . . ? C71 N5 Cu2 130.3(2) . . ? C82 N5 Cu2 111.0(2) . . ? C80 N6 C81 119.2(3) . . ? C80 N6 Cu2 129.7(2) . . ? C81 N6 Cu2 111.1(2) . . ? C2 C1 C6 118.8(2) . . ? C2 C1 N1 118.4(2) . . ? C6 C1 N1 122.8(2) . . ? C1 C2 C3 121.5(2) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 N2 123.2(2) . . ? C5 C4 N2 117.8(2) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? N1 C7 P1 113.52(18) . . ? N1 C7 H7A 108.9 . . ? P1 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? P1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C13 118.5(3) . . ? C9 C8 P1 117.6(2) . . ? C13 C8 P1 123.8(2) . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C12 C13 C8 120.4(3) . . ? C12 C13 H13A 119.8 . . ? C8 C13 H13A 119.8 . . ? C15 C14 C19 118.2(3) . . ? C15 C14 P1 118.3(2) . . ? C19 C14 P1 123.4(2) . . ? C14 C15 C16 121.3(3) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C14 120.5(3) . . ? C18 C19 H19A 119.7 . . ? C14 C19 H19A 119.7 . . ? N1 C20 P2 112.68(18) . . ? N1 C20 H20A 109.1 . . ? P2 C20 H20A 109.1 . . ? N1 C20 H20B 109.1 . . ? P2 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C26 118.1(3) . . ? C22 C21 P2 124.1(2) . . ? C26 C21 P2 117.8(2) . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H26A 119.7 . . ? C21 C26 H26A 119.7 . . ? C32 C27 C28 118.4(3) . . ? C32 C27 P2 117.5(2) . . ? C28 C27 P2 124.0(2) . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.7(3) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C27 121.2(3) . . ? C31 C32 H32A 119.4 . . ? C27 C32 H32A 119.4 . . ? N2 C33 P3 113.50(18) . . ? N2 C33 H33A 108.9 . . ? P3 C33 H33A 108.9 . . ? N2 C33 H33B 108.9 . . ? P3 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C39 118.6(3) . . ? C35 C34 P3 118.3(2) . . ? C39 C34 P3 123.1(2) . . ? C36 C35 C34 120.9(3) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C37 C36 C35 119.7(3) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C38 C39 C34 120.4(3) . . ? C38 C39 H39A 119.8 . . ? C34 C39 H39A 119.8 . . ? C41 C40 C45 118.4(3) . . ? C41 C40 P3 123.9(2) . . ? C45 C40 P3 117.5(2) . . ? C40 C41 C42 120.4(3) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C44 C43 C42 119.8(3) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C43 C44 C45 120.8(3) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C44 C45 C40 120.2(3) . . ? C44 C45 H45A 119.9 . . ? C40 C45 H45A 119.9 . . ? N2 C46 P4 113.07(19) . . ? N2 C46 H46A 109.0 . . ? P4 C46 H46A 109.0 . . ? N2 C46 H46B 109.0 . . ? P4 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C48 C47 C52 118.8(3) . . ? C48 C47 P4 123.5(2) . . ? C52 C47 P4 117.6(2) . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48A 119.9 . . ? C47 C48 H48A 119.9 . . ? C50 C49 C48 120.6(3) . . ? C50 C49 H49A 119.7 . . ? C48 C49 H49A 119.7 . . ? C49 C50 C51 119.8(3) . . ? C49 C50 H50A 120.1 . . ? C51 C50 H50A 120.1 . . ? C52 C51 C50 120.2(3) . . ? C52 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? C51 C52 C47 120.5(3) . . ? C51 C52 H52A 119.7 . . ? C47 C52 H52A 119.7 . . ? C58 C53 C54 118.6(3) . . ? C58 C53 P4 123.9(2) . . ? C54 C53 P4 117.4(2) . . ? C55 C54 C53 120.7(3) . . ? C55 C54 H54A 119.7 . . ? C53 C54 H54A 119.7 . . ? C54 C55 C56 120.2(3) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C57 C56 C55 119.5(3) . . ? C57 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? C56 C57 C58 120.3(3) . . ? C56 C57 H57A 119.8 . . ? C58 C57 H57A 119.8 . . ? C57 C58 C53 120.6(3) . . ? C57 C58 H58A 119.7 . . ? C53 C58 H58A 119.7 . . ? N3 C59 C60 122.6(3) . . ? N3 C59 H59A 118.7 . . ? C60 C59 H59A 118.7 . . ? C61 C60 C59 119.6(3) . . ? C61 C60 H60A 120.2 . . ? C59 C60 H60A 120.2 . . ? C60 C61 C62 119.8(3) . . ? C60 C61 H61A 120.1 . . ? C62 C61 H61A 120.1 . . ? C61 C62 C70 116.7(3) . . ? C61 C62 C63 123.9(3) . . ? C70 C62 C63 119.4(3) . . ? C64 C63 C62 121.6(3) . . ? C64 C63 H63A 119.2 . . ? C62 C63 H63A 119.2 . . ? C63 C64 C65 120.5(3) . . ? C63 C64 H64A 119.7 . . ? C65 C64 H64A 119.7 . . ? C66 C65 C69 117.4(3) . . ? C66 C65 C64 123.2(3) . . ? C69 C65 C64 119.4(3) . . ? C67 C66 C65 119.4(3) . . ? C67 C66 H66A 120.3 . . ? C65 C66 H66A 120.3 . . ? C66 C67 C68 119.8(3) . . ? C66 C67 H67A 120.1 . . ? C68 C67 H67A 120.1 . . ? N4 C68 C67 122.9(3) . . ? N4 C68 H68A 118.5 . . ? C67 C68 H68A 118.5 . . ? N4 C69 C65 122.8(3) . . ? N4 C69 C70 117.4(2) . . ? C65 C69 C70 119.8(2) . . ? N3 C70 C62 123.4(3) . . ? N3 C70 C69 117.6(2) . . ? C62 C70 C69 119.0(2) . . ? N5 C71 C72 122.3(4) . . ? N5 C71 H71A 118.8 . . ? C72 C71 H71A 118.8 . . ? C73 C72 C71 118.8(4) . . ? C73 C72 H72A 120.6 . . ? C71 C72 H72A 120.6 . . ? C72 C73 C74 120.6(3) . . ? C72 C73 H73A 119.7 . . ? C74 C73 H73A 119.7 . . ? C73 C74 C82 117.1(4) . . ? C73 C74 C75 125.0(4) . . ? C82 C74 C75 117.9(4) . . ? C76 C75 C74 120.5(4) . . ? C76 C75 H75A 119.8 . . ? C74 C75 H75A 119.8 . . ? C75 C76 C77 122.5(4) . . ? C75 C76 H76A 118.8 . . ? C77 C76 H76A 118.8 . . ? C76 C77 C78 126.3(4) . . ? C76 C77 C81 118.8(4) . . ? C78 C77 C81 114.9(4) . . ? C79 C78 C77 122.1(3) . . ? C79 C78 H78A 118.9 . . ? C77 C78 H78A 118.9 . . ? C78 C79 C80 118.1(4) . . ? C78 C79 H79A 120.9 . . ? C80 C79 H79A 120.9 . . ? N6 C80 C79 123.6(4) . . ? N6 C80 H80A 118.2 . . ? C79 C80 H80A 118.2 . . ? N6 C81 C77 122.0(3) . . ? N6 C81 C82 118.1(3) . . ? C77 C81 C82 119.9(3) . . ? N5 C82 C74 122.8(3) . . ? N5 C82 C81 116.9(3) . . ? C74 C82 C81 120.3(3) . . ? F2 B1 F1 109.3(4) . . ? F2 B1 F3 112.0(3) . . ? F1 B1 F3 109.0(3) . . ? F2 B1 F4 109.3(3) . . ? F1 B1 F4 106.3(3) . . ? F3 B1 F4 110.8(3) . . ? F5 B2 F6 110.0(3) . . ? F5 B2 F8 114.5(4) . . ? F6 B2 F8 107.8(3) . . ? F5 B2 F7 106.2(3) . . ? F6 B2 F7 112.1(4) . . ? F8 B2 F7 106.2(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 62.60 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.789 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.060 # start Validation Reply Form _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 205 A**3 RESPONSE: Actually the crystals of 2a are extraordinary unstable, and the crystal data have to be recorded very carefully at low temperature. The large solvent accessible voids of 205 A**3 in the crystal structure indicate that there may be solvents occupied in the voids. However, they can't be found in the crystal structure. Maybe they are likely too diffuse / disordered to be resolved. We tried to search for the solvent evidence from elemental analysis, but also unsuccessful, possibly the solvents escape out during the sample for elemental analysis being dried in vacuo. ; # end Validation Reply Form # Attachment '- 2b.CIF' data_2b _database_code_depnum_ccdc_archive 'CCDC 815814' #TrackingRef '- 2b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H76 B2 Cu2 F8 N6 P4' _chemical_formula_weight 1618.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.469(3) _cell_length_b 20.695(5) _cell_length_c 20.233(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.396(6) _cell_angle_gamma 90.00 _cell_volume 3899.6(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2925 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 52.24 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 17.22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16850 _diffrn_reflns_av_R_equivalents 0.1315 _diffrn_reflns_av_sigmaI/netI 0.1933 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6822 _reflns_number_gt 2928 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0707P)^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 6822 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1718 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.45708(8) 0.45165(3) 0.77084(3) 0.0274(2) Uani 1 1 d . . . P1 P 0.21834(17) 0.46561(7) 0.75458(7) 0.0259(4) Uani 1 1 d . . . P2 P 0.50071(16) 0.45820(8) 0.66565(7) 0.0265(4) Uani 1 1 d . . . N1 N 0.2094(5) 0.4722(2) 0.6161(2) 0.0231(12) Uani 1 1 d . . . N2 N 0.5228(5) 0.3688(2) 0.8262(2) 0.0299(12) Uani 1 1 d . . . N3 N 0.5860(5) 0.4946(3) 0.8508(2) 0.0330(13) Uani 1 1 d . . . C1 C 0.1046(6) 0.4859(3) 0.5564(2) 0.0186(13) Uani 1 1 d . . . C2 C 0.0074(6) 0.5348(3) 0.5583(3) 0.0261(14) Uani 1 1 d . . . H2A H 0.0128 0.5596 0.5982 0.031 Uiso 1 1 calc R . . C3 C 0.0985(6) 0.4511(3) 0.4965(2) 0.0239(13) Uani 1 1 d . . . H3A H 0.1665 0.4180 0.4936 0.029 Uiso 1 1 calc R . . C4 C 0.1379(6) 0.4427(3) 0.6680(2) 0.0276(14) Uani 1 1 d . . . H4A H 0.1418 0.3951 0.6639 0.033 Uiso 1 1 calc R . . H4B H 0.0355 0.4556 0.6594 0.033 Uiso 1 1 calc R . . C5 C 0.1261(6) 0.4112(3) 0.8027(3) 0.0256(14) Uani 1 1 d . . . C6 C 0.2003(7) 0.3887(3) 0.8637(3) 0.0356(16) Uani 1 1 d . . . H6A H 0.2920 0.4062 0.8814 0.043 Uiso 1 1 calc R . . C7 C 0.1430(7) 0.3410(3) 0.8994(3) 0.0422(18) Uani 1 1 d . . . H7A H 0.1955 0.3264 0.9412 0.051 Uiso 1 1 calc R . . C8 C 0.0122(8) 0.3152(3) 0.8746(3) 0.050(2) Uani 1 1 d . . . H8A H -0.0254 0.2814 0.8981 0.060 Uiso 1 1 calc R . . C9 C -0.0661(8) 0.3385(3) 0.8148(3) 0.055(2) Uani 1 1 d . . . H9A H -0.1593 0.3219 0.7982 0.066 Uiso 1 1 calc R . . C10 C -0.0100(7) 0.3850(3) 0.7797(3) 0.0378(17) Uani 1 1 d . . . H10A H -0.0646 0.4001 0.7386 0.045 Uiso 1 1 calc R . . C11 C 0.1416(6) 0.5456(3) 0.7632(3) 0.0306(15) Uani 1 1 d . . . C12 C 0.0526(7) 0.5587(3) 0.8085(3) 0.0411(17) Uani 1 1 d . . . H12A H 0.0240 0.5247 0.8347 0.049 Uiso 1 1 calc R . . C13 C 0.0048(8) 0.6210(4) 0.8161(4) 0.054(2) Uani 1 1 d . . . H13A H -0.0567 0.6292 0.8474 0.064 Uiso 1 1 calc R . . C14 C 0.0448(8) 0.6712(4) 0.7790(4) 0.051(2) Uani 1 1 d . . . H14A H 0.0127 0.7139 0.7852 0.062 Uiso 1 1 calc R . . C15 C 0.1323(8) 0.6591(3) 0.7325(3) 0.0503(19) Uani 1 1 d . . . H15A H 0.1586 0.6932 0.7058 0.060 Uiso 1 1 calc R . . C16 C 0.1817(7) 0.5964(3) 0.7250(3) 0.0415(18) Uani 1 1 d . . . H16A H 0.2433 0.5882 0.6937 0.050 Uiso 1 1 calc R . . C17 C 0.3364(6) 0.4370(3) 0.6055(3) 0.0278(15) Uani 1 1 d . . . H17A H 0.3528 0.4458 0.5593 0.033 Uiso 1 1 calc R . . H17B H 0.3183 0.3901 0.6089 0.033 Uiso 1 1 calc R . . C18 C 0.5564(6) 0.5362(3) 0.6360(3) 0.0304(15) Uani 1 1 d . . . C19 C 0.4862(7) 0.5675(3) 0.5787(3) 0.0340(16) Uani 1 1 d . . . H19A H 0.3980 0.5511 0.5547 0.041 Uiso 1 1 calc R . . C20 C 0.5461(8) 0.6230(3) 0.5570(3) 0.0428(18) Uani 1 1 d . . . H20A H 0.4987 0.6442 0.5175 0.051 Uiso 1 1 calc R . . C21 C 0.6722(8) 0.6479(3) 0.5915(4) 0.0482(19) Uani 1 1 d . . . H21A H 0.7130 0.6855 0.5757 0.058 Uiso 1 1 calc R . . C22 C 0.7384(7) 0.6180(4) 0.6486(4) 0.049(2) Uani 1 1 d . . . H22A H 0.8248 0.6355 0.6732 0.059 Uiso 1 1 calc R . . C23 C 0.6820(7) 0.5625(3) 0.6715(3) 0.0367(17) Uani 1 1 d . . . H23A H 0.7295 0.5424 0.7116 0.044 Uiso 1 1 calc R . . C24 C 0.6252(6) 0.4021(3) 0.6365(3) 0.0263(14) Uani 1 1 d . . . C25 C 0.7209(7) 0.4187(3) 0.5953(3) 0.0387(17) Uani 1 1 d . . . H25A H 0.7257 0.4623 0.5812 0.046 Uiso 1 1 calc R . . C26 C 0.8100(7) 0.3731(4) 0.5743(3) 0.0465(19) Uani 1 1 d . . . H26A H 0.8767 0.3861 0.5470 0.056 Uiso 1 1 calc R . . C27 C 0.8037(7) 0.3105(4) 0.5920(3) 0.0456(18) Uani 1 1 d . . . H27A H 0.8657 0.2796 0.5774 0.055 Uiso 1 1 calc R . . C28 C 0.7066(8) 0.2918(3) 0.6313(4) 0.062(2) Uani 1 1 d . . . H28A H 0.6994 0.2477 0.6433 0.074 Uiso 1 1 calc R . . C29 C 0.6193(7) 0.3378(3) 0.6533(3) 0.054(2) Uani 1 1 d . . . H29A H 0.5534 0.3246 0.6809 0.065 Uiso 1 1 calc R . . C30 C 0.4875(7) 0.3062(3) 0.8143(3) 0.0391(17) Uani 1 1 d . . . C31 C 0.5559(8) 0.2569(3) 0.8553(4) 0.053(2) Uani 1 1 d . . . H31A H 0.5332 0.2130 0.8443 0.064 Uiso 1 1 calc R . . C32 C 0.6541(9) 0.2714(4) 0.9103(4) 0.067(2) Uani 1 1 d . . . H32A H 0.7000 0.2377 0.9381 0.080 Uiso 1 1 calc R . . C33 C 0.6886(8) 0.3360(4) 0.9266(3) 0.056(2) Uani 1 1 d . . . C34 C 0.6242(6) 0.3834(3) 0.8825(3) 0.0348(16) Uani 1 1 d . . . C35 C 0.7906(9) 0.3545(5) 0.9853(4) 0.081(3) Uani 1 1 d . . . H35A H 0.8370 0.3224 1.0150 0.097 Uiso 1 1 calc R . . C36 C 0.8198(9) 0.4169(5) 0.9977(4) 0.078(3) Uani 1 1 d . . . H36A H 0.8864 0.4286 1.0368 0.093 Uiso 1 1 calc R . . C37 C 0.7530(8) 0.4667(4) 0.9535(4) 0.059(2) Uani 1 1 d . . . C38 C 0.6552(6) 0.4498(3) 0.8949(3) 0.0373(16) Uani 1 1 d . . . C39 C 0.7777(9) 0.5324(5) 0.9645(4) 0.079(3) Uani 1 1 d . . . H39A H 0.8456 0.5460 1.0024 0.095 Uiso 1 1 calc R . . C40 C 0.7073(9) 0.5775(4) 0.9225(4) 0.067(2) Uani 1 1 d . . . H40A H 0.7229 0.6222 0.9315 0.081 Uiso 1 1 calc R . . C41 C 0.6101(8) 0.5568(3) 0.8648(3) 0.0489(19) Uani 1 1 d . . . C42 C 0.3682(7) 0.2907(3) 0.7581(3) 0.0470(19) Uani 1 1 d . . . H42A H 0.3324 0.3306 0.7349 0.071 Uiso 1 1 calc R . . H42B H 0.2903 0.2697 0.7759 0.071 Uiso 1 1 calc R . . H42C H 0.4032 0.2616 0.7264 0.071 Uiso 1 1 calc R . . C43 C 0.5284(8) 0.6062(3) 0.8179(4) 0.063(2) Uani 1 1 d . . . H43A H 0.4660 0.5840 0.7809 0.095 Uiso 1 1 calc R . . H43B H 0.5963 0.6338 0.7998 0.095 Uiso 1 1 calc R . . H43C H 0.4697 0.6327 0.8426 0.095 Uiso 1 1 calc R . . B1 B 0.1644(10) 0.2435(4) 1.0613(5) 0.050(2) Uani 1 1 d . . . F1 F 0.1638(6) 0.2106(3) 1.1177(3) 0.133(2) Uani 1 1 d . . . F2 F 0.0947(7) 0.2048(3) 1.0101(3) 0.135(2) Uani 1 1 d . . . F3 F 0.3001(5) 0.2547(2) 1.0487(3) 0.1090(19) Uani 1 1 d . . . F4 F 0.0900(4) 0.29740(18) 1.0581(2) 0.0659(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0287(4) 0.0288(4) 0.0221(4) 0.0018(4) -0.0025(3) -0.0018(4) P1 0.0279(9) 0.0291(10) 0.0196(8) 0.0023(7) 0.0010(7) -0.0003(7) P2 0.0188(8) 0.0352(10) 0.0241(8) 0.0031(8) 0.0003(7) 0.0026(8) N1 0.019(3) 0.032(3) 0.018(2) 0.003(2) 0.003(2) 0.009(2) N2 0.029(3) 0.033(3) 0.029(3) 0.004(3) 0.008(3) -0.001(3) N3 0.033(3) 0.034(3) 0.033(3) -0.001(3) 0.006(3) -0.010(3) C1 0.019(3) 0.026(3) 0.010(3) -0.004(3) -0.002(3) 0.003(3) C2 0.024(3) 0.032(4) 0.022(3) -0.005(3) 0.003(3) 0.005(3) C3 0.028(3) 0.023(3) 0.022(3) 0.006(3) 0.006(3) 0.009(3) C4 0.026(3) 0.031(4) 0.028(3) 0.005(3) 0.013(3) 0.008(3) C5 0.029(4) 0.027(4) 0.020(3) 0.009(3) 0.002(3) 0.003(3) C6 0.038(4) 0.042(4) 0.026(3) 0.005(3) 0.002(3) -0.002(3) C7 0.050(5) 0.048(5) 0.028(4) 0.013(4) 0.007(4) -0.001(4) C8 0.061(5) 0.043(5) 0.048(4) 0.008(4) 0.017(4) -0.011(4) C9 0.049(5) 0.063(5) 0.052(5) 0.010(4) 0.006(4) -0.021(4) C10 0.035(4) 0.047(4) 0.030(4) 0.009(3) 0.002(3) -0.004(3) C11 0.037(4) 0.026(4) 0.026(3) -0.004(3) -0.001(3) 0.007(3) C12 0.045(4) 0.043(5) 0.034(4) 0.002(3) 0.004(3) 0.014(4) C13 0.048(5) 0.059(5) 0.053(5) -0.014(4) 0.006(4) 0.012(4) C14 0.052(5) 0.036(5) 0.059(5) -0.013(4) -0.010(4) 0.007(4) C15 0.056(5) 0.038(5) 0.054(5) 0.003(4) -0.001(4) 0.003(4) C16 0.049(5) 0.035(4) 0.040(4) -0.004(4) 0.007(3) 0.007(4) C17 0.018(3) 0.039(4) 0.024(3) 0.003(3) -0.004(3) -0.002(3) C18 0.033(4) 0.030(4) 0.027(3) -0.006(3) 0.003(3) -0.003(3) C19 0.038(4) 0.033(4) 0.028(4) 0.000(3) 0.000(3) 0.004(3) C20 0.060(5) 0.037(4) 0.031(4) 0.000(3) 0.009(4) 0.004(4) C21 0.056(5) 0.034(4) 0.062(5) -0.008(4) 0.029(4) -0.005(4) C22 0.033(4) 0.059(5) 0.055(5) -0.022(4) 0.008(4) -0.011(4) C23 0.036(4) 0.036(4) 0.035(4) 0.000(3) -0.001(3) -0.007(3) C24 0.015(3) 0.040(4) 0.023(3) 0.002(3) 0.001(3) 0.001(3) C25 0.035(4) 0.041(4) 0.039(4) -0.007(3) 0.006(3) -0.005(3) C26 0.028(4) 0.065(6) 0.048(4) -0.018(4) 0.011(3) -0.005(4) C27 0.031(4) 0.050(5) 0.054(5) -0.008(4) 0.003(4) 0.007(4) C28 0.069(6) 0.040(5) 0.086(6) 0.027(4) 0.039(5) 0.024(4) C29 0.053(5) 0.048(5) 0.068(5) 0.026(4) 0.033(4) 0.027(4) C30 0.038(4) 0.039(4) 0.042(4) 0.017(4) 0.011(3) 0.002(4) C31 0.055(5) 0.041(5) 0.065(5) 0.018(4) 0.014(4) 0.004(4) C32 0.082(7) 0.055(6) 0.063(6) 0.042(5) 0.013(5) 0.017(5) C33 0.048(5) 0.075(6) 0.040(4) 0.031(4) -0.002(4) 0.009(4) C34 0.031(4) 0.039(4) 0.031(4) 0.008(3) -0.002(3) -0.006(3) C35 0.066(6) 0.118(9) 0.052(6) 0.023(6) -0.006(5) 0.010(6) C36 0.078(7) 0.106(8) 0.033(5) 0.014(5) -0.033(4) 0.003(6) C37 0.060(5) 0.067(6) 0.047(5) -0.006(5) -0.001(4) -0.026(5) C38 0.031(4) 0.059(5) 0.018(3) -0.002(4) -0.005(3) 0.001(4) C39 0.068(6) 0.117(9) 0.040(5) -0.013(5) -0.022(4) -0.037(6) C40 0.082(7) 0.061(6) 0.057(5) -0.032(5) 0.003(5) -0.032(5) C41 0.052(5) 0.045(5) 0.046(4) -0.007(4) 0.000(4) -0.014(4) C42 0.045(5) 0.033(4) 0.063(5) 0.000(4) 0.008(4) -0.007(3) C43 0.078(6) 0.036(4) 0.073(5) -0.003(4) 0.006(5) -0.012(4) B1 0.055(6) 0.023(5) 0.074(7) 0.021(5) 0.023(5) 0.004(4) F1 0.100(5) 0.159(6) 0.137(5) 0.117(5) 0.015(4) 0.020(4) F2 0.181(6) 0.085(4) 0.158(5) -0.065(4) 0.083(5) -0.048(4) F3 0.047(3) 0.109(4) 0.180(5) 0.036(4) 0.046(3) 0.011(3) F4 0.073(3) 0.043(3) 0.083(3) 0.006(2) 0.017(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.046(5) . ? Cu1 N2 2.080(5) . ? Cu1 P1 2.2435(18) . ? Cu1 P2 2.2440(17) . ? P1 C5 1.812(6) . ? P1 C11 1.829(6) . ? P1 C4 1.841(5) . ? P2 C24 1.827(6) . ? P2 C18 1.832(6) . ? P2 C17 1.847(5) . ? N1 C1 1.446(6) . ? N1 C17 1.455(7) . ? N1 C4 1.481(6) . ? N2 C30 1.348(8) . ? N2 C34 1.384(7) . ? N3 C41 1.329(8) . ? N3 C38 1.368(7) . ? C1 C2 1.373(7) . ? C1 C3 1.402(7) . ? C2 C3 1.385(7) 3_566 ? C2 H2A 0.9500 . ? C3 C2 1.385(7) 3_566 ? C3 H3A 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.385(7) . ? C5 C10 1.398(8) . ? C6 C7 1.390(8) . ? C6 H6A 0.9500 . ? C7 C8 1.359(8) . ? C7 H7A 0.9500 . ? C8 C9 1.387(8) . ? C8 H8A 0.9500 . ? C9 C10 1.360(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.379(8) . ? C11 C16 1.397(8) . ? C12 C13 1.383(9) . ? C12 H12A 0.9500 . ? C13 C14 1.374(9) . ? C13 H13A 0.9500 . ? C14 C15 1.384(9) . ? C14 H14A 0.9500 . ? C15 C16 1.396(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.386(8) . ? C18 C19 1.388(7) . ? C19 C20 1.388(8) . ? C19 H19A 0.9500 . ? C20 C21 1.370(9) . ? C20 H20A 0.9500 . ? C21 C22 1.361(9) . ? C21 H21A 0.9500 . ? C22 C23 1.380(8) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.376(8) . ? C24 C25 1.381(8) . ? C25 C26 1.383(8) . ? C25 H25A 0.9500 . ? C26 C27 1.348(9) . ? C26 H26A 0.9500 . ? C27 C28 1.376(9) . ? C27 H27A 0.9500 . ? C28 C29 1.385(9) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.398(8) . ? C30 C42 1.486(8) . ? C31 C32 1.349(9) . ? C31 H31A 0.9500 . ? C32 C33 1.400(10) . ? C32 H32A 0.9500 . ? C33 C34 1.393(8) . ? C33 C35 1.440(10) . ? C34 C38 1.418(9) . ? C35 C36 1.333(11) . ? C35 H35A 0.9500 . ? C36 C37 1.434(10) . ? C36 H36A 0.9500 . ? C37 C39 1.392(10) . ? C37 C38 1.411(8) . ? C39 C40 1.354(10) . ? C39 H39A 0.9500 . ? C40 C41 1.417(9) . ? C40 H40A 0.9500 . ? C41 C43 1.508(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? B1 F4 1.315(9) . ? B1 F1 1.329(9) . ? B1 F3 1.374(9) . ? B1 F2 1.378(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 81.6(2) . . ? N3 Cu1 P1 120.12(15) . . ? N2 Cu1 P1 112.39(14) . . ? N3 Cu1 P2 122.55(14) . . ? N2 Cu1 P2 118.14(14) . . ? P1 Cu1 P2 101.90(6) . . ? C5 P1 C11 105.8(3) . . ? C5 P1 C4 101.2(3) . . ? C11 P1 C4 102.7(3) . . ? C5 P1 Cu1 114.32(19) . . ? C11 P1 Cu1 120.7(2) . . ? C4 P1 Cu1 109.82(18) . . ? C24 P2 C18 102.4(3) . . ? C24 P2 C17 98.8(3) . . ? C18 P2 C17 104.5(3) . . ? C24 P2 Cu1 120.49(19) . . ? C18 P2 Cu1 118.48(19) . . ? C17 P2 Cu1 109.50(19) . . ? C1 N1 C17 115.8(4) . . ? C1 N1 C4 109.9(4) . . ? C17 N1 C4 113.2(4) . . ? C30 N2 C34 118.0(5) . . ? C30 N2 Cu1 130.9(4) . . ? C34 N2 Cu1 111.0(4) . . ? C41 N3 C38 118.3(5) . . ? C41 N3 Cu1 130.1(5) . . ? C38 N3 Cu1 111.6(4) . . ? C2 C1 C3 118.6(5) . . ? C2 C1 N1 118.9(5) . . ? C3 C1 N1 122.4(5) . . ? C1 C2 C3 121.7(5) . 3_566 ? C1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 3_566 . ? C2 C3 C1 119.7(5) 3_566 . ? C2 C3 H3A 120.2 3_566 . ? C1 C3 H3A 120.2 . . ? N1 C4 P1 113.9(4) . . ? N1 C4 H4A 108.8 . . ? P1 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? P1 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C10 117.0(5) . . ? C6 C5 P1 118.1(5) . . ? C10 C5 P1 124.5(4) . . ? C5 C6 C7 121.3(6) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C8 C7 C6 120.2(6) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C9 119.5(6) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 120.3(7) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C5 121.6(6) . . ? C9 C10 H10A 119.2 . . ? C5 C10 H10A 119.2 . . ? C12 C11 C16 118.6(6) . . ? C12 C11 P1 122.8(5) . . ? C16 C11 P1 118.4(5) . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 121.1(7) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 119.5(7) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C14 C15 C16 119.7(7) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C11 120.6(6) . . ? C15 C16 H16A 119.7 . . ? C11 C16 H16A 119.7 . . ? N1 C17 P2 113.8(4) . . ? N1 C17 H17A 108.8 . . ? P2 C17 H17A 108.8 . . ? N1 C17 H17B 108.8 . . ? P2 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C23 C18 C19 119.1(6) . . ? C23 C18 P2 116.6(5) . . ? C19 C18 P2 124.2(5) . . ? C20 C19 C18 119.3(6) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? C21 C20 C19 121.2(6) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C22 C21 C20 119.2(7) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 121.1(7) . . ? C21 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C22 C23 C18 120.1(6) . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? C29 C24 C25 116.8(6) . . ? C29 C24 P2 118.5(5) . . ? C25 C24 P2 124.6(5) . . ? C26 C25 C24 121.2(6) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C27 C26 C25 121.1(7) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 119.3(7) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C27 C28 C29 119.5(7) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C24 C29 C28 122.1(6) . . ? C24 C29 H29A 119.0 . . ? C28 C29 H29A 119.0 . . ? N2 C30 C31 121.5(6) . . ? N2 C30 C42 118.3(6) . . ? C31 C30 C42 120.2(6) . . ? C32 C31 C30 120.2(7) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 120.3(7) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 117.7(7) . . ? C34 C33 C35 119.4(8) . . ? C32 C33 C35 122.8(8) . . ? N2 C34 C33 122.2(6) . . ? N2 C34 C38 116.6(6) . . ? C33 C34 C38 121.1(6) . . ? C36 C35 C33 119.9(9) . . ? C36 C35 H35A 120.0 . . ? C33 C35 H35A 120.0 . . ? C35 C36 C37 121.6(8) . . ? C35 C36 H36A 119.2 . . ? C37 C36 H36A 119.2 . . ? C39 C37 C38 116.3(8) . . ? C39 C37 C36 124.1(8) . . ? C38 C37 C36 119.6(7) . . ? N3 C38 C37 123.0(7) . . ? N3 C38 C34 118.8(5) . . ? C37 C38 C34 118.2(7) . . ? C40 C39 C37 121.6(7) . . ? C40 C39 H39A 119.2 . . ? C37 C39 H39A 119.2 . . ? C39 C40 C41 118.9(7) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N3 C41 C40 121.9(7) . . ? N3 C41 C43 118.2(6) . . ? C40 C41 C43 119.8(7) . . ? C30 C42 H42A 109.5 . . ? C30 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C30 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? F4 B1 F1 113.0(8) . . ? F4 B1 F3 111.0(7) . . ? F1 B1 F3 113.2(7) . . ? F4 B1 F2 106.1(7) . . ? F1 B1 F2 105.8(7) . . ? F3 B1 F2 107.2(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.734 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.100 # Attachment '- 3a.CIF' data_3a _database_code_depnum_ccdc_archive 'CCDC 815815' #TrackingRef '- 3a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H86 B2 Cu2 F8 N6 P4' _chemical_formula_weight 1796.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1247(6) _cell_length_b 17.5097(6) _cell_length_c 18.4113(6) _cell_angle_alpha 68.401(3) _cell_angle_beta 76.139(3) _cell_angle_gamma 87.182(3) _cell_volume 4397.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9816 _cell_measurement_theta_min 2.7144 _cell_measurement_theta_max 62.4679 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89892 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22395 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 62.56 _reflns_number_total 13584 _reflns_number_gt 10107 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1462P)^2^+3.5517P] 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 13584 _refine_ls_number_parameters 1087 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.2128 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.68120(4) 0.04400(4) 0.28734(4) 0.0358(2) Uani 1 1 d . . . P1 P 0.72546(9) 0.12709(8) 0.15718(7) 0.0413(3) Uani 1 1 d . . . P2 P 0.80118(8) -0.03427(7) 0.30148(7) 0.0374(3) Uani 1 1 d . . . N1 N 0.8881(3) 0.0433(3) 0.1433(2) 0.0444(10) Uani 1 1 d . . . N2 N 0.6442(3) 0.1117(2) 0.3594(2) 0.0368(9) Uani 1 1 d . . . N3 N 0.5461(3) 0.0027(2) 0.3351(2) 0.0404(9) Uani 1 1 d . . . C2 C 1.0561(4) 0.0599(4) 0.0847(4) 0.0607(15) Uani 1 1 d . . . H2A H 1.0630 0.0809 0.1227 0.073 Uiso 1 1 calc R . . C3 C 0.9711(4) 0.0351(3) 0.0869(3) 0.0478(12) Uani 1 1 d . . . C4 C 0.9624(3) 0.0036(3) 0.0296(3) 0.0401(11) Uani 1 1 d . . . C5 C 0.8734(4) -0.0245(3) 0.0288(3) 0.0505(13) Uani 1 1 d . . . H5A H 0.8219 -0.0213 0.0669 0.061 Uiso 1 1 calc R . . C1 C 1.1341(4) 0.0548(4) 0.0264(4) 0.0601(15) Uani 1 1 d . . . H1A H 1.1910 0.0727 0.0266 0.072 Uiso 1 1 calc R . . C6 C 0.8488(4) 0.1239(3) 0.1122(3) 0.0465(12) Uani 1 1 d . . . H6A H 0.8578 0.1403 0.0545 0.056 Uiso 1 1 calc R . . H6B H 0.8820 0.1639 0.1217 0.056 Uiso 1 1 calc R . . C7 C 0.6704(5) 0.1126(4) 0.0848(2) 0.137(2) Uani 1 1 d GU . . C8 C 0.6887(5) 0.1630(4) 0.0040(3) 0.136(2) Uani 1 1 d GU . . H8A H 0.7317 0.2065 -0.0161 0.163 Uiso 1 1 calc R . . C9 C 0.6427(5) 0.1485(4) -0.0469(2) 0.137(2) Uani 1 1 d GU . . H9A H 0.6549 0.1822 -0.1010 0.164 Uiso 1 1 calc R . . C10 C 0.5784(5) 0.0835(4) -0.0169(3) 0.140(2) Uani 1 1 d GU . . H10A H 0.5476 0.0738 -0.0509 0.168 Uiso 1 1 calc R . . C11 C 0.5601(5) 0.0331(4) 0.0640(3) 0.141(2) Uani 1 1 d GU . . H11A H 0.5171 -0.0103 0.0841 0.170 Uiso 1 1 calc R . . C12 C 0.6061(5) 0.0477(4) 0.1148(2) 0.140(2) Uani 1 1 d GU . . H12A H 0.5939 0.0140 0.1690 0.168 Uiso 1 1 calc R . . C13 C 0.7152(3) 0.2355(3) 0.1431(3) 0.0441(12) Uani 1 1 d . . . C14 C 0.6448(4) 0.2800(4) 0.1132(3) 0.0599(16) Uani 1 1 d . . . H14A H 0.6070 0.2573 0.0926 0.072 Uiso 1 1 calc R . . C15 C 0.6311(5) 0.3591(5) 0.1142(4) 0.081(2) Uani 1 1 d . . . H15A H 0.5832 0.3885 0.0950 0.097 Uiso 1 1 calc R . . C16 C 0.6864(6) 0.3936(4) 0.1427(4) 0.077(2) Uani 1 1 d . . . H16A H 0.6771 0.4466 0.1424 0.092 Uiso 1 1 calc R . . C17 C 0.7588(5) 0.3483(4) 0.1731(4) 0.0679(17) Uani 1 1 d . . . H17A H 0.7974 0.3714 0.1926 0.081 Uiso 1 1 calc R . . C18 C 0.7708(4) 0.2708(3) 0.1732(3) 0.0539(14) Uani 1 1 d . . . H18A H 0.8174 0.2407 0.1940 0.065 Uiso 1 1 calc R . . C19 C 0.9027(3) 0.0226(3) 0.2239(3) 0.0444(12) Uani 1 1 d . . . H19A H 0.9147 0.0726 0.2318 0.053 Uiso 1 1 calc R . . H19B H 0.9555 -0.0109 0.2294 0.053 Uiso 1 1 calc R . . C20 C 0.8014(4) -0.1301(3) 0.2850(3) 0.0442(12) Uani 1 1 d . . . C21 C 0.7223(5) -0.1568(4) 0.2759(4) 0.0675(17) Uani 1 1 d . . . H21A H 0.6710 -0.1254 0.2775 0.081 Uiso 1 1 calc R . . C22 C 0.7190(6) -0.2311(5) 0.2643(5) 0.087(2) Uani 1 1 d . . . H22A H 0.6650 -0.2507 0.2603 0.104 Uiso 1 1 calc R . . C23 C 0.7971(6) -0.2747(4) 0.2590(4) 0.080(2) Uani 1 1 d . . . H23A H 0.7958 -0.3234 0.2498 0.096 Uiso 1 1 calc R . . C24 C 0.8759(5) -0.2480(4) 0.2669(4) 0.0655(17) Uani 1 1 d . . . H24A H 0.9280 -0.2782 0.2633 0.079 Uiso 1 1 calc R . . C25 C 0.8776(4) -0.1767(3) 0.2800(3) 0.0552(14) Uani 1 1 d . . . H25A H 0.9315 -0.1587 0.2857 0.066 Uiso 1 1 calc R . . C26 C 0.8427(3) -0.0586(3) 0.3919(3) 0.0416(11) Uani 1 1 d . . . C27 C 0.8662(3) 0.0060(3) 0.4114(3) 0.0451(12) Uani 1 1 d . . . H27A H 0.8653 0.0597 0.3756 0.054 Uiso 1 1 calc R . . C28 C 0.8910(4) -0.0075(4) 0.4831(3) 0.0528(13) Uani 1 1 d . . . H28A H 0.9062 0.0366 0.4951 0.063 Uiso 1 1 calc R . . C29 C 0.8929(4) -0.0875(4) 0.5364(4) 0.0634(16) Uani 1 1 d . . . H29A H 0.9105 -0.0973 0.5840 0.076 Uiso 1 1 calc R . . C30 C 0.8688(4) -0.1521(4) 0.5190(3) 0.0593(15) Uani 1 1 d . . . H30A H 0.8687 -0.2055 0.5556 0.071 Uiso 1 1 calc R . . C31 C 0.8445(4) -0.1389(3) 0.4474(3) 0.0493(13) Uani 1 1 d . . . H31A H 0.8294 -0.1835 0.4361 0.059 Uiso 1 1 calc R . . C32 C 0.6923(4) 0.1659(3) 0.3704(3) 0.0479(12) Uani 1 1 d . . . H32A H 0.7546 0.1726 0.3471 0.057 Uiso 1 1 calc R . . C33 C 0.6533(4) 0.2136(4) 0.4159(4) 0.0623(16) Uani 1 1 d . . . H33A H 0.6892 0.2520 0.4212 0.075 Uiso 1 1 calc R . . C34 C 0.5618(4) 0.2033(4) 0.4526(4) 0.0622(16) Uani 1 1 d . . . H34A H 0.5354 0.2344 0.4830 0.075 Uiso 1 1 calc R . . C35 C 0.5090(4) 0.1453(3) 0.4436(3) 0.0463(12) Uani 1 1 d . . . C36 C 0.4128(4) 0.1307(4) 0.4784(3) 0.0551(15) Uani 1 1 d . . . H36A H 0.3830 0.1603 0.5092 0.066 Uiso 1 1 calc R . . C37 C 0.3650(4) 0.0748(4) 0.4673(3) 0.0534(14) Uani 1 1 d . . . H37A H 0.3031 0.0657 0.4916 0.064 Uiso 1 1 calc R . . C38 C 0.4070(3) 0.0298(3) 0.4194(3) 0.0488(13) Uani 1 1 d . . . C39 C 0.3593(4) -0.0280(4) 0.4058(4) 0.0572(14) Uani 1 1 d . . . H39A H 0.2971 -0.0382 0.4286 0.069 Uiso 1 1 calc R . . C40 C 0.4040(4) -0.0695(4) 0.3590(4) 0.0642(16) Uani 1 1 d . . . H40A H 0.3729 -0.1084 0.3500 0.077 Uiso 1 1 calc R . . C41 C 0.4973(4) -0.0523(4) 0.3248(3) 0.0519(13) Uani 1 1 d . . . H41A H 0.5271 -0.0810 0.2930 0.062 Uiso 1 1 calc R . . C42 C 0.5009(3) 0.0424(3) 0.3836(3) 0.0394(11) Uani 1 1 d . . . C43 C 0.5525(3) 0.1010(3) 0.3962(3) 0.0388(11) Uani 1 1 d . . . Cu2 Cu 0.21522(5) 0.49655(4) 0.33109(4) 0.0412(2) Uani 1 1 d . . . P3 P 0.35025(9) 0.43943(8) 0.30890(7) 0.0413(3) Uani 1 1 d . . . P4 P 0.20550(8) 0.56871(7) 0.20545(7) 0.0366(3) Uani 1 1 d . . . N4 N 0.3845(3) 0.5346(2) 0.1478(2) 0.0378(9) Uani 1 1 d . . . N5 N 0.2197(3) 0.5555(3) 0.4089(2) 0.0427(10) Uani 1 1 d . . . N6 N 0.1172(3) 0.4249(2) 0.4287(2) 0.0428(10) Uani 1 1 d . . . C45 C 0.5089(4) 0.6218(3) 0.0395(3) 0.0536(14) Uani 1 1 d . . . H45A H 0.5002 0.6612 0.0631 0.064 Uiso 1 1 calc R . . C46 C 0.4542(3) 0.5522(3) 0.0731(3) 0.0398(11) Uani 1 1 d . . . C47 C 0.4652(3) 0.4936(3) 0.0358(3) 0.0365(10) Uani 1 1 d . . . C48 C 0.4087(4) 0.4202(3) 0.0676(3) 0.0465(12) Uani 1 1 d . . . H48A H 0.3629 0.4102 0.1143 0.056 Uiso 1 1 calc R . . C44 C 0.5791(4) 0.6349(4) -0.0311(3) 0.0600(16) Uani 1 1 d . . . H44A H 0.6171 0.6820 -0.0524 0.072 Uiso 1 1 calc R . . C49 C 0.3231(3) 0.6030(3) 0.1439(3) 0.0384(11) Uani 1 1 d . . . H49A H 0.3209 0.6326 0.0884 0.046 Uiso 1 1 calc R . . H49B H 0.3477 0.6407 0.1624 0.046 Uiso 1 1 calc R . . C50 C 0.1591(4) 0.5145(3) 0.1541(3) 0.0470(12) Uani 1 1 d . . . C51 C 0.0896(4) 0.4565(3) 0.1976(3) 0.0512(13) Uani 1 1 d . . . H51A H 0.0696 0.4443 0.2527 0.061 Uiso 1 1 calc R . . C52 C 0.0490(5) 0.4162(4) 0.1624(4) 0.0710(18) Uani 1 1 d . . . H52A H 0.0015 0.3776 0.1933 0.085 Uiso 1 1 calc R . . C53 C 0.0783(6) 0.4326(6) 0.0822(4) 0.096(3) Uani 1 1 d . . . H53A H 0.0516 0.4045 0.0581 0.116 Uiso 1 1 calc R . . C54 C 0.1470(7) 0.4904(6) 0.0368(4) 0.117(4) Uani 1 1 d . . . H54A H 0.1666 0.5020 -0.0181 0.140 Uiso 1 1 calc R . . C55 C 0.1875(6) 0.5315(5) 0.0722(4) 0.083(2) Uani 1 1 d . . . H55A H 0.2341 0.5709 0.0410 0.100 Uiso 1 1 calc R . . C56 C 0.1531(3) 0.6687(3) 0.1778(3) 0.0391(11) Uani 1 1 d . . . C57 C 0.1769(4) 0.7261(3) 0.2062(3) 0.0490(13) Uani 1 1 d . . . H57A H 0.2166 0.7119 0.2402 0.059 Uiso 1 1 calc R . . C58 C 0.1426(5) 0.8038(4) 0.1850(3) 0.0629(16) Uani 1 1 d . . . H58A H 0.1610 0.8424 0.2027 0.075 Uiso 1 1 calc R . . C59 C 0.0809(5) 0.8235(4) 0.1372(4) 0.0659(18) Uani 1 1 d . . . H59A H 0.0571 0.8756 0.1233 0.079 Uiso 1 1 calc R . . C60 C 0.0550(4) 0.7688(4) 0.1108(4) 0.0622(16) Uani 1 1 d . . . H60A H 0.0128 0.7831 0.0792 0.075 Uiso 1 1 calc R . . C61 C 0.0904(4) 0.6898(3) 0.1300(3) 0.0499(13) Uani 1 1 d . . . H61A H 0.0722 0.6522 0.1110 0.060 Uiso 1 1 calc R . . C62 C 0.4275(3) 0.5097(3) 0.2166(3) 0.0415(11) Uani 1 1 d . . . H62A H 0.4429 0.5582 0.2255 0.050 Uiso 1 1 calc R . . H62B H 0.4834 0.4826 0.2045 0.050 Uiso 1 1 calc R . . C63 C 0.4148(4) 0.4195(3) 0.3862(3) 0.0506(14) Uani 1 1 d . . . C64 C 0.5029(5) 0.4455(4) 0.3727(4) 0.0707(18) Uani 1 1 d . . . H64A H 0.5353 0.4740 0.3203 0.085 Uiso 1 1 calc R . . C65 C 0.5449(7) 0.4305(5) 0.4352(5) 0.091(2) Uani 1 1 d . . . H65A H 0.6046 0.4498 0.4246 0.109 Uiso 1 1 calc R . . C66 C 0.4988(7) 0.3874(5) 0.5126(5) 0.085(2) Uani 1 1 d . . . H66A H 0.5273 0.3766 0.5546 0.101 Uiso 1 1 calc R . . C67 C 0.4116(7) 0.3604(5) 0.5276(4) 0.093(3) Uani 1 1 d . . . H67A H 0.3805 0.3306 0.5802 0.111 Uiso 1 1 calc R . . C68 C 0.3675(5) 0.3770(4) 0.4650(3) 0.0716(19) Uani 1 1 d . . . H68A H 0.3069 0.3598 0.4760 0.086 Uiso 1 1 calc R . . C69 C 0.3534(4) 0.3447(3) 0.2902(3) 0.0434(12) Uani 1 1 d . . . C70 C 0.2730(4) 0.3134(4) 0.2861(3) 0.0588(15) Uani 1 1 d . . . H70A H 0.2193 0.3406 0.2942 0.071 Uiso 1 1 calc R . . C71 C 0.2721(5) 0.2418(4) 0.2701(4) 0.0721(18) Uani 1 1 d . . . H71A H 0.2180 0.2209 0.2678 0.086 Uiso 1 1 calc R . . C72 C 0.3519(5) 0.2022(4) 0.2578(4) 0.0667(18) Uani 1 1 d . . . H72A H 0.3513 0.1542 0.2473 0.080 Uiso 1 1 calc R . . C73 C 0.4321(5) 0.2324(3) 0.2606(3) 0.0587(15) Uani 1 1 d . . . H73A H 0.4858 0.2056 0.2513 0.070 Uiso 1 1 calc R . . C74 C 0.4330(4) 0.3030(3) 0.2776(3) 0.0504(13) Uani 1 1 d . . . H74A H 0.4874 0.3228 0.2805 0.061 Uiso 1 1 calc R . . C75 C 0.2713(4) 0.6195(3) 0.3989(3) 0.0530(13) Uani 1 1 d . . . H75A H 0.3120 0.6447 0.3494 0.064 Uiso 1 1 calc R . . C76 C 0.2673(4) 0.6505(4) 0.4589(4) 0.0593(15) Uani 1 1 d . . . H76A H 0.3033 0.6965 0.4488 0.071 Uiso 1 1 calc R . . C77 C 0.2108(5) 0.6134(4) 0.5323(4) 0.0618(16) Uani 1 1 d . . . H77A H 0.2078 0.6338 0.5728 0.074 Uiso 1 1 calc R . . C78 C 0.1573(4) 0.5448(4) 0.5468(3) 0.0511(14) Uani 1 1 d . . . C79 C 0.0945(5) 0.5008(4) 0.6222(3) 0.0651(18) Uani 1 1 d . . . H79A H 0.0904 0.5174 0.6654 0.078 Uiso 1 1 calc R . . C80 C 0.0423(4) 0.4374(4) 0.6319(3) 0.0636(18) Uani 1 1 d . . . H80A H 0.0011 0.4118 0.6810 0.076 Uiso 1 1 calc R . . C81 C 0.0481(4) 0.4074(4) 0.5681(3) 0.0551(15) Uani 1 1 d . . . C82 C -0.0054(4) 0.3401(4) 0.5749(3) 0.0592(16) Uani 1 1 d . . . H82A H -0.0469 0.3117 0.6230 0.071 Uiso 1 1 calc R . . C83 C 0.0043(4) 0.3172(4) 0.5101(4) 0.0581(15) Uani 1 1 d . . . H83A H -0.0296 0.2724 0.5141 0.070 Uiso 1 1 calc R . . C84 C 0.0659(4) 0.3617(3) 0.4377(3) 0.0493(13) Uani 1 1 d . . . H84A H 0.0708 0.3460 0.3938 0.059 Uiso 1 1 calc R . . C85 C 0.1639(4) 0.5172(3) 0.4825(3) 0.0452(12) Uani 1 1 d . . . C86 C 0.1089(3) 0.4480(3) 0.4934(3) 0.0430(12) Uani 1 1 d . . . C87 C 0.2482(5) -0.0204(7) 0.2266(5) 0.090(3) Uani 1 1 d . . . H87A H 0.2906 -0.0586 0.2185 0.108 Uiso 1 1 calc R . . C88 C 0.2586(7) 0.0601(8) 0.1746(5) 0.104(3) Uani 1 1 d . . . H88A H 0.3095 0.0756 0.1315 0.124 Uiso 1 1 calc R . . C89 C 0.1988(9) 0.1176(9) 0.1829(8) 0.128(4) Uani 1 1 d . . . H89A H 0.2078 0.1717 0.1467 0.153 Uiso 1 1 calc R . . C90 C 0.1203(8) 0.0920(10) 0.2501(9) 0.133(5) Uani 1 1 d . . . H90A H 0.0758 0.1286 0.2579 0.160 Uiso 1 1 calc R . . C91 C 0.1137(6) 0.0109(9) 0.3026(7) 0.106(3) Uani 1 1 d . . . H91A H 0.0649 -0.0056 0.3475 0.128 Uiso 1 1 calc R . . C92 C 0.1725(7) -0.0437(8) 0.2922(6) 0.112(3) Uani 1 1 d . . . C93 C 0.1545(9) -0.1284(8) 0.3535(6) 0.155(6) Uani 1 1 d . . . H93A H 0.0991 -0.1304 0.3928 0.233 Uiso 1 1 calc R . . H93B H 0.2042 -0.1434 0.3795 0.233 Uiso 1 1 calc R . . H93C H 0.1487 -0.1661 0.3279 0.233 Uiso 1 1 calc R . . C94 C 0.8163(9) 0.6789(11) 0.0724(9) 0.153(6) Uani 1 1 d . . . H94A H 0.8431 0.7219 0.0252 0.183 Uiso 1 1 calc R . . C95 C 0.8666(9) 0.6079(12) 0.1102(10) 0.150(6) Uani 1 1 d . . . H95A H 0.9277 0.6053 0.0864 0.180 Uiso 1 1 calc R . . C96 C 0.8253(9) 0.5431(9) 0.1819(9) 0.125(4) Uani 1 1 d . . . H96A H 0.8599 0.4992 0.2043 0.150 Uiso 1 1 calc R . . C97 C 0.7333(9) 0.5432(7) 0.2203(8) 0.131(4) Uani 1 1 d . . . H97A H 0.7058 0.5013 0.2681 0.157 Uiso 1 1 calc R . . C98 C 0.6831(8) 0.6139(7) 0.1801(8) 0.113(3) Uani 1 1 d . . . H98A H 0.6211 0.6163 0.2009 0.136 Uiso 1 1 calc R . . C99 C 0.7283(9) 0.6774(8) 0.1110(7) 0.120(4) Uani 1 1 d . . . C100 C 0.6745(10) 0.7582(9) 0.0716(8) 0.157(5) Uani 1 1 d . . . H10B H 0.7150 0.7961 0.0250 0.236 Uiso 1 1 calc R . . H10C H 0.6528 0.7839 0.1102 0.236 Uiso 1 1 calc R . . H10D H 0.6238 0.7427 0.0563 0.236 Uiso 1 1 calc R . . F1 F 0.8846(4) 0.1989(3) 0.4248(2) 0.0929(14) Uani 1 1 d . . . F2 F 0.8874(3) 0.3205(2) 0.3236(2) 0.0883(13) Uani 1 1 d . . . F3 F 1.0202(3) 0.2583(3) 0.3397(3) 0.0886(13) Uani 1 1 d . . . F4 F 0.9202(2) 0.2070(2) 0.2954(2) 0.0677(9) Uani 1 1 d . . . B1 B 0.9272(5) 0.2461(4) 0.3475(4) 0.0553(16) Uani 1 1 d . . . F5 F 0.4476(6) 0.7159(4) 0.2221(4) 0.161(3) Uani 1 1 d . . . F6 F 0.3561(4) 0.7966(4) 0.2574(4) 0.135(2) Uani 1 1 d . . . F7 F 0.4575(4) 0.7549(3) 0.3244(3) 0.122(2) Uani 1 1 d . . . F8 F 0.5012(4) 0.8403(3) 0.1997(3) 0.120(2) Uani 1 1 d . . . B2 B 0.4469(7) 0.7720(6) 0.2508(5) 0.079(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 Cu1 0.0358(4) 0.0382(4) 0.0260(3) -0.0074(3) -0.0014(3) 0.0041(3) P1 0.0448(7) 0.0442(7) 0.0244(6) -0.0033(5) -0.0039(5) 0.0025(5) P2 0.0396(7) 0.0363(6) 0.0265(6) -0.0058(5) -0.0006(5) 0.0070(5) N1 0.051(2) 0.043(2) 0.027(2) -0.0101(17) 0.0069(17) 0.0067(19) N2 0.036(2) 0.038(2) 0.030(2) -0.0096(17) -0.0018(16) 0.0061(17) N3 0.038(2) 0.042(2) 0.034(2) -0.0074(18) -0.0059(17) 0.0032(18) C2 0.048(3) 0.074(4) 0.058(4) -0.030(3) 0.002(3) -0.008(3) C3 0.052(3) 0.045(3) 0.038(3) -0.011(2) -0.005(2) 0.009(2) C4 0.049(3) 0.037(3) 0.023(2) -0.0043(18) -0.0021(19) 0.013(2) C5 0.053(3) 0.056(3) 0.043(3) -0.018(3) -0.011(2) 0.004(3) C1 0.048(3) 0.081(4) 0.054(3) -0.031(3) -0.006(3) -0.009(3) C6 0.049(3) 0.047(3) 0.029(2) -0.005(2) 0.003(2) 0.004(2) C7 0.183(4) 0.166(4) 0.0377(17) 0.009(2) -0.032(2) -0.108(3) C8 0.182(4) 0.165(4) 0.0368(17) 0.007(2) -0.032(2) -0.108(3) C9 0.183(4) 0.166(4) 0.0388(17) 0.007(2) -0.033(2) -0.109(3) C10 0.184(4) 0.168(4) 0.0427(17) 0.008(2) -0.033(2) -0.111(3) C11 0.185(4) 0.169(4) 0.0438(17) 0.009(2) -0.032(2) -0.111(3) C12 0.185(4) 0.168(4) 0.0416(17) 0.009(2) -0.032(2) -0.110(3) C13 0.041(3) 0.043(3) 0.028(2) 0.003(2) 0.001(2) 0.007(2) C14 0.054(3) 0.074(4) 0.035(3) -0.007(3) -0.007(2) 0.030(3) C15 0.086(5) 0.083(5) 0.042(3) 0.002(3) -0.007(3) 0.049(4) C16 0.100(6) 0.043(3) 0.054(4) 0.000(3) 0.009(4) 0.024(4) C17 0.074(4) 0.045(3) 0.070(4) -0.016(3) 0.001(3) -0.001(3) C18 0.051(3) 0.041(3) 0.054(3) -0.004(2) -0.006(3) 0.005(2) C19 0.040(3) 0.046(3) 0.036(3) -0.008(2) 0.000(2) 0.009(2) C20 0.054(3) 0.040(3) 0.027(2) -0.006(2) 0.003(2) 0.002(2) C21 0.079(5) 0.058(4) 0.067(4) -0.032(3) -0.006(3) 0.005(3) C22 0.093(6) 0.076(5) 0.108(6) -0.052(5) -0.025(5) -0.002(4) C23 0.122(7) 0.054(4) 0.066(4) -0.034(3) -0.007(4) 0.011(4) C24 0.087(5) 0.052(4) 0.051(3) -0.020(3) -0.005(3) 0.014(3) C25 0.068(4) 0.047(3) 0.044(3) -0.015(2) -0.006(3) 0.009(3) C26 0.036(3) 0.048(3) 0.030(2) -0.007(2) -0.0010(19) 0.008(2) C27 0.038(3) 0.046(3) 0.041(3) -0.007(2) -0.004(2) 0.001(2) C28 0.046(3) 0.067(4) 0.043(3) -0.021(3) -0.007(2) 0.001(3) C29 0.061(4) 0.086(5) 0.042(3) -0.019(3) -0.021(3) 0.019(3) C30 0.073(4) 0.058(4) 0.038(3) -0.009(3) -0.014(3) 0.025(3) C31 0.064(3) 0.041(3) 0.035(3) -0.009(2) -0.007(2) 0.015(2) C32 0.049(3) 0.048(3) 0.043(3) -0.018(2) -0.001(2) 0.000(2) C33 0.067(4) 0.058(4) 0.068(4) -0.036(3) -0.006(3) 0.000(3) C34 0.074(4) 0.054(4) 0.056(4) -0.028(3) 0.002(3) 0.009(3) C35 0.052(3) 0.043(3) 0.031(3) -0.007(2) -0.001(2) 0.013(2) C36 0.054(3) 0.059(3) 0.036(3) -0.010(2) 0.004(2) 0.021(3) C37 0.043(3) 0.059(3) 0.037(3) -0.003(2) 0.006(2) 0.010(3) C38 0.041(3) 0.058(3) 0.029(2) 0.001(2) -0.001(2) 0.007(2) C39 0.038(3) 0.067(4) 0.053(3) -0.011(3) -0.001(2) -0.008(3) C40 0.051(3) 0.071(4) 0.063(4) -0.019(3) -0.006(3) -0.012(3) C41 0.045(3) 0.061(3) 0.051(3) -0.023(3) -0.009(2) 0.000(3) C42 0.040(3) 0.040(3) 0.024(2) 0.0011(19) -0.0036(19) 0.007(2) C43 0.041(3) 0.038(3) 0.026(2) -0.0026(19) -0.0020(19) 0.012(2) Cu2 0.0471(4) 0.0402(4) 0.0247(4) -0.0033(3) -0.0016(3) 0.0044(3) P3 0.0480(7) 0.0406(7) 0.0240(6) -0.0018(5) -0.0056(5) 0.0084(5) P4 0.0416(7) 0.0358(6) 0.0236(6) -0.0042(5) -0.0029(5) 0.0052(5) N4 0.041(2) 0.039(2) 0.0246(19) -0.0054(16) -0.0022(16) 0.0086(17) N5 0.049(2) 0.042(2) 0.027(2) -0.0029(17) -0.0073(17) 0.0080(19) N6 0.043(2) 0.042(2) 0.030(2) -0.0017(17) -0.0056(17) 0.0104(19) C45 0.062(4) 0.049(3) 0.042(3) -0.018(2) 0.006(2) -0.010(3) C46 0.042(3) 0.042(3) 0.025(2) -0.004(2) -0.0030(19) 0.003(2) C47 0.039(3) 0.038(3) 0.025(2) -0.0036(18) -0.0085(18) 0.0081(19) C48 0.051(3) 0.040(3) 0.037(3) -0.008(2) 0.002(2) -0.002(2) C44 0.073(4) 0.048(3) 0.048(3) -0.019(3) 0.012(3) -0.023(3) C49 0.042(3) 0.035(2) 0.028(2) -0.0018(19) -0.0076(19) 0.004(2) C50 0.048(3) 0.046(3) 0.042(3) -0.014(2) -0.005(2) -0.001(2) C51 0.056(3) 0.052(3) 0.037(3) -0.008(2) -0.006(2) -0.005(3) C52 0.080(5) 0.073(4) 0.049(4) -0.012(3) -0.006(3) -0.029(4) C53 0.118(7) 0.115(7) 0.057(4) -0.038(4) -0.001(4) -0.055(5) C54 0.151(8) 0.153(8) 0.040(4) -0.039(5) 0.017(4) -0.097(7) C55 0.102(6) 0.102(6) 0.038(3) -0.025(3) 0.008(3) -0.049(5) C56 0.041(3) 0.040(3) 0.024(2) -0.0032(19) -0.0007(19) 0.007(2) C57 0.059(3) 0.047(3) 0.031(3) -0.007(2) -0.007(2) 0.008(2) C58 0.088(5) 0.044(3) 0.043(3) -0.012(3) 0.000(3) 0.013(3) C59 0.075(4) 0.049(3) 0.045(3) -0.001(3) 0.006(3) 0.027(3) C60 0.054(3) 0.064(4) 0.047(3) 0.001(3) -0.010(3) 0.021(3) C61 0.047(3) 0.056(3) 0.034(3) -0.004(2) -0.008(2) 0.006(2) C62 0.046(3) 0.040(3) 0.028(2) -0.002(2) -0.008(2) 0.007(2) C63 0.072(4) 0.045(3) 0.030(3) -0.009(2) -0.017(2) 0.023(3) C64 0.076(5) 0.075(4) 0.055(4) -0.005(3) -0.034(3) -0.001(3) C65 0.112(6) 0.087(5) 0.087(6) -0.025(5) -0.062(5) 0.017(5) C66 0.123(7) 0.096(6) 0.066(5) -0.048(4) -0.060(5) 0.057(5) C67 0.126(7) 0.113(6) 0.032(3) -0.020(4) -0.026(4) 0.060(6) C68 0.079(4) 0.084(5) 0.035(3) -0.005(3) -0.014(3) 0.031(4) C69 0.052(3) 0.039(3) 0.023(2) 0.0026(19) -0.003(2) 0.007(2) C70 0.066(4) 0.054(3) 0.042(3) -0.009(3) -0.001(3) -0.003(3) C71 0.082(5) 0.066(4) 0.063(4) -0.023(3) -0.004(3) -0.018(4) C72 0.100(5) 0.043(3) 0.046(3) -0.011(3) -0.005(3) 0.001(3) C73 0.085(4) 0.042(3) 0.035(3) -0.002(2) -0.011(3) 0.014(3) C74 0.065(3) 0.042(3) 0.032(3) -0.001(2) -0.011(2) 0.012(2) C75 0.059(3) 0.051(3) 0.044(3) -0.013(3) -0.012(3) 0.001(3) C76 0.070(4) 0.059(4) 0.053(4) -0.023(3) -0.018(3) 0.007(3) C77 0.078(4) 0.067(4) 0.054(4) -0.034(3) -0.025(3) 0.022(3) C78 0.056(3) 0.060(3) 0.032(3) -0.014(2) -0.010(2) 0.027(3) C79 0.076(4) 0.075(4) 0.034(3) -0.017(3) -0.004(3) 0.034(4) C80 0.064(4) 0.066(4) 0.032(3) 0.000(3) 0.010(3) 0.029(3) C81 0.047(3) 0.054(3) 0.041(3) -0.001(2) 0.001(2) 0.023(3) C82 0.041(3) 0.053(3) 0.047(3) 0.011(3) 0.007(2) 0.011(3) C83 0.046(3) 0.048(3) 0.055(4) 0.006(3) -0.006(3) 0.004(2) C84 0.043(3) 0.043(3) 0.050(3) -0.005(2) -0.009(2) 0.005(2) C85 0.047(3) 0.046(3) 0.032(3) -0.006(2) -0.007(2) 0.020(2) C86 0.039(3) 0.045(3) 0.032(3) -0.002(2) -0.006(2) 0.019(2) C87 0.076(5) 0.144(8) 0.058(4) -0.046(5) -0.008(4) -0.018(5) C88 0.087(6) 0.154(10) 0.072(6) -0.048(6) -0.006(4) -0.034(6) C89 0.130(10) 0.159(11) 0.142(10) -0.097(9) -0.053(8) 0.008(8) C90 0.105(8) 0.212(15) 0.162(12) -0.141(12) -0.070(9) 0.051(9) C91 0.069(5) 0.179(11) 0.100(7) -0.087(8) -0.015(5) 0.001(7) C92 0.108(7) 0.171(10) 0.078(6) -0.063(7) -0.022(5) -0.036(7) C93 0.200(13) 0.175(12) 0.073(6) -0.021(7) -0.018(7) -0.097(11) C94 0.097(9) 0.247(18) 0.155(12) -0.135(13) -0.007(8) 0.004(10) C95 0.104(9) 0.240(18) 0.168(13) -0.157(14) -0.008(9) -0.025(11) C96 0.111(9) 0.151(11) 0.172(12) -0.119(10) -0.048(8) 0.020(7) C97 0.122(9) 0.110(8) 0.171(12) -0.077(8) -0.011(8) -0.009(7) C98 0.112(8) 0.111(8) 0.143(10) -0.077(8) -0.026(7) -0.013(6) C99 0.141(10) 0.141(10) 0.101(8) -0.065(7) -0.035(7) -0.018(8) C100 0.188(14) 0.163(12) 0.125(10) -0.046(9) -0.051(10) -0.024(11) F1 0.138(4) 0.074(3) 0.045(2) -0.0010(18) -0.011(2) -0.029(2) F2 0.121(3) 0.069(2) 0.058(2) -0.0166(19) -0.004(2) 0.026(2) F3 0.087(3) 0.087(3) 0.096(3) -0.017(2) -0.050(2) -0.020(2) F4 0.064(2) 0.073(2) 0.069(2) -0.0302(19) -0.0118(17) -0.0124(17) B1 0.070(4) 0.049(4) 0.043(3) -0.010(3) -0.014(3) -0.010(3) F5 0.226(8) 0.114(5) 0.141(5) -0.063(4) 0.001(5) -0.066(5) F6 0.123(5) 0.120(4) 0.136(5) 0.000(4) -0.053(4) -0.022(4) F7 0.153(5) 0.124(4) 0.071(3) 0.004(3) -0.053(3) -0.026(4) F8 0.162(5) 0.102(4) 0.073(3) -0.009(3) -0.007(3) -0.071(3) B2 0.084(6) 0.085(6) 0.067(5) -0.016(4) -0.028(4) -0.027(5) _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 2.054(4) . ? Cu1 N3 2.071(4) . ? Cu1 P2 2.2266(13) . ? Cu1 P1 2.2512(13) . ? P1 C13 1.823(5) . ? P1 C7 1.825(3) . ? P1 C6 1.859(5) . ? P2 C20 1.811(5) . ? P2 C26 1.816(5) . ? P2 C19 1.855(5) . ? N1 C19 1.462(7) . ? N1 C3 1.464(6) . ? N1 C6 1.469(7) . ? N2 C32 1.323(7) . ? N2 C43 1.378(6) . ? N3 C41 1.335(7) . ? N3 C42 1.366(6) . ? C2 C3 1.363(8) . ? C2 C1 1.416(8) . ? C2 H2A 0.9300 . ? C3 C4 1.391(7) . ? C4 C4 1.411(9) 2_755 ? C4 C5 1.461(8) . ? C5 C1 1.338(8) 2_755 ? C5 H5A 0.9300 . ? C1 C5 1.338(8) 2_755 ? C1 H1A 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.387(8) . ? C13 C14 1.388(7) . ? C14 C15 1.395(10) . ? C14 H14A 0.9300 . ? C15 C16 1.355(11) . ? C15 H15A 0.9300 . ? C16 C17 1.423(10) . ? C16 H16A 0.9300 . ? C17 C18 1.360(8) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.374(9) . ? C20 C25 1.384(8) . ? C21 C22 1.399(9) . ? C21 H21A 0.9300 . ? C22 C23 1.379(11) . ? C22 H22A 0.9300 . ? C23 C24 1.360(11) . ? C23 H23A 0.9300 . ? C24 C25 1.359(8) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.392(7) . ? C26 C31 1.405(7) . ? C27 C28 1.392(8) . ? C27 H27A 0.9300 . ? C28 C29 1.387(9) . ? C28 H28A 0.9300 . ? C29 C30 1.371(9) . ? C29 H29A 0.9300 . ? C30 C31 1.387(8) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.407(8) . ? C32 H32A 0.9300 . ? C33 C34 1.375(9) . ? C33 H33A 0.9300 . ? C34 C35 1.403(8) . ? C34 H34A 0.9300 . ? C35 C43 1.403(7) . ? C35 C36 1.436(8) . ? C36 C37 1.345(9) . ? C36 H36A 0.9300 . ? C37 C38 1.412(8) . ? C37 H37A 0.9300 . ? C38 C39 1.398(8) . ? C38 C42 1.406(7) . ? C39 C40 1.363(9) . ? C39 H39A 0.9300 . ? C40 C41 1.399(8) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C43 1.435(7) . ? Cu2 N6 2.061(4) . ? Cu2 N5 2.064(4) . ? Cu2 P4 2.2276(13) . ? Cu2 P3 2.2447(14) . ? P3 C69 1.810(5) . ? P3 C63 1.834(5) . ? P3 C62 1.848(5) . ? P4 C50 1.825(5) . ? P4 C56 1.832(5) . ? P4 C49 1.856(5) . ? N4 C46 1.458(6) . ? N4 C49 1.470(6) . ? N4 C62 1.475(6) . ? N5 C75 1.329(7) . ? N5 C85 1.355(7) . ? N6 C84 1.320(7) . ? N6 C86 1.370(7) . ? C45 C46 1.360(7) . ? C45 C44 1.419(8) . ? C45 H45A 0.9300 . ? C46 C47 1.415(7) . ? C47 C47 1.426(9) 2_665 ? C47 C48 1.428(7) . ? C48 C44 1.349(8) 2_665 ? C48 H48A 0.9300 . ? C44 C48 1.349(8) 2_665 ? C44 H44A 0.9300 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.370(8) . ? C50 C55 1.385(8) . ? C51 C52 1.367(8) . ? C51 H51A 0.9300 . ? C52 C53 1.360(10) . ? C52 H52A 0.9300 . ? C53 C54 1.367(10) . ? C53 H53A 0.9300 . ? C54 C55 1.378(9) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 C57 1.386(7) . ? C56 C61 1.391(7) . ? C57 C58 1.382(8) . ? C57 H57A 0.9300 . ? C58 C59 1.380(10) . ? C58 H58A 0.9300 . ? C59 C60 1.334(9) . ? C59 H59A 0.9300 . ? C60 C61 1.409(8) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.365(9) . ? C63 C68 1.389(8) . ? C64 C65 1.380(9) . ? C64 H64A 0.9300 . ? C65 C66 1.368(12) . ? C65 H65A 0.9300 . ? C66 C67 1.353(12) . ? C66 H66A 0.9300 . ? C67 C68 1.401(10) . ? C67 H67A 0.9300 . ? C68 H68A 0.9300 . ? C69 C70 1.386(8) . ? C69 C74 1.394(7) . ? C70 C71 1.392(9) . ? C70 H70A 0.9300 . ? C71 C72 1.375(10) . ? C71 H71A 0.9300 . ? C72 C73 1.367(10) . ? C72 H72A 0.9300 . ? C73 C74 1.382(8) . ? C73 H73A 0.9300 . ? C74 H74A 0.9300 . ? C75 C76 1.388(8) . ? C75 H75A 0.9300 . ? C76 C77 1.354(9) . ? C76 H76A 0.9300 . ? C77 C78 1.386(9) . ? C77 H77A 0.9300 . ? C78 C85 1.418(7) . ? C78 C79 1.440(8) . ? C79 C80 1.327(10) . ? C79 H79A 0.9300 . ? C80 C81 1.437(9) . ? C80 H80A 0.9300 . ? C81 C86 1.407(7) . ? C81 C82 1.412(9) . ? C82 C83 1.367(9) . ? C82 H82A 0.9300 . ? C83 C84 1.402(8) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? C85 C86 1.428(8) . ? C87 C88 1.372(13) . ? C87 C92 1.399(12) . ? C87 H87A 0.9300 . ? C88 C89 1.346(15) . ? C88 H88A 0.9300 . ? C89 C90 1.443(18) . ? C89 H89A 0.9300 . ? C90 C91 1.384(17) . ? C90 H90A 0.9300 . ? C91 C92 1.308(15) . ? C91 H91A 0.9300 . ? C92 C93 1.486(15) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 C99 1.348(16) . ? C94 C95 1.46(2) . ? C94 H94A 0.9300 . ? C95 C96 1.412(18) . ? C95 H95A 0.9300 . ? C96 C97 1.401(15) . ? C96 H96A 0.9300 . ? C97 C98 1.469(16) . ? C97 H97A 0.9300 . ? C98 C99 1.392(15) . ? C98 H98A 0.9300 . ? C99 C100 1.613(18) . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C100 H10D 0.9600 . ? F1 B1 1.367(8) . ? F2 B1 1.373(8) . ? F3 B1 1.398(8) . ? F4 B1 1.392(7) . ? F5 B2 1.275(11) . ? F6 B2 1.410(12) . ? F7 B2 1.323(9) . ? F8 B2 1.374(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 81.66(16) . . ? N2 Cu1 P2 118.27(11) . . ? N3 Cu1 P2 125.41(12) . . ? N2 Cu1 P1 110.67(11) . . ? N3 Cu1 P1 119.22(12) . . ? P2 Cu1 P1 101.16(5) . . ? C13 P1 C7 105.5(3) . . ? C13 P1 C6 101.3(2) . . ? C7 P1 C6 103.3(3) . . ? C13 P1 Cu1 112.41(16) . . ? C7 P1 Cu1 118.69(16) . . ? C6 P1 Cu1 113.76(16) . . ? C20 P2 C26 105.2(2) . . ? C20 P2 C19 102.0(2) . . ? C26 P2 C19 100.4(2) . . ? C20 P2 Cu1 118.73(19) . . ? C26 P2 Cu1 118.97(16) . . ? C19 P2 Cu1 108.74(16) . . ? C19 N1 C3 111.5(4) . . ? C19 N1 C6 113.7(4) . . ? C3 N1 C6 111.7(4) . . ? C32 N2 C43 117.7(4) . . ? C32 N2 Cu1 130.3(3) . . ? C43 N2 Cu1 111.8(3) . . ? C41 N3 C42 116.7(4) . . ? C41 N3 Cu1 131.7(3) . . ? C42 N3 Cu1 111.6(3) . . ? C3 C2 C1 122.2(6) . . ? C3 C2 H2A 118.9 . . ? C1 C2 H2A 118.9 . . ? C2 C3 C4 117.9(5) . . ? C2 C3 N1 124.0(5) . . ? C4 C3 N1 118.1(5) . . ? C3 C4 C4 122.6(6) . 2_755 ? C3 C4 C5 120.7(5) . . ? C4 C4 C5 116.7(6) 2_755 . ? C1 C5 C4 120.2(5) 2_755 . ? C1 C5 H5A 119.9 2_755 . ? C4 C5 H5A 119.9 . . ? C5 C1 C2 120.3(6) 2_755 . ? C5 C1 H1A 119.8 2_755 . ? C2 C1 H1A 119.8 . . ? N1 C6 P1 114.7(3) . . ? N1 C6 H6A 108.6 . . ? P1 C6 H6A 108.6 . . ? N1 C6 H6B 108.6 . . ? P1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 123.6(3) . . ? C12 C7 P1 116.4(3) . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? C18 C13 C14 119.1(5) . . ? C18 C13 P1 119.1(4) . . ? C14 C13 P1 121.2(5) . . ? C13 C14 C15 119.6(7) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 119.1(7) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C13 121.6(6) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? N1 C19 P2 110.6(4) . . ? N1 C19 H19A 109.5 . . ? P2 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C25 118.7(5) . . ? C21 C20 P2 118.1(4) . . ? C25 C20 P2 123.2(5) . . ? C20 C21 C22 120.1(7) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 118.8(7) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C24 C23 C22 121.3(6) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C23 119.2(7) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C24 C25 C20 121.8(6) . . ? C24 C25 H25A 119.1 . . ? C20 C25 H25A 119.1 . . ? C27 C26 C31 117.6(5) . . ? C27 C26 P2 118.3(4) . . ? C31 C26 P2 123.8(4) . . ? C28 C27 C26 121.8(5) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C29 C28 C27 119.2(6) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 120.8(5) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C26 120.5(5) . . ? C30 C31 H31A 119.8 . . ? C26 C31 H31A 119.8 . . ? N2 C32 C33 122.8(5) . . ? N2 C32 H32A 118.6 . . ? C33 C32 H32A 118.6 . . ? C34 C33 C32 119.8(6) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C35 119.1(5) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C43 C35 C34 117.8(5) . . ? C43 C35 C36 118.7(5) . . ? C34 C35 C36 123.4(5) . . ? C37 C36 C35 121.1(5) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 121.4(5) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C39 C38 C42 117.5(5) . . ? C39 C38 C37 122.9(5) . . ? C42 C38 C37 119.6(5) . . ? C40 C39 C38 120.0(5) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 118.8(6) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N3 C41 C40 123.8(5) . . ? N3 C41 H41A 118.1 . . ? C40 C41 H41A 118.1 . . ? N3 C42 C38 123.2(5) . . ? N3 C42 C43 117.5(4) . . ? C38 C42 C43 119.3(4) . . ? N2 C43 C35 122.8(5) . . ? N2 C43 C42 117.2(4) . . ? C35 C43 C42 119.9(4) . . ? N6 Cu2 N5 81.34(17) . . ? N6 Cu2 P4 129.89(12) . . ? N5 Cu2 P4 120.34(12) . . ? N6 Cu2 P3 115.74(11) . . ? N5 Cu2 P3 107.16(12) . . ? P4 Cu2 P3 100.84(5) . . ? C69 P3 C63 104.6(2) . . ? C69 P3 C62 102.6(2) . . ? C63 P3 C62 103.7(3) . . ? C69 P3 Cu2 118.36(18) . . ? C63 P3 Cu2 116.03(17) . . ? C62 P3 Cu2 109.86(16) . . ? C50 P4 C56 104.1(2) . . ? C50 P4 C49 105.0(2) . . ? C56 P4 C49 98.4(2) . . ? C50 P4 Cu2 116.99(18) . . ? C56 P4 Cu2 122.16(15) . . ? C49 P4 Cu2 107.43(15) . . ? C46 N4 C49 111.6(4) . . ? C46 N4 C62 110.0(4) . . ? C49 N4 C62 113.9(4) . . ? C75 N5 C85 117.7(5) . . ? C75 N5 Cu2 130.4(4) . . ? C85 N5 Cu2 111.8(4) . . ? C84 N6 C86 118.0(4) . . ? C84 N6 Cu2 130.4(4) . . ? C86 N6 Cu2 111.6(3) . . ? C46 C45 C44 120.6(5) . . ? C46 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? C45 C46 C47 119.8(4) . . ? C45 C46 N4 122.3(4) . . ? C47 C46 N4 117.9(4) . . ? C46 C47 C47 120.2(6) . 2_665 ? C46 C47 C48 122.1(4) . . ? C47 C47 C48 117.7(5) 2_665 . ? C44 C48 C47 121.0(5) 2_665 . ? C44 C48 H48A 119.5 2_665 . ? C47 C48 H48A 119.5 . . ? C48 C44 C45 120.7(5) 2_665 . ? C48 C44 H44A 119.6 2_665 . ? C45 C44 H44A 119.6 . . ? N4 C49 P4 113.0(3) . . ? N4 C49 H49A 109.0 . . ? P4 C49 H49A 109.0 . . ? N4 C49 H49B 109.0 . . ? P4 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? C51 C50 C55 117.8(5) . . ? C51 C50 P4 118.8(4) . . ? C55 C50 P4 123.3(4) . . ? C52 C51 C50 121.9(5) . . ? C52 C51 H51A 119.1 . . ? C50 C51 H51A 119.1 . . ? C53 C52 C51 119.8(6) . . ? C53 C52 H52A 120.1 . . ? C51 C52 H52A 120.1 . . ? C52 C53 C54 119.8(6) . . ? C52 C53 H53A 120.1 . . ? C54 C53 H53A 120.1 . . ? C53 C54 C55 120.3(6) . . ? C53 C54 H54A 119.8 . . ? C55 C54 H54A 119.8 . . ? C54 C55 C50 120.3(6) . . ? C54 C55 H55A 119.8 . . ? C50 C55 H55A 119.8 . . ? C57 C56 C61 118.5(5) . . ? C57 C56 P4 118.3(4) . . ? C61 C56 P4 123.1(4) . . ? C58 C57 C56 121.2(5) . . ? C58 C57 H57A 119.4 . . ? C56 C57 H57A 119.4 . . ? C59 C58 C57 119.3(6) . . ? C59 C58 H58A 120.3 . . ? C57 C58 H58A 120.3 . . ? C60 C59 C58 120.7(5) . . ? C60 C59 H59A 119.7 . . ? C58 C59 H59A 119.7 . . ? C59 C60 C61 121.2(6) . . ? C59 C60 H60A 119.4 . . ? C61 C60 H60A 119.4 . . ? C56 C61 C60 119.0(6) . . ? C56 C61 H61A 120.5 . . ? C60 C61 H61A 120.5 . . ? N4 C62 P3 111.0(3) . . ? N4 C62 H62A 109.4 . . ? P3 C62 H62A 109.4 . . ? N4 C62 H62B 109.4 . . ? P3 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C68 118.3(6) . . ? C64 C63 P3 125.6(4) . . ? C68 C63 P3 116.1(5) . . ? C63 C64 C65 121.6(7) . . ? C63 C64 H64A 119.2 . . ? C65 C64 H64A 119.2 . . ? C66 C65 C64 120.1(8) . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C67 C66 C65 119.7(6) . . ? C67 C66 H66A 120.2 . . ? C65 C66 H66A 120.2 . . ? C66 C67 C68 120.8(7) . . ? C66 C67 H67A 119.6 . . ? C68 C67 H67A 119.6 . . ? C63 C68 C67 119.6(7) . . ? C63 C68 H68A 120.2 . . ? C67 C68 H68A 120.2 . . ? C70 C69 C74 118.5(5) . . ? C70 C69 P3 118.3(4) . . ? C74 C69 P3 123.2(4) . . ? C69 C70 C71 120.6(6) . . ? C69 C70 H70A 119.7 . . ? C71 C70 H70A 119.7 . . ? C72 C71 C70 119.5(7) . . ? C72 C71 H71A 120.3 . . ? C70 C71 H71A 120.3 . . ? C73 C72 C71 120.9(6) . . ? C73 C72 H72A 119.5 . . ? C71 C72 H72A 119.5 . . ? C72 C73 C74 119.7(6) . . ? C72 C73 H73A 120.1 . . ? C74 C73 H73A 120.1 . . ? C73 C74 C69 120.7(6) . . ? C73 C74 H74A 119.6 . . ? C69 C74 H74A 119.6 . . ? N5 C75 C76 123.0(6) . . ? N5 C75 H75A 118.5 . . ? C76 C75 H75A 118.5 . . ? C77 C76 C75 119.7(6) . . ? C77 C76 H76A 120.2 . . ? C75 C76 H76A 120.2 . . ? C76 C77 C78 119.8(5) . . ? C76 C77 H77A 120.1 . . ? C78 C77 H77A 120.1 . . ? C77 C78 C85 117.5(5) . . ? C77 C78 C79 124.6(6) . . ? C85 C78 C79 117.9(6) . . ? C80 C79 C78 122.1(6) . . ? C80 C79 H79A 119.0 . . ? C78 C79 H79A 119.0 . . ? C79 C80 C81 121.3(5) . . ? C79 C80 H80A 119.4 . . ? C81 C80 H80A 119.4 . . ? C86 C81 C82 117.3(5) . . ? C86 C81 C80 118.8(6) . . ? C82 C81 C80 123.9(5) . . ? C83 C82 C81 119.3(5) . . ? C83 C82 H82A 120.3 . . ? C81 C82 H82A 120.3 . . ? C82 C83 C84 119.5(6) . . ? C82 C83 H83A 120.2 . . ? C84 C83 H83A 120.2 . . ? N6 C84 C83 123.1(6) . . ? N6 C84 H84A 118.4 . . ? C83 C84 H84A 118.4 . . ? N5 C85 C78 122.3(5) . . ? N5 C85 C86 117.7(5) . . ? C78 C85 C86 120.0(5) . . ? N6 C86 C81 122.7(5) . . ? N6 C86 C85 117.4(4) . . ? C81 C86 C85 120.0(5) . . ? C88 C87 C92 118.5(10) . . ? C88 C87 H87A 120.8 . . ? C92 C87 H87A 120.8 . . ? C89 C88 C87 123.3(10) . . ? C89 C88 H88A 118.4 . . ? C87 C88 H88A 118.4 . . ? C88 C89 C90 117.4(13) . . ? C88 C89 H89A 121.3 . . ? C90 C89 H89A 121.3 . . ? C91 C90 C89 117.6(11) . . ? C91 C90 H90A 121.2 . . ? C89 C90 H90A 121.2 . . ? C92 C91 C90 123.4(11) . . ? C92 C91 H91A 118.3 . . ? C90 C91 H91A 118.3 . . ? C91 C92 C87 119.9(12) . . ? C91 C92 C93 116.5(11) . . ? C87 C92 C93 123.6(12) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C99 C94 C95 114.9(16) . . ? C99 C94 H94A 122.5 . . ? C95 C94 H94A 122.5 . . ? C96 C95 C94 122.0(13) . . ? C96 C95 H95A 119.0 . . ? C94 C95 H95A 119.0 . . ? C97 C96 C95 121.6(13) . . ? C97 C96 H96A 119.2 . . ? C95 C96 H96A 119.2 . . ? C96 C97 C98 115.6(13) . . ? C96 C97 H97A 122.2 . . ? C98 C97 H97A 122.2 . . ? C99 C98 C97 120.2(12) . . ? C99 C98 H98A 119.9 . . ? C97 C98 H98A 119.9 . . ? C94 C99 C98 125.6(15) . . ? C94 C99 C100 114.7(14) . . ? C98 C99 C100 119.7(12) . . ? C99 C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10B C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? F1 B1 F2 110.3(6) . . ? F1 B1 F4 110.3(5) . . ? F2 B1 F4 108.1(5) . . ? F1 B1 F3 111.3(5) . . ? F2 B1 F3 109.8(5) . . ? F4 B1 F3 107.0(6) . . ? F5 B2 F7 121.4(9) . . ? F5 B2 F8 113.7(8) . . ? F7 B2 F8 108.4(6) . . ? F5 B2 F6 102.5(7) . . ? F7 B2 F6 102.4(8) . . ? F8 B2 F6 106.5(8) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 62.56 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.136 _refine_diff_density_min -1.871 _refine_diff_density_rms 0.094 # Attachment '- 3b.CIF' data_3b _database_code_depnum_ccdc_archive 'CCDC 815816' #TrackingRef '- 3b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H94 B2 Cu2 F8 N6 P4' _chemical_formula_weight 1852.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7492(5) _cell_length_b 17.7212(6) _cell_length_c 21.2195(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.035(4) _cell_angle_gamma 90.00 _cell_volume 4720.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4340 _cell_measurement_theta_min 3.2673 _cell_measurement_theta_max 61.1561 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8455 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16492 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 61.24 _reflns_number_total 7133 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1508P)^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 7133 _refine_ls_number_parameters 556 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2347 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.985 _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 0.73817(7) 0.73718(5) 0.67860(4) 0.0445(3) Uani 1 1 d . . . P1 P 0.74243(14) 0.86350(9) 0.68798(8) 0.0455(4) Uani 1 1 d . . . P2 P 0.58357(13) 0.71320(9) 0.61515(7) 0.0430(4) Uani 1 1 d . . . N1 N 0.5540(4) 0.8672(3) 0.5958(2) 0.0418(12) Uani 1 1 d . . . N2 N 0.8728(4) 0.6764(3) 0.6680(2) 0.0454(13) Uani 1 1 d . . . N3 N 0.7719(4) 0.6923(3) 0.7693(2) 0.0422(12) Uani 1 1 d . . . C1 C 0.3780(5) 0.9270(3) 0.5605(3) 0.0440(15) Uani 1 1 d . . . H1A H 0.3473 0.8940 0.5861 0.053 Uiso 1 1 calc R . . C2 C 0.4845(5) 0.9221(3) 0.5577(3) 0.0432(16) Uani 1 1 d . . . C3 C 0.5335(5) 0.9717(3) 0.5181(3) 0.0421(15) Uani 1 1 d . . . C4 C 0.6417(5) 0.9679(3) 0.5126(3) 0.0433(15) Uani 1 1 d . . . H4A H 0.6845 0.9306 0.5347 0.052 Uiso 1 1 calc R . . C5 C 0.6846(5) 1.0171(4) 0.4761(3) 0.0464(16) Uani 1 1 d . . . H5A H 0.7570 1.0143 0.4748 0.056 Uiso 1 1 calc R . . C6 C 0.6085(5) 0.9032(3) 0.6561(3) 0.0423(15) Uani 1 1 d . . . H6A H 0.5638 0.8978 0.6884 0.051 Uiso 1 1 calc R . . H6B H 0.6160 0.9568 0.6484 0.051 Uiso 1 1 calc R . . C7 C 0.8376(5) 0.9179(4) 0.6512(3) 0.0527(15) Uani 1 1 d U . . C8 C 0.9129(7) 0.8811(5) 0.6266(5) 0.087(2) Uani 1 1 d U . . H8A H 0.9169 0.8288 0.6301 0.105 Uiso 1 1 calc R . . C9 C 0.9845(8) 0.9187(6) 0.5964(6) 0.108(3) Uani 1 1 d U . . H9A H 1.0360 0.8918 0.5796 0.129 Uiso 1 1 calc R . . C10 C 0.9798(8) 0.9964(5) 0.5909(5) 0.086(2) Uani 1 1 d U . . H10A H 1.0272 1.0221 0.5699 0.103 Uiso 1 1 calc R . . C11 C 0.9065(6) 1.0341(4) 0.6161(4) 0.0637(17) Uani 1 1 d U . . H11A H 0.9039 1.0865 0.6135 0.076 Uiso 1 1 calc R . . C12 C 0.8351(6) 0.9965(4) 0.6459(3) 0.0539(16) Uani 1 1 d U . . H12A H 0.7841 1.0237 0.6628 0.065 Uiso 1 1 calc R . . C13 C 0.7615(5) 0.9000(3) 0.7702(3) 0.0485(17) Uani 1 1 d . . . C14 C 0.8382(6) 0.8643(4) 0.8160(3) 0.0578(19) Uani 1 1 d . . . H14A H 0.8821 0.8275 0.8031 0.069 Uiso 1 1 calc R . . C15 C 0.8492(6) 0.8832(4) 0.8803(3) 0.061(2) Uani 1 1 d . . . H15A H 0.9000 0.8588 0.9101 0.074 Uiso 1 1 calc R . . C16 C 0.7866(7) 0.9371(4) 0.8998(3) 0.074(2) Uani 1 1 d . . . H16A H 0.7933 0.9484 0.9431 0.089 Uiso 1 1 calc R . . C17 C 0.7125(7) 0.9754(4) 0.8554(3) 0.073(2) Uani 1 1 d . . . H17A H 0.6710 1.0134 0.8686 0.088 Uiso 1 1 calc R . . C18 C 0.7012(6) 0.9566(4) 0.7910(3) 0.061(2) Uani 1 1 d . . . H18A H 0.6519 0.9825 0.7613 0.074 Uiso 1 1 calc R . . C19 C 0.4968(5) 0.7982(3) 0.6072(3) 0.0440(15) Uani 1 1 d . . . H19A H 0.4382 0.7908 0.5719 0.053 Uiso 1 1 calc R . . H19B H 0.4671 0.8043 0.6459 0.053 Uiso 1 1 calc R . . C20 C 0.5900(5) 0.6867(3) 0.5325(3) 0.0463(16) Uani 1 1 d . . . C21 C 0.5989(6) 0.6112(4) 0.5173(3) 0.060(2) Uani 1 1 d . . . H21A H 0.5937 0.5744 0.5480 0.072 Uiso 1 1 calc R . . C22 C 0.6152(7) 0.5901(4) 0.4581(4) 0.072(2) Uani 1 1 d . . . H22A H 0.6197 0.5391 0.4487 0.087 Uiso 1 1 calc R . . C23 C 0.6253(7) 0.6437(5) 0.4113(4) 0.069(2) Uani 1 1 d . . . H23A H 0.6391 0.6291 0.3715 0.083 Uiso 1 1 calc R . . C24 C 0.6142(6) 0.7189(4) 0.4258(3) 0.063(2) Uani 1 1 d . . . H24A H 0.6184 0.7552 0.3947 0.075 Uiso 1 1 calc R . . C25 C 0.5969(6) 0.7410(4) 0.4854(3) 0.0530(17) Uani 1 1 d . . . H25A H 0.5898 0.7919 0.4944 0.064 Uiso 1 1 calc R . . C26 C 0.4952(5) 0.6422(3) 0.6398(3) 0.0457(16) Uani 1 1 d . . . C27 C 0.3888(6) 0.6374(4) 0.6103(3) 0.0556(18) Uani 1 1 d . . . H27A H 0.3624 0.6704 0.5773 0.067 Uiso 1 1 calc R . . C28 C 0.3224(6) 0.5840(4) 0.6298(4) 0.0615(19) Uani 1 1 d . . . H28A H 0.2513 0.5814 0.6102 0.074 Uiso 1 1 calc R . . C29 C 0.3623(6) 0.5339(4) 0.6789(3) 0.0609(19) Uani 1 1 d . . . H29A H 0.3178 0.4983 0.6928 0.073 Uiso 1 1 calc R . . C30 C 0.4673(6) 0.5379(4) 0.7063(3) 0.062(2) Uani 1 1 d . . . H30A H 0.4949 0.5036 0.7381 0.075 Uiso 1 1 calc R . . C31 C 0.5327(6) 0.5922(4) 0.6875(3) 0.0555(18) Uani 1 1 d . . . H31A H 0.6035 0.5948 0.7076 0.067 Uiso 1 1 calc R . . C32 C 0.9177(6) 0.6647(4) 0.6172(3) 0.0560(18) Uani 1 1 d . . . C33 C 1.0123(6) 0.6217(4) 0.6205(4) 0.065(2) Uani 1 1 d . . . H33A H 1.0413 0.6128 0.5839 0.078 Uiso 1 1 calc R . . C34 C 1.0594(6) 0.5938(4) 0.6777(4) 0.067(2) Uani 1 1 d . . . H34A H 1.1223 0.5664 0.6806 0.080 Uiso 1 1 calc R . . C35 C 1.0148(5) 0.6056(4) 0.7325(3) 0.0540(18) Uani 1 1 d . . . C36 C 0.9195(5) 0.6463(3) 0.7255(3) 0.0456(16) Uani 1 1 d . . . C37 C 1.0613(6) 0.5783(4) 0.7954(4) 0.066(2) Uani 1 1 d . . . H37A H 1.1233 0.5497 0.8003 0.079 Uiso 1 1 calc R . . C38 C 1.0169(6) 0.5934(4) 0.8466(4) 0.062(2) Uani 1 1 d . . . H38A H 1.0511 0.5780 0.8869 0.075 Uiso 1 1 calc R . . C39 C 0.9185(6) 0.6326(3) 0.8407(3) 0.0520(18) Uani 1 1 d . . . C40 C 0.8665(7) 0.6473(4) 0.8914(3) 0.061(2) Uani 1 1 d . . . H40A H 0.8976 0.6329 0.9326 0.073 Uiso 1 1 calc R . . C41 C 0.7704(7) 0.6828(4) 0.8819(3) 0.063(2) Uani 1 1 d . . . H41A H 0.7356 0.6922 0.9161 0.076 Uiso 1 1 calc R . . C42 C 0.7242(6) 0.7051(4) 0.8193(3) 0.0528(17) Uani 1 1 d . . . C43 C 0.8681(5) 0.6576(3) 0.7790(3) 0.0431(15) Uani 1 1 d . . . C44 C 0.8645(7) 0.6968(5) 0.5538(3) 0.074(2) Uani 1 1 d . . . H44A H 0.8019 0.7242 0.5594 0.111 Uiso 1 1 calc R . . H44B H 0.8449 0.6564 0.5239 0.111 Uiso 1 1 calc R . . H44C H 0.9129 0.7301 0.5376 0.111 Uiso 1 1 calc R . . C45 C 0.6177(6) 0.7426(4) 0.8083(4) 0.0633(19) Uani 1 1 d . . . H45A H 0.5971 0.7540 0.7636 0.095 Uiso 1 1 calc R . . H45B H 0.6215 0.7885 0.8326 0.095 Uiso 1 1 calc R . . H45C H 0.5660 0.7095 0.8215 0.095 Uiso 1 1 calc R . . C46 C 0.8898(11) 0.6821(10) 0.3447(7) 0.236(7) Uani 1 1 d GDU . . H46A H 0.9368 0.6777 0.3833 0.283 Uiso 1 1 calc R . . C47 C 0.8752(11) 0.6219(6) 0.3021(10) 0.246(7) Uani 1 1 d GDU . . H47A H 0.9125 0.5772 0.3121 0.295 Uiso 1 1 calc R . . C48 C 0.8049(14) 0.6285(8) 0.2444(8) 0.260(8) Uani 1 1 d GDU . . H48A H 0.7951 0.5883 0.2159 0.312 Uiso 1 1 calc R . . C49 C 0.7491(12) 0.6954(11) 0.2294(6) 0.260(8) Uani 1 1 d GDU . . H49A H 0.7020 0.6998 0.1908 0.311 Uiso 1 1 calc R . . C50 C 0.7636(12) 0.7556(7) 0.2720(10) 0.234(7) Uani 1 1 d GDU . . H50A H 0.7263 0.8003 0.2620 0.280 Uiso 1 1 calc R . . C51 C 0.8340(13) 0.7490(7) 0.3297(8) 0.229(7) Uani 1 1 d GDU . . C52 C 0.8386(10) 0.8270(8) 0.3622(10) 0.219(8) Uani 1 1 d DU . . H52A H 0.7906 0.8609 0.3363 0.329 Uiso 1 1 calc R . . H52B H 0.9098 0.8465 0.3672 0.329 Uiso 1 1 calc R . . H52C H 0.8182 0.8222 0.4035 0.329 Uiso 1 1 calc R . . B1 B 1.1489(8) 0.7552(7) 0.5216(4) 0.079(3) Uani 1 1 d . . . F1 F 1.1418(6) 0.6769(4) 0.5084(3) 0.137(2) Uani 1 1 d . . . F2 F 1.0845(5) 0.7907(5) 0.4750(3) 0.142(3) Uani 1 1 d . . . F3 F 1.2519(4) 0.7720(4) 0.5227(3) 0.119(2) Uani 1 1 d . . . F4 F 1.1149(6) 0.7620(3) 0.5787(3) 0.1148(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0530(6) 0.0322(5) 0.0423(5) 0.0048(4) -0.0081(4) 0.0033(4) P1 0.0541(10) 0.0303(8) 0.0446(9) 0.0034(7) -0.0122(8) 0.0014(7) P2 0.0526(10) 0.0286(8) 0.0419(8) 0.0034(7) -0.0086(7) 0.0019(7) N1 0.050(3) 0.027(3) 0.041(3) 0.002(2) -0.012(2) 0.003(2) N2 0.050(3) 0.036(3) 0.048(3) 0.002(2) 0.001(3) -0.003(2) N3 0.052(3) 0.031(3) 0.042(3) 0.002(2) 0.003(3) 0.000(2) C1 0.049(4) 0.034(4) 0.045(3) 0.000(3) -0.003(3) 0.003(3) C2 0.059(4) 0.028(3) 0.034(3) -0.001(3) -0.014(3) 0.005(3) C3 0.059(4) 0.026(3) 0.034(3) -0.003(2) -0.013(3) 0.002(3) C4 0.053(4) 0.031(3) 0.041(3) 0.000(3) -0.006(3) 0.008(3) C5 0.052(4) 0.039(4) 0.043(3) -0.002(3) -0.007(3) 0.004(3) C6 0.053(4) 0.030(3) 0.036(3) 0.002(3) -0.013(3) 0.003(3) C7 0.057(4) 0.034(3) 0.062(4) 0.000(3) -0.004(3) 0.003(3) C8 0.090(5) 0.047(4) 0.134(6) 0.005(4) 0.046(4) 0.002(4) C9 0.109(5) 0.064(4) 0.167(7) 0.000(5) 0.069(5) 0.000(4) C10 0.097(5) 0.054(4) 0.116(5) -0.003(4) 0.045(4) -0.012(4) C11 0.074(4) 0.044(4) 0.071(4) 0.002(3) 0.005(3) -0.009(3) C12 0.062(4) 0.040(3) 0.055(3) 0.000(3) -0.003(3) -0.003(3) C13 0.065(4) 0.027(3) 0.045(3) 0.006(3) -0.014(3) 0.000(3) C14 0.065(5) 0.037(4) 0.061(4) 0.000(3) -0.019(4) -0.003(3) C15 0.077(5) 0.047(4) 0.048(4) -0.001(3) -0.021(4) -0.004(4) C16 0.113(7) 0.050(5) 0.047(4) -0.005(4) -0.019(4) -0.006(5) C17 0.104(6) 0.048(5) 0.058(4) -0.015(4) -0.014(4) 0.011(4) C18 0.080(5) 0.040(4) 0.054(4) -0.006(3) -0.017(4) 0.007(4) C19 0.048(4) 0.030(3) 0.047(3) 0.003(3) -0.010(3) 0.003(3) C20 0.054(4) 0.037(4) 0.041(3) 0.001(3) -0.010(3) 0.001(3) C21 0.085(5) 0.042(4) 0.047(4) 0.002(3) -0.006(4) 0.011(4) C22 0.108(6) 0.039(4) 0.063(5) -0.003(4) -0.005(4) 0.016(4) C23 0.088(6) 0.064(5) 0.052(4) -0.009(4) -0.001(4) 0.009(4) C24 0.081(5) 0.056(5) 0.047(4) 0.007(3) 0.001(4) -0.006(4) C25 0.069(5) 0.038(4) 0.046(4) -0.003(3) -0.005(3) -0.001(3) C26 0.054(4) 0.031(3) 0.049(3) -0.006(3) -0.002(3) 0.001(3) C27 0.062(4) 0.035(4) 0.065(4) 0.003(3) -0.005(4) 0.005(3) C28 0.057(4) 0.048(4) 0.077(5) -0.001(4) 0.006(4) -0.003(4) C29 0.074(5) 0.040(4) 0.069(5) -0.002(4) 0.015(4) -0.010(4) C30 0.075(5) 0.044(4) 0.063(4) 0.011(3) -0.004(4) -0.001(4) C31 0.064(4) 0.034(4) 0.061(4) 0.010(3) -0.009(4) -0.003(3) C32 0.059(4) 0.051(4) 0.057(4) 0.005(3) 0.007(4) -0.002(4) C33 0.064(5) 0.061(5) 0.074(5) 0.008(4) 0.024(4) 0.004(4) C34 0.055(4) 0.054(5) 0.090(6) 0.018(4) 0.009(4) 0.010(4) C35 0.057(4) 0.042(4) 0.060(4) 0.006(3) 0.001(4) -0.001(3) C36 0.048(4) 0.030(3) 0.052(4) 0.001(3) -0.009(3) -0.001(3) C37 0.060(5) 0.046(4) 0.084(5) 0.024(4) -0.009(4) 0.006(4) C38 0.068(5) 0.049(5) 0.061(5) 0.019(4) -0.013(4) -0.005(4) C39 0.064(4) 0.032(4) 0.053(4) 0.006(3) -0.011(4) -0.002(3) C40 0.080(5) 0.049(5) 0.046(4) 0.010(3) -0.011(4) -0.010(4) C41 0.087(6) 0.051(5) 0.045(4) 0.000(3) -0.003(4) -0.007(4) C42 0.055(4) 0.034(4) 0.065(4) 0.011(3) 0.000(4) -0.005(3) C43 0.052(4) 0.027(3) 0.047(3) 0.002(3) -0.002(3) -0.005(3) C44 0.073(5) 0.097(7) 0.050(4) 0.007(4) 0.002(4) -0.002(5) C45 0.070(5) 0.056(5) 0.064(4) -0.002(4) 0.012(4) -0.004(4) C46 0.210(14) 0.153(11) 0.328(17) 0.001(12) 0.002(13) -0.046(11) C47 0.261(16) 0.127(10) 0.338(19) 0.027(11) 0.019(14) -0.071(11) C48 0.315(18) 0.162(12) 0.289(18) -0.003(13) 0.017(14) -0.043(13) C49 0.320(17) 0.184(14) 0.256(16) 0.051(12) 0.001(14) -0.013(14) C50 0.239(15) 0.133(11) 0.307(17) 0.057(11) -0.011(13) 0.011(12) C51 0.203(14) 0.158(11) 0.319(17) 0.003(12) 0.023(12) -0.029(11) C52 0.094(9) 0.121(10) 0.42(2) 0.012(13) -0.003(13) -0.036(8) B1 0.068(6) 0.116(10) 0.047(5) 0.014(6) -0.003(5) 0.004(6) F1 0.162(6) 0.125(6) 0.131(5) -0.040(4) 0.043(5) -0.029(5) F2 0.088(4) 0.230(8) 0.106(4) 0.071(5) 0.014(3) 0.045(4) F3 0.078(3) 0.145(5) 0.117(4) 0.061(4) -0.028(3) -0.024(3) F4 0.167(6) 0.094(4) 0.086(4) 0.002(3) 0.028(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.057(5) . ? Cu1 N2 2.071(6) . ? Cu1 P2 2.2257(17) . ? Cu1 P1 2.2472(18) . ? P1 C7 1.828(7) . ? P1 C13 1.837(6) . ? P1 C6 1.862(6) . ? P2 C26 1.825(7) . ? P2 C20 1.831(6) . ? P2 C19 1.859(6) . ? N1 C2 1.462(7) . ? N1 C19 1.464(8) . ? N1 C6 1.488(7) . ? N2 C32 1.322(9) . ? N2 C36 1.369(8) . ? N3 C42 1.331(9) . ? N3 C43 1.356(8) . ? C1 C2 1.373(9) . ? C1 C5 1.416(8) 3_676 ? C1 H1A 0.9300 . ? C2 C3 1.431(9) . ? C3 C4 1.406(9) . ? C3 C3 1.448(11) 3_676 ? C4 C5 1.343(9) . ? C4 H4A 0.9300 . ? C5 C1 1.416(8) 3_676 ? C5 H5A 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.338(11) . ? C7 C12 1.398(9) . ? C8 C9 1.377(12) . ? C8 H8A 0.9300 . ? C9 C10 1.383(13) . ? C9 H9A 0.9300 . ? C10 C11 1.335(11) . ? C10 H10A 0.9300 . ? C11 C12 1.368(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.382(10) . ? C13 C14 1.404(8) . ? C14 C15 1.387(10) . ? C14 H14A 0.9300 . ? C15 C16 1.354(11) . ? C15 H15A 0.9300 . ? C16 C17 1.390(10) . ? C16 H16A 0.9300 . ? C17 C18 1.389(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.387(9) . ? C20 C25 1.401(9) . ? C21 C22 1.361(10) . ? C21 H21A 0.9300 . ? C22 C23 1.396(11) . ? C22 H22A 0.9300 . ? C23 C24 1.380(10) . ? C23 H23A 0.9300 . ? C24 C25 1.379(10) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C31 1.368(9) . ? C26 C27 1.395(9) . ? C27 C28 1.380(10) . ? C27 H27A 0.9300 . ? C28 C29 1.396(10) . ? C28 H28A 0.9300 . ? C29 C30 1.366(10) . ? C29 H29A 0.9300 . ? C30 C31 1.376(10) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.418(10) . ? C32 C44 1.509(10) . ? C33 C34 1.351(10) . ? C33 H33A 0.9300 . ? C34 C35 1.397(10) . ? C34 H34A 0.9300 . ? C35 C36 1.399(9) . ? C35 C37 1.445(9) . ? C36 C43 1.421(9) . ? C37 C38 1.337(11) . ? C37 H37A 0.9300 . ? C38 C39 1.420(10) . ? C38 H38A 0.9300 . ? C39 C40 1.384(10) . ? C39 C43 1.424(9) . ? C40 C41 1.359(11) . ? C40 H40A 0.9300 . ? C41 C42 1.412(9) . ? C41 H41A 0.9300 . ? C42 C45 1.494(10) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C46 H46A 0.9300 . ? C47 C48 1.3900 . ? C47 H47A 0.9300 . ? C48 C49 1.3900 . ? C48 H48A 0.9300 . ? C49 C50 1.3900 . ? C49 H49A 0.9300 . ? C50 C51 1.3900 . ? C50 H50A 0.9300 . ? C51 C52 1.543(14) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? B1 F2 1.328(10) . ? B1 F3 1.342(11) . ? B1 F4 1.362(11) . ? B1 F1 1.415(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 81.9(2) . . ? N3 Cu1 P2 120.71(16) . . ? N2 Cu1 P2 119.89(15) . . ? N3 Cu1 P1 107.71(14) . . ? N2 Cu1 P1 121.33(15) . . ? P2 Cu1 P1 104.41(7) . . ? C7 P1 C13 103.4(3) . . ? C7 P1 C6 106.3(3) . . ? C13 P1 C6 100.0(3) . . ? C7 P1 Cu1 119.7(2) . . ? C13 P1 Cu1 115.6(2) . . ? C6 P1 Cu1 109.8(2) . . ? C26 P2 C20 103.3(3) . . ? C26 P2 C19 101.4(3) . . ? C20 P2 C19 104.2(3) . . ? C26 P2 Cu1 118.9(2) . . ? C20 P2 Cu1 116.5(2) . . ? C19 P2 Cu1 110.5(2) . . ? C2 N1 C19 112.1(5) . . ? C2 N1 C6 109.7(4) . . ? C19 N1 C6 112.9(5) . . ? C32 N2 C36 118.8(6) . . ? C32 N2 Cu1 130.9(4) . . ? C36 N2 Cu1 110.2(4) . . ? C42 N3 C43 118.8(5) . . ? C42 N3 Cu1 129.1(4) . . ? C43 N3 Cu1 110.8(4) . . ? C2 C1 C5 119.1(6) . 3_676 ? C2 C1 H1A 120.4 . . ? C5 C1 H1A 120.4 3_676 . ? C1 C2 C3 121.6(5) . . ? C1 C2 N1 121.7(6) . . ? C3 C2 N1 116.7(5) . . ? C4 C3 C2 123.7(5) . . ? C4 C3 C3 119.0(7) . 3_676 ? C2 C3 C3 117.3(8) . 3_676 ? C5 C4 C3 121.4(6) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C1 121.6(6) . 3_676 ? C4 C5 H5A 119.2 . . ? C1 C5 H5A 119.2 3_676 . ? N1 C6 P1 114.3(4) . . ? N1 C6 H6A 108.7 . . ? P1 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? P1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C12 117.6(7) . . ? C8 C7 P1 118.9(6) . . ? C12 C7 P1 123.5(6) . . ? C7 C8 C9 121.6(8) . . ? C7 C8 H8A 119.2 . . ? C9 C8 H8A 119.2 . . ? C10 C9 C8 119.9(9) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 119.2(9) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C10 C11 C12 120.7(7) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 121.0(7) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? C18 C13 C14 117.7(6) . . ? C18 C13 P1 124.7(5) . . ? C14 C13 P1 117.4(5) . . ? C15 C14 C13 120.6(7) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 120.3(7) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C13 C18 C17 121.4(6) . . ? C13 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? N1 C19 P2 112.7(4) . . ? N1 C19 H19A 109.0 . . ? P2 C19 H19A 109.0 . . ? N1 C19 H19B 109.0 . . ? P2 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C25 118.6(6) . . ? C21 C20 P2 119.3(5) . . ? C25 C20 P2 121.7(5) . . ? C22 C21 C20 120.7(7) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C21 C22 C23 121.2(7) . . ? C21 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C24 C23 C22 118.2(7) . . ? C24 C23 H23A 120.9 . . ? C22 C23 H23A 120.9 . . ? C25 C24 C23 121.2(7) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C20 120.0(6) . . ? C24 C25 H25A 120.0 . . ? C20 C25 H25A 120.0 . . ? C31 C26 C27 118.6(6) . . ? C31 C26 P2 120.4(5) . . ? C27 C26 P2 120.9(5) . . ? C28 C27 C26 120.5(6) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 119.8(7) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 119.2(7) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C29 C30 C31 120.7(7) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C26 C31 C30 121.1(6) . . ? C26 C31 H31A 119.4 . . ? C30 C31 H31A 119.4 . . ? N2 C32 C33 122.0(6) . . ? N2 C32 C44 118.5(6) . . ? C33 C32 C44 119.5(7) . . ? C34 C33 C32 118.8(7) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C33 C34 C35 120.8(7) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C34 C35 C36 117.4(6) . . ? C34 C35 C37 123.9(7) . . ? C36 C35 C37 118.6(7) . . ? N2 C36 C35 122.0(6) . . ? N2 C36 C43 117.9(6) . . ? C35 C36 C43 120.0(6) . . ? C38 C37 C35 121.3(7) . . ? C38 C37 H37A 119.3 . . ? C35 C37 H37A 119.3 . . ? C37 C38 C39 121.2(6) . . ? C37 C38 H38A 119.4 . . ? C39 C38 H38A 119.4 . . ? C40 C39 C43 117.1(6) . . ? C40 C39 C38 124.0(6) . . ? C43 C39 C38 118.9(7) . . ? C41 C40 C39 120.8(6) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C40 C41 C42 119.2(7) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? N3 C42 C41 121.9(7) . . ? N3 C42 C45 118.6(6) . . ? C41 C42 C45 119.4(7) . . ? N3 C43 C39 122.2(6) . . ? N3 C43 C36 118.2(5) . . ? C39 C43 C36 119.6(6) . . ? C32 C44 H44A 109.5 . . ? C32 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C32 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 120.0 . . ? C47 C46 H46A 120.0 . . ? C51 C46 H46A 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 C52 106.7(16) . . ? C46 C51 C52 133.1(15) . . ? 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 . . ? F2 B1 F3 112.6(9) . . ? F2 B1 F4 111.6(9) . . ? F3 B1 F4 115.2(8) . . ? F2 B1 F1 107.9(9) . . ? F3 B1 F1 104.5(9) . . ? F4 B1 F1 104.1(8) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 61.24 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.215 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.102 # Attachment '- 4a.CIF' data_4a _database_code_depnum_ccdc_archive 'CCDC 815817' #TrackingRef '- 4a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H75 B2 Cu2 F8 N7 O0 P4' _chemical_formula_weight 1679.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.227(2) _cell_length_b 23.148(3) _cell_length_c 16.976(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.134(2) _cell_angle_gamma 90.00 _cell_volume 8123.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2167 _cell_measurement_theta_min 5.283 _cell_measurement_theta_max 53.851 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7565 _exptl_absorpt_correction_T_max 0.8394 _exptl_absorpt_process_details ? _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 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 17.22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35319 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14209 _reflns_number_gt 10597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0920P)^2^+1.8663P] 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 14209 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.068311(18) 0.423876(15) 0.24912(2) 0.02494(12) Uani 1 1 d . . . Cu2 Cu 0.426150(17) -0.158221(15) 0.22533(2) 0.02529(12) Uani 1 1 d . . . P1 P 0.04461(4) 0.37447(3) 0.13303(5) 0.02425(19) Uani 1 1 d . . . P2 P 0.08889(4) 0.35954(3) 0.34800(5) 0.02450(19) Uani 1 1 d . . . P3 P 0.43555(4) -0.10665(3) 0.33823(5) 0.02550(19) Uani 1 1 d . . . P4 P 0.41867(4) -0.09558(3) 0.12395(5) 0.02582(19) Uani 1 1 d . . . N1 N 0.07322(12) 0.27658(10) 0.22434(15) 0.0245(6) Uani 1 1 d . . . N2 N 0.42289(12) -0.01019(11) 0.23803(16) 0.0275(6) Uani 1 1 d . . . N3 N -0.00934(12) 0.47508(11) 0.25443(16) 0.0283(6) Uani 1 1 d . . . N4 N 0.11452(12) 0.50220(10) 0.25572(15) 0.0255(6) Uani 1 1 d . . . N5 N 0.50626(12) -0.20985(12) 0.23469(16) 0.0299(6) Uani 1 1 d . . . N6 N 0.37938(13) -0.23583(11) 0.20720(18) 0.0336(7) Uani 1 1 d . . . C1 C 0.12321(14) 0.23864(12) 0.21763(18) 0.0221(6) Uani 1 1 d . . . C2 C 0.17481(15) 0.22992(12) 0.28338(19) 0.0261(7) Uani 1 1 d . . . H2A H 0.1784 0.2532 0.3303 0.031 Uiso 1 1 calc R . . C3 C 0.22095(14) 0.18817(12) 0.28206(19) 0.0246(7) Uani 1 1 d . . . H3A H 0.2556 0.1836 0.3282 0.030 Uiso 1 1 calc R . . C4 C 0.21850(15) 0.15264(12) 0.21570(19) 0.0245(7) Uani 1 1 d . . . C5 C 0.16837(15) 0.16309(13) 0.14880(19) 0.0283(7) Uani 1 1 d . . . H5A H 0.1661 0.1408 0.1012 0.034 Uiso 1 1 calc R . . C6 C 0.12169(15) 0.20480(13) 0.14897(19) 0.0283(7) Uani 1 1 d . . . H6A H 0.0882 0.2105 0.1019 0.034 Uiso 1 1 calc R . . C7 C 0.26650(14) 0.10605(12) 0.21814(19) 0.0239(7) Uani 1 1 d . . . C8 C 0.29263(15) 0.07699(13) 0.28995(19) 0.0267(7) Uani 1 1 d . . . H8A H 0.2760 0.0850 0.3362 0.032 Uiso 1 1 calc R . . C9 C 0.34186(15) 0.03690(13) 0.29647(19) 0.0273(7) Uani 1 1 d . . . H9A H 0.3580 0.0177 0.3464 0.033 Uiso 1 1 calc R . . C10 C 0.36796(14) 0.02450(12) 0.22993(19) 0.0252(7) Uani 1 1 d . . . C11 C 0.33909(15) 0.05047(13) 0.1565(2) 0.0299(7) Uani 1 1 d . . . H11A H 0.3536 0.0406 0.1093 0.036 Uiso 1 1 calc R . . C12 C 0.28990(15) 0.09019(13) 0.1510(2) 0.0289(7) Uani 1 1 d . . . H12A H 0.2715 0.1072 0.1000 0.035 Uiso 1 1 calc R . . C13 C 0.02624(14) 0.29813(12) 0.15441(19) 0.0250(7) Uani 1 1 d . . . H13A H -0.0177 0.2958 0.1648 0.030 Uiso 1 1 calc R . . H13B H 0.0272 0.2739 0.1067 0.030 Uiso 1 1 calc R . . C14 C 0.10789(15) 0.36825(13) 0.07659(19) 0.0264(7) Uani 1 1 d . . . C15 C 0.17126(16) 0.37883(16) 0.1177(2) 0.0382(8) Uani 1 1 d . . . H15A H 0.1802 0.3882 0.1736 0.046 Uiso 1 1 calc R . . C16 C 0.22162(19) 0.37583(18) 0.0782(3) 0.0490(10) Uani 1 1 d . . . H16A H 0.2649 0.3826 0.1069 0.059 Uiso 1 1 calc R . . C17 C 0.20808(19) 0.36299(17) -0.0030(2) 0.0473(10) Uani 1 1 d . . . H17A H 0.2423 0.3610 -0.0306 0.057 Uiso 1 1 calc R . . C18 C 0.14539(19) 0.35297(16) -0.0446(2) 0.0424(9) Uani 1 1 d . . . H18A H 0.1365 0.3444 -0.1008 0.051 Uiso 1 1 calc R . . C19 C 0.09547(17) 0.35530(14) -0.0051(2) 0.0358(8) Uani 1 1 d . . . H19A H 0.0524 0.3480 -0.0340 0.043 Uiso 1 1 calc R . . C20 C -0.02682(15) 0.39630(13) 0.05715(19) 0.0281(7) Uani 1 1 d . . . C21 C -0.06626(17) 0.35788(15) 0.0044(2) 0.0366(8) Uani 1 1 d . . . H21A H -0.0564 0.3178 0.0076 0.044 Uiso 1 1 calc R . . C22 C -0.11910(17) 0.37719(17) -0.0522(2) 0.0429(9) Uani 1 1 d . . . H22A H -0.1451 0.3507 -0.0883 0.051 Uiso 1 1 calc R . . C23 C -0.13425(17) 0.43560(17) -0.0563(2) 0.0413(9) Uani 1 1 d . . . H23A H -0.1710 0.4490 -0.0950 0.050 Uiso 1 1 calc R . . C24 C -0.09653(17) 0.47427(16) -0.0047(2) 0.0374(8) Uani 1 1 d . . . H24A H -0.1071 0.5142 -0.0078 0.045 Uiso 1 1 calc R . . C25 C -0.04282(16) 0.45467(14) 0.0521(2) 0.0308(7) Uani 1 1 d . . . H25A H -0.0168 0.4814 0.0878 0.037 Uiso 1 1 calc R . . C26 C 0.05850(15) 0.28847(12) 0.30252(19) 0.0250(7) Uani 1 1 d . . . H26A H 0.0774 0.2574 0.3407 0.030 Uiso 1 1 calc R . . H26B H 0.0110 0.2872 0.2962 0.030 Uiso 1 1 calc R . . C27 C 0.17154(15) 0.34393(12) 0.40184(19) 0.0259(7) Uani 1 1 d . . . C28 C 0.22315(16) 0.36643(14) 0.3734(2) 0.0324(8) Uani 1 1 d . . . H28A H 0.2152 0.3941 0.3310 0.039 Uiso 1 1 calc R . . C29 C 0.28574(16) 0.34882(15) 0.4062(2) 0.0384(8) Uani 1 1 d . . . H29A H 0.3203 0.3638 0.3854 0.046 Uiso 1 1 calc R . . C30 C 0.29827(17) 0.30997(15) 0.4686(2) 0.0375(8) Uani 1 1 d . . . H30A H 0.3415 0.2982 0.4911 0.045 Uiso 1 1 calc R . . C31 C 0.24792(17) 0.28765(14) 0.4992(2) 0.0356(8) Uani 1 1 d . . . H31A H 0.2566 0.2609 0.5428 0.043 Uiso 1 1 calc R . . C32 C 0.18525(16) 0.30455(13) 0.46595(19) 0.0304(7) Uani 1 1 d . . . H32A H 0.1509 0.2892 0.4869 0.036 Uiso 1 1 calc R . . C33 C 0.04485(16) 0.36911(14) 0.42816(19) 0.0305(7) Uani 1 1 d . . . C34 C -0.00545(17) 0.33402(18) 0.4391(2) 0.0453(10) Uani 1 1 d . . . H34A H -0.0164 0.3004 0.4069 0.054 Uiso 1 1 calc R . . C35 C -0.03964(19) 0.3479(2) 0.4967(2) 0.0558(12) Uani 1 1 d . . . H35A H -0.0746 0.3240 0.5030 0.067 Uiso 1 1 calc R . . C36 C -0.0239(2) 0.3955(2) 0.5448(2) 0.0544(12) Uani 1 1 d . . . H36A H -0.0480 0.4046 0.5839 0.065 Uiso 1 1 calc R . . C37 C 0.0270(2) 0.43019(17) 0.5363(2) 0.0517(11) Uani 1 1 d . . . H37A H 0.0385 0.4629 0.5704 0.062 Uiso 1 1 calc R . . C38 C 0.06169(19) 0.41735(15) 0.4777(2) 0.0415(9) Uani 1 1 d . . . H38A H 0.0966 0.4414 0.4716 0.050 Uiso 1 1 calc R . . C39 C 0.45879(15) -0.03180(13) 0.3163(2) 0.0295(7) Uani 1 1 d . . . H39A H 0.4512 -0.0057 0.3594 0.035 Uiso 1 1 calc R . . H39B H 0.5056 -0.0310 0.3175 0.035 Uiso 1 1 calc R . . C40 C 0.36890(16) -0.09541(14) 0.3871(2) 0.0321(8) Uani 1 1 d . . . C41 C 0.3776(2) -0.06707(16) 0.4610(2) 0.0451(10) Uani 1 1 d . . . H41A H 0.4198 -0.0567 0.4901 0.054 Uiso 1 1 calc R . . C42 C 0.3237(3) -0.0539(2) 0.4921(3) 0.0646(14) Uani 1 1 d . . . H42A H 0.3290 -0.0348 0.5427 0.078 Uiso 1 1 calc R . . C43 C 0.2624(3) -0.0690(2) 0.4485(4) 0.0747(16) Uani 1 1 d . . . H43A H 0.2257 -0.0586 0.4688 0.090 Uiso 1 1 calc R . . C44 C 0.2537(2) -0.0984(2) 0.3776(3) 0.0686(14) Uani 1 1 d . . . H44A H 0.2115 -0.1096 0.3496 0.082 Uiso 1 1 calc R . . C45 C 0.30713(17) -0.11187(16) 0.3460(3) 0.0443(9) Uani 1 1 d . . . H45A H 0.3013 -0.1324 0.2964 0.053 Uiso 1 1 calc R . . C46 C 0.50149(16) -0.12903(15) 0.4214(2) 0.0341(8) Uani 1 1 d . . . C47 C 0.55917(18) -0.0991(2) 0.4455(2) 0.0510(10) Uani 1 1 d . . . H47A H 0.5650 -0.0633 0.4208 0.061 Uiso 1 1 calc R . . C48 C 0.6087(2) -0.1216(2) 0.5062(3) 0.0638(13) Uani 1 1 d . . . H48A H 0.6479 -0.1006 0.5232 0.077 Uiso 1 1 calc R . . C49 C 0.6017(2) -0.1731(2) 0.5414(3) 0.0610(12) Uani 1 1 d . . . H49A H 0.6363 -0.1884 0.5815 0.073 Uiso 1 1 calc R . . C50 C 0.5445(2) -0.2032(2) 0.5189(3) 0.0699(14) Uani 1 1 d . . . H50A H 0.5391 -0.2388 0.5443 0.084 Uiso 1 1 calc R . . C51 C 0.4942(2) -0.18074(18) 0.4584(3) 0.0565(11) Uani 1 1 d . . . H51A H 0.4546 -0.2014 0.4427 0.068 Uiso 1 1 calc R . . C52 C 0.45059(15) -0.02520(13) 0.1698(2) 0.0289(7) Uani 1 1 d . . . H52A H 0.4982 -0.0276 0.1882 0.035 Uiso 1 1 calc R . . H52B H 0.4403 0.0056 0.1284 0.035 Uiso 1 1 calc R . . C53 C 0.33892(16) -0.07600(13) 0.0641(2) 0.0302(7) Uani 1 1 d . . . C54 C 0.28496(16) -0.09027(16) 0.0931(2) 0.0400(9) Uani 1 1 d . . . H54A H 0.2897 -0.1134 0.1404 0.048 Uiso 1 1 calc R . . C55 C 0.22372(19) -0.07092(19) 0.0534(3) 0.0559(11) Uani 1 1 d . . . H55A H 0.1868 -0.0804 0.0736 0.067 Uiso 1 1 calc R . . C56 C 0.2175(2) -0.03795(19) -0.0155(3) 0.0591(12) Uani 1 1 d . . . H56A H 0.1760 -0.0246 -0.0428 0.071 Uiso 1 1 calc R . . C57 C 0.27131(19) -0.02398(17) -0.0453(2) 0.0484(10) Uani 1 1 d . . . H57A H 0.2665 -0.0011 -0.0928 0.058 Uiso 1 1 calc R . . C58 C 0.33146(18) -0.04329(15) -0.0062(2) 0.0394(8) Uani 1 1 d . . . H58A H 0.3681 -0.0343 -0.0273 0.047 Uiso 1 1 calc R . . C59 C 0.46651(16) -0.10734(14) 0.0484(2) 0.0323(8) Uani 1 1 d . . . C60 C 0.52742(17) -0.08293(15) 0.0549(2) 0.0381(8) Uani 1 1 d . . . H60A H 0.5446 -0.0576 0.0985 0.046 Uiso 1 1 calc R . . C61 C 0.56309(19) -0.09536(17) -0.0020(2) 0.0444(9) Uani 1 1 d . . . H61A H 0.6047 -0.0788 0.0029 0.053 Uiso 1 1 calc R . . C62 C 0.5381(2) -0.13176(17) -0.0654(2) 0.0488(10) Uani 1 1 d . . . H62A H 0.5624 -0.1397 -0.1047 0.059 Uiso 1 1 calc R . . C63 C 0.4786(2) -0.15667(19) -0.0725(3) 0.0581(12) Uani 1 1 d . . . H63A H 0.4618 -0.1821 -0.1162 0.070 Uiso 1 1 calc R . . C64 C 0.4427(2) -0.14444(17) -0.0149(2) 0.0496(10) Uani 1 1 d . . . H64A H 0.4015 -0.1619 -0.0194 0.059 Uiso 1 1 calc R . . C65 C -0.07012(16) 0.46083(16) 0.2521(2) 0.0380(8) Uani 1 1 d . . . H65A H -0.0807 0.4212 0.2557 0.046 Uiso 1 1 calc R . . C66 C -0.11963(18) 0.50232(18) 0.2444(2) 0.0469(10) Uani 1 1 d . . . H66A H -0.1628 0.4908 0.2432 0.056 Uiso 1 1 calc R . . C67 C -0.10511(19) 0.55850(18) 0.2388(2) 0.0474(10) Uani 1 1 d . . . H67A H -0.1384 0.5867 0.2326 0.057 Uiso 1 1 calc R . . C68 C -0.04117(18) 0.57579(15) 0.2420(2) 0.0375(8) Uani 1 1 d . . . C69 C 0.00549(16) 0.53208(13) 0.24985(19) 0.0280(7) Uani 1 1 d . . . C70 C -0.0203(2) 0.63490(16) 0.2399(2) 0.0472(10) Uani 1 1 d . . . H70A H -0.0517 0.6649 0.2334 0.057 Uiso 1 1 calc R . . C71 C 0.0421(2) 0.64882(15) 0.2467(2) 0.0434(10) Uani 1 1 d . . . H71A H 0.0542 0.6883 0.2464 0.052 Uiso 1 1 calc R . . C72 C 0.09053(18) 0.60501(14) 0.2544(2) 0.0352(8) Uani 1 1 d . . . C73 C 0.07181(15) 0.54692(13) 0.25307(18) 0.0266(7) Uani 1 1 d . . . C74 C 0.15638(18) 0.61754(14) 0.2628(2) 0.0378(8) Uani 1 1 d . . . H74A H 0.1710 0.6564 0.2661 0.045 Uiso 1 1 calc R . . C75 C 0.19944(18) 0.57268(14) 0.2661(2) 0.0363(8) Uani 1 1 d . . . H75A H 0.2443 0.5800 0.2722 0.044 Uiso 1 1 calc R . . C76 C 0.17588(16) 0.51604(13) 0.2603(2) 0.0301(7) Uani 1 1 d . . . H76A H 0.2057 0.4856 0.2597 0.036 Uiso 1 1 calc R . . C77 C 0.56831(16) -0.19614(18) 0.2494(2) 0.0420(9) Uani 1 1 d . . . H77A H 0.5808 -0.1568 0.2570 0.050 Uiso 1 1 calc R . . C78 C 0.6167(2) -0.2395(2) 0.2541(3) 0.0571(12) Uani 1 1 d . . . H78A H 0.6611 -0.2291 0.2659 0.069 Uiso 1 1 calc R . . C79 C 0.5991(2) -0.2961(2) 0.2418(3) 0.0600(12) Uani 1 1 d . . . H79A H 0.6312 -0.3251 0.2448 0.072 Uiso 1 1 calc R . . C80 C 0.5344(2) -0.31125(17) 0.2249(2) 0.0478(10) Uani 1 1 d . . . C81 C 0.48854(17) -0.26688(14) 0.22264(19) 0.0328(8) Uani 1 1 d . . . C82 C 0.5108(3) -0.36938(18) 0.2107(3) 0.0635(13) Uani 1 1 d . . . H82A H 0.5410 -0.3997 0.2109 0.076 Uiso 1 1 calc R . . C83 C 0.4484(3) -0.38206(17) 0.1974(3) 0.0603(12) Uani 1 1 d . . . H83A H 0.4350 -0.4212 0.1894 0.072 Uiso 1 1 calc R . . C84 C 0.4006(2) -0.33806(15) 0.1948(2) 0.0465(10) Uani 1 1 d . . . C85 C 0.42130(17) -0.28034(14) 0.2077(2) 0.0347(8) Uani 1 1 d . . . C86 C 0.3345(2) -0.34928(16) 0.1827(3) 0.0555(12) Uani 1 1 d . . . H86A H 0.3187 -0.3877 0.1744 0.067 Uiso 1 1 calc R . . C87 C 0.2931(2) -0.30459(18) 0.1831(3) 0.0600(12) Uani 1 1 d . . . H87A H 0.2479 -0.3116 0.1748 0.072 Uiso 1 1 calc R . . C88 C 0.31693(18) -0.24856(15) 0.1958(3) 0.0468(10) Uani 1 1 d . . . H88A H 0.2872 -0.2180 0.1963 0.056 Uiso 1 1 calc R . . N7 N 0.6640(5) 0.2585(4) 0.0301(10) 0.312(9) Uani 1 1 d . . . C89 C 0.7838(5) 0.2461(4) 0.0296(5) 0.162(4) Uani 1 1 d . . . H89A H 0.8002 0.2070 0.0443 0.243 Uiso 1 1 calc R . . H89B H 0.8083 0.2740 0.0680 0.243 Uiso 1 1 calc R . . H89C H 0.7886 0.2552 -0.0251 0.243 Uiso 1 1 calc R . . C90 C 0.7196(6) 0.2487(5) 0.0317(6) 0.159(4) Uani 1 1 d . . . F1 F 0.12591(14) 0.75445(11) 0.15318(18) 0.0796(8) Uani 1 1 d . . . F2 F 0.17959(12) 0.83742(11) 0.18986(19) 0.0796(9) Uani 1 1 d . . . F3 F 0.09944(11) 0.81178(12) 0.24779(17) 0.0687(7) Uani 1 1 d . . . F4 F 0.19387(11) 0.76189(10) 0.27476(16) 0.0629(7) Uani 1 1 d . . . B1 B 0.1499(2) 0.79164(18) 0.2161(3) 0.0450(11) Uani 1 1 d . . . F5 F 0.3572(2) -0.00439(15) 0.80750(19) 0.1098(12) Uani 1 1 d . . . F6 F 0.39481(12) 0.04756(14) 0.7183(2) 0.0901(10) Uani 1 1 d . . . F7 F 0.30558(12) 0.07408(11) 0.75422(19) 0.0790(9) Uani 1 1 d . . . F8 F 0.30388(12) -0.00462(10) 0.67852(15) 0.0606(6) Uani 1 1 d . . . B2 B 0.34148(19) 0.02790(17) 0.7396(3) 0.0367(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0239(2) 0.0180(2) 0.0340(2) -0.00055(15) 0.00880(16) 0.00271(15) Cu2 0.0214(2) 0.0190(2) 0.0365(2) 0.00180(15) 0.00849(16) 0.00316(15) P1 0.0241(4) 0.0203(4) 0.0291(4) -0.0004(3) 0.0075(3) 0.0033(3) P2 0.0249(4) 0.0203(4) 0.0289(4) -0.0009(3) 0.0075(3) 0.0016(3) P3 0.0205(4) 0.0245(4) 0.0318(5) 0.0011(3) 0.0065(3) 0.0041(3) P4 0.0245(4) 0.0226(4) 0.0324(5) 0.0025(3) 0.0107(3) 0.0044(3) N1 0.0258(14) 0.0185(13) 0.0301(14) -0.0009(11) 0.0078(11) 0.0030(10) N2 0.0275(15) 0.0201(13) 0.0366(15) -0.0020(11) 0.0111(12) 0.0040(11) N3 0.0249(15) 0.0304(15) 0.0310(15) -0.0036(11) 0.0095(11) 0.0046(11) N4 0.0281(15) 0.0188(13) 0.0308(14) -0.0003(11) 0.0090(11) 0.0015(11) N5 0.0259(15) 0.0339(15) 0.0318(15) 0.0033(12) 0.0109(12) 0.0100(12) N6 0.0313(16) 0.0234(14) 0.0493(18) 0.0000(12) 0.0159(13) 0.0011(12) C1 0.0199(16) 0.0141(14) 0.0335(17) 0.0026(12) 0.0086(13) -0.0023(11) C2 0.0292(18) 0.0194(15) 0.0313(17) -0.0045(13) 0.0100(14) -0.0017(13) C3 0.0228(16) 0.0205(15) 0.0306(17) 0.0002(13) 0.0060(13) -0.0004(12) C4 0.0252(17) 0.0193(15) 0.0312(17) 0.0018(13) 0.0107(13) -0.0030(12) C5 0.0304(18) 0.0266(17) 0.0302(18) -0.0042(13) 0.0113(14) 0.0011(14) C6 0.0282(18) 0.0286(17) 0.0282(17) 0.0017(13) 0.0066(13) 0.0044(14) C7 0.0227(16) 0.0155(14) 0.0348(18) -0.0004(13) 0.0088(13) -0.0032(12) C8 0.0274(17) 0.0242(16) 0.0313(18) -0.0027(13) 0.0125(14) 0.0000(13) C9 0.0295(18) 0.0219(16) 0.0313(18) 0.0018(13) 0.0087(14) 0.0004(13) C10 0.0238(16) 0.0152(14) 0.0384(18) -0.0007(13) 0.0106(14) -0.0034(12) C11 0.0355(19) 0.0238(16) 0.0352(19) -0.0008(14) 0.0178(15) 0.0029(14) C12 0.0297(18) 0.0238(16) 0.0340(18) 0.0052(13) 0.0086(14) 0.0021(13) C13 0.0206(16) 0.0207(15) 0.0339(18) -0.0011(13) 0.0067(13) 0.0004(12) C14 0.0253(17) 0.0200(15) 0.0361(18) 0.0032(13) 0.0113(14) 0.0027(13) C15 0.0294(19) 0.048(2) 0.039(2) -0.0045(16) 0.0100(16) 0.0028(16) C16 0.035(2) 0.061(3) 0.055(3) -0.010(2) 0.0183(18) -0.0046(19) C17 0.044(2) 0.051(2) 0.056(3) -0.0064(19) 0.029(2) -0.0024(19) C18 0.048(2) 0.044(2) 0.040(2) -0.0068(17) 0.0209(18) 0.0022(18) C19 0.033(2) 0.0343(19) 0.040(2) -0.0070(15) 0.0097(16) 0.0009(15) C20 0.0280(18) 0.0291(17) 0.0291(17) 0.0023(13) 0.0107(14) 0.0041(14) C21 0.037(2) 0.0312(18) 0.040(2) 0.0032(15) 0.0036(16) 0.0046(15) C22 0.034(2) 0.054(2) 0.038(2) 0.0046(17) 0.0033(16) -0.0054(18) C23 0.032(2) 0.058(2) 0.034(2) 0.0156(18) 0.0081(16) 0.0090(18) C24 0.037(2) 0.040(2) 0.038(2) 0.0091(16) 0.0136(16) 0.0099(16) C25 0.0306(18) 0.0317(18) 0.0320(18) 0.0037(14) 0.0109(14) 0.0033(14) C26 0.0218(16) 0.0204(15) 0.0339(17) 0.0006(13) 0.0087(13) -0.0023(12) C27 0.0256(17) 0.0196(15) 0.0324(18) -0.0079(13) 0.0060(13) -0.0003(12) C28 0.0325(19) 0.0250(17) 0.040(2) -0.0026(14) 0.0091(15) -0.0024(14) C29 0.0254(19) 0.037(2) 0.054(2) -0.0022(17) 0.0123(16) -0.0025(15) C30 0.0264(19) 0.0344(19) 0.049(2) -0.0041(16) 0.0029(16) 0.0068(15) C31 0.040(2) 0.0261(17) 0.037(2) -0.0019(14) 0.0009(15) 0.0026(15) C32 0.0319(19) 0.0277(17) 0.0310(18) -0.0040(14) 0.0060(14) -0.0018(14) C33 0.0279(18) 0.0355(18) 0.0287(18) 0.0018(14) 0.0079(14) 0.0108(14) C34 0.032(2) 0.067(3) 0.039(2) -0.0112(19) 0.0135(17) -0.0067(18) C35 0.031(2) 0.096(4) 0.044(2) -0.007(2) 0.0156(18) -0.003(2) C36 0.041(2) 0.089(3) 0.036(2) 0.001(2) 0.0145(18) 0.027(2) C37 0.077(3) 0.045(2) 0.035(2) -0.0047(17) 0.017(2) 0.020(2) C38 0.055(2) 0.035(2) 0.037(2) -0.0002(16) 0.0157(18) 0.0066(17) C39 0.0206(16) 0.0253(16) 0.043(2) -0.0063(14) 0.0086(14) -0.0006(13) C40 0.0305(19) 0.0312(18) 0.038(2) 0.0113(15) 0.0138(15) 0.0098(14) C41 0.057(3) 0.039(2) 0.046(2) 0.0112(17) 0.0251(19) 0.0176(18) C42 0.091(4) 0.064(3) 0.054(3) 0.017(2) 0.046(3) 0.030(3) C43 0.060(3) 0.085(4) 0.098(4) 0.032(3) 0.059(3) 0.033(3) C44 0.037(3) 0.079(3) 0.100(4) 0.019(3) 0.035(3) 0.012(2) C45 0.031(2) 0.046(2) 0.060(3) 0.0106(19) 0.0189(18) 0.0084(17) C46 0.0291(19) 0.039(2) 0.0325(19) -0.0030(15) 0.0033(14) 0.0118(15) C47 0.033(2) 0.067(3) 0.048(2) 0.004(2) -0.0015(18) -0.0003(19) C48 0.033(2) 0.099(4) 0.052(3) 0.007(3) -0.0050(19) -0.001(2) C49 0.041(3) 0.082(3) 0.051(3) 0.000(2) -0.007(2) 0.022(2) C50 0.072(3) 0.053(3) 0.070(3) 0.013(2) -0.014(3) 0.013(2) C51 0.046(2) 0.046(2) 0.065(3) 0.011(2) -0.012(2) 0.0035(19) C52 0.0279(18) 0.0234(16) 0.0398(19) 0.0015(14) 0.0166(15) 0.0020(13) C53 0.0294(18) 0.0262(17) 0.0335(19) -0.0002(14) 0.0038(14) 0.0063(13) C54 0.029(2) 0.043(2) 0.046(2) 0.0055(17) 0.0055(16) 0.0068(16) C55 0.032(2) 0.065(3) 0.070(3) 0.003(2) 0.009(2) 0.0061(19) C56 0.045(3) 0.063(3) 0.060(3) 0.001(2) -0.008(2) 0.024(2) C57 0.048(2) 0.047(2) 0.044(2) 0.0037(18) -0.0028(19) 0.0085(19) C58 0.044(2) 0.0335(19) 0.039(2) 0.0024(16) 0.0065(17) 0.0021(16) C59 0.037(2) 0.0275(17) 0.0361(19) 0.0078(14) 0.0153(15) 0.0106(15) C60 0.038(2) 0.039(2) 0.039(2) 0.0044(16) 0.0148(16) 0.0076(16) C61 0.042(2) 0.050(2) 0.046(2) 0.0118(19) 0.0214(18) 0.0081(18) C62 0.054(3) 0.054(2) 0.047(2) 0.0076(19) 0.029(2) 0.016(2) C63 0.071(3) 0.058(3) 0.052(3) -0.015(2) 0.029(2) -0.001(2) C64 0.051(3) 0.049(2) 0.054(3) -0.0123(19) 0.023(2) -0.0068(19) C65 0.031(2) 0.043(2) 0.042(2) -0.0071(16) 0.0105(16) 0.0049(16) C66 0.028(2) 0.057(3) 0.056(2) -0.014(2) 0.0104(17) 0.0100(18) C67 0.039(2) 0.055(3) 0.049(2) -0.0071(19) 0.0118(18) 0.0264(19) C68 0.043(2) 0.040(2) 0.0326(19) -0.0005(15) 0.0142(16) 0.0154(16) C69 0.0350(19) 0.0241(16) 0.0265(17) -0.0017(13) 0.0104(14) 0.0093(14) C70 0.067(3) 0.031(2) 0.047(2) 0.0023(17) 0.020(2) 0.0246(19) C71 0.066(3) 0.0236(18) 0.047(2) 0.0042(16) 0.026(2) 0.0167(18) C72 0.054(2) 0.0251(17) 0.0303(18) 0.0040(14) 0.0177(16) 0.0078(16) C73 0.0376(19) 0.0218(16) 0.0217(16) -0.0005(12) 0.0095(14) 0.0055(13) C74 0.053(2) 0.0223(17) 0.043(2) 0.0007(15) 0.0207(18) -0.0042(16) C75 0.037(2) 0.0321(19) 0.041(2) 0.0037(15) 0.0127(16) -0.0053(15) C76 0.0325(19) 0.0219(16) 0.0373(19) 0.0018(14) 0.0107(15) 0.0010(14) C77 0.030(2) 0.049(2) 0.048(2) 0.0031(17) 0.0114(16) 0.0093(16) C78 0.031(2) 0.085(3) 0.053(3) -0.003(2) 0.0067(18) 0.025(2) C79 0.054(3) 0.067(3) 0.059(3) -0.002(2) 0.012(2) 0.039(2) C80 0.054(3) 0.046(2) 0.044(2) 0.0057(18) 0.0124(19) 0.028(2) C81 0.042(2) 0.0294(18) 0.0285(18) 0.0050(14) 0.0120(15) 0.0147(15) C82 0.093(4) 0.033(2) 0.065(3) 0.005(2) 0.020(3) 0.039(2) C83 0.091(4) 0.026(2) 0.067(3) 0.0006(19) 0.023(3) 0.015(2) C84 0.072(3) 0.0248(19) 0.047(2) 0.0000(16) 0.023(2) 0.0014(18) C85 0.047(2) 0.0216(17) 0.039(2) 0.0017(14) 0.0172(16) 0.0042(15) C86 0.072(3) 0.031(2) 0.073(3) -0.0070(19) 0.035(2) -0.016(2) C87 0.051(3) 0.043(2) 0.092(3) -0.013(2) 0.030(2) -0.019(2) C88 0.040(2) 0.031(2) 0.073(3) -0.0055(18) 0.021(2) -0.0091(16) N7 0.194(10) 0.147(8) 0.62(3) -0.195(12) 0.151(14) -0.065(8) C89 0.178(10) 0.217(11) 0.086(6) -0.027(6) 0.017(6) 0.030(8) C90 0.161(9) 0.183(10) 0.150(8) -0.066(7) 0.068(8) -0.085(9) F1 0.083(2) 0.0568(16) 0.089(2) -0.0148(14) -0.0009(16) 0.0158(14) F2 0.0510(16) 0.0644(17) 0.125(3) 0.0338(16) 0.0223(16) -0.0109(13) F3 0.0337(13) 0.0824(18) 0.094(2) -0.0049(15) 0.0236(13) 0.0060(12) F4 0.0487(15) 0.0545(14) 0.0824(18) 0.0122(13) 0.0084(13) 0.0095(11) B1 0.030(2) 0.032(2) 0.072(3) 0.003(2) 0.008(2) -0.0009(18) F5 0.156(3) 0.097(2) 0.0637(19) 0.0350(17) -0.0016(19) -0.027(2) F6 0.0444(16) 0.122(3) 0.118(2) 0.013(2) 0.0469(16) -0.0086(16) F7 0.0497(16) 0.0773(18) 0.108(2) -0.0491(16) 0.0141(15) 0.0131(13) F8 0.0724(17) 0.0480(14) 0.0604(15) -0.0157(12) 0.0127(13) -0.0019(12) B2 0.030(2) 0.035(2) 0.048(3) 0.0036(18) 0.0156(19) 0.0016(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.049(2) . ? Cu1 N4 2.052(2) . ? Cu1 P2 2.2120(9) . ? Cu1 P1 2.2347(9) . ? Cu2 N6 2.042(3) . ? Cu2 N5 2.055(2) . ? Cu2 P3 2.2281(9) . ? Cu2 P4 2.2284(9) . ? P1 C20 1.824(3) . ? P1 C14 1.824(3) . ? P1 C13 1.863(3) . ? P2 C27 1.821(3) . ? P2 C33 1.831(3) . ? P2 C26 1.869(3) . ? P3 C40 1.814(3) . ? P3 C46 1.823(3) . ? P3 C39 1.862(3) . ? P4 C53 1.823(3) . ? P4 C59 1.828(3) . ? P4 C52 1.865(3) . ? N1 C1 1.402(4) . ? N1 C13 1.454(4) . ? N1 C26 1.457(4) . ? N2 C10 1.397(4) . ? N2 C52 1.454(4) . ? N2 C39 1.462(4) . ? N3 C65 1.324(4) . ? N3 C69 1.363(4) . ? N4 C76 1.326(4) . ? N4 C73 1.370(4) . ? N5 C77 1.322(4) . ? N5 C81 1.375(4) . ? N6 C88 1.329(4) . ? N6 C85 1.360(4) . ? C1 C2 1.389(4) . ? C1 C6 1.399(4) . ? C2 C3 1.380(4) . ? C2 H2A 0.9500 . ? C3 C4 1.386(4) . ? C3 H3A 0.9500 . ? C4 C5 1.390(5) . ? C4 C7 1.478(4) . ? C5 C6 1.384(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.392(4) . ? C7 C12 1.393(4) . ? C8 C9 1.383(4) . ? C8 H8A 0.9500 . ? C9 C10 1.396(4) . ? C9 H9A 0.9500 . ? C10 C11 1.394(5) . ? C11 C12 1.378(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.384(5) . ? C14 C15 1.389(5) . ? C15 C16 1.387(5) . ? C15 H15A 0.9500 . ? C16 C17 1.376(6) . ? C16 H16A 0.9500 . ? C17 C18 1.377(5) . ? C17 H17A 0.9500 . ? C18 C19 1.379(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.391(4) . ? C20 C21 1.398(5) . ? C21 C22 1.375(5) . ? C21 H21A 0.9500 . ? C22 C23 1.388(5) . ? C22 H22A 0.9500 . ? C23 C24 1.375(5) . ? C23 H23A 0.9500 . ? C24 C25 1.392(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.395(4) . ? C27 C32 1.399(5) . ? C28 C29 1.380(5) . ? C28 H28A 0.9500 . ? C29 C30 1.369(5) . ? C29 H29A 0.9500 . ? C30 C31 1.390(5) . ? C30 H30A 0.9500 . ? C31 C32 1.378(5) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.387(5) . ? C33 C38 1.395(5) . ? C34 C35 1.381(5) . ? C34 H34A 0.9500 . ? C35 C36 1.366(6) . ? C35 H35A 0.9500 . ? C36 C37 1.381(6) . ? C36 H36A 0.9500 . ? C37 C38 1.397(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.391(5) . ? C40 C45 1.391(5) . ? C41 C42 1.399(5) . ? C41 H41A 0.9500 . ? C42 C43 1.387(7) . ? C42 H42A 0.9500 . ? C43 C44 1.359(8) . ? C43 H43A 0.9500 . ? C44 C45 1.395(5) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C51 1.377(5) . ? C46 C47 1.385(5) . ? C47 C48 1.395(6) . ? C47 H47A 0.9500 . ? C48 C49 1.356(7) . ? C48 H48A 0.9500 . ? C49 C50 1.377(6) . ? C49 H49A 0.9500 . ? C50 C51 1.403(6) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.386(5) . ? C53 C58 1.392(5) . ? C54 C55 1.395(5) . ? C54 H54A 0.9500 . ? C55 C56 1.377(6) . ? C55 H55A 0.9500 . ? C56 C57 1.389(6) . ? C56 H56A 0.9500 . ? C57 C58 1.373(5) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C64 1.379(5) . ? C59 C60 1.392(5) . ? C60 C61 1.385(5) . ? C60 H60A 0.9500 . ? C61 C62 1.376(6) . ? C61 H61A 0.9500 . ? C62 C63 1.369(6) . ? C62 H62A 0.9500 . ? C63 C64 1.399(5) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C66 1.408(5) . ? C65 H65A 0.9500 . ? C66 C67 1.345(6) . ? C66 H66A 0.9500 . ? C67 C68 1.404(5) . ? C67 H67A 0.9500 . ? C68 C69 1.401(4) . ? C68 C70 1.441(5) . ? C69 C73 1.438(4) . ? C70 C71 1.342(6) . ? C70 H70A 0.9500 . ? C71 C72 1.429(5) . ? C71 H71A 0.9500 . ? C72 C73 1.401(5) . ? C72 C74 1.403(5) . ? C74 C75 1.376(5) . ? C74 H74A 0.9500 . ? C75 C76 1.399(4) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C78 1.426(5) . ? C77 H77A 0.9500 . ? C78 C79 1.366(6) . ? C78 H78A 0.9500 . ? C79 C80 1.383(6) . ? C79 H79A 0.9500 . ? C80 C81 1.409(5) . ? C80 C82 1.437(6) . ? C81 C85 1.426(5) . ? C82 C83 1.326(6) . ? C82 H82A 0.9500 . ? C83 C84 1.431(6) . ? C83 H83A 0.9500 . ? C84 C86 1.395(6) . ? C84 C85 1.408(5) . ? C86 C87 1.359(6) . ? C86 H86A 0.9500 . ? C87 C88 1.391(5) . ? C87 H87A 0.9500 . ? C88 H88A 0.9500 . ? N7 C90 1.196(13) . ? C89 C90 1.371(11) . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? F1 B1 1.376(5) . ? F2 B1 1.358(5) . ? F3 B1 1.385(5) . ? F4 B1 1.384(5) . ? F5 B2 1.350(5) . ? F6 B2 1.344(4) . ? F7 B2 1.368(4) . ? F8 B2 1.380(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N4 82.29(10) . . ? N3 Cu1 P2 112.22(8) . . ? N4 Cu1 P2 122.94(8) . . ? N3 Cu1 P1 108.22(8) . . ? N4 Cu1 P1 120.62(7) . . ? P2 Cu1 P1 106.90(3) . . ? N6 Cu2 N5 82.26(11) . . ? N6 Cu2 P3 123.13(8) . . ? N5 Cu2 P3 109.53(8) . . ? N6 Cu2 P4 120.61(9) . . ? N5 Cu2 P4 110.53(7) . . ? P3 Cu2 P4 107.00(3) . . ? C20 P1 C14 104.13(14) . . ? C20 P1 C13 102.90(14) . . ? C14 P1 C13 103.83(13) . . ? C20 P1 Cu1 117.74(10) . . ? C14 P1 Cu1 117.29(11) . . ? C13 P1 Cu1 109.20(10) . . ? C27 P2 C33 104.32(15) . . ? C27 P2 C26 103.62(14) . . ? C33 P2 C26 103.11(14) . . ? C27 P2 Cu1 121.08(10) . . ? C33 P2 Cu1 115.87(11) . . ? C26 P2 Cu1 106.80(10) . . ? C40 P3 C46 103.19(15) . . ? C40 P3 C39 103.14(14) . . ? C46 P3 C39 103.15(16) . . ? C40 P3 Cu2 122.91(12) . . ? C46 P3 Cu2 114.64(11) . . ? C39 P3 Cu2 107.62(11) . . ? C53 P4 C59 103.86(15) . . ? C53 P4 C52 102.65(15) . . ? C59 P4 C52 102.48(15) . . ? C53 P4 Cu2 119.12(11) . . ? C59 P4 Cu2 119.43(10) . . ? C52 P4 Cu2 106.88(11) . . ? C1 N1 C13 122.7(2) . . ? C1 N1 C26 121.0(2) . . ? C13 N1 C26 115.4(2) . . ? C10 N2 C52 122.6(3) . . ? C10 N2 C39 122.5(2) . . ? C52 N2 C39 114.9(2) . . ? C65 N3 C69 118.4(3) . . ? C65 N3 Cu1 130.0(2) . . ? C69 N3 Cu1 111.0(2) . . ? C76 N4 C73 116.9(3) . . ? C76 N4 Cu1 131.9(2) . . ? C73 N4 Cu1 111.2(2) . . ? C77 N5 C81 119.1(3) . . ? C77 N5 Cu2 130.3(2) . . ? C81 N5 Cu2 110.7(2) . . ? C88 N6 C85 117.6(3) . . ? C88 N6 Cu2 130.7(2) . . ? C85 N6 Cu2 111.8(2) . . ? C2 C1 C6 116.9(3) . . ? C2 C1 N1 119.9(3) . . ? C6 C1 N1 123.0(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 122.2(3) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C3 C4 C5 116.2(3) . . ? C3 C4 C7 120.8(3) . . ? C5 C4 C7 123.0(3) . . ? C6 C5 C4 122.4(3) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? C8 C7 C12 116.4(3) . . ? C8 C7 C4 120.8(3) . . ? C12 C7 C4 122.8(3) . . ? C9 C8 C7 122.5(3) . . ? C9 C8 H8A 118.7 . . ? C7 C8 H8A 118.7 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 117.4(3) . . ? C11 C10 N2 121.6(3) . . ? C9 C10 N2 121.0(3) . . ? C12 C11 C10 121.4(3) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C7 121.7(3) . . ? C11 C12 H12A 119.1 . . ? C7 C12 H12A 119.1 . . ? N1 C13 P1 110.4(2) . . ? N1 C13 H13A 109.6 . . ? P1 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? P1 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C19 C14 C15 118.9(3) . . ? C19 C14 P1 123.2(3) . . ? C15 C14 P1 117.8(2) . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C17 C16 C15 119.2(4) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.3(3) . . ? C18 C19 H19A 119.9 . . ? C14 C19 H19A 119.9 . . ? C25 C20 C21 118.4(3) . . ? C25 C20 P1 117.7(2) . . ? C21 C20 P1 123.9(2) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 119.6(4) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C20 C25 C24 120.6(3) . . ? C20 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? N1 C26 P2 114.65(19) . . ? N1 C26 H26A 108.6 . . ? P2 C26 H26A 108.6 . . ? N1 C26 H26B 108.6 . . ? P2 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P2 119.7(2) . . ? C32 C27 P2 121.8(2) . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C27 121.0(3) . . ? C31 C32 H32A 119.5 . . ? C27 C32 H32A 119.5 . . ? C34 C33 C38 119.2(3) . . ? C34 C33 P2 124.6(3) . . ? C38 C33 P2 116.2(3) . . ? C35 C34 C33 120.2(4) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C37 119.9(3) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C36 C37 C38 120.1(4) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C33 C38 C37 119.7(4) . . ? C33 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? N2 C39 P3 113.1(2) . . ? N2 C39 H39A 109.0 . . ? P3 C39 H39A 109.0 . . ? N2 C39 H39B 109.0 . . ? P3 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C45 119.9(3) . . ? C41 C40 P3 121.5(3) . . ? C45 C40 P3 118.4(3) . . ? C40 C41 C42 119.4(4) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C43 C42 C41 119.6(4) . . ? C43 C42 H42A 120.2 . . ? C41 C42 H42A 120.2 . . ? C44 C43 C42 121.4(4) . . ? C44 C43 H43A 119.3 . . ? C42 C43 H43A 119.3 . . ? C43 C44 C45 119.6(5) . . ? C43 C44 H44A 120.2 . . ? C45 C44 H44A 120.2 . . ? C40 C45 C44 120.1(4) . . ? C40 C45 H45A 119.9 . . ? C44 C45 H45A 119.9 . . ? C51 C46 C47 118.9(3) . . ? C51 C46 P3 117.0(3) . . ? C47 C46 P3 124.0(3) . . ? C46 C47 C48 120.0(4) . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C49 C48 C47 120.8(4) . . ? C49 C48 H48A 119.6 . . ? C47 C48 H48A 119.6 . . ? C48 C49 C50 120.1(4) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C49 C50 C51 119.5(4) . . ? C49 C50 H50A 120.2 . . ? C51 C50 H50A 120.2 . . ? C46 C51 C50 120.6(4) . . ? C46 C51 H51A 119.7 . . ? C50 C51 H51A 119.7 . . ? N2 C52 P4 111.5(2) . . ? N2 C52 H52A 109.3 . . ? P4 C52 H52A 109.3 . . ? N2 C52 H52B 109.3 . . ? P4 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C58 119.5(3) . . ? C54 C53 P4 118.7(3) . . ? C58 C53 P4 121.6(3) . . ? C53 C54 C55 120.4(4) . . ? C53 C54 H54A 119.8 . . ? C55 C54 H54A 119.8 . . ? C56 C55 C54 119.2(4) . . ? C56 C55 H55A 120.4 . . ? C54 C55 H55A 120.4 . . ? C55 C56 C57 120.7(4) . . ? C55 C56 H56A 119.7 . . ? C57 C56 H56A 119.7 . . ? C58 C57 C56 120.0(4) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C57 C58 C53 120.2(3) . . ? C57 C58 H58A 119.9 . . ? C53 C58 H58A 119.9 . . ? C64 C59 C60 118.9(3) . . ? C64 C59 P4 118.4(3) . . ? C60 C59 P4 122.6(3) . . ? C61 C60 C59 120.4(4) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C62 C61 C60 119.9(4) . . ? C62 C61 H61A 120.1 . . ? C60 C61 H61A 120.1 . . ? C63 C62 C61 120.7(3) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C62 C63 C64 119.5(4) . . ? C62 C63 H63A 120.3 . . ? C64 C63 H63A 120.3 . . ? C59 C64 C63 120.6(4) . . ? C59 C64 H64A 119.7 . . ? C63 C64 H64A 119.7 . . ? N3 C65 C66 122.3(4) . . ? N3 C65 H65A 118.8 . . ? C66 C65 H65A 118.8 . . ? C67 C66 C65 119.2(4) . . ? C67 C66 H66A 120.4 . . ? C65 C66 H66A 120.4 . . ? C66 C67 C68 120.5(3) . . ? C66 C67 H67A 119.7 . . ? C68 C67 H67A 119.7 . . ? C69 C68 C67 117.0(3) . . ? C69 C68 C70 118.3(3) . . ? C67 C68 C70 124.7(3) . . ? N3 C69 C68 122.5(3) . . ? N3 C69 C73 117.8(3) . . ? C68 C69 C73 119.7(3) . . ? C71 C70 C68 121.9(3) . . ? C71 C70 H70A 119.1 . . ? C68 C70 H70A 119.1 . . ? C70 C71 C72 120.9(3) . . ? C70 C71 H71A 119.6 . . ? C72 C71 H71A 119.6 . . ? C73 C72 C74 118.2(3) . . ? C73 C72 C71 118.9(3) . . ? C74 C72 C71 122.9(3) . . ? N4 C73 C72 122.8(3) . . ? N4 C73 C69 117.1(3) . . ? C72 C73 C69 120.1(3) . . ? C75 C74 C72 119.0(3) . . ? C75 C74 H74A 120.5 . . ? C72 C74 H74A 120.5 . . ? C74 C75 C76 118.7(3) . . ? C74 C75 H75A 120.6 . . ? C76 C75 H75A 120.6 . . ? N4 C76 C75 124.2(3) . . ? N4 C76 H76A 117.9 . . ? C75 C76 H76A 117.9 . . ? N5 C77 C78 121.0(4) . . ? N5 C77 H77A 119.5 . . ? C78 C77 H77A 119.5 . . ? C79 C78 C77 119.9(4) . . ? C79 C78 H78A 120.1 . . ? C77 C78 H78A 120.1 . . ? C78 C79 C80 120.0(4) . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C79 C80 C81 117.9(4) . . ? C79 C80 C82 124.3(4) . . ? C81 C80 C82 117.8(4) . . ? N5 C81 C80 122.1(3) . . ? N5 C81 C85 117.7(3) . . ? C80 C81 C85 120.2(3) . . ? C83 C82 C80 122.2(4) . . ? C83 C82 H82A 118.9 . . ? C80 C82 H82A 118.9 . . ? C82 C83 C84 121.4(4) . . ? C82 C83 H83A 119.3 . . ? C84 C83 H83A 119.3 . . ? C86 C84 C85 117.9(3) . . ? C86 C84 C83 123.6(4) . . ? C85 C84 C83 118.5(4) . . ? N6 C85 C84 122.5(3) . . ? N6 C85 C81 117.5(3) . . ? C84 C85 C81 120.0(3) . . ? C87 C86 C84 119.2(4) . . ? C87 C86 H86A 120.4 . . ? C84 C86 H86A 120.4 . . ? C86 C87 C88 119.8(4) . . ? C86 C87 H87A 120.1 . . ? C88 C87 H87A 120.1 . . ? N6 C88 C87 123.1(4) . . ? N6 C88 H88A 118.5 . . ? C87 C88 H88A 118.5 . . ? C90 C89 H89A 109.5 . . ? C90 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C90 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N7 C90 C89 171.2(14) . . ? F2 B1 F1 110.6(4) . . ? F2 B1 F4 109.7(3) . . ? F1 B1 F4 108.5(3) . . ? F2 B1 F3 108.8(3) . . ? F1 B1 F3 109.2(3) . . ? F4 B1 F3 110.0(4) . . ? F6 B2 F5 111.0(4) . . ? F6 B2 F7 108.8(3) . . ? F5 B2 F7 108.5(4) . . ? F6 B2 F8 111.2(3) . . ? F5 B2 F8 109.1(3) . . ? F7 B2 F8 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.059 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.087 # Attachment '- 4b.CIF' data_4b _database_code_depnum_ccdc_archive 'CCDC 815818' #TrackingRef '- 4b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H80 B2 Cu2 F8 N6 O2 P4' _chemical_formula_weight 1726.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.3858(4) _cell_length_b 16.0439(3) _cell_length_c 19.7920(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.402(2) _cell_angle_gamma 90.00 _cell_volume 8371.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12059 _cell_measurement_theta_min 2.7343 _cell_measurement_theta_max 62.4305 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 1.935 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.59676 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29931 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 62.52 _reflns_number_total 13180 _reflns_number_gt 9932 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1327P)^2^+3.1985P] 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 13180 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 -0.43785(2) 0.19419(4) -0.16367(2) 0.04581(18) Uani 1 1 d . . . Cu2 Cu -0.05958(2) 0.29672(5) -0.78561(3) 0.0637(2) Uani 1 1 d . . . P1 P -0.37429(4) 0.10679(6) -0.18611(5) 0.0461(2) Uani 1 1 d . . . P2 P -0.41347(4) 0.31501(6) -0.21177(4) 0.0442(2) Uani 1 1 d . . . P3 P -0.11575(4) 0.40010(8) -0.76974(6) 0.0578(3) Uani 1 1 d . . . P4 P -0.10560(4) 0.17799(8) -0.78212(5) 0.0560(3) Uani 1 1 d . . . N1 N -0.33149(12) 0.2345(2) -0.26427(15) 0.0466(7) Uani 1 1 d . . . N2 N -0.17507(14) 0.2723(2) -0.71573(17) 0.0571(9) Uani 1 1 d . . . N3 N -0.51426(12) 0.1644(2) -0.16426(15) 0.0465(7) Uani 1 1 d . . . N4 N -0.45354(13) 0.2276(2) -0.06470(15) 0.0463(7) Uani 1 1 d . . . N5 N 0.0007(2) 0.3099(3) -0.8486(3) 0.1025(19) Uani 1 1 d . . . N6 N 0.00006(19) 0.2973(3) -0.7111(3) 0.0917(15) Uani 1 1 d . . . C1 C -0.30450(13) 0.2394(2) -0.32538(19) 0.0445(8) Uani 1 1 d . . . C2 C -0.29098(15) 0.3147(3) -0.3548(2) 0.0495(9) Uani 1 1 d . . . H2A H -0.2985 0.3646 -0.3334 0.059 Uiso 1 1 calc R . . C3 C -0.26651(16) 0.3164(3) -0.4151(2) 0.0503(9) Uani 1 1 d . . . H3A H -0.2579 0.3678 -0.4332 0.060 Uiso 1 1 calc R . . C4 C -0.25434(14) 0.2446(2) -0.44992(19) 0.0466(9) Uani 1 1 d . . . C5 C -0.26772(15) 0.1695(3) -0.4207(2) 0.0497(9) Uani 1 1 d . . . H5A H -0.2601 0.1199 -0.4424 0.060 Uiso 1 1 calc R . . C6 C -0.29233(16) 0.1666(3) -0.3596(2) 0.0498(9) Uani 1 1 d . . . H6A H -0.3007 0.1152 -0.3414 0.060 Uiso 1 1 calc R . . C7 C -0.23159(15) 0.2486(3) -0.5175(2) 0.0487(9) Uani 1 1 d . . . C8 C -0.20389(16) 0.3180(3) -0.5370(2) 0.0569(10) Uani 1 1 d . . . H8A H -0.1980 0.3611 -0.5063 0.068 Uiso 1 1 calc R . . C9 C -0.18489(18) 0.3244(3) -0.6012(2) 0.0624(11) Uani 1 1 d . . . H9A H -0.1660 0.3711 -0.6122 0.075 Uiso 1 1 calc R . . C10 C -0.19354(15) 0.2621(3) -0.6496(2) 0.0518(9) Uani 1 1 d . . . C11 C -0.22054(15) 0.1925(3) -0.6307(2) 0.0503(9) Uani 1 1 d . . . H11A H -0.2262 0.1493 -0.6614 0.060 Uiso 1 1 calc R . . C12 C -0.23939(16) 0.1864(3) -0.5657(2) 0.0520(9) Uani 1 1 d . . . H12A H -0.2577 0.1393 -0.5545 0.062 Uiso 1 1 calc R . . C13 C -0.31860(15) 0.1667(3) -0.2167(2) 0.0495(9) Uani 1 1 d . . . H13A H -0.3001 0.1901 -0.1778 0.059 Uiso 1 1 calc R . . H13B H -0.2961 0.1282 -0.2385 0.059 Uiso 1 1 calc R . . C14 C -0.38281(15) 0.0291(3) -0.25262(19) 0.0509(9) Uani 1 1 d . . . C15 C -0.39468(16) 0.0567(3) -0.3180(2) 0.0541(10) Uani 1 1 d . . . H15A H -0.3988 0.1135 -0.3259 0.065 Uiso 1 1 calc R . . C16 C -0.40044(18) 0.0013(3) -0.3714(2) 0.0643(11) Uani 1 1 d . . . H16A H -0.4071 0.0209 -0.4151 0.077 Uiso 1 1 calc R . . C17 C -0.3963(2) -0.0834(3) -0.3592(2) 0.0738(14) Uani 1 1 d . . . H17A H -0.4008 -0.1210 -0.3947 0.089 Uiso 1 1 calc R . . C18 C -0.3855(2) -0.1118(3) -0.2950(3) 0.0744(13) Uani 1 1 d . . . H18A H -0.3833 -0.1688 -0.2870 0.089 Uiso 1 1 calc R . . C19 C -0.37783(19) -0.0565(3) -0.2419(2) 0.0619(11) Uani 1 1 d . . . H19A H -0.3693 -0.0765 -0.1988 0.074 Uiso 1 1 calc R . . C20 C -0.34429(16) 0.0510(3) -0.1153(2) 0.0530(10) Uani 1 1 d . . . C21 C -0.29637(19) 0.0153(3) -0.1188(3) 0.0708(13) Uani 1 1 d . . . H21A H -0.2795 0.0171 -0.1590 0.085 Uiso 1 1 calc R . . C22 C -0.2739(2) -0.0228(4) -0.0627(3) 0.0798(14) Uani 1 1 d . . . H22A H -0.2420 -0.0469 -0.0654 0.096 Uiso 1 1 calc R . . C23 C -0.2987(2) -0.0253(3) -0.0018(3) 0.0755(14) Uani 1 1 d . . . H23A H -0.2833 -0.0504 0.0361 0.091 Uiso 1 1 calc R . . C24 C -0.3448(2) 0.0086(3) 0.0016(2) 0.0704(13) Uani 1 1 d . . . H24A H -0.3615 0.0056 0.0419 0.084 Uiso 1 1 calc R . . C25 C -0.36838(19) 0.0481(3) -0.0535(2) 0.0593(11) Uani 1 1 d . . . H25A H -0.4000 0.0727 -0.0495 0.071 Uiso 1 1 calc R . . C26 C -0.34538(15) 0.3113(2) -0.2301(2) 0.0484(9) Uani 1 1 d . . . H26A H -0.3373 0.3585 -0.2584 0.058 Uiso 1 1 calc R . . H26B H -0.3254 0.3161 -0.1881 0.058 Uiso 1 1 calc R . . C27 C -0.44723(15) 0.3565(3) -0.28736(18) 0.0493(9) Uani 1 1 d . . . C28 C -0.42693(19) 0.4116(3) -0.3322(2) 0.0637(11) Uani 1 1 d . . . H28A H -0.3929 0.4265 -0.3273 0.076 Uiso 1 1 calc R . . C29 C -0.4569(2) 0.4449(4) -0.3847(3) 0.0769(14) Uani 1 1 d . . . H29A H -0.4431 0.4827 -0.4144 0.092 Uiso 1 1 calc R . . C30 C -0.5074(2) 0.4220(4) -0.3927(2) 0.0751(15) Uani 1 1 d . . . H30A H -0.5275 0.4442 -0.4280 0.090 Uiso 1 1 calc R . . C31 C -0.52762(19) 0.3668(3) -0.3489(2) 0.0689(13) Uani 1 1 d . . . H31A H -0.5615 0.3515 -0.3543 0.083 Uiso 1 1 calc R . . C32 C -0.49791(17) 0.3338(3) -0.2967(2) 0.0605(11) Uani 1 1 d . . . H32A H -0.5119 0.2957 -0.2673 0.073 Uiso 1 1 calc R . . C33 C -0.41580(17) 0.4040(3) -0.15374(18) 0.0496(9) Uani 1 1 d . . . C34 C -0.46170(17) 0.4167(3) -0.12311(18) 0.0522(10) Uani 1 1 d . . . H34A H -0.4894 0.3827 -0.1341 0.063 Uiso 1 1 calc R . . C35 C -0.46608(19) 0.4803(3) -0.07617(19) 0.0606(12) Uani 1 1 d . . . H35A H -0.4970 0.4897 -0.0565 0.073 Uiso 1 1 calc R . . C36 C -0.4251(2) 0.5293(3) -0.0587(2) 0.0667(13) Uani 1 1 d . . . H36A H -0.4281 0.5706 -0.0260 0.080 Uiso 1 1 calc R . . C37 C -0.3792(2) 0.5183(3) -0.0889(2) 0.0667(12) Uani 1 1 d . . . H37A H -0.3517 0.5522 -0.0771 0.080 Uiso 1 1 calc R . . C38 C -0.37474(17) 0.4558(3) -0.1372(2) 0.0571(10) Uani 1 1 d . . . H38A H -0.3443 0.4487 -0.1584 0.068 Uiso 1 1 calc R . . C39 C -0.42257(18) 0.2590(3) -0.01672(19) 0.0542(10) Uani 1 1 d . . . C40 C -0.4411(2) 0.2890(3) 0.0443(2) 0.0638(12) Uani 1 1 d . . . H40A H -0.4187 0.3105 0.0774 0.077 Uiso 1 1 calc R . . C41 C -0.4912(2) 0.2867(3) 0.0548(2) 0.0680(14) Uani 1 1 d . . . H41A H -0.5031 0.3070 0.0952 0.082 Uiso 1 1 calc R . . C42 C -0.52586(18) 0.2540(3) 0.00543(19) 0.0565(11) Uani 1 1 d . . . C43 C -0.5789(2) 0.2468(3) 0.0126(2) 0.0642(12) Uani 1 1 d . . . H43A H -0.5930 0.2664 0.0519 0.077 Uiso 1 1 calc R . . C44 C -0.60920(19) 0.2125(3) -0.0356(2) 0.0628(12) Uani 1 1 d . . . H44A H -0.6437 0.2074 -0.0288 0.075 Uiso 1 1 calc R . . C45 C -0.58917(16) 0.1834(3) -0.0978(2) 0.0524(10) Uani 1 1 d . . . C46 C -0.61876(17) 0.1486(3) -0.1509(2) 0.0618(11) Uani 1 1 d . . . H46A H -0.6537 0.1438 -0.1476 0.074 Uiso 1 1 calc R . . C47 C -0.59604(17) 0.1218(3) -0.2076(2) 0.0604(11) Uani 1 1 d . . . H47A H -0.6155 0.0980 -0.2428 0.072 Uiso 1 1 calc R . . C48 C -0.54315(16) 0.1300(3) -0.21295(19) 0.0545(10) Uani 1 1 d . . . C49 C -0.50416(16) 0.2245(2) -0.05454(17) 0.0466(9) Uani 1 1 d . . . C50 C -0.53659(16) 0.1902(2) -0.10650(18) 0.0466(9) Uani 1 1 d . . . C51 C -0.36758(18) 0.2635(3) -0.0285(2) 0.0644(11) Uani 1 1 d . . . H51A H -0.3612 0.2406 -0.0722 0.097 Uiso 1 1 calc R . . H51B H -0.3492 0.2321 0.0058 0.097 Uiso 1 1 calc R . . H51C H -0.3567 0.3206 -0.0268 0.097 Uiso 1 1 calc R . . C52 C -0.51747(18) 0.0980(3) -0.2738(2) 0.0651(12) Uani 1 1 d . . . H52A H -0.4817 0.1086 -0.2688 0.098 Uiso 1 1 calc R . . H52B H -0.5311 0.1257 -0.3135 0.098 Uiso 1 1 calc R . . H52C H -0.5232 0.0391 -0.2780 0.098 Uiso 1 1 calc R . . C53 C -0.17766(16) 0.3539(3) -0.7470(2) 0.0597(11) Uani 1 1 d . . . H53A H -0.1938 0.3918 -0.7163 0.072 Uiso 1 1 calc R . . H53B H -0.1993 0.3502 -0.7877 0.072 Uiso 1 1 calc R . . C54 C -0.10095(19) 0.4772(3) -0.7039(2) 0.0659(12) Uani 1 1 d . . . C55 C -0.1376(2) 0.5295(3) -0.6780(3) 0.0768(14) Uani 1 1 d . . . H55A H -0.1714 0.5233 -0.6925 0.092 Uiso 1 1 calc R . . C56 C -0.1244(3) 0.5899(4) -0.6316(3) 0.096(2) Uani 1 1 d . . . H56A H -0.1489 0.6253 -0.6152 0.115 Uiso 1 1 calc R . . C57 C -0.0744(4) 0.5976(5) -0.6096(3) 0.106(2) Uani 1 1 d . . . H57A H -0.0652 0.6384 -0.5780 0.127 Uiso 1 1 calc R . . C58 C -0.0385(3) 0.5467(5) -0.6334(4) 0.109(2) Uani 1 1 d . . . H58A H -0.0051 0.5514 -0.6172 0.131 Uiso 1 1 calc R . . C59 C -0.0516(2) 0.4871(4) -0.6822(3) 0.0830(15) Uani 1 1 d . . . H59A H -0.0266 0.4538 -0.7001 0.100 Uiso 1 1 calc R . . C60 C -0.13500(18) 0.4651(3) -0.8422(2) 0.0666(12) Uani 1 1 d . . . C61 C -0.1542(2) 0.4235(4) -0.9001(3) 0.0828(15) Uani 1 1 d . . . H61A H -0.1577 0.3659 -0.9002 0.099 Uiso 1 1 calc R . . C62 C -0.1678(3) 0.4697(5) -0.9574(3) 0.0963(19) Uani 1 1 d . . . H62A H -0.1817 0.4434 -0.9957 0.116 Uiso 1 1 calc R . . C63 C -0.1606(2) 0.5552(5) -0.9572(3) 0.099(2) Uani 1 1 d . . . H63A H -0.1698 0.5859 -0.9956 0.119 Uiso 1 1 calc R . . C64 C -0.1407(3) 0.5941(4) -0.9024(3) 0.0908(17) Uani 1 1 d . . . H64A H -0.1355 0.6514 -0.9037 0.109 Uiso 1 1 calc R . . C65 C -0.1278(2) 0.5505(4) -0.8442(3) 0.0789(14) Uani 1 1 d . . . H65A H -0.1143 0.5784 -0.8063 0.095 Uiso 1 1 calc R . . C66 C -0.17205(16) 0.2025(3) -0.7617(2) 0.0539(10) Uani 1 1 d . . . H66A H -0.1914 0.2152 -0.8032 0.065 Uiso 1 1 calc R . . H66B H -0.1872 0.1538 -0.7415 0.065 Uiso 1 1 calc R . . C67 C -0.08215(16) 0.1104(3) -0.7131(2) 0.0580(10) Uani 1 1 d . . . C68 C -0.1121(2) 0.0744(4) -0.6666(3) 0.0805(15) Uani 1 1 d . . . H68A H -0.1471 0.0798 -0.6712 0.097 Uiso 1 1 calc R . . C69 C -0.0909(3) 0.0305(4) -0.6133(3) 0.096(2) Uani 1 1 d . . . H69A H -0.1116 0.0062 -0.5819 0.115 Uiso 1 1 calc R . . C70 C -0.0391(3) 0.0222(4) -0.6061(3) 0.0871(17) Uani 1 1 d . . . H70A H -0.0246 -0.0062 -0.5691 0.105 Uiso 1 1 calc R . . C71 C -0.0093(2) 0.0553(4) -0.6528(3) 0.0893(17) Uani 1 1 d . . . H71A H 0.0257 0.0481 -0.6490 0.107 Uiso 1 1 calc R . . C72 C -0.03067(19) 0.0996(4) -0.7064(3) 0.0742(13) Uani 1 1 d . . . H72A H -0.0099 0.1225 -0.7384 0.089 Uiso 1 1 calc R . . C73 C -0.11672(17) 0.1052(3) -0.8530(2) 0.0600(11) Uani 1 1 d . . . C74 C -0.1529(2) 0.0433(4) -0.8503(3) 0.0725(13) Uani 1 1 d . . . H74A H -0.1720 0.0383 -0.8121 0.087 Uiso 1 1 calc R . . C75 C -0.1610(2) -0.0118(4) -0.9041(3) 0.0790(14) Uani 1 1 d . . . H75A H -0.1857 -0.0530 -0.9018 0.095 Uiso 1 1 calc R . . C76 C -0.1331(2) -0.0056(4) -0.9595(3) 0.0774(14) Uani 1 1 d . . . H76A H -0.1381 -0.0431 -0.9950 0.093 Uiso 1 1 calc R . . C77 C -0.0978(2) 0.0552(4) -0.9635(2) 0.0822(16) Uani 1 1 d . . . H77A H -0.0790 0.0593 -1.0021 0.099 Uiso 1 1 calc R . . C78 C -0.0891(2) 0.1124(3) -0.9103(2) 0.0705(13) Uani 1 1 d . . . H78A H -0.0650 0.1544 -0.9138 0.085 Uiso 1 1 calc R . . C79 C -0.0011(5) 0.3171(4) -0.9145(5) 0.135(4) Uani 1 1 d . . . C80 C 0.0456(6) 0.3209(6) -0.9507(8) 0.197(8) Uani 1 1 d . . . H80A H 0.0452 0.3266 -0.9975 0.237 Uiso 1 1 calc R . . C81 C 0.0921(7) 0.3157(7) -0.9119(13) 0.269(14) Uani 1 1 d . . . H81A H 0.1226 0.3142 -0.9338 0.323 Uiso 1 1 calc R . . C82 C 0.0925(2) 0.3130(4) -0.8415(5) 0.183(7) Uani 1 1 d G . . C83 C 0.13775(15) 0.3154(4) -0.8029(7) 0.274(15) Uani 1 1 d G . . H83A H 0.1685 0.3191 -0.8239 0.329 Uiso 1 1 calc R . . C84 C 0.13697(16) 0.3123(4) -0.7327(6) 0.287(16) Uani 1 1 d G . . H84A H 0.1672 0.3139 -0.7069 0.344 Uiso 1 1 calc R . . C85 C 0.0910(2) 0.3068(4) -0.7012(5) 0.175(7) Uani 1 1 d G . . C86 C 0.0876(6) 0.3077(7) -0.6306(11) 0.217(10) Uani 1 1 d . . . H86A H 0.1168 0.3129 -0.6031 0.260 Uiso 1 1 calc R . . C87 C 0.0416(5) 0.3010(5) -0.6022(7) 0.169(6) Uani 1 1 d . . . H87A H 0.0399 0.3010 -0.5553 0.202 Uiso 1 1 calc R . . C88 C -0.0038(4) 0.2941(4) -0.6429(5) 0.120(3) Uani 1 1 d . . . C89 C 0.04579(15) 0.3044(3) -0.7399(4) 0.116(3) Uani 1 1 d G . . C90 C 0.04657(15) 0.3075(3) -0.8100(4) 0.122(3) Uani 1 1 d G . . C91 C -0.0503(5) 0.3291(6) -0.9499(4) 0.158(5) Uani 1 1 d . . . H91A H -0.0768 0.3245 -0.9183 0.237 Uiso 1 1 calc R . . H91B H -0.0550 0.2874 -0.9844 0.237 Uiso 1 1 calc R . . H91C H -0.0515 0.3834 -0.9703 0.237 Uiso 1 1 calc R . . C92 C -0.0547(4) 0.2870(5) -0.6143(3) 0.114(2) Uani 1 1 d . . . H92A H -0.0800 0.2831 -0.6505 0.171 Uiso 1 1 calc R . . H92B H -0.0611 0.3353 -0.5874 0.171 Uiso 1 1 calc R . . H92C H -0.0559 0.2379 -0.5866 0.171 Uiso 1 1 calc R . . B1 B -0.2715(2) -0.0440(4) -0.7603(4) 0.0753(16) Uani 1 1 d . . . B2 B -0.2243(5) 0.7653(8) -1.0183(11) 0.167(6) Uani 1 1 d . . . F1 F -0.24686(17) -0.0912(3) -0.8053(3) 0.1438(18) Uani 1 1 d . . . F2 F -0.23940(16) 0.0118(3) -0.7281(2) 0.1197(14) Uani 1 1 d . . . F3 F -0.29172(15) -0.0983(3) -0.7128(2) 0.1198(14) Uani 1 1 d . . . F4 F -0.30943(13) -0.0028(2) -0.7912(2) 0.1055(11) Uani 1 1 d . . . F5 F -0.2275(6) 0.6881(5) -1.0312(7) 0.321(7) Uani 1 1 d . . . F6 F -0.1859(4) 0.7888(8) -0.9979(5) 0.267(6) Uani 1 1 d . . . F7 F -0.2637(4) 0.7871(6) -0.9927(10) 0.434(13) Uani 1 1 d . . . F8 F -0.2280(6) 0.7965(8) -1.0889(9) 0.349(9) Uani 1 1 d . . . O1 O -0.2389(4) 0.5285(5) -1.0876(5) 0.208(4) Uani 1 1 d . . . O2 O -0.6562(3) 0.2534(4) 0.1527(3) 0.159(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 Cu1 0.0458(3) 0.0564(3) 0.0361(3) -0.0058(2) 0.0116(2) -0.0045(2) Cu2 0.0514(4) 0.0755(5) 0.0654(4) -0.0002(3) 0.0179(3) -0.0052(3) P1 0.0503(5) 0.0496(5) 0.0393(5) -0.0018(4) 0.0118(4) -0.0031(4) P2 0.0439(5) 0.0520(5) 0.0375(5) -0.0046(4) 0.0116(4) 0.0006(4) P3 0.0520(6) 0.0669(7) 0.0554(6) 0.0023(5) 0.0123(5) -0.0045(5) P4 0.0502(6) 0.0677(7) 0.0513(6) -0.0038(5) 0.0171(5) -0.0018(5) N1 0.0497(18) 0.0464(17) 0.0451(16) -0.0007(14) 0.0191(14) 0.0011(14) N2 0.057(2) 0.062(2) 0.0538(19) -0.0037(16) 0.0263(16) -0.0051(17) N3 0.0476(17) 0.0559(19) 0.0368(15) -0.0020(14) 0.0092(13) -0.0063(15) N4 0.0544(19) 0.0475(17) 0.0376(15) -0.0008(13) 0.0079(14) 0.0017(15) N5 0.102(4) 0.067(3) 0.144(5) 0.001(3) 0.079(4) -0.004(3) N6 0.068(3) 0.068(3) 0.138(5) -0.011(3) -0.015(3) -0.005(2) C1 0.0355(18) 0.051(2) 0.0476(19) 0.0007(17) 0.0115(15) -0.0008(16) C2 0.050(2) 0.052(2) 0.048(2) -0.0048(17) 0.0125(17) -0.0033(18) C3 0.052(2) 0.054(2) 0.046(2) 0.0008(17) 0.0134(17) -0.0066(18) C4 0.041(2) 0.053(2) 0.0457(19) 0.0010(17) 0.0088(16) -0.0028(17) C5 0.050(2) 0.047(2) 0.053(2) -0.0050(17) 0.0159(18) 0.0034(17) C6 0.054(2) 0.044(2) 0.053(2) -0.0003(17) 0.0190(18) -0.0004(18) C7 0.044(2) 0.054(2) 0.049(2) -0.0007(17) 0.0158(16) -0.0010(17) C8 0.055(2) 0.061(3) 0.056(2) -0.0109(19) 0.0185(19) -0.011(2) C9 0.064(3) 0.061(3) 0.065(3) -0.006(2) 0.028(2) -0.015(2) C10 0.042(2) 0.060(2) 0.054(2) -0.0041(19) 0.0184(17) 0.0002(18) C11 0.045(2) 0.056(2) 0.051(2) -0.0065(17) 0.0164(17) -0.0031(18) C12 0.047(2) 0.055(2) 0.055(2) 0.0015(18) 0.0170(18) -0.0007(18) C13 0.047(2) 0.053(2) 0.050(2) -0.0023(17) 0.0124(17) 0.0028(18) C14 0.051(2) 0.058(2) 0.045(2) -0.0037(17) 0.0147(17) -0.0062(19) C15 0.057(2) 0.056(2) 0.049(2) -0.0038(18) 0.0133(18) -0.0025(19) C16 0.070(3) 0.076(3) 0.047(2) -0.012(2) 0.009(2) -0.005(2) C17 0.090(4) 0.072(3) 0.061(3) -0.023(2) 0.020(2) -0.010(3) C18 0.092(4) 0.053(3) 0.079(3) -0.010(2) 0.018(3) -0.004(3) C19 0.077(3) 0.052(2) 0.057(2) -0.003(2) 0.015(2) -0.007(2) C20 0.058(2) 0.053(2) 0.049(2) 0.0008(17) 0.0109(18) -0.0070(19) C21 0.068(3) 0.077(3) 0.068(3) 0.011(2) 0.017(2) -0.002(3) C22 0.072(3) 0.078(3) 0.089(4) 0.018(3) 0.000(3) 0.006(3) C23 0.088(4) 0.071(3) 0.067(3) 0.018(2) -0.006(3) -0.009(3) C24 0.087(4) 0.073(3) 0.051(2) 0.010(2) 0.011(2) -0.010(3) C25 0.071(3) 0.060(3) 0.049(2) 0.0005(19) 0.013(2) -0.004(2) C26 0.048(2) 0.050(2) 0.048(2) -0.0008(17) 0.0140(17) 0.0033(17) C27 0.051(2) 0.058(2) 0.0401(19) -0.0102(17) 0.0087(16) 0.0061(19) C28 0.063(3) 0.075(3) 0.053(2) 0.009(2) 0.005(2) 0.001(2) C29 0.092(4) 0.076(3) 0.063(3) 0.013(2) 0.005(3) 0.014(3) C30 0.086(4) 0.083(3) 0.055(3) -0.012(2) -0.012(2) 0.032(3) C31 0.060(3) 0.085(3) 0.061(3) -0.019(3) -0.004(2) 0.005(2) C32 0.058(3) 0.075(3) 0.050(2) -0.010(2) 0.0074(19) -0.001(2) C33 0.066(3) 0.050(2) 0.0334(17) -0.0027(16) 0.0112(17) 0.0019(19) C34 0.062(2) 0.057(2) 0.0384(19) 0.0004(17) 0.0172(17) 0.009(2) C35 0.079(3) 0.066(3) 0.0374(19) 0.0025(19) 0.018(2) 0.019(2) C36 0.103(4) 0.061(3) 0.037(2) -0.0065(19) 0.006(2) 0.021(3) C37 0.088(3) 0.053(3) 0.059(2) -0.008(2) -0.007(2) 0.004(2) C38 0.061(3) 0.055(2) 0.056(2) -0.0124(19) 0.0039(19) 0.002(2) C39 0.075(3) 0.048(2) 0.0387(19) 0.0003(16) -0.0020(19) -0.001(2) C40 0.093(4) 0.062(3) 0.036(2) -0.0031(18) 0.000(2) -0.004(2) C41 0.116(4) 0.056(3) 0.033(2) -0.0028(18) 0.018(2) -0.001(3) C42 0.081(3) 0.051(2) 0.040(2) 0.0012(17) 0.028(2) 0.006(2) C43 0.084(3) 0.055(3) 0.056(2) 0.003(2) 0.036(3) 0.005(2) C44 0.065(3) 0.056(3) 0.071(3) 0.009(2) 0.036(2) 0.004(2) C45 0.055(2) 0.051(2) 0.053(2) 0.0075(18) 0.0210(19) 0.0011(18) C46 0.051(2) 0.061(3) 0.074(3) 0.007(2) 0.013(2) -0.005(2) C47 0.053(2) 0.068(3) 0.060(2) 0.000(2) 0.0022(19) -0.018(2) C48 0.061(2) 0.060(2) 0.043(2) 0.0020(18) 0.0054(18) -0.009(2) C49 0.064(3) 0.0427(19) 0.0345(18) 0.0029(15) 0.0154(17) 0.0010(18) C50 0.057(2) 0.046(2) 0.0384(18) 0.0018(15) 0.0157(17) 0.0007(17) C51 0.069(3) 0.068(3) 0.056(2) -0.006(2) -0.009(2) -0.006(2) C52 0.068(3) 0.082(3) 0.045(2) -0.017(2) 0.009(2) -0.017(2) C53 0.050(2) 0.072(3) 0.058(2) 0.004(2) 0.0148(19) -0.001(2) C54 0.073(3) 0.071(3) 0.054(2) 0.004(2) 0.010(2) -0.011(2) C55 0.092(4) 0.068(3) 0.072(3) 0.001(3) 0.026(3) -0.011(3) C56 0.150(6) 0.070(3) 0.071(3) -0.004(3) 0.035(4) -0.021(4) C57 0.158(7) 0.079(4) 0.079(4) -0.008(3) -0.006(4) -0.032(5) C58 0.131(6) 0.092(5) 0.102(5) 0.004(4) -0.032(4) -0.024(5) C59 0.083(4) 0.077(3) 0.088(4) 0.002(3) -0.011(3) -0.012(3) C60 0.060(3) 0.076(3) 0.064(3) 0.009(2) 0.011(2) -0.006(2) C61 0.085(4) 0.095(4) 0.069(3) 0.016(3) 0.007(3) -0.019(3) C62 0.097(4) 0.119(5) 0.072(3) 0.024(3) 0.003(3) -0.033(4) C63 0.090(4) 0.124(6) 0.084(4) 0.041(4) 0.006(3) -0.019(4) C64 0.103(4) 0.084(4) 0.087(4) 0.022(3) 0.025(3) -0.007(3) C65 0.073(3) 0.083(4) 0.083(3) 0.007(3) 0.025(3) 0.000(3) C66 0.046(2) 0.067(3) 0.050(2) -0.0048(19) 0.0120(17) -0.0053(19) C67 0.055(2) 0.069(3) 0.050(2) -0.012(2) 0.0103(18) 0.009(2) C68 0.070(3) 0.095(4) 0.078(3) 0.020(3) 0.027(3) 0.017(3) C69 0.117(5) 0.096(4) 0.078(3) 0.019(3) 0.044(3) 0.037(4) C70 0.114(5) 0.087(4) 0.060(3) 0.003(3) -0.005(3) 0.023(4) C71 0.071(3) 0.086(4) 0.109(4) 0.000(3) -0.013(3) 0.004(3) C72 0.064(3) 0.083(3) 0.076(3) 0.007(3) 0.012(2) 0.000(3) C73 0.060(3) 0.067(3) 0.053(2) -0.002(2) 0.0104(19) 0.011(2) C74 0.069(3) 0.083(3) 0.066(3) -0.011(3) 0.014(2) 0.005(3) C75 0.077(3) 0.075(3) 0.085(3) -0.016(3) 0.001(3) 0.004(3) C76 0.095(4) 0.076(3) 0.061(3) -0.015(2) -0.007(3) 0.017(3) C77 0.110(4) 0.088(4) 0.050(3) -0.001(2) 0.014(3) 0.018(3) C78 0.081(3) 0.074(3) 0.058(3) 0.003(2) 0.016(2) 0.004(3) C79 0.205(10) 0.074(4) 0.136(7) 0.019(4) 0.127(8) 0.011(5) C80 0.258(15) 0.084(5) 0.268(15) 0.034(7) 0.221(14) 0.031(8) C81 0.234(16) 0.080(6) 0.52(3) 0.004(11) 0.30(2) 0.010(8) C82 0.092(7) 0.073(5) 0.39(2) -0.012(8) 0.118(10) -0.007(4) C83 0.046(6) 0.097(7) 0.68(5) 0.035(13) 0.063(11) -0.003(5) C84 0.076(9) 0.109(9) 0.67(5) -0.020(15) -0.078(14) -0.005(6) C85 0.074(6) 0.068(4) 0.38(2) -0.015(8) -0.068(9) -0.003(3) C86 0.135(9) 0.094(6) 0.41(3) -0.018(11) -0.157(15) -0.006(6) C87 0.208(12) 0.079(5) 0.207(11) -0.016(6) -0.133(10) 0.006(6) C88 0.174(8) 0.066(4) 0.113(6) -0.010(4) -0.080(6) 0.013(4) C89 0.059(4) 0.064(4) 0.224(10) -0.009(5) 0.000(5) -0.003(3) C90 0.058(4) 0.065(4) 0.247(11) -0.009(5) 0.059(6) -0.006(3) C91 0.270(14) 0.135(7) 0.074(5) 0.016(5) 0.072(7) 0.038(9) C92 0.161(8) 0.110(6) 0.069(4) -0.001(3) -0.009(4) 0.000(5) B1 0.055(3) 0.076(4) 0.096(4) 0.003(3) 0.016(3) -0.007(3) B2 0.113(8) 0.095(8) 0.30(2) 0.043(10) 0.051(11) 0.030(7) F1 0.101(3) 0.128(3) 0.206(5) -0.046(3) 0.047(3) 0.014(3) F2 0.112(3) 0.131(3) 0.117(3) -0.015(2) 0.010(2) -0.048(3) F3 0.105(3) 0.116(3) 0.138(3) 0.044(3) -0.008(2) -0.028(2) F4 0.082(2) 0.0709(19) 0.165(3) 0.021(2) 0.011(2) -0.0016(17) F5 0.446(19) 0.126(6) 0.381(16) -0.009(7) -0.103(14) 0.044(8) F6 0.221(9) 0.375(15) 0.209(8) -0.064(9) 0.042(7) -0.138(10) F7 0.251(10) 0.225(9) 0.85(3) 0.181(14) 0.371(17) 0.113(8) F8 0.41(2) 0.246(11) 0.399(19) 0.108(13) 0.124(16) 0.136(12) O1 0.282(11) 0.144(6) 0.194(7) 0.011(6) -0.056(7) 0.022(6) O2 0.210(7) 0.134(5) 0.133(5) -0.017(4) 0.030(5) 0.030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.072(3) . ? Cu1 N4 2.089(3) . ? Cu1 P1 2.2445(11) . ? Cu1 P2 2.2647(11) . ? Cu2 N5 2.072(5) . ? Cu2 N6 2.111(5) . ? Cu2 P3 2.2550(14) . ? Cu2 P4 2.2617(14) . ? P1 C20 1.816(4) . ? P1 C14 1.820(4) . ? P1 C13 1.878(4) . ? P2 C27 1.834(4) . ? P2 C33 1.834(4) . ? P2 C26 1.849(4) . ? P3 C54 1.828(5) . ? P3 C60 1.828(5) . ? P3 C53 1.866(4) . ? P4 C67 1.832(5) . ? P4 C73 1.839(5) . ? P4 C66 1.857(4) . ? N1 C1 1.431(5) . ? N1 C26 1.459(5) . ? N1 C13 1.468(5) . ? N2 C10 1.425(5) . ? N2 C66 1.448(6) . ? N2 C53 1.449(6) . ? N3 C48 1.324(5) . ? N3 C50 1.372(5) . ? N4 C39 1.326(5) . ? N4 C49 1.360(5) . ? N5 C79 1.309(12) . ? N5 C90 1.405(9) . ? N6 C88 1.358(11) . ? N6 C89 1.360(7) . ? C1 C2 1.394(6) . ? C1 C6 1.394(6) . ? C2 C3 1.382(6) . ? C2 H2A 0.9300 . ? C3 C4 1.387(6) . ? C3 H3A 0.9300 . ? C4 C5 1.387(6) . ? C4 C7 1.490(5) . ? C5 C6 1.398(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.390(6) . ? C7 C8 1.395(6) . ? C8 C9 1.389(6) . ? C8 H8A 0.9300 . ? C9 C10 1.397(6) . ? C9 H9A 0.9300 . ? C10 C11 1.385(6) . ? C11 C12 1.400(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.390(6) . ? C14 C19 1.396(6) . ? C15 C16 1.384(6) . ? C15 H15A 0.9300 . ? C16 C17 1.384(7) . ? C16 H16A 0.9300 . ? C17 C18 1.369(8) . ? C17 H17A 0.9300 . ? C18 C19 1.384(7) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.393(7) . ? C20 C25 1.403(6) . ? C21 C22 1.379(7) . ? C21 H21A 0.9300 . ? C22 C23 1.397(8) . ? C22 H22A 0.9300 . ? C23 C24 1.337(8) . ? C23 H23A 0.9300 . ? C24 C25 1.386(7) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.376(6) . ? C27 C32 1.391(6) . ? C28 C29 1.386(7) . ? C28 H28A 0.9300 . ? C29 C30 1.384(8) . ? C29 H29A 0.9300 . ? C30 C31 1.363(8) . ? C30 H30A 0.9300 . ? C31 C32 1.377(7) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.392(6) . ? C33 C38 1.394(6) . ? C34 C35 1.388(6) . ? C34 H34A 0.9300 . ? C35 C36 1.370(7) . ? C35 H35A 0.9300 . ? C36 C37 1.383(7) . ? C36 H36A 0.9300 . ? C37 C38 1.394(6) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.407(6) . ? C39 C51 1.481(7) . ? C40 C41 1.347(8) . ? C40 H40A 0.9300 . ? C41 C42 1.411(7) . ? C41 H41A 0.9300 . ? C42 C43 1.416(7) . ? C42 C49 1.421(5) . ? C43 C44 1.339(7) . ? C43 H43A 0.9300 . ? C44 C45 1.437(6) . ? C44 H44A 0.9300 . ? C45 C46 1.399(7) . ? C45 C50 1.409(6) . ? C46 C47 1.363(6) . ? C46 H46A 0.9300 . ? C47 C48 1.410(6) . ? C47 H47A 0.9300 . ? C48 C52 1.497(6) . ? C49 C50 1.421(6) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C59 1.363(8) . ? C54 C55 1.394(7) . ? C55 C56 1.371(8) . ? C55 H55A 0.9300 . ? C56 C57 1.379(11) . ? C56 H56A 0.9300 . ? C57 C58 1.349(11) . ? C57 H57A 0.9300 . ? C58 C59 1.392(9) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C65 1.385(8) . ? C60 C61 1.402(8) . ? C61 C62 1.389(8) . ? C61 H61A 0.9300 . ? C62 C63 1.383(10) . ? C62 H62A 0.9300 . ? C63 C64 1.341(9) . ? C63 H63A 0.9300 . ? C64 C65 1.379(8) . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.365(7) . ? C67 C72 1.370(7) . ? C68 C69 1.369(8) . ? C68 H68A 0.9300 . ? C69 C70 1.375(9) . ? C69 H69A 0.9300 . ? C70 C71 1.347(9) . ? C70 H70A 0.9300 . ? C71 C72 1.377(8) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C74 1.380(7) . ? C73 C78 1.380(6) . ? C74 C75 1.394(7) . ? C74 H74A 0.9300 . ? C75 C76 1.352(8) . ? C75 H75A 0.9300 . ? C76 C77 1.353(8) . ? C76 H76A 0.9300 . ? C77 C78 1.408(8) . ? C77 H77A 0.9300 . ? C78 H78A 0.9300 . ? C79 C80 1.454(12) . ? C79 C91 1.461(15) . ? C80 C81 1.42(3) . ? C80 H80A 0.9300 . ? C81 C82 1.39(3) . ? C81 H81A 0.9300 . ? C82 C83 1.3900 . ? C82 C90 1.3900 . ? C83 C84 1.3900 . ? C83 H83A 0.9300 . ? C84 C85 1.3900 . ? C84 H84A 0.9300 . ? C85 C89 1.3900 . ? C85 C86 1.40(2) . ? C86 C87 1.36(2) . ? C86 H86A 0.9300 . ? C87 C88 1.421(12) . ? C87 H87A 0.9300 . ? C88 C92 1.483(13) . ? C89 C90 1.3900 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? B1 F4 1.327(8) . ? B1 F1 1.356(8) . ? B1 F2 1.371(8) . ? B1 F3 1.403(7) . ? B2 F6 1.139(17) . ? B2 F7 1.224(14) . ? B2 F5 1.267(16) . ? B2 F8 1.48(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N4 80.40(12) . . ? N3 Cu1 P1 126.15(10) . . ? N4 Cu1 P1 121.66(10) . . ? N3 Cu1 P2 119.24(10) . . ? N4 Cu1 P2 104.22(9) . . ? P1 Cu1 P2 102.93(4) . . ? N5 Cu2 N6 81.5(3) . . ? N5 Cu2 P3 122.27(15) . . ? N6 Cu2 P3 112.00(15) . . ? N5 Cu2 P4 122.08(15) . . ? N6 Cu2 P4 111.56(15) . . ? P3 Cu2 P4 104.97(5) . . ? C20 P1 C14 104.91(19) . . ? C20 P1 C13 100.35(19) . . ? C14 P1 C13 101.06(17) . . ? C20 P1 Cu1 117.42(14) . . ? C14 P1 Cu1 120.02(14) . . ? C13 P1 Cu1 110.19(13) . . ? C27 P2 C33 101.54(18) . . ? C27 P2 C26 107.10(18) . . ? C33 P2 C26 101.93(19) . . ? C27 P2 Cu1 121.14(14) . . ? C33 P2 Cu1 112.65(13) . . ? C26 P2 Cu1 110.52(13) . . ? C54 P3 C60 102.6(2) . . ? C54 P3 C53 105.0(2) . . ? C60 P3 C53 101.5(2) . . ? C54 P3 Cu2 118.37(18) . . ? C60 P3 Cu2 118.23(17) . . ? C53 P3 Cu2 109.20(16) . . ? C67 P4 C73 103.3(2) . . ? C67 P4 C66 104.80(19) . . ? C73 P4 C66 100.2(2) . . ? C67 P4 Cu2 110.89(16) . . ? C73 P4 Cu2 125.47(15) . . ? C66 P4 Cu2 109.97(15) . . ? C1 N1 C26 119.2(3) . . ? C1 N1 C13 118.2(3) . . ? C26 N1 C13 112.6(3) . . ? C10 N2 C66 121.3(4) . . ? C10 N2 C53 118.9(4) . . ? C66 N2 C53 115.7(3) . . ? C48 N3 C50 118.6(3) . . ? C48 N3 Cu1 129.1(3) . . ? C50 N3 Cu1 112.2(3) . . ? C39 N4 C49 119.2(3) . . ? C39 N4 Cu1 129.0(3) . . ? C49 N4 Cu1 111.3(2) . . ? C79 N5 C90 122.7(7) . . ? C79 N5 Cu2 127.7(7) . . ? C90 N5 Cu2 109.6(5) . . ? C88 N6 C89 121.6(7) . . ? C88 N6 Cu2 127.5(6) . . ? C89 N6 Cu2 110.8(5) . . ? C2 C1 C6 117.1(3) . . ? C2 C1 N1 123.1(3) . . ? C6 C1 N1 119.8(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 122.6(4) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C5 C4 C3 116.5(3) . . ? C5 C4 C7 122.1(4) . . ? C3 C4 C7 121.3(4) . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 121.1(4) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C12 C7 C8 116.5(4) . . ? C12 C7 C4 122.1(4) . . ? C8 C7 C4 121.3(4) . . ? C9 C8 C7 121.8(4) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C10 121.3(4) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 117.5(4) . . ? C11 C10 N2 122.7(4) . . ? C9 C10 N2 119.7(4) . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C7 C12 C11 122.1(4) . . ? C7 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? N1 C13 P1 115.0(3) . . ? N1 C13 H13A 108.5 . . ? P1 C13 H13A 108.5 . . ? N1 C13 H13B 108.5 . . ? P1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C19 118.1(4) . . ? C15 C14 P1 118.1(3) . . ? C19 C14 P1 123.7(3) . . ? C16 C15 C14 121.3(4) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C18 C17 C16 120.0(4) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.7(5) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C18 C19 C14 120.3(4) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? C21 C20 C25 118.3(4) . . ? C21 C20 P1 122.2(3) . . ? C25 C20 P1 119.4(3) . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C24 C23 C22 119.5(5) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 121.8(4) . . ? C23 C24 H24A 119.1 . . ? C25 C24 H24A 119.1 . . ? C24 C25 C20 119.8(5) . . ? C24 C25 H25A 120.1 . . ? C20 C25 H25A 120.1 . . ? N1 C26 P2 112.5(3) . . ? N1 C26 H26A 109.1 . . ? P2 C26 H26A 109.1 . . ? N1 C26 H26B 109.1 . . ? P2 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C32 118.7(4) . . ? C28 C27 P2 124.8(3) . . ? C32 C27 P2 116.4(3) . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 120.0(5) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 120.0(5) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.1(5) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C27 120.8(5) . . ? C31 C32 H32A 119.6 . . ? C27 C32 H32A 119.6 . . ? C34 C33 C38 119.4(4) . . ? C34 C33 P2 116.1(3) . . ? C38 C33 P2 124.4(3) . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 120.8(4) . . ? C35 C36 H36A 119.6 . . ? C37 C36 H36A 119.6 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H37A 120.3 . . ? C38 C37 H37A 120.3 . . ? C37 C38 C33 120.2(4) . . ? C37 C38 H38A 119.9 . . ? C33 C38 H38A 119.9 . . ? N4 C39 C40 121.3(4) . . ? N4 C39 C51 119.0(4) . . ? C40 C39 C51 119.8(4) . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C40 C41 C42 120.9(4) . . ? C40 C41 H41A 119.5 . . ? C42 C41 H41A 119.5 . . ? C41 C42 C43 125.1(4) . . ? C41 C42 C49 115.5(4) . . ? C43 C42 C49 119.4(4) . . ? C44 C43 C42 121.7(4) . . ? C44 C43 H43A 119.2 . . ? C42 C43 H43A 119.2 . . ? C43 C44 C45 120.9(4) . . ? C43 C44 H44A 119.5 . . ? C45 C44 H44A 119.5 . . ? C46 C45 C50 117.4(4) . . ? C46 C45 C44 124.0(4) . . ? C50 C45 C44 118.6(4) . . ? C47 C46 C45 119.6(4) . . ? C47 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C46 C47 C48 120.2(4) . . ? C46 C47 H47A 119.9 . . ? C48 C47 H47A 119.9 . . ? N3 C48 C47 121.7(4) . . ? N3 C48 C52 117.5(4) . . ? C47 C48 C52 120.7(4) . . ? N4 C49 C50 118.2(3) . . ? N4 C49 C42 122.9(4) . . ? C50 C49 C42 118.8(4) . . ? N3 C50 C45 122.6(4) . . ? N3 C50 C49 117.0(4) . . ? C45 C50 C49 120.5(3) . . ? C39 C51 H51A 109.5 . . ? C39 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C39 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52A 109.5 . . ? C48 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C48 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N2 C53 P3 115.8(3) . . ? N2 C53 H53A 108.3 . . ? P3 C53 H53A 108.3 . . ? N2 C53 H53B 108.3 . . ? P3 C53 H53B 108.3 . . ? H53A C53 H53B 107.4 . . ? C59 C54 C55 119.0(5) . . ? C59 C54 P3 118.4(4) . . ? C55 C54 P3 122.5(4) . . ? C56 C55 C54 120.7(6) . . ? C56 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? C55 C56 C57 119.3(7) . . ? C55 C56 H56A 120.4 . . ? C57 C56 H56A 120.4 . . ? C58 C57 C56 120.7(6) . . ? C58 C57 H57A 119.6 . . ? C56 C57 H57A 119.6 . . ? C57 C58 C59 120.1(7) . . ? C57 C58 H58A 119.9 . . ? C59 C58 H58A 119.9 . . ? C54 C59 C58 120.2(7) . . ? C54 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? C65 C60 C61 119.6(5) . . ? C65 C60 P3 123.5(4) . . ? C61 C60 P3 116.7(4) . . ? C62 C61 C60 119.0(6) . . ? C62 C61 H61A 120.5 . . ? C60 C61 H61A 120.5 . . ? C63 C62 C61 119.7(6) . . ? C63 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? C64 C63 C62 120.8(6) . . ? C64 C63 H63A 119.6 . . ? C62 C63 H63A 119.6 . . ? C63 C64 C65 121.0(6) . . ? C63 C64 H64A 119.5 . . ? C65 C64 H64A 119.5 . . ? C64 C65 C60 119.7(6) . . ? C64 C65 H65A 120.1 . . ? C60 C65 H65A 120.1 . . ? N2 C66 P4 112.2(3) . . ? N2 C66 H66A 109.2 . . ? P4 C66 H66A 109.2 . . ? N2 C66 H66B 109.2 . . ? P4 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? C68 C67 C72 118.8(5) . . ? C68 C67 P4 124.5(4) . . ? C72 C67 P4 116.7(4) . . ? C67 C68 C69 120.5(5) . . ? C67 C68 H68A 119.7 . . ? C69 C68 H68A 119.7 . . ? C68 C69 C70 120.2(5) . . ? C68 C69 H69A 119.9 . . ? C70 C69 H69A 119.9 . . ? C71 C70 C69 119.7(5) . . ? C71 C70 H70A 120.1 . . ? C69 C70 H70A 120.1 . . ? C70 C71 C72 120.1(6) . . ? C70 C71 H71A 120.0 . . ? C72 C71 H71A 120.0 . . ? C67 C72 C71 120.8(5) . . ? C67 C72 H72A 119.6 . . ? C71 C72 H72A 119.6 . . ? C74 C73 C78 118.8(5) . . ? C74 C73 P4 121.1(3) . . ? C78 C73 P4 120.1(4) . . ? C73 C74 C75 120.8(5) . . ? C73 C74 H74A 119.6 . . ? C75 C74 H74A 119.6 . . ? C76 C75 C74 120.1(6) . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C77 120.1(5) . . ? C75 C76 H76A 120.0 . . ? C77 C76 H76A 120.0 . . ? C76 C77 C78 121.2(5) . . ? C76 C77 H77A 119.4 . . ? C78 C77 H77A 119.4 . . ? C73 C78 C77 119.0(5) . . ? C73 C78 H78A 120.5 . . ? C77 C78 H78A 120.5 . . ? N5 C79 C80 119.9(13) . . ? N5 C79 C91 119.0(7) . . ? C80 C79 C91 120.9(11) . . ? C81 C80 C79 117.5(14) . . ? C81 C80 H80A 121.3 . . ? C79 C80 H80A 121.3 . . ? C82 C81 C80 120.8(8) . . ? C82 C81 H81A 119.6 . . ? C80 C81 H81A 119.6 . . ? C83 C82 C90 120.0 . . ? C83 C82 C81 121.3(9) . . ? C90 C82 C81 118.7(9) . . ? C82 C83 C84 120.0 . . ? C82 C83 H83A 120.0 . . ? C84 C83 H83A 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C89 C85 C84 120.0 . . ? C89 C85 C86 117.3(8) . . ? C84 C85 C86 122.7(8) . . ? C87 C86 C85 120.4(9) . . ? C87 C86 H86A 119.8 . . ? C85 C86 H86A 119.8 . . ? C86 C87 C88 121.0(13) . . ? C86 C87 H87A 119.5 . . ? C88 C87 H87A 119.5 . . ? N6 C88 C87 117.6(11) . . ? N6 C88 C92 119.3(6) . . ? C87 C88 C92 123.0(10) . . ? N6 C89 C90 118.1(5) . . ? N6 C89 C85 121.8(5) . . ? C90 C89 C85 120.0 . . ? C89 C90 C82 120.0 . . ? C89 C90 N5 119.7(4) . . ? C82 C90 N5 120.2(4) . . ? C79 C91 H91A 109.5 . . ? C79 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C79 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C88 C92 H92A 109.5 . . ? C88 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C88 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? F4 B1 F1 110.4(6) . . ? F4 B1 F2 109.1(6) . . ? F1 B1 F2 111.5(5) . . ? F4 B1 F3 108.5(5) . . ? F1 B1 F3 107.5(6) . . ? F2 B1 F3 109.9(5) . . ? F6 B2 F7 121(2) . . ? F6 B2 F5 116.4(13) . . ? F7 B2 F5 108.3(14) . . ? F6 B2 F8 104.2(14) . . ? F7 B2 F8 105.6(14) . . ? F5 B2 F8 98.0(18) . . ? 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 _platon_squeeze_void_content 1 0.266 0.130 0.335 131 31 ' ' 2 0.734 -0.131 0.665 131 30 ' ' 3 0.266 0.369 0.835 131 31 ' ' 4 0.734 0.631 0.165 131 31 ' ' _platon_squeeze_details ; ? ; _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 62.52 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.783 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.083