# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Javier Ruiz' _publ_contact_author_email JRUIZ@UNIOVI.ES _publ_section_title ; Synthesis and Reactivity of Diphosphine Metal Complexes Bearing Peripheral Ketenimine Functionalities ; loop_ _publ_author_name 'Javier Ruiz' 'Marta P. Gonzalo' 'Marta E G Mosquera' 'Roberto Quesada' 'Marilin Vivanco' # Attachment '3a_5b_11.cif' #============================================================================= data_3a _database_code_depnum_ccdc_archive 'CCDC 720842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H58 Ag2 Cl2 N2 O8 P4' _chemical_formula_weight 1345.60 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.6256(2) _cell_length_b 13.3816(3) _cell_length_c 22.2405(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.0440(10) _cell_angle_gamma 90.00 _cell_volume 2848.78(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5459 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 70.02 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 7.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.277 _exptl_absorpt_correction_T_max 0.387 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43690 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 65.00 _reflns_number_total 4865 _reflns_number_gt 3972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1274P)^2^+19.3987P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4865 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2210 _refine_ls_wR_factor_gt 0.2146 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Ag1 Ag 0.64213(6) 0.03003(4) 0.02955(2) 0.0294(2) Uani 1 1 d . . . P2 P 0.55320(19) 0.19840(15) 0.00595(8) 0.0232(4) Uani 1 1 d . . . P3 P 0.7544(2) -0.12396(15) 0.00130(8) 0.0249(4) Uani 1 1 d . . . Cl1 Cl 0.61905(19) 0.03777(14) 0.20378(7) 0.0259(4) Uani 1 1 d . . . O1 O 0.5800(6) 0.0380(5) 0.1385(2) 0.0394(15) Uani 1 1 d . . . O2 O 0.7124(8) -0.0419(6) 0.2187(3) 0.0540(19) Uani 1 1 d . . . O3 O 0.6863(7) 0.1302(5) 0.2200(3) 0.0480(17) Uani 1 1 d . . . O4 O 0.4958(7) 0.0267(5) 0.2338(3) 0.0447(17) Uani 1 1 d . . . N1 N 0.6976(6) -0.3654(5) -0.0814(3) 0.0254(14) Uani 1 1 d . . . C1 C 0.6229(8) -0.2147(6) -0.0249(3) 0.0238(16) Uani 1 1 d . . . C2 C 0.6581(7) -0.2929(6) -0.0568(3) 0.0238(16) Uani 1 1 d . . . C4 C 0.7111(8) -0.3899(6) -0.1465(3) 0.0274(17) Uani 1 1 d . . . C5 C 0.6510(11) -0.4941(7) -0.1559(4) 0.043(2) Uani 1 1 d . . . H5A H 0.5528 -0.4927 -0.1517 0.064 Uiso 1 1 calc R . . H5B H 0.6970 -0.5386 -0.1263 0.064 Uiso 1 1 calc R . . H5C H 0.6652 -0.5171 -0.1957 0.064 Uiso 1 1 calc R . . C6 C 0.6334(10) -0.3158(8) -0.1878(4) 0.040(2) Uani 1 1 d . . . H6A H 0.5355 -0.3194 -0.1832 0.060 Uiso 1 1 calc R . . H6B H 0.6476 -0.3309 -0.2289 0.060 Uiso 1 1 calc R . . H6C H 0.6672 -0.2497 -0.1779 0.060 Uiso 1 1 calc R . . C7 C 0.8650(9) -0.3874(8) -0.1522(4) 0.037(2) Uani 1 1 d . . . H7A H 0.9117 -0.4359 -0.1255 0.055 Uiso 1 1 calc R . . H7B H 0.9009 -0.3220 -0.1418 0.055 Uiso 1 1 calc R . . H7C H 0.8809 -0.4026 -0.1931 0.055 Uiso 1 1 calc R . . C11 C 0.8493(8) -0.1014(6) -0.0642(3) 0.0228(15) Uani 1 1 d . . . C12 C 0.7702(8) -0.0744(6) -0.1174(4) 0.0313(18) Uani 1 1 d . . . H12 H 0.6736 -0.0708 -0.1182 0.038 Uiso 1 1 calc R . . C13 C 0.8319(9) -0.0528(7) -0.1695(4) 0.0349(19) Uani 1 1 d . . . H13 H 0.7773 -0.0341 -0.2047 0.042 Uiso 1 1 calc R . . C14 C 0.9771(9) -0.0595(7) -0.1684(4) 0.0318(18) Uani 1 1 d . . . H14 H 1.0204 -0.0449 -0.2028 0.038 Uiso 1 1 calc R . . C15 C 1.0568(8) -0.0886(6) -0.1146(4) 0.0301(17) Uani 1 1 d . . . H15 H 1.1532 -0.0954 -0.1138 0.036 Uiso 1 1 calc R . . C16 C 0.9929(8) -0.1073(6) -0.0627(3) 0.0281(17) Uani 1 1 d . . . H16 H 1.0467 -0.1237 -0.0269 0.034 Uiso 1 1 calc R . . C21 C 0.5447(8) 0.2244(6) -0.0747(3) 0.0252(16) Uani 1 1 d . . . C22 C 0.6456(9) 0.1796(7) -0.1068(4) 0.0347(19) Uani 1 1 d . . . H22 H 0.7146 0.1392 -0.0870 0.042 Uiso 1 1 calc R . . C23 C 0.6415(10) 0.1963(7) -0.1686(4) 0.039(2) Uani 1 1 d . . . H23 H 0.7098 0.1683 -0.1900 0.047 Uiso 1 1 calc R . . C24 C 0.5398(11) 0.2524(7) -0.1980(4) 0.041(2) Uani 1 1 d . . . H24 H 0.5367 0.2604 -0.2397 0.049 Uiso 1 1 calc R . . C25 C 0.4407(9) 0.2979(7) -0.1672(4) 0.0352(19) Uani 1 1 d . . . H25 H 0.3724 0.3380 -0.1878 0.042 Uiso 1 1 calc R . . C26 C 0.4434(9) 0.2836(7) -0.1047(4) 0.0318(18) Uani 1 1 d . . . H26 H 0.3767 0.3142 -0.0835 0.038 Uiso 1 1 calc R . . C31 C 0.8707(8) -0.1922(6) 0.0558(3) 0.0266(16) Uani 1 1 d . . . C32 C 0.9509(9) -0.2731(7) 0.0381(4) 0.0349(19) Uani 1 1 d . . . H32 H 0.9545 -0.2869 -0.0027 0.042 Uiso 1 1 calc R . . C33 C 1.0244(10) -0.3320(8) 0.0819(5) 0.045(2) Uani 1 1 d . . . H33 H 1.0799 -0.3845 0.0710 0.053 Uiso 1 1 calc R . . C34 C 1.0129(11) -0.3099(9) 0.1448(5) 0.056(3) Uani 1 1 d . . . H34 H 1.0594 -0.3497 0.1748 0.067 Uiso 1 1 calc R . . C35 C 0.9345(10) -0.2314(9) 0.1604(4) 0.046(2) Uani 1 1 d . . . H35 H 0.9289 -0.2177 0.2011 0.056 Uiso 1 1 calc R . . C36 C 0.8629(9) -0.1716(7) 0.1170(4) 0.036(2) Uani 1 1 d . . . H36 H 0.8100 -0.1180 0.1283 0.043 Uiso 1 1 calc R . . C41 C 0.6451(7) 0.3017(6) 0.0451(3) 0.0232(15) Uani 1 1 d . . . C42 C 0.6675(9) 0.3937(6) 0.0167(4) 0.0314(18) Uani 1 1 d . . . H42 H 0.6385 0.4023 -0.0242 0.038 Uiso 1 1 calc R . . C43 C 0.7324(10) 0.4707(6) 0.0498(4) 0.036(2) Uani 1 1 d . . . H43 H 0.7483 0.5311 0.0309 0.043 Uiso 1 1 calc R . . C44 C 0.7748(9) 0.4591(7) 0.1116(4) 0.0342(19) Uani 1 1 d . . . H44 H 0.8180 0.5115 0.1338 0.041 Uiso 1 1 calc R . . C45 C 0.7519(8) 0.3689(7) 0.1392(4) 0.0301(18) Uani 1 1 d . . . H45 H 0.7795 0.3609 0.1803 0.036 Uiso 1 1 calc R . . C46 C 0.6881(8) 0.2903(6) 0.1064(4) 0.0277(17) Uani 1 1 d . . . H46 H 0.6741 0.2298 0.1254 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0309(4) 0.0307(4) 0.0267(4) -0.0039(2) 0.0035(2) -0.0011(2) P2 0.0219(9) 0.0310(10) 0.0177(9) -0.0048(7) 0.0062(7) -0.0044(8) P3 0.0241(10) 0.0303(10) 0.0210(9) -0.0071(8) 0.0062(7) -0.0050(8) Cl1 0.0263(9) 0.0365(10) 0.0152(8) 0.0026(7) 0.0043(7) -0.0012(7) O1 0.036(3) 0.069(5) 0.013(3) -0.004(3) 0.002(2) -0.003(3) O2 0.065(5) 0.056(4) 0.044(4) 0.017(3) 0.016(3) 0.023(4) O3 0.059(4) 0.050(4) 0.035(3) -0.004(3) 0.003(3) -0.023(3) O4 0.037(3) 0.070(5) 0.030(3) -0.008(3) 0.016(3) -0.012(3) N1 0.022(3) 0.033(4) 0.022(3) -0.003(3) 0.004(3) 0.000(3) C1 0.021(4) 0.034(4) 0.016(3) -0.005(3) 0.002(3) -0.006(3) C2 0.018(3) 0.034(4) 0.020(3) 0.002(3) 0.001(3) -0.006(3) C4 0.031(4) 0.035(4) 0.018(4) -0.005(3) 0.008(3) -0.001(3) C5 0.057(6) 0.044(5) 0.028(4) -0.015(4) 0.007(4) -0.013(5) C6 0.047(5) 0.054(6) 0.020(4) 0.000(4) 0.005(4) 0.016(4) C7 0.029(4) 0.054(6) 0.028(4) -0.005(4) 0.008(3) 0.003(4) C11 0.026(4) 0.022(4) 0.022(3) -0.008(3) 0.010(3) -0.004(3) C12 0.017(4) 0.036(5) 0.042(5) 0.006(4) 0.007(3) 0.004(3) C13 0.031(4) 0.048(5) 0.026(4) 0.011(4) 0.004(3) 0.001(4) C14 0.029(4) 0.041(5) 0.027(4) 0.002(4) 0.006(3) -0.010(4) C15 0.020(4) 0.034(4) 0.037(4) -0.001(4) 0.005(3) -0.004(3) C16 0.027(4) 0.036(4) 0.021(4) -0.005(3) 0.001(3) -0.010(3) C21 0.026(4) 0.028(4) 0.022(4) -0.008(3) 0.006(3) -0.011(3) C22 0.040(5) 0.036(5) 0.030(4) -0.006(4) 0.014(4) -0.001(4) C23 0.049(5) 0.043(5) 0.029(4) -0.001(4) 0.019(4) -0.001(4) C24 0.063(6) 0.042(5) 0.020(4) -0.005(4) 0.011(4) -0.018(5) C25 0.037(5) 0.043(5) 0.026(4) 0.003(4) 0.003(3) -0.009(4) C26 0.029(4) 0.039(5) 0.028(4) -0.001(4) 0.006(3) -0.005(4) C31 0.022(4) 0.033(4) 0.024(4) 0.006(3) -0.002(3) -0.004(3) C32 0.030(4) 0.041(5) 0.032(4) 0.002(4) -0.005(3) -0.008(4) C33 0.035(5) 0.044(5) 0.052(6) 0.014(5) -0.007(4) -0.007(4) C34 0.042(6) 0.073(8) 0.049(6) 0.037(6) -0.018(5) -0.025(6) C35 0.040(5) 0.066(7) 0.033(5) 0.005(5) 0.001(4) -0.023(5) C36 0.035(5) 0.046(5) 0.026(4) 0.003(4) 0.000(3) -0.016(4) C41 0.019(4) 0.033(4) 0.019(3) -0.002(3) 0.009(3) -0.002(3) C42 0.039(5) 0.033(4) 0.022(4) 0.005(3) 0.003(3) -0.006(4) C43 0.043(5) 0.034(5) 0.028(4) 0.002(3) -0.003(4) -0.013(4) C44 0.031(4) 0.039(5) 0.033(4) -0.015(4) 0.003(4) -0.006(4) C45 0.025(4) 0.041(5) 0.022(4) -0.005(3) -0.003(3) -0.004(3) C46 0.028(4) 0.028(4) 0.027(4) 0.000(3) 0.004(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P3 2.440(2) . ? Ag1 P2 2.447(2) . ? Ag1 O1 2.559(5) . ? Ag1 Ag1 3.0170(11) 3_655 ? P2 C1 1.803(7) 3_655 ? P2 C41 1.813(8) . ? P2 C21 1.821(8) . ? P3 C1 1.806(7) . ? P3 C31 1.808(8) . ? P3 C11 1.824(7) . ? Cl1 O2 1.411(7) . ? Cl1 O3 1.425(7) . ? Cl1 O4 1.429(6) . ? Cl1 O1 1.460(6) . ? N1 C2 1.195(10) . ? N1 C4 1.503(9) . ? C1 C2 1.328(11) . ? C1 P2 1.803(7) 3_655 ? C4 C6 1.499(12) . ? C4 C7 1.501(11) . ? C4 C5 1.515(12) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C11 C12 1.385(11) . ? C11 C16 1.382(11) . ? C12 C13 1.387(12) . ? C12 H12 0.9300 . ? C13 C14 1.399(12) . ? C13 H13 0.9300 . ? C14 C15 1.407(12) . ? C14 H14 0.9300 . ? C15 C16 1.386(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.374(12) . ? C21 C22 1.399(11) . ? C22 C23 1.388(12) . ? C22 H22 0.9300 . ? C23 C24 1.347(14) . ? C23 H23 0.9300 . ? C24 C25 1.373(13) . ? C24 H24 0.9300 . ? C25 C26 1.402(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.398(11) . ? C31 C32 1.409(12) . ? C32 C33 1.388(12) . ? C32 H32 0.9300 . ? C33 C34 1.446(16) . ? C33 H33 0.9300 . ? C34 C35 1.360(17) . ? C34 H34 0.9300 . ? C35 C36 1.381(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.391(11) . ? C41 C42 1.410(11) . ? C42 C43 1.378(12) . ? C42 H42 0.9300 . ? C43 C44 1.399(12) . ? C43 H43 0.9300 . ? C44 C45 1.383(12) . ? C44 H44 0.9300 . ? C45 C46 1.386(11) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? 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 P3 Ag1 P2 151.25(7) . . ? P3 Ag1 O1 115.67(16) . . ? P2 Ag1 O1 93.06(16) . . ? P3 Ag1 Ag1 93.95(5) . 3_655 ? P2 Ag1 Ag1 82.60(5) . 3_655 ? O1 Ag1 Ag1 97.60(14) . 3_655 ? C1 P2 C41 102.7(3) 3_655 . ? C1 P2 C21 105.2(3) 3_655 . ? C41 P2 C21 107.2(3) . . ? C1 P2 Ag1 112.2(3) 3_655 . ? C41 P2 Ag1 117.2(3) . . ? C21 P2 Ag1 111.5(3) . . ? C1 P3 C31 103.9(4) . . ? C1 P3 C11 104.2(3) . . ? C31 P3 C11 107.0(4) . . ? C1 P3 Ag1 109.7(3) . . ? C31 P3 Ag1 120.9(3) . . ? C11 P3 Ag1 109.8(3) . . ? O2 Cl1 O3 109.6(5) . . ? O2 Cl1 O4 110.6(4) . . ? O3 Cl1 O4 110.4(4) . . ? O2 Cl1 O1 109.0(4) . . ? O3 Cl1 O1 108.2(4) . . ? O4 Cl1 O1 109.0(4) . . ? Cl1 O1 Ag1 151.6(4) . . ? C2 N1 C4 133.0(7) . . ? C2 C1 P2 121.3(6) . 3_655 ? C2 C1 P3 119.5(6) . . ? P2 C1 P3 119.2(4) 3_655 . ? N1 C2 C1 174.4(8) . . ? C6 C4 N1 111.0(6) . . ? C6 C4 C7 111.5(7) . . ? N1 C4 C7 105.3(6) . . ? C6 C4 C5 111.4(8) . . ? N1 C4 C5 105.3(6) . . ? C7 C4 C5 112.0(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C11 C16 119.6(7) . . ? C12 C11 P3 116.7(6) . . ? C16 C11 P3 123.7(6) . . ? C11 C12 C13 121.5(7) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 119.1(8) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.2(7) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.0(7) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C26 C21 C22 119.6(7) . . ? C26 C21 P2 123.0(6) . . ? C22 C21 P2 117.3(6) . . ? C23 C22 C21 119.1(9) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 120.9(9) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.8(8) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C26 119.5(9) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 119.9(8) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C36 C31 C32 120.7(8) . . ? C36 C31 P3 117.4(7) . . ? C32 C31 P3 121.3(6) . . ? C33 C32 C31 119.7(9) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 118.5(10) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C35 C34 C33 120.4(9) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 121.2(9) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C31 119.5(9) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C46 C41 C42 119.4(7) . . ? C46 C41 P2 117.8(6) . . ? C42 C41 P2 122.7(6) . . ? C43 C42 C41 119.7(7) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.7(8) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 119.4(7) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C44 120.6(7) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C41 120.2(8) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 7.766 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.192 #=====END data_5b _database_code_depnum_ccdc_archive 'CCDC 720843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C96 H75 Ag3 I2 N3 P6, Cl O4, C6 H14' _chemical_formula_sum 'C102 H89 Ag3 Cl I2 N3 O4 P6' _chemical_formula_weight 2219.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 12.8216(5) _cell_length_b 19.2320(7) _cell_length_c 20.9922(8) _cell_angle_alpha 110.960(2) _cell_angle_beta 104.228(2) _cell_angle_gamma 92.629(3) _cell_volume 4634.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1658 _cell_measurement_theta_min 1.767 _cell_measurement_theta_max 70.076 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 11.933 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.3798 _exptl_absorpt_correction_T_max 0.7092 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type kappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27111 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 65.00 _reflns_number_total 15745 _reflns_number_gt 12264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000) ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0969P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15745 _refine_ls_number_parameters 1051 _refine_ls_number_restraints 953 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1537 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.045 0.740 0.118 12.1 -0.4 2 0.500 1.000 0.500 291.6 151.7 3 0.954 0.259 0.882 12.1 1.7 _platon_squeeze_details ; A molecule of hexane crystallize with every molecule of this compound but presented severe disorder and it was not possible to get a chemical sensible model for it, so Squeeze procedure was used to remove their contribution to the structure factors. ; 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 Ag1 Ag 0.70858(4) 0.57657(2) 0.82525(2) 0.04403(14) Uani 1 1 d U . . Ag2 Ag 0.82257(4) 0.57689(2) 0.71218(2) 0.04516(14) Uani 1 1 d U . . Ag3 Ag 0.77334(4) 0.73136(3) 0.81991(2) 0.04496(14) Uani 1 1 d U . . I1 I 0.59704(3) 0.61781(2) 0.70643(2) 0.04464(13) Uani 1 1 d U . . I2 I 0.93695(3) 0.64012(2) 0.86307(2) 0.04894(14) Uani 1 1 d U . . Cl1A Cl 0.3088(12) 0.0778(5) 0.7308(4) 0.077(3) Uani 0.537(18) 1 d PDU A 1 O1A O 0.3951(19) 0.0739(17) 0.7028(16) 0.098(6) Uani 0.537(18) 1 d PDU A 1 O2A O 0.2586(16) 0.1444(10) 0.7281(12) 0.116(6) Uani 0.537(18) 1 d PDU A 1 O3A O 0.2171(13) 0.0195(9) 0.6837(9) 0.111(6) Uani 0.537(18) 1 d PDU A 1 O4A O 0.3313(18) 0.0760(18) 0.7978(12) 0.149(8) Uani 0.537(18) 1 d PDU A 1 Cl1B Cl 0.330(2) 0.0716(12) 0.7285(11) 0.136(7) Uiso 0.463(18) 1 d PDU A 2 O1B O 0.402(3) 0.082(2) 0.688(2) 0.131(9) Uani 0.463(18) 1 d PDU A 2 O2B O 0.232(2) 0.091(2) 0.7025(15) 0.160(12) Uani 0.463(18) 1 d PDU A 2 O3B O 0.380(2) 0.1198(19) 0.8013(12) 0.167(11) Uani 0.463(18) 1 d PDU A 2 O4B O 0.3217(19) -0.0015(12) 0.7281(15) 0.149(9) Uani 0.463(18) 1 d PDU A 2 P1 P 0.79979(12) 0.43758(9) 0.67163(9) 0.0396(3) Uani 1 1 d U . . P2 P 0.70627(13) 0.44024(9) 0.79536(9) 0.0404(3) Uani 1 1 d U . . P3 P 0.61932(13) 0.64080(9) 0.91721(9) 0.0410(4) Uani 1 1 d U . . P4 P 0.69310(14) 0.79717(9) 0.91680(9) 0.0423(4) Uani 1 1 d U . . P5 P 0.84337(13) 0.79709(9) 0.75434(9) 0.0430(4) Uani 1 1 d U B . P6 P 0.88171(13) 0.64733(9) 0.64598(9) 0.0410(4) Uani 1 1 d U B . N2 N 0.8990(5) 0.2949(4) 0.7463(3) 0.0621(15) Uani 1 1 d U . . N4 N 0.4097(5) 0.7637(3) 0.9425(4) 0.0634(15) Uani 1 1 d U . . N6 N 0.7748(8) 0.7901(4) 0.5686(4) 0.094(3) Uani 1 1 d U . . C1 C 0.7908(5) 0.3990(3) 0.7380(4) 0.0425(12) Uani 1 1 d U . . C2 C 0.8410(6) 0.3404(4) 0.7402(4) 0.0483(14) Uani 1 1 d U . . C3 C 0.5923(5) 0.7355(3) 0.9269(3) 0.0433(12) Uani 1 1 d U . . C4 C 0.5014(6) 0.7557(4) 0.9412(4) 0.0483(14) Uani 1 1 d U . . C5 C 0.8373(6) 0.7394(4) 0.6637(4) 0.0492(13) Uani 1 1 d U . . C6 C 0.8137(7) 0.7680(4) 0.6149(4) 0.0601(17) Uani 1 1 d U B . C10 C 0.9126(5) 0.3956(4) 0.6413(4) 0.0479(13) Uani 1 1 d U . . C11 C 0.6831(5) 0.3884(4) 0.5943(4) 0.0495(13) Uani 1 1 d U . . C20 C 0.7578(5) 0.4204(4) 0.8749(4) 0.0479(13) Uani 1 1 d U . . C21 C 0.5744(5) 0.3805(4) 0.7527(3) 0.0438(12) Uani 1 1 d U . . C24 C 0.8805(7) 0.2137(5) 0.7143(5) 0.073(2) Uani 1 1 d U . . C25 C 0.9658(8) 0.1764(5) 0.7093(5) 0.084(2) Uani 1 1 d U . . H25 H 1.0356 0.2035 0.7265 0.101 Uiso 1 1 calc R . . C26 C 0.9523(10) 0.0979(6) 0.6789(6) 0.102(3) Uani 1 1 d U . . H26 H 1.0123 0.0727 0.6765 0.122 Uiso 1 1 calc R . . C27 C 0.8508(11) 0.0593(6) 0.6531(8) 0.130(4) Uani 1 1 d U . . H27 H 0.8413 0.0070 0.6329 0.156 Uiso 1 1 calc R . . C28 C 0.7583(11) 0.0963(7) 0.6559(9) 0.136(4) Uani 1 1 d U . . H28 H 0.6885 0.0693 0.6381 0.163 Uiso 1 1 calc R . . C29 C 0.7756(9) 0.1747(6) 0.6863(7) 0.114(3) Uani 1 1 d U . . H29 H 0.7165 0.2009 0.6878 0.137 Uiso 1 1 calc R . . C30 C 0.6815(6) 0.6502(4) 1.0076(4) 0.0483(13) Uani 1 1 d U . . C31 C 0.4842(5) 0.5878(4) 0.8912(4) 0.0450(12) Uani 1 1 d U . . C40 C 0.7945(6) 0.8398(4) 1.0034(4) 0.0557(14) Uani 1 1 d U . . C41 C 0.6193(6) 0.8725(4) 0.9064(4) 0.0509(13) Uani 1 1 d U . . C44 C 0.3595(7) 0.7841(4) 0.9992(5) 0.0692(17) Uani 1 1 d U . . C45 C 0.4200(9) 0.8121(5) 1.0691(6) 0.082(2) Uani 1 1 d U . . H45 H 0.4953 0.8226 1.0805 0.098 Uiso 1 1 calc R . . C46 C 0.3689(10) 0.8251(6) 1.1237(7) 0.100(2) Uani 1 1 d U . . H46 H 0.4094 0.8432 1.1712 0.120 Uiso 1 1 calc R . . C47 C 0.2580(10) 0.8102(6) 1.1048(8) 0.110(3) Uani 1 1 d U . . H47 H 0.2227 0.8177 1.1399 0.132 Uiso 1 1 calc R . . C48 C 0.1975(9) 0.7841(6) 1.0345(8) 0.108(3) Uani 1 1 d U . . H48 H 0.1219 0.7760 1.0231 0.130 Uiso 1 1 calc R . . C49 C 0.2484(8) 0.7696(5) 0.9795(7) 0.089(2) Uani 1 1 d U . . H49 H 0.2081 0.7510 0.9319 0.106 Uiso 1 1 calc R . . C50 C 0.9808(6) 0.8468(4) 0.7924(5) 0.0635(16) Uani 1 1 d U . . C51 C 0.7590(7) 0.8686(4) 0.7443(4) 0.0616(16) Uani 1 1 d DU . . C60 C 1.0252(5) 0.6677(4) 0.6561(4) 0.0538(14) Uani 1 1 d U . . C64 C 0.8490(12) 0.8373(8) 0.5459(7) 0.065(3) Uiso 0.467(12) 1 d PGU B 1 C65 C 0.9591(12) 0.8682(8) 0.5764(7) 0.070(4) Uiso 0.467(12) 1 d PGU B 1 H65 H 0.9989 0.8616 0.6168 0.084 Uiso 0.467(12) 1 calc PR B 1 C66 C 1.0084(13) 0.9087(9) 0.5457(8) 0.085(4) Uiso 0.467(12) 1 d PGU B 1 H66 H 1.0816 0.9291 0.5654 0.102 Uiso 0.467(12) 1 calc PR B 1 C67 C 0.9480(14) 0.9186(9) 0.4855(8) 0.091(4) Uiso 0.467(12) 1 d PGU B 1 H67 H 0.9807 0.9463 0.4654 0.110 Uiso 0.467(12) 1 calc PR B 1 C68 C 0.8377(14) 0.8869(9) 0.4551(8) 0.089(4) Uiso 0.467(12) 1 d PGU B 1 H68 H 0.7978 0.8932 0.4146 0.106 Uiso 0.467(12) 1 calc PR B 1 C69 C 0.7883(13) 0.8465(8) 0.4854(7) 0.081(4) Uiso 0.467(12) 1 d PGU B 1 H69 H 0.7153 0.8257 0.4655 0.097 Uiso 0.467(12) 1 calc PR B 1 C64' C 0.7988(11) 0.8317(7) 0.5357(6) 0.064(3) Uiso 0.533(12) 1 d PGU B 2 C65' C 0.9095(10) 0.8545(7) 0.5533(7) 0.073(3) Uiso 0.533(12) 1 d PGU B 2 H65' H 0.9569 0.8417 0.5873 0.088 Uiso 0.533(12) 1 calc PR B 2 C66' C 0.9506(11) 0.8963(8) 0.5204(7) 0.086(4) Uiso 0.533(12) 1 d PGU B 2 H66' H 1.0252 0.9117 0.5328 0.103 Uiso 0.533(12) 1 calc PR B 2 C67' C 0.8805(11) 0.9152(8) 0.4690(7) 0.086(4) Uiso 0.533(12) 1 d PGU B 2 H67' H 0.9081 0.9426 0.4466 0.103 Uiso 0.533(12) 1 calc PR B 2 C68' C 0.7699(12) 0.8932(7) 0.4514(7) 0.086(4) Uiso 0.533(12) 1 d PGU B 2 H68' H 0.7227 0.9061 0.4174 0.104 Uiso 0.533(12) 1 calc PR B 2 C69' C 0.7289(11) 0.8513(7) 0.4846(6) 0.079(4) Uiso 0.533(12) 1 d PGU B 2 H69' H 0.6544 0.8364 0.4726 0.095 Uiso 0.533(12) 1 calc PR B 2 C101 C 0.9010(6) 0.3255(4) 0.5909(4) 0.0635(18) Uani 1 1 d U . . H101 H 0.8318 0.2976 0.5691 0.076 Uiso 1 1 calc R . . C102 C 0.9878(7) 0.2942(5) 0.5711(5) 0.074(2) Uani 1 1 d U . . H102 H 0.9772 0.2457 0.5370 0.089 Uiso 1 1 calc R . . C103 C 1.0882(7) 0.3341(6) 0.6012(5) 0.094(3) Uani 1 1 d U . . H103 H 1.1481 0.3125 0.5900 0.113 Uiso 1 1 calc R . . C104 C 1.1016(7) 0.4087(6) 0.6497(6) 0.105(3) Uani 1 1 d U . . H104 H 1.1699 0.4380 0.6688 0.126 Uiso 1 1 calc R . . C105 C 1.0155(6) 0.4374(5) 0.6684(5) 0.086(3) Uani 1 1 d U . . H105 H 1.0251 0.4868 0.7006 0.104 Uiso 1 1 calc R . . C111 C 0.6239(6) 0.3218(4) 0.5845(4) 0.0611(17) Uani 1 1 d U . . H111 H 0.6387 0.3018 0.6195 0.073 Uiso 1 1 calc R . . C112 C 0.5420(7) 0.2851(5) 0.5217(5) 0.078(2) Uani 1 1 d U . . H112 H 0.5008 0.2405 0.5146 0.094 Uiso 1 1 calc R . . C113 C 0.5217(7) 0.3151(6) 0.4695(5) 0.082(2) Uani 1 1 d U . . H113 H 0.4691 0.2892 0.4266 0.098 Uiso 1 1 calc R . . C114 C 0.5773(7) 0.3811(6) 0.4803(5) 0.086(2) Uani 1 1 d U . . H114 H 0.5618 0.4015 0.4456 0.103 Uiso 1 1 calc R . . C115 C 0.6580(7) 0.4188(5) 0.5434(4) 0.0711(19) Uani 1 1 d U . . H115 H 0.6954 0.4650 0.5513 0.085 Uiso 1 1 calc R . . C201 C 0.8680(6) 0.4297(5) 0.9069(4) 0.0601(16) Uani 1 1 d U . . H201 H 0.9175 0.4424 0.8856 0.072 Uiso 1 1 calc R . . C202 C 0.9052(7) 0.4202(5) 0.9708(4) 0.0681(18) Uani 1 1 d U . . H202 H 0.9796 0.4258 0.9917 0.082 Uiso 1 1 calc R . . C203 C 0.8328(7) 0.4026(5) 1.0033(5) 0.0727(19) Uani 1 1 d U . . H203 H 0.8579 0.3960 1.0459 0.087 Uiso 1 1 calc R . . C204 C 0.7243(7) 0.3948(5) 0.9725(5) 0.0717(18) Uani 1 1 d U . . H204 H 0.6751 0.3832 0.9945 0.086 Uiso 1 1 calc R . . C205 C 0.6866(6) 0.4039(4) 0.9092(4) 0.0594(16) Uani 1 1 d U . . H205 H 0.6121 0.3989 0.8891 0.071 Uiso 1 1 calc R . . C211 C 0.4863(6) 0.4108(4) 0.7263(4) 0.0575(16) Uani 1 1 d U . . H211 H 0.4936 0.4610 0.7315 0.069 Uiso 1 1 calc R . . C212 C 0.3878(6) 0.3652(5) 0.6922(5) 0.077(2) Uani 1 1 d U . . H212 H 0.3292 0.3844 0.6717 0.093 Uiso 1 1 calc R . . C213 C 0.3729(7) 0.2920(5) 0.6873(5) 0.075(2) Uani 1 1 d U . . H213 H 0.3041 0.2634 0.6665 0.090 Uiso 1 1 calc R . . C214 C 0.4596(7) 0.2616(5) 0.7130(5) 0.0697(19) Uani 1 1 d U . . H214 H 0.4508 0.2120 0.7096 0.084 Uiso 1 1 calc R . . C215 C 0.5610(6) 0.3057(4) 0.7443(4) 0.0638(18) Uani 1 1 d U . . H215 H 0.6210 0.2846 0.7599 0.077 Uiso 1 1 calc R . . C301 C 0.6321(8) 0.6825(5) 1.0614(4) 0.0691(17) Uani 1 1 d U . . H301 H 0.5626 0.6948 1.0495 0.083 Uiso 1 1 calc R . . C302 C 0.6837(9) 0.6967(5) 1.1321(5) 0.083(2) Uani 1 1 d U . . H302 H 0.6487 0.7167 1.1671 0.100 Uiso 1 1 calc R . . C303 C 0.7885(9) 0.6804(6) 1.1493(5) 0.087(2) Uani 1 1 d U . . H303 H 0.8260 0.6918 1.1966 0.104 Uiso 1 1 calc R . . C304 C 0.8370(8) 0.6478(6) 1.0971(5) 0.082(2) Uani 1 1 d U . . H304 H 0.9062 0.6351 1.1091 0.099 Uiso 1 1 calc R . . C305 C 0.7853(6) 0.6333(5) 1.0267(4) 0.0647(17) Uani 1 1 d U . . H305 H 0.8205 0.6121 0.9921 0.078 Uiso 1 1 calc R . . C311 C 0.4032(6) 0.5939(4) 0.8373(4) 0.0546(15) Uani 1 1 d U . . H311 H 0.4170 0.6270 0.8161 0.065 Uiso 1 1 calc R . . C312 C 0.3015(6) 0.5514(5) 0.8144(5) 0.0651(17) Uani 1 1 d U . . H312 H 0.2463 0.5574 0.7796 0.078 Uiso 1 1 calc R . . C313 C 0.2828(7) 0.5003(5) 0.8434(5) 0.075(2) Uani 1 1 d U . . H313 H 0.2145 0.4716 0.8284 0.090 Uiso 1 1 calc R . . C314 C 0.3640(7) 0.4916(5) 0.8942(5) 0.076(2) Uani 1 1 d U . . H314 H 0.3521 0.4554 0.9125 0.091 Uiso 1 1 calc R . . C315 C 0.4642(6) 0.5361(4) 0.9188(5) 0.0604(17) Uani 1 1 d U . . H315 H 0.5186 0.5308 0.9545 0.073 Uiso 1 1 calc R . . C401 C 0.7798(9) 0.8441(5) 1.0654(4) 0.087(2) Uani 1 1 d U . . H401 H 0.7117 0.8274 1.0673 0.105 Uiso 1 1 calc R . . C402 C 0.8692(10) 0.8745(6) 1.1298(5) 0.103(3) Uani 1 1 d U . . H402 H 0.8596 0.8762 1.1728 0.123 Uiso 1 1 calc R . . C403 C 0.9619(10) 0.8990(7) 1.1267(6) 0.107(3) Uani 1 1 d U . . H403 H 1.0190 0.9168 1.1683 0.128 Uiso 1 1 calc R . . C404 C 0.9826(9) 0.9008(7) 1.0660(6) 0.107(3) Uani 1 1 d U . . H404 H 1.0496 0.9221 1.0667 0.129 Uiso 1 1 calc R . . C405 C 0.8970(7) 0.8685(6) 1.0029(5) 0.092(2) Uani 1 1 d U . . H405 H 0.9084 0.8662 0.9601 0.111 Uiso 1 1 calc R . . C411 C 0.6444(9) 0.9451(5) 0.9554(6) 0.099(3) Uani 1 1 d U . . H411 H 0.7022 0.9577 0.9962 0.119 Uiso 1 1 calc R . . C412 C 0.5849(10) 0.9994(6) 0.9446(7) 0.119(3) Uani 1 1 d U . . H412 H 0.6004 1.0480 0.9792 0.143 Uiso 1 1 calc R . . C413 C 0.5019(8) 0.9823(6) 0.8826(6) 0.095(3) Uani 1 1 d U . . H413 H 0.4647 1.0199 0.8739 0.114 Uiso 1 1 calc R . . C414 C 0.4757(8) 0.9116(5) 0.8355(5) 0.078(2) Uani 1 1 d U . . H414 H 0.4182 0.8996 0.7946 0.094 Uiso 1 1 calc R . . C415 C 0.5328(7) 0.8564(5) 0.8467(5) 0.075(2) Uani 1 1 d U . . H415 H 0.5128 0.8072 0.8134 0.090 Uiso 1 1 calc R . . C501 C 1.0424(7) 0.8504(5) 0.8550(6) 0.084(2) Uani 1 1 d U B . H501 H 1.0141 0.8262 0.8797 0.101 Uiso 1 1 calc R . . C502 C 1.1492(8) 0.8899(7) 0.8848(7) 0.110(3) Uani 1 1 d U . . H502 H 1.1906 0.8919 0.9287 0.133 Uiso 1 1 calc R B . C503 C 1.1901(9) 0.9241(7) 0.8499(8) 0.114(3) Uani 1 1 d U B . H503 H 1.2609 0.9497 0.8694 0.137 Uiso 1 1 calc R . . C504 C 1.1310(9) 0.9225(7) 0.7866(7) 0.119(3) Uani 1 1 d U . . H504 H 1.1608 0.9475 0.7632 0.143 Uiso 1 1 calc R B . C505 C 1.0253(8) 0.8834(6) 0.7560(6) 0.101(3) Uani 1 1 d U B . H505 H 0.9848 0.8817 0.7120 0.121 Uiso 1 1 calc R . . C511 C 0.7923(10) 0.9414(6) 0.7777(7) 0.134(4) Uani 1 1 d DU B . H511 H 0.8635 0.9585 0.8065 0.161 Uiso 1 1 calc R . . C512 C 0.7218(12) 0.9938(7) 0.7705(8) 0.161(4) Uani 1 1 d DU . . H512 H 0.7476 1.0449 0.7953 0.193 Uiso 1 1 calc R B . C513 C 0.6211(11) 0.9733(7) 0.7302(8) 0.130(4) Uani 1 1 d DU B . H513 H 0.5759 1.0088 0.7256 0.156 Uiso 1 1 calc R . . C514 C 0.5875(10) 0.9029(7) 0.6974(7) 0.115(3) Uani 1 1 d DU . . H514 H 0.5170 0.8867 0.6673 0.137 Uiso 1 1 calc R B . C515 C 0.6552(8) 0.8485(6) 0.7057(6) 0.099(3) Uani 1 1 d DU B . H515 H 0.6265 0.7976 0.6838 0.118 Uiso 1 1 calc R . . C601 C 1.1007(6) 0.6707(4) 0.7182(4) 0.0626(17) Uani 1 1 d U B . H601 H 1.0773 0.6583 0.7518 0.075 Uiso 1 1 calc R . . C602 C 1.2112(6) 0.6925(6) 0.7296(5) 0.080(2) Uani 1 1 d U . . H602 H 1.2614 0.6925 0.7700 0.096 Uiso 1 1 calc R B . C603 C 1.2464(8) 0.7139(7) 0.6818(6) 0.098(2) Uani 1 1 d U B . H603 H 1.3195 0.7317 0.6913 0.118 Uiso 1 1 calc R . . C604 C 1.1738(7) 0.7089(7) 0.6206(6) 0.094(2) Uani 1 1 d U . . H604 H 1.1992 0.7201 0.5869 0.112 Uiso 1 1 calc R B . C605 C 1.0646(7) 0.6881(6) 0.6069(5) 0.076(2) Uani 1 1 d U B . H605 H 1.0165 0.6873 0.5654 0.091 Uiso 1 1 calc R . . C61 C 0.8201(5) 0.5945(4) 0.5510(4) 0.0477(13) Uani 1 1 d U . . C612 C 0.6607(6) 0.5525(5) 0.4498(4) 0.0646(18) Uani 1 1 d U . . H612 H 0.5895 0.5568 0.4293 0.077 Uiso 1 1 calc R B . C613 C 0.7114(7) 0.5007(6) 0.4127(5) 0.082(2) Uani 1 1 d U B . H613 H 0.6761 0.4698 0.3658 0.099 Uiso 1 1 calc R . . C614 C 0.8158(8) 0.4926(6) 0.4434(5) 0.104(3) Uani 1 1 d U . . H614 H 0.8499 0.4550 0.4181 0.125 Uiso 1 1 calc R B . C615 C 0.8696(7) 0.5407(6) 0.5124(5) 0.085(3) Uani 1 1 d U B . H615 H 0.9408 0.5360 0.5326 0.102 Uiso 1 1 calc R . . C611 C 0.7138(6) 0.5996(4) 0.5185(4) 0.0552(15) Uani 1 1 d U B . H611 H 0.6778 0.6357 0.5439 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0502(3) 0.0384(2) 0.0472(3) 0.0158(2) 0.0198(2) 0.0114(2) Ag2 0.0531(3) 0.0391(3) 0.0458(3) 0.0168(2) 0.0170(2) 0.0080(2) Ag3 0.0493(3) 0.0437(3) 0.0431(3) 0.0146(2) 0.0184(2) 0.0049(2) I1 0.0406(2) 0.0463(2) 0.0428(2) 0.01679(18) 0.00476(17) 0.00598(17) I2 0.0403(2) 0.0577(3) 0.0454(2) 0.0203(2) 0.00543(18) 0.00575(19) Cl1A 0.116(7) 0.062(3) 0.056(3) 0.020(2) 0.036(3) -0.007(3) O1A 0.090(8) 0.099(12) 0.143(16) 0.083(12) 0.047(9) 0.003(6) O2A 0.135(13) 0.086(7) 0.140(16) 0.048(10) 0.053(11) 0.019(8) O3A 0.096(9) 0.095(8) 0.126(11) 0.029(9) 0.028(7) -0.024(7) O4A 0.127(15) 0.24(2) 0.107(9) 0.117(14) 0.018(9) -0.008(13) O1B 0.196(19) 0.108(17) 0.153(17) 0.088(14) 0.103(18) 0.035(15) O2B 0.141(15) 0.21(3) 0.124(18) 0.07(2) 0.011(12) 0.08(2) O3B 0.15(2) 0.21(2) 0.080(11) 0.001(15) 0.006(11) 0.017(19) O4B 0.164(19) 0.124(14) 0.21(2) 0.116(14) 0.071(17) 0.007(12) P1 0.0385(8) 0.0358(8) 0.0432(8) 0.0129(6) 0.0123(7) 0.0068(6) P2 0.0432(9) 0.0368(8) 0.0447(9) 0.0171(7) 0.0153(7) 0.0094(6) P3 0.0474(9) 0.0371(8) 0.0416(8) 0.0148(7) 0.0178(7) 0.0084(7) P4 0.0491(9) 0.0374(8) 0.0417(8) 0.0140(7) 0.0165(7) 0.0072(7) P5 0.0477(9) 0.0390(8) 0.0436(9) 0.0142(7) 0.0179(7) 0.0048(7) P6 0.0442(9) 0.0401(8) 0.0413(8) 0.0147(7) 0.0172(7) 0.0080(7) N2 0.076(4) 0.058(3) 0.064(4) 0.030(3) 0.025(3) 0.028(3) N4 0.060(3) 0.052(3) 0.095(4) 0.033(3) 0.040(3) 0.019(3) N6 0.179(8) 0.050(4) 0.062(4) 0.030(3) 0.033(5) 0.029(5) C1 0.044(3) 0.039(3) 0.051(3) 0.017(2) 0.022(2) 0.009(2) C2 0.055(4) 0.047(3) 0.052(4) 0.022(3) 0.025(3) 0.015(3) C3 0.051(3) 0.038(2) 0.045(3) 0.016(2) 0.020(2) 0.013(2) C4 0.053(3) 0.039(3) 0.058(4) 0.019(3) 0.022(3) 0.010(3) C5 0.062(4) 0.044(3) 0.048(3) 0.019(2) 0.024(3) 0.010(3) C6 0.086(5) 0.047(3) 0.051(3) 0.020(3) 0.024(4) 0.011(3) C10 0.042(2) 0.052(3) 0.049(3) 0.012(3) 0.019(2) 0.011(2) C11 0.043(3) 0.048(3) 0.052(3) 0.013(2) 0.013(2) 0.011(2) C20 0.051(3) 0.047(3) 0.050(3) 0.021(3) 0.017(2) 0.017(3) C21 0.044(2) 0.045(3) 0.046(3) 0.017(3) 0.019(2) 0.008(2) C24 0.079(4) 0.054(3) 0.090(5) 0.029(4) 0.024(4) 0.027(3) C25 0.091(4) 0.061(3) 0.087(5) 0.016(4) 0.016(4) 0.034(3) C26 0.115(5) 0.064(4) 0.108(6) 0.015(4) 0.019(5) 0.043(4) C27 0.133(6) 0.061(4) 0.159(7) 0.015(5) 0.014(7) 0.024(4) C28 0.110(5) 0.071(4) 0.186(8) 0.014(6) 0.024(6) 0.005(4) C29 0.090(4) 0.069(4) 0.157(7) 0.020(5) 0.024(5) 0.020(3) C30 0.058(3) 0.047(3) 0.045(2) 0.021(2) 0.017(2) 0.005(3) C31 0.047(3) 0.041(3) 0.050(3) 0.017(2) 0.019(2) 0.007(2) C40 0.072(3) 0.039(3) 0.046(2) 0.008(2) 0.012(2) 0.003(3) C41 0.061(4) 0.044(3) 0.059(3) 0.025(3) 0.028(2) 0.011(2) C44 0.070(4) 0.046(4) 0.113(4) 0.033(4) 0.057(3) 0.022(3) C45 0.094(4) 0.052(4) 0.108(4) 0.019(4) 0.060(3) 0.025(4) C46 0.116(5) 0.069(5) 0.117(5) 0.013(5) 0.071(4) 0.022(5) C47 0.114(5) 0.069(5) 0.149(5) 0.011(5) 0.089(5) 0.015(5) C48 0.087(5) 0.076(5) 0.161(6) 0.015(5) 0.080(4) 0.010(4) C49 0.073(4) 0.062(4) 0.142(5) 0.030(4) 0.062(4) 0.022(4) C50 0.054(3) 0.051(4) 0.081(4) 0.020(3) 0.020(3) -0.004(3) C51 0.072(3) 0.056(3) 0.071(4) 0.032(3) 0.031(3) 0.023(3) C60 0.042(2) 0.061(4) 0.061(4) 0.025(3) 0.018(2) 0.006(3) C101 0.050(3) 0.055(3) 0.070(4) 0.003(3) 0.023(3) 0.008(3) C102 0.062(4) 0.072(4) 0.071(4) 0.000(3) 0.031(3) 0.016(3) C103 0.046(3) 0.110(5) 0.089(5) -0.010(4) 0.021(4) 0.024(4) C104 0.038(3) 0.116(5) 0.105(6) -0.022(5) 0.017(4) 0.008(4) C105 0.040(3) 0.086(5) 0.088(5) -0.018(4) 0.015(3) 0.007(3) C111 0.055(4) 0.051(3) 0.066(4) 0.012(3) 0.014(3) 0.001(3) C112 0.058(4) 0.067(4) 0.081(5) 0.005(3) 0.008(3) -0.003(3) C113 0.050(4) 0.086(5) 0.076(4) 0.008(4) -0.007(4) 0.006(3) C114 0.069(4) 0.097(5) 0.070(4) 0.029(4) -0.012(4) 0.004(4) C115 0.064(4) 0.076(4) 0.061(4) 0.028(3) -0.005(3) -0.001(3) C201 0.052(3) 0.073(4) 0.053(3) 0.023(3) 0.012(3) 0.008(3) C202 0.064(4) 0.081(4) 0.059(4) 0.030(3) 0.011(3) 0.023(4) C203 0.077(4) 0.090(5) 0.059(4) 0.039(4) 0.016(3) 0.021(4) C204 0.074(3) 0.090(5) 0.066(4) 0.046(4) 0.021(3) 0.015(4) C205 0.058(3) 0.070(4) 0.061(4) 0.036(3) 0.020(3) 0.014(3) C211 0.046(3) 0.057(3) 0.061(4) 0.020(3) 0.006(3) 0.010(2) C212 0.049(3) 0.079(4) 0.084(5) 0.024(4) -0.001(3) 0.001(3) C213 0.060(4) 0.078(4) 0.072(5) 0.018(4) 0.010(3) -0.011(3) C214 0.066(4) 0.059(4) 0.076(5) 0.019(3) 0.019(4) -0.010(3) C215 0.062(3) 0.047(3) 0.076(4) 0.019(3) 0.014(3) 0.003(3) C301 0.096(4) 0.066(4) 0.050(3) 0.022(3) 0.028(3) 0.018(4) C302 0.122(5) 0.078(5) 0.048(3) 0.020(4) 0.026(4) 0.005(4) C303 0.101(5) 0.093(5) 0.051(4) 0.027(4) 0.001(3) -0.021(4) C304 0.074(4) 0.106(5) 0.061(4) 0.041(4) -0.002(3) -0.012(4) C305 0.056(3) 0.086(5) 0.057(3) 0.038(3) 0.009(3) -0.001(3) C311 0.053(3) 0.049(3) 0.060(4) 0.022(3) 0.012(3) 0.004(3) C312 0.053(3) 0.066(4) 0.070(4) 0.024(3) 0.008(3) 0.009(3) C313 0.059(4) 0.065(4) 0.087(5) 0.025(3) 0.009(3) -0.012(3) C314 0.069(4) 0.065(4) 0.090(5) 0.038(4) 0.006(4) -0.015(3) C315 0.056(3) 0.053(4) 0.074(4) 0.032(3) 0.009(3) 0.000(3) C401 0.113(5) 0.078(5) 0.049(3) 0.013(4) 0.009(3) -0.022(4) C402 0.132(6) 0.098(6) 0.057(4) 0.027(4) -0.003(4) -0.011(5) C403 0.102(5) 0.103(6) 0.081(4) 0.023(5) -0.012(4) 0.004(5) C404 0.076(4) 0.117(6) 0.082(5) -0.003(5) 0.008(4) 0.000(5) C405 0.064(4) 0.105(6) 0.069(4) -0.010(4) 0.017(3) 0.000(4) C411 0.104(5) 0.046(3) 0.115(6) 0.015(3) -0.004(4) 0.020(4) C412 0.121(6) 0.057(4) 0.138(6) 0.015(4) -0.007(5) 0.032(4) C413 0.094(5) 0.066(4) 0.121(6) 0.035(4) 0.020(4) 0.035(4) C414 0.084(5) 0.075(4) 0.082(5) 0.035(3) 0.022(4) 0.030(4) C415 0.085(5) 0.067(4) 0.069(4) 0.024(3) 0.014(3) 0.031(3) C501 0.055(4) 0.083(5) 0.103(5) 0.037(4) 0.002(3) -0.005(3) C502 0.071(4) 0.101(6) 0.130(6) 0.035(5) -0.004(4) -0.016(4) C503 0.061(5) 0.116(6) 0.138(6) 0.021(5) 0.029(4) -0.020(5) C504 0.090(5) 0.126(6) 0.119(6) 0.021(5) 0.041(4) -0.043(5) C505 0.091(5) 0.105(6) 0.094(5) 0.027(4) 0.032(4) -0.040(4) C511 0.120(6) 0.060(3) 0.167(7) 0.009(5) -0.010(6) 0.039(4) C512 0.149(7) 0.070(4) 0.199(8) 0.014(6) -0.011(6) 0.052(5) C513 0.129(6) 0.091(4) 0.158(8) 0.045(6) 0.016(6) 0.063(5) C514 0.100(5) 0.103(5) 0.131(7) 0.042(5) 0.013(5) 0.053(4) C515 0.085(4) 0.084(4) 0.114(6) 0.030(5) 0.013(4) 0.039(3) C601 0.050(3) 0.066(4) 0.071(4) 0.032(3) 0.008(3) 0.004(3) C602 0.043(3) 0.096(5) 0.091(5) 0.036(4) 0.006(3) 0.007(4) C603 0.053(4) 0.127(6) 0.110(6) 0.043(5) 0.023(3) -0.004(4) C604 0.061(4) 0.136(6) 0.095(5) 0.049(5) 0.037(3) -0.004(4) C605 0.056(3) 0.109(5) 0.074(4) 0.043(4) 0.029(3) 0.010(4) C61 0.043(3) 0.056(3) 0.043(2) 0.013(2) 0.019(2) 0.007(3) C612 0.057(4) 0.077(4) 0.052(3) 0.020(3) 0.007(3) 0.009(3) C613 0.079(4) 0.092(5) 0.049(4) 0.003(3) 0.006(3) 0.015(4) C614 0.076(4) 0.110(6) 0.071(4) -0.024(4) 0.010(4) 0.028(4) C615 0.057(4) 0.096(5) 0.063(4) -0.015(4) 0.015(3) 0.026(3) C611 0.047(3) 0.061(4) 0.054(3) 0.017(3) 0.014(2) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P3 2.4640(17) . ? Ag1 P2 2.4649(16) . ? Ag1 I2 2.9210(6) . ? Ag1 I1 2.9431(6) . ? Ag1 Ag2 3.0797(7) . ? Ag1 Ag3 3.1019(6) . ? Ag2 P6 2.4724(16) . ? Ag2 P1 2.4824(16) . ? Ag2 I2 2.9085(6) . ? Ag2 I1 3.0167(6) . ? Ag2 Ag3 3.2259(7) . ? Ag3 P5 2.4591(17) . ? Ag3 P4 2.4704(17) . ? Ag3 I1 2.9550(6) . ? Ag3 I2 2.9735(6) . ? Cl1A O1A 1.37(3) . ? Cl1A O4A 1.377(18) . ? Cl1A O3A 1.460(17) . ? Cl1A O2A 1.47(2) . ? Cl1B O2B 1.37(3) . ? Cl1B O4B 1.40(2) . ? Cl1B O3B 1.43(2) . ? Cl1B O1B 1.45(3) . ? P1 C1 1.821(7) . ? P1 C10 1.828(7) . ? P1 C11 1.829(7) . ? P2 C1 1.814(7) . ? P2 C20 1.818(7) . ? P2 C21 1.823(7) . ? P3 C30 1.807(7) . ? P3 C3 1.819(6) . ? P3 C31 1.821(7) . ? P4 C3 1.814(7) . ? P4 C41 1.814(7) . ? P4 C40 1.828(7) . ? P5 C5 1.807(7) . ? P5 C50 1.807(8) . ? P5 C51 1.828(8) . ? P6 C60 1.807(7) . ? P6 C5 1.822(7) . ? P6 C61 1.826(7) . ? N2 C2 1.195(9) . ? N2 C24 1.443(10) . ? N4 C4 1.197(9) . ? N4 C44 1.434(11) . ? N6 C6 1.205(10) . ? N6 C64' 1.300(12) . ? N6 C64 1.552(15) . ? C1 C2 1.332(9) . ? C3 C4 1.316(9) . ? C5 C6 1.307(10) . ? C10 C101 1.358(10) . ? C10 C105 1.384(10) . ? C11 C115 1.371(11) . ? C11 C111 1.380(10) . ? C20 C201 1.379(10) . ? C20 C205 1.383(10) . ? C21 C215 1.382(10) . ? C21 C211 1.381(9) . ? C24 C25 1.341(12) . ? C24 C29 1.385(14) . ? C25 C26 1.396(13) . ? C25 H25 0.9300 . ? C26 C27 1.348(16) . ? C26 H26 0.9300 . ? C27 C28 1.413(17) . ? C27 H27 0.9300 . ? C28 C29 1.393(16) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C305 1.381(10) . ? C30 C301 1.396(11) . ? C31 C315 1.360(10) . ? C31 C311 1.379(10) . ? C40 C401 1.336(11) . ? C40 C405 1.406(12) . ? C41 C411 1.371(12) . ? C41 C415 1.381(11) . ? C44 C49 1.367(12) . ? C44 C45 1.371(14) . ? C45 C46 1.409(13) . ? C45 H45 0.9300 . ? C46 C47 1.365(16) . ? C46 H46 0.9300 . ? C47 C48 1.380(18) . ? C47 H47 0.9300 . ? C48 C49 1.412(15) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C501 1.332(12) . ? C50 C505 1.403(12) . ? C51 C511 1.315(13) . ? C51 C515 1.332(12) . ? C60 C601 1.399(10) . ? C60 C605 1.417(11) . ? C64 C69 1.392(8) . ? C64 C65 1.402(9) . ? C65 C66 1.391(9) . ? C65 H65 0.9300 . ? C66 C67 1.392(8) . ? C66 H66 0.9300 . ? C67 C68 1.407(9) . ? C67 H67 0.9300 . ? C68 C69 1.384(8) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C64' C65' 1.383(7) . ? C64' C69' 1.394(7) . ? C65' C66' 1.393(7) . ? C65' H65' 0.9300 . ? C66' C67' 1.393(7) . ? C66' H66' 0.9300 . ? C67' C68' 1.378(7) . ? C67' H67' 0.9300 . ? C68' C69' 1.399(7) . ? C68' H68' 0.9300 . ? C69' H69' 0.9300 . ? C101 C102 1.372(11) . ? C101 H101 0.9300 . ? C102 C103 1.345(12) . ? C102 H102 0.9300 . ? C103 C104 1.405(14) . ? C103 H103 0.9300 . ? C104 C105 1.339(12) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C111 C112 1.386(11) . ? C111 H111 0.9300 . ? C112 C113 1.390(14) . ? C112 H112 0.9300 . ? C113 C114 1.342(13) . ? C113 H113 0.9300 . ? C114 C115 1.386(11) . ? C114 H114 0.9300 . ? C115 H115 0.9300 . ? C201 C202 1.390(11) . ? C201 H201 0.9300 . ? C202 C203 1.375(12) . ? C202 H202 0.9300 . ? C203 C204 1.358(12) . ? C203 H203 0.9300 . ? C204 C205 1.375(11) . ? C204 H204 0.9300 . ? C205 H205 0.9300 . ? C211 C212 1.372(10) . ? C211 H211 0.9300 . ? C212 C213 1.374(13) . ? C212 H212 0.9300 . ? C213 C214 1.364(12) . ? C213 H213 0.9300 . ? C214 C215 1.386(11) . ? C214 H214 0.9300 . ? C215 H215 0.9300 . ? C301 C302 1.388(12) . ? C301 H301 0.9300 . ? C302 C303 1.384(14) . ? C302 H302 0.9300 . ? C303 C304 1.363(14) . ? C303 H303 0.9300 . ? C304 C305 1.381(11) . ? C304 H304 0.9300 . ? C305 H305 0.9300 . ? C311 C312 1.383(10) . ? C311 H311 0.9300 . ? C312 C313 1.367(12) . ? C312 H312 0.9300 . ? C313 C314 1.360(12) . ? C313 H313 0.9300 . ? C314 C315 1.381(10) . ? C314 H314 0.9300 . ? C315 H315 0.9300 . ? C401 C402 1.447(13) . ? C401 H401 0.9300 . ? C402 C403 1.285(16) . ? C402 H402 0.9300 . ? C403 C404 1.374(16) . ? C403 H403 0.9300 . ? C404 C405 1.408(13) . ? C404 H404 0.9300 . ? C405 H405 0.9300 . ? C411 C412 1.372(13) . ? C411 H411 0.9300 . ? C412 C413 1.385(15) . ? C412 H412 0.9300 . ? C413 C414 1.332(13) . ? C413 H413 0.9300 . ? C414 C415 1.374(12) . ? C414 H414 0.9300 . ? C415 H415 0.9300 . ? C501 C502 1.410(13) . ? C501 H501 0.9300 . ? C502 C503 1.322(17) . ? C502 H502 0.9300 . ? C503 C504 1.347(18) . ? C503 H503 0.9300 . ? C504 C505 1.395(14) . ? C504 H504 0.9300 . ? C505 H505 0.9300 . ? C511 C512 1.408(15) . ? C511 H511 0.9300 . ? C512 C513 1.310(17) . ? C512 H512 0.9300 . ? C513 C514 1.277(16) . ? C513 H513 0.9300 . ? C514 C515 1.421(14) . ? C514 H514 0.9300 . ? C515 H515 0.9300 . ? C601 C602 1.395(11) . ? C601 H601 0.9300 . ? C602 C603 1.370(14) . ? C602 H602 0.9300 . ? C603 C604 1.358(15) . ? C603 H603 0.9300 . ? C604 C605 1.369(12) . ? C604 H604 0.9300 . ? C605 H605 0.9300 . ? C61 C615 1.358(11) . ? C61 C611 1.391(10) . ? C612 C613 1.333(12) . ? C612 C611 1.375(11) . ? C612 H612 0.9300 . ? C613 C614 1.378(13) . ? C613 H613 0.9300 . ? C614 C615 1.386(12) . ? C614 H614 0.9300 . ? C615 H615 0.9300 . ? C611 H611 0.9300 . ? 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 P3 Ag1 P2 115.62(6) . . ? P3 Ag1 I2 112.64(4) . . ? P2 Ag1 I2 105.79(4) . . ? P3 Ag1 I1 102.30(4) . . ? P2 Ag1 I1 114.80(4) . . ? I2 Ag1 I1 105.416(18) . . ? P3 Ag1 Ag2 151.14(4) . . ? P2 Ag1 Ag2 93.10(4) . . ? I2 Ag1 Ag2 57.913(15) . . ? I1 Ag1 Ag2 60.065(15) . . ? P3 Ag1 Ag3 88.59(4) . . ? P2 Ag1 Ag3 155.64(4) . . ? I2 Ag1 Ag3 59.076(15) . . ? I1 Ag1 Ag3 58.457(14) . . ? Ag2 Ag1 Ag3 62.912(15) . . ? P6 Ag2 P1 123.84(6) . . ? P6 Ag2 I2 112.88(4) . . ? P1 Ag2 I2 108.12(4) . . ? P6 Ag2 I1 100.20(4) . . ? P1 Ag2 I1 105.46(4) . . ? I2 Ag2 I1 103.863(19) . . ? P6 Ag2 Ag1 147.46(4) . . ? P1 Ag2 Ag1 87.15(4) . . ? I2 Ag2 Ag1 58.307(15) . . ? I1 Ag2 Ag1 57.721(15) . . ? P6 Ag2 Ag3 89.40(4) . . ? P1 Ag2 Ag3 145.96(4) . . ? I2 Ag2 Ag3 57.710(15) . . ? I1 Ag2 Ag3 56.386(14) . . ? Ag1 Ag2 Ag3 58.881(15) . . ? P5 Ag3 P4 121.89(6) . . ? P5 Ag3 I1 102.13(4) . . ? P4 Ag3 I1 106.40(4) . . ? P5 Ag3 I2 109.12(4) . . ? P4 Ag3 I2 111.52(4) . . ? I1 Ag3 I2 103.798(18) . . ? P5 Ag3 Ag1 145.87(4) . . ? P4 Ag3 Ag1 91.64(4) . . ? I1 Ag3 Ag1 58.083(15) . . ? I2 Ag3 Ag1 57.428(15) . . ? P5 Ag3 Ag2 87.96(4) . . ? P4 Ag3 Ag2 149.80(4) . . ? I1 Ag3 Ag2 58.230(15) . . ? I2 Ag3 Ag2 55.781(15) . . ? Ag1 Ag3 Ag2 58.208(15) . . ? Ag1 I1 Ag3 63.459(15) . . ? Ag1 I1 Ag2 62.214(15) . . ? Ag3 I1 Ag2 65.384(15) . . ? Ag2 I2 Ag1 63.780(16) . . ? Ag2 I2 Ag3 66.509(15) . . ? Ag1 I2 Ag3 63.497(15) . . ? O1A Cl1A O4A 115.6(17) . . ? O1A Cl1A O3A 111.8(15) . . ? O4A Cl1A O3A 108.9(12) . . ? O1A Cl1A O2A 108.8(15) . . ? O4A Cl1A O2A 111.6(17) . . ? O3A Cl1A O2A 98.8(14) . . ? O2B Cl1B O4B 113(3) . . ? O2B Cl1B O3B 112(2) . . ? O4B Cl1B O3B 105(2) . . ? O2B Cl1B O1B 108(3) . . ? O4B Cl1B O1B 112(3) . . ? O3B Cl1B O1B 107(3) . . ? C1 P1 C10 102.0(3) . . ? C1 P1 C11 106.3(3) . . ? C10 P1 C11 102.1(3) . . ? C1 P1 Ag2 116.2(2) . . ? C10 P1 Ag2 114.1(2) . . ? C11 P1 Ag2 114.5(2) . . ? C1 P2 C20 105.6(3) . . ? C1 P2 C21 105.0(3) . . ? C20 P2 C21 103.4(3) . . ? C1 P2 Ag1 113.5(2) . . ? C20 P2 Ag1 111.0(2) . . ? C21 P2 Ag1 117.2(2) . . ? C30 P3 C3 103.2(3) . . ? C30 P3 C31 106.1(3) . . ? C3 P3 C31 103.4(3) . . ? C30 P3 Ag1 118.6(2) . . ? C3 P3 Ag1 116.9(2) . . ? C31 P3 Ag1 107.2(2) . . ? C3 P4 C41 102.8(3) . . ? C3 P4 C40 106.3(3) . . ? C41 P4 C40 105.3(3) . . ? C3 P4 Ag3 112.9(2) . . ? C41 P4 Ag3 115.8(2) . . ? C40 P4 Ag3 112.8(3) . . ? C5 P5 C50 104.5(4) . . ? C5 P5 C51 103.1(4) . . ? C50 P5 C51 104.7(4) . . ? C5 P5 Ag3 115.4(2) . . ? C50 P5 Ag3 117.9(3) . . ? C51 P5 Ag3 109.7(3) . . ? C60 P6 C5 103.0(3) . . ? C60 P6 C61 105.4(3) . . ? C5 P6 C61 105.0(3) . . ? C60 P6 Ag2 119.2(2) . . ? C5 P6 Ag2 114.4(2) . . ? C61 P6 Ag2 108.6(2) . . ? C2 N2 C24 131.3(7) . . ? C4 N4 C44 132.2(8) . . ? C6 N6 C64' 142.5(11) . . ? C6 N6 C64 120.0(10) . . ? C64' N6 C64 22.9(6) . . ? C2 C1 P2 123.1(5) . . ? C2 C1 P1 119.6(5) . . ? P2 C1 P1 117.2(3) . . ? N2 C2 C1 170.9(8) . . ? C4 C3 P4 123.7(5) . . ? C4 C3 P3 118.3(5) . . ? P4 C3 P3 118.0(4) . . ? N4 C4 C3 168.0(8) . . ? C6 C5 P5 119.2(6) . . ? C6 C5 P6 122.0(6) . . ? P5 C5 P6 118.2(4) . . ? N6 C6 C5 169.4(9) . . ? C101 C10 C105 116.9(7) . . ? C101 C10 P1 123.6(5) . . ? C105 C10 P1 119.5(6) . . ? C115 C11 C111 119.9(7) . . ? C115 C11 P1 117.2(5) . . ? C111 C11 P1 122.8(6) . . ? C201 C20 C205 118.3(7) . . ? C201 C20 P2 121.2(5) . . ? C205 C20 P2 120.0(5) . . ? C215 C21 C211 119.4(6) . . ? C215 C21 P2 122.1(5) . . ? C211 C21 P2 118.5(5) . . ? C25 C24 C29 120.2(9) . . ? C25 C24 N2 119.2(8) . . ? C29 C24 N2 120.6(8) . . ? C24 C25 C26 121.4(10) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 118.9(10) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 121.6(11) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C29 C28 C27 117.6(12) . . ? C29 C28 H28 121.2 . . ? C27 C28 H28 121.2 . . ? C24 C29 C28 120.3(11) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C305 C30 C301 117.9(7) . . ? C305 C30 P3 120.4(6) . . ? C301 C30 P3 121.4(6) . . ? C315 C31 C311 118.8(6) . . ? C315 C31 P3 121.1(5) . . ? C311 C31 P3 119.8(5) . . ? C401 C40 C405 118.5(8) . . ? C401 C40 P4 125.7(7) . . ? C405 C40 P4 115.8(6) . . ? C411 C41 C415 117.8(8) . . ? C411 C41 P4 123.4(7) . . ? C415 C41 P4 118.9(6) . . ? C49 C44 C45 122.2(9) . . ? C49 C44 N4 116.0(9) . . ? C45 C44 N4 121.6(8) . . ? C44 C45 C46 120.5(10) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 117.9(12) . . ? C47 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C46 C47 C48 121.2(11) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C49 121.0(11) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C44 C49 C48 117.1(12) . . ? C44 C49 H49 121.5 . . ? C48 C49 H49 121.5 . . ? C501 C50 C505 118.1(8) . . ? C501 C50 P5 121.9(7) . . ? C505 C50 P5 120.0(7) . . ? C511 C51 C515 116.1(9) . . ? C511 C51 P5 123.5(8) . . ? C515 C51 P5 120.2(7) . . ? C601 C60 C605 118.0(7) . . ? C601 C60 P6 119.2(6) . . ? C605 C60 P6 122.5(6) . . ? C69 C64 C65 121.0 . . ? C69 C64 N6 108.9(8) . . ? C65 C64 N6 130.1(8) . . ? C66 C65 C64 119.4 . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C65 C66 C67 119.9 . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C66 C67 C68 120.1 . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? C69 C68 C67 120.2 . . ? C69 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C68 C69 C64 119.4 . . ? C68 C69 H69 120.3 . . ? C64 C69 H69 120.3 . . ? N6 C64' C65' 112.6(9) . . ? N6 C64' C69' 128.3(9) . . ? C65' C64' C69' 119.0 . . ? C64' C65' C66' 120.5 . . ? C64' C65' H65' 119.7 . . ? C66' C65' H65' 119.7 . . ? C67' C66' C65' 120.2 . . ? C67' C66' H66' 119.9 . . ? C65' C66' H66' 119.9 . . ? C68' C67' C66' 119.8 . . ? C68' C67' H67' 120.1 . . ? C66' C67' H67' 120.1 . . ? C67' C68' C69' 119.8 . . ? C67' C68' H68' 120.1 . . ? C69' C68' H68' 120.1 . . ? C64' C69' C68' 120.6 . . ? C64' C69' H69' 119.7 . . ? C68' C69' H69' 119.7 . . ? C10 C101 C102 122.4(7) . . ? C10 C101 H101 118.8 . . ? C102 C101 H101 118.8 . . ? C103 C102 C101 119.7(8) . . ? C103 C102 H102 120.2 . . ? C101 C102 H102 120.2 . . ? C102 C103 C104 119.2(8) . . ? C102 C103 H103 120.4 . . ? C104 C103 H103 120.4 . . ? C105 C104 C103 119.5(8) . . ? C105 C104 H104 120.2 . . ? C103 C104 H104 120.2 . . ? C104 C105 C10 122.0(8) . . ? C104 C105 H105 119.0 . . ? C10 C105 H105 119.0 . . ? C112 C111 C11 119.1(8) . . ? C112 C111 H111 120.4 . . ? C11 C111 H111 120.4 . . ? C111 C112 C113 119.8(8) . . ? C111 C112 H112 120.1 . . ? C113 C112 H112 120.1 . . ? C114 C113 C112 120.7(8) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.8(9) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C11 C115 C114 120.5(8) . . ? C11 C115 H115 119.7 . . ? C114 C115 H115 119.7 . . ? C20 C201 C202 120.2(7) . . ? C20 C201 H201 119.9 . . ? C202 C201 H201 119.9 . . ? C203 C202 C201 120.4(8) . . ? C203 C202 H202 119.8 . . ? C201 C202 H202 119.8 . . ? C204 C203 C202 119.5(8) . . ? C204 C203 H203 120.3 . . ? C202 C203 H203 120.3 . . ? C203 C204 C205 120.6(8) . . ? C203 C204 H204 119.7 . . ? C205 C204 H204 119.7 . . ? C204 C205 C20 121.0(7) . . ? C204 C205 H205 119.5 . . ? C20 C205 H205 119.5 . . ? C212 C211 C21 118.5(7) . . ? C212 C211 H211 120.7 . . ? C21 C211 H211 120.7 . . ? C211 C212 C213 122.1(8) . . ? C211 C212 H212 119.0 . . ? C213 C212 H212 119.0 . . ? C214 C213 C212 119.6(8) . . ? C214 C213 H213 120.2 . . ? C212 C213 H213 120.2 . . ? C213 C214 C215 119.0(8) . . ? C213 C214 H214 120.5 . . ? C215 C214 H214 120.5 . . ? C21 C215 C214 121.2(8) . . ? C21 C215 H215 119.4 . . ? C214 C215 H215 119.4 . . ? C302 C301 C30 121.9(9) . . ? C302 C301 H301 119.0 . . ? C30 C301 H301 119.0 . . ? C303 C302 C301 118.3(9) . . ? C303 C302 H302 120.8 . . ? C301 C302 H302 120.8 . . ? C304 C303 C302 120.2(9) . . ? C304 C303 H303 119.9 . . ? C302 C303 H303 119.9 . . ? C303 C304 C305 121.2(10) . . ? C303 C304 H304 119.4 . . ? C305 C304 H304 119.4 . . ? C30 C305 C304 120.3(9) . . ? C30 C305 H305 119.9 . . ? C304 C305 H305 119.9 . . ? C31 C311 C312 120.6(7) . . ? C31 C311 H311 119.7 . . ? C312 C311 H311 119.7 . . ? C313 C312 C311 119.6(7) . . ? C313 C312 H312 120.2 . . ? C311 C312 H312 120.2 . . ? C314 C313 C312 119.9(7) . . ? C314 C313 H313 120.1 . . ? C312 C313 H313 120.1 . . ? C313 C314 C315 120.3(8) . . ? C313 C314 H314 119.8 . . ? C315 C314 H314 119.8 . . ? C31 C315 C314 120.7(7) . . ? C31 C315 H315 119.7 . . ? C314 C315 H315 119.7 . . ? C40 C401 C402 120.3(10) . . ? C40 C401 H401 119.8 . . ? C402 C401 H401 119.8 . . ? C403 C402 C401 119.0(11) . . ? C403 C402 H402 120.5 . . ? C401 C402 H402 120.5 . . ? C402 C403 C404 124.5(11) . . ? C402 C403 H403 117.7 . . ? C404 C403 H403 117.7 . . ? C403 C404 C405 116.4(11) . . ? C403 C404 H404 121.8 . . ? C405 C404 H404 121.8 . . ? C404 C405 C40 121.0(10) . . ? C404 C405 H405 119.5 . . ? C40 C405 H405 119.5 . . ? C41 C411 C412 120.6(10) . . ? C41 C411 H411 119.7 . . ? C412 C411 H411 119.7 . . ? C411 C412 C413 120.3(10) . . ? C411 C412 H412 119.9 . . ? C413 C412 H412 119.9 . . ? C414 C413 C412 119.4(9) . . ? C414 C413 H413 120.3 . . ? C412 C413 H413 120.3 . . ? C413 C414 C415 120.6(9) . . ? C413 C414 H414 119.7 . . ? C415 C414 H414 119.7 . . ? C414 C415 C41 121.2(9) . . ? C414 C415 H415 119.4 . . ? C41 C415 H415 119.4 . . ? C50 C501 C502 121.8(10) . . ? C50 C501 H501 119.1 . . ? C502 C501 H501 119.1 . . ? C503 C502 C501 119.5(12) . . ? C503 C502 H502 120.3 . . ? C501 C502 H502 120.3 . . ? C502 C503 C504 121.0(10) . . ? C502 C503 H503 119.5 . . ? C504 C503 H503 119.5 . . ? C503 C504 C505 120.4(11) . . ? C503 C504 H504 119.8 . . ? C505 C504 H504 119.8 . . ? C504 C505 C50 119.2(11) . . ? C504 C505 H505 120.4 . . ? C50 C505 H505 120.4 . . ? C51 C511 C512 120.9(12) . . ? C51 C511 H511 119.6 . . ? C512 C511 H511 119.6 . . ? C513 C512 C511 122.5(12) . . ? C513 C512 H512 118.8 . . ? C511 C512 H512 118.8 . . ? C514 C513 C512 117.4(11) . . ? C514 C513 H513 121.3 . . ? C512 C513 H513 121.3 . . ? C513 C514 C515 121.5(12) . . ? C513 C514 H514 119.2 . . ? C515 C514 H514 119.2 . . ? C51 C515 C514 121.5(11) . . ? C51 C515 H515 119.3 . . ? C514 C515 H515 119.3 . . ? C602 C601 C60 119.9(8) . . ? C602 C601 H601 120.0 . . ? C60 C601 H601 120.0 . . ? C603 C602 C601 120.6(9) . . ? C603 C602 H602 119.7 . . ? C601 C602 H602 119.7 . . ? C604 C603 C602 119.6(9) . . ? C604 C603 H603 120.2 . . ? C602 C603 H603 120.2 . . ? C603 C604 C605 122.0(9) . . ? C603 C604 H604 119.0 . . ? C605 C604 H604 119.0 . . ? C604 C605 C60 119.7(8) . . ? C604 C605 H605 120.2 . . ? C60 C605 H605 120.2 . . ? C615 C61 C611 117.4(7) . . ? C615 C61 P6 121.0(6) . . ? C611 C61 P6 120.8(5) . . ? C613 C612 C611 119.9(8) . . ? C613 C612 H612 120.1 . . ? C611 C612 H612 120.1 . . ? C612 C613 C614 120.3(8) . . ? C612 C613 H613 119.8 . . ? C614 C613 H613 119.8 . . ? C613 C614 C615 119.6(9) . . ? C613 C614 H614 120.2 . . ? C615 C614 H614 120.2 . . ? C61 C615 C614 121.0(8) . . ? C61 C615 H615 119.5 . . ? C614 C615 H615 119.5 . . ? C612 C611 C61 121.6(7) . . ? C612 C611 H611 119.2 . . ? C61 C611 H611 119.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.282 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.136 #=====END data_11 _database_code_depnum_ccdc_archive 'CCDC 720844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 B Cu F4 N2 O4 P4, 2(C H Cl3), B F4 ' _chemical_formula_sum 'C62 H60 B2 Cl6 Cu F8 N2 O4 P4' _chemical_formula_weight 1470.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.6068(2) _cell_length_b 17.5173(2) _cell_length_c 39.3124(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13502.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13445 _cell_measurement_theta_min 2.067 _cell_measurement_theta_max 70.93 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6044 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 4.128 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.401 _exptl_absorpt_correction_T_max 0.4320 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71577 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 69.99 _reflns_number_total 12679 _reflns_number_gt 9397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0644P)^2^+13.5665P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12679 _refine_ls_number_parameters 839 _refine_ls_number_restraints 342 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.062 _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 0.61305(2) 0.94849(2) 0.138115(11) 0.02132(12) Uani 1 1 d . . . P1 P 0.47299(4) 0.85457(4) 0.131653(19) 0.02284(17) Uani 1 1 d . . . P2 P 0.75425(4) 0.86676(4) 0.12732(2) 0.02436(18) Uani 1 1 d . . . P3 P 0.46813(4) 1.02759(4) 0.12223(2) 0.02339(17) Uani 1 1 d . . . P4 P 0.75402(4) 1.04032(4) 0.129532(19) 0.02317(17) Uani 1 1 d . . . N4 N 0.91739(13) 0.95270(15) 0.15950(7) 0.0311(6) Uani 1 1 d . . . N3 N 0.31077(14) 0.94353(16) 0.16099(8) 0.0358(7) Uani 1 1 d . . . O1 O 0.54918(10) 0.86463(12) 0.13472(6) 0.0285(5) Uani 1 1 d . . . O2 O 0.68246(10) 0.87083(12) 0.14113(6) 0.0283(5) Uani 1 1 d . . . O3 O 0.54493(10) 1.02277(12) 0.12354(5) 0.0271(5) Uani 1 1 d . . . O4 O 0.67938(10) 1.03052(12) 0.13714(6) 0.0280(5) Uani 1 1 d . . . C1 C 0.42988(15) 0.94273(17) 0.13714(8) 0.0253(6) Uani 1 1 d U . . C3 C 0.36754(16) 0.94393(18) 0.15145(8) 0.0287(7) Uani 1 1 d U . . C2 C 0.79868(14) 0.95329(17) 0.13514(7) 0.0230(6) Uani 1 1 d U . . C4 C 0.86061(16) 0.95245(17) 0.14976(8) 0.0262(7) Uani 1 1 d U . . C11 C 0.45331(16) 0.81543(18) 0.09073(8) 0.0291(7) Uani 1 1 d U . . C12 C 0.5012(2) 0.7713(3) 0.07425(12) 0.0665(13) Uani 1 1 d U . . H12 H 0.5433 0.7624 0.0844 0.080 Uiso 1 1 calc R . . C13 C 0.4871(2) 0.7402(4) 0.04282(14) 0.0841(16) Uani 1 1 d U . . H13 H 0.5195 0.7103 0.0318 0.101 Uiso 1 1 calc R . . C14 C 0.4248(2) 0.7537(3) 0.02777(11) 0.0639(12) Uani 1 1 d U . . H14 H 0.4155 0.7335 0.0064 0.077 Uiso 1 1 calc R . . C15 C 0.3769(2) 0.7962(2) 0.04394(10) 0.0514(10) Uani 1 1 d U . . H15 H 0.3347 0.8045 0.0338 0.062 Uiso 1 1 calc R . . C16 C 0.39116(18) 0.8273(2) 0.07549(9) 0.0407(8) Uani 1 1 d U . . H16 H 0.3583 0.8565 0.0865 0.049 Uiso 1 1 calc R . . C21 C 0.80257(15) 0.79487(18) 0.14847(8) 0.0282(7) Uani 1 1 d U . . C22 C 0.79429(16) 0.78910(19) 0.18359(8) 0.0317(7) Uani 1 1 d U . . H22 H 0.7637 0.8208 0.1949 0.038 Uiso 1 1 calc R . . C23 C 0.83195(18) 0.7358(2) 0.20149(10) 0.0404(8) Uani 1 1 d U . . H23 H 0.8267 0.7319 0.2249 0.048 Uiso 1 1 calc R . . C24 C 0.87745(17) 0.6881(2) 0.18486(10) 0.0409(8) Uani 1 1 d U . . H24 H 0.9020 0.6518 0.1971 0.049 Uiso 1 1 calc R . . C25 C 0.88634(17) 0.69439(19) 0.15013(10) 0.0401(8) Uani 1 1 d U . . H25 H 0.9174 0.6629 0.1391 0.048 Uiso 1 1 calc R . . C26 C 0.84888(16) 0.74788(18) 0.13148(9) 0.0331(7) Uani 1 1 d U . . H26 H 0.8547 0.7521 0.1081 0.040 Uiso 1 1 calc R . . C30 C 0.26365(16) 0.94708(19) 0.19032(8) 0.0318(7) Uani 1 1 d U . . C31 C 0.44131(16) 0.79113(17) 0.16369(8) 0.0287(7) Uani 1 1 d U . . C32 C 0.39220(19) 0.7367(2) 0.15690(10) 0.0421(9) Uani 1 1 d U . . H32 H 0.3728 0.7336 0.1353 0.050 Uiso 1 1 calc R . . C33 C 0.3716(2) 0.6862(2) 0.18246(10) 0.0513(10) Uani 1 1 d U . . H33 H 0.3389 0.6493 0.1778 0.062 Uiso 1 1 calc R . . C34 C 0.3996(2) 0.6910(2) 0.21418(10) 0.0480(10) Uani 1 1 d U . . H34 H 0.3861 0.6569 0.2310 0.058 Uiso 1 1 calc R . . C35 C 0.44754(19) 0.7460(2) 0.22153(9) 0.0434(9) Uani 1 1 d U . . H35 H 0.4658 0.7493 0.2433 0.052 Uiso 1 1 calc R . . C36 C 0.46882(17) 0.7968(2) 0.19648(8) 0.0335(7) Uani 1 1 d U . . H36 H 0.5010 0.8341 0.2014 0.040 Uiso 1 1 calc R . . C37 C 0.2694(2) 0.8709(2) 0.20908(11) 0.0531(10) Uani 1 1 d U . . H37A H 0.2562 0.8302 0.1941 0.080 Uiso 1 1 calc R . . H37B H 0.2400 0.8714 0.2286 0.080 Uiso 1 1 calc R . . H37C H 0.3157 0.8633 0.2163 0.080 Uiso 1 1 calc R . . C38 C 0.19206(18) 0.9574(3) 0.17591(10) 0.0489(10) Uani 1 1 d U . . H38A H 0.1807 0.9142 0.1620 0.073 Uiso 1 1 calc R . . H38B H 0.1905 1.0030 0.1624 0.073 Uiso 1 1 calc R . . H38C H 0.1599 0.9614 0.1943 0.073 Uiso 1 1 calc R . . C39 C 0.2833(2) 1.0138(2) 0.21212(10) 0.0454(9) Uani 1 1 d U . . H39A H 0.2789 1.0601 0.1992 0.068 Uiso 1 1 calc R . . H39B H 0.3297 1.0081 0.2195 0.068 Uiso 1 1 calc R . . H39C H 0.2538 1.0160 0.2316 0.068 Uiso 1 1 calc R . . C40 C 0.96036(17) 0.94947(19) 0.19058(9) 0.0332(7) Uani 1 1 d U . . C41 C 0.75069(16) 0.84773(18) 0.08261(8) 0.0300(7) Uani 1 1 d U . . C42 C 0.69274(18) 0.8108(2) 0.07010(9) 0.0402(8) Uani 1 1 d U . . H42 H 0.6576 0.7974 0.0848 0.048 Uiso 1 1 calc R . . C43 C 0.6876(2) 0.7942(2) 0.03576(10) 0.0489(10) Uani 1 1 d U . . H43 H 0.6489 0.7698 0.0274 0.059 Uiso 1 1 calc R . . C44 C 0.7396(2) 0.8135(2) 0.01398(10) 0.0485(10) Uani 1 1 d U . . H44 H 0.7359 0.8019 -0.0090 0.058 Uiso 1 1 calc R . . C45 C 0.7967(2) 0.8498(2) 0.02593(10) 0.0460(9) Uani 1 1 d U . . H45 H 0.8315 0.8629 0.0110 0.055 Uiso 1 1 calc R . . C46 C 0.80291(18) 0.8670(2) 0.06026(9) 0.0364(8) Uani 1 1 d U . . H46 H 0.8419 0.8914 0.0683 0.044 Uiso 1 1 calc R . . C47 C 0.9999(2) 1.0234(2) 0.19160(11) 0.0498(10) Uani 1 1 d U . . H47A H 1.0279 1.0273 0.1717 0.075 Uiso 1 1 calc R . . H47B H 1.0283 1.0243 0.2115 0.075 Uiso 1 1 calc R . . H47C H 0.9687 1.0656 0.1923 0.075 Uiso 1 1 calc R . . C48 C 1.00664(19) 0.8801(2) 0.18615(10) 0.0452(9) Uani 1 1 d U . . H48A H 0.9795 0.8346 0.1858 0.068 Uiso 1 1 calc R . . H48B H 1.0384 0.8777 0.2047 0.068 Uiso 1 1 calc R . . H48C H 1.0312 0.8845 0.1651 0.068 Uiso 1 1 calc R . . C49 C 0.9150(2) 0.9404(2) 0.22180(9) 0.0469(9) Uani 1 1 d U . . H49A H 0.8908 0.8929 0.2204 0.070 Uiso 1 1 calc R . . H49B H 0.8830 0.9819 0.2227 0.070 Uiso 1 1 calc R . . H49C H 0.9427 0.9408 0.2419 0.070 Uiso 1 1 calc R . . C51 C 0.43587(15) 1.10120(17) 0.14940(8) 0.0264(7) Uani 1 1 d U . . C52 C 0.45394(16) 1.09689(18) 0.18376(8) 0.0305(7) Uani 1 1 d U . . H52 H 0.4808 1.0568 0.1915 0.037 Uiso 1 1 calc R . . C53 C 0.43152(17) 1.15289(19) 0.20632(9) 0.0348(7) Uani 1 1 d U . . H53 H 0.4440 1.1506 0.2291 0.042 Uiso 1 1 calc R . . C54 C 0.39082(18) 1.2116(2) 0.19482(10) 0.0407(8) Uani 1 1 d U . . H54 H 0.3751 1.2483 0.2100 0.049 Uiso 1 1 calc R . . C55 C 0.3732(2) 1.2164(2) 0.16075(10) 0.0455(9) Uani 1 1 d U . . H55 H 0.3464 1.2568 0.1532 0.055 Uiso 1 1 calc R . . C56 C 0.39531(17) 1.1613(2) 0.13788(9) 0.0366(8) Uani 1 1 d U . . H56 H 0.3832 1.1644 0.1151 0.044 Uiso 1 1 calc R . . C61 C 0.79506(14) 1.10637(17) 0.15753(8) 0.0240(6) Uani 1 1 d U . . C62 C 0.83713(15) 1.16528(17) 0.14605(8) 0.0283(7) Uani 1 1 d U . . H62 H 0.8430 1.1730 0.1228 0.034 Uiso 1 1 calc R . . C63 C 0.87004(16) 1.21209(19) 0.16912(9) 0.0331(7) Uani 1 1 d U . . H63 H 0.8984 1.2509 0.1613 0.040 Uiso 1 1 calc R . . C64 C 0.86115(17) 1.20169(19) 0.20357(9) 0.0340(7) Uani 1 1 d U . . H64 H 0.8832 1.2335 0.2190 0.041 Uiso 1 1 calc R . . C65 C 0.81897(17) 1.14330(19) 0.21526(9) 0.0350(8) Uani 1 1 d U . . H65 H 0.8130 1.1363 0.2385 0.042 Uiso 1 1 calc R . . C66 C 0.78595(16) 1.09571(18) 0.19257(8) 0.0299(7) Uani 1 1 d U . . H66 H 0.7579 1.0568 0.2005 0.036 Uiso 1 1 calc R . . C71 C 0.44263(16) 1.04437(18) 0.07903(8) 0.0285(7) Uani 1 1 d U . . C72 C 0.37542(18) 1.0309(2) 0.06853(9) 0.0393(8) Uani 1 1 d U . . H72 H 0.3429 1.0150 0.0842 0.047 Uiso 1 1 calc R . . C73 C 0.3575(2) 1.0413(2) 0.03491(10) 0.0500(10) Uani 1 1 d U . . H73 H 0.3130 1.0319 0.0280 0.060 Uiso 1 1 calc R . . C74 C 0.4055(2) 1.0656(2) 0.01148(10) 0.0512(10) Uani 1 1 d U . . H74 H 0.3931 1.0730 -0.0111 0.061 Uiso 1 1 calc R . . C75 C 0.4715(2) 1.0788(2) 0.02172(9) 0.0478(9) Uani 1 1 d U . . H75 H 0.5038 1.0949 0.0060 0.057 Uiso 1 1 calc R . . C76 C 0.49017(19) 1.0681(2) 0.05536(9) 0.0385(8) Uani 1 1 d U . . H76 H 0.5350 1.0770 0.0620 0.046 Uiso 1 1 calc R . . C81 C 0.76411(17) 1.06967(18) 0.08611(8) 0.0309(7) Uani 1 1 d U . . C82 C 0.7060(2) 1.0899(2) 0.06794(9) 0.0437(9) Uani 1 1 d U . . H82 H 0.6639 1.0917 0.0788 0.052 Uiso 1 1 calc R . . C83 C 0.7112(3) 1.1074(3) 0.03374(11) 0.0600(11) Uani 1 1 d U . . H83 H 0.6724 1.1218 0.0217 0.072 Uiso 1 1 calc R . . C84 C 0.7724(3) 1.1037(2) 0.01740(10) 0.0574(11) Uani 1 1 d U . . H84 H 0.7750 1.1148 -0.0057 0.069 Uiso 1 1 calc R . . C85 C 0.8305(2) 1.0835(2) 0.03495(10) 0.0537(10) Uani 1 1 d U . . H85 H 0.8722 1.0813 0.0237 0.064 Uiso 1 1 calc R . . C86 C 0.8268(2) 1.0663(2) 0.06949(9) 0.0394(8) Uani 1 1 d U . . H86 H 0.8659 1.0526 0.0814 0.047 Uiso 1 1 calc R . . B1 B 0.62511(19) 0.9527(2) 0.22417(9) 0.0313(8) Uani 1 1 d . . . F11 F 0.58639(10) 0.96167(12) 0.19405(5) 0.0408(5) Uani 1 1 d . . . F12 F 0.69287(10) 0.94162(12) 0.21572(5) 0.0417(5) Uani 1 1 d . . . F13 F 0.61903(12) 1.01845(13) 0.24333(6) 0.0545(6) Uani 1 1 d . . . F14 F 0.60091(11) 0.89070(14) 0.24166(5) 0.0540(6) Uani 1 1 d . . . B2 B 0.2914(2) 0.3445(3) 0.08785(12) 0.0483(11) Uani 1 1 d . . . F21 F 0.30494(18) 0.3074(2) 0.05814(7) 0.0950(10) Uani 1 1 d . . . F22 F 0.25202(12) 0.40830(15) 0.08075(8) 0.0712(8) Uani 1 1 d . . . F23 F 0.25683(13) 0.29847(15) 0.11047(7) 0.0720(8) Uani 1 1 d . . . F24 F 0.35256(11) 0.36855(13) 0.10255(5) 0.0501(5) Uani 1 1 d . . . C1D C 0.4797(11) 0.3568(17) 0.0578(8) 0.041(3) Uani 0.723(17) 1 d PU A 1 H1D H 0.4308 0.3678 0.0595 0.049 Uiso 0.723(17) 1 calc PR A 1 Cl1 Cl 0.51160(15) 0.40809(17) 0.02258(7) 0.0461(9) Uani 0.723(17) 1 d P A 1 Cl2 Cl 0.51880(14) 0.39323(14) 0.09478(7) 0.0512(9) Uani 0.723(17) 1 d P A 1 Cl3 Cl 0.4887(2) 0.2610(2) 0.05499(11) 0.0727(10) Uani 0.723(17) 1 d P A 1 C1D' C 0.467(3) 0.365(4) 0.059(2) 0.039(6) Uani 0.277(17) 1 d PU A 2 H1D' H 0.4223 0.3887 0.0637 0.046 Uiso 0.277(17) 1 calc PR A 2 Cl1' Cl 0.5085(8) 0.4106(11) 0.0255(5) 0.136(7) Uani 0.277(17) 1 d P A 2 Cl2' Cl 0.5152(5) 0.354(3) 0.0946(3) 0.169(9) Uani 0.277(17) 1 d P A 2 Cl3' Cl 0.4578(15) 0.2650(8) 0.0423(6) 0.128(7) Uani 0.277(17) 1 d P A 2 C2D C 0.3508(2) 0.5506(2) 0.08467(10) 0.0530(10) Uani 1 1 d . . . H2D H 0.3334 0.5054 0.0965 0.064 Uiso 1 1 calc R . . Cl4 Cl 0.42930(8) 0.57437(10) 0.10226(4) 0.1035(6) Uani 1 1 d . . . Cl5 Cl 0.35972(8) 0.52793(7) 0.04142(3) 0.0712(3) Uani 1 1 d . . . Cl6 Cl 0.29334(6) 0.62432(7) 0.09078(3) 0.0704(3) 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 0.0204(2) 0.0214(2) 0.0222(2) 0.00057(17) -0.00084(16) 0.00033(16) P1 0.0218(4) 0.0220(4) 0.0247(4) 0.0003(3) -0.0011(3) -0.0013(3) P2 0.0218(4) 0.0220(4) 0.0293(4) -0.0007(3) -0.0021(3) 0.0010(3) P3 0.0224(4) 0.0219(4) 0.0259(4) 0.0026(3) -0.0014(3) 0.0006(3) P4 0.0225(4) 0.0223(4) 0.0247(4) 0.0020(3) -0.0018(3) -0.0010(3) N4 0.0253(14) 0.0326(15) 0.0352(16) -0.0010(12) -0.0058(12) 0.0007(11) N3 0.0342(16) 0.0342(16) 0.0391(17) 0.0010(13) 0.0062(13) 0.0013(12) O1 0.0240(11) 0.0223(11) 0.0391(13) 0.0005(9) -0.0038(9) 0.0007(8) O2 0.0250(11) 0.0221(11) 0.0380(13) 0.0024(9) 0.0005(9) -0.0006(8) O3 0.0251(10) 0.0224(11) 0.0338(12) 0.0031(9) -0.0009(9) 0.0002(9) O4 0.0246(11) 0.0217(11) 0.0375(13) 0.0007(9) -0.0030(9) 0.0011(8) C1 0.0227(14) 0.0269(16) 0.0264(16) 0.0015(13) 0.0005(12) -0.0003(12) C3 0.0309(17) 0.0244(16) 0.0310(18) 0.0006(13) -0.0010(13) 0.0011(13) C2 0.0213(14) 0.0248(16) 0.0229(15) 0.0002(12) -0.0010(11) -0.0001(12) C4 0.0326(17) 0.0227(15) 0.0234(16) -0.0008(12) 0.0021(13) 0.0007(13) C11 0.0329(16) 0.0284(16) 0.0259(16) -0.0014(13) 0.0044(13) -0.0052(13) C12 0.036(2) 0.099(3) 0.065(3) -0.046(3) 0.0011(19) 0.001(2) C13 0.054(3) 0.126(4) 0.072(3) -0.064(3) 0.012(2) -0.009(3) C14 0.063(3) 0.095(3) 0.034(2) -0.021(2) 0.0080(19) -0.029(2) C15 0.061(2) 0.056(2) 0.037(2) -0.0022(18) -0.0148(18) -0.0045(19) C16 0.0439(19) 0.040(2) 0.038(2) -0.0067(16) -0.0101(16) 0.0058(16) C21 0.0232(14) 0.0243(16) 0.0370(18) -0.0016(13) -0.0047(13) 0.0003(12) C22 0.0309(16) 0.0286(17) 0.0357(18) 0.0016(14) -0.0034(13) 0.0013(13) C23 0.0392(18) 0.0381(19) 0.044(2) 0.0087(16) -0.0084(16) -0.0016(15) C24 0.0363(18) 0.0312(18) 0.055(2) 0.0109(17) -0.0127(16) 0.0017(15) C25 0.0305(17) 0.0249(17) 0.065(2) -0.0048(16) -0.0081(16) 0.0055(14) C26 0.0311(16) 0.0253(17) 0.0429(19) -0.0015(14) -0.0032(14) -0.0008(13) C30 0.0274(16) 0.0372(19) 0.0307(18) -0.0040(14) 0.0070(13) -0.0025(14) C31 0.0326(16) 0.0232(16) 0.0304(17) 0.0004(13) 0.0060(13) 0.0028(13) C32 0.058(2) 0.0349(19) 0.0335(19) -0.0042(15) 0.0084(16) -0.0156(16) C33 0.077(3) 0.0317(19) 0.045(2) -0.0040(17) 0.021(2) -0.0176(18) C34 0.076(3) 0.0311(19) 0.037(2) 0.0079(16) 0.0270(19) 0.0124(18) C35 0.052(2) 0.049(2) 0.0292(18) 0.0089(16) 0.0067(16) 0.0165(18) C36 0.0342(17) 0.0345(18) 0.0317(18) 0.0011(14) 0.0001(14) 0.0058(14) C37 0.057(2) 0.049(2) 0.053(3) 0.009(2) 0.016(2) 0.0006(19) C38 0.036(2) 0.065(3) 0.046(2) -0.009(2) 0.0019(17) 0.0007(18) C39 0.049(2) 0.047(2) 0.040(2) -0.0094(18) 0.0035(17) -0.0082(18) C40 0.0313(16) 0.0356(18) 0.0328(18) -0.0011(15) -0.0095(14) 0.0007(14) C41 0.0310(16) 0.0261(16) 0.0328(17) -0.0011(14) -0.0061(13) 0.0030(13) C42 0.0437(19) 0.0375(19) 0.039(2) -0.0016(16) -0.0099(16) -0.0042(15) C43 0.055(2) 0.048(2) 0.043(2) -0.0056(18) -0.0185(18) -0.0019(18) C44 0.068(2) 0.045(2) 0.033(2) -0.0076(17) -0.0129(18) 0.0150(19) C45 0.053(2) 0.050(2) 0.035(2) -0.0024(17) 0.0044(17) 0.0099(18) C46 0.0394(18) 0.0342(18) 0.0355(19) -0.0040(15) -0.0004(14) 0.0024(15) C47 0.050(2) 0.052(2) 0.048(2) 0.0036(19) -0.0163(18) -0.0119(18) C48 0.045(2) 0.046(2) 0.045(2) -0.0054(18) -0.0137(17) 0.0125(17) C49 0.051(2) 0.056(2) 0.034(2) 0.0030(18) -0.0023(17) 0.0013(18) C51 0.0255(14) 0.0212(15) 0.0326(17) 0.0020(13) 0.0015(12) -0.0015(12) C52 0.0300(15) 0.0263(16) 0.0353(18) -0.0013(14) -0.0014(13) -0.0026(13) C53 0.0391(18) 0.0354(18) 0.0299(18) -0.0050(14) 0.0007(14) -0.0043(15) C54 0.0453(19) 0.0315(18) 0.045(2) -0.0063(16) 0.0093(16) 0.0013(15) C55 0.056(2) 0.0351(19) 0.046(2) -0.0010(17) 0.0021(18) 0.0130(17) C56 0.0424(18) 0.0311(18) 0.0364(19) 0.0027(15) -0.0012(15) 0.0077(15) C61 0.0242(14) 0.0208(15) 0.0271(16) 0.0015(12) -0.0022(12) 0.0028(12) C62 0.0277(15) 0.0235(16) 0.0337(17) 0.0057(13) -0.0023(13) -0.0016(12) C63 0.0334(16) 0.0258(16) 0.0401(19) 0.0074(14) -0.0068(14) -0.0066(13) C64 0.0373(17) 0.0267(17) 0.0381(19) 0.0019(14) -0.0106(14) -0.0050(14) C65 0.0424(18) 0.0346(18) 0.0281(17) 0.0011(14) -0.0054(14) -0.0023(15) C66 0.0352(16) 0.0269(16) 0.0276(17) 0.0010(13) -0.0015(13) -0.0022(13) C71 0.0337(16) 0.0239(16) 0.0279(17) -0.0009(13) -0.0019(13) 0.0018(13) C72 0.0348(18) 0.047(2) 0.0359(19) 0.0037(16) -0.0061(14) 0.0020(15) C73 0.050(2) 0.057(2) 0.043(2) -0.0033(19) -0.0210(18) 0.0083(18) C74 0.071(3) 0.051(2) 0.032(2) -0.0017(17) -0.0093(19) 0.017(2) C75 0.063(2) 0.052(2) 0.0289(19) 0.0044(17) 0.0071(17) 0.0064(19) C76 0.0403(18) 0.041(2) 0.0346(19) 0.0052(15) 0.0004(15) 0.0005(15) C81 0.0412(18) 0.0233(16) 0.0283(17) 0.0007(13) -0.0034(14) -0.0006(13) C82 0.056(2) 0.041(2) 0.035(2) 0.0042(16) -0.0094(16) 0.0039(17) C83 0.084(3) 0.058(3) 0.038(2) 0.0092(19) -0.020(2) 0.005(2) C84 0.093(3) 0.050(2) 0.029(2) 0.0041(18) -0.005(2) 0.000(2) C85 0.076(3) 0.044(2) 0.041(2) -0.0010(18) 0.017(2) -0.003(2) C86 0.050(2) 0.0358(19) 0.0326(19) 0.0032(15) 0.0066(16) 0.0002(16) B1 0.037(2) 0.039(2) 0.0183(18) -0.0014(16) 0.0000(15) -0.0002(16) F11 0.0391(11) 0.0580(13) 0.0253(10) -0.0021(9) -0.0021(8) 0.0064(9) F12 0.0380(11) 0.0492(12) 0.0377(12) 0.0014(9) -0.0012(9) 0.0001(9) F13 0.0709(15) 0.0510(14) 0.0417(13) -0.0190(11) 0.0008(11) 0.0043(11) F14 0.0606(14) 0.0616(15) 0.0398(12) 0.0153(11) 0.0038(10) -0.0159(12) B2 0.055(3) 0.047(3) 0.043(3) 0.000(2) -0.003(2) -0.001(2) F21 0.132(3) 0.098(2) 0.0545(17) -0.0220(16) -0.0262(17) 0.014(2) F22 0.0493(14) 0.0560(15) 0.108(2) 0.0280(15) -0.0079(14) -0.0051(12) F23 0.0669(16) 0.0673(17) 0.0817(19) 0.0324(15) -0.0153(14) -0.0208(13) F24 0.0463(12) 0.0618(15) 0.0423(13) -0.0002(11) 0.0032(10) -0.0041(10) C1D 0.039(9) 0.052(7) 0.032(3) -0.010(4) 0.006(6) 0.011(5) Cl1 0.0465(14) 0.0550(16) 0.0369(13) 0.0085(10) 0.0063(9) -0.0010(10) Cl2 0.0373(10) 0.081(2) 0.0358(10) -0.0184(10) 0.0023(7) -0.0015(8) Cl3 0.113(2) 0.0464(12) 0.0586(17) -0.0097(11) 0.0338(14) -0.0059(12) C1D' 0.039(14) 0.043(11) 0.034(7) -0.005(9) 0.008(11) 0.008(10) Cl1' 0.129(11) 0.152(13) 0.126(12) 0.036(9) 0.028(8) 0.008(9) Cl2' 0.064(4) 0.38(3) 0.062(5) 0.059(9) -0.017(3) -0.041(9) Cl3' 0.200(16) 0.086(5) 0.099(10) -0.034(6) 0.095(10) -0.047(8) C2D 0.078(3) 0.044(2) 0.037(2) -0.0008(18) -0.002(2) -0.003(2) Cl4 0.0857(10) 0.1235(13) 0.1013(11) -0.0389(10) -0.0380(8) 0.0410(9) Cl5 0.1218(10) 0.0564(7) 0.0355(6) -0.0021(5) 0.0077(6) -0.0008(7) Cl6 0.0558(6) 0.0675(7) 0.0879(9) -0.0284(6) -0.0055(6) 0.0009(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 O2 1.928(2) . ? Cu1 O1 1.935(2) . ? Cu1 O4 1.938(2) . ? Cu1 O3 1.951(2) . ? Cu1 F11 2.2719(19) . ? P1 O1 1.509(2) . ? P1 C1 1.774(3) . ? P1 C11 1.791(3) . ? P1 C31 1.791(3) . ? P2 O2 1.510(2) . ? P2 C2 1.775(3) . ? P2 C21 1.782(3) . ? P2 C41 1.790(3) . ? P3 O3 1.509(2) . ? P3 C1 1.765(3) . ? P3 C51 1.790(3) . ? P3 C71 1.794(3) . ? P4 O4 1.504(2) . ? P4 C2 1.772(3) . ? P4 C61 1.788(3) . ? P4 C81 1.794(3) . ? N4 C4 1.177(4) . ? N4 C40 1.485(4) . ? N3 C3 1.175(4) . ? N3 C30 1.479(4) . ? C1 C3 1.346(4) . ? C2 C4 1.343(4) . ? C11 C16 1.374(5) . ? C11 C12 1.378(5) . ? C12 C13 1.378(6) . ? C12 H12 0.9300 . ? C13 C14 1.377(7) . ? C13 H13 0.9300 . ? C14 C15 1.357(6) . ? C14 H14 0.9300 . ? C15 C16 1.383(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.396(5) . ? C21 C22 1.394(5) . ? C22 C23 1.383(5) . ? C22 H22 0.9300 . ? C23 C24 1.387(5) . ? C23 H23 0.9300 . ? C24 C25 1.380(6) . ? C24 H24 0.9300 . ? C25 C26 1.398(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 C39 1.500(5) . ? C30 C38 1.524(5) . ? C30 C37 1.529(5) . ? C31 C32 1.381(5) . ? C31 C36 1.401(5) . ? C32 C33 1.398(5) . ? C32 H32 0.9300 . ? C33 C34 1.364(6) . ? C33 H33 0.9300 . ? C34 C35 1.377(6) . ? C34 H34 0.9300 . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C47 1.510(5) . ? C40 C49 1.524(5) . ? C40 C48 1.526(5) . ? C41 C46 1.391(5) . ? C41 C42 1.397(5) . ? C42 C43 1.385(5) . ? C42 H42 0.9300 . ? C43 C44 1.373(6) . ? C43 H43 0.9300 . ? C44 C45 1.372(6) . ? C44 H44 0.9300 . ? C45 C46 1.388(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C51 C52 1.398(4) . ? C51 C56 1.395(4) . ? C52 C53 1.394(5) . ? C52 H52 0.9300 . ? C53 C54 1.379(5) . ? C53 H53 0.9300 . ? C54 C55 1.386(5) . ? C54 H54 0.9300 . ? C55 C56 1.389(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C66 1.401(4) . ? C61 C62 1.396(4) . ? C62 C63 1.383(5) . ? C62 H62 0.9300 . ? C63 C64 1.378(5) . ? C63 H63 0.9300 . ? C64 C65 1.393(5) . ? C64 H64 0.9300 . ? C65 C66 1.382(5) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C76 1.381(5) . ? C71 C72 1.401(5) . ? C72 C73 1.379(5) . ? C72 H72 0.9300 . ? C73 C74 1.383(6) . ? C73 H73 0.9300 . ? C74 C75 1.375(6) . ? C74 H74 0.9300 . ? C75 C76 1.385(5) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C82 1.390(5) . ? C81 C86 1.392(5) . ? C82 C83 1.382(6) . ? C82 H82 0.9300 . ? C83 C84 1.363(6) . ? C83 H83 0.9300 . ? C84 C85 1.378(6) . ? C84 H84 0.9300 . ? C85 C86 1.393(5) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? B1 F14 1.370(4) . ? B1 F12 1.383(4) . ? B1 F13 1.382(4) . ? B1 F11 1.415(4) . ? B2 F21 1.363(5) . ? B2 F23 1.379(5) . ? B2 F22 1.387(5) . ? B2 F24 1.396(5) . ? C1D Cl2 1.76(3) . ? C1D Cl1 1.77(3) . ? C1D Cl3 1.69(3) . ? C1D H1D 0.9800 . ? C1D' Cl3' 1.88(8) . ? C1D' Cl2' 1.71(9) . ? C1D' Cl1' 1.74(9) . ? C1D' H1D' 0.9800 . ? C2D Cl6 1.730(4) . ? C2D Cl4 1.738(5) . ? C2D Cl5 1.755(4) . ? C2D H2D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 85.72(9) . . ? O2 Cu1 O4 92.91(9) . . ? O1 Cu1 O4 174.64(10) . . ? O2 Cu1 O3 166.42(9) . . ? O1 Cu1 O3 92.46(9) . . ? O4 Cu1 O3 87.65(9) . . ? O2 Cu1 F11 100.06(8) . . ? O1 Cu1 F11 89.72(9) . . ? O4 Cu1 F11 95.63(8) . . ? O3 Cu1 F11 93.38(8) . . ? O1 P1 C1 111.11(13) . . ? O1 P1 C11 109.25(14) . . ? C1 P1 C11 109.88(15) . . ? O1 P1 C31 111.08(14) . . ? C1 P1 C31 106.82(14) . . ? C11 P1 C31 108.64(15) . . ? O2 P2 C2 110.78(13) . . ? O2 P2 C21 111.17(14) . . ? C2 P2 C21 105.18(14) . . ? O2 P2 C41 108.98(14) . . ? C2 P2 C41 110.37(15) . . ? C21 P2 C41 110.33(15) . . ? O3 P3 C1 111.43(13) . . ? O3 P3 C51 111.87(13) . . ? C1 P3 C51 104.96(14) . . ? O3 P3 C71 108.64(14) . . ? C1 P3 C71 109.51(15) . . ? C51 P3 C71 110.39(14) . . ? O4 P4 C2 110.98(13) . . ? O4 P4 C61 112.92(13) . . ? C2 P4 C61 104.94(14) . . ? O4 P4 C81 109.23(14) . . ? C2 P4 C81 108.09(15) . . ? C61 P4 C81 110.53(15) . . ? C4 N4 C40 143.5(3) . . ? C3 N3 C30 147.2(3) . . ? P1 O1 Cu1 137.30(13) . . ? P2 O2 Cu1 132.00(13) . . ? P3 O3 Cu1 136.94(13) . . ? P4 O4 Cu1 137.86(13) . . ? C3 C1 P3 120.8(2) . . ? C3 C1 P1 119.8(2) . . ? P3 C1 P1 119.36(17) . . ? N3 C3 C1 173.8(4) . . ? C4 C2 P4 120.6(2) . . ? C4 C2 P2 120.5(2) . . ? P4 C2 P2 118.08(16) . . ? N4 C4 C2 173.6(3) . . ? C16 C11 C12 118.9(3) . . ? C16 C11 P1 121.7(3) . . ? C12 C11 P1 119.4(3) . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.7(4) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C26 C21 C22 120.5(3) . . ? C26 C21 P2 122.6(3) . . ? C22 C21 P2 116.8(2) . . ? C23 C22 C21 119.4(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.7(4) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 119.1(3) . . ? C21 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N3 C30 C39 108.6(3) . . ? N3 C30 C38 106.9(3) . . ? C39 C30 C38 110.9(3) . . ? N3 C30 C37 107.1(3) . . ? C39 C30 C37 112.7(3) . . ? C38 C30 C37 110.5(3) . . ? C32 C31 C36 119.7(3) . . ? C32 C31 P1 122.3(3) . . ? C36 C31 P1 118.0(2) . . ? C31 C32 C33 119.9(4) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.2(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.6(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 120.2(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 119.4(3) . . ? C31 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C38 H38A 109.5 . . ? C30 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C30 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C30 C39 H39A 109.5 . . ? C30 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C30 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 C47 106.3(3) . . ? N4 C40 C49 109.6(3) . . ? C47 C40 C49 111.6(3) . . ? N4 C40 C48 105.9(3) . . ? C47 C40 C48 112.3(3) . . ? C49 C40 C48 110.9(3) . . ? C46 C41 C42 119.3(3) . . ? C46 C41 P2 123.1(3) . . ? C42 C41 P2 117.6(3) . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 119.8(3) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C40 C47 H47A 109.5 . . ? C40 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C40 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C40 C48 H48A 109.5 . . ? C40 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C40 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C40 C49 H49A 109.5 . . ? C40 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C40 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 C56 119.9(3) . . ? C52 C51 P3 116.6(2) . . ? C56 C51 P3 123.5(3) . . ? C51 C52 C53 119.8(3) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.4(3) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C54 C55 C56 120.4(3) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C51 119.5(3) . . ? C55 C56 H56 120.2 . . ? C51 C56 H56 120.2 . . ? C66 C61 C62 119.4(3) . . ? C66 C61 P4 117.5(2) . . ? C62 C61 P4 123.0(2) . . ? C63 C62 C61 120.1(3) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.5(3) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 119.8(3) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C66 C65 C64 120.5(3) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C61 119.6(3) . . ? C65 C66 H66 120.2 . . ? C61 C66 H66 120.2 . . ? C76 C71 C72 119.1(3) . . ? C76 C71 P3 119.9(3) . . ? C72 C71 P3 120.9(3) . . ? C73 C72 C71 120.0(4) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C74 C73 C72 120.4(4) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C75 C74 C73 119.8(4) . . ? C75 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C74 C75 C76 120.4(4) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C71 C76 C75 120.4(3) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C82 C81 C86 119.5(3) . . ? C82 C81 P4 118.1(3) . . ? C86 C81 P4 122.1(3) . . ? C83 C82 C81 119.8(4) . . ? C83 C82 H82 120.1 . . ? C81 C82 H82 120.1 . . ? C84 C83 C82 120.8(4) . . ? C84 C83 H83 119.6 . . ? C82 C83 H83 119.6 . . ? C83 C84 C85 120.3(4) . . ? C83 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C84 C85 C86 120.0(4) . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C81 C86 C85 119.7(4) . . ? C81 C86 H86 120.2 . . ? C85 C86 H86 120.2 . . ? F14 B1 F12 110.0(3) . . ? F14 B1 F13 110.9(3) . . ? F12 B1 F13 109.3(3) . . ? F14 B1 F11 108.8(3) . . ? F12 B1 F11 109.3(3) . . ? F13 B1 F11 108.5(3) . . ? B1 F11 Cu1 132.45(19) . . ? F21 B2 F23 111.7(4) . . ? F21 B2 F22 108.7(4) . . ? F23 B2 F22 109.1(4) . . ? F21 B2 F24 109.4(4) . . ? F23 B2 F24 109.4(4) . . ? F22 B2 F24 108.6(4) . . ? Cl2 C1D Cl1 108.0(16) . . ? Cl2 C1D Cl3 111.6(17) . . ? Cl1 C1D Cl3 114.5(15) . . ? Cl2 C1D H1D 107.5 . . ? Cl1 C1D H1D 107.5 . . ? Cl3 C1D H1D 107.5 . . ? Cl3' C1D' Cl2' 103(4) . . ? Cl3' C1D' Cl1' 102(4) . . ? Cl2' C1D' Cl1' 114(4) . . ? Cl3' C1D' H1D' 112.2 . . ? Cl2' C1D' H1D' 112.2 . . ? Cl1' C1D' H1D' 112.2 . . ? Cl6 C2D Cl4 110.0(2) . . ? Cl6 C2D Cl5 111.6(2) . . ? Cl4 C2D Cl5 110.5(3) . . ? Cl6 C2D H2D 108.2 . . ? Cl4 C2D H2D 108.2 . . ? Cl5 C2D H2D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.556 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.068 #==========END #==========END data_13I _database_code_depnum_ccdc_archive 'CCDC 720845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H89 Cu2 N3 O2 P6, 2(C H2 Cl2), 2(B F4)' _chemical_formula_sum 'C92 H93 B2 Cl4 Cu2 F8 N3 O2 P6' _chemical_formula_weight 1901.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 14.212(3) _cell_length_b 40.569(8) _cell_length_c 17.545(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.41(3) _cell_angle_gamma 90.00 _cell_volume 9752(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min 3.124 _cell_measurement_theta_max 15.361 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.791 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133579 _diffrn_reflns_av_R_equivalents 0.1498 _diffrn_reflns_av_sigmaI/netI 0.1349 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17103 _reflns_number_gt 9893 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17103 _refine_ls_number_parameters 1117 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2364 _refine_ls_R_factor_gt 0.1684 _refine_ls_wR_factor_ref 0.4585 _refine_ls_wR_factor_gt 0.4302 _refine_ls_goodness_of_fit_ref 1.470 _refine_ls_restrained_S_all 1.470 _refine_ls_shift/su_max 0.299 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.2187(2) 0.37779(9) 0.33844(17) 0.0265(7) Uani 0.70 1 d P A 1 Cu2 Cu 1.0498(2) 0.39219(10) 0.21668(18) 0.0318(7) Uani 0.70 1 d P A 1 Cu1' Cu 1.1860(7) 0.3805(3) 0.3203(8) 0.102(5) Uani 0.30 1 d P A 2 Cu2' Cu 1.0185(8) 0.3932(3) 0.1926(9) 0.123(6) Uani 0.30 1 d P A 2 P1 P 0.9286(2) 0.36310(8) 0.2531(2) 0.0516(9) Uani 1 1 d . . . P2 P 1.1174(2) 0.33884(7) 0.36842(18) 0.0420(8) Uani 1 1 d . . . P3 P 1.1082(2) 0.37890(8) 0.1126(2) 0.0553(9) Uani 1 1 d . . . P4 P 1.3009(2) 0.38557(8) 0.2457(2) 0.0507(9) Uani 1 1 d . . . P5 P 1.4071(3) 0.35493(8) 0.5071(2) 0.0598(10) Uani 1 1 d . A . P6 P 1.0406(2) 0.44548(8) 0.2575(3) 0.0647(11) Uani 1 1 d . . . N1 N 1.1765(8) 0.4654(2) 0.4759(8) 0.070(3) Uani 1 1 d . . . N2 N 0.8942(7) 0.3155(2) 0.4305(6) 0.054(3) Uani 1 1 d . A . N4 N 1.3258(9) 0.3663(4) 0.0396(8) 0.103(5) Uani 1 1 d . A . O1 O 1.2057(6) 0.42222(19) 0.4005(6) 0.065(3) Uani 1 1 d . . . O5 O 1.3453(5) 0.3629(2) 0.4328(6) 0.065(3) Uani 1 1 d . . . C1 C 0.9857(7) 0.3435(3) 0.3430(7) 0.045(3) Uani 1 1 d . A . C2 C 0.9371(8) 0.3291(3) 0.3927(8) 0.051(3) Uani 1 1 d . . . C3 C 1.2397(9) 0.3800(3) 0.1558(12) 0.090(6) Uani 1 1 d . A . C4 C 1.2868(10) 0.3712(4) 0.0921(10) 0.084(5) Uani 1 1 d . . . C5 C 1.0519(10) 0.4491(3) 0.3608(10) 0.074(4) Uani 1 1 d . A . H5A H 1.0284 0.4712 0.3709 0.089 Uiso 1 1 calc R . . H5B H 1.0079 0.4327 0.3752 0.089 Uiso 1 1 calc R . . C6 C 1.1527(10) 0.4444(3) 0.4151(10) 0.068(4) Uani 1 1 d . A . C11 C 1.1489(8) 0.3345(3) 0.4750(8) 0.050(3) Uani 1 1 d . A . C12 C 1.1910(9) 0.3066(3) 0.5169(8) 0.053(3) Uani 1 1 d . . . H12 H 1.2004 0.2875 0.4887 0.063 Uiso 1 1 calc R A . C13 C 1.2194(10) 0.3062(4) 0.5986(8) 0.064(4) Uani 1 1 d . A . H13 H 1.2497 0.2872 0.6262 0.076 Uiso 1 1 calc R . . C14 C 1.2038(12) 0.3328(4) 0.6385(9) 0.076(4) Uani 1 1 d . . . H14 H 1.2247 0.3328 0.6946 0.091 Uiso 1 1 calc R A . C15 C 1.1573(11) 0.3605(3) 0.5985(10) 0.077(5) Uani 1 1 d . A . H15 H 1.1433 0.3787 0.6278 0.092 Uiso 1 1 calc R . . C16 C 1.1317(9) 0.3617(3) 0.5184(8) 0.056(3) Uani 1 1 d . . . H16 H 1.1022 0.3810 0.4918 0.067 Uiso 1 1 calc R A . C20 C 0.8613(10) 0.3188(3) 0.5054(9) 0.067(4) Uani 1 1 d . . . C21 C 0.8275(9) 0.3861(3) 0.2724(9) 0.057(4) Uani 1 1 d . A . C22 C 0.8346(10) 0.3991(3) 0.3469(9) 0.063(4) Uani 1 1 d . . . H22 H 0.8902 0.3939 0.3890 0.076 Uiso 1 1 calc R A . C23 C 0.7622(10) 0.4194(3) 0.3613(10) 0.068(4) Uani 1 1 d . A . H23 H 0.7687 0.4282 0.4126 0.081 Uiso 1 1 calc R . . C24 C 0.6837(11) 0.4263(3) 0.3024(11) 0.066(4) Uani 1 1 d . . . H24 H 0.6353 0.4406 0.3123 0.079 Uiso 1 1 calc R A . C25 C 0.6708(9) 0.4134(4) 0.2273(10) 0.071(4) Uani 1 1 d . A . H25 H 0.6126 0.4175 0.1869 0.086 Uiso 1 1 calc R . . C26 C 0.7476(9) 0.3933(3) 0.2119(8) 0.059(3) Uani 1 1 d . . . H26 H 0.7426 0.3852 0.1602 0.071 Uiso 1 1 calc R A . C27 C 0.7535(11) 0.3090(5) 0.4833(10) 0.098(6) Uani 1 1 d . A . H27A H 0.7161 0.3243 0.4433 0.146 Uiso 1 1 calc R . . H27B H 0.7289 0.3099 0.5304 0.146 Uiso 1 1 calc R . . H27C H 0.7465 0.2865 0.4619 0.146 Uiso 1 1 calc R . . C28 C 0.8651(15) 0.3543(4) 0.5288(12) 0.119(8) Uani 1 1 d . A . H28A H 0.8237 0.3672 0.4855 0.179 Uiso 1 1 calc R . . H28B H 0.9325 0.3622 0.5400 0.179 Uiso 1 1 calc R . . H28C H 0.8416 0.3567 0.5762 0.179 Uiso 1 1 calc R . . C29 C 0.9243(12) 0.2961(4) 0.5657(8) 0.081(5) Uani 1 1 d . A . H29A H 0.9176 0.2735 0.5451 0.122 Uiso 1 1 calc R . . H29B H 0.9037 0.2970 0.6147 0.122 Uiso 1 1 calc R . . H29C H 0.9926 0.3030 0.5764 0.122 Uiso 1 1 calc R . . C31 C 1.1330(9) 0.2977(3) 0.3328(7) 0.048(3) Uani 1 1 d . A . C32 C 1.0618(10) 0.2753(3) 0.3038(7) 0.058(3) Uani 1 1 d . . . H32 H 0.9956 0.2814 0.2973 0.069 Uiso 1 1 calc R A . C33 C 1.0836(11) 0.2432(3) 0.2830(8) 0.063(4) Uani 1 1 d . A . H33 H 1.0324 0.2277 0.2645 0.076 Uiso 1 1 calc R . . C34 C 1.1789(12) 0.2341(3) 0.2893(8) 0.071(4) Uani 1 1 d . . . H34 H 1.1934 0.2129 0.2728 0.085 Uiso 1 1 calc R A . C35 C 1.2522(11) 0.2561(3) 0.3197(8) 0.065(4) Uani 1 1 d . A . H35 H 1.3178 0.2493 0.3261 0.078 Uiso 1 1 calc R . . C36 C 1.2347(9) 0.2882(3) 0.3417(7) 0.054(3) Uani 1 1 d . . . H36 H 1.2867 0.3032 0.3617 0.065 Uiso 1 1 calc R A . C41 C 0.8631(8) 0.3330(4) 0.1837(7) 0.060(3) Uani 1 1 d . A . C42 C 0.8630(13) 0.3340(6) 0.1055(12) 0.109(7) Uani 1 1 d . . . H42 H 0.9030 0.3506 0.0921 0.131 Uiso 1 1 calc R A . C43 C 0.8146(13) 0.3150(6) 0.0449(14) 0.119(7) Uani 1 1 d . A . H43 H 0.8125 0.3191 -0.0089 0.143 Uiso 1 1 calc R . . C44 C 0.7682(14) 0.2886(5) 0.0700(14) 0.115(7) Uani 1 1 d . . . H44 H 0.7387 0.2718 0.0339 0.137 Uiso 1 1 calc R A . C45 C 0.7653(13) 0.2872(6) 0.1495(13) 0.108(7) Uani 1 1 d . A . H45 H 0.7246 0.2706 0.1621 0.129 Uiso 1 1 calc R . . C46 C 0.8130(13) 0.3063(4) 0.2094(11) 0.092(5) Uani 1 1 d . . . H46 H 0.8136 0.3027 0.2630 0.111 Uiso 1 1 calc R A . C50 C 1.0820(8) 0.3389(3) 0.0635(7) 0.051(3) Uani 1 1 d . A . C51 C 1.3661(16) 0.3417(8) -0.0014(12) 0.131(9) Uani 1 1 d . . . C52 C 1.3348(15) 0.3109(7) 0.0112(15) 0.134(9) Uani 1 1 d . A . H52A H 1.2636 0.3099 -0.0083 0.201 Uiso 1 1 calc R . . H52B H 1.3544 0.3061 0.0679 0.201 Uiso 1 1 calc R . . H52C H 1.3641 0.2947 -0.0170 0.201 Uiso 1 1 calc R . . C53 C 1.339(2) 0.3526(9) -0.0826(16) 0.234(19) Uani 1 1 d . A . H53A H 1.2672 0.3528 -0.1023 0.351 Uiso 1 1 calc R . . H53B H 1.3660 0.3376 -0.1148 0.351 Uiso 1 1 calc R . . H53C H 1.3637 0.3749 -0.0859 0.351 Uiso 1 1 calc R . . C54 C 1.4767(14) 0.3432(5) 0.0355(16) 0.156(11) Uani 1 1 d . A . H54A H 1.4900 0.3447 0.0931 0.234 Uiso 1 1 calc R . . H54B H 1.5036 0.3627 0.0155 0.234 Uiso 1 1 calc R . . H54C H 1.5073 0.3233 0.0214 0.234 Uiso 1 1 calc R . . C55 C 1.0556(11) 0.3345(4) -0.0171(10) 0.075(4) Uani 1 1 d . . . H55 H 1.0482 0.3536 -0.0495 0.090 Uiso 1 1 calc R A . C56 C 1.0399(11) 0.3055(6) -0.0525(9) 0.100(7) Uani 1 1 d . A . H56 H 1.0218 0.3040 -0.1086 0.120 Uiso 1 1 calc R . . C57 C 1.0514(12) 0.2743(4) -0.0016(10) 0.082(5) Uani 1 1 d . . . H57 H 1.0408 0.2529 -0.0239 0.099 Uiso 1 1 calc R A . C58 C 1.0779(11) 0.2796(3) 0.0779(10) 0.075(4) Uani 1 1 d . A . H58 H 1.0869 0.2611 0.1123 0.089 Uiso 1 1 calc R . . C59 C 1.0921(10) 0.3110(3) 0.1103(8) 0.058(3) Uani 1 1 d . . . H59 H 1.1093 0.3134 0.1661 0.069 Uiso 1 1 calc R A . C61 C 0.9195(9) 0.4628(3) 0.2127(10) 0.070(4) Uani 1 1 d . A . C62 C 0.8773(12) 0.4868(5) 0.2465(13) 0.112(7) Uani 1 1 d . . . H62 H 0.9096 0.4962 0.2963 0.135 Uiso 1 1 calc R A . C63 C 0.787(2) 0.4969(8) 0.206(2) 0.157(12) Uani 1 1 d . A . H63 H 0.7530 0.5098 0.2349 0.189 Uiso 1 1 calc R . . C64 C 0.7410(16) 0.4918(8) 0.135(2) 0.133(12) Uani 1 1 d . . . H64 H 0.6855 0.5042 0.1084 0.159 Uiso 1 1 calc R A . C65 C 0.7801(19) 0.4656(8) 0.1001(14) 0.168(14) Uani 1 1 d . A . H65 H 0.7437 0.4565 0.0513 0.202 Uiso 1 1 calc R . . C66 C 0.8730(13) 0.4531(5) 0.1376(10) 0.093(5) Uani 1 1 d . . . H66 H 0.9036 0.4379 0.1107 0.112 Uiso 1 1 calc R A . C71 C 1.0765(10) 0.4082(4) 0.0328(8) 0.073(4) Uani 1 1 d . A . C72 C 1.1420(12) 0.4297(5) 0.0124(11) 0.103(6) Uani 1 1 d . . . H72 H 1.2101 0.4270 0.0352 0.124 Uiso 1 1 calc R A . C73 C 1.1081(16) 0.4549(5) -0.0409(13) 0.136(9) Uani 1 1 d . A . H73 H 1.1537 0.4700 -0.0522 0.163 Uiso 1 1 calc R . . C74 C 1.0136(16) 0.4587(6) -0.0769(13) 0.131(8) Uani 1 1 d . . . H74 H 0.9920 0.4763 -0.1128 0.157 Uiso 1 1 calc R A . C75 C 0.9478(16) 0.4366(7) -0.0611(17) 0.182(13) Uani 1 1 d . A . H75 H 0.8818 0.4373 -0.0921 0.219 Uiso 1 1 calc R . . C76 C 0.9748(14) 0.4137(5) -0.0019(12) 0.127(8) Uani 1 1 d . . . H76 H 0.9270 0.4017 0.0157 0.153 Uiso 1 1 calc R A . C80 C 1.2704(12) 0.4668(4) 0.5428(11) 0.085(5) Uani 1 1 d . . . C81 C 1.3650(8) 0.4245(3) 0.2475(8) 0.052(3) Uani 1 1 d . A . C82 C 1.3762(8) 0.4448(4) 0.3096(9) 0.066(4) Uani 1 1 d . . . H82 H 1.3504 0.4379 0.3517 0.079 Uiso 1 1 calc R A . C83 C 1.4217(9) 0.4747(3) 0.3166(10) 0.075(4) Uani 1 1 d . A . H83 H 1.4241 0.4886 0.3606 0.090 Uiso 1 1 calc R . . C84 C 1.4654(10) 0.4843(4) 0.2567(12) 0.078(5) Uani 1 1 d . . . H84 H 1.5021 0.5041 0.2620 0.093 Uiso 1 1 calc R A . C85 C 1.4549(12) 0.4651(4) 0.1907(13) 0.097(6) Uani 1 1 d . A . H85 H 1.4760 0.4726 0.1467 0.116 Uiso 1 1 calc R . . C86 C 1.4122(10) 0.4341(4) 0.1903(11) 0.091(5) Uani 1 1 d . . . H86 H 1.4153 0.4189 0.1497 0.109 Uiso 1 1 calc R A . C87 C 1.2566(13) 0.4936(5) 0.5909(14) 0.134(9) Uani 1 1 d . . . H87A H 1.2428 0.5137 0.5588 0.201 Uiso 1 1 calc R . . H87B H 1.3159 0.4968 0.6340 0.201 Uiso 1 1 calc R . . H87C H 1.2016 0.4888 0.6130 0.201 Uiso 1 1 calc R . . C88 C 1.2881(16) 0.4335(4) 0.5824(10) 0.110(6) Uani 1 1 d . . . H88A H 1.2973 0.4170 0.5442 0.165 Uiso 1 1 calc R . . H88B H 1.2317 0.4274 0.6016 0.165 Uiso 1 1 calc R . . H88C H 1.3466 0.4345 0.6270 0.165 Uiso 1 1 calc R . . C89 C 1.3506(14) 0.4760(6) 0.5008(13) 0.127(7) Uani 1 1 d . . . H89A H 1.3583 0.4579 0.4660 0.190 Uiso 1 1 calc R . . H89B H 1.4126 0.4798 0.5405 0.190 Uiso 1 1 calc R . . H89C H 1.3312 0.4960 0.4694 0.190 Uiso 1 1 calc R . . C91 C 1.3990(10) 0.3557(3) 0.2553(8) 0.058(3) Uani 1 1 d . A . C92 C 1.4990(11) 0.3641(3) 0.2831(10) 0.077(5) Uani 1 1 d . . . H92 H 1.5165 0.3862 0.2984 0.092 Uiso 1 1 calc R A . C93 C 1.5716(10) 0.3409(3) 0.2885(10) 0.074(4) Uani 1 1 d . A . H93 H 1.6377 0.3480 0.3043 0.088 Uiso 1 1 calc R . . C94 C 1.5525(11) 0.3089(4) 0.2724(8) 0.071(4) Uani 1 1 d . . . H94 H 1.6038 0.2932 0.2799 0.085 Uiso 1 1 calc R A . C95 C 1.4508(13) 0.2988(3) 0.2432(9) 0.081(5) Uani 1 1 d . A . H95 H 1.4338 0.2766 0.2283 0.097 Uiso 1 1 calc R . . C96 C 1.3788(9) 0.3230(3) 0.2380(7) 0.059(3) Uani 1 1 d . . . H96 H 1.3123 0.3164 0.2215 0.071 Uiso 1 1 calc R A . C101 C 1.5103(12) 0.3808(3) 0.5335(9) 0.078(5) Uani 1 1 d D . . C102 C 1.5247(11) 0.4039(4) 0.4863(12) 0.112(7) Uani 1 1 d D A . H102 H 1.4776 0.4069 0.4371 0.134 Uiso 1 1 calc R . . C103 C 1.6069(12) 0.4246(4) 0.5050(13) 0.096(6) Uani 1 1 d D . . H103 H 1.6150 0.4403 0.4671 0.115 Uiso 1 1 calc R A . C104 C 1.6720(19) 0.4229(6) 0.5727(15) 0.169(13) Uani 1 1 d D A . H104 H 1.7207 0.4394 0.5888 0.203 Uiso 1 1 calc R . . C105 C 1.6678(16) 0.3975(6) 0.6177(16) 0.156(10) Uani 1 1 d D . . H105 H 1.7212 0.3932 0.6623 0.187 Uiso 1 1 calc R A . C106 C 1.5870(14) 0.3768(5) 0.6018(10) 0.116(7) Uani 1 1 d D A . H106 H 1.5838 0.3596 0.6379 0.140 Uiso 1 1 calc R . . C111 C 1.4561(8) 0.3139(3) 0.5154(8) 0.058(3) Uani 1 1 d D . . C112 C 1.4833(8) 0.3006(3) 0.4505(8) 0.055(3) Uani 1 1 d D A . H112 H 1.4770 0.3136 0.4044 0.066 Uiso 1 1 calc R . . C113 C 1.5184(10) 0.2695(3) 0.4526(10) 0.081(5) Uani 1 1 d D . . H113 H 1.5368 0.2609 0.4083 0.097 Uiso 1 1 calc R A . C114 C 1.5275(10) 0.2504(4) 0.5195(12) 0.084(5) Uani 1 1 d D A . H114 H 1.5485 0.2281 0.5200 0.100 Uiso 1 1 calc R . . C115 C 1.5066(12) 0.2633(4) 0.5840(11) 0.089(5) Uani 1 1 d D . . H115 H 1.5171 0.2504 0.6307 0.107 Uiso 1 1 calc R A . C116 C 1.4712(11) 0.2940(4) 0.5834(9) 0.075(4) Uani 1 1 d D A . H116 H 1.4563 0.3025 0.6293 0.091 Uiso 1 1 calc R . . C121 C 1.1238(10) 0.4791(4) 0.2418(11) 0.081(5) Uani 1 1 d . A . C122 C 1.1698(11) 0.4754(4) 0.1860(12) 0.097(6) Uani 1 1 d . . . H122 H 1.1662 0.4553 0.1579 0.116 Uiso 1 1 calc R A . C123 C 1.2253(12) 0.5027(6) 0.1692(14) 0.106(7) Uani 1 1 d . A . H123 H 1.2570 0.5000 0.1282 0.128 Uiso 1 1 calc R . . C124 C 1.2340(14) 0.5278(6) 0.2024(14) 0.100(7) Uani 1 1 d . . . H124 H 1.2707 0.5449 0.1869 0.120 Uiso 1 1 calc R A . C125 C 1.1886(14) 0.5336(5) 0.2686(13) 0.112(7) Uani 1 1 d . A . H125 H 1.1970 0.5535 0.2981 0.135 Uiso 1 1 calc R . . C126 C 1.1342(12) 0.5080(4) 0.2833(9) 0.079(4) Uani 1 1 d . . . H126 H 1.1020 0.5103 0.3241 0.095 Uiso 1 1 calc R A . B1 B 0.5025(13) 0.3005(5) 0.7987(9) 0.060(4) Uani 1 1 d . . . B2 B 0.9699(15) 0.4438(6) 0.5688(17) 0.101(8) Uani 1 1 d . . . F11 F 0.9836(13) 0.4776(3) 0.5563(11) 0.182(7) Uani 1 1 d . . . F12 F 0.9857(8) 0.4272(2) 0.5087(8) 0.123(4) Uani 1 1 d . . . F13 F 0.9040(11) 0.4357(5) 0.5985(10) 0.203(8) Uani 1 1 d . . . F14 F 1.0532(13) 0.4434(6) 0.6401(13) 0.240(10) Uani 1 1 d . . . F21 F 0.4106(10) 0.2985(4) 0.7909(11) 0.198(7) Uani 1 1 d . . . F22 F 0.5464(9) 0.3061(3) 0.8784(7) 0.128(4) Uani 1 1 d . . . F23 F 0.5226(9) 0.3296(3) 0.7622(7) 0.131(4) Uani 1 1 d . . . F24 F 0.5410(11) 0.2754(3) 0.7789(7) 0.151(5) Uani 1 1 d . . . C1D C 0.759(2) 0.2005(9) 0.311(2) 0.26(2) Uani 1 1 d . . . H1D1 H 0.7849 0.1843 0.3539 0.308 Uiso 1 1 calc R . . H1D2 H 0.6870 0.2005 0.2998 0.308 Uiso 1 1 calc R . . Cl1 Cl 0.8055(5) 0.24040(14) 0.3426(4) 0.142(2) Uani 1 1 d . . . Cl2 Cl 0.7929(11) 0.1895(2) 0.2286(7) 0.281(7) Uani 1 1 d . . . C2D C 0.667(2) 0.3833(9) 0.914(2) 0.116(12) Uani 0.60 1 d P B 3 H2D1 H 0.6055 0.3859 0.8715 0.139 Uiso 0.60 1 calc PR B 3 H2D2 H 0.6612 0.3621 0.9402 0.139 Uiso 0.60 1 calc PR B 3 Cl3 Cl 0.6653(17) 0.4076(6) 0.9690(14) 0.303(13) Uani 0.60 1 d P B 3 Cl4 Cl 0.7500(13) 0.3778(4) 0.8697(10) 0.222(8) Uani 0.60 1 d P B 3 C3D C 1.028(4) 0.3994(13) 0.7636(16) 0.17(3) Uani 0.40 1 d P . 4 H3D1 H 1.0047 0.4157 0.7962 0.207 Uiso 0.40 1 calc PR . 4 H3D2 H 1.0061 0.4070 0.7081 0.207 Uiso 0.40 1 calc PR . 4 Cl5 Cl 1.1591(12) 0.4013(5) 0.7920(6) 0.197(10) Uani 0.40 1 d P . 4 Cl6 Cl 1.978(3) 0.3679(5) 0.7686(7) 0.35(3) Uani 0.40 1 d P . 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0148(13) 0.0294(15) 0.0386(11) 0.0022(9) 0.0128(10) 0.0050(11) Cu2 0.0241(14) 0.0339(16) 0.0414(11) 0.0120(10) 0.0154(10) 0.0130(12) Cu1' 0.077(7) 0.050(4) 0.230(14) 0.062(6) 0.132(9) 0.046(5) Cu2' 0.104(9) 0.055(5) 0.275(17) 0.086(9) 0.166(11) 0.056(6) P1 0.0464(18) 0.0444(18) 0.079(2) 0.0105(16) 0.0432(17) 0.0100(14) P2 0.0430(16) 0.0376(16) 0.0573(19) 0.0015(14) 0.0340(15) -0.0001(13) P3 0.0544(19) 0.059(2) 0.068(2) 0.0255(17) 0.0428(17) 0.0189(16) P4 0.0488(18) 0.0432(18) 0.074(2) 0.0102(16) 0.0402(18) 0.0029(14) P5 0.064(2) 0.049(2) 0.081(3) -0.0050(18) 0.043(2) -0.0097(17) P6 0.055(2) 0.0373(17) 0.119(3) 0.0169(18) 0.054(2) 0.0081(15) N1 0.070(8) 0.026(5) 0.130(10) -0.023(6) 0.056(8) -0.008(5) N2 0.061(6) 0.044(6) 0.075(7) 0.003(5) 0.047(6) -0.004(5) N4 0.059(8) 0.177(15) 0.091(10) -0.001(9) 0.052(8) 0.018(9) O1 0.067(6) 0.038(5) 0.108(7) -0.019(5) 0.056(5) -0.002(4) O5 0.031(4) 0.052(5) 0.118(8) 0.013(5) 0.030(5) 0.013(4) C1 0.029(5) 0.046(6) 0.075(8) 0.009(6) 0.038(6) -0.002(5) C2 0.047(7) 0.041(7) 0.079(9) -0.006(6) 0.043(7) 0.001(5) C3 0.026(6) 0.055(8) 0.200(19) 0.056(10) 0.053(9) 0.016(6) C4 0.044(8) 0.127(14) 0.094(12) 0.015(10) 0.042(8) 0.012(8) C5 0.070(9) 0.021(6) 0.143(14) -0.008(7) 0.048(10) 0.010(6) C6 0.063(9) 0.020(6) 0.139(14) 0.007(7) 0.061(9) -0.006(6) C11 0.045(7) 0.042(7) 0.078(9) -0.005(6) 0.042(6) -0.010(5) C12 0.060(8) 0.033(6) 0.078(10) 0.005(6) 0.039(7) -0.003(6) C13 0.070(9) 0.061(9) 0.067(10) 0.009(7) 0.032(7) -0.015(7) C14 0.102(12) 0.056(9) 0.080(10) 0.004(8) 0.040(9) -0.037(9) C15 0.107(12) 0.047(8) 0.101(12) -0.021(8) 0.070(10) -0.031(8) C16 0.073(9) 0.046(7) 0.063(9) -0.008(6) 0.043(7) -0.013(6) C20 0.081(9) 0.060(8) 0.091(10) 0.002(7) 0.075(9) -0.006(7) C21 0.049(7) 0.048(7) 0.095(10) 0.024(7) 0.056(8) 0.007(6) C22 0.062(8) 0.037(7) 0.115(12) -0.015(7) 0.069(8) -0.016(6) C23 0.057(9) 0.030(6) 0.131(13) -0.009(7) 0.051(9) 0.003(6) C24 0.064(9) 0.024(6) 0.134(14) 0.000(7) 0.068(10) 0.009(6) C25 0.049(8) 0.070(9) 0.108(12) 0.039(9) 0.043(8) 0.017(7) C26 0.042(7) 0.073(9) 0.073(9) 0.012(7) 0.034(7) 0.012(7) C27 0.070(10) 0.129(15) 0.119(14) 0.019(11) 0.069(10) -0.011(10) C28 0.19(2) 0.070(11) 0.158(17) -0.038(11) 0.148(17) -0.024(12) C29 0.106(12) 0.093(11) 0.057(9) 0.009(8) 0.044(9) -0.004(10) C31 0.060(8) 0.050(7) 0.047(7) -0.006(6) 0.038(6) 0.001(6) C32 0.075(9) 0.048(7) 0.064(8) -0.013(6) 0.043(7) -0.004(7) C33 0.087(10) 0.051(8) 0.063(9) -0.014(6) 0.040(8) -0.001(7) C34 0.102(12) 0.047(8) 0.081(10) -0.015(7) 0.053(9) 0.010(8) C35 0.078(9) 0.049(8) 0.089(10) 0.011(7) 0.056(8) 0.030(8) C36 0.048(7) 0.058(8) 0.071(8) 0.014(6) 0.041(6) 0.014(6) C41 0.040(7) 0.090(10) 0.055(8) 0.002(7) 0.023(6) 0.022(7) C42 0.081(12) 0.162(19) 0.113(15) -0.029(14) 0.077(12) -0.019(12) C43 0.074(12) 0.17(2) 0.121(17) -0.024(16) 0.041(12) -0.034(13) C44 0.091(14) 0.110(16) 0.15(2) -0.048(14) 0.041(14) 0.007(12) C45 0.072(11) 0.131(17) 0.118(16) 0.053(14) 0.020(12) -0.004(11) C46 0.102(13) 0.073(11) 0.092(12) -0.005(9) 0.010(11) -0.045(10) C50 0.046(7) 0.058(8) 0.053(8) 0.015(6) 0.019(6) 0.013(6) C51 0.102(16) 0.23(3) 0.076(13) -0.020(17) 0.057(12) 0.068(18) C52 0.073(13) 0.17(2) 0.14(2) -0.043(19) 0.006(13) 0.023(15) C53 0.24(3) 0.35(5) 0.14(2) 0.02(3) 0.10(2) 0.19(3) C54 0.098(15) 0.129(18) 0.28(3) -0.086(19) 0.127(19) -0.028(13) C55 0.068(9) 0.091(12) 0.075(11) 0.022(9) 0.037(8) 0.014(9) C56 0.065(10) 0.19(2) 0.047(9) -0.033(12) 0.012(8) -0.010(12) C57 0.088(11) 0.080(11) 0.074(11) -0.011(9) 0.014(9) 0.019(9) C58 0.089(11) 0.049(8) 0.081(11) 0.008(7) 0.014(9) 0.019(8) C59 0.078(9) 0.042(7) 0.068(9) 0.010(6) 0.047(7) 0.015(6) C61 0.043(7) 0.064(9) 0.114(13) 0.035(8) 0.041(9) 0.011(7) C62 0.059(10) 0.114(15) 0.160(18) -0.017(13) 0.022(11) 0.053(10) C63 0.10(2) 0.18(3) 0.21(3) -0.01(3) 0.09(2) 0.04(2) C64 0.059(14) 0.16(2) 0.21(3) 0.08(2) 0.091(19) 0.038(15) C65 0.113(19) 0.23(3) 0.119(19) 0.11(2) -0.050(16) -0.07(2) C66 0.085(12) 0.120(15) 0.069(11) 0.028(10) 0.011(10) 0.028(11) C71 0.077(10) 0.077(9) 0.079(10) 0.059(8) 0.045(8) 0.035(8) C72 0.075(11) 0.122(14) 0.130(15) 0.081(12) 0.056(11) 0.032(10) C73 0.107(16) 0.16(2) 0.17(2) 0.112(17) 0.078(15) 0.029(14) C74 0.092(15) 0.17(2) 0.145(19) 0.071(16) 0.049(14) 0.012(15) C75 0.082(14) 0.22(3) 0.23(3) 0.16(2) 0.009(16) 0.031(16) C76 0.087(13) 0.147(18) 0.135(17) 0.107(15) 0.008(12) 0.008(12) C80 0.087(12) 0.056(9) 0.129(14) -0.034(9) 0.056(11) -0.025(8) C81 0.043(7) 0.048(7) 0.069(9) 0.022(7) 0.024(6) -0.002(6) C82 0.025(6) 0.085(10) 0.096(11) 0.027(9) 0.033(7) 0.002(6) C83 0.039(7) 0.060(9) 0.132(14) 0.006(9) 0.035(8) -0.008(7) C84 0.048(8) 0.045(8) 0.142(15) 0.026(9) 0.030(9) -0.001(7) C85 0.086(12) 0.069(11) 0.153(18) 0.039(12) 0.061(12) -0.011(9) C86 0.057(9) 0.098(12) 0.129(14) 0.027(10) 0.047(10) 0.001(9) C87 0.083(12) 0.118(15) 0.22(2) -0.108(16) 0.078(14) -0.046(11) C88 0.168(19) 0.087(13) 0.080(12) -0.006(10) 0.043(12) 0.005(13) C89 0.102(14) 0.149(19) 0.151(19) -0.013(15) 0.072(14) -0.027(13) C91 0.074(9) 0.035(7) 0.086(10) 0.000(6) 0.059(8) 0.004(6) C92 0.089(11) 0.033(7) 0.139(14) 0.024(8) 0.083(10) 0.010(7) C93 0.057(8) 0.054(9) 0.131(13) 0.027(8) 0.062(9) 0.019(7) C94 0.066(10) 0.083(11) 0.077(10) 0.025(8) 0.042(8) 0.023(8) C95 0.126(14) 0.042(8) 0.090(11) -0.012(7) 0.057(10) 0.032(9) C96 0.061(8) 0.059(8) 0.069(9) 0.001(6) 0.038(7) -0.002(6) C101 0.109(12) 0.066(9) 0.067(10) 0.005(7) 0.039(9) -0.040(9) C102 0.053(9) 0.118(15) 0.169(19) 0.025(14) 0.035(11) -0.026(10) C103 0.074(11) 0.073(11) 0.151(18) 0.022(11) 0.047(12) -0.034(9) C104 0.18(3) 0.15(2) 0.13(2) 0.017(17) -0.036(18) -0.12(2) C105 0.087(15) 0.16(2) 0.19(3) 0.05(2) -0.019(16) -0.008(16) C106 0.117(15) 0.126(16) 0.075(12) -0.017(10) -0.029(11) -0.064(13) C111 0.059(8) 0.046(7) 0.086(10) -0.017(7) 0.047(7) -0.022(6) C112 0.052(7) 0.050(7) 0.073(9) 0.002(6) 0.034(7) 0.000(6) C113 0.101(12) 0.039(8) 0.121(14) -0.023(8) 0.059(10) -0.018(8) C114 0.072(10) 0.048(8) 0.155(17) 0.004(10) 0.071(11) 0.001(7) C115 0.083(11) 0.084(12) 0.106(14) 0.043(10) 0.034(10) 0.016(10) C116 0.082(10) 0.083(11) 0.069(10) 0.002(8) 0.032(8) -0.009(9) C121 0.051(8) 0.058(9) 0.152(15) 0.016(10) 0.059(10) 0.026(7) C122 0.064(10) 0.081(11) 0.156(17) 0.050(11) 0.051(11) 0.017(9) C123 0.058(10) 0.117(16) 0.150(19) 0.075(16) 0.037(11) 0.025(12) C124 0.078(12) 0.081(13) 0.145(19) 0.037(13) 0.038(12) 0.025(11) C125 0.107(14) 0.079(12) 0.126(16) 0.036(11) -0.011(13) -0.032(11) C126 0.091(11) 0.068(10) 0.078(11) 0.006(8) 0.025(9) -0.012(9) B1 0.070(11) 0.084(12) 0.033(8) -0.012(8) 0.028(8) -0.014(9) B2 0.057(11) 0.101(17) 0.16(2) -0.046(15) 0.060(15) -0.005(11) F11 0.253(17) 0.061(7) 0.303(19) -0.027(9) 0.195(16) 0.011(9) F12 0.129(8) 0.047(5) 0.231(12) -0.033(6) 0.115(9) -0.010(5) F13 0.152(12) 0.267(19) 0.231(16) -0.083(14) 0.125(12) -0.100(13) F14 0.146(14) 0.34(3) 0.25(2) -0.11(2) 0.070(15) -0.013(16) F21 0.107(10) 0.221(17) 0.245(18) 0.001(13) 0.011(11) -0.060(11) F22 0.153(10) 0.120(9) 0.120(9) -0.001(7) 0.051(8) -0.022(8) F23 0.171(11) 0.106(8) 0.120(8) 0.002(6) 0.045(8) -0.065(8) F24 0.204(14) 0.141(11) 0.120(10) -0.035(8) 0.062(9) -0.042(10) C1D 0.24(3) 0.26(4) 0.34(5) -0.21(4) 0.20(3) -0.16(3) Cl1 0.186(6) 0.108(4) 0.136(5) -0.006(3) 0.050(4) -0.016(4) Cl2 0.471(18) 0.196(9) 0.269(11) -0.112(8) 0.261(13) -0.083(10) C2D 0.076(18) 0.13(3) 0.16(3) -0.07(2) 0.07(2) -0.003(18) Cl3 0.36(3) 0.29(2) 0.31(2) -0.17(2) 0.19(2) -0.16(2) Cl4 0.270(18) 0.170(12) 0.218(14) 0.007(10) 0.051(13) -0.130(13) C3D 0.22(5) 0.21(5) 0.002(15) -0.03(2) -0.10(2) 0.18(5) Cl5 0.194(15) 0.31(2) 0.037(6) -0.054(9) -0.060(7) 0.176(16) Cl6 0.78(7) 0.207(19) 0.025(6) 0.025(8) 0.023(15) -0.27(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 2.138(8) . ? Cu1 O5 2.181(9) . ? Cu1 P2 2.291(5) . ? Cu1 P4 2.264(4) . ? Cu1 Cu2 2.818(4) . ? Cu2 P3 2.263(5) . ? Cu2 P1 2.315(5) . ? Cu2 P6 2.292(5) . ? Cu1' P4 2.358(10) . ? Cu1' P2 2.226(11) . ? Cu1' Cu2' 2.849(18) . ? Cu1' P3 3.517(15) . ? Cu2' P3 2.211(12) . ? Cu2' P1 2.231(11) . ? Cu2' P6 2.387(16) . ? P1 C1 1.760(12) . ? P1 C41 1.799(14) . ? P1 C21 1.819(11) . ? P2 C11 1.812(13) . ? P2 C1 1.815(10) . ? P2 C31 1.817(11) . ? P3 C3 1.821(13) . ? P3 C71 1.800(11) . ? P3 C50 1.829(13) . ? P4 C3 1.60(2) . ? P4 C91 1.822(12) . ? P4 C81 1.818(12) . ? P5 O5 1.403(10) . ? P5 C101 1.763(15) . ? P5 C111 1.797(13) . ? P6 C61 1.832(14) . ? P6 C5 1.783(16) . ? P6 C121 1.872(15) . ? N1 C6 1.337(18) . ? N1 C80 1.53(2) . ? N2 C2 1.154(13) . ? N2 C20 1.515(15) . ? N4 C4 1.212(17) . ? N4 C51 1.43(2) . ? O1 C6 1.243(14) . ? C1 C2 1.379(15) . ? C3 C4 1.49(2) . ? C5 C6 1.51(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C11 C16 1.400(16) . ? C11 C12 1.393(16) . ? C12 C13 1.383(18) . ? C12 H12 0.9500 . ? C13 C14 1.335(19) . ? C13 H13 0.9500 . ? C14 C15 1.40(2) . ? C14 H14 0.9500 . ? C15 C16 1.356(19) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C20 C29 1.51(2) . ? C20 C28 1.492(19) . ? C20 C27 1.530(19) . ? C21 C26 1.364(18) . ? C21 C22 1.386(18) . ? C22 C23 1.393(16) . ? C22 H22 0.9500 . ? C23 C24 1.33(2) . ? C23 H23 0.9500 . ? C24 C25 1.39(2) . ? C24 H24 0.9500 . ? C25 C26 1.444(17) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.356(16) . ? C31 C36 1.463(15) . ? C32 C33 1.409(17) . ? C32 H32 0.9500 . ? C33 C34 1.378(19) . ? C33 H33 0.9500 . ? C34 C35 1.368(19) . ? C34 H34 0.9500 . ? C35 C36 1.397(17) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.37(2) . ? C41 C46 1.433(19) . ? C42 C43 1.34(2) . ? C42 H42 0.9500 . ? C43 C44 1.39(3) . ? C43 H43 0.9500 . ? C44 C45 1.41(3) . ? C44 H44 0.9500 . ? C45 C46 1.34(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C50 C55 1.375(19) . ? C50 C59 1.382(16) . ? C51 C54 1.53(3) . ? C51 C53 1.44(3) . ? C51 C52 1.36(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.32(2) . ? C55 H55 0.9500 . ? C56 C57 1.53(3) . ? C56 H56 0.9500 . ? C57 C58 1.36(2) . ? C57 H57 0.9500 . ? C58 C59 1.388(18) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C61 C66 1.36(2) . ? C61 C62 1.36(2) . ? C62 C63 1.36(3) . ? C62 H62 0.9500 . ? C63 C64 1.25(3) . ? C63 H63 0.9500 . ? C64 C65 1.42(4) . ? C64 H64 0.9500 . ? C65 C66 1.40(3) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.43(2) . ? C71 C72 1.39(2) . ? C72 C73 1.38(2) . ? C72 H72 0.9500 . ? C73 C74 1.33(3) . ? C73 H73 0.9500 . ? C74 C75 1.37(3) . ? C74 H74 0.9500 . ? C75 C76 1.37(2) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C80 C87 1.42(2) . ? C80 C88 1.51(2) . ? C80 C89 1.56(2) . ? C81 C82 1.342(19) . ? C81 C86 1.403(18) . ? C82 C83 1.364(19) . ? C82 H82 0.9500 . ? C83 C84 1.41(2) . ? C83 H83 0.9500 . ? C84 C85 1.37(2) . ? C84 H84 0.9500 . ? C85 C86 1.40(2) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C91 C92 1.416(19) . ? C91 C96 1.372(17) . ? C92 C93 1.378(17) . ? C92 H92 0.9500 . ? C93 C94 1.34(2) . ? C93 H93 0.9500 . ? C94 C95 1.46(2) . ? C94 H94 0.9500 . ? C95 C96 1.403(18) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C101 C102 1.30(2) . ? C101 C106 1.40(2) . ? C102 C103 1.40(2) . ? C102 H102 0.9500 . ? C103 C104 1.30(3) . ? C103 H103 0.9500 . ? C104 C105 1.31(3) . ? C104 H104 0.9500 . ? C105 C106 1.39(3) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C111 C116 1.406(19) . ? C111 C112 1.403(16) . ? C112 C113 1.352(17) . ? C112 H112 0.9500 . ? C113 C114 1.39(2) . ? C113 H113 0.9500 . ? C114 C115 1.35(2) . ? C114 H114 0.9500 . ? C115 C116 1.34(2) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.32(2) . ? C121 C126 1.37(2) . ? C122 C123 1.43(2) . ? C122 H122 0.9500 . ? C123 C124 1.16(3) . ? C123 H123 0.9500 . ? C124 C125 1.49(3) . ? C124 H124 0.9500 . ? C125 C126 1.36(2) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? B1 F24 1.25(2) . ? B1 F21 1.28(2) . ? B1 F22 1.389(18) . ? B1 F23 1.409(19) . ? B2 F13 1.23(2) . ? B2 F12 1.32(2) . ? B2 F11 1.41(3) . ? B2 F14 1.48(3) . ? C1D Cl2 1.71(3) . ? C1D Cl1 1.78(3) . ? C1D H1D1 0.9900 . ? C1D H1D2 0.9900 . ? C2D Cl3 1.39(3) . ? C2D Cl4 1.59(3) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C3D Cl6 1.48(7) 1_455 ? C3D Cl5 1.79(6) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? Cl6 C3D 1.48(7) 1_655 ? 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 O1 Cu1 O5 90.7(4) . . ? O1 Cu1 P2 108.7(3) . . ? O5 Cu1 P2 94.4(3) . . ? O1 Cu1 P4 112.3(3) . . ? O5 Cu1 P4 96.0(3) . . ? P2 Cu1 P4 137.48(17) . . ? O1 Cu1 Cu2 92.3(3) . . ? O5 Cu1 Cu2 175.7(3) . . ? P2 Cu1 Cu2 81.75(15) . . ? P4 Cu1 Cu2 85.66(16) . . ? P3 Cu2 P1 124.1(2) . . ? P3 Cu2 P6 122.7(2) . . ? P1 Cu2 P6 106.63(18) . . ? P3 Cu2 Cu1 98.13(16) . . ? P1 Cu2 Cu1 103.39(18) . . ? P6 Cu2 Cu1 93.81(16) . . ? P4 Cu1' P2 135.6(5) . . ? P4 Cu1' Cu2' 96.0(5) . . ? P2 Cu1' Cu2' 94.5(5) . . ? P4 Cu1' P3 60.0(3) . . ? P2 Cu1' P3 109.3(5) . . ? Cu2' Cu1' P3 38.9(3) . . ? P3 Cu2' P1 131.2(7) . . ? P3 Cu2' Cu1' 87.1(4) . . ? P1 Cu2' Cu1' 89.5(5) . . ? P3 Cu2' P6 120.8(5) . . ? P1 Cu2' P6 106.2(5) . . ? Cu1' Cu2' P6 79.0(5) . . ? C1 P1 C41 109.5(6) . . ? C1 P1 C21 105.3(6) . . ? C41 P1 C21 100.5(6) . . ? C1 P1 Cu2 106.1(3) . . ? C41 P1 Cu2 116.6(4) . . ? C21 P1 Cu2 118.2(4) . . ? C1 P1 Cu2' 119.1(5) . . ? C41 P1 Cu2' 108.0(6) . . ? C21 P1 Cu2' 112.8(5) . . ? Cu2 P1 Cu2' 13.2(4) . . ? C11 P2 C1 102.7(5) . . ? C11 P2 C31 104.3(5) . . ? C1 P2 C31 103.0(5) . . ? C11 P2 Cu1 107.9(4) . . ? C1 P2 Cu1 122.7(4) . . ? C31 P2 Cu1 114.4(4) . . ? C11 P2 Cu1' 116.9(5) . . ? C1 P2 Cu1' 110.7(4) . . ? C31 P2 Cu1' 117.5(5) . . ? Cu1 P2 Cu1' 12.6(3) . . ? C3 P3 C71 109.0(7) . . ? C3 P3 C50 106.0(6) . . ? C71 P3 C50 104.0(7) . . ? C3 P3 Cu2' 115.5(8) . . ? C71 P3 Cu2' 104.7(5) . . ? C50 P3 Cu2' 116.9(5) . . ? C3 P3 Cu2 102.4(7) . . ? C71 P3 Cu2 113.6(5) . . ? C50 P3 Cu2 121.2(4) . . ? Cu2' P3 Cu2 13.5(4) . . ? C3 P3 Cu1' 64.1(6) . . ? C71 P3 Cu1' 137.6(6) . . ? C50 P3 Cu1' 118.2(4) . . ? Cu2' P3 Cu1' 54.0(4) . . ? Cu2 P3 Cu1' 40.61(16) . . ? C3 P4 C91 101.4(7) . . ? C3 P4 C81 106.2(6) . . ? C91 P4 C81 102.0(6) . . ? C3 P4 Cu1 116.1(5) . . ? C91 P4 Cu1 111.7(4) . . ? C81 P4 Cu1 117.4(5) . . ? C3 P4 Cu1' 105.1(6) . . ? C91 P4 Cu1' 121.1(5) . . ? C81 P4 Cu1' 118.9(5) . . ? Cu1 P4 Cu1' 12.2(3) . . ? O5 P5 C101 112.2(6) . . ? O5 P5 C111 115.0(6) . . ? C101 P5 C111 104.7(7) . . ? C61 P6 C5 103.0(7) . . ? C61 P6 C121 102.5(6) . . ? C5 P6 C121 101.5(7) . . ? C61 P6 Cu2 110.6(6) . . ? C5 P6 Cu2 113.5(4) . . ? C121 P6 Cu2 123.4(5) . . ? C61 P6 Cu2' 98.4(6) . . ? C5 P6 Cu2' 121.5(5) . . ? C121 P6 Cu2' 125.8(6) . . ? Cu2 P6 Cu2' 12.7(3) . . ? C6 N1 C80 128.3(11) . . ? C2 N2 C20 141.9(11) . . ? C4 N4 C51 145(2) . . ? C6 O1 Cu1 148.6(9) . . ? P5 O5 Cu1 162.9(6) . . ? C2 C1 P1 124.6(8) . . ? C2 C1 P2 117.3(9) . . ? P1 C1 P2 117.9(5) . . ? N2 C2 C1 175.4(13) . . ? C4 C3 P4 122.6(10) . . ? C4 C3 P3 107.3(13) . . ? P4 C3 P3 129.9(10) . . ? N4 C4 C3 175.6(18) . . ? C6 C5 P6 116.4(10) . . ? C6 C5 H5A 108.2 . . ? P6 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? P6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? O1 C6 N1 126.0(14) . . ? O1 C6 C5 119.2(13) . . ? N1 C6 C5 114.8(11) . . ? C16 C11 C12 117.7(12) . . ? C16 C11 P2 117.0(10) . . ? C12 C11 P2 125.3(9) . . ? C13 C12 C11 121.6(12) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 119.3(14) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 120.7(15) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.7(13) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 119.9(13) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? N2 C20 C29 106.9(10) . . ? N2 C20 C28 109.1(10) . . ? C29 C20 C28 115.2(15) . . ? N2 C20 C27 106.0(12) . . ? C29 C20 C27 112.8(12) . . ? C28 C20 C27 106.4(13) . . ? C26 C21 C22 119.4(12) . . ? C26 C21 P1 120.0(10) . . ? C22 C21 P1 120.4(11) . . ? C23 C22 C21 121.5(15) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C24 C23 C22 119.4(15) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 121.9(12) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C24 C25 C26 118.4(13) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C21 C26 C25 119.3(13) . . ? C21 C26 H26 120.3 . . ? C25 C26 H26 120.4 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 C29 H29A 109.5 . . ? C20 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C20 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 118.8(11) . . ? C32 C31 P2 126.8(9) . . ? C36 C31 P2 114.4(9) . . ? C31 C32 C33 121.6(12) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 120.2(13) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.2(12) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 122.8(12) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C31 C36 C35 117.3(12) . . ? C31 C36 H36 121.3 . . ? C35 C36 H36 121.3 . . ? C42 C41 C46 117.9(15) . . ? C42 C41 P1 121.4(13) . . ? C46 C41 P1 120.6(11) . . ? C43 C42 C41 129.7(19) . . ? C43 C42 H42 115.2 . . ? C41 C42 H42 115.1 . . ? C42 C43 C44 112(2) . . ? C42 C43 H43 123.9 . . ? C44 C43 H43 124.0 . . ? C45 C44 C43 119(2) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 127.8(19) . . ? C44 C45 H45 116.1 . . ? C46 C45 H45 116.1 . . ? C45 C46 C41 112.4(16) . . ? C45 C46 H46 123.8 . . ? C41 C46 H46 123.8 . . ? C55 C50 C59 117.5(13) . . ? C55 C50 P3 124.4(10) . . ? C59 C50 P3 118.2(10) . . ? N4 C51 C54 105.2(19) . . ? N4 C51 C53 104(2) . . ? C54 C51 C53 113(2) . . ? N4 C51 C52 111.3(19) . . ? C54 C51 C52 108(2) . . ? C53 C51 C52 115(3) . . ? C51 C52 H52A 109.4 . . ? 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 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.6 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.4 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 C56 124.4(15) . . ? C50 C55 H55 117.8 . . ? C56 C55 H55 117.8 . . ? C55 C56 C57 118.8(14) . . ? C55 C56 H56 120.6 . . ? C57 C56 H56 120.6 . . ? C58 C57 C56 115.2(14) . . ? C58 C57 H57 122.4 . . ? C56 C57 H57 122.4 . . ? C57 C58 C59 122.2(14) . . ? C57 C58 H58 118.9 . . ? C59 C58 H58 118.9 . . ? C50 C59 C58 121.8(13) . . ? C50 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C66 C61 C62 118.1(15) . . ? C66 C61 P6 117.6(12) . . ? C62 C61 P6 124.0(15) . . ? C61 C62 C63 117(2) . . ? C61 C62 H62 121.6 . . ? C63 C62 H62 121.7 . . ? C64 C63 C62 130(3) . . ? C64 C63 H63 115.0 . . ? C62 C63 H63 115.0 . . ? C63 C64 C65 113(3) . . ? C63 C64 H64 123.4 . . ? C65 C64 H64 123.4 . . ? C66 C65 C64 120(2) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.2 . . ? C61 C66 C65 120(2) . . ? C61 C66 H66 119.9 . . ? C65 C66 H66 120.0 . . ? C76 C71 C72 117.6(12) . . ? C76 C71 P3 116.7(10) . . ? C72 C71 P3 124.6(12) . . ? C71 C72 C73 120.1(15) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 119.9 . . ? C74 C73 C72 122.1(19) . . ? C74 C73 H73 119.0 . . ? C72 C73 H73 118.9 . . ? C73 C74 C75 119.0(19) . . ? C73 C74 H74 120.5 . . ? C75 C74 H74 120.5 . . ? C76 C75 C74 122(2) . . ? C76 C75 H75 119.2 . . ? C74 C75 H75 119.1 . . ? C71 C76 C75 118.5(17) . . ? C71 C76 H76 120.8 . . ? C75 C76 H76 120.7 . . ? N1 C80 C87 104.7(15) . . ? N1 C80 C88 109.1(12) . . ? C87 C80 C88 116.4(18) . . ? N1 C80 C89 104.1(15) . . ? C87 C80 C89 109.3(14) . . ? C88 C80 C89 112.3(16) . . ? C82 C81 C86 115.7(13) . . ? C82 C81 P4 119.9(9) . . ? C86 C81 P4 124.2(12) . . ? C81 C82 C83 124.7(13) . . ? C81 C82 H82 117.6 . . ? C83 C82 H82 117.6 . . ? C82 C83 C84 118.1(16) . . ? C82 C83 H83 120.9 . . ? C84 C83 H83 121.0 . . ? C85 C84 C83 120.1(14) . . ? C85 C84 H84 119.9 . . ? C83 C84 H84 119.9 . . ? C86 C85 C84 117.9(16) . . ? C86 C85 H85 121.1 . . ? C84 C85 H85 121.1 . . ? C85 C86 C81 122.4(18) . . ? C85 C86 H86 118.8 . . ? C81 C86 H86 118.8 . . ? C80 C87 H87A 109.4 . . ? C80 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C80 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C80 C88 H88A 109.5 . . ? C80 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C80 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C80 C89 H89A 109.5 . . ? C80 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C80 C89 H89C 109.4 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C92 C91 C96 116.1(11) . . ? C92 C91 P4 123.0(9) . . ? C96 C91 P4 120.8(10) . . ? C93 C92 C91 121.6(13) . . ? C93 C92 H92 119.2 . . ? C91 C92 H92 119.2 . . ? C94 C93 C92 122.6(14) . . ? C94 C93 H93 118.7 . . ? C92 C93 H93 118.7 . . ? C93 C94 C95 118.1(13) . . ? C93 C94 H94 121.0 . . ? C95 C94 H94 121.0 . . ? C96 C95 C94 117.7(13) . . ? C96 C95 H95 121.2 . . ? C94 C95 H95 121.2 . . ? C91 C96 C95 123.7(13) . . ? C91 C96 H96 118.2 . . ? C95 C96 H96 118.1 . . ? C102 C101 C106 114.3(16) . . ? C102 C101 P5 121.5(14) . . ? C106 C101 P5 124.0(12) . . ? C103 C102 C101 122.9(19) . . ? C103 C102 H102 118.6 . . ? C101 C102 H102 118.6 . . ? C104 C103 C102 122.0(18) . . ? C104 C103 H103 119.1 . . ? C102 C103 H103 119.0 . . ? C103 C104 C105 117.2(19) . . ? C103 C104 H104 121.4 . . ? C105 C104 H104 121.4 . . ? C106 C105 C104 122(2) . . ? C106 C105 H105 119.3 . . ? C104 C105 H105 119.2 . . ? C105 C106 C101 120.9(19) . . ? C105 C106 H106 119.5 . . ? C101 C106 H106 119.5 . . ? C116 C111 C112 117.1(12) . . ? C116 C111 P5 124.6(10) . . ? C112 C111 P5 118.3(10) . . ? C113 C112 C111 120.9(13) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.6 . . ? C112 C113 C114 119.9(14) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C113 C114 C115 120.0(14) . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C116 121.2(15) . . ? C114 C115 H115 119.4 . . ? C116 C115 H115 119.4 . . ? C111 C116 C115 120.7(14) . . ? C111 C116 H116 119.7 . . ? C115 C116 H116 119.6 . . ? C122 C121 C126 119.1(15) . . ? C122 C121 P6 118.9(14) . . ? C126 C121 P6 121.9(12) . . ? C121 C122 C123 118.3(19) . . ? C121 C122 H122 120.9 . . ? C123 C122 H122 120.8 . . ? C124 C123 C122 124(2) . . ? C124 C123 H123 117.9 . . ? C122 C123 H123 117.9 . . ? C123 C124 C125 121(2) . . ? C123 C124 H124 119.4 . . ? C125 C124 H124 119.4 . . ? C126 C125 C124 114.4(19) . . ? C126 C125 H125 122.8 . . ? C124 C125 H125 122.8 . . ? C125 C126 C121 122.7(18) . . ? C125 C126 H126 118.7 . . ? C121 C126 H126 118.6 . . ? F24 B1 F21 115.4(17) . . ? F24 B1 F22 107.5(16) . . ? F21 B1 F22 106.9(14) . . ? F24 B1 F23 113.7(13) . . ? F21 B1 F23 109.2(17) . . ? F22 B1 F23 103.3(13) . . ? F13 B2 F12 121(2) . . ? F13 B2 F11 118.5(18) . . ? F12 B2 F11 108(2) . . ? F13 B2 F14 100(2) . . ? F12 B2 F14 113.8(16) . . ? F11 B2 F14 91.6(18) . . ? Cl2 C1D Cl1 109.6(17) . . ? Cl2 C1D H1D1 109.8 . . ? Cl1 C1D H1D1 109.8 . . ? Cl2 C1D H1D2 109.7 . . ? Cl1 C1D H1D2 109.7 . . ? H1D1 C1D H1D2 108.2 . . ? Cl3 C2D Cl4 126(2) . . ? Cl3 C2D H2D1 105.8 . . ? Cl4 C2D H2D1 105.7 . . ? Cl3 C2D H2D2 105.8 . . ? Cl4 C2D H2D2 105.8 . . ? H2D1 C2D H2D2 106.2 . . ? Cl6 C3D Cl5 120(3) 1_455 . ? Cl6 C3D H3D1 107.5 1_455 . ? Cl5 C3D H3D1 107.2 . . ? Cl6 C3D H3D2 107.2 1_455 . ? Cl5 C3D H3D2 107.1 . . ? H3D1 C3D H3D2 106.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.905 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.153