# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Regis Reau' _publ_contact_author_address ; Chemistry University of Rennes1 Campus de Beaulieu; UMR 6226 Rennes 35042 FRANCE ; _publ_contact_author_email REGIS.REAU@UNIV-RENNES1.FR _publ_section_title ; Stereoselective Coordination of Ditopic Phospholyl-Azahelicenes: A Novel Approach Towards Structural Diversity in Chiral pi-Conjugated Assemblies ; loop_ _publ_author_name 'Regis Reau' 'Jeanne Crassous' 'Sebastien Graule' 'Christophe Lescop' 'Wenting Shen' #===END # Attachment 'compound2A.cif' data_compound2a _database_code_depnum_ccdc_archive 'CCDC 651119' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H28 N P' _chemical_formula_weight 517.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5107(4) _cell_length_b 10.9272(5) _cell_length_c 14.1036(6) _cell_angle_alpha 72.146(3) _cell_angle_beta 70.845(3) _cell_angle_gamma 84.199(3) _cell_volume 1317.89(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 CCD _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 18731 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.24 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4428 _reflns_number_gt 3255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.6396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4428 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 P1 P 0.82074(6) 0.48439(5) 0.60353(4) 0.01738(15) Uani 1 1 d . . . N1 N 0.82713(18) 0.09980(15) 0.69194(12) 0.0185(4) Uani 1 1 d . . . C1 C 0.8368(2) 0.32360(19) 0.59370(15) 0.0170(4) Uani 1 1 d . . . C2 C 0.8203(2) 0.32375(18) 0.50088(15) 0.0165(4) Uani 1 1 d . . . C3 C 0.8640(2) 0.21479(19) 0.45185(15) 0.0204(5) Uani 1 1 d . . . H3A H 0.8227 0.1335 0.5056 0.024 Uiso 1 1 calc R . . H3B H 0.9739 0.2069 0.4292 0.024 Uiso 1 1 calc R . . C4 C 0.8101(2) 0.23271(19) 0.35789(15) 0.0226(5) Uani 1 1 d . . . H4A H 0.8619 0.1709 0.3191 0.027 Uiso 1 1 calc R . . H4B H 0.7020 0.2148 0.3827 0.027 Uiso 1 1 calc R . . C5 C 0.8400(3) 0.36934(19) 0.28470(15) 0.0232(5) Uani 1 1 d . . . H5A H 0.9469 0.3900 0.2640 0.028 Uiso 1 1 calc R . . H5B H 0.8149 0.3767 0.2204 0.028 Uiso 1 1 calc R . . C6 C 0.7461(2) 0.46325(19) 0.34041(15) 0.0202(5) Uani 1 1 d . . . H6A H 0.7726 0.5522 0.2951 0.024 Uiso 1 1 calc R . . H6B H 0.6397 0.4498 0.3518 0.024 Uiso 1 1 calc R . . C7 C 0.7687(2) 0.44707(18) 0.44469(15) 0.0164(4) Uani 1 1 d . . . C8 C 0.7487(2) 0.54026(18) 0.49395(15) 0.0165(4) Uani 1 1 d . . . C9 C 0.6921(2) 0.67161(18) 0.46316(14) 0.0170(4) Uani 1 1 d . . . C10 C 0.5771(2) 0.70000(19) 0.41887(15) 0.0190(5) Uani 1 1 d . . . H10 H 0.5342 0.6330 0.4076 0.023 Uiso 1 1 calc R . . C11 C 0.5245(2) 0.82481(19) 0.39102(15) 0.0208(5) Uani 1 1 d . . . H11 H 0.4466 0.8426 0.3604 0.025 Uiso 1 1 calc R . . C12 C 0.5845(3) 0.9229(2) 0.40748(16) 0.0251(5) Uani 1 1 d . . . H12 H 0.5492 1.0084 0.3875 0.030 Uiso 1 1 calc R . . C13 C 0.6964(2) 0.8964(2) 0.45324(16) 0.0250(5) Uani 1 1 d . . . H13 H 0.7372 0.9638 0.4655 0.030 Uiso 1 1 calc R . . C14 C 0.7494(2) 0.77235(19) 0.48134(15) 0.0208(5) Uani 1 1 d . . . H14 H 0.8257 0.7553 0.5134 0.025 Uiso 1 1 calc R . . C15 C 0.8810(2) 0.21604(18) 0.67157(14) 0.0167(4) Uani 1 1 d . . . C16 C 0.9696(2) 0.23848(19) 0.72746(15) 0.0178(5) Uani 1 1 d . . . H16 H 0.9968 0.3238 0.7177 0.021 Uiso 1 1 calc R . . C17 C 1.0163(2) 0.13806(19) 0.79535(15) 0.0180(5) Uani 1 1 d . . . H17 H 1.0773 0.1536 0.8320 0.022 Uiso 1 1 calc R . . C18 C 0.9746(2) 0.01077(18) 0.81150(14) 0.0166(4) Uani 1 1 d . . . C19 C 1.0219(2) -0.10395(19) 0.87897(15) 0.0179(5) Uani 1 1 d . . . C20 C 1.1528(2) -0.11037(19) 0.91234(15) 0.0190(5) Uani 1 1 d . . . C21 C 1.2680(2) -0.0177(2) 0.86445(16) 0.0218(5) Uani 1 1 d . . . H21 H 1.2607 0.0539 0.8075 0.026 Uiso 1 1 calc R . . C22 C 1.3896(2) -0.0286(2) 0.89785(16) 0.0259(5) Uani 1 1 d . . . H22 H 1.4651 0.0353 0.8639 0.031 Uiso 1 1 calc R . . C23 C 1.4038(2) -0.1327(2) 0.98148(16) 0.0259(5) Uani 1 1 d . . . H23 H 1.4856 -0.1374 1.0071 0.031 Uiso 1 1 calc R . . C24 C 1.2991(2) -0.2277(2) 1.02595(16) 0.0238(5) Uani 1 1 d . . . H24 H 1.3103 -0.2998 1.0813 0.029 Uiso 1 1 calc R . . C25 C 1.1746(2) -0.22096(19) 0.99139(15) 0.0201(5) Uani 1 1 d . . . C26 C 1.0742(2) -0.3269(2) 1.03128(15) 0.0225(5) Uani 1 1 d . . . H26 H 1.0847 -0.3984 1.0873 0.027 Uiso 1 1 calc R . . C27 C 0.9649(2) -0.32628(19) 0.99008(15) 0.0205(5) Uani 1 1 d . . . H27 H 0.9050 -0.4008 1.0134 0.025 Uiso 1 1 calc R . . C28 C 0.9369(2) -0.21631(19) 0.91215(15) 0.0195(5) Uani 1 1 d . . . C29 C 0.8253(2) -0.2216(2) 0.86686(16) 0.0218(5) Uani 1 1 d . . . H29 H 0.7696 -0.2985 0.8898 0.026 Uiso 1 1 calc R . . C30 C 0.7961(2) -0.12026(19) 0.79200(16) 0.0211(5) Uani 1 1 d . . . H30 H 0.7268 -0.1288 0.7588 0.025 Uiso 1 1 calc R . . C31 C 0.8695(2) -0.00054(19) 0.76304(15) 0.0180(5) Uani 1 1 d . . . C32 C 0.6588(2) 0.48553(19) 0.71752(15) 0.0175(4) Uani 1 1 d . . . C33 C 0.5540(2) 0.38647(19) 0.76809(15) 0.0197(5) Uani 1 1 d . . . H33 H 0.5660 0.3127 0.7439 0.024 Uiso 1 1 calc R . . C34 C 0.4325(2) 0.3950(2) 0.85327(16) 0.0229(5) Uani 1 1 d . . . H34 H 0.3615 0.3274 0.8872 0.027 Uiso 1 1 calc R . . C35 C 0.4147(2) 0.5022(2) 0.88882(16) 0.0256(5) Uani 1 1 d . . . H35 H 0.3313 0.5081 0.9471 0.031 Uiso 1 1 calc R . . C36 C 0.5176(3) 0.6004(2) 0.83999(17) 0.0324(6) Uani 1 1 d . . . H36 H 0.5048 0.6741 0.8643 0.039 Uiso 1 1 calc R . . C37 C 0.6397(2) 0.5915(2) 0.75541(16) 0.0268(5) Uani 1 1 d . . . H37 H 0.7112 0.6587 0.7229 0.032 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 P1 0.0193(3) 0.0166(3) 0.0177(3) -0.0046(2) -0.0074(2) -0.0020(2) N1 0.0190(10) 0.0181(9) 0.0198(9) -0.0054(7) -0.0077(8) -0.0010(7) C1 0.0128(11) 0.0188(11) 0.0182(10) -0.0044(8) -0.0034(9) -0.0032(8) C2 0.0127(11) 0.0167(11) 0.0197(10) -0.0037(8) -0.0047(9) -0.0037(8) C3 0.0244(13) 0.0170(11) 0.0220(11) -0.0074(9) -0.0088(10) 0.0011(9) C4 0.0274(13) 0.0216(12) 0.0218(11) -0.0102(9) -0.0081(10) -0.0004(9) C5 0.0295(13) 0.0234(12) 0.0191(11) -0.0072(9) -0.0101(10) 0.0014(9) C6 0.0238(12) 0.0186(11) 0.0199(11) -0.0043(9) -0.0101(10) -0.0009(9) C7 0.0122(11) 0.0174(11) 0.0186(10) -0.0034(8) -0.0037(9) -0.0057(8) C8 0.0144(11) 0.0161(11) 0.0174(10) -0.0015(8) -0.0049(9) -0.0044(8) C9 0.0179(12) 0.0177(11) 0.0127(10) -0.0029(8) -0.0017(9) -0.0030(8) C10 0.0195(12) 0.0190(11) 0.0172(10) -0.0044(8) -0.0032(9) -0.0051(9) C11 0.0209(12) 0.0202(12) 0.0201(11) -0.0034(9) -0.0079(10) 0.0022(9) C12 0.0331(14) 0.0159(11) 0.0219(11) -0.0039(9) -0.0055(10) 0.0040(9) C13 0.0310(14) 0.0200(12) 0.0255(12) -0.0092(9) -0.0073(10) -0.0040(10) C14 0.0213(12) 0.0209(12) 0.0208(11) -0.0064(9) -0.0068(10) -0.0008(9) C15 0.0159(11) 0.0178(11) 0.0156(10) -0.0060(8) -0.0026(9) -0.0001(8) C16 0.0192(12) 0.0158(11) 0.0186(10) -0.0058(8) -0.0050(9) -0.0014(9) C17 0.0163(11) 0.0218(11) 0.0173(10) -0.0066(9) -0.0058(9) -0.0015(9) C18 0.0168(11) 0.0191(11) 0.0132(10) -0.0046(8) -0.0036(9) -0.0009(8) C19 0.0182(12) 0.0205(11) 0.0142(10) -0.0068(8) -0.0026(9) 0.0008(9) C20 0.0204(12) 0.0218(11) 0.0159(10) -0.0083(9) -0.0049(9) 0.0013(9) C21 0.0242(13) 0.0209(12) 0.0199(11) -0.0042(9) -0.0078(10) -0.0003(9) C22 0.0245(13) 0.0269(12) 0.0287(12) -0.0079(10) -0.0112(11) -0.0018(10) C23 0.0251(13) 0.0306(13) 0.0285(12) -0.0110(10) -0.0154(11) 0.0027(10) C24 0.0291(13) 0.0253(12) 0.0193(11) -0.0067(9) -0.0121(10) 0.0064(10) C25 0.0232(12) 0.0210(11) 0.0167(10) -0.0070(9) -0.0067(9) 0.0042(9) C26 0.0288(13) 0.0179(11) 0.0178(11) -0.0018(9) -0.0076(10) 0.0042(9) C27 0.0217(12) 0.0157(11) 0.0214(11) -0.0034(9) -0.0054(10) 0.0005(9) C28 0.0193(12) 0.0196(11) 0.0191(10) -0.0063(9) -0.0049(9) 0.0014(9) C29 0.0210(12) 0.0185(11) 0.0256(11) -0.0047(9) -0.0077(10) -0.0024(9) C30 0.0210(12) 0.0197(11) 0.0262(11) -0.0065(9) -0.0115(10) -0.0025(9) C31 0.0190(12) 0.0178(11) 0.0170(10) -0.0059(8) -0.0049(9) 0.0016(9) C32 0.0197(12) 0.0183(11) 0.0167(10) -0.0032(8) -0.0103(9) 0.0001(8) C33 0.0221(12) 0.0194(11) 0.0202(11) -0.0051(9) -0.0110(10) 0.0009(9) C34 0.0191(12) 0.0255(12) 0.0224(11) -0.0009(9) -0.0091(10) -0.0033(9) C35 0.0213(13) 0.0338(13) 0.0210(11) -0.0101(10) -0.0037(10) 0.0007(10) C36 0.0365(15) 0.0312(13) 0.0317(13) -0.0186(11) -0.0035(11) -0.0044(11) C37 0.0288(14) 0.0258(12) 0.0258(12) -0.0105(10) -0.0030(10) -0.0088(10) _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 P1 C1 1.792(2) . ? P1 C8 1.8059(19) . ? P1 C32 1.827(2) . ? N1 C15 1.330(2) . ? N1 C31 1.368(2) . ? C1 C2 1.368(3) . ? C1 C15 1.475(3) . ? C2 C7 1.467(3) . ? C2 C3 1.511(3) . ? C3 C4 1.525(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.524(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.510(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.365(3) . ? C8 C9 1.467(3) . ? C9 C10 1.394(3) . ? C9 C14 1.400(3) . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.375(3) . ? C11 H11 0.9500 . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.410(3) . ? C16 C17 1.362(3) . ? C16 H16 0.9500 . ? C17 C18 1.415(3) . ? C17 H17 0.9500 . ? C18 C31 1.416(3) . ? C18 C19 1.455(3) . ? C19 C28 1.407(3) . ? C19 C20 1.457(3) . ? C20 C21 1.414(3) . ? C20 C25 1.422(3) . ? C21 C22 1.367(3) . ? C21 H21 0.9500 . ? C22 C23 1.399(3) . ? C22 H22 0.9500 . ? C23 C24 1.365(3) . ? C23 H23 0.9500 . ? C24 C25 1.408(3) . ? C24 H24 0.9500 . ? C25 C26 1.429(3) . ? C26 C27 1.345(3) . ? C26 H26 0.9500 . ? C27 C28 1.429(3) . ? C27 H27 0.9500 . ? C28 C29 1.420(3) . ? C29 C30 1.353(3) . ? C29 H29 0.9500 . ? C30 C31 1.427(3) . ? C30 H30 0.9500 . ? C32 C37 1.390(3) . ? C32 C33 1.398(3) . ? C33 C34 1.387(3) . ? C33 H33 0.9500 . ? C34 C35 1.384(3) . ? C34 H34 0.9500 . ? C35 C36 1.378(3) . ? C35 H35 0.9500 . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C8 91.27(9) . . ? C1 P1 C32 106.36(9) . . ? C8 P1 C32 104.10(9) . . ? C15 N1 C31 118.26(17) . . ? C2 C1 C15 128.34(18) . . ? C2 C1 P1 109.76(14) . . ? C15 C1 P1 121.43(14) . . ? C1 C2 C7 113.67(18) . . ? C1 C2 C3 125.15(17) . . ? C7 C2 C3 120.90(17) . . ? C2 C3 C4 113.45(16) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 110.77(17) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 109.45(17) . . ? C6 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C7 C6 C5 112.12(16) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C2 114.03(17) . . ? C8 C7 C6 125.79(18) . . ? C2 C7 C6 120.16(17) . . ? C7 C8 C9 128.73(18) . . ? C7 C8 P1 109.35(15) . . ? C9 C8 P1 121.70(14) . . ? C10 C9 C14 117.76(18) . . ? C10 C9 C8 121.86(18) . . ? C14 C9 C8 120.34(18) . . ? C11 C10 C9 120.92(19) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.66(19) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 120.9(2) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? N1 C15 C16 121.36(18) . . ? N1 C15 C1 118.08(17) . . ? C16 C15 C1 120.42(17) . . ? C17 C16 C15 120.15(18) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.32(18) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C31 115.28(17) . . ? C17 C18 C19 125.14(18) . . ? C31 C18 C19 119.40(17) . . ? C28 C19 C18 117.49(18) . . ? C28 C19 C20 118.25(18) . . ? C18 C19 C20 124.26(18) . . ? C21 C20 C25 116.93(19) . . ? C21 C20 C19 123.86(18) . . ? C25 C20 C19 118.98(18) . . ? C22 C21 C20 121.76(19) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.6(2) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 119.3(2) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 121.32(19) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C20 119.72(19) . . ? C24 C25 C26 120.54(18) . . ? C20 C25 C26 119.66(19) . . ? C27 C26 C25 120.53(18) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 121.60(19) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C19 C28 C29 120.20(18) . . ? C19 C28 C27 119.89(19) . . ? C29 C28 C27 119.89(19) . . ? C30 C29 C28 121.91(19) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 119.82(19) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? N1 C31 C18 123.66(18) . . ? N1 C31 C30 116.52(18) . . ? C18 C31 C30 119.74(17) . . ? C37 C32 C33 118.55(19) . . ? C37 C32 P1 117.69(15) . . ? C33 C32 P1 123.75(15) . . ? C34 C33 C32 120.49(19) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.92(19) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.2(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 119.9(2) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C32 120.9(2) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.394 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.046 #===END # Attachment 'compound4b.cif' data_compound4b _database_code_depnum_ccdc_archive 'CCDC 651120' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C153 H122 Cl14 Cu4 N4 P4' _chemical_formula_weight 2890.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.938(2) _cell_length_b 19.9650(10) _cell_length_c 24.4490(10) _cell_angle_alpha 90.00 _cell_angle_beta 124.683(2) _cell_angle_gamma 90.00 _cell_volume 13221.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5928 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _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 68081 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13411 _reflns_number_gt 10702 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A twist disorder on two positions of one cyclohexane system and disorder of a CuCl2 anion and a dichloromethane molecule on three positions are refined anisotropically with the help of 325 ADP- and distances-restraints. ; _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^)+(0.0570P)^2^+47.5659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13411 _refine_ls_number_parameters 969 _refine_ls_number_restraints 325 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.028 _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 0.231293(11) 0.962218(16) 0.685125(15) 0.01454(9) Uani 1 1 d . . . P1 P 0.19546(2) 0.92194(3) 0.57920(3) 0.01331(14) Uani 1 1 d . A . P2 P 0.31553(2) 0.97467(3) 0.75439(3) 0.01358(14) Uani 1 1 d . . . N1 N 0.18298(8) 1.04427(11) 0.64039(11) 0.0149(4) Uani 1 1 d . A . N2 N 0.23701(8) 0.91103(12) 0.76382(11) 0.0186(5) Uani 1 1 d . . . C1 C 0.13983(10) 0.96808(13) 0.55101(13) 0.0157(5) Uani 1 1 d . A . C2 C 0.09985(10) 0.92712(14) 0.51698(13) 0.0174(5) Uani 1 1 d DU . . C3 C 0.0486(3) 0.9453(6) 0.4977(9) 0.022(3) Uani 0.502(11) 1 d PDU A 1 H3A H 0.0517 0.9739 0.5331 0.026 Uiso 0.502(11) 1 calc PR A 1 H3B H 0.0317 0.9720 0.4563 0.026 Uiso 0.502(11) 1 calc PR A 1 C4 C 0.0170(2) 0.8856(3) 0.4873(4) 0.0254(18) Uani 0.502(11) 1 d PDU A 1 H4A H -0.0175 0.9001 0.4674 0.030 Uiso 0.502(11) 1 calc PR A 1 H4B H 0.0294 0.8639 0.5305 0.030 Uiso 0.502(11) 1 calc PR A 1 C5 C 0.0187(4) 0.8361(6) 0.4409(7) 0.029(3) Uani 0.502(11) 1 d PDU A 1 H5A H -0.0049 0.7991 0.4295 0.035 Uiso 0.502(11) 1 calc PR A 1 H5B H 0.0089 0.8590 0.3992 0.035 Uiso 0.502(11) 1 calc PR A 1 C6 C 0.0705(3) 0.8080(4) 0.4746(5) 0.029(2) Uani 0.502(11) 1 d PDU A 1 H6A H 0.0719 0.7809 0.4418 0.035 Uiso 0.502(11) 1 calc PR A 1 H6B H 0.0770 0.7775 0.5108 0.035 Uiso 0.502(11) 1 calc PR A 1 C7 C 0.11126(10) 0.86049(14) 0.50372(14) 0.0197(6) Uani 1 1 d DU A . C3' C 0.0487(4) 0.9395(7) 0.5006(10) 0.032(4) Uani 0.498(11) 1 d PDU A 2 H3'1 H 0.0395 0.9868 0.4869 0.038 Uiso 0.498(11) 1 calc PR A 2 H3'2 H 0.0493 0.9323 0.5411 0.038 Uiso 0.498(11) 1 calc PR A 2 C4' C 0.0096(2) 0.8942(4) 0.4455(5) 0.035(2) Uani 0.498(11) 1 d PDU A 2 H4'1 H -0.0212 0.8979 0.4434 0.043 Uiso 0.498(11) 1 calc PR A 2 H4'2 H 0.0024 0.9097 0.4023 0.043 Uiso 0.498(11) 1 calc PR A 2 C5' C 0.0256(5) 0.8212(6) 0.4559(9) 0.039(4) Uani 0.498(11) 1 d PDU A 2 H5'1 H 0.0338 0.8058 0.4996 0.046 Uiso 0.498(11) 1 calc PR A 2 H5'2 H -0.0018 0.7933 0.4209 0.046 Uiso 0.498(11) 1 calc PR A 2 C6' C 0.0705(3) 0.8131(5) 0.4535(4) 0.021(2) Uani 0.498(11) 1 d PDU A 2 H6'1 H 0.0614 0.8235 0.4082 0.026 Uiso 0.498(11) 1 calc PR A 2 H6'2 H 0.0824 0.7663 0.4641 0.026 Uiso 0.498(11) 1 calc PR A 2 C8 C 0.16002(10) 0.84936(13) 0.53157(13) 0.0171(5) Uani 1 1 d . . . C9 C 0.18430(10) 0.78810(14) 0.52986(14) 0.0186(6) Uani 1 1 d . A . C10 C 0.16839(11) 0.75550(15) 0.47002(15) 0.0232(6) Uani 1 1 d . . . H10 H 0.1413 0.7729 0.4291 0.028 Uiso 1 1 calc R A . C11 C 0.19206(12) 0.69789(15) 0.47023(16) 0.0265(7) Uani 1 1 d . A . H11 H 0.1805 0.6757 0.4295 0.032 Uiso 1 1 calc R . . C12 C 0.23229(11) 0.67246(15) 0.52916(16) 0.0256(6) Uani 1 1 d . . . H12 H 0.2487 0.6334 0.5288 0.031 Uiso 1 1 calc R A . C13 C 0.24855(11) 0.70444(15) 0.58877(16) 0.0239(6) Uani 1 1 d . A . H13 H 0.2759 0.6869 0.6294 0.029 Uiso 1 1 calc R . . C14 C 0.22499(10) 0.76183(14) 0.58912(14) 0.0199(6) Uani 1 1 d . . . H14 H 0.2366 0.7836 0.6301 0.024 Uiso 1 1 calc R A . C15 C 0.14564(9) 1.03592(13) 0.57745(13) 0.0150(5) Uani 1 1 d . . . C16 C 0.11394(9) 1.08982(14) 0.53614(13) 0.0166(5) Uani 1 1 d . A . C17 C 0.08144(10) 1.08134(15) 0.46551(14) 0.0229(6) Uani 1 1 d . . . H17 H 0.0805 1.0396 0.4461 0.028 Uiso 1 1 calc R A . C18 C 0.05218(11) 1.13199(16) 0.42631(15) 0.0262(6) Uani 1 1 d . A . H18 H 0.0333 1.1271 0.3793 0.031 Uiso 1 1 calc R . . C19 C 0.04929(10) 1.19240(15) 0.45444(15) 0.0238(6) Uani 1 1 d . . . C20 C 0.01555(11) 1.24334(17) 0.41282(16) 0.0291(7) Uani 1 1 d . A . H20 H -0.0033 1.2384 0.3658 0.035 Uiso 1 1 calc R . . C21 C 0.01009(12) 1.29936(17) 0.44016(17) 0.0323(8) Uani 1 1 d . . . H21 H -0.0114 1.3341 0.4121 0.039 Uiso 1 1 calc R A . C22 C 0.03582(12) 1.30585(16) 0.50875(17) 0.0299(7) Uani 1 1 d . A . H22 H 0.0299 1.3435 0.5270 0.036 Uiso 1 1 calc R . . C23 C 0.06960(10) 1.25871(15) 0.55032(16) 0.0233(6) Uani 1 1 d . . . H23 H 0.0866 1.2639 0.5971 0.028 Uiso 1 1 calc R A . C24 C 0.07968(10) 1.20210(14) 0.52475(15) 0.0205(6) Uani 1 1 d . A . C25 C 0.11729(10) 1.15233(13) 0.56532(14) 0.0177(5) Uani 1 1 d . . . C26 C 0.15983(10) 1.16323(14) 0.63230(13) 0.0169(5) Uani 1 1 d . A . C27 C 0.17591(10) 1.22661(14) 0.66382(14) 0.0205(6) Uani 1 1 d . . . H27 H 0.1568 1.2652 0.6407 0.025 Uiso 1 1 calc R A . C28 C 0.21791(11) 1.23410(15) 0.72636(15) 0.0239(6) Uani 1 1 d . A . H28 H 0.2273 1.2773 0.7460 0.029 Uiso 1 1 calc R . . C29 C 0.24720(11) 1.17845(15) 0.76177(15) 0.0259(6) Uani 1 1 d . . . H29 H 0.2760 1.1837 0.8056 0.031 Uiso 1 1 calc R A . C30 C 0.23399(10) 1.11642(15) 0.73269(14) 0.0223(6) Uani 1 1 d . A . H30 H 0.2538 1.0787 0.7568 0.027 Uiso 1 1 calc R . . C31 C 0.19169(10) 1.10767(14) 0.66781(13) 0.0166(5) Uani 1 1 d . . . C32 C 0.21910(10) 0.95850(13) 0.53394(14) 0.0170(5) Uani 1 1 d . . . C33 C 0.18629(12) 0.97713(16) 0.46754(15) 0.0262(7) Uani 1 1 d . A . H33 H 0.1521 0.9676 0.4449 0.031 Uiso 1 1 calc R . . C34 C 0.20366(14) 1.00963(18) 0.43462(18) 0.0372(8) Uani 1 1 d . . . H34 H 0.1813 1.0230 0.3896 0.045 Uiso 1 1 calc R A . C35 C 0.25374(15) 1.02260(17) 0.4676(2) 0.0371(8) Uani 1 1 d . A . H35 H 0.2654 1.0455 0.4450 0.045 Uiso 1 1 calc R . . C36 C 0.28671(13) 1.00280(16) 0.53236(18) 0.0312(7) Uani 1 1 d . . . H36 H 0.3211 1.0105 0.5540 0.037 Uiso 1 1 calc R A . C37 C 0.26924(11) 0.97116(14) 0.56616(15) 0.0224(6) Uani 1 1 d . A . H37 H 0.2917 0.9583 0.6113 0.027 Uiso 1 1 calc R . . C41 C 0.31273(10) 0.96973(14) 0.82602(13) 0.0166(5) Uani 1 1 d . . . C42 C 0.33520(10) 1.02408(14) 0.86577(13) 0.0189(6) Uani 1 1 d D . . C43 C 0.32922(11) 1.04863(17) 0.91935(15) 0.0276(7) Uani 1 1 d D . . H43A H 0.3277 1.0096 0.9431 0.033 Uiso 1 1 calc R . . H43B H 0.2976 1.0733 0.8984 0.033 Uiso 1 1 calc R . . C44 C 0.37147(13) 1.0943(2) 0.96928(17) 0.0465(11) Uani 1 1 d D . . H44A H 0.3639 1.1137 0.9998 0.056 Uiso 1 1 calc R . . H44B H 0.4021 1.0676 0.9962 0.056 Uiso 1 1 calc R . . C45 C 0.37959(13) 1.1501(2) 0.93506(19) 0.0460(11) Uani 1 1 d D . . H45A H 0.4062 1.1798 0.9690 0.055 Uiso 1 1 calc R . . H45B H 0.3491 1.1771 0.9087 0.055 Uiso 1 1 calc R . . C46 C 0.39357(11) 1.12364(16) 0.88931(15) 0.0261(7) Uani 1 1 d D . . H46A H 0.3909 1.1606 0.8604 0.031 Uiso 1 1 calc R . . H46B H 0.4285 1.1089 0.9168 0.031 Uiso 1 1 calc R . . C47 C 0.36172(9) 1.06591(14) 0.84595(13) 0.0183(6) Uani 1 1 d D . . C48 C 0.35527(9) 1.04719(13) 0.78819(13) 0.0165(5) Uani 1 1 d . . . C49 C 0.37594(10) 1.07881(13) 0.75478(13) 0.0184(6) Uani 1 1 d . . . C50 C 0.42672(11) 1.09223(15) 0.78962(15) 0.0235(6) Uani 1 1 d . . . H50 H 0.4483 1.0790 0.8348 0.028 Uiso 1 1 calc R . . C51 C 0.44534(11) 1.12465(18) 0.75835(16) 0.0312(7) Uani 1 1 d . . . H51 H 0.4796 1.1342 0.7825 0.037 Uiso 1 1 calc R . . C52 C 0.41458(12) 1.14323(17) 0.69230(16) 0.0316(7) Uani 1 1 d . . . H52 H 0.4276 1.1660 0.6714 0.038 Uiso 1 1 calc R . . C53 C 0.36428(12) 1.12843(16) 0.65644(15) 0.0275(7) Uani 1 1 d . . . H53 H 0.3431 1.1403 0.6108 0.033 Uiso 1 1 calc R . . C54 C 0.34530(10) 1.09640(14) 0.68754(14) 0.0219(6) Uani 1 1 d . . . H54 H 0.3111 1.0863 0.6629 0.026 Uiso 1 1 calc R . . C55 C 0.27914(10) 0.91939(14) 0.82338(13) 0.0176(5) Uani 1 1 d . . . C56 C 0.29335(10) 0.87687(14) 0.87942(13) 0.0180(6) Uani 1 1 d . . . C57 C 0.34166(10) 0.88270(14) 0.93964(13) 0.0196(6) Uani 1 1 d . . . H57 H 0.3637 0.9159 0.9432 0.023 Uiso 1 1 calc R . . C58 C 0.35618(10) 0.84127(15) 0.99160(14) 0.0211(6) Uani 1 1 d . . . H58 H 0.3868 0.8490 1.0330 0.025 Uiso 1 1 calc R . . C59 C 0.32614(10) 0.78624(15) 0.98499(14) 0.0204(6) Uani 1 1 d . . . C60 C 0.34463(11) 0.73777(16) 1.03641(14) 0.0246(6) Uani 1 1 d . . . H60 H 0.3749 0.7460 1.0780 0.030 Uiso 1 1 calc R . . C61 C 0.31976(12) 0.67952(16) 1.02721(15) 0.0292(7) Uani 1 1 d . . . H61 H 0.3322 0.6480 1.0624 0.035 Uiso 1 1 calc R . . C62 C 0.27560(12) 0.66668(17) 0.96515(16) 0.0315(7) Uani 1 1 d . . . H62 H 0.2591 0.6252 0.9577 0.038 Uiso 1 1 calc R . . C63 C 0.25609(11) 0.71340(16) 0.91516(15) 0.0274(7) Uani 1 1 d . . . H63 H 0.2263 0.7034 0.8735 0.033 Uiso 1 1 calc R . . C64 C 0.27913(10) 0.77615(15) 0.92408(14) 0.0214(6) Uani 1 1 d . . . C65 C 0.26066(10) 0.82691(15) 0.87250(14) 0.0202(6) Uani 1 1 d . . . C66 C 0.21092(10) 0.82792(16) 0.81249(14) 0.0234(6) Uani 1 1 d . . . C67 C 0.16975(11) 0.79470(18) 0.80398(16) 0.0335(8) Uani 1 1 d . . . H67 H 0.1734 0.7726 0.8409 0.040 Uiso 1 1 calc R . . C68 C 0.12496(13) 0.7936(2) 0.74415(19) 0.0465(10) Uani 1 1 d . . . H68 H 0.0981 0.7701 0.7397 0.056 Uiso 1 1 calc R . . C69 C 0.11838(12) 0.8269(2) 0.68906(18) 0.0469(11) Uani 1 1 d . . . H69 H 0.0878 0.8236 0.6468 0.056 Uiso 1 1 calc R . . C70 C 0.15584(11) 0.86406(18) 0.69628(16) 0.0324(8) Uani 1 1 d . . . H70 H 0.1507 0.8881 0.6593 0.039 Uiso 1 1 calc R . . C71 C 0.20208(10) 0.86724(15) 0.75801(14) 0.0223(6) Uani 1 1 d . . . C72 C 0.35638(10) 0.90685(14) 0.76446(14) 0.0173(5) Uani 1 1 d . . . C73 C 0.33850(11) 0.85564(14) 0.71731(15) 0.0226(6) Uani 1 1 d . . . H73 H 0.3053 0.8568 0.6794 0.027 Uiso 1 1 calc R . . C74 C 0.36920(12) 0.80286(16) 0.72571(17) 0.0315(7) Uani 1 1 d . . . H74 H 0.3569 0.7679 0.6937 0.038 Uiso 1 1 calc R . . C75 C 0.41769(12) 0.80132(17) 0.78073(17) 0.0327(7) Uani 1 1 d . . . H75 H 0.4387 0.7655 0.7863 0.039 Uiso 1 1 calc R . . C76 C 0.43568(12) 0.85191(18) 0.82776(16) 0.0319(7) Uani 1 1 d . . . H76 H 0.4689 0.8505 0.8656 0.038 Uiso 1 1 calc R . . C77 C 0.40543(10) 0.90463(16) 0.82000(15) 0.0238(6) Uani 1 1 d . . . H77 H 0.4180 0.9393 0.8524 0.029 Uiso 1 1 calc R . . C90A C 0.5466(4) 0.9134(4) 0.8385(6) 0.046(2) Uani 0.601(8) 1 d PDU B 1 H90A H 0.5550 0.9325 0.8811 0.055 Uiso 0.601(8) 1 calc PR B 1 H90B H 0.5116 0.9242 0.8040 0.055 Uiso 0.601(8) 1 calc PR B 1 Cl1A Cl 0.5534(3) 0.8270(2) 0.8464(3) 0.0504(13) Uani 0.601(8) 1 d PDU B 1 Cl2A Cl 0.58361(9) 0.95078(11) 0.81718(10) 0.0455(8) Uani 0.601(8) 1 d PDU B 1 C90B C 0.5332(6) 0.9286(6) 0.8487(7) 0.057(4) Uani 0.399(8) 1 d PDU B 2 H90C H 0.4977 0.9333 0.8127 0.068 Uiso 0.399(8) 1 calc PR B 2 H90D H 0.5375 0.9387 0.8914 0.068 Uiso 0.399(8) 1 calc PR B 2 Cl1B Cl 0.5668(2) 0.9868(5) 0.8359(4) 0.146(5) Uani 0.399(8) 1 d PDU B 2 Cl2B Cl 0.5518(4) 0.8448(4) 0.8503(5) 0.061(2) Uani 0.399(8) 1 d PDU B 2 Cu2 Cu 0.48390(7) 0.98571(11) 1.02508(13) 0.0487(8) Uani 0.50 1 d PU C -8 Cl2 Cl 0.54495(11) 1.04059(15) 0.92596(16) 0.0497(9) Uani 0.405(4) 1 d P D -8 Cl3 Cl 0.4933(3) 0.9942(4) 1.0068(3) 0.055(5) Uani 0.367(6) 1 d PU C -8 Cl4 Cl 0.4708(3) 0.9761(3) 1.0537(3) 0.056(3) Uani 0.228(7) 1 d PU C -8 Cu3 Cu 0.03755(4) 1.12282(5) 0.28033(5) 0.0434(2) Uani 0.50 1 d PU E -1 Cl5 Cl 0.07719(7) 1.03576(13) 0.31685(9) 0.0612(7) Uani 0.50 1 d PU E -1 Cl6 Cl 0.0000 1.21181(7) 0.2500 0.0626(5) Uani 1 2 d SU . . C100 C 0.0000 0.9060(4) 0.2500 0.100(3) Uani 1 2 d SDU . . H10A H -0.0307 0.9245 0.2424 0.120 Uiso 0.50 1 calc PR F . H10B H 0.0048 0.9245 0.2164 0.120 Uiso 0.50 1 calc PR . . Cl10 Cl 0.0000 0.82119(11) 0.2500 0.1038(8) Uani 1 2 d SDU F . Cl11 Cl 0.0566(2) 0.9225(4) 0.33967(19) 0.241(4) Uani 0.50 1 d PDU F -1 C101 C -0.1163(6) 0.9698(7) 0.2801(10) 0.065(4) Uani 0.355(3) 1 d PDU G 1 H10C H -0.1197 0.9731 0.3177 0.078 Uiso 0.355(3) 1 calc PR G 1 H10D H -0.1463 0.9900 0.2409 0.078 Uiso 0.355(3) 1 calc PR G 1 Cl12 Cl -0.1164(2) 0.8818(4) 0.2625(3) 0.0665(16) Uani 0.355(3) 1 d PDU G 1 Cl13 Cl -0.0644(3) 1.0216(2) 0.3001(4) 0.136(3) Uani 0.355(3) 1 d PDU G 1 C102 C -0.1321(4) 0.9718(5) 0.2606(5) 0.056(3) Uani 0.508(4) 1 d PDU H 2 H10E H -0.1620 0.9797 0.2601 0.067 Uiso 0.508(4) 1 calc PR H 2 H10F H -0.1312 1.0058 0.2318 0.067 Uiso 0.508(4) 1 calc PR H 2 Cl14 Cl -0.1340(2) 0.8899(3) 0.2302(3) 0.1059(19) Uani 0.508(4) 1 d PDU H 2 Cl15 Cl -0.0774(1) 0.9793(2) 0.3448(1) 0.0800(11) Uani 0.508(4) 1 d PDU H 2 C103 C -0.1156(9) 0.9600(15) 0.2957(12) 0.060(5) Uani 0.137(4) 1 d PDU I 3 H10G H -0.0916 0.9942 0.3014 0.073 Uiso 0.137(4) 1 calc PR I 3 H10H H -0.1161 0.9601 0.3357 0.073 Uiso 0.137(4) 1 calc PR I 3 Cl16 Cl -0.1772(3) 0.9778(5) 0.2211(4) 0.057(3) Uani 0.137(4) 1 d PDU I 3 Cl17 Cl -0.0985(8) 0.8779(12) 0.2832(13) 0.132(7) Uani 0.137(4) 1 d PDU I 3 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 0.01169(16) 0.01631(17) 0.01460(16) 0.00133(12) 0.00688(13) 0.00194(12) P1 0.0126(3) 0.0126(3) 0.0159(3) -0.0005(2) 0.0089(3) 0.0002(2) P2 0.0115(3) 0.0141(3) 0.0156(3) -0.0006(2) 0.0079(3) 0.0001(2) N1 0.0123(10) 0.0153(11) 0.0174(11) -0.0001(9) 0.0087(9) 0.0022(9) N2 0.0139(11) 0.0233(12) 0.0202(12) 0.0033(9) 0.0106(10) 0.0025(9) C1 0.0156(12) 0.0176(13) 0.0149(12) 0.0020(10) 0.0093(11) 0.0021(10) C2 0.0163(13) 0.0193(14) 0.0166(13) 0.0010(10) 0.0094(11) -0.0010(11) C3 0.007(5) 0.027(5) 0.023(6) 0.001(4) 0.004(5) -0.002(4) C4 0.020(3) 0.028(3) 0.029(4) 0.001(3) 0.014(3) 0.000(2) C5 0.018(4) 0.033(5) 0.035(6) -0.008(4) 0.014(4) -0.009(3) C6 0.026(4) 0.022(4) 0.037(6) -0.009(4) 0.016(4) -0.005(3) C7 0.0169(13) 0.0180(14) 0.0214(14) -0.0003(11) 0.0092(12) -0.0026(11) C3' 0.025(7) 0.034(6) 0.045(9) -0.011(6) 0.024(7) 0.001(5) C4' 0.015(3) 0.043(4) 0.045(5) -0.010(4) 0.015(3) -0.005(3) C5' 0.026(5) 0.036(6) 0.051(8) -0.018(5) 0.021(5) -0.015(4) C6' 0.016(3) 0.027(4) 0.016(4) -0.005(3) 0.007(3) -0.006(3) C8 0.0199(13) 0.0152(13) 0.0167(13) -0.0011(10) 0.0108(11) -0.0029(11) C9 0.0175(13) 0.0147(13) 0.0239(14) -0.0007(11) 0.0121(12) -0.0023(11) C10 0.0235(15) 0.0195(14) 0.0250(15) -0.0036(11) 0.0127(13) -0.0031(12) C11 0.0313(16) 0.0208(15) 0.0326(17) -0.0079(12) 0.0212(14) -0.0044(13) C12 0.0281(16) 0.0144(14) 0.0425(18) -0.0024(12) 0.0250(15) 0.0013(12) C13 0.0218(14) 0.0186(14) 0.0307(16) 0.0021(12) 0.0146(13) 0.0018(11) C14 0.0208(14) 0.0161(13) 0.0239(14) -0.0020(11) 0.0133(12) -0.0029(11) C15 0.0126(12) 0.0175(13) 0.0188(13) 0.0006(10) 0.0112(11) 0.0011(10) C16 0.0118(12) 0.0178(13) 0.0182(13) 0.0013(10) 0.0074(11) 0.0007(10) C17 0.0202(14) 0.0214(15) 0.0213(15) -0.0016(11) 0.0083(12) 0.0002(12) C18 0.0189(14) 0.0290(16) 0.0196(14) 0.0032(12) 0.0045(12) 0.0003(12) C19 0.0152(13) 0.0245(15) 0.0275(15) 0.0069(12) 0.0097(12) 0.0033(11) C20 0.0193(14) 0.0356(18) 0.0303(17) 0.0130(14) 0.0128(13) 0.0067(13) C21 0.0274(16) 0.0333(18) 0.0415(19) 0.0186(15) 0.0228(15) 0.0179(14) C22 0.0303(16) 0.0256(16) 0.0440(19) 0.0117(14) 0.0272(16) 0.0124(13) C23 0.0194(14) 0.0232(15) 0.0319(16) 0.0055(12) 0.0173(13) 0.0030(12) C24 0.0140(13) 0.0197(14) 0.0275(15) 0.0047(11) 0.0117(12) 0.0010(11) C25 0.0146(13) 0.0156(13) 0.0236(14) 0.0023(11) 0.0113(12) 0.0010(10) C26 0.0147(12) 0.0179(13) 0.0219(14) -0.0002(11) 0.0126(11) 0.0002(10) C27 0.0204(14) 0.0164(14) 0.0278(15) 0.0011(11) 0.0155(13) 0.0014(11) C28 0.0244(15) 0.0186(14) 0.0280(16) -0.0063(12) 0.0145(13) -0.0037(12) C29 0.0216(14) 0.0260(16) 0.0210(15) -0.0062(12) 0.0068(12) -0.0010(12) C30 0.0189(14) 0.0219(15) 0.0208(14) -0.0004(11) 0.0080(12) 0.0060(11) C31 0.0151(12) 0.0171(13) 0.0199(13) -0.0013(10) 0.0114(11) 0.0005(10) C32 0.0222(14) 0.0124(13) 0.0227(14) -0.0001(10) 0.0165(12) 0.0019(11) C33 0.0266(15) 0.0319(17) 0.0266(16) 0.0071(13) 0.0190(14) 0.0083(13) C34 0.052(2) 0.039(2) 0.0360(19) 0.0169(15) 0.0341(18) 0.0175(17) C35 0.060(2) 0.0251(17) 0.059(2) 0.0039(15) 0.054(2) 0.0004(16) C36 0.0394(19) 0.0246(16) 0.048(2) -0.0082(14) 0.0357(17) -0.0089(14) C37 0.0254(15) 0.0189(14) 0.0289(16) -0.0081(11) 0.0190(13) -0.0041(12) C41 0.0140(12) 0.0208(14) 0.0159(13) 0.0027(10) 0.0091(11) 0.0061(11) C42 0.0120(12) 0.0251(15) 0.0164(13) 0.0015(11) 0.0062(11) 0.0077(11) C43 0.0244(15) 0.0370(18) 0.0249(15) -0.0048(13) 0.0162(13) 0.0064(13) C44 0.0221(16) 0.089(3) 0.0245(17) -0.0239(19) 0.0111(15) 0.0043(18) C45 0.0219(16) 0.058(2) 0.049(2) -0.039(2) 0.0149(16) -0.0066(16) C46 0.0161(14) 0.0261(16) 0.0272(16) -0.0109(12) 0.0070(12) -0.0024(12) C47 0.0119(12) 0.0177(13) 0.0199(14) -0.0024(11) 0.0058(11) 0.0046(10) C48 0.0098(12) 0.0145(13) 0.0188(13) -0.0005(10) 0.0044(11) 0.0010(10) C49 0.0168(13) 0.0157(13) 0.0188(14) -0.0026(10) 0.0078(11) -0.0028(11) C50 0.0178(14) 0.0277(16) 0.0210(14) -0.0011(12) 0.0087(12) -0.0042(12) C51 0.0197(15) 0.0405(19) 0.0308(17) -0.0047(14) 0.0128(14) -0.0124(14) C52 0.0272(16) 0.0388(19) 0.0282(17) 0.0022(14) 0.0154(14) -0.0110(14) C53 0.0273(16) 0.0287(16) 0.0220(15) 0.0025(12) 0.0113(13) -0.0041(13) C54 0.0172(13) 0.0212(14) 0.0214(14) -0.0007(11) 0.0075(12) -0.0049(11) C55 0.0156(13) 0.0226(14) 0.0192(13) 0.0027(11) 0.0127(11) 0.0054(11) C56 0.0161(13) 0.0216(14) 0.0192(14) 0.0013(11) 0.0118(12) 0.0039(11) C57 0.0168(13) 0.0238(15) 0.0193(14) -0.0007(11) 0.0110(12) 0.0017(11) C58 0.0184(13) 0.0269(15) 0.0166(13) -0.0015(11) 0.0093(12) 0.0039(12) C59 0.0209(14) 0.0262(15) 0.0168(13) 0.0024(11) 0.0124(12) 0.0052(12) C60 0.0237(15) 0.0312(17) 0.0166(14) 0.0039(12) 0.0100(12) 0.0063(13) C61 0.0341(17) 0.0310(17) 0.0226(15) 0.0091(13) 0.0162(14) 0.0052(14) C62 0.0335(17) 0.0311(17) 0.0266(16) 0.0071(13) 0.0151(14) -0.0023(14) C63 0.0245(15) 0.0333(17) 0.0212(15) 0.0047(12) 0.0111(13) -0.0007(13) C64 0.0205(14) 0.0286(16) 0.0187(14) 0.0038(11) 0.0134(12) 0.0030(12) C65 0.0187(13) 0.0269(15) 0.0183(14) 0.0030(11) 0.0125(12) 0.0041(12) C66 0.0168(13) 0.0334(17) 0.0205(14) 0.0059(12) 0.0109(12) 0.0000(12) C67 0.0220(15) 0.047(2) 0.0294(17) 0.0164(15) 0.0136(14) -0.0017(14) C68 0.0202(16) 0.067(3) 0.041(2) 0.0241(19) 0.0109(16) -0.0090(17) C69 0.0176(15) 0.074(3) 0.0300(18) 0.0205(18) 0.0019(14) -0.0120(17) C70 0.0177(15) 0.049(2) 0.0232(16) 0.0143(14) 0.0071(13) -0.0023(14) C71 0.0149(13) 0.0300(16) 0.0214(14) 0.0061(12) 0.0099(12) 0.0009(12) C72 0.0155(13) 0.0173(13) 0.0225(14) 0.0023(11) 0.0128(12) 0.0028(10) C73 0.0206(14) 0.0180(14) 0.0265(15) -0.0011(11) 0.0118(13) 0.0002(11) C74 0.0367(18) 0.0213(16) 0.0358(18) -0.0045(13) 0.0202(16) 0.0047(13) C75 0.0317(17) 0.0299(17) 0.0388(19) 0.0037(14) 0.0214(16) 0.0150(14) C76 0.0203(15) 0.0412(19) 0.0297(17) 0.0033(14) 0.0115(14) 0.0120(14) C77 0.0173(14) 0.0304(16) 0.0219(15) -0.0027(12) 0.0100(12) 0.0035(12) C90A 0.057(6) 0.044(4) 0.040(4) 0.003(3) 0.029(4) -0.007(4) Cl1A 0.0360(13) 0.0371(15) 0.082(3) 0.0205(18) 0.0358(19) 0.0064(12) Cl2A 0.0462(12) 0.0423(11) 0.0520(11) -0.0007(7) 0.0303(9) -0.0127(8) C90B 0.051(9) 0.062(7) 0.027(7) 0.014(6) 0.005(5) -0.022(6) Cl1B 0.069(3) 0.146(7) 0.148(6) 0.093(6) 0.019(3) -0.036(4) Cl2B 0.038(3) 0.089(5) 0.053(3) -0.024(4) 0.024(2) -0.008(4) Cu2 0.0415(7) 0.0323(6) 0.0604(16) 0.0061(8) 0.0218(7) 0.0176(5) Cl2 0.0325(13) 0.0399(14) 0.0397(15) -0.0078(11) -0.0014(11) 0.0079(11) Cl3 0.050(5) 0.037(4) 0.031(4) -0.014(3) -0.006(3) 0.019(3) Cl4 0.056(3) 0.047(3) 0.046(3) 0.004(2) 0.018(3) 0.020(2) Cu3 0.0433(5) 0.0517(6) 0.0372(5) -0.0090(4) 0.0240(4) 0.0000(4) Cl5 0.0376(10) 0.1041(18) 0.0260(9) -0.0095(10) 0.0086(8) 0.0385(11) Cl6 0.1187(15) 0.0350(7) 0.0643(10) 0.000 0.0700(11) 0.000 C100 0.076(6) 0.085(5) 0.120(7) 0.000 0.045(5) 0.000 Cl10 0.167(2) 0.0627(12) 0.160(2) 0.000 0.140(2) 0.000 Cl11 0.179(4) 0.491(11) 0.071(2) -0.118(4) 0.081(3) -0.248(6) C101 0.066(6) 0.092(6) 0.054(7) 0.022(6) 0.043(6) 0.024(5) Cl12 0.054(4) 0.100(3) 0.063(3) -0.012(3) 0.043(3) 0.003(3) Cl13 0.177(5) 0.070(3) 0.265(7) 0.043(4) 0.188(6) 0.039(3) C102 0.061(6) 0.071(5) 0.036(5) 0.025(4) 0.027(4) 0.007(5) Cl14 0.087(3) 0.086(3) 0.145(5) -0.046(3) 0.066(3) -0.035(3) Cl15 0.0617(15) 0.127(2) 0.0339(12) 0.0104(12) 0.0169(11) 0.0435(15) C103 0.065(7) 0.094(7) 0.043(8) 0.029(7) 0.043(6) 0.007(7) Cl16 0.058(4) 0.077(6) 0.057(5) 0.005(4) 0.046(4) -0.004(4) Cl17 0.090(11) 0.095(8) 0.160(13) 0.001(9) 0.041(9) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.090(2) . ? Cu1 N1 2.105(2) . ? Cu1 P1 2.2952(7) . ? Cu1 P2 2.2979(7) . ? P1 C1 1.801(3) . ? P1 C8 1.809(3) . ? P1 C32 1.829(3) . ? P2 C48 1.806(3) . ? P2 C41 1.808(3) . ? P2 C72 1.824(3) . ? N1 C15 1.324(3) . ? N1 C31 1.384(3) . ? N2 C55 1.332(4) . ? N2 C71 1.386(4) . ? C1 C2 1.359(4) . ? C1 C15 1.466(4) . ? C2 C7 1.468(4) . ? C2 C3' 1.515(10) . ? C2 C3 1.518(10) . ? C3 C4 1.505(11) . ? C4 C5 1.529(12) . ? C5 C6 1.518(11) . ? C6 C7 1.525(9) . ? C7 C8 1.359(4) . ? C7 C6' 1.526(9) . ? C3' C4' 1.522(13) . ? C4' C5' 1.522(12) . ? C5' C6' 1.521(12) . ? C8 C9 1.475(4) . ? C9 C14 1.400(4) . ? C9 C10 1.402(4) . ? C10 C11 1.388(4) . ? C11 C12 1.384(5) . ? C12 C13 1.389(4) . ? C13 C14 1.386(4) . ? C15 C16 1.438(4) . ? C16 C25 1.410(4) . ? C16 C17 1.433(4) . ? C17 C18 1.349(4) . ? C18 C19 1.418(4) . ? C19 C20 1.421(4) . ? C19 C24 1.427(4) . ? C20 C21 1.366(5) . ? C21 C22 1.389(5) . ? C22 C23 1.367(4) . ? C23 C24 1.419(4) . ? C24 C25 1.452(4) . ? C25 C26 1.443(4) . ? C26 C27 1.418(4) . ? C26 C31 1.431(4) . ? C27 C28 1.366(4) . ? C28 C29 1.402(4) . ? C29 C30 1.370(4) . ? C30 C31 1.404(4) . ? C32 C37 1.390(4) . ? C32 C33 1.395(4) . ? C33 C34 1.386(4) . ? C34 C35 1.387(5) . ? C35 C36 1.374(5) . ? C36 C37 1.398(4) . ? C41 C42 1.360(4) . ? C41 C55 1.469(4) . ? C42 C47 1.476(4) . ? C42 C43 1.513(4) . ? C43 C44 1.525(5) . ? C44 C45 1.506(6) . ? C45 C46 1.526(4) . ? C46 C47 1.512(4) . ? C47 C48 1.356(4) . ? C48 C49 1.471(4) . ? C49 C54 1.399(4) . ? C49 C50 1.405(4) . ? C50 C51 1.383(4) . ? C51 C52 1.382(5) . ? C52 C53 1.396(4) . ? C53 C54 1.385(4) . ? C55 C56 1.445(4) . ? C56 C65 1.405(4) . ? C56 C57 1.431(4) . ? C57 C58 1.355(4) . ? C58 C59 1.425(4) . ? C59 C60 1.420(4) . ? C59 C64 1.425(4) . ? C60 C61 1.365(5) . ? C61 C62 1.404(5) . ? C62 C63 1.372(4) . ? C63 C64 1.416(4) . ? C64 C65 1.454(4) . ? C65 C66 1.450(4) . ? C66 C67 1.415(4) . ? C66 C71 1.426(4) . ? C67 C68 1.364(5) . ? C68 C69 1.404(5) . ? C69 C70 1.362(5) . ? C70 C71 1.409(4) . ? C72 C73 1.396(4) . ? C72 C77 1.400(4) . ? C73 C74 1.393(4) . ? C74 C75 1.384(5) . ? C75 C76 1.385(5) . ? C76 C77 1.386(4) . ? C90A Cl1A 1.735(8) . ? C90A Cl2A 1.744(8) . ? C90B Cl1B 1.751(12) . ? C90B Cl2B 1.776(13) . ? Cu2 Cl3 0.694(5) . ? Cu2 Cl4 1.027(11) . ? Cl3 Cl4 1.720(12) . ? Cu3 Cl6 2.0476(16) . ? Cu3 Cl5 2.048(2) . ? Cl6 Cu3 2.0476(16) 2 ? C100 Cl10 1.694(9) . ? C100 Cl11 1.933(4) 2 ? C100 Cl11 1.933(4) . ? C101 Cl12 1.808(13) . ? C101 Cl13 1.810(14) . ? C102 Cl14 1.783(10) . ? C102 Cl15 1.811(9) . ? C103 Cl17 1.814(16) . ? C103 Cl16 1.833(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 120.28(9) . . ? N2 Cu1 P1 125.91(7) . . ? N1 Cu1 P1 86.28(6) . . ? N2 Cu1 P2 86.33(6) . . ? N1 Cu1 P2 122.51(6) . . ? P1 Cu1 P2 119.96(3) . . ? C1 P1 C8 91.14(13) . . ? C1 P1 C32 104.78(12) . . ? C8 P1 C32 105.74(12) . . ? C1 P1 Cu1 90.60(9) . . ? C8 P1 Cu1 137.41(9) . . ? C32 P1 Cu1 114.86(9) . . ? C48 P2 C41 91.35(13) . . ? C48 P2 C72 104.27(12) . . ? C41 P2 C72 105.60(12) . . ? C48 P2 Cu1 132.91(9) . . ? C41 P2 Cu1 90.13(9) . . ? C72 P2 Cu1 120.51(9) . . ? C15 N1 C31 118.5(2) . . ? C15 N1 Cu1 115.68(17) . . ? C31 N1 Cu1 124.96(17) . . ? C55 N2 C71 118.6(2) . . ? C55 N2 Cu1 115.91(18) . . ? C71 N2 Cu1 125.39(18) . . ? C2 C1 C15 131.6(2) . . ? C2 C1 P1 110.3(2) . . ? C15 C1 P1 117.05(19) . . ? C1 C2 C7 113.6(2) . . ? C1 C2 C3' 127.4(5) . . ? C7 C2 C3' 118.4(5) . . ? C1 C2 C3 124.4(5) . . ? C7 C2 C3 121.9(5) . . ? C3' C2 C3 5.1(12) . . ? C4 C3 C2 113.7(8) . . ? C3 C4 C5 109.0(9) . . ? C6 C5 C4 109.9(9) . . ? C5 C6 C7 114.8(8) . . ? C8 C7 C2 114.5(2) . . ? C8 C7 C6 126.7(4) . . ? C2 C7 C6 117.2(4) . . ? C8 C7 C6' 123.4(4) . . ? C2 C7 C6' 121.4(4) . . ? C6 C7 C6' 19.9(4) . . ? C2 C3' C4' 113.0(8) . . ? C5' C4' C3' 112.5(10) . . ? C6' C5' C4' 110.3(10) . . ? C5' C6' C7 109.4(8) . . ? C7 C8 C9 128.8(3) . . ? C7 C8 P1 109.7(2) . . ? C9 C8 P1 121.4(2) . . ? C14 C9 C10 118.4(3) . . ? C14 C9 C8 119.8(2) . . ? C10 C9 C8 121.8(3) . . ? C11 C10 C9 120.3(3) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 119.5(3) . . ? C14 C13 C12 120.2(3) . . ? C13 C14 C9 120.8(3) . . ? N1 C15 C16 123.0(2) . . ? N1 C15 C1 115.5(2) . . ? C16 C15 C1 121.4(2) . . ? C25 C16 C17 120.3(2) . . ? C25 C16 C15 119.4(2) . . ? C17 C16 C15 120.3(2) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C19 120.7(3) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 C24 120.3(3) . . ? C20 C19 C24 119.5(3) . . ? C21 C20 C19 120.2(3) . . ? C20 C21 C22 120.5(3) . . ? C23 C22 C21 120.8(3) . . ? C22 C23 C24 121.1(3) . . ? C23 C24 C19 117.3(3) . . ? C23 C24 C25 124.5(3) . . ? C19 C24 C25 118.1(3) . . ? C16 C25 C26 117.0(2) . . ? C16 C25 C24 118.0(2) . . ? C26 C25 C24 124.9(3) . . ? C27 C26 C31 116.3(2) . . ? C27 C26 C25 124.9(2) . . ? C31 C26 C25 118.4(2) . . ? C28 C27 C26 122.2(3) . . ? C27 C28 C29 120.5(3) . . ? C30 C29 C28 119.5(3) . . ? C29 C30 C31 121.1(3) . . ? N1 C31 C30 117.4(2) . . ? N1 C31 C26 122.5(2) . . ? C30 C31 C26 120.2(2) . . ? C37 C32 C33 119.7(3) . . ? C37 C32 P1 120.5(2) . . ? C33 C32 P1 119.7(2) . . ? C34 C33 C32 119.9(3) . . ? C33 C34 C35 119.9(3) . . ? C36 C35 C34 120.9(3) . . ? C35 C36 C37 119.4(3) . . ? C32 C37 C36 120.2(3) . . ? C42 C41 C55 131.8(3) . . ? C42 C41 P2 110.0(2) . . ? C55 C41 P2 116.6(2) . . ? C41 C42 C47 113.6(2) . . ? C41 C42 C43 126.2(3) . . ? C47 C42 C43 119.6(3) . . ? C42 C43 C44 112.2(3) . . ? C45 C44 C43 111.6(3) . . ? C44 C45 C46 112.0(3) . . ? C47 C46 C45 113.5(3) . . ? C48 C47 C42 114.5(2) . . ? C48 C47 C46 125.1(3) . . ? C42 C47 C46 120.4(2) . . ? C47 C48 C49 127.8(2) . . ? C47 C48 P2 109.9(2) . . ? C49 C48 P2 122.3(2) . . ? C54 C49 C50 118.6(3) . . ? C54 C49 C48 120.5(2) . . ? C50 C49 C48 120.9(2) . . ? C51 C50 C49 120.2(3) . . ? C52 C51 C50 120.7(3) . . ? C51 C52 C53 119.8(3) . . ? C54 C53 C52 119.9(3) . . ? C53 C54 C49 120.8(3) . . ? N2 C55 C56 122.5(3) . . ? N2 C55 C41 115.1(2) . . ? C56 C55 C41 122.1(2) . . ? C65 C56 C57 120.6(2) . . ? C65 C56 C55 119.4(2) . . ? C57 C56 C55 119.9(3) . . ? C58 C57 C56 120.5(3) . . ? C57 C58 C59 120.8(3) . . ? C60 C59 C58 120.3(3) . . ? C60 C59 C64 119.5(3) . . ? C58 C59 C64 119.9(3) . . ? C61 C60 C59 121.3(3) . . ? C60 C61 C62 119.3(3) . . ? C63 C62 C61 120.7(3) . . ? C62 C63 C64 121.7(3) . . ? C63 C64 C59 117.0(3) . . ? C63 C64 C65 124.1(3) . . ? C59 C64 C65 118.5(3) . . ? C56 C65 C66 117.3(2) . . ? C56 C65 C64 118.5(3) . . ? C66 C65 C64 124.2(3) . . ? C67 C66 C71 116.9(3) . . ? C67 C66 C65 125.4(3) . . ? C71 C66 C65 117.7(3) . . ? C68 C67 C66 121.8(3) . . ? C67 C68 C69 120.2(3) . . ? C70 C69 C68 120.0(3) . . ? C69 C70 C71 120.7(3) . . ? N2 C71 C70 117.8(3) . . ? N2 C71 C66 122.3(3) . . ? C70 C71 C66 119.8(3) . . ? C73 C72 C77 119.3(3) . . ? C73 C72 P2 120.0(2) . . ? C77 C72 P2 120.7(2) . . ? C74 C73 C72 120.2(3) . . ? C75 C74 C73 120.0(3) . . ? C74 C75 C76 120.2(3) . . ? C75 C76 C77 120.4(3) . . ? C76 C77 C72 120.0(3) . . ? Cl1A C90A Cl2A 113.0(5) . . ? Cl1B C90B Cl2B 112.6(10) . . ? Cl3 Cu2 Cl4 176.3(8) . . ? Cu2 Cl3 Cl4 2.2(4) . . ? Cu2 Cl4 Cl3 1.5(3) . . ? Cl6 Cu3 Cl5 176.32(7) . . ? Cu3 Cl6 Cu3 59.61(7) 2 . ? Cl10 C100 Cl11 99.8(4) . 2 ? Cl10 C100 Cl11 99.8(4) . . ? Cl11 C100 Cl11 160.4(7) 2 . ? Cl12 C101 Cl13 119.5(10) . . ? Cl14 C102 Cl15 109.1(6) . . ? Cl17 C103 Cl16 106.4(15) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.580 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.076 #===END #===END # Attachment 'compound4a.cif' data_compound4a _database_code_depnum_ccdc_archive 'CCDC 651121' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76.50 H61 Cl5 Cu F6 N2 P3' _chemical_formula_weight 1455.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.431(2) _cell_length_b 21.614(3) _cell_length_c 22.007(3) _cell_angle_alpha 82.315(4) _cell_angle_beta 85.456(5) _cell_angle_gamma 75.858(4) _cell_volume 6588.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2988 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 CCD _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 37977 _diffrn_reflns_av_R_equivalents 0.0996 _diffrn_reflns_av_sigmaI/netI 0.1611 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 18196 _reflns_number_gt 9642 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A twist disorder on two positions of one cyclohexane system, a disorder on two positions of one helical aromatic system and a disorder of a non coordinated dichloromethane molecule on three positions are refined anisotropically with the help of 788 ADP- and distances-restraints. ; _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^)+(0.0992P)^2^+12.0911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18196 _refine_ls_number_parameters 1914 _refine_ls_number_restraints 788 _refine_ls_R_factor_all 0.1628 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2282 _refine_ls_wR_factor_gt 0.1887 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _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 0.29206(7) 0.47364(4) 0.74810(5) 0.0249(3) Uani 1 1 d . . . Cu2 Cu 0.69004(7) 0.00674(4) 0.74324(5) 0.0240(3) Uani 1 1 d . . . P1 P 0.19142(15) 0.40389(10) 0.75263(10) 0.0265(5) Uani 1 1 d . A . P2 P 0.39145(15) 0.46203(10) 0.82797(10) 0.0250(5) Uani 1 1 d . . . P3 P 0.59517(16) 0.00378(10) 0.66613(10) 0.0264(5) Uani 1 1 d . . . P4 P 0.78252(15) 0.08054(10) 0.73186(11) 0.0259(5) Uani 1 1 d . . . N1 N 0.3350(5) 0.4482(3) 0.6603(3) 0.0247(16) Uani 1 1 d . A . N2 N 0.2612(4) 0.5715(3) 0.7538(3) 0.0242(16) Uani 1 1 d . . . N3 N 0.5658(4) 0.0119(3) 0.7994(3) 0.0243(16) Uani 1 1 d . . . N4 N 0.8120(4) -0.0627(3) 0.7702(3) 0.0214(16) Uani 1 1 d . . . C1 C 0.1884(6) 0.4148(4) 0.6715(4) 0.030(2) Uani 1 1 d . A . C2 C 0.0982(6) 0.4267(4) 0.6526(4) 0.034(2) Uani 1 1 d DU . . C3 C 0.0696(11) 0.448(3) 0.5873(7) 0.043(6) Uani 0.59(2) 1 d PDU A 1 H3A H 0.1113 0.4187 0.5604 0.052 Uiso 0.59(2) 1 calc PR A 1 H3B H 0.0815 0.4916 0.5750 0.052 Uiso 0.59(2) 1 calc PR A 1 C4 C -0.0338(12) 0.4510(13) 0.5765(8) 0.067(6) Uani 0.59(2) 1 d PDU A 1 H4A H -0.0393 0.4079 0.5691 0.081 Uiso 0.59(2) 1 calc PR A 1 H4B H -0.0535 0.4811 0.5393 0.081 Uiso 0.59(2) 1 calc PR A 1 C5 C -0.1015(13) 0.4728(11) 0.6308(8) 0.067(6) Uani 0.59(2) 1 d PDU A 1 H5A H -0.0976 0.5163 0.6381 0.081 Uiso 0.59(2) 1 calc PR A 1 H5B H -0.1682 0.4747 0.6214 0.081 Uiso 0.59(2) 1 calc PR A 1 C6 C -0.0740(9) 0.4260(14) 0.6872(8) 0.055(7) Uani 0.59(2) 1 d PDU A 1 H6A H -0.0813 0.3832 0.6802 0.066 Uiso 0.59(2) 1 calc PR A 1 H6B H -0.1179 0.4403 0.7222 0.066 Uiso 0.59(2) 1 calc PR A 1 C7 C 0.0284(6) 0.4204(4) 0.7036(4) 0.037(2) Uani 1 1 d DU A . C3' C 0.0644(12) 0.455(4) 0.5890(11) 0.050(9) Uani 0.41(2) 1 d PDU A 2 H3'1 H 0.0801 0.4202 0.5618 0.060 Uiso 0.41(2) 1 calc PR A 2 H3'2 H 0.0996 0.4877 0.5721 0.060 Uiso 0.41(2) 1 calc PR A 2 C4' C -0.0426(14) 0.4850(13) 0.5880(11) 0.050(7) Uani 0.41(2) 1 d PDU A 2 H4'1 H -0.0640 0.4904 0.5456 0.060 Uiso 0.41(2) 1 calc PR A 2 H4'2 H -0.0562 0.5280 0.6024 0.060 Uiso 0.41(2) 1 calc PR A 2 C5' C -0.0966(17) 0.4417(15) 0.6301(10) 0.061(7) Uani 0.41(2) 1 d PDU A 2 H5'1 H -0.1661 0.4565 0.6238 0.074 Uiso 0.41(2) 1 calc PR A 2 H5'2 H -0.0749 0.3970 0.6201 0.074 Uiso 0.41(2) 1 calc PR A 2 C6' C -0.0777(11) 0.4445(18) 0.6954(9) 0.056(8) Uani 0.41(2) 1 d PDU A 2 H6'1 H -0.1131 0.4173 0.7232 0.067 Uiso 0.41(2) 1 calc PR A 2 H6'2 H -0.0995 0.4892 0.7055 0.067 Uiso 0.41(2) 1 calc PR A 2 C8 C 0.0660(6) 0.4047(4) 0.7594(4) 0.026(2) Uani 1 1 d . . . C9 C 0.0097(6) 0.3951(4) 0.8177(4) 0.032(2) Uani 1 1 d . A . C10 C -0.0460(7) 0.3504(5) 0.8256(4) 0.052(3) Uani 1 1 d . . . H10 H -0.0450 0.3243 0.7939 0.062 Uiso 1 1 calc R A . C11 C -0.1022(8) 0.3427(5) 0.8777(5) 0.061(3) Uani 1 1 d . A . H11 H -0.1430 0.3139 0.8810 0.073 Uiso 1 1 calc R . . C12 C -0.0989(7) 0.3774(5) 0.9252(5) 0.047(3) Uani 1 1 d . . . H12 H -0.1371 0.3719 0.9618 0.056 Uiso 1 1 calc R A . C13 C -0.0419(7) 0.4192(5) 0.9204(5) 0.047(3) Uani 1 1 d . A . H13 H -0.0390 0.4420 0.9540 0.056 Uiso 1 1 calc R . . C14 C 0.0122(6) 0.4289(4) 0.8667(5) 0.039(2) Uani 1 1 d . . . H14 H 0.0513 0.4589 0.8633 0.046 Uiso 1 1 calc R A . C15 C 0.2761(6) 0.4195(4) 0.6351(4) 0.035(2) Uani 1 1 d DU . . C16 C 0.3078(11) 0.3814(8) 0.5859(7) 0.041(3) Uani 0.598(7) 1 d PDU A 1 H16 H 0.2671 0.3623 0.5665 0.050 Uiso 0.598(7) 1 calc PR A 1 C17 C 0.3962(10) 0.3756(8) 0.5704(7) 0.045(3) Uani 0.598(7) 1 d PDU A 1 H17 H 0.4300 0.3376 0.5538 0.053 Uiso 0.598(7) 1 calc PR A 1 C18 C 0.4487(13) 0.4243(16) 0.5770(13) 0.034(2) Uani 0.598(7) 1 d PDU A 1 C19 C 0.5429(17) 0.4264(19) 0.5496(18) 0.0347(19) Uani 0.598(7) 1 d PDU A 1 C20 C 0.5777(10) 0.4009(8) 0.4922(6) 0.034(2) Uani 0.598(7) 1 d PDU A 1 C21 C 0.5372(11) 0.3671(8) 0.4552(6) 0.048(3) Uani 0.598(7) 1 d PDU A 1 H21 H 0.4744 0.3631 0.4684 0.058 Uiso 0.598(7) 1 calc PR A 1 C22 C 0.5718(11) 0.3401(7) 0.4052(7) 0.050(3) Uani 0.598(7) 1 d PDU A 1 H22 H 0.5367 0.3171 0.3858 0.060 Uiso 0.598(7) 1 calc PR A 1 C23 C 0.6586(11) 0.3466(8) 0.3830(7) 0.048(3) Uani 0.598(7) 1 d PDU A 1 H23 H 0.6853 0.3291 0.3464 0.058 Uiso 0.598(7) 1 calc PR A 1 C24 C 0.7093(11) 0.3785(8) 0.4132(7) 0.051(3) Uani 0.598(7) 1 d PDU A 1 H24 H 0.7721 0.3805 0.3982 0.062 Uiso 0.598(7) 1 calc PR A 1 C25 C 0.6698(10) 0.4083(9) 0.4659(7) 0.042(2) Uani 0.598(7) 1 d PDU A 1 C26 C 0.7133(11) 0.4509(8) 0.4899(7) 0.041(3) Uani 0.598(7) 1 d PDU A 1 H26 H 0.7706 0.4593 0.4700 0.050 Uiso 0.598(7) 1 calc PR A 1 C27 C 0.6766(11) 0.4806(8) 0.5403(7) 0.038(2) Uani 0.598(7) 1 d PDU A 1 H27 H 0.7063 0.5105 0.5540 0.046 Uiso 0.598(7) 1 calc PR A 1 C28 C 0.592(2) 0.466(2) 0.5726(19) 0.034(2) Uani 0.598(7) 1 d PDU A 1 C29 C 0.5574(13) 0.4944(7) 0.6281(7) 0.029(3) Uani 0.598(7) 1 d PDU A 1 H29 H 0.5934 0.5189 0.6447 0.035 Uiso 0.598(7) 1 calc PR A 1 C30 C 0.4734(13) 0.4864(8) 0.6570(8) 0.027(3) Uani 0.598(7) 1 d PDU A 1 H30 H 0.4520 0.5032 0.6947 0.033 Uiso 0.598(7) 1 calc PR A 1 C16' C 0.2988(12) 0.4101(12) 0.5716(8) 0.036(3) Uani 0.402(7) 1 d PDU A 2 H16' H 0.2487 0.4075 0.5473 0.043 Uiso 0.402(7) 1 calc PR A 2 C17' C 0.3840(11) 0.4049(9) 0.5457(9) 0.033(3) Uani 0.402(7) 1 d PDU A 2 H17' H 0.3962 0.3913 0.5059 0.040 Uiso 0.402(7) 1 calc PR A 2 C18' C 0.4617(18) 0.419(2) 0.5761(19) 0.033(2) Uani 0.402(7) 1 d PDU A 2 C19' C 0.553(2) 0.425(3) 0.546(3) 0.035(2) Uani 0.402(7) 1 d PDU A 2 C20' C 0.6138(15) 0.3753(10) 0.5127(11) 0.043(2) Uani 0.402(7) 1 d PDU A 2 C21' C 0.5939(13) 0.3166(10) 0.5043(12) 0.055(3) Uani 0.402(7) 1 d PDU A 2 H21' H 0.5338 0.3096 0.5204 0.066 Uiso 0.402(7) 1 calc PR A 2 C22' C 0.6513(17) 0.2697(12) 0.4758(13) 0.069(4) Uani 0.402(7) 1 d PDU A 2 H22' H 0.6310 0.2317 0.4727 0.083 Uiso 0.402(7) 1 calc PR A 2 C23' C 0.7373(18) 0.2758(13) 0.4516(14) 0.074(4) Uani 0.402(7) 1 d PDU A 2 H23' H 0.7755 0.2431 0.4293 0.089 Uiso 0.402(7) 1 calc PR A 2 C24' C 0.7713(17) 0.3291(12) 0.4586(13) 0.065(4) Uani 0.402(7) 1 d PDU A 2 H24' H 0.8350 0.3315 0.4461 0.079 Uiso 0.402(7) 1 calc PR A 2 C25' C 0.7063(15) 0.3795(11) 0.4853(12) 0.050(3) Uani 0.402(7) 1 d PDU A 2 C26' C 0.7427(15) 0.4283(11) 0.5027(11) 0.041(3) Uani 0.402(7) 1 d PDU A 2 H26' H 0.8011 0.4360 0.4839 0.050 Uiso 0.402(7) 1 calc PR A 2 C27' C 0.6958(13) 0.4646(10) 0.5460(9) 0.039(3) Uani 0.402(7) 1 d PDU A 2 H27' H 0.7293 0.4905 0.5630 0.047 Uiso 0.402(7) 1 calc PR A 2 C28' C 0.600(3) 0.467(3) 0.568(3) 0.034(2) Uani 0.402(7) 1 d PDU A 2 C29' C 0.5532(19) 0.5080(12) 0.6125(11) 0.031(3) Uani 0.402(7) 1 d PDU A 2 H29' H 0.5797 0.5421 0.6205 0.037 Uiso 0.402(7) 1 calc PR A 2 C30' C 0.472(2) 0.4989(13) 0.6437(12) 0.028(3) Uani 0.402(7) 1 d PDU A 2 H30' H 0.4470 0.5239 0.6762 0.034 Uiso 0.402(7) 1 calc PR A 2 C31 C 0.4198(6) 0.4530(4) 0.6302(4) 0.0257(16) Uani 1 1 d U . . C32 C 0.2546(6) 0.3209(4) 0.7758(4) 0.034(2) Uani 1 1 d . . . C33 C 0.2497(8) 0.2947(5) 0.8339(5) 0.061(3) Uani 1 1 d . A . H33 H 0.2112 0.3188 0.8638 0.074 Uiso 1 1 calc R . . C34 C 0.3014(11) 0.2316(6) 0.8509(7) 0.083(4) Uani 1 1 d . . . H34 H 0.2980 0.2138 0.8927 0.099 Uiso 1 1 calc R A . C35 C 0.3544(10) 0.1964(6) 0.8107(8) 0.078(4) Uani 1 1 d . A . H35 H 0.3856 0.1529 0.8229 0.094 Uiso 1 1 calc R . . C36 C 0.3641(9) 0.2230(5) 0.7516(7) 0.076(4) Uani 1 1 d . . . H36 H 0.4047 0.1988 0.7227 0.091 Uiso 1 1 calc R A . C37 C 0.3148(8) 0.2853(5) 0.7337(6) 0.066(3) Uani 1 1 d . A . H37 H 0.3219 0.3040 0.6926 0.079 Uiso 1 1 calc R . . C201 C 0.4061(6) 0.5424(4) 0.8047(4) 0.026(2) Uani 1 1 d . . . C202 C 0.5016(6) 0.5419(3) 0.7991(4) 0.025(2) Uani 1 1 d D . . C203 C 0.5433(5) 0.5959(4) 0.7663(4) 0.030(2) Uani 1 1 d D . . H20A H 0.5374 0.5977 0.7216 0.036 Uiso 1 1 calc R . . H20B H 0.5054 0.6372 0.7793 0.036 Uiso 1 1 calc R . . C204 C 0.6471(6) 0.5885(4) 0.7790(4) 0.037(2) Uani 1 1 d D . . H20C H 0.6515 0.5979 0.8213 0.044 Uiso 1 1 calc R . . H20D H 0.6736 0.6198 0.7503 0.044 Uiso 1 1 calc R . . C205 C 0.7057(6) 0.5209(4) 0.7717(4) 0.035(2) Uani 1 1 d D . . H20E H 0.6997 0.5108 0.7298 0.042 Uiso 1 1 calc R . . H20F H 0.7740 0.5185 0.7770 0.042 Uiso 1 1 calc R . . C206 C 0.6723(5) 0.4727(4) 0.8179(4) 0.030(2) Uani 1 1 d D . . H20G H 0.6914 0.4774 0.8589 0.036 Uiso 1 1 calc R . . H20H H 0.7051 0.4291 0.8082 0.036 Uiso 1 1 calc R . . C207 C 0.5651(5) 0.4790(3) 0.8204(4) 0.0215(19) Uani 1 1 d D . . C208 C 0.5173(6) 0.4331(4) 0.8394(4) 0.025(2) Uani 1 1 d . . . C209 C 0.5557(6) 0.3672(4) 0.8690(4) 0.027(2) Uani 1 1 d . . . C210 C 0.6277(6) 0.3541(4) 0.9106(4) 0.033(2) Uani 1 1 d . . . H210 H 0.6551 0.3877 0.9185 0.039 Uiso 1 1 calc R . . C211 C 0.6601(6) 0.2928(4) 0.9407(4) 0.033(2) Uani 1 1 d . . . H211 H 0.7102 0.2844 0.9683 0.040 Uiso 1 1 calc R . . C212 C 0.6188(6) 0.2442(4) 0.9301(4) 0.037(2) Uani 1 1 d . . . H212 H 0.6406 0.2022 0.9508 0.045 Uiso 1 1 calc R . . C213 C 0.5478(7) 0.2555(4) 0.8906(5) 0.048(3) Uani 1 1 d . . . H213 H 0.5198 0.2217 0.8837 0.058 Uiso 1 1 calc R . . C214 C 0.5157(6) 0.3173(4) 0.8600(4) 0.036(2) Uani 1 1 d . . . H214 H 0.4656 0.3252 0.8325 0.044 Uiso 1 1 calc R . . C215 C 0.3248(6) 0.5918(4) 0.7813(4) 0.023(2) Uani 1 1 d . . . C216 C 0.3093(6) 0.6570(4) 0.7917(4) 0.031(2) Uani 1 1 d . . . H216 H 0.3512 0.6697 0.8161 0.037 Uiso 1 1 calc R . . C217 C 0.2352(6) 0.7004(4) 0.7668(4) 0.027(2) Uani 1 1 d . . . H217 H 0.2231 0.7435 0.7756 0.033 Uiso 1 1 calc R . . C218 C 0.1736(5) 0.6833(4) 0.7273(4) 0.024(2) Uani 1 1 d . . . C219 C 0.0987(6) 0.7275(4) 0.6936(4) 0.027(2) Uani 1 1 d . . . C220 C 0.0926(6) 0.7960(4) 0.6772(4) 0.027(2) Uani 1 1 d . . . C221 C 0.1682(6) 0.8269(4) 0.6812(4) 0.033(2) Uani 1 1 d . . . H221 H 0.2285 0.8011 0.6935 0.040 Uiso 1 1 calc R . . C222 C 0.1587(6) 0.8915(4) 0.6682(4) 0.036(2) Uani 1 1 d . . . H222 H 0.2104 0.9102 0.6728 0.044 Uiso 1 1 calc R . . C223 C 0.0707(7) 0.9298(4) 0.6478(4) 0.039(2) Uani 1 1 d . . . H223 H 0.0604 0.9752 0.6410 0.047 Uiso 1 1 calc R . . C224 C 0.0004(6) 0.9009(4) 0.6379(4) 0.034(2) Uani 1 1 d . . . H224 H -0.0569 0.9269 0.6211 0.041 Uiso 1 1 calc R . . C225 C 0.0079(6) 0.8357(4) 0.6508(4) 0.027(2) Uani 1 1 d . . . C226 C -0.0638(6) 0.8075(4) 0.6370(4) 0.034(2) Uani 1 1 d . . . H226 H -0.1218 0.8343 0.6219 0.041 Uiso 1 1 calc R . . C227 C -0.0535(6) 0.7434(4) 0.6445(4) 0.036(2) Uani 1 1 d . . . H227 H -0.1015 0.7258 0.6311 0.043 Uiso 1 1 calc R . . C228 C 0.0281(6) 0.7015(4) 0.6722(4) 0.031(2) Uani 1 1 d . . . C229 C 0.0387(6) 0.6340(4) 0.6776(4) 0.035(2) Uani 1 1 d . . . H229 H -0.0099 0.6180 0.6628 0.042 Uiso 1 1 calc R . . C230 C 0.1146(6) 0.5918(4) 0.7027(4) 0.032(2) Uani 1 1 d . . . H230 H 0.1213 0.5468 0.7038 0.038 Uiso 1 1 calc R . . C231 C 0.1840(6) 0.6160(4) 0.7275(4) 0.029(2) Uani 1 1 d . . . C232 C 0.3372(6) 0.4628(4) 0.9048(4) 0.027(2) Uani 1 1 d . . . C233 C 0.3804(6) 0.4823(4) 0.9517(4) 0.037(2) Uani 1 1 d . . . H233 H 0.4387 0.4954 0.9429 0.044 Uiso 1 1 calc R . . C234 C 0.3387(7) 0.4827(5) 1.0104(5) 0.049(3) Uani 1 1 d . . . H234 H 0.3701 0.4939 1.0422 0.059 Uiso 1 1 calc R . . C235 C 0.2526(7) 0.4670(4) 1.0230(5) 0.041(2) Uani 1 1 d . . . H235 H 0.2230 0.4692 1.0630 0.049 Uiso 1 1 calc R . . C236 C 0.2090(7) 0.4482(4) 0.9785(5) 0.043(3) Uani 1 1 d . . . H236 H 0.1499 0.4363 0.9880 0.052 Uiso 1 1 calc R . . C237 C 0.2494(6) 0.4461(4) 0.9200(4) 0.033(2) Uani 1 1 d . . . H237 H 0.2175 0.4332 0.8894 0.039 Uiso 1 1 calc R . . C301 C 0.5158(5) -0.0322(4) 0.7177(4) 0.024(2) Uani 1 1 d . . . C302 C 0.4968(5) -0.0835(4) 0.6957(4) 0.027(2) Uani 1 1 d . . . C303 C 0.4398(6) -0.1297(4) 0.7291(4) 0.038(2) Uani 1 1 d . . . H30A H 0.3707 -0.1088 0.7278 0.045 Uiso 1 1 calc R . . H30B H 0.4565 -0.1391 0.7727 0.045 Uiso 1 1 calc R . . C304 C 0.4588(7) -0.1927(4) 0.7010(5) 0.044(3) Uani 1 1 d . . . H30C H 0.4125 -0.2179 0.7191 0.053 Uiso 1 1 calc R . . H30D H 0.5241 -0.2184 0.7100 0.053 Uiso 1 1 calc R . . C305 C 0.4489(7) -0.1781(4) 0.6313(5) 0.046(3) Uani 1 1 d . . . H30E H 0.3867 -0.1478 0.6224 0.056 Uiso 1 1 calc R . . H30F H 0.4508 -0.2182 0.6137 0.056 Uiso 1 1 calc R . . C306 C 0.5315(6) -0.1483(4) 0.6017(4) 0.037(2) Uani 1 1 d . . . H30G H 0.5921 -0.1818 0.6035 0.044 Uiso 1 1 calc R . . H30H H 0.5192 -0.1331 0.5580 0.044 Uiso 1 1 calc R . . C307 C 0.5422(6) -0.0929(4) 0.6334(4) 0.032(2) Uani 1 1 d . . . C308 C 0.5937(6) -0.0500(4) 0.6104(4) 0.029(2) Uani 1 1 d . . . C309 C 0.6536(6) -0.0491(4) 0.5533(4) 0.029(2) Uani 1 1 d . . . C310 C 0.7254(6) -0.1045(4) 0.5415(4) 0.037(2) Uani 1 1 d . . . H310 H 0.7305 -0.1433 0.5683 0.044 Uiso 1 1 calc R . . C311 C 0.7876(7) -0.1018(5) 0.4910(5) 0.046(3) Uani 1 1 d . . . H311 H 0.8359 -0.1391 0.4837 0.055 Uiso 1 1 calc R . . C312 C 0.7818(8) -0.0471(5) 0.4509(5) 0.053(3) Uani 1 1 d . . . H312 H 0.8254 -0.0458 0.4163 0.063 Uiso 1 1 calc R . . C313 C 0.7107(8) 0.0064(5) 0.4624(5) 0.057(3) Uani 1 1 d . . . H313 H 0.7051 0.0447 0.4349 0.068 Uiso 1 1 calc R . . C314 C 0.6480(7) 0.0055(4) 0.5123(4) 0.042(2) Uani 1 1 d . . . H314 H 0.5999 0.0431 0.5188 0.050 Uiso 1 1 calc R . . C315 C 0.4960(6) -0.0115(4) 0.7790(4) 0.024(2) Uani 1 1 d . . . C316 C 0.4129(6) -0.0140(4) 0.8153(4) 0.031(2) Uani 1 1 d . . . H316 H 0.3665 -0.0332 0.8020 0.037 Uiso 1 1 calc R . . C317 C 0.3989(6) 0.0103(4) 0.8684(4) 0.030(2) Uani 1 1 d . . . H317 H 0.3433 0.0063 0.8931 0.036 Uiso 1 1 calc R . . C318 C 0.4622(6) 0.0419(4) 0.8901(4) 0.026(2) Uani 1 1 d . . . C319 C 0.4510(6) 0.0720(4) 0.9463(4) 0.025(2) Uani 1 1 d . . . C320 C 0.3599(6) 0.0891(4) 0.9809(4) 0.027(2) Uani 1 1 d . . . C321 C 0.2662(6) 0.0939(4) 0.9604(4) 0.036(2) Uani 1 1 d . . . H321 H 0.2616 0.0874 0.9190 0.043 Uiso 1 1 calc R . . C322 C 0.1857(7) 0.1067(5) 0.9946(5) 0.046(3) Uani 1 1 d . . . H322 H 0.1261 0.1090 0.9778 0.055 Uiso 1 1 calc R . . C323 C 0.1896(7) 0.1171(5) 1.0566(5) 0.048(3) Uani 1 1 d . . . H323 H 0.1339 0.1221 1.0832 0.057 Uiso 1 1 calc R . . C324 C 0.2761(7) 0.1198(4) 1.0771(4) 0.038(2) Uani 1 1 d . . . H324 H 0.2784 0.1302 1.1175 0.045 Uiso 1 1 calc R . . C325 C 0.3593(6) 0.1078(4) 1.0409(4) 0.031(2) Uani 1 1 d . . . C326 C 0.4470(7) 0.1165(4) 1.0623(4) 0.032(2) Uani 1 1 d . . . H326 H 0.4472 0.1281 1.1024 0.038 Uiso 1 1 calc R . . C327 C 0.5275(7) 0.1085(4) 1.0270(4) 0.030(2) Uani 1 1 d . . . H327 H 0.5825 0.1183 1.0408 0.036 Uiso 1 1 calc R . . C328 C 0.5320(6) 0.0857(4) 0.9692(4) 0.023(2) Uani 1 1 d . . . C329 C 0.6193(6) 0.0746(4) 0.9334(4) 0.024(2) Uani 1 1 d . . . H329 H 0.6738 0.0830 0.9492 0.029 Uiso 1 1 calc R . . C330 C 0.6287(6) 0.0528(4) 0.8784(4) 0.024(2) Uani 1 1 d . . . H330 H 0.6880 0.0483 0.8554 0.029 Uiso 1 1 calc R . . C331 C 0.5500(6) 0.0365(4) 0.8543(4) 0.026(2) Uani 1 1 d . . . C332 C 0.5251(6) 0.0809(4) 0.6336(4) 0.031(2) Uani 1 1 d . . . C333 C 0.4320(7) 0.0895(4) 0.6169(4) 0.042(3) Uani 1 1 d . . . H333 H 0.4015 0.0547 0.6246 0.051 Uiso 1 1 calc R . . C334 C 0.3831(7) 0.1479(5) 0.5891(5) 0.044(3) Uani 1 1 d . . . H334 H 0.3201 0.1524 0.5766 0.053 Uiso 1 1 calc R . . C335 C 0.4226(8) 0.1985(5) 0.5793(5) 0.060(3) Uani 1 1 d . . . H335 H 0.3867 0.2387 0.5614 0.072 Uiso 1 1 calc R . . C336 C 0.5164(8) 0.1922(5) 0.5953(7) 0.087(5) Uani 1 1 d . . . H336 H 0.5459 0.2275 0.5877 0.104 Uiso 1 1 calc R . . C337 C 0.5647(7) 0.1334(5) 0.6224(5) 0.056(3) Uani 1 1 d . . . H337 H 0.6282 0.1288 0.6341 0.068 Uiso 1 1 calc R . . C401 C 0.8658(5) 0.0297(4) 0.7839(4) 0.026(2) Uani 1 1 d . . . C402 C 0.8846(5) 0.0629(4) 0.8284(4) 0.025(2) Uani 1 1 d . . . C403 C 0.9296(7) 0.0334(4) 0.8889(4) 0.037(2) Uani 1 1 d . . . H40A H 0.9877 -0.0004 0.8808 0.044 Uiso 1 1 calc R . . H40B H 0.8841 0.0127 0.9151 0.044 Uiso 1 1 calc R . . C404 C 0.9569(7) 0.0824(4) 0.9237(5) 0.047(3) Uani 1 1 d . . . H40C H 0.9694 0.0631 0.9666 0.057 Uiso 1 1 calc R . . H40D H 1.0169 0.0922 0.9046 0.057 Uiso 1 1 calc R . . C405 C 0.8827(8) 0.1427(4) 0.9245(4) 0.049(3) Uani 1 1 d . . . H40E H 0.9049 0.1718 0.9481 0.058 Uiso 1 1 calc R . . H40F H 0.8239 0.1332 0.9459 0.058 Uiso 1 1 calc R . . C406 C 0.8583(6) 0.1773(4) 0.8606(4) 0.035(2) Uani 1 1 d . . . H40G H 0.9112 0.1970 0.8434 0.042 Uiso 1 1 calc R . . H40H H 0.7999 0.2122 0.8641 0.042 Uiso 1 1 calc R . . C407 C 0.8416(6) 0.1323(4) 0.8165(4) 0.029(2) Uani 1 1 d . . . C408 C 0.7876(6) 0.1496(3) 0.7679(4) 0.024(2) Uani 1 1 d . . . C409 C 0.7328(6) 0.2153(4) 0.7445(4) 0.030(2) Uani 1 1 d . . . C410 C 0.7748(7) 0.2677(4) 0.7376(4) 0.038(2) Uani 1 1 d . . . H410 H 0.8395 0.2613 0.7478 0.045 Uiso 1 1 calc R . . C411 C 0.7248(8) 0.3279(4) 0.7165(5) 0.049(3) Uani 1 1 d . . . H411 H 0.7542 0.3632 0.7127 0.059 Uiso 1 1 calc R . . C412 C 0.6320(8) 0.3372(5) 0.7007(5) 0.054(3) Uani 1 1 d . . . H412 H 0.5964 0.3789 0.6860 0.064 Uiso 1 1 calc R . . C413 C 0.5910(7) 0.2856(6) 0.7065(6) 0.065(3) Uani 1 1 d . . . H413 H 0.5271 0.2918 0.6948 0.078 Uiso 1 1 calc R . . C414 C 0.6403(7) 0.2259(5) 0.7285(5) 0.053(3) Uani 1 1 d . . . H414 H 0.6100 0.1911 0.7328 0.064 Uiso 1 1 calc R . . C415 C 0.8840(6) -0.0399(4) 0.7844(4) 0.0227(19) Uani 1 1 d . . . C416 C 0.9748(5) -0.0805(4) 0.7972(4) 0.0208(19) Uani 1 1 d . . . H416 H 1.0277 -0.0629 0.8018 0.025 Uiso 1 1 calc R . . C417 C 0.9851(6) -0.1433(4) 0.8027(3) 0.027(2) Uani 1 1 d . . . H417 H 1.0468 -0.1704 0.8096 0.033 Uiso 1 1 calc R . . C418 C 0.9072(5) -0.1721(4) 0.7987(3) 0.0197(18) Uani 1 1 d . . . C419 C 0.9098(5) -0.2390(4) 0.8107(3) 0.0222(19) Uani 1 1 d . . . C420 C 0.9839(6) -0.2855(4) 0.8448(4) 0.030(2) Uani 1 1 d . . . C421 C 1.0472(6) -0.2707(4) 0.8841(4) 0.028(2) Uani 1 1 d . . . H421 H 1.0378 -0.2273 0.8918 0.033 Uiso 1 1 calc R . . C422 C 1.1196(6) -0.3149(4) 0.9107(4) 0.033(2) Uani 1 1 d . . . H422 H 1.1627 -0.3020 0.9340 0.040 Uiso 1 1 calc R . . C423 C 1.1315(7) -0.3793(4) 0.9042(4) 0.039(2) Uani 1 1 d . . . H423 H 1.1844 -0.4103 0.9213 0.047 Uiso 1 1 calc R . . C424 C 1.0676(7) -0.3978(4) 0.8735(4) 0.039(2) Uani 1 1 d . . . H424 H 1.0740 -0.4423 0.8714 0.047 Uiso 1 1 calc R . . C425 C 0.9902(6) -0.3518(4) 0.8438(4) 0.034(2) Uani 1 1 d . . . C426 C 0.9199(7) -0.3723(4) 0.8151(5) 0.044(3) Uani 1 1 d . . . H426 H 0.9257 -0.4168 0.8134 0.053 Uiso 1 1 calc R . . C427 C 0.8446(7) -0.3286(4) 0.7901(5) 0.042(3) Uani 1 1 d . . . H427 H 0.7956 -0.3432 0.7742 0.050 Uiso 1 1 calc R . . C428 C 0.8366(6) -0.2616(4) 0.7870(4) 0.029(2) Uani 1 1 d . . . C429 C 0.7564(6) -0.2167(4) 0.7599(4) 0.030(2) Uani 1 1 d . . . H429 H 0.7082 -0.2324 0.7441 0.036 Uiso 1 1 calc R . . C430 C 0.7471(6) -0.1525(4) 0.7561(4) 0.028(2) Uani 1 1 d . . . H430 H 0.6910 -0.1235 0.7406 0.034 Uiso 1 1 calc R . . C431 C 0.8232(5) -0.1284(4) 0.7758(4) 0.0200(19) Uani 1 1 d . . . C432 C 0.8474(6) 0.0891(4) 0.6585(4) 0.030(2) Uani 1 1 d . . . C433 C 0.9180(7) 0.1232(5) 0.6496(5) 0.047(3) Uani 1 1 d . . . H433 H 0.9302 0.1445 0.6822 0.057 Uiso 1 1 calc R . . C434 C 0.9708(8) 0.1273(5) 0.5953(5) 0.056(3) Uani 1 1 d . . . H434 H 1.0195 0.1505 0.5906 0.068 Uiso 1 1 calc R . . C435 C 0.9522(8) 0.0967(5) 0.5462(5) 0.058(3) Uani 1 1 d . . . H435 H 0.9876 0.0997 0.5081 0.070 Uiso 1 1 calc R . . C436 C 0.8824(7) 0.0623(5) 0.5541(5) 0.053(3) Uani 1 1 d . . . H436 H 0.8689 0.0419 0.5213 0.064 Uiso 1 1 calc R . . C437 C 0.8320(7) 0.0578(4) 0.6101(4) 0.040(2) Uani 1 1 d . . . H437 H 0.7856 0.0327 0.6157 0.047 Uiso 1 1 calc R . . P10 P 0.72550(17) 0.66565(11) 0.59620(11) 0.0340(6) Uani 1 1 d . . . F10 F 0.6846(4) 0.6058(3) 0.6181(3) 0.0710(19) Uani 1 1 d . . . F11 F 0.6406(4) 0.6956(3) 0.5513(3) 0.0630(18) Uani 1 1 d . . . F12 F 0.6668(6) 0.7012(3) 0.6501(3) 0.104(3) Uani 1 1 d . . . F13 F 0.7850(5) 0.6291(4) 0.5440(3) 0.099(3) Uani 1 1 d . . . F14 F 0.8099(4) 0.6370(3) 0.6408(3) 0.0657(18) Uani 1 1 d . . . F15 F 0.7638(5) 0.7278(3) 0.5741(3) 0.091(3) Uani 1 1 d . . . P20 P 0.22274(16) 0.87016(11) 0.89190(11) 0.0288(6) Uani 1 1 d . . . F20 F 0.2117(4) 0.8275(4) 0.8426(3) 0.088(2) Uani 1 1 d . . . F21 F 0.2488(4) 0.8122(3) 0.9420(3) 0.093(3) Uani 1 1 d . . . F22 F 0.1119(3) 0.8785(2) 0.9127(2) 0.0412(13) Uani 1 1 d . . . F23 F 0.3335(3) 0.8629(2) 0.8706(2) 0.0413(13) Uani 1 1 d . . . F24 F 0.1958(5) 0.9317(3) 0.8432(4) 0.097(3) Uani 1 1 d . . . F25 F 0.2322(4) 0.9167(4) 0.9401(4) 0.100(3) Uani 1 1 d . . . C900 C 0.8712(9) 0.7518(7) 0.3412(7) 0.100(5) Uani 1 1 d D . . H90A H 0.8476 0.7230 0.3181 0.120 Uiso 1 1 calc R . . H90B H 0.8336 0.7962 0.3295 0.120 Uiso 1 1 calc R . . Cl1 Cl 0.9819(3) 0.7484(2) 0.3198(3) 0.1408(19) Uani 1 1 d D . . Cl2 Cl 0.8490(3) 0.73152(18) 0.41770(18) 0.0993(12) Uani 1 1 d D . . C910 C 0.4749(8) 0.7240(5) 0.9129(6) 0.073(4) Uani 1 1 d . . . H91A H 0.4121 0.7525 0.9018 0.087 Uiso 1 1 calc R . . H91B H 0.4917 0.7352 0.9521 0.087 Uiso 1 1 calc R . . Cl11 Cl 0.4653(2) 0.64349(13) 0.92297(12) 0.0648(8) Uani 1 1 d . . . Cl12 Cl 0.5613(2) 0.73751(15) 0.85565(15) 0.0743(9) Uani 1 1 d . . . C920 C 0.7603(8) 0.7119(6) 0.9593(5) 0.070(3) Uani 1 1 d . . . H92A H 0.7675 0.6754 0.9351 0.084 Uiso 1 1 calc R . . H92B H 0.7517 0.7519 0.9304 0.084 Uiso 1 1 calc R . . Cl21 Cl 0.8637(2) 0.70205(15) 0.99945(16) 0.0778(9) Uani 1 1 d . . . Cl22 Cl 0.6578(2) 0.71591(15) 1.01003(15) 0.0773(9) Uani 1 1 d . . . C930 C 0.8669(9) 0.9264(7) 0.2261(6) 0.081(4) Uani 1 1 d . . . H93A H 0.8527 0.9640 0.1944 0.097 Uiso 1 1 calc R . . H93B H 0.9349 0.9189 0.2357 0.097 Uiso 1 1 calc R . . Cl31 Cl 0.7951(3) 0.9451(2) 0.29307(18) 0.1104(13) Uani 1 1 d . . . Cl32 Cl 0.8521(4) 0.8628(3) 0.1971(2) 0.1464(19) Uani 1 1 d . . . C94A C 0.941(3) 0.299(4) 0.547(3) 0.160(9) Uani 0.249(4) 1 d PDU B 3 H94A H 0.9651 0.3120 0.5831 0.192 Uiso 0.249(4) 1 calc PR B 3 H94B H 0.9820 0.2568 0.5395 0.192 Uiso 0.249(4) 1 calc PR B 3 Cl4A Cl 0.9591(13) 0.3496(10) 0.4888(7) 0.123(6) Uani 0.249(4) 1 d PDU B 3 Cl5A Cl 0.8269(16) 0.2900(9) 0.5659(9) 0.142(7) Uani 0.249(4) 1 d PDU B 3 C94B C 0.831(2) 0.2449(18) 0.4910(14) 0.189(8) Uani 0.548(10) 1 d PDU C 4 H94C H 0.8640 0.2014 0.4812 0.227 Uiso 0.548(10) 1 calc PR C 4 H94D H 0.7985 0.2681 0.4536 0.227 Uiso 0.548(10) 1 calc PR C 4 Cl4B Cl 0.9113(9) 0.2809(6) 0.5034(6) 0.181(5) Uani 0.548(10) 1 d PDU C 4 Cl5B Cl 0.7435(9) 0.2365(8) 0.5471(12) 0.353(17) Uani 0.548(10) 1 d PDU C 4 C94C C 0.820(2) 0.2210(16) 0.4640(10) 0.192(9) Uani 0.203(10) 1 d PDU D 5 H94E H 0.8365 0.2264 0.5054 0.231 Uiso 0.203(10) 1 calc PR D 5 H94F H 0.7917 0.2645 0.4435 0.231 Uiso 0.203(10) 1 calc PR D 5 Cl4C Cl 0.737(3) 0.1821(13) 0.4727(12) 0.186(9) Uani 0.203(10) 1 d PDU D 5 Cl5C Cl 0.925(5) 0.191(4) 0.424(7) 1.1(3) Uani 0.203(10) 1 d PDU . 5 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 0.0241(6) 0.0205(5) 0.0318(6) -0.0093(5) -0.0075(5) -0.0034(4) Cu2 0.0203(6) 0.0231(6) 0.0299(6) -0.0062(5) -0.0079(5) -0.0040(4) P1 0.0259(13) 0.0249(12) 0.0300(14) -0.0049(10) -0.0080(11) -0.0056(10) P2 0.0242(12) 0.0211(12) 0.0299(13) -0.0055(10) -0.0089(10) -0.0017(10) P3 0.0277(13) 0.0261(12) 0.0268(13) -0.0067(10) -0.0077(11) -0.0051(10) P4 0.0227(12) 0.0227(12) 0.0332(14) -0.0063(10) -0.0037(11) -0.0050(10) N1 0.024(4) 0.024(4) 0.029(4) -0.010(3) -0.007(3) -0.005(3) N2 0.019(4) 0.022(4) 0.032(4) -0.007(3) -0.009(3) 0.000(3) N3 0.022(4) 0.023(4) 0.029(4) -0.010(3) -0.008(3) -0.003(3) N4 0.020(4) 0.024(4) 0.025(4) -0.008(3) -0.003(3) -0.010(3) C1 0.024(5) 0.023(5) 0.046(6) -0.010(4) -0.005(4) -0.008(4) C2 0.034(5) 0.033(5) 0.035(5) -0.004(4) -0.010(4) -0.008(4) C3 0.045(8) 0.043(14) 0.041(7) -0.002(11) -0.016(8) -0.006(10) C4 0.055(9) 0.100(16) 0.054(9) 0.000(10) -0.027(7) -0.027(11) C5 0.040(8) 0.080(15) 0.073(11) 0.017(10) -0.017(7) -0.005(10) C6 0.029(7) 0.079(15) 0.056(10) -0.001(10) -0.012(8) -0.010(9) C7 0.026(4) 0.041(5) 0.044(5) -0.003(5) -0.001(4) -0.005(4) C3' 0.049(10) 0.05(2) 0.043(10) 0.012(16) -0.013(11) -0.010(14) C4' 0.052(10) 0.056(15) 0.042(12) -0.001(11) -0.030(10) -0.008(10) C5' 0.040(11) 0.093(18) 0.050(12) -0.001(12) -0.015(9) -0.012(12) C6' 0.029(7) 0.09(2) 0.048(10) -0.009(13) -0.011(10) -0.020(12) C8 0.027(5) 0.024(5) 0.031(5) -0.008(4) -0.006(4) -0.006(4) C9 0.022(5) 0.038(5) 0.035(6) 0.000(4) -0.007(4) -0.006(4) C10 0.061(7) 0.072(7) 0.041(7) -0.022(6) 0.015(6) -0.047(6) C11 0.075(8) 0.066(8) 0.059(8) -0.017(6) 0.005(7) -0.048(7) C12 0.041(6) 0.058(7) 0.038(6) 0.000(5) 0.010(5) -0.011(5) C13 0.048(6) 0.060(7) 0.034(6) -0.022(5) 0.004(5) -0.009(6) C14 0.035(6) 0.037(5) 0.051(7) -0.018(5) -0.010(5) -0.015(4) C15 0.041(6) 0.047(6) 0.025(5) -0.017(4) -0.009(4) -0.017(5) C16 0.038(5) 0.051(7) 0.049(6) -0.021(6) -0.001(5) -0.029(6) C17 0.044(5) 0.049(6) 0.048(5) -0.019(5) -0.003(5) -0.018(5) C18 0.032(4) 0.044(5) 0.033(4) -0.013(4) 0.000(4) -0.016(4) C19 0.030(4) 0.045(4) 0.033(4) -0.014(3) 0.002(4) -0.013(4) C20 0.025(5) 0.048(5) 0.033(5) -0.014(4) -0.001(4) -0.014(4) C21 0.040(6) 0.059(6) 0.059(6) -0.036(5) 0.019(5) -0.027(5) C22 0.046(6) 0.060(7) 0.052(7) -0.036(6) 0.022(6) -0.024(6) C23 0.037(6) 0.068(7) 0.044(7) -0.027(6) 0.015(5) -0.016(6) C24 0.031(5) 0.079(6) 0.048(6) -0.023(5) 0.016(5) -0.018(5) C25 0.026(5) 0.067(5) 0.037(5) -0.014(4) 0.003(4) -0.015(4) C26 0.022(5) 0.068(6) 0.037(5) -0.006(5) 0.003(4) -0.019(4) C27 0.024(5) 0.057(5) 0.038(5) -0.008(4) -0.006(4) -0.014(4) C28 0.026(4) 0.046(4) 0.033(4) -0.010(4) -0.001(3) -0.011(4) C29 0.026(4) 0.034(5) 0.031(5) -0.008(4) -0.002(4) -0.011(4) C30 0.030(5) 0.028(6) 0.026(6) -0.009(5) 0.000(5) -0.008(4) C16' 0.039(6) 0.043(8) 0.037(6) -0.012(6) -0.005(6) -0.028(7) C17' 0.038(5) 0.043(6) 0.031(5) -0.012(5) -0.003(5) -0.027(5) C18' 0.033(4) 0.041(5) 0.032(4) -0.015(4) -0.002(4) -0.017(4) C19' 0.029(4) 0.046(4) 0.034(4) -0.013(4) 0.002(4) -0.015(4) C20' 0.036(5) 0.059(5) 0.043(5) -0.021(4) 0.005(4) -0.020(4) C21' 0.051(7) 0.067(6) 0.058(7) -0.037(6) 0.015(6) -0.027(5) C22' 0.066(8) 0.078(8) 0.072(9) -0.045(7) 0.022(8) -0.024(7) C23' 0.066(8) 0.083(8) 0.077(9) -0.037(8) 0.023(8) -0.017(7) C24' 0.050(7) 0.082(7) 0.065(7) -0.025(6) 0.017(6) -0.015(6) C25' 0.035(5) 0.071(5) 0.047(5) -0.018(5) 0.010(5) -0.017(4) C26' 0.023(5) 0.066(6) 0.038(5) -0.009(5) 0.000(5) -0.014(5) C27' 0.024(5) 0.059(6) 0.038(5) -0.010(5) -0.003(5) -0.015(5) C28' 0.026(4) 0.046(4) 0.033(5) -0.010(4) -0.001(4) -0.011(4) C29' 0.026(5) 0.038(5) 0.033(6) -0.010(5) -0.002(5) -0.012(4) C30' 0.028(5) 0.031(6) 0.030(6) -0.014(5) -0.003(5) -0.010(5) C31 0.028(4) 0.026(4) 0.027(4) -0.006(3) -0.002(3) -0.011(3) C32 0.035(6) 0.026(5) 0.046(6) -0.009(5) -0.018(5) -0.008(4) C33 0.090(9) 0.032(6) 0.054(8) 0.005(5) -0.016(7) -0.001(6) C34 0.134(13) 0.047(8) 0.074(10) 0.015(7) -0.039(10) -0.035(8) C35 0.082(10) 0.032(7) 0.117(13) -0.004(8) -0.052(9) 0.006(7) C36 0.074(9) 0.040(7) 0.106(12) -0.006(7) -0.012(8) 0.003(6) C37 0.058(7) 0.034(6) 0.095(10) 0.002(6) 0.004(7) 0.002(6) C201 0.030(5) 0.017(4) 0.035(5) -0.013(4) -0.014(4) -0.006(4) C202 0.034(5) 0.022(5) 0.020(5) -0.003(4) -0.009(4) -0.007(4) C203 0.027(5) 0.033(5) 0.031(5) -0.009(4) -0.003(4) -0.004(4) C204 0.045(6) 0.030(5) 0.039(6) -0.006(4) -0.007(5) -0.014(4) C205 0.029(5) 0.044(6) 0.035(6) -0.014(5) -0.009(4) -0.008(4) C206 0.028(5) 0.029(5) 0.030(5) -0.009(4) -0.003(4) 0.003(4) C207 0.017(4) 0.026(5) 0.021(5) -0.006(4) -0.006(4) -0.003(4) C208 0.026(5) 0.034(5) 0.017(5) -0.011(4) -0.010(4) -0.006(4) C209 0.038(5) 0.019(4) 0.020(5) -0.003(4) -0.002(4) 0.003(4) C210 0.037(5) 0.029(5) 0.033(5) -0.011(4) -0.004(5) -0.005(4) C211 0.033(5) 0.038(6) 0.026(5) 0.000(4) -0.008(4) -0.002(4) C212 0.041(6) 0.024(5) 0.045(6) 0.001(4) -0.011(5) -0.004(4) C213 0.049(6) 0.026(5) 0.071(8) 0.003(5) -0.025(6) -0.009(5) C214 0.030(5) 0.035(5) 0.046(6) -0.005(5) -0.012(5) -0.008(4) C215 0.024(5) 0.018(4) 0.032(5) -0.010(4) -0.012(4) -0.005(4) C216 0.020(5) 0.037(5) 0.036(6) -0.011(4) -0.011(4) 0.000(4) C217 0.024(5) 0.021(5) 0.037(5) -0.012(4) -0.005(4) -0.002(4) C218 0.021(5) 0.022(5) 0.029(5) -0.012(4) -0.007(4) 0.001(4) C219 0.022(5) 0.027(5) 0.034(5) -0.015(4) -0.008(4) -0.002(4) C220 0.025(5) 0.022(5) 0.034(5) -0.005(4) -0.004(4) -0.001(4) C221 0.032(5) 0.033(5) 0.031(5) -0.007(4) -0.012(4) 0.005(4) C222 0.030(5) 0.037(6) 0.042(6) 0.001(4) -0.008(5) -0.007(4) C223 0.047(6) 0.033(5) 0.033(6) 0.004(4) -0.003(5) -0.004(5) C224 0.030(5) 0.039(6) 0.030(5) 0.001(4) -0.001(4) -0.002(4) C225 0.036(5) 0.023(5) 0.016(5) -0.005(4) 0.000(4) 0.004(4) C226 0.023(5) 0.041(6) 0.037(6) -0.006(4) -0.016(4) -0.001(4) C227 0.024(5) 0.035(6) 0.053(6) -0.011(5) -0.016(5) -0.006(4) C228 0.030(5) 0.032(5) 0.030(5) -0.009(4) -0.008(4) -0.001(4) C229 0.034(5) 0.019(5) 0.056(6) -0.018(4) -0.017(5) -0.002(4) C230 0.030(5) 0.020(5) 0.048(6) -0.015(4) -0.020(5) -0.001(4) C231 0.033(5) 0.026(5) 0.030(5) -0.014(4) -0.001(4) -0.005(4) C232 0.028(5) 0.014(4) 0.032(5) -0.002(4) -0.006(4) 0.006(4) C233 0.027(5) 0.049(6) 0.038(6) -0.010(5) 0.000(5) -0.014(4) C234 0.050(7) 0.063(7) 0.034(6) -0.014(5) -0.014(6) -0.004(6) C235 0.036(6) 0.050(6) 0.036(6) -0.016(5) 0.002(5) -0.004(5) C236 0.046(6) 0.042(6) 0.043(7) -0.011(5) 0.015(5) -0.015(5) C237 0.037(6) 0.028(5) 0.040(6) -0.017(4) -0.002(5) -0.014(4) C301 0.020(5) 0.024(5) 0.029(5) -0.008(4) -0.008(4) -0.003(4) C302 0.014(4) 0.036(5) 0.035(6) -0.017(4) -0.004(4) -0.004(4) C303 0.030(5) 0.039(5) 0.049(6) -0.015(5) -0.002(5) -0.013(4) C304 0.046(6) 0.032(5) 0.066(8) -0.019(5) 0.003(5) -0.025(5) C305 0.041(6) 0.047(6) 0.060(7) -0.035(5) 0.008(5) -0.016(5) C306 0.039(6) 0.025(5) 0.048(6) -0.016(4) -0.001(5) -0.006(4) C307 0.024(5) 0.027(5) 0.044(6) -0.012(4) -0.010(5) 0.003(4) C308 0.024(5) 0.030(5) 0.032(6) -0.004(4) -0.019(4) 0.003(4) C309 0.035(5) 0.035(5) 0.025(5) -0.011(4) -0.012(4) -0.014(4) C310 0.039(6) 0.041(6) 0.038(6) -0.011(5) -0.013(5) -0.018(5) C311 0.040(6) 0.054(7) 0.050(7) -0.031(6) 0.003(5) -0.012(5) C312 0.066(8) 0.059(7) 0.039(7) -0.012(6) 0.015(6) -0.030(6) C313 0.078(8) 0.056(7) 0.043(7) 0.000(6) -0.012(7) -0.028(7) C314 0.054(7) 0.034(6) 0.035(6) -0.003(5) 0.002(5) -0.008(5) C315 0.024(5) 0.022(4) 0.031(5) -0.012(4) -0.003(4) -0.009(4) C316 0.033(5) 0.025(5) 0.040(6) -0.011(4) -0.012(5) -0.010(4) C317 0.021(5) 0.033(5) 0.036(6) -0.003(4) -0.004(4) -0.007(4) C318 0.024(5) 0.021(4) 0.032(5) -0.007(4) -0.007(4) -0.002(4) C319 0.032(5) 0.025(5) 0.022(5) -0.004(4) -0.005(4) -0.010(4) C320 0.030(5) 0.026(5) 0.025(5) 0.001(4) -0.007(4) -0.007(4) C321 0.034(6) 0.042(6) 0.035(6) -0.010(4) -0.009(5) -0.011(4) C322 0.031(6) 0.064(7) 0.053(7) -0.023(6) -0.005(5) -0.020(5) C323 0.046(7) 0.055(7) 0.048(7) -0.014(5) 0.004(5) -0.021(5) C324 0.047(6) 0.042(6) 0.030(6) -0.011(4) -0.008(5) -0.017(5) C325 0.026(5) 0.041(5) 0.023(5) -0.005(4) 0.000(4) -0.004(4) C326 0.047(6) 0.032(5) 0.023(5) -0.007(4) -0.011(5) -0.016(4) C327 0.041(6) 0.023(5) 0.029(5) -0.002(4) -0.015(5) -0.008(4) C328 0.025(5) 0.019(4) 0.030(5) -0.005(4) -0.009(4) -0.010(4) C329 0.020(5) 0.026(5) 0.031(5) -0.005(4) -0.012(4) -0.009(4) C330 0.017(5) 0.026(5) 0.031(5) -0.007(4) -0.004(4) -0.005(4) C331 0.029(5) 0.015(4) 0.034(6) -0.002(4) -0.009(4) -0.005(4) C332 0.036(5) 0.025(5) 0.033(5) -0.003(4) -0.024(5) -0.001(4) C333 0.048(6) 0.034(6) 0.052(7) -0.013(5) -0.018(5) -0.013(5) C334 0.036(6) 0.039(6) 0.055(7) -0.012(5) -0.028(5) 0.006(5) C335 0.060(8) 0.041(7) 0.073(8) 0.000(6) -0.036(7) 0.007(6) C336 0.056(8) 0.037(7) 0.160(14) 0.029(8) -0.028(9) -0.011(6) C337 0.041(6) 0.038(6) 0.086(9) 0.015(6) -0.027(6) -0.005(5) C401 0.014(4) 0.029(5) 0.037(5) -0.006(4) -0.012(4) -0.005(4) C402 0.017(4) 0.027(5) 0.035(5) -0.015(4) 0.004(4) -0.008(4) C403 0.045(6) 0.033(5) 0.036(6) -0.010(4) -0.015(5) -0.010(4) C404 0.051(6) 0.043(6) 0.047(7) -0.007(5) -0.026(5) -0.001(5) C405 0.073(8) 0.038(6) 0.043(6) -0.018(5) -0.019(6) -0.016(5) C406 0.023(5) 0.032(5) 0.052(6) -0.019(5) -0.008(5) -0.001(4) C407 0.020(5) 0.032(5) 0.039(6) -0.013(4) 0.000(4) -0.011(4) C408 0.022(5) 0.013(4) 0.037(5) -0.011(4) 0.003(4) -0.002(4) C409 0.028(5) 0.030(5) 0.034(5) -0.011(4) 0.006(4) -0.012(4) C410 0.037(6) 0.035(6) 0.046(6) -0.016(5) 0.000(5) -0.012(5) C411 0.059(7) 0.020(5) 0.074(8) -0.012(5) -0.005(6) -0.014(5) C412 0.051(7) 0.041(6) 0.063(8) -0.002(5) -0.010(6) 0.000(5) C413 0.030(6) 0.077(9) 0.088(9) 0.005(7) -0.022(6) -0.015(6) C414 0.036(6) 0.035(6) 0.082(8) 0.010(5) -0.016(6) -0.003(5) C415 0.025(5) 0.021(4) 0.026(5) -0.008(4) -0.005(4) -0.009(4) C416 0.020(5) 0.021(5) 0.026(5) -0.005(4) -0.008(4) -0.011(4) C417 0.030(5) 0.024(5) 0.023(5) -0.008(4) -0.012(4) 0.009(4) C418 0.023(5) 0.021(4) 0.018(5) -0.015(4) -0.003(4) -0.003(4) C419 0.025(5) 0.022(4) 0.019(5) -0.008(4) -0.006(4) 0.001(4) C420 0.032(5) 0.026(5) 0.031(5) -0.005(4) -0.008(4) -0.001(4) C421 0.032(5) 0.022(5) 0.029(5) -0.008(4) -0.008(4) -0.004(4) C422 0.035(5) 0.033(5) 0.029(5) 0.000(4) -0.012(4) 0.000(4) C423 0.045(6) 0.027(5) 0.040(6) -0.002(4) -0.016(5) 0.006(4) C424 0.051(6) 0.010(4) 0.053(6) -0.002(4) -0.017(5) 0.005(4) C425 0.045(6) 0.026(5) 0.034(6) -0.002(4) -0.008(5) -0.013(4) C426 0.053(7) 0.027(5) 0.056(7) -0.008(5) -0.011(6) -0.011(5) C427 0.039(6) 0.033(6) 0.062(7) -0.020(5) -0.002(5) -0.019(5) C428 0.027(5) 0.021(5) 0.037(6) -0.007(4) -0.004(4) -0.002(4) C429 0.022(5) 0.040(6) 0.035(6) -0.014(4) 0.001(4) -0.015(4) C430 0.023(5) 0.032(5) 0.033(5) -0.010(4) -0.007(4) -0.006(4) C431 0.022(5) 0.021(4) 0.022(5) -0.012(4) -0.004(4) -0.007(4) C432 0.028(5) 0.032(5) 0.034(6) -0.005(4) -0.007(4) -0.011(4) C433 0.050(6) 0.052(6) 0.043(7) -0.020(5) 0.016(5) -0.018(5) C434 0.059(7) 0.055(7) 0.059(8) -0.014(6) 0.020(6) -0.023(6) C435 0.061(8) 0.057(7) 0.056(8) -0.019(6) 0.010(6) -0.010(6) C436 0.052(7) 0.077(8) 0.038(7) -0.025(6) 0.003(6) -0.022(6) C437 0.037(6) 0.043(6) 0.039(6) -0.008(5) -0.002(5) -0.008(5) P10 0.0399(15) 0.0329(13) 0.0352(15) -0.0090(11) -0.0143(12) -0.0133(11) F10 0.061(4) 0.058(4) 0.101(5) 0.014(4) -0.026(4) -0.033(3) F11 0.061(4) 0.055(4) 0.076(4) -0.004(3) -0.044(4) -0.009(3) F12 0.167(7) 0.062(4) 0.047(4) -0.017(3) 0.002(5) 0.044(5) F13 0.104(6) 0.115(6) 0.051(4) -0.015(4) 0.016(4) 0.023(5) F14 0.075(4) 0.056(4) 0.071(4) 0.011(3) -0.052(4) -0.020(3) F15 0.097(5) 0.069(4) 0.123(6) 0.043(4) -0.068(5) -0.058(4) P20 0.0265(13) 0.0330(13) 0.0313(14) -0.0062(11) -0.0109(11) -0.0110(10) F20 0.051(4) 0.139(6) 0.110(6) -0.095(5) 0.027(4) -0.057(4) F21 0.046(4) 0.111(6) 0.088(5) 0.051(4) 0.002(4) 0.010(4) F22 0.027(3) 0.055(3) 0.045(3) -0.007(3) -0.009(2) -0.011(2) F23 0.031(3) 0.059(3) 0.041(3) -0.017(3) -0.008(2) -0.018(3) F24 0.063(4) 0.079(5) 0.129(7) 0.054(5) -0.005(4) -0.011(4) F25 0.055(4) 0.128(6) 0.145(7) -0.101(6) 0.011(4) -0.037(4) C900 0.085(10) 0.096(11) 0.111(13) -0.020(9) 0.013(9) -0.007(8) Cl1 0.124(4) 0.141(4) 0.179(5) -0.075(4) 0.051(3) -0.062(3) Cl2 0.113(3) 0.084(3) 0.094(3) -0.018(2) -0.011(2) -0.005(2) C910 0.066(8) 0.062(8) 0.101(10) -0.042(7) 0.004(8) -0.022(6) Cl11 0.097(2) 0.0470(16) 0.0432(17) -0.0093(13) -0.0136(16) 0.0018(15) Cl12 0.086(2) 0.0649(19) 0.076(2) -0.0349(17) 0.0057(18) -0.0135(17) C920 0.080(9) 0.056(7) 0.066(8) -0.003(6) 0.003(7) -0.006(6) Cl21 0.077(2) 0.075(2) 0.080(2) 0.0002(17) 0.0060(18) -0.0243(17) Cl22 0.073(2) 0.077(2) 0.073(2) 0.0060(17) -0.0123(18) -0.0050(17) C930 0.066(8) 0.105(11) 0.067(9) 0.021(8) -0.010(7) -0.027(8) Cl31 0.144(4) 0.119(3) 0.071(3) -0.007(2) -0.017(3) -0.035(3) Cl32 0.167(5) 0.173(5) 0.107(4) -0.023(3) 0.026(3) -0.062(4) C94A 0.172(14) 0.160(17) 0.124(16) 0.005(14) -0.034(16) 0.002(15) Cl4A 0.134(13) 0.153(15) 0.079(10) -0.041(9) -0.020(9) -0.012(11) Cl5A 0.190(16) 0.115(15) 0.095(13) 0.001(10) -0.010(13) 0.006(13) C94B 0.255(17) 0.149(17) 0.141(16) -0.015(14) -0.091(13) 0.020(12) Cl4B 0.177(9) 0.160(10) 0.160(9) 0.063(8) -0.007(8) 0.005(7) Cl5B 0.145(9) 0.214(16) 0.59(4) 0.26(2) -0.028(13) 0.012(9) C94C 0.264(19) 0.148(18) 0.144(17) -0.020(16) -0.099(15) 0.020(14) Cl4C 0.29(2) 0.126(17) 0.140(16) -0.047(13) -0.138(16) 0.015(15) Cl5C 0.41(11) 0.61(18) 1.8(5) 0.3(3) 0.6(3) 0.31(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.071(6) . ? Cu1 N1 2.085(7) . ? Cu1 P2 2.306(2) . ? Cu1 P1 2.323(2) . ? Cu2 N4 2.082(6) . ? Cu2 N3 2.084(7) . ? Cu2 P3 2.280(2) . ? Cu2 P4 2.295(2) . ? P1 C1 1.771(9) . ? P1 C8 1.800(8) . ? P1 C32 1.828(9) . ? P2 C208 1.796(8) . ? P2 C201 1.803(8) . ? P2 C232 1.807(9) . ? P3 C301 1.788(8) . ? P3 C308 1.804(9) . ? P3 C332 1.812(8) . ? P4 C401 1.789(8) . ? P4 C408 1.800(8) . ? P4 C432 1.811(9) . ? N1 C15 1.356(10) . ? N1 C31 1.365(10) . ? N2 C215 1.325(9) . ? N2 C231 1.389(10) . ? N3 C315 1.360(10) . ? N3 C331 1.366(10) . ? N4 C415 1.328(9) . ? N4 C431 1.379(9) . ? C1 C2 1.351(11) . ? C1 C15 1.461(12) . ? C2 C7 1.462(11) . ? C2 C3 1.508(13) . ? C2 C3' 1.519(15) . ? C3 C4 1.515(18) . ? C4 C5 1.530(17) . ? C5 C6 1.506(17) . ? C6 C7 1.519(14) . ? C7 C8 1.351(11) . ? C7 C6' 1.509(16) . ? C3' C4' 1.523(19) . ? C4' C5' 1.533(18) . ? C5' C6' 1.496(19) . ? C8 C9 1.482(12) . ? C9 C10 1.386(12) . ? C9 C14 1.389(12) . ? C10 C11 1.366(13) . ? C11 C12 1.376(14) . ? C12 C13 1.353(13) . ? C13 C14 1.386(13) . ? C15 C16 1.428(15) . ? C15 C16' 1.440(18) . ? C16 C17 1.274(15) . ? C17 C18 1.47(2) . ? C18 C31 1.385(19) . ? C18 C19 1.452(14) . ? C19 C28 1.402(14) . ? C19 C20 1.45(2) . ? C20 C21 1.407(17) . ? C20 C25 1.445(16) . ? C21 C22 1.320(17) . ? C22 C23 1.341(19) . ? C23 C24 1.376(19) . ? C24 C25 1.414(18) . ? C25 C26 1.410(16) . ? C26 C27 1.361(16) . ? C27 C28 1.442(17) . ? C28 C29 1.439(17) . ? C29 C30 1.361(15) . ? C30 C31 1.39(2) . ? C16' C17' 1.299(17) . ? C17' C18' 1.47(2) . ? C18' C19' 1.449(17) . ? C18' C31 1.49(2) . ? C19' C28' 1.402(16) . ? C19' C20' 1.45(2) . ? C20' C21' 1.40(2) . ? C20' C25' 1.439(19) . ? C21' C22' 1.34(2) . ? C22' C23' 1.34(2) . ? C23' C24' 1.39(2) . ? C24' C25' 1.41(2) . ? C25' C26' 1.395(19) . ? C26' C27' 1.348(18) . ? C27' C28' 1.425(19) . ? C28' C29' 1.430(19) . ? C29' C30' 1.359(17) . ? C30' C31 1.45(3) . ? C32 C33 1.330(13) . ? C32 C37 1.392(14) . ? C33 C34 1.403(15) . ? C34 C35 1.318(17) . ? C35 C36 1.362(18) . ? C36 C37 1.383(14) . ? C201 C202 1.370(11) . ? C201 C215 1.456(10) . ? C202 C207 1.482(9) . ? C202 C203 1.514(10) . ? C203 C204 1.511(10) . ? C204 C205 1.521(10) . ? C205 C206 1.495(10) . ? C206 C207 1.517(10) . ? C207 C208 1.347(10) . ? C208 C209 1.477(11) . ? C209 C214 1.383(11) . ? C209 C210 1.391(11) . ? C210 C211 1.387(11) . ? C211 C212 1.382(12) . ? C212 C213 1.351(12) . ? C213 C214 1.400(12) . ? C215 C216 1.417(11) . ? C216 C217 1.338(10) . ? C217 C218 1.432(11) . ? C218 C231 1.426(11) . ? C218 C219 1.436(10) . ? C219 C228 1.414(11) . ? C219 C220 1.458(11) . ? C220 C221 1.427(12) . ? C220 C225 1.427(11) . ? C220 Cl5C 2.23(15) 2_666 ? C221 C222 1.360(11) . ? C222 C223 1.407(12) . ? C223 C224 1.359(12) . ? C224 C225 1.377(11) . ? C225 C226 1.394(12) . ? C225 Cl5C 1.93(10) 2_666 ? C226 C227 1.345(11) . ? C227 C228 1.422(11) . ? C228 C229 1.420(11) . ? C229 C230 1.347(11) . ? C230 C231 1.412(11) . ? C232 C237 1.405(11) . ? C232 C233 1.406(12) . ? C233 C234 1.382(13) . ? C234 C235 1.365(13) . ? C235 C236 1.360(13) . ? C236 C237 1.372(12) . ? C301 C302 1.361(11) . ? C301 C315 1.463(11) . ? C302 C307 1.490(12) . ? C302 C303 1.524(11) . ? C303 C304 1.524(11) . ? C304 C305 1.535(13) . ? C305 C306 1.548(12) . ? C306 C307 1.507(11) . ? C307 C308 1.350(11) . ? C308 C309 1.469(12) . ? C309 C314 1.376(12) . ? C309 C310 1.416(12) . ? C310 C311 1.376(12) . ? C311 C312 1.367(14) . ? C312 C313 1.381(14) . ? C313 C314 1.367(14) . ? C315 C316 1.397(11) . ? C316 C317 1.326(11) . ? C317 C318 1.410(11) . ? C318 C331 1.426(11) . ? C318 C319 1.453(11) . ? C319 C328 1.419(11) . ? C319 C320 1.457(11) . ? C320 C325 1.430(11) . ? C320 C321 1.436(11) . ? C321 C322 1.323(12) . ? C322 C323 1.420(13) . ? C323 C324 1.378(12) . ? C324 C325 1.376(12) . ? C325 C326 1.446(12) . ? C326 C327 1.334(12) . ? C327 C328 1.415(11) . ? C328 C329 1.418(11) . ? C329 C330 1.342(11) . ? C330 C331 1.427(11) . ? C332 C337 1.377(12) . ? C332 C333 1.384(12) . ? C333 C334 1.375(12) . ? C334 C335 1.337(13) . ? C335 C336 1.396(14) . ? C336 C337 1.374(13) . ? C401 C402 1.368(11) . ? C401 C415 1.460(11) . ? C402 C407 1.473(11) . ? C402 C403 1.521(11) . ? C403 C404 1.526(12) . ? C404 C405 1.472(13) . ? C405 C406 1.524(12) . ? C406 C407 1.533(11) . ? C407 C408 1.332(11) . ? C408 C409 1.493(11) . ? C409 C414 1.365(12) . ? C409 C410 1.394(11) . ? C410 C411 1.366(12) . ? C411 C412 1.371(13) . ? C412 C413 1.371(14) . ? C413 C414 1.359(13) . ? C415 C416 1.415(10) . ? C416 C417 1.319(10) . ? C417 C418 1.425(11) . ? C418 C431 1.423(10) . ? C418 C419 1.427(10) . ? C419 C428 1.426(11) . ? C419 C420 1.455(10) . ? C420 C425 1.416(11) . ? C420 C421 1.424(11) . ? C421 C422 1.345(10) . ? C422 C423 1.387(12) . ? C423 C424 1.348(12) . ? C424 C425 1.436(11) . ? C425 C426 1.422(12) . ? C426 C427 1.352(12) . ? C427 C428 1.416(11) . ? C428 C429 1.429(11) . ? C429 C430 1.354(11) . ? C430 C431 1.441(11) . ? C432 C433 1.384(12) . ? C432 C437 1.395(12) . ? C433 C434 1.370(13) . ? C434 C435 1.415(14) . ? C435 C436 1.378(14) . ? C436 C437 1.386(13) . ? P10 F10 1.555(6) . ? P10 F13 1.560(7) . ? P10 F12 1.575(7) . ? P10 F14 1.578(5) . ? P10 F15 1.579(6) . ? P10 F11 1.591(5) . ? P20 F21 1.547(6) . ? P20 F20 1.555(6) . ? P20 F24 1.582(6) . ? P20 F25 1.591(6) . ? P20 F22 1.601(5) . ? P20 F23 1.606(5) . ? C900 Cl1 1.616(13) . ? C900 Cl2 1.708(14) . ? C910 Cl12 1.748(12) . ? C910 Cl11 1.763(11) . ? C920 Cl21 1.748(12) . ? C920 Cl22 1.773(12) . ? C930 Cl32 1.656(14) . ? C930 Cl31 1.766(13) . ? C94A Cl4A 1.61(2) . ? C94A Cl5A 1.72(2) . ? C94B Cl4B 1.61(2) . ? C94B Cl5B 1.72(2) . ? C94C Cl4C 1.60(2) . ? C94C Cl5C 1.72(2) . ? Cl5C C225 1.93(10) 2_666 ? Cl5C C220 2.23(15) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 114.4(3) . . ? N2 Cu1 P2 86.80(18) . . ? N1 Cu1 P2 125.61(19) . . ? N2 Cu1 P1 130.60(19) . . ? N1 Cu1 P1 86.31(19) . . ? P2 Cu1 P1 118.03(9) . . ? N4 Cu2 N3 118.0(2) . . ? N4 Cu2 P3 126.27(18) . . ? N3 Cu2 P3 85.02(19) . . ? N4 Cu2 P4 87.52(18) . . ? N3 Cu2 P4 125.27(19) . . ? P3 Cu2 P4 119.42(9) . . ? C1 P1 C8 90.6(4) . . ? C1 P1 C32 107.8(4) . . ? C8 P1 C32 106.0(4) . . ? C1 P1 Cu1 90.4(3) . . ? C8 P1 Cu1 140.2(3) . . ? C32 P1 Cu1 111.5(3) . . ? C208 P2 C201 91.1(4) . . ? C208 P2 C232 104.1(4) . . ? C201 P2 C232 105.7(4) . . ? C208 P2 Cu1 136.4(3) . . ? C201 P2 Cu1 89.5(3) . . ? C232 P2 Cu1 117.6(3) . . ? C301 P3 C308 91.3(4) . . ? C301 P3 C332 106.6(4) . . ? C308 P3 C332 104.6(4) . . ? C301 P3 Cu2 92.4(3) . . ? C308 P3 Cu2 136.5(3) . . ? C332 P3 Cu2 115.7(3) . . ? C401 P4 C408 90.6(4) . . ? C401 P4 C432 106.6(4) . . ? C408 P4 C432 105.0(4) . . ? C401 P4 Cu2 90.7(3) . . ? C408 P4 Cu2 136.5(3) . . ? C432 P4 Cu2 116.2(3) . . ? C15 N1 C31 119.3(7) . . ? C15 N1 Cu1 115.3(6) . . ? C31 N1 Cu1 125.1(5) . . ? C215 N2 C231 119.4(6) . . ? C215 N2 Cu1 115.7(5) . . ? C231 N2 Cu1 124.7(5) . . ? C315 N3 C331 118.5(7) . . ? C315 N3 Cu2 116.5(5) . . ? C331 N3 Cu2 125.0(5) . . ? C415 N4 C431 118.4(6) . . ? C415 N4 Cu2 115.1(5) . . ? C431 N4 Cu2 126.5(5) . . ? C2 C1 C15 128.6(8) . . ? C2 C1 P1 111.9(7) . . ? C15 C1 P1 118.7(6) . . ? C1 C2 C7 112.5(7) . . ? C1 C2 C3 125.0(10) . . ? C7 C2 C3 122.5(9) . . ? C1 C2 C3' 126.8(12) . . ? C7 C2 C3' 119.9(9) . . ? C3 C2 C3' 6(5) . . ? C2 C3 C4 114.9(13) . . ? C3 C4 C5 112.5(18) . . ? C6 C5 C4 109.4(18) . . ? C5 C6 C7 112.3(14) . . ? C8 C7 C2 114.5(7) . . ? C8 C7 C6' 122.5(10) . . ? C2 C7 C6' 121.6(9) . . ? C8 C7 C6 128.2(9) . . ? C2 C7 C6 117.1(9) . . ? C6' C7 C6 17(2) . . ? C2 C3' C4' 113.5(16) . . ? C3' C4' C5' 109(2) . . ? C6' C5' C4' 109.0(19) . . ? C5' C6' C7 108.4(17) . . ? C7 C8 C9 124.3(7) . . ? C7 C8 P1 109.9(6) . . ? C9 C8 P1 125.6(6) . . ? C10 C9 C14 117.6(9) . . ? C10 C9 C8 120.7(8) . . ? C14 C9 C8 121.7(8) . . ? C11 C10 C9 121.8(9) . . ? C10 C11 C12 119.1(9) . . ? C13 C12 C11 120.7(10) . . ? C12 C13 C14 120.2(9) . . ? C13 C14 C9 120.4(9) . . ? N1 C15 C16 122.1(9) . . ? N1 C15 C16' 115.0(11) . . ? C16 C15 C16' 25.9(10) . . ? N1 C15 C1 115.5(7) . . ? C16 C15 C1 120.4(9) . . ? C16' C15 C1 128.2(10) . . ? C17 C16 C15 113.3(12) . . ? C16 C17 C18 123.5(15) . . ? C31 C18 C19 117.9(12) . . ? C31 C18 C17 111.8(15) . . ? C19 C18 C17 125.7(15) . . ? C28 C19 C20 118.8(14) . . ? C28 C19 C18 117.7(11) . . ? C20 C19 C18 122.1(14) . . ? C21 C20 C25 110.2(11) . . ? C21 C20 C19 131.0(12) . . ? C25 C20 C19 118.9(11) . . ? C22 C21 C20 130.8(13) . . ? C21 C22 C23 117.2(14) . . ? C22 C23 C24 120.2(14) . . ? C23 C24 C25 121.5(13) . . ? C26 C25 C24 121.5(13) . . ? C26 C25 C20 118.3(12) . . ? C24 C25 C20 119.8(12) . . ? C27 C26 C25 122.8(13) . . ? C26 C27 C28 119.3(12) . . ? C19 C28 C29 120.3(13) . . ? C19 C28 C27 120.7(14) . . ? C29 C28 C27 118.9(12) . . ? C30 C29 C28 120.7(13) . . ? C29 C30 C31 118.6(14) . . ? C17' C16' C15 123.8(16) . . ? C16' C17' C18' 121.8(17) . . ? C19' C18' C17' 125(3) . . ? C19' C18' C31 122.5(15) . . ? C17' C18' C31 108.4(15) . . ? C28' C19' C18' 117.6(15) . . ? C28' C19' C20' 116(2) . . ? C18' C19' C20' 123(2) . . ? C21' C20' C25' 110.6(15) . . ? C21' C20' C19' 126.1(17) . . ? C25' C20' C19' 123.3(16) . . ? C22' C21' C20' 126.3(18) . . ? C21' C22' C23' 121(2) . . ? C22' C23' C24' 121(2) . . ? C23' C24' C25' 116.6(19) . . ? C26' C25' C24' 117.6(17) . . ? C26' C25' C20' 115.3(15) . . ? C24' C25' C20' 124.3(17) . . ? C27' C26' C25' 120.6(17) . . ? C26' C27' C28' 124.5(16) . . ? C19' C28' C27' 117.6(16) . . ? C19' C28' C29' 120.8(16) . . ? C27' C28' C29' 121.6(16) . . ? C30' C29' C28' 120.6(19) . . ? C29' C30' C31 123.8(19) . . ? N1 C31 C18 120.2(9) . . ? N1 C31 C30 115.9(9) . . ? C18 C31 C30 123.9(11) . . ? N1 C31 C30' 121.7(11) . . ? C18 C31 C30' 116.7(13) . . ? C30 C31 C30' 14.7(15) . . ? N1 C31 C18' 124.5(10) . . ? C18 C31 C18' 7(3) . . ? C30 C31 C18' 119.2(11) . . ? C30' C31 C18' 113.3(14) . . ? C33 C32 C37 118.6(9) . . ? C33 C32 P1 121.0(8) . . ? C37 C32 P1 120.3(8) . . ? C32 C33 C34 119.9(12) . . ? C35 C34 C33 121.9(12) . . ? C34 C35 C36 119.3(12) . . ? C35 C36 C37 119.8(13) . . ? C36 C37 C32 120.3(12) . . ? C202 C201 C215 129.3(7) . . ? C202 C201 P2 109.7(6) . . ? C215 C201 P2 119.0(6) . . ? C201 C202 C207 114.0(7) . . ? C201 C202 C203 125.1(7) . . ? C207 C202 C203 120.5(7) . . ? C204 C203 C202 113.2(6) . . ? C203 C204 C205 111.4(7) . . ? C206 C205 C204 110.7(7) . . ? C205 C206 C207 114.0(6) . . ? C208 C207 C202 113.2(6) . . ? C208 C207 C206 127.9(7) . . ? C202 C207 C206 118.9(6) . . ? C207 C208 C209 128.0(7) . . ? C207 C208 P2 111.4(6) . . ? C209 C208 P2 120.5(6) . . ? C214 C209 C210 117.6(7) . . ? C214 C209 C208 120.8(8) . . ? C210 C209 C208 121.4(7) . . ? C211 C210 C209 121.2(8) . . ? C212 C211 C210 119.4(8) . . ? C213 C212 C211 120.9(8) . . ? C212 C213 C214 119.6(9) . . ? C209 C214 C213 121.3(8) . . ? N2 C215 C216 121.4(7) . . ? N2 C215 C201 115.9(7) . . ? C216 C215 C201 122.5(7) . . ? C217 C216 C215 119.4(7) . . ? C216 C217 C218 121.7(7) . . ? C231 C218 C217 114.8(7) . . ? C231 C218 C219 119.3(7) . . ? C217 C218 C219 125.6(7) . . ? C228 C219 C218 117.0(7) . . ? C228 C219 C220 117.7(7) . . ? C218 C219 C220 125.2(7) . . ? C221 C220 C225 115.6(7) . . ? C221 C220 C219 125.1(7) . . ? C225 C220 C219 119.1(7) . . ? C221 C220 Cl5C 101(2) . 2_666 ? C225 C220 Cl5C 58.8(15) . 2_666 ? C219 C220 Cl5C 103(2) . 2_666 ? C222 C221 C220 123.6(8) . . ? C221 C222 C223 118.5(8) . . ? C224 C223 C222 119.1(8) . . ? C223 C224 C225 123.5(8) . . ? C224 C225 C226 121.7(8) . . ? C224 C225 C220 119.1(8) . . ? C226 C225 C220 119.2(7) . . ? C224 C225 Cl5C 99(3) . 2_666 ? C226 C225 Cl5C 88(3) . 2_666 ? C220 C225 Cl5C 82(4) . 2_666 ? C227 C226 C225 122.0(8) . . ? C226 C227 C228 121.1(8) . . ? C219 C228 C229 120.4(7) . . ? C219 C228 C227 119.7(8) . . ? C229 C228 C227 119.8(8) . . ? C230 C229 C228 122.8(8) . . ? C229 C230 C231 118.3(8) . . ? N2 C231 C230 117.3(7) . . ? N2 C231 C218 121.4(7) . . ? C230 C231 C218 121.2(7) . . ? C237 C232 C233 117.1(8) . . ? C237 C232 P2 122.0(7) . . ? C233 C232 P2 120.9(7) . . ? C234 C233 C232 120.7(9) . . ? C235 C234 C233 120.2(9) . . ? C236 C235 C234 120.3(9) . . ? C235 C236 C237 120.8(9) . . ? C236 C237 C232 120.7(9) . . ? C302 C301 C315 129.7(8) . . ? C302 C301 P3 111.5(6) . . ? C315 C301 P3 117.7(6) . . ? C301 C302 C307 112.2(7) . . ? C301 C302 C303 126.7(8) . . ? C307 C302 C303 121.1(7) . . ? C302 C303 C304 112.6(7) . . ? C303 C304 C305 109.3(8) . . ? C304 C305 C306 109.8(7) . . ? C307 C306 C305 112.4(7) . . ? C308 C307 C302 114.7(8) . . ? C308 C307 C306 125.0(8) . . ? C302 C307 C306 120.3(8) . . ? C307 C308 C309 128.3(8) . . ? C307 C308 P3 110.0(7) . . ? C309 C308 P3 121.1(6) . . ? C314 C309 C310 117.9(9) . . ? C314 C309 C308 122.3(8) . . ? C310 C309 C308 119.7(8) . . ? C311 C310 C309 119.7(9) . . ? C312 C311 C310 121.9(10) . . ? C311 C312 C313 117.9(10) . . ? C314 C313 C312 121.8(10) . . ? C313 C314 C309 120.9(9) . . ? N3 C315 C316 120.6(7) . . ? N3 C315 C301 114.8(7) . . ? C316 C315 C301 124.6(7) . . ? C317 C316 C315 119.7(8) . . ? C316 C317 C318 123.6(8) . . ? C317 C318 C331 113.4(7) . . ? C317 C318 C319 127.3(8) . . ? C331 C318 C319 118.9(7) . . ? C328 C319 C318 119.1(7) . . ? C328 C319 C320 117.6(7) . . ? C318 C319 C320 123.3(7) . . ? C325 C320 C321 113.6(8) . . ? C325 C320 C319 118.9(7) . . ? C321 C320 C319 127.3(8) . . ? C322 C321 C320 125.1(8) . . ? C321 C322 C323 119.1(9) . . ? C324 C323 C322 118.4(9) . . ? C325 C324 C323 122.0(9) . . ? C324 C325 C320 120.9(8) . . ? C324 C325 C326 120.2(8) . . ? C320 C325 C326 118.9(8) . . ? C327 C326 C325 121.6(8) . . ? C326 C327 C328 120.7(8) . . ? C327 C328 C329 120.2(7) . . ? C327 C328 C319 121.5(8) . . ? C329 C328 C319 118.4(7) . . ? C330 C329 C328 123.3(7) . . ? C329 C330 C331 120.3(8) . . ? N3 C331 C318 123.3(7) . . ? N3 C331 C330 117.3(8) . . ? C318 C331 C330 119.3(8) . . ? C337 C332 C333 117.0(8) . . ? C337 C332 P3 120.6(6) . . ? C333 C332 P3 122.4(7) . . ? C334 C333 C332 120.6(9) . . ? C335 C334 C333 121.4(9) . . ? C334 C335 C336 120.2(9) . . ? C337 C336 C335 117.8(10) . . ? C336 C337 C332 123.0(9) . . ? C402 C401 C415 127.8(7) . . ? C402 C401 P4 111.0(6) . . ? C415 C401 P4 118.9(6) . . ? C401 C402 C407 112.2(7) . . ? C401 C402 C403 125.9(7) . . ? C407 C402 C403 121.2(7) . . ? C402 C403 C404 113.2(7) . . ? C405 C404 C403 113.4(8) . . ? C404 C405 C406 113.5(8) . . ? C405 C406 C407 112.7(7) . . ? C408 C407 C402 114.8(7) . . ? C408 C407 C406 125.9(7) . . ? C402 C407 C406 119.3(7) . . ? C407 C408 C409 128.0(8) . . ? C407 C408 P4 110.9(6) . . ? C409 C408 P4 121.1(6) . . ? C414 C409 C410 117.9(8) . . ? C414 C409 C408 120.9(8) . . ? C410 C409 C408 121.2(8) . . ? C411 C410 C409 121.3(9) . . ? C410 C411 C412 119.5(9) . . ? C413 C412 C411 119.2(9) . . ? C414 C413 C412 121.1(9) . . ? C413 C414 C409 120.8(9) . . ? N4 C415 C416 121.8(7) . . ? N4 C415 C401 116.7(7) . . ? C416 C415 C401 121.5(7) . . ? C417 C416 C415 119.0(7) . . ? C416 C417 C418 122.6(7) . . ? C431 C418 C417 114.1(7) . . ? C431 C418 C419 119.6(7) . . ? C417 C418 C419 126.0(7) . . ? C428 C419 C418 118.1(7) . . ? C428 C419 C420 118.3(7) . . ? C418 C419 C420 123.7(7) . . ? C425 C420 C421 115.6(7) . . ? C425 C420 C419 118.6(7) . . ? C421 C420 C419 125.5(7) . . ? C422 C421 C420 123.3(8) . . ? C421 C422 C423 120.1(8) . . ? C424 C423 C422 119.8(8) . . ? C423 C424 C425 121.5(8) . . ? C420 C425 C426 120.4(8) . . ? C420 C425 C424 118.8(8) . . ? C426 C425 C424 120.8(8) . . ? C427 C426 C425 120.2(8) . . ? C426 C427 C428 122.0(8) . . ? C427 C428 C419 119.5(7) . . ? C427 C428 C429 120.5(8) . . ? C419 C428 C429 119.9(7) . . ? C430 C429 C428 121.8(7) . . ? C429 C430 C431 119.4(7) . . ? N4 C431 C418 122.3(6) . . ? N4 C431 C430 117.7(7) . . ? C418 C431 C430 119.9(7) . . ? C433 C432 C437 117.6(9) . . ? C433 C432 P4 121.6(7) . . ? C437 C432 P4 120.7(7) . . ? C434 C433 C432 122.1(10) . . ? C433 C434 C435 119.4(10) . . ? C436 C435 C434 119.5(10) . . ? C435 C436 C437 119.6(10) . . ? C436 C437 C432 121.8(9) . . ? F10 P10 F13 89.1(4) . . ? F10 P10 F12 90.2(4) . . ? F13 P10 F12 178.5(4) . . ? F10 P10 F14 88.8(3) . . ? F13 P10 F14 90.2(4) . . ? F12 P10 F14 88.5(4) . . ? F10 P10 F15 178.2(4) . . ? F13 P10 F15 92.2(5) . . ? F12 P10 F15 88.6(5) . . ? F14 P10 F15 92.4(3) . . ? F10 P10 F11 92.0(3) . . ? F13 P10 F11 90.2(4) . . ? F12 P10 F11 91.1(4) . . ? F14 P10 F11 179.1(3) . . ? F15 P10 F11 86.8(3) . . ? F21 P20 F20 93.3(5) . . ? F21 P20 F24 177.1(5) . . ? F20 P20 F24 89.5(5) . . ? F21 P20 F25 89.4(5) . . ? F20 P20 F25 177.3(5) . . ? F24 P20 F25 87.8(5) . . ? F21 P20 F22 89.8(3) . . ? F20 P20 F22 90.1(3) . . ? F24 P20 F22 89.7(3) . . ? F25 P20 F22 89.6(3) . . ? F21 P20 F23 91.0(3) . . ? F20 P20 F23 90.1(3) . . ? F24 P20 F23 89.4(3) . . ? F25 P20 F23 90.1(3) . . ? F22 P20 F23 179.1(3) . . ? Cl1 C900 Cl2 115.9(9) . . ? Cl12 C910 Cl11 112.2(6) . . ? Cl21 C920 Cl22 111.3(7) . . ? Cl32 C930 Cl31 114.8(7) . . ? Cl4A C94A Cl5A 119(2) . . ? Cl4B C94B Cl5B 119.3(18) . . ? Cl4C C94C Cl5C 120(3) . . ? C94C Cl5C C225 150(9) . 2_666 ? C94C Cl5C C220 112(7) . 2_666 ? C225 Cl5C C220 39(3) 2_666 2_666 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.842 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.096 #===END # Attachment 'compound3b.cif' data_compound3b _database_code_depnum_ccdc_archive 'CCDC 651122' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75.50 H59 Cl3 F12 N2 P2 Pd Sb2' _chemical_formula_weight 1740.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 18.695(5) _cell_length_b 18.695(5) _cell_length_c 81.280(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28408(11) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13808 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _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 86356 _diffrn_reflns_av_R_equivalents 0.2627 _diffrn_reflns_av_sigmaI/netI 0.1297 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -90 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.25 _reflns_number_total 10112 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A twist disorder on two positions of one cyclohexane system and a disorder on two positions of a non coordinated dichloromethane molecule are refined anisotropically with the help of 397 ADP- and distances-restraints. ; _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^)+(0.0000P)^2^+1228.4668P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10112 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 397 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_gt 0.1074 _refine_ls_wR_factor_ref 0.2542 _refine_ls_wR_factor_gt 0.2213 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.75293(7) 0.04420(7) 0.556361(15) 0.0502(4) Uani 1 1 d . . . P1 P 0.6878(3) 0.0695(2) 0.57887(5) 0.0542(13) Uani 1 1 d . A . P2 P 0.8166(2) -0.0524(3) 0.56389(5) 0.0502(12) Uani 1 1 d . . . N1 N 0.6815(7) 0.1209(7) 0.54590(15) 0.047(3) Uani 1 1 d . A . N2 N 0.8253(6) 0.0420(7) 0.53646(15) 0.040(3) Uani 1 1 d . . . C1 C 0.6820(11) 0.1598(10) 0.57322(19) 0.062(5) Uani 1 1 d . A . C2 C 0.7147(11) 0.2038(10) 0.5835(2) 0.066(5) Uani 1 1 d DU . . C3 C 0.747(2) 0.2755(12) 0.5809(3) 0.072(7) Uani 0.75(3) 1 d PDU A 1 H3A H 0.7149 0.3032 0.5735 0.087 Uiso 0.75(3) 1 calc PR A 1 H3B H 0.7929 0.2692 0.5750 0.087 Uiso 0.75(3) 1 calc PR A 1 C4 C 0.7603(19) 0.3186(13) 0.5960(3) 0.079(7) Uani 0.75(3) 1 d PDU A 1 H4A H 0.7145 0.3305 0.6015 0.094 Uiso 0.75(3) 1 calc PR A 1 H4B H 0.7850 0.3638 0.5932 0.094 Uiso 0.75(3) 1 calc PR A 1 C5 C 0.8098(16) 0.2707(14) 0.6081(3) 0.079(7) Uani 0.75(3) 1 d PDU A 1 H5A H 0.8552 0.2588 0.6024 0.095 Uiso 0.75(3) 1 calc PR A 1 H5B H 0.8214 0.2985 0.6181 0.095 Uiso 0.75(3) 1 calc PR A 1 C6 C 0.773(2) 0.2048(12) 0.6127(2) 0.067(7) Uani 0.75(3) 1 d PDU A 1 H6A H 0.7361 0.2168 0.6210 0.080 Uiso 0.75(3) 1 calc PR A 1 H6B H 0.8078 0.1725 0.6180 0.080 Uiso 0.75(3) 1 calc PR A 1 C7 C 0.7367(11) 0.1642(11) 0.59879(19) 0.065(5) Uani 1 1 d DU A . C3' C 0.734(6) 0.281(2) 0.5831(8) 0.073(10) Uani 0.25(3) 1 d PDU A 2 H3'1 H 0.6901 0.3097 0.5847 0.087 Uiso 0.25(3) 1 calc PR A 2 H3'2 H 0.7528 0.2925 0.5720 0.087 Uiso 0.25(3) 1 calc PR A 2 C4' C 0.788(4) 0.304(3) 0.5955(7) 0.075(10) Uani 0.25(3) 1 d PDU A 2 H4'1 H 0.7949 0.3566 0.5951 0.090 Uiso 0.25(3) 1 calc PR A 2 H4'2 H 0.8348 0.2808 0.5933 0.090 Uiso 0.25(3) 1 calc PR A 2 C5' C 0.758(5) 0.280(2) 0.6134(6) 0.077(9) Uani 0.25(3) 1 d PDU A 2 H5'1 H 0.7902 0.2993 0.6221 0.092 Uiso 0.25(3) 1 calc PR A 2 H5'2 H 0.7100 0.3007 0.6151 0.092 Uiso 0.25(3) 1 calc PR A 2 C6' C 0.755(7) 0.203(2) 0.6146(5) 0.068(10) Uani 0.25(3) 1 d PDU A 2 H6'1 H 0.7189 0.1897 0.6230 0.082 Uiso 0.25(3) 1 calc PR A 2 H6'2 H 0.8019 0.1849 0.6185 0.082 Uiso 0.25(3) 1 calc PR A 2 C8 C 0.7256(9) 0.0923(10) 0.59857(17) 0.051(5) Uani 1 1 d . . . C9 C 0.7322(11) 0.0430(11) 0.61298(19) 0.070(6) Uani 1 1 d . A . C10 C 0.6929(13) 0.0515(13) 0.6267(2) 0.099(8) Uani 1 1 d . . . H10 H 0.6572 0.0877 0.6269 0.119 Uiso 1 1 calc R A . C11 C 0.7026(13) 0.0092(14) 0.6406(3) 0.110(9) Uani 1 1 d . A . H11 H 0.6742 0.0160 0.6502 0.132 Uiso 1 1 calc R . . C12 C 0.7540(12) -0.0418(12) 0.6401(2) 0.087(7) Uani 1 1 d . . . H12 H 0.7601 -0.0721 0.6494 0.105 Uiso 1 1 calc R A . C13 C 0.7984(9) -0.0519(9) 0.6265(2) 0.060(5) Uani 1 1 d . A . H13 H 0.8357 -0.0865 0.6266 0.072 Uiso 1 1 calc R . . C14 C 0.7856(10) -0.0092(11) 0.6128(2) 0.064(5) Uani 1 1 d . . . H14 H 0.8137 -0.0156 0.6031 0.077 Uiso 1 1 calc R A . C15 C 0.6610(9) 0.1736(9) 0.55558(19) 0.053(5) Uani 1 1 d . . . C16 C 0.6191(9) 0.2311(8) 0.55038(18) 0.044(4) Uani 1 1 d . A . C17 C 0.5888(10) 0.2807(11) 0.5614(2) 0.066(5) Uani 1 1 d . . . H17 H 0.5938 0.2723 0.5729 0.079 Uiso 1 1 calc R A . C18 C 0.5532(10) 0.3391(9) 0.5565(2) 0.064(5) Uani 1 1 d . A . H18 H 0.5280 0.3675 0.5643 0.077 Uiso 1 1 calc R . . C19 C 0.5535(8) 0.3582(10) 0.5393(2) 0.050(4) Uani 1 1 d . . . C20 C 0.5246(9) 0.4248(9) 0.5345(2) 0.060(5) Uani 1 1 d . A . H20 H 0.5018 0.4545 0.5424 0.073 Uiso 1 1 calc R . . C21 C 0.5297(11) 0.4470(11) 0.5182(2) 0.073(6) Uani 1 1 d . . . H21 H 0.5101 0.4913 0.5146 0.087 Uiso 1 1 calc R A . C22 C 0.5653(11) 0.4008(10) 0.5070(2) 0.064(5) Uani 1 1 d . A . H22 H 0.5711 0.4154 0.4959 0.077 Uiso 1 1 calc R . . C23 C 0.5908(10) 0.3379(9) 0.5117(2) 0.061(5) Uani 1 1 d . . . H23 H 0.6159 0.3098 0.5039 0.073 Uiso 1 1 calc R A . C24 C 0.5824(9) 0.3107(9) 0.52776(19) 0.053(5) Uani 1 1 d . A . C25 C 0.6113(8) 0.2433(8) 0.53303(19) 0.044(4) Uani 1 1 d . . . C26 C 0.6285(8) 0.1831(8) 0.52263(18) 0.045(4) Uani 1 1 d . A . C27 C 0.6025(9) 0.1755(9) 0.50600(17) 0.048(4) Uani 1 1 d . . . H27 H 0.5723 0.2114 0.5015 0.057 Uiso 1 1 calc R A . C28 C 0.6203(10) 0.1179(10) 0.4966(2) 0.060(5) Uani 1 1 d . A . H28 H 0.6076 0.1169 0.4853 0.072 Uiso 1 1 calc R . . C29 C 0.6564(10) 0.0612(10) 0.5034(2) 0.061(5) Uani 1 1 d . . . H29 H 0.6673 0.0207 0.4968 0.073 Uiso 1 1 calc R A . C30 C 0.6773(8) 0.0626(10) 0.51989(19) 0.054(5) Uani 1 1 d . A . H30 H 0.7019 0.0231 0.5246 0.065 Uiso 1 1 calc R . . C31 C 0.6620(9) 0.1209(9) 0.52909(19) 0.049(4) Uani 1 1 d . . . C32 C 0.6021(10) 0.0329(9) 0.58070(19) 0.054(5) Uani 1 1 d . . . C33 C 0.5765(10) -0.0221(10) 0.5702(2) 0.059(5) Uani 1 1 d . A . H33 H 0.6087 -0.0427 0.5625 0.071 Uiso 1 1 calc R . . C34 C 0.5095(12) -0.0462(13) 0.5707(2) 0.082(7) Uani 1 1 d . . . H34 H 0.4936 -0.0802 0.5628 0.098 Uiso 1 1 calc R A . C35 C 0.4626(11) -0.0210(13) 0.5828(3) 0.087(7) Uani 1 1 d . A . H35 H 0.4158 -0.0404 0.5838 0.104 Uiso 1 1 calc R . . C36 C 0.4845(12) 0.0304(14) 0.5929(2) 0.080(7) Uani 1 1 d . . . H36 H 0.4517 0.0491 0.6008 0.096 Uiso 1 1 calc R A . C37 C 0.5531(10) 0.0577(10) 0.5925(2) 0.059(5) Uani 1 1 d . A . H37 H 0.5672 0.0932 0.6002 0.071 Uiso 1 1 calc R . . C101 C 0.8322(11) -0.0790(10) 0.54239(19) 0.062(5) Uani 1 1 d . . . C102 C 0.7980(9) -0.1424(8) 0.5400(2) 0.046(4) Uani 1 1 d . . . C103 C 0.7815(10) -0.1739(11) 0.5238(2) 0.068(5) Uani 1 1 d . . . H10A H 0.8262 -0.1929 0.5189 0.081 Uiso 1 1 calc R . . H10B H 0.7637 -0.1356 0.5164 0.081 Uiso 1 1 calc R . . C104 C 0.7275(13) -0.2324(12) 0.5243(2) 0.086(7) Uani 1 1 d . . . H10C H 0.7275 -0.2583 0.5137 0.104 Uiso 1 1 calc R . . H10D H 0.6793 -0.2116 0.5260 0.104 Uiso 1 1 calc R . . C105 C 0.7437(12) -0.2847(10) 0.5382(3) 0.080(6) Uani 1 1 d . . . H10E H 0.7098 -0.3254 0.5376 0.096 Uiso 1 1 calc R . . H10F H 0.7927 -0.3039 0.5368 0.096 Uiso 1 1 calc R . . C106 C 0.7375(10) -0.2490(10) 0.5547(2) 0.066(5) Uani 1 1 d . . . H10G H 0.6862 -0.2443 0.5576 0.079 Uiso 1 1 calc R . . H10H H 0.7603 -0.2798 0.5631 0.079 Uiso 1 1 calc R . . C107 C 0.7712(8) -0.1773(9) 0.5552(2) 0.045(4) Uani 1 1 d . . . C108 C 0.7780(8) -0.1364(9) 0.56887(19) 0.048(4) Uani 1 1 d . . . C109 C 0.7553(10) -0.1626(9) 0.5855(2) 0.054(5) Uani 1 1 d . . . C110 C 0.6924(12) -0.1398(12) 0.5925(2) 0.084(7) Uani 1 1 d . . . H110 H 0.6646 -0.1040 0.5872 0.101 Uiso 1 1 calc R . . C111 C 0.6699(11) -0.1688(12) 0.6071(3) 0.087(7) Uani 1 1 d . . . H111 H 0.6245 -0.1557 0.6113 0.105 Uiso 1 1 calc R . . C112 C 0.7117(11) -0.2163(13) 0.6156(3) 0.084(7) Uani 1 1 d . . . H112 H 0.6969 -0.2335 0.6261 0.101 Uiso 1 1 calc R . . C113 C 0.7752(12) -0.2386(11) 0.6089(2) 0.076(6) Uani 1 1 d . . . H113 H 0.8030 -0.2737 0.6144 0.091 Uiso 1 1 calc R . . C114 C 0.7996(9) -0.2105(10) 0.5940(2) 0.061(5) Uani 1 1 d . . . H114 H 0.8451 -0.2235 0.5897 0.074 Uiso 1 1 calc R . . C115 C 0.8489(8) -0.0187(9) 0.53158(19) 0.041(4) Uani 1 1 d . . . C116 C 0.8858(9) -0.0279(9) 0.5158(2) 0.051(4) Uani 1 1 d . . . C117 C 0.9216(9) -0.0911(10) 0.5119(2) 0.059(5) Uani 1 1 d . . . H117 H 0.9264 -0.1273 0.5201 0.071 Uiso 1 1 calc R . . C118 C 0.9494(11) -0.1016(13) 0.4969(3) 0.080(7) Uani 1 1 d . . . H118 H 0.9763 -0.1436 0.4947 0.096 Uiso 1 1 calc R . . C119 C 0.9385(11) -0.0487(13) 0.4842(2) 0.072(6) Uani 1 1 d . . . C120 C 0.9606(11) -0.0631(14) 0.4676(3) 0.088(7) Uani 1 1 d . . . H120 H 0.9861 -0.1057 0.4650 0.105 Uiso 1 1 calc R . . C121 C 0.9448(16) -0.0157(17) 0.4556(3) 0.101(9) Uani 1 1 d . . . H121 H 0.9610 -0.0246 0.4448 0.121 Uiso 1 1 calc R . . C122 C 0.9073(16) 0.0433(18) 0.4586(3) 0.107(9) Uani 1 1 d . . . H122 H 0.8959 0.0748 0.4498 0.128 Uiso 1 1 calc R . . C123 C 0.8842(12) 0.0594(14) 0.4746(3) 0.093(7) Uani 1 1 d . . . H123 H 0.8563 0.1010 0.4765 0.111 Uiso 1 1 calc R . . C124 C 0.9023(11) 0.0143(12) 0.4879(2) 0.067(6) Uani 1 1 d . . . C125 C 0.8813(10) 0.0287(10) 0.5049(2) 0.059(5) Uani 1 1 d . . . C126 C 0.8651(9) 0.0981(10) 0.5111(2) 0.055(5) Uani 1 1 d . . . C127 C 0.8783(9) 0.1631(11) 0.5035(2) 0.060(5) Uani 1 1 d . . . H127 H 0.8947 0.1625 0.4925 0.073 Uiso 1 1 calc R . . C128 C 0.8693(13) 0.2271(13) 0.5109(3) 0.093(7) Uani 1 1 d . . . H128 H 0.8792 0.2696 0.5049 0.111 Uiso 1 1 calc R . . C129 C 0.8449(11) 0.2322(10) 0.5276(3) 0.072(6) Uani 1 1 d . . . H129 H 0.8381 0.2768 0.5330 0.087 Uiso 1 1 calc R . . C130 C 0.8321(9) 0.1684(10) 0.5352(2) 0.061(5) Uani 1 1 d . . . H130 H 0.8174 0.1693 0.5464 0.073 Uiso 1 1 calc R . . C131 C 0.8390(8) 0.1034(9) 0.52771(19) 0.046(4) Uani 1 1 d . . . C132 C 0.8960(9) -0.0358(10) 0.57552(18) 0.048(4) Uani 1 1 d . . . C133 C 0.9401(9) -0.0940(9) 0.58090(18) 0.049(4) Uani 1 1 d . . . H133 H 0.9277 -0.1421 0.5784 0.059 Uiso 1 1 calc R . . C134 C 0.9998(10) -0.0788(12) 0.5896(2) 0.060(5) Uani 1 1 d . . . H134 H 1.0282 -0.1174 0.5936 0.072 Uiso 1 1 calc R . . C135 C 1.0207(11) -0.0114(13) 0.5930(2) 0.064(5) Uani 1 1 d . . . H135 H 1.0643 -0.0034 0.5987 0.077 Uiso 1 1 calc R . . C136 C 0.9806(12) 0.0443(12) 0.58835(19) 0.066(6) Uani 1 1 d . . . H136 H 0.9942 0.0919 0.5910 0.079 Uiso 1 1 calc R . . C137 C 0.9171(10) 0.0304(12) 0.5793(2) 0.064(5) Uani 1 1 d . . . H137 H 0.8885 0.0697 0.5759 0.077 Uiso 1 1 calc R . . Sb1 Sb -0.0097(14) 0.2549(15) 0.56675(4) 0.107(5) Uani 0.50 1 d PDU B -1 F1 F 0.0647(19) 0.3192(17) 0.5645(5) 0.159(16) Uani 0.50 1 d PDU B -1 F2 F 0.0566(16) 0.1819(17) 0.5691(7) 0.150(17) Uani 0.50 1 d PDU B -1 F3 F -0.008(3) 0.269(3) 0.58920(15) 0.15(2) Uani 0.50 1 d PDU B -1 F4 F -0.0839(15) 0.1913(16) 0.5693(4) 0.091(10) Uani 0.50 1 d PDU B -1 F5 F -0.0741(18) 0.3286(15) 0.5644(6) 0.170(18) Uani 0.50 1 d PDU B -1 F6 F -0.011(3) 0.240(2) 0.54434(17) 0.112(12) Uani 0.50 1 d PDU B -1 Sb2 Sb 1.0000 0.7500 0.630612(19) 0.0572(5) Uani 1 2 d SD . . F21 F 1.0000 0.7500 0.65339(12) 0.109(6) Uani 1 2 d SD . . F22 F 0.9408(6) 0.6706(6) 0.63054(13) 0.088(3) Uani 1 1 d D . . F23 F 0.9231(7) 0.8091(6) 0.63099(19) 0.117(5) Uani 1 1 d . . . F24 F 1.0000 0.7500 0.60793(14) 0.147(10) Uani 1 2 d SD . . Sb3 Sb 1.0000 0.7500 0.54809(2) 0.0603(5) Uani 1 2 d S . . F31 F 0.9330(8) 0.7342(7) 0.56421(17) 0.117(5) Uani 1 1 d . . . F32 F 0.9826(6) 0.8450(5) 0.54782(11) 0.077(3) Uani 1 1 d . . . F33 F 1.0660(8) 0.7625(8) 0.53201(17) 0.130(5) Uani 1 1 d . . . Sb4 Sb 0.5077(14) 0.7584(16) 0.54130(2) 0.075(4) Uani 0.50 1 d PDU C -1 F41 F 0.5757(16) 0.6864(18) 0.5402(6) 0.075(9) Uani 0.50 1 d PDU C -1 F42 F 0.557(3) 0.796(3) 0.5590(3) 0.119(11) Uani 0.50 1 d PDU C -1 F43 F 0.5632(12) 0.8133(12) 0.5274(3) 0.094(7) Uani 0.50 1 d PDU C -1 F44 F 0.4411(17) 0.8311(19) 0.5425(5) 0.089(9) Uani 0.50 1 d PDU C -1 F45 F 0.4620(12) 0.7211(12) 0.5232(2) 0.075(6) Uani 0.50 1 d PDU C -1 F46 F 0.452(3) 0.703(3) 0.5551(3) 0.101(8) Uani 0.50 1 d PDU C -1 C201 C 0.251(9) 0.059(4) 0.5591(9) 0.28(2) Uani 0.46(3) 1 d PDU D 1 H20A H 0.2822 0.0871 0.5666 0.335 Uiso 0.46(3) 1 calc PR D 1 H20B H 0.2010 0.0646 0.5628 0.335 Uiso 0.46(3) 1 calc PR D 1 Cl3 Cl 0.2766(19) -0.0338(16) 0.5595(6) 0.38(2) Uani 0.46(3) 1 d PDU D 1 Cl4 Cl 0.2600(19) 0.0938(19) 0.5384(8) 0.271(16) Uani 0.46(3) 1 d PDU D 1 C202 C 0.227(5) 0.085(6) 0.5475(4) 0.26(2) Uani 0.54(3) 1 d PDU D 2 H20C H 0.2294 0.1348 0.5513 0.308 Uiso 0.54(3) 1 calc PR D 2 H20D H 0.1767 0.0683 0.5485 0.308 Uiso 0.54(3) 1 calc PR D 2 Cl3' Cl 0.284(2) 0.0294(14) 0.5602(5) 0.357(17) Uani 0.54(3) 1 d PDU D 2 Cl4' Cl 0.2549(17) 0.0798(17) 0.5261(4) 0.306(15) Uani 0.54(3) 1 d PDU D 2 C200 C 0.510(3) -0.261(4) 0.6578(5) 0.22(3) Uani 0.50 1 d PDU E -1 H20E H 0.4946 -0.2393 0.6683 0.262 Uiso 0.50 1 calc PR E -1 H20F H 0.5392 -0.3036 0.6602 0.262 Uiso 0.50 1 calc PR E -1 Cl1 Cl 0.5621(16) -0.197(3) 0.6462(6) 0.36(3) Uani 0.50 1 d PDU E -1 Cl2 Cl 0.4319(16) -0.2874(17) 0.6461(3) 0.180(10) Uani 0.50 1 d PDU E -1 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 Pd1 0.0625(10) 0.0552(9) 0.0330(7) 0.0062(6) 0.0038(6) 0.0189(7) P1 0.075(4) 0.054(3) 0.034(2) 0.007(2) 0.006(2) 0.019(2) P2 0.054(3) 0.062(3) 0.034(2) 0.002(2) 0.004(2) 0.016(2) N1 0.055(9) 0.047(9) 0.039(8) 0.010(7) -0.008(7) 0.018(7) N2 0.040(8) 0.038(8) 0.043(8) 0.010(7) -0.006(6) 0.000(6) C1 0.095(15) 0.065(13) 0.027(9) 0.009(9) 0.014(9) 0.022(11) C2 0.110(14) 0.058(9) 0.031(7) -0.001(7) -0.001(8) 0.011(9) C3 0.113(18) 0.060(11) 0.044(11) 0.008(8) -0.001(12) 0.009(12) C4 0.120(19) 0.060(12) 0.057(11) -0.002(8) 0.005(12) -0.002(13) C5 0.119(19) 0.074(13) 0.043(12) -0.004(10) 0.000(11) -0.006(11) C6 0.10(2) 0.067(12) 0.029(10) 0.000(8) 0.006(11) 0.010(11) C7 0.095(13) 0.069(10) 0.031(8) 0.010(6) 0.001(8) -0.001(9) C3' 0.12(2) 0.056(13) 0.047(15) 0.002(14) -0.004(17) 0.013(18) C4' 0.11(2) 0.057(17) 0.054(16) -0.001(14) -0.003(16) 0.009(16) C5' 0.11(2) 0.069(14) 0.049(13) -0.001(14) -0.004(17) 0.017(19) C6' 0.10(3) 0.069(16) 0.032(13) 0.001(12) 0.004(19) 0.02(2) C8 0.059(12) 0.071(13) 0.022(8) -0.003(8) 0.001(7) 0.018(9) C9 0.082(15) 0.099(16) 0.030(9) -0.005(10) 0.012(9) 0.023(12) C10 0.14(2) 0.112(19) 0.050(12) 0.033(12) 0.034(13) 0.043(16) C11 0.11(2) 0.14(2) 0.076(15) 0.075(16) 0.030(14) 0.041(17) C12 0.117(19) 0.090(17) 0.055(12) 0.034(11) 0.013(12) 0.053(14) C13 0.054(12) 0.058(12) 0.068(12) 0.013(10) 0.011(10) 0.032(9) C14 0.070(14) 0.089(15) 0.034(9) -0.010(10) 0.011(9) 0.009(12) C15 0.067(12) 0.055(11) 0.039(9) 0.002(9) 0.005(9) 0.032(9) C16 0.057(11) 0.037(10) 0.038(9) 0.011(8) -0.005(8) 0.012(8) C17 0.081(15) 0.078(15) 0.040(10) -0.012(10) 0.005(10) -0.003(11) C18 0.076(14) 0.043(11) 0.073(13) 0.014(10) 0.020(11) 0.022(10) C19 0.020(9) 0.073(13) 0.058(11) 0.016(10) 0.006(8) 0.000(8) C20 0.062(13) 0.043(11) 0.077(14) -0.005(10) -0.009(10) 0.018(9) C21 0.083(15) 0.068(14) 0.067(13) 0.012(12) -0.040(12) 0.004(11) C22 0.096(16) 0.052(12) 0.046(11) 0.007(10) -0.010(10) 0.001(11) C23 0.091(15) 0.048(12) 0.043(10) 0.010(9) -0.012(10) 0.024(10) C24 0.059(12) 0.058(12) 0.042(10) 0.002(9) -0.001(8) 0.021(9) C25 0.040(10) 0.039(10) 0.051(10) 0.012(8) 0.004(8) 0.013(8) C26 0.049(11) 0.042(10) 0.044(9) 0.014(8) 0.006(8) 0.012(8) C27 0.063(12) 0.052(11) 0.028(8) 0.009(8) -0.004(8) 0.010(9) C28 0.071(13) 0.075(14) 0.034(9) 0.010(10) 0.003(9) 0.005(11) C29 0.072(13) 0.074(14) 0.038(10) 0.000(9) -0.009(9) 0.012(10) C30 0.040(10) 0.080(14) 0.043(10) 0.002(9) 0.012(8) 0.028(9) C31 0.046(11) 0.059(12) 0.042(10) 0.007(9) -0.003(8) 0.016(9) C32 0.076(13) 0.055(12) 0.030(9) -0.004(8) 0.002(9) 0.023(10) C33 0.059(13) 0.079(14) 0.038(10) 0.001(9) 0.002(9) 0.033(10) C34 0.057(14) 0.13(2) 0.059(13) -0.010(13) -0.029(11) 0.000(13) C35 0.049(13) 0.11(2) 0.099(18) -0.008(16) 0.007(13) 0.012(13) C36 0.069(16) 0.12(2) 0.051(12) 0.002(13) 0.014(11) 0.031(14) C37 0.059(13) 0.070(13) 0.048(10) 0.010(9) 0.000(9) 0.010(10) C101 0.102(16) 0.052(12) 0.033(9) -0.002(8) 0.022(9) 0.027(11) C102 0.050(11) 0.031(10) 0.056(11) -0.004(8) -0.006(8) 0.008(8) C103 0.067(13) 0.087(15) 0.050(11) -0.007(10) -0.005(10) -0.009(11) C104 0.12(2) 0.084(17) 0.057(13) -0.019(12) -0.005(13) -0.002(15) C105 0.087(16) 0.049(13) 0.103(17) -0.003(12) 0.008(13) -0.022(11) C106 0.067(13) 0.072(14) 0.059(12) -0.002(11) 0.000(10) -0.004(10) C107 0.041(10) 0.047(11) 0.048(10) 0.001(9) 0.003(8) 0.009(8) C108 0.040(10) 0.059(12) 0.045(10) 0.014(9) 0.000(8) 0.015(8) C109 0.056(12) 0.055(11) 0.050(10) 0.021(9) -0.002(9) 0.003(9) C110 0.091(17) 0.104(18) 0.057(12) 0.026(12) 0.014(12) 0.030(13) C111 0.062(14) 0.113(19) 0.087(15) 0.043(14) 0.020(12) 0.028(13) C112 0.053(14) 0.14(2) 0.060(13) 0.014(13) 0.004(11) -0.016(13) C113 0.074(16) 0.093(16) 0.061(13) 0.026(12) -0.016(11) -0.004(12) C114 0.040(11) 0.082(14) 0.062(12) 0.003(10) 0.000(9) 0.013(10) C115 0.027(9) 0.046(11) 0.051(10) 0.022(8) 0.002(7) -0.007(8) C116 0.064(12) 0.039(10) 0.050(10) -0.010(9) 0.015(9) 0.015(8) C117 0.058(12) 0.060(13) 0.059(12) -0.012(10) 0.006(9) 0.003(10) C118 0.065(14) 0.104(18) 0.071(14) -0.035(13) 0.030(11) -0.025(12) C119 0.070(14) 0.089(17) 0.057(13) -0.009(12) 0.022(11) -0.014(12) C120 0.071(15) 0.12(2) 0.076(15) -0.037(15) 0.019(12) -0.018(13) C121 0.14(3) 0.13(2) 0.035(13) -0.010(15) 0.024(14) -0.033(19) C122 0.13(2) 0.14(3) 0.044(14) -0.002(15) -0.003(14) -0.02(2) C123 0.097(18) 0.12(2) 0.060(14) 0.000(14) 0.012(12) -0.014(14) C124 0.079(15) 0.088(16) 0.034(10) -0.007(10) 0.011(9) -0.021(12) C125 0.074(14) 0.067(14) 0.037(10) -0.001(9) 0.009(9) 0.008(10) C126 0.065(13) 0.059(13) 0.041(10) 0.014(9) -0.006(9) 0.010(9) C127 0.054(12) 0.067(14) 0.060(11) 0.028(11) -0.001(9) -0.016(10) C128 0.13(2) 0.061(16) 0.090(17) 0.024(13) -0.027(15) -0.016(14) C129 0.096(16) 0.038(12) 0.082(15) 0.005(11) 0.002(12) 0.001(10) C130 0.058(12) 0.060(13) 0.065(12) 0.002(11) -0.012(10) 0.015(10) C131 0.035(10) 0.055(12) 0.048(10) -0.004(9) 0.000(8) 0.003(8) C132 0.062(12) 0.046(11) 0.034(9) -0.008(8) 0.008(8) 0.002(9) C133 0.058(12) 0.048(11) 0.040(9) -0.009(8) 0.000(9) 0.004(9) C134 0.055(12) 0.087(16) 0.039(10) 0.015(10) -0.010(9) 0.003(11) C135 0.076(14) 0.088(17) 0.027(9) 0.003(10) -0.001(9) 0.013(13) C136 0.093(16) 0.076(15) 0.028(9) -0.009(9) 0.015(10) -0.024(12) C137 0.066(14) 0.088(16) 0.037(10) 0.011(10) 0.013(10) 0.026(11) Sb1 0.156(12) 0.078(6) 0.0888(18) -0.012(6) 0.034(7) -0.027(7) F1 0.27(4) 0.15(3) 0.053(19) -0.06(2) 0.03(2) -0.13(3) F2 0.093(16) 0.16(3) 0.20(4) 0.02(3) 0.03(2) -0.005(18) F3 0.11(3) 0.26(6) 0.086(8) -0.040(18) 0.023(18) -0.09(3) F4 0.098(14) 0.066(15) 0.11(3) -0.007(16) -0.017(15) 0.006(9) F5 0.30(4) 0.063(16) 0.15(3) -0.007(19) 0.06(4) 0.04(2) F6 0.13(3) 0.11(3) 0.101(9) -0.06(2) 0.007(18) -0.039(18) Sb2 0.0642(12) 0.0632(12) 0.0440(9) 0.000 0.000 -0.0105(9) F21 0.20(2) 0.102(14) 0.019(7) 0.000 0.000 0.023(13) F22 0.087(8) 0.081(8) 0.094(8) -0.011(7) 0.002(7) -0.012(6) F23 0.095(10) 0.069(8) 0.187(15) -0.014(9) -0.014(9) -0.005(7) F24 0.31(3) 0.110(15) 0.019(7) 0.000 0.000 -0.074(17) Sb3 0.0663(13) 0.0639(13) 0.0506(10) 0.000 0.000 0.0147(10) F31 0.128(11) 0.092(10) 0.130(11) 0.016(8) 0.061(9) -0.008(8) F32 0.115(9) 0.065(7) 0.050(6) 0.011(5) -0.013(6) -0.020(6) F33 0.140(12) 0.134(12) 0.115(10) 0.011(9) 0.086(10) 0.004(10) Sb4 0.062(9) 0.129(11) 0.0336(9) -0.002(3) -0.002(2) 0.037(6) F41 0.058(13) 0.121(16) 0.05(2) 0.026(13) 0.015(12) 0.029(11) F42 0.067(17) 0.20(3) 0.091(14) -0.046(18) -0.039(15) 0.050(14) F43 0.084(17) 0.088(17) 0.109(17) 0.004(12) 0.000(12) 0.006(9) F44 0.10(2) 0.14(2) 0.030(14) -0.016(14) -0.028(15) 0.057(14) F45 0.075(10) 0.084(10) 0.066(7) -0.003(7) -0.016(7) 0.015(8) F46 0.09(2) 0.13(2) 0.076(10) -0.005(14) 0.047(14) 0.042(11) C201 0.27(6) 0.13(3) 0.44(4) -0.12(4) 0.07(5) 0.00(4) Cl3 0.29(3) 0.13(2) 0.71(5) -0.10(2) -0.31(4) 0.00(2) Cl4 0.16(2) 0.18(2) 0.47(4) -0.10(3) 0.15(3) -0.015(19) C202 0.26(5) 0.17(4) 0.35(4) -0.10(4) 0.11(4) -0.01(4) Cl3' 0.37(4) 0.079(17) 0.63(4) -0.11(2) -0.04(3) 0.00(2) Cl4' 0.18(2) 0.33(3) 0.40(3) -0.26(2) 0.18(2) -0.090(18) C200 0.11(4) 0.45(10) 0.10(3) 0.11(5) 0.08(2) 0.15(5) Cl1 0.095(16) 0.57(6) 0.42(5) 0.30(4) 0.06(2) 0.116(18) Cl2 0.20(2) 0.25(2) 0.088(12) 0.073(16) 0.049(13) 0.139(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.109(13) . ? Pd1 N1 2.136(12) . ? Pd1 P2 2.247(5) . ? Pd1 P1 2.249(4) . ? P1 C32 1.75(2) . ? P1 C1 1.754(18) . ? P1 C8 1.801(15) . ? P2 C108 1.776(17) . ? P2 C132 1.786(18) . ? P2 C101 1.840(15) . ? N1 C15 1.319(19) . ? N1 C31 1.414(19) . ? N2 C115 1.280(19) . ? N2 C131 1.375(19) . ? C1 C2 1.32(2) . ? C1 C15 1.51(2) . ? C2 C3 1.49(3) . ? C2 C3' 1.49(3) . ? C2 C7 1.50(2) . ? C3 C4 1.49(3) . ? C4 C5 1.62(3) . ? C5 C6 1.46(3) . ? C6 C7 1.52(3) . ? C7 C8 1.36(2) . ? C7 C6' 1.51(3) . ? C3' C4' 1.49(4) . ? C4' C5' 1.62(4) . ? C5' C6' 1.46(3) . ? C8 C9 1.50(2) . ? C9 C10 1.35(2) . ? C9 C14 1.40(2) . ? C10 C11 1.39(2) . ? C11 C12 1.35(3) . ? C12 C13 1.40(2) . ? C13 C14 1.39(2) . ? C15 C16 1.39(2) . ? C16 C17 1.41(2) . ? C16 C25 1.44(2) . ? C17 C18 1.34(2) . ? C18 C19 1.45(2) . ? C19 C24 1.40(2) . ? C19 C20 1.41(2) . ? C20 C21 1.39(2) . ? C21 C22 1.42(3) . ? C22 C23 1.33(2) . ? C23 C24 1.41(2) . ? C24 C25 1.44(2) . ? C25 C26 1.44(2) . ? C26 C31 1.42(2) . ? C26 C27 1.44(2) . ? C27 C28 1.36(2) . ? C28 C29 1.37(2) . ? C29 C30 1.40(2) . ? C30 C31 1.35(2) . ? C32 C37 1.41(2) . ? C32 C33 1.42(2) . ? C33 C34 1.33(2) . ? C34 C35 1.40(3) . ? C35 C36 1.33(3) . ? C36 C37 1.38(3) . ? C101 C102 1.36(2) . ? C101 C115 1.46(2) . ? C102 C103 1.48(2) . ? C102 C107 1.48(2) . ? C103 C104 1.49(3) . ? C104 C105 1.52(3) . ? C105 C106 1.51(3) . ? C106 C107 1.48(2) . ? C107 C108 1.35(2) . ? C108 C109 1.50(2) . ? C109 C110 1.37(2) . ? C109 C114 1.40(2) . ? C110 C111 1.37(3) . ? C111 C112 1.37(3) . ? C112 C113 1.37(3) . ? C113 C114 1.40(2) . ? C115 C116 1.47(2) . ? C116 C125 1.38(2) . ? C116 C117 1.39(2) . ? C117 C118 1.34(2) . ? C118 C119 1.45(3) . ? C119 C124 1.39(3) . ? C119 C120 1.44(3) . ? C120 C121 1.35(3) . ? C121 C122 1.33(3) . ? C122 C123 1.40(3) . ? C123 C124 1.41(3) . ? C124 C125 1.46(2) . ? C125 C126 1.43(2) . ? C126 C127 1.39(2) . ? C126 C131 1.44(2) . ? C127 C128 1.35(3) . ? C128 C129 1.44(3) . ? C129 C130 1.36(2) . ? C130 C131 1.37(2) . ? C132 C137 1.34(2) . ? C132 C133 1.43(2) . ? C133 C134 1.35(2) . ? C134 C135 1.35(2) . ? C135 C136 1.34(3) . ? C136 C137 1.42(3) . ? Sb1 F5 1.839(15) . ? Sb1 F4 1.840(15) . ? Sb1 F6 1.842(12) . ? Sb1 F3 1.845(13) . ? Sb1 F1 1.847(16) . ? Sb1 F2 1.853(15) . ? Sb2 F23 1.813(13) 2_765 ? Sb2 F23 1.813(13) . ? Sb2 F24 1.843(11) . ? Sb2 F22 1.851(11) 2_765 ? Sb2 F22 1.851(11) . ? Sb2 F21 1.851(10) . ? Sb3 F32 1.806(10) . ? Sb3 F32 1.806(10) 2_765 ? Sb3 F33 1.813(11) . ? Sb3 F33 1.813(11) 2_765 ? Sb3 F31 1.837(12) 2_765 ? Sb3 F31 1.837(12) . ? Sb4 F45 1.840(14) . ? Sb4 F44 1.846(16) . ? Sb4 F43 1.848(15) . ? Sb4 F46 1.848(16) . ? Sb4 F41 1.854(16) . ? Sb4 F42 1.855(15) . ? C201 Cl3 1.81(3) . ? C201 Cl4 1.81(3) . ? C202 Cl3' 1.81(3) . ? C202 Cl4' 1.81(3) . ? C200 Cl1 1.80(3) . ? C200 Cl2 1.81(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 96.3(5) . . ? N2 Pd1 P2 81.5(4) . . ? N1 Pd1 P2 168.2(4) . . ? N2 Pd1 P1 167.4(4) . . ? N1 Pd1 P1 81.0(4) . . ? P2 Pd1 P1 103.56(16) . . ? C32 P1 C1 110.0(9) . . ? C32 P1 C8 112.1(8) . . ? C1 P1 C8 91.7(9) . . ? C32 P1 Pd1 118.9(6) . . ? C1 P1 Pd1 91.3(5) . . ? C8 P1 Pd1 124.1(6) . . ? C108 P2 C132 111.7(8) . . ? C108 P2 C101 92.4(8) . . ? C132 P2 C101 114.7(8) . . ? C108 P2 Pd1 123.9(5) . . ? C132 P2 Pd1 116.4(6) . . ? C101 P2 Pd1 92.5(6) . . ? C15 N1 C31 120.1(13) . . ? C15 N1 Pd1 116.5(10) . . ? C31 N1 Pd1 123.1(10) . . ? C115 N2 C131 121.0(13) . . ? C115 N2 Pd1 118.4(10) . . ? C131 N2 Pd1 120.0(10) . . ? C2 C1 C15 128.0(17) . . ? C2 C1 P1 113.8(13) . . ? C15 C1 P1 115.5(13) . . ? C1 C2 C3 130.9(16) . . ? C1 C2 C3' 134(2) . . ? C3 C2 C3' 12(6) . . ? C1 C2 C7 110.1(17) . . ? C3 C2 C7 117.1(18) . . ? C3' C2 C7 116(2) . . ? C2 C3 C4 116(2) . . ? C3 C4 C5 107(3) . . ? C6 C5 C4 111(2) . . ? C5 C6 C7 116.2(17) . . ? C8 C7 C2 115.8(16) . . ? C8 C7 C6' 121(2) . . ? C2 C7 C6' 122(2) . . ? C8 C7 C6 124.9(16) . . ? C2 C7 C6 119.3(18) . . ? C6' C7 C6 14(6) . . ? C2 C3' C4' 115(3) . . ? C3' C4' C5' 107(4) . . ? C6' C5' C4' 110(3) . . ? C5' C6' C7 115(3) . . ? C7 C8 C9 125.9(15) . . ? C7 C8 P1 107.8(12) . . ? C9 C8 P1 125.6(14) . . ? C10 C9 C14 118.9(18) . . ? C10 C9 C8 122.1(18) . . ? C14 C9 C8 118.7(15) . . ? C9 C10 C11 122(2) . . ? C12 C11 C10 118(2) . . ? C11 C12 C13 122.9(17) . . ? C14 C13 C12 117.0(15) . . ? C13 C14 C9 120.9(15) . . ? N1 C15 C16 124.0(14) . . ? N1 C15 C1 111.3(13) . . ? C16 C15 C1 124.5(14) . . ? C15 C16 C17 122.6(15) . . ? C15 C16 C25 118.5(14) . . ? C17 C16 C25 118.7(14) . . ? C18 C17 C16 123.1(17) . . ? C17 C18 C19 119.2(17) . . ? C24 C19 C20 121.4(16) . . ? C24 C19 C18 119.5(15) . . ? C20 C19 C18 119.0(16) . . ? C21 C20 C19 120.0(17) . . ? C20 C21 C22 117.4(17) . . ? C23 C22 C21 121.6(17) . . ? C22 C23 C24 123.2(17) . . ? C19 C24 C23 115.7(15) . . ? C19 C24 C25 120.1(15) . . ? C23 C24 C25 123.5(15) . . ? C16 C25 C24 118.1(14) . . ? C16 C25 C26 115.4(13) . . ? C24 C25 C26 126.4(14) . . ? C31 C26 C25 121.3(14) . . ? C31 C26 C27 114.4(15) . . ? C25 C26 C27 123.3(14) . . ? C28 C27 C26 121.3(15) . . ? C27 C28 C29 120.6(16) . . ? C28 C29 C30 120.6(17) . . ? C31 C30 C29 119.1(16) . . ? C30 C31 N1 118.7(14) . . ? C30 C31 C26 123.3(15) . . ? N1 C31 C26 118.1(15) . . ? C37 C32 C33 115.4(17) . . ? C37 C32 P1 121.8(14) . . ? C33 C32 P1 122.8(13) . . ? C34 C33 C32 123.1(17) . . ? C33 C34 C35 120(2) . . ? C36 C35 C34 119(2) . . ? C35 C36 C37 122.5(19) . . ? C36 C37 C32 120.1(19) . . ? C102 C101 C115 133.3(16) . . ? C102 C101 P2 107.3(13) . . ? C115 C101 P2 113.2(13) . . ? C101 C102 C103 125.0(16) . . ? C101 C102 C107 115.0(14) . . ? C103 C102 C107 119.9(15) . . ? C102 C103 C104 114.0(16) . . ? C103 C104 C105 111.1(18) . . ? C106 C105 C104 111.1(16) . . ? C107 C106 C105 113.1(15) . . ? C108 C107 C106 124.9(15) . . ? C108 C107 C102 113.8(15) . . ? C106 C107 C102 121.3(15) . . ? C107 C108 C109 122.0(16) . . ? C107 C108 P2 110.5(12) . . ? C109 C108 P2 127.5(13) . . ? C110 C109 C114 120.1(16) . . ? C110 C109 C108 120.9(15) . . ? C114 C109 C108 119.0(16) . . ? C111 C110 C109 119.9(19) . . ? C110 C111 C112 121(2) . . ? C111 C112 C113 119.2(19) . . ? C112 C113 C114 120.9(19) . . ? C113 C114 C109 118.3(17) . . ? N2 C115 C101 115.1(14) . . ? N2 C115 C116 122.5(14) . . ? C101 C115 C116 122.4(15) . . ? C125 C116 C117 122.4(16) . . ? C125 C116 C115 116.3(14) . . ? C117 C116 C115 121.3(16) . . ? C118 C117 C116 120.9(19) . . ? C117 C118 C119 120(2) . . ? C124 C119 C120 120(2) . . ? C124 C119 C118 119.5(17) . . ? C120 C119 C118 120(2) . . ? C121 C120 C119 119(2) . . ? C122 C121 C120 122(2) . . ? C121 C122 C123 121(3) . . ? C122 C123 C124 120(2) . . ? C119 C124 C123 117.2(18) . . ? C119 C124 C125 119.4(18) . . ? C123 C124 C125 123(2) . . ? C116 C125 C126 118.7(14) . . ? C116 C125 C124 116.6(17) . . ? C126 C125 C124 124.2(17) . . ? C127 C126 C125 126.9(17) . . ? C127 C126 C131 114.8(17) . . ? C125 C126 C131 118.0(15) . . ? C128 C127 C126 123.9(19) . . ? C127 C128 C129 121.2(19) . . ? C130 C129 C128 115.1(19) . . ? C129 C130 C131 124.2(19) . . ? C130 C131 N2 119.7(15) . . ? C130 C131 C126 120.7(17) . . ? N2 C131 C126 119.4(15) . . ? C137 C132 C133 117.5(17) . . ? C137 C132 P2 122.0(14) . . ? C133 C132 P2 120.5(13) . . ? C134 C133 C132 118.4(17) . . ? C135 C134 C133 122.8(19) . . ? C136 C135 C134 121(2) . . ? C135 C136 C137 118.2(19) . . ? C132 C137 C136 122.5(18) . . ? F5 Sb1 F4 90.1(10) . . ? F5 Sb1 F6 90.0(9) . . ? F4 Sb1 F6 90.1(9) . . ? F5 Sb1 F3 90.5(10) . . ? F4 Sb1 F3 89.9(10) . . ? F6 Sb1 F3 179.5(14) . . ? F5 Sb1 F1 89.8(12) . . ? F4 Sb1 F1 179.4(9) . . ? F6 Sb1 F1 90.5(9) . . ? F3 Sb1 F1 89.5(9) . . ? F5 Sb1 F2 178.9(14) . . ? F4 Sb1 F2 90.9(11) . . ? F6 Sb1 F2 90.1(11) . . ? F3 Sb1 F2 89.4(9) . . ? F1 Sb1 F2 89.2(10) . . ? F23 Sb2 F23 178.1(10) 2_765 . ? F23 Sb2 F24 91.0(5) 2_765 . ? F23 Sb2 F24 91.0(5) . . ? F23 Sb2 F22 90.8(6) 2_765 2_765 ? F23 Sb2 F22 89.2(6) . 2_765 ? F24 Sb2 F22 89.8(3) . 2_765 ? F23 Sb2 F22 89.2(6) 2_765 . ? F23 Sb2 F22 90.8(6) . . ? F24 Sb2 F22 89.8(3) . . ? F22 Sb2 F22 179.6(7) 2_765 . ? F23 Sb2 F21 89.0(5) 2_765 . ? F23 Sb2 F21 89.0(5) . . ? F24 Sb2 F21 180.000(2) . . ? F22 Sb2 F21 90.2(3) 2_765 . ? F22 Sb2 F21 90.2(3) . . ? F32 Sb3 F32 178.6(6) . 2_765 ? F32 Sb3 F33 89.2(6) . . ? F32 Sb3 F33 89.7(6) 2_765 . ? F32 Sb3 F33 89.7(6) . 2_765 ? F32 Sb3 F33 89.2(6) 2_765 2_765 ? F33 Sb3 F33 87.7(11) . 2_765 ? F32 Sb3 F31 88.5(5) . 2_765 ? F32 Sb3 F31 92.5(5) 2_765 2_765 ? F33 Sb3 F31 91.7(8) . 2_765 ? F33 Sb3 F31 178.1(6) 2_765 2_765 ? F32 Sb3 F31 92.5(5) . . ? F32 Sb3 F31 88.5(5) 2_765 . ? F33 Sb3 F31 178.1(6) . . ? F33 Sb3 F31 91.7(8) 2_765 . ? F31 Sb3 F31 89.0(10) 2_765 . ? F45 Sb4 F44 90.6(11) . . ? F45 Sb4 F43 88.9(10) . . ? F44 Sb4 F43 90.2(10) . . ? F45 Sb4 F46 90.5(12) . . ? F44 Sb4 F46 90.1(12) . . ? F43 Sb4 F46 179.4(12) . . ? F45 Sb4 F41 90.2(10) . . ? F44 Sb4 F41 179.0(14) . . ? F43 Sb4 F41 89.3(11) . . ? F46 Sb4 F41 90.4(10) . . ? F45 Sb4 F42 177.5(14) . . ? F44 Sb4 F42 90.9(9) . . ? F43 Sb4 F42 89.1(12) . . ? F46 Sb4 F42 91.5(9) . . ? F41 Sb4 F42 88.3(11) . . ? Cl3 C201 Cl4 110(3) . . ? Cl3' C202 Cl4' 110(3) . . ? Cl1 C200 Cl2 110(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.324 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.129