# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Ramon Vilar' _publ_contact_author_address ; ICIQ - Institute of Chemical Research of Catalonia Avgda. Paisos Catalans 16 Tarragona 43007 SPAIN ; _publ_contact_author_email RVILAR@ICIQ.ES _publ_section_title ; A di-palladium urea complex as molecular receptor for anions ; loop_ _publ_author_name R.Vilar-Compte J.A.T.-C.Romero A.J.P.White data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 276098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H82 F6 N4 O9 P4 Pd2 S4' _chemical_formula_weight 1798.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.557(3) _cell_length_b 23.299(3) _cell_length_c 26.168(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.921(11) _cell_angle_gamma 90.00 _cell_volume 8768(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.71 _cell_measurement_theta_max 11.57 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale brown/orange' _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4402 _exptl_absorpt_correction_T_max 0.8145 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 17.82 _diffrn_reflns_number 13406 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.50 _reflns_number_total 12837 _reflns_number_gt 7744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12837 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 1100 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.007 _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 0.72183(4) 0.70889(2) 0.704421(19) 0.05541(16) Uani 1 1 d . . . Pd2 Pd 0.55257(4) 0.63265(2) 0.747840(19) 0.05590(16) Uani 1 1 d . . . S1 S 0.61830(13) 0.63402(8) 0.67029(6) 0.0559(4) Uani 1 1 d . . . S2 S 0.69449(16) 0.67501(9) 0.78691(7) 0.0673(5) Uani 1 1 d . . . P1 P 0.73659(19) 0.74012(11) 0.62322(8) 0.0768(7) Uani 1 1 d . . . P2 P 0.81830(18) 0.78072(9) 0.74155(8) 0.0720(6) Uani 1 1 d . . . P3 P 0.49231(19) 0.63841(10) 0.82358(7) 0.0719(6) Uani 1 1 d . . . P4 P 0.41576(17) 0.59797(9) 0.70391(7) 0.0638(5) Uani 1 1 d . . . C1 C 0.6852(7) 0.5666(3) 0.6751(3) 0.069(2) Uani 1 1 d . . . H1A H 0.7449 0.5723 0.6966 0.083 Uiso 1 1 calc R . . H1B H 0.6518 0.5371 0.6908 0.083 Uiso 1 1 calc R . . C2 C 0.6996(7) 0.5476(4) 0.6214(3) 0.074(2) Uani 1 1 d . . . H2A H 0.6404 0.5370 0.6013 0.089 Uiso 1 1 calc R . . H2B H 0.7255 0.5790 0.6039 0.089 Uiso 1 1 calc R . . N3 N 0.7620(6) 0.4993(4) 0.6256(3) 0.091(3) Uani 1 1 d . . . H3 H 0.8114 0.4994 0.6509 0.109 Uiso 1 1 calc R . . C4 C 0.7500(7) 0.4547(4) 0.5937(3) 0.077(2) Uani 1 1 d . . . O4 O 0.6804(6) 0.4492(3) 0.5610(3) 0.105(2) Uani 1 1 d U . . N5 N 0.8187(6) 0.4133(3) 0.6015(3) 0.081(2) Uani 1 1 d . . . H5 H 0.8639 0.4188 0.6287 0.097 Uiso 1 1 calc R . . C6 C 0.8262(4) 0.3646(2) 0.57245(19) 0.069(2) Uani 1 1 d G . . C7 C 0.7751(4) 0.3552(3) 0.5237(2) 0.090(3) Uani 1 1 d G . . H7A H 0.7340 0.3831 0.5085 0.108 Uiso 1 1 calc R . . C8 C 0.7854(5) 0.3041(3) 0.4978(2) 0.101(3) Uani 1 1 d G . . H8A H 0.7512 0.2978 0.4652 0.121 Uiso 1 1 calc R . . C9 C 0.8469(5) 0.2625(2) 0.5206(3) 0.102(4) Uani 1 1 d G . . H9A H 0.8538 0.2283 0.5032 0.122 Uiso 1 1 calc R . . C10 C 0.8980(5) 0.2719(2) 0.5693(3) 0.100(3) Uani 1 1 d G . . H10A H 0.9391 0.2440 0.5845 0.120 Uiso 1 1 calc R . . C11 C 0.8877(4) 0.3230(3) 0.5952(2) 0.085(3) Uani 1 1 d G . . H11A H 0.9219 0.3293 0.6278 0.102 Uiso 1 1 calc R . . C12 C 0.7729(7) 0.6149(4) 0.8041(4) 0.084(3) Uani 1 1 d . . . H12A H 0.7396 0.5836 0.8173 0.101 Uiso 1 1 calc R . . H12B H 0.7969 0.6015 0.7736 0.101 Uiso 1 1 calc R . . C13 C 0.8532(8) 0.6337(6) 0.8451(4) 0.102(4) Uani 1 1 d . . . H13A H 0.8765 0.6708 0.8361 0.123 Uiso 1 1 calc R . . H13B H 0.8324 0.6371 0.8784 0.123 Uiso 1 1 calc R . . N14 N 0.9264(7) 0.5907(4) 0.8476(4) 0.117(4) Uani 1 1 d . . . H14 H 0.9178 0.5581 0.8290 0.141 Uiso 1 1 calc R . . C15 C 1.0095(9) 0.6015(5) 0.8797(4) 0.095(3) Uani 1 1 d . . . O15 O 1.0168(7) 0.6403(4) 0.9102(3) 0.127(3) Uani 1 1 d . . . N16 N 1.0810(8) 0.5635(4) 0.8723(4) 0.111(3) Uani 1 1 d . . . H16 H 1.0696 0.5387 0.8458 0.133 Uiso 1 1 calc R . . C17 C 1.1691(5) 0.5613(3) 0.9031(3) 0.090(3) Uani 1 1 d G . . C18 C 1.2087(6) 0.6059(3) 0.9343(3) 0.120(4) Uani 1 1 d G . . H18A H 1.1759 0.6399 0.9364 0.145 Uiso 1 1 calc R . . C19 C 1.2973(6) 0.5997(5) 0.9624(3) 0.137(6) Uani 1 1 d G . . H19A H 1.3238 0.6296 0.9833 0.164 Uiso 1 1 calc R . . C20 C 1.3463(5) 0.5490(5) 0.9594(3) 0.139(5) Uani 1 1 d GU . . H20A H 1.4056 0.5449 0.9782 0.167 Uiso 1 1 calc R . . C21 C 1.3067(6) 0.5044(4) 0.9282(4) 0.145(6) Uani 1 1 d G . . H21A H 1.3395 0.4704 0.9261 0.174 Uiso 1 1 calc R . . C22 C 1.2181(7) 0.5105(3) 0.9001(3) 0.116(4) Uani 1 1 d G . . H22A H 1.1916 0.4807 0.8792 0.139 Uiso 1 1 calc R . . C23 C 0.7465(10) 0.8178(5) 0.6160(5) 0.113(4) Uani 1 1 d U . . H23A H 0.7530 0.8263 0.5805 0.135 Uiso 1 1 calc R . . H23B H 0.6894 0.8356 0.6229 0.135 Uiso 1 1 calc R . . C24 C 0.8280(12) 0.8443(5) 0.6516(5) 0.133(6) Uani 1 1 d . . . H24A H 0.8395 0.8825 0.6393 0.160 Uiso 1 1 calc R . . H24B H 0.8832 0.8214 0.6504 0.160 Uiso 1 1 calc R . . C25 C 0.8103(11) 0.8481(4) 0.7079(5) 0.119(5) Uani 1 1 d . . . H25A H 0.7487 0.8640 0.7082 0.143 Uiso 1 1 calc R . . H25B H 0.8549 0.8745 0.7266 0.143 Uiso 1 1 calc R . . C26 C 0.8365(5) 0.7104(4) 0.6005(2) 0.090(3) Uani 1 1 d G . . C27 C 0.8733(6) 0.6592(4) 0.6218(3) 0.112(4) Uani 1 1 d G . . H27A H 0.8492 0.6425 0.6492 0.134 Uiso 1 1 calc R . . C28 C 0.9462(7) 0.6328(4) 0.6023(4) 0.179(9) Uani 1 1 d G . . H28A H 0.9708 0.5985 0.6166 0.215 Uiso 1 1 calc R . . C29 C 0.9822(6) 0.6577(6) 0.5614(4) 0.161(7) Uani 1 1 d GU . . H29A H 1.0310 0.6401 0.5483 0.193 Uiso 1 1 calc R . . C30 C 0.9454(7) 0.7089(6) 0.5400(3) 0.153(6) Uani 1 1 d GU . . H30A H 0.9695 0.7256 0.5126 0.184 Uiso 1 1 calc R . . C31 C 0.8725(6) 0.7353(4) 0.5596(3) 0.134(5) Uani 1 1 d GU . . H31A H 0.8479 0.7696 0.5453 0.161 Uiso 1 1 calc R . . C32 C 0.6381(4) 0.7221(3) 0.57452(19) 0.080(3) Uani 1 1 d G . . C33 C 0.6456(5) 0.6844(3) 0.5343(2) 0.104(4) Uani 1 1 d G . . H33A H 0.7027 0.6676 0.5315 0.124 Uiso 1 1 calc R . . C34 C 0.5679(6) 0.6716(4) 0.4981(2) 0.119(5) Uani 1 1 d G . . H34A H 0.5729 0.6463 0.4712 0.142 Uiso 1 1 calc R . . C35 C 0.4827(5) 0.6966(4) 0.5022(3) 0.121(4) Uani 1 1 d GU . . H35A H 0.4306 0.6880 0.4780 0.145 Uiso 1 1 calc R . . C36 C 0.4751(5) 0.7343(4) 0.5425(3) 0.133(5) Uani 1 1 d G . . H36A H 0.4181 0.7511 0.5452 0.160 Uiso 1 1 calc R . . C37 C 0.5529(6) 0.7471(3) 0.5786(2) 0.110(4) Uani 1 1 d G . . H37A H 0.5479 0.7724 0.6056 0.132 Uiso 1 1 calc R . . C38 C 0.7945(5) 0.8011(3) 0.8046(2) 0.086(3) Uani 1 1 d G . . C39 C 0.7074(5) 0.8236(4) 0.8083(3) 0.133(6) Uani 1 1 d G . . H39A H 0.6650 0.8305 0.7786 0.160 Uiso 1 1 calc R . . C40 C 0.6837(6) 0.8359(5) 0.8566(4) 0.174(9) Uani 1 1 d G . . H40A H 0.6255 0.8510 0.8591 0.209 Uiso 1 1 calc R . . C41 C 0.7471(8) 0.8257(6) 0.9011(3) 0.185(8) Uani 1 1 d GU . . H41A H 0.7313 0.8339 0.9334 0.222 Uiso 1 1 calc R . . C42 C 0.8342(8) 0.8031(5) 0.8973(2) 0.157(6) Uani 1 1 d GU . . H42A H 0.8767 0.7963 0.9271 0.188 Uiso 1 1 calc R . . C43 C 0.8579(5) 0.7908(4) 0.8491(3) 0.115(4) Uani 1 1 d G . . H43A H 0.9162 0.7757 0.8465 0.139 Uiso 1 1 calc R . . C44 C 0.9400(4) 0.7597(3) 0.7498(3) 0.084(3) Uani 1 1 d G . . C45 C 1.0102(6) 0.8007(3) 0.7579(3) 0.111(4) Uani 1 1 d G . . H45A H 0.9953 0.8395 0.7575 0.133 Uiso 1 1 calc R . . C46 C 1.1028(5) 0.7836(4) 0.7666(4) 0.145(6) Uani 1 1 d G . . H46A H 1.1498 0.8110 0.7721 0.174 Uiso 1 1 calc R . . C47 C 1.1252(4) 0.7256(5) 0.7672(4) 0.147(6) Uani 1 1 d GU . . H47A H 1.1872 0.7141 0.7730 0.177 Uiso 1 1 calc R . . C48 C 1.0550(6) 0.6846(3) 0.7590(4) 0.138(5) Uani 1 1 d G . . H48A H 1.0700 0.6458 0.7594 0.166 Uiso 1 1 calc R . . C49 C 0.9624(5) 0.7017(3) 0.7503(3) 0.100(3) Uani 1 1 d G . . H49A H 0.9154 0.6743 0.7449 0.120 Uiso 1 1 calc R . . C50 C 0.4057(9) 0.5843(5) 0.8331(4) 0.100(4) Uani 1 1 d . . . H50A H 0.4358 0.5471 0.8366 0.120 Uiso 1 1 calc R . . H50B H 0.3832 0.5924 0.8654 0.120 Uiso 1 1 calc R . . C51 C 0.3230(9) 0.5808(6) 0.7903(4) 0.103(4) Uani 1 1 d . . . H51A H 0.2990 0.6192 0.7825 0.124 Uiso 1 1 calc R . . H51B H 0.2743 0.5584 0.8023 0.124 Uiso 1 1 calc R . . C52 C 0.3474(8) 0.5534(5) 0.7406(4) 0.090(3) Uani 1 1 d . . . H52A H 0.2900 0.5432 0.7184 0.108 Uiso 1 1 calc R . . H52B H 0.3815 0.5182 0.7499 0.108 Uiso 1 1 calc R . . C53 C 0.5787(5) 0.6301(3) 0.8815(2) 0.086(3) Uani 1 1 d G . . C54 C 0.6150(7) 0.5761(3) 0.8951(3) 0.129(5) Uani 1 1 d GU . . H54A H 0.5941 0.5443 0.8752 0.155 Uiso 1 1 calc R . . C55 C 0.6824(7) 0.5697(3) 0.9385(3) 0.150(7) Uani 1 1 d G . . H55A H 0.7067 0.5335 0.9477 0.180 Uiso 1 1 calc R . . C56 C 0.7136(6) 0.6172(5) 0.9683(3) 0.145(6) Uani 1 1 d GU . . H56A H 0.7587 0.6129 0.9974 0.174 Uiso 1 1 calc R . . C57 C 0.6773(7) 0.6712(4) 0.9547(3) 0.152(6) Uani 1 1 d GU . . H57A H 0.6982 0.7031 0.9746 0.182 Uiso 1 1 calc R . . C58 C 0.6099(7) 0.6777(3) 0.9113(3) 0.124(5) Uani 1 1 d GU . . H58A H 0.5856 0.7138 0.9021 0.149 Uiso 1 1 calc R . . C59 C 0.4375(5) 0.7070(2) 0.8308(2) 0.074(2) Uani 1 1 d G . . C60 C 0.3740(5) 0.7135(3) 0.8649(2) 0.105(4) Uani 1 1 d G . . H60A H 0.3583 0.6822 0.8838 0.126 Uiso 1 1 calc R . . C61 C 0.3339(5) 0.7668(4) 0.8706(3) 0.118(4) Uani 1 1 d G . . H61A H 0.2913 0.7711 0.8934 0.141 Uiso 1 1 calc R . . C62 C 0.3574(6) 0.8135(3) 0.8423(4) 0.126(5) Uani 1 1 d G . . H62A H 0.3305 0.8492 0.8462 0.151 Uiso 1 1 calc R . . C63 C 0.4209(6) 0.8070(2) 0.8082(3) 0.123(5) Uani 1 1 d G . . H63A H 0.4366 0.8383 0.7892 0.148 Uiso 1 1 calc R . . C64 C 0.4610(5) 0.7537(3) 0.8024(3) 0.101(3) Uani 1 1 d G . . H64A H 0.5036 0.7494 0.7796 0.121 Uiso 1 1 calc R . . C65 C 0.3403(5) 0.6573(2) 0.6787(2) 0.073(2) Uani 1 1 d G . . C66 C 0.3798(4) 0.7111(3) 0.6747(3) 0.098(3) Uani 1 1 d G . . H66A H 0.4435 0.7161 0.6842 0.118 Uiso 1 1 calc R . . C67 C 0.3240(7) 0.7574(2) 0.6564(4) 0.143(6) Uani 1 1 d G . . H67A H 0.3505 0.7934 0.6537 0.171 Uiso 1 1 calc R . . C68 C 0.2288(7) 0.7500(4) 0.6422(4) 0.138(6) Uani 1 1 d G . . H68A H 0.1915 0.7810 0.6300 0.165 Uiso 1 1 calc R . . C69 C 0.1892(4) 0.6962(5) 0.6463(3) 0.133(5) Uani 1 1 d G . . H69A H 0.1255 0.6912 0.6368 0.160 Uiso 1 1 calc R . . C70 C 0.2450(5) 0.6499(4) 0.6645(3) 0.113(4) Uani 1 1 d G . . H70A H 0.2185 0.6139 0.6672 0.135 Uiso 1 1 calc R . . C71 C 0.4305(4) 0.5531(2) 0.64914(16) 0.066(2) Uani 1 1 d G . . C72 C 0.4129(5) 0.5754(2) 0.59929(19) 0.081(3) Uani 1 1 d G . . H72A H 0.3922 0.6130 0.5940 0.098 Uiso 1 1 calc R . . C73 C 0.4263(5) 0.5414(3) 0.55739(15) 0.104(4) Uani 1 1 d G . . H73A H 0.4145 0.5563 0.5240 0.124 Uiso 1 1 calc R . . C74 C 0.4573(5) 0.4852(3) 0.5653(2) 0.105(4) Uani 1 1 d G . . H74A H 0.4662 0.4625 0.5373 0.125 Uiso 1 1 calc R . . C75 C 0.4749(6) 0.4630(2) 0.6152(3) 0.110(4) Uani 1 1 d G . . H75A H 0.4956 0.4254 0.6205 0.133 Uiso 1 1 calc R . . C76 C 0.4615(5) 0.4969(2) 0.65707(19) 0.094(3) Uani 1 1 d G . . H76A H 0.4733 0.4820 0.6904 0.112 Uiso 1 1 calc R . . S80A S 0.9756(10) 0.4855(7) 0.7329(6) 0.063(4) Uani 0.256(3) 1 d PDU A 1 O81A O 0.9345(18) 0.4317(10) 0.7124(9) 0.067(6) Uiso 0.256(3) 1 d PDU A 1 O82A O 0.918(2) 0.5356(12) 0.7219(14) 0.127(19) Uiso 0.256(3) 1 d PDU A 1 O83A O 1.0354(18) 0.4832(12) 0.7820(7) 0.085(8) Uiso 0.256(3) 1 d PDU A 1 C80A C 1.0609(17) 0.4976(9) 0.6906(9) 0.132(17) Uiso 0.256(3) 1 d PDU A 1 F81A F 1.1035(18) 0.5458(10) 0.7019(11) 0.133(10) Uiso 0.256(3) 1 d PDU A 1 F82A F 1.1217(17) 0.4569(11) 0.6958(12) 0.137(11) Uiso 0.256(3) 1 d PDU A 1 F83A F 1.022(2) 0.4992(14) 0.6431(7) 0.145(11) Uiso 0.256(3) 1 d PDU A 1 S80B S 0.9452(10) 0.4720(6) 0.7457(4) 0.102(5) Uani 0.375(3) 1 d PDU B 2 O81B O 0.9655(18) 0.4400(11) 0.7010(8) 0.110(8) Uiso 0.375(3) 1 d PDU B 2 O82B O 0.9154(18) 0.5299(8) 0.7330(11) 0.103(8) Uiso 0.375(3) 1 d PDU B 2 O83B O 1.0151(18) 0.4627(13) 0.7901(8) 0.112(8) Uiso 0.375(3) 1 d PDU B 2 C80B C 0.8450(17) 0.4429(11) 0.7702(10) 0.22(2) Uiso 0.375(3) 1 d PDU B 2 F81B F 0.817(2) 0.4733(13) 0.8077(11) 0.204(12) Uiso 0.375(3) 1 d PDU B 2 F82B F 0.868(2) 0.3925(12) 0.7909(12) 0.206(13) Uiso 0.375(3) 1 d PDU B 2 F83B F 0.7678(17) 0.4370(13) 0.7374(10) 0.187(11) Uiso 0.375(3) 1 d PDU B 2 S80C S 0.9680(16) 0.4984(10) 0.7307(10) 0.109(9) Uani 0.244(3) 1 d PDU C 3 O81C O 0.928(3) 0.4499(14) 0.7008(14) 0.109(12) Uiso 0.244(3) 1 d PDU C 3 O82C O 0.926(3) 0.5522(13) 0.7137(17) 0.139(15) Uiso 0.244(3) 1 d PDU C 3 O83C O 0.988(3) 0.4879(16) 0.7860(10) 0.109(11) Uiso 0.244(3) 1 d PDU C 3 C80C C 1.0846(19) 0.5083(12) 0.7172(11) 0.102(13) Uiso 0.244(3) 1 d PDU C 3 F81C F 1.087(3) 0.523(2) 0.6696(12) 0.198(17) Uiso 0.244(3) 1 d PDU C 3 F82C F 1.121(2) 0.5478(15) 0.7485(14) 0.160(13) Uiso 0.244(3) 1 d PDU C 3 F83C F 1.136(2) 0.4630(15) 0.7245(17) 0.179(16) Uiso 0.244(3) 1 d PDU C 3 S80D S 0.902(2) 0.4679(14) 0.7620(12) 0.132(11) Uiso 0.125(3) 1 d PDU D 4 O81D O 0.895(4) 0.434(2) 0.7153(14) 0.080(14) Uiso 0.125(3) 1 d PDU D 4 O82D O 0.883(4) 0.5279(15) 0.752(2) 0.14(2) Uiso 0.125(3) 1 d PDU D 4 O83D O 0.983(3) 0.457(2) 0.7999(16) 0.086(15) Uiso 0.125(3) 1 d PDU D 4 C80D C 0.810(3) 0.446(2) 0.7969(18) 0.28(5) Uiso 0.125(3) 1 d PDU D 4 F81D F 0.732(3) 0.474(3) 0.785(3) 0.21(3) Uiso 0.125(3) 1 d PDU D 4 F82D F 0.837(5) 0.452(4) 0.8466(17) 0.21(3) Uiso 0.125(3) 1 d PDU D 4 F83D F 0.786(5) 0.392(2) 0.790(3) 0.16(2) Uiso 0.125(3) 1 d PDU D 4 S90A S 0.4660(12) 0.3971(7) 0.8244(6) 0.128(7) Uani 0.415(4) 1 d PDU E 1 O91A O 0.4451(17) 0.3370(7) 0.8151(9) 0.109(7) Uiso 0.415(4) 1 d PDU E 1 O92A O 0.3819(14) 0.4311(10) 0.8215(9) 0.119(7) Uiso 0.415(4) 1 d PDU E 1 O93A O 0.532(2) 0.4222(16) 0.7952(12) 0.203(17) Uiso 0.415(4) 1 d PDU E 1 C90A C 0.5210(13) 0.4072(8) 0.8901(8) 0.090(7) Uiso 0.415(4) 1 d PDU E 1 F91A F 0.5243(17) 0.4601(8) 0.9068(8) 0.141(7) Uiso 0.415(4) 1 d PDU E 1 F92A F 0.6045(15) 0.3853(11) 0.8965(10) 0.166(9) Uiso 0.415(4) 1 d PDU E 1 F93A F 0.4737(15) 0.3817(9) 0.9228(7) 0.142(7) Uiso 0.415(4) 1 d PDU E 1 S90B S 0.4790(14) 0.4028(10) 0.8054(8) 0.143(8) Uani 0.373(9) 1 d PDU F 2 O91B O 0.483(2) 0.3430(11) 0.8202(14) 0.138(12) Uiso 0.373(9) 1 d PDU F 2 O92B O 0.435(3) 0.4412(17) 0.8374(15) 0.23(2) Uiso 0.373(9) 1 d PDU F 2 O93B O 0.448(2) 0.4108(16) 0.7505(9) 0.190(14) Uiso 0.373(9) 1 d PDU F 2 C90B C 0.596(2) 0.4313(12) 0.8118(12) 0.23(3) Uiso 0.373(9) 1 d PDU F 2 F91B F 0.602(2) 0.4830(12) 0.7930(14) 0.215(14) Uiso 0.373(9) 1 d PDU F 2 F92B F 0.647(2) 0.3976(14) 0.7886(14) 0.225(15) Uiso 0.373(9) 1 d PDU F 2 F93B F 0.634(3) 0.436(2) 0.8603(12) 0.258(19) Uiso 0.373(9) 1 d PDU F 2 S90C S 0.4731(19) 0.4007(9) 0.8198(10) 0.102(10) Uani 0.212(9) 1 d PDU G 3 O91C O 0.483(4) 0.3452(13) 0.7966(19) 0.16(2) Uiso 0.212(9) 1 d PDU G 3 O92C O 0.387(2) 0.408(2) 0.8406(18) 0.151(18) Uiso 0.212(9) 1 d PDU G 3 O93C O 0.500(3) 0.4503(14) 0.7920(13) 0.113(12) Uiso 0.212(9) 1 d PDU G 3 C90C C 0.563(2) 0.4052(12) 0.8758(12) 0.118(18) Uiso 0.212(9) 1 d PDU G 3 F91C F 0.571(3) 0.4553(12) 0.8978(12) 0.115(11) Uiso 0.212(9) 1 d PDU G 3 F92C F 0.642(2) 0.397(3) 0.8594(18) 0.22(2) Uiso 0.212(9) 1 d PDU G 3 F93C F 0.557(3) 0.3670(15) 0.9116(13) 0.139(13) Uiso 0.212(9) 1 d PDU G 3 O100 O 1.017(4) 0.380(2) 0.945(3) 0.30(3) Uiso 0.358(3) 1 d PD H 1 C101 C 1.011(3) 0.431(2) 0.970(2) 0.18(2) Uiso 0.358(3) 1 d PD H 1 H10B H 1.0581 0.4579 0.9623 0.210 Uiso 0.358(3) 1 calc PR H 1 H10C H 1.0194 0.4256 1.0074 0.210 Uiso 0.358(3) 1 calc PR H 1 C102 C 0.919(3) 0.4531(19) 0.951(2) 0.16(2) Uiso 0.358(3) 1 d PD H 1 H10D H 0.8806 0.4518 0.9788 0.188 Uiso 0.358(3) 1 calc PR H 1 H10E H 0.9221 0.4925 0.9402 0.188 Uiso 0.358(3) 1 calc PR H 1 C103 C 0.878(3) 0.418(3) 0.909(2) 0.20(3) Uiso 0.358(3) 1 d PD H 1 H10F H 0.8200 0.4013 0.9156 0.243 Uiso 0.358(3) 1 calc PR H 1 H10G H 0.8667 0.4399 0.8773 0.243 Uiso 0.358(3) 1 calc PR H 1 C104 C 0.945(4) 0.3734(19) 0.9050(17) 0.149(16) Uiso 0.358(3) 1 d PD H 1 H10H H 0.9166 0.3360 0.9069 0.179 Uiso 0.358(3) 1 calc PR H 1 H10I H 0.9678 0.3763 0.8721 0.179 Uiso 0.358(3) 1 calc PR H 1 O105 O 1.049(3) 0.386(2) 0.945(2) 0.087(14) Uiso 0.142(3) 1 d PD I 2 C106 C 1.028(4) 0.439(2) 0.923(4) 0.13(3) Uiso 0.142(3) 1 d PD I 2 H10J H 1.0358 0.4397 0.8871 0.152 Uiso 0.142(3) 1 calc PR I 2 H10K H 1.0677 0.4683 0.9415 0.152 Uiso 0.142(3) 1 calc PR I 2 C107 C 0.931(4) 0.450(2) 0.928(4) 0.11(3) Uiso 0.142(3) 1 d PD I 2 H10L H 0.9272 0.4772 0.9560 0.134 Uiso 0.142(3) 1 calc PR I 2 H10M H 0.8982 0.4666 0.8961 0.134 Uiso 0.142(3) 1 calc PR I 2 C108 C 0.892(3) 0.395(3) 0.939(3) 0.090(19) Uiso 0.142(3) 1 d PD I 2 H10N H 0.8473 0.3829 0.9093 0.108 Uiso 0.142(3) 1 calc PR I 2 H10O H 0.8601 0.3982 0.9686 0.108 Uiso 0.142(3) 1 calc PR I 2 C109 C 0.968(4) 0.355(2) 0.949(4) 0.13(3) Uiso 0.142(3) 1 d PD I 2 H10P H 0.9719 0.3386 0.9829 0.157 Uiso 0.142(3) 1 calc PR I 2 H10Q H 0.9601 0.3240 0.9235 0.157 Uiso 0.142(3) 1 calc PR I 2 O110 O 1.164(3) 0.5157(19) 0.5578(17) 0.185(17) Uiso 0.323(3) 1 d PD J 3 C111 C 1.125(6) 0.468(3) 0.5307(17) 0.21(3) Uiso 0.323(3) 1 d PD J 3 H11B H 1.1723 0.4461 0.5173 0.249 Uiso 0.323(3) 1 calc PR J 3 H11C H 1.0781 0.4798 0.5021 0.249 Uiso 0.323(3) 1 calc PR J 3 C112 C 1.083(5) 0.435(2) 0.568(3) 0.21(3) Uiso 0.323(3) 1 d PD J 3 H11D H 1.0158 0.4363 0.5598 0.255 Uiso 0.323(3) 1 calc PR J 3 H11E H 1.1022 0.3948 0.5670 0.255 Uiso 0.323(3) 1 calc PR J 3 C113 C 1.114(6) 0.458(3) 0.619(2) 0.25(4) Uiso 0.323(3) 1 d PD J 3 H11F H 1.1574 0.4329 0.6396 0.298 Uiso 0.323(3) 1 calc PR J 3 H11G H 1.0612 0.4647 0.6373 0.298 Uiso 0.323(3) 1 calc PR J 3 C114 C 1.158(4) 0.513(2) 0.6099(16) 0.16(2) Uiso 0.323(3) 1 d PD J 3 H11H H 1.1219 0.5448 0.6198 0.188 Uiso 0.323(3) 1 calc PR J 3 H11I H 1.2199 0.5148 0.6300 0.188 Uiso 0.323(3) 1 calc PR J 3 O115 O 1.190(6) 0.451(4) 0.561(3) 0.23(4) Uiso 0.177(3) 1 d PD K 4 C116 C 1.179(4) 0.465(3) 0.509(2) 0.103(19) Uiso 0.177(3) 1 d PD K 4 H11J H 1.1806 0.4305 0.4878 0.123 Uiso 0.177(3) 1 calc PR K 4 H11K H 1.2284 0.4904 0.5017 0.123 Uiso 0.177(3) 1 calc PR K 4 C117 C 1.089(5) 0.493(5) 0.497(3) 0.16(4) Uiso 0.177(3) 1 d PD K 4 H11L H 1.0944 0.5290 0.4790 0.197 Uiso 0.177(3) 1 calc PR K 4 H11M H 1.0448 0.4688 0.4754 0.197 Uiso 0.177(3) 1 calc PR K 4 C118 C 1.058(6) 0.504(5) 0.546(4) 0.16(4) Uiso 0.177(3) 1 d PD K 4 H11N H 0.9945 0.4898 0.5451 0.195 Uiso 0.177(3) 1 calc PR K 4 H11O H 1.0587 0.5444 0.5536 0.195 Uiso 0.177(3) 1 calc PR K 4 C119 C 1.121(11) 0.473(10) 0.586(3) 0.35(13) Uiso 0.177(3) 1 d PD K 4 H11P H 1.1465 0.4991 0.6132 0.418 Uiso 0.177(3) 1 calc PR K 4 H11Q H 1.0881 0.4425 0.6006 0.418 Uiso 0.177(3) 1 calc PR K 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0692(3) 0.0534(3) 0.0408(2) -0.0029(2) -0.0006(2) -0.0034(3) Pd2 0.0740(4) 0.0550(3) 0.0389(2) -0.0021(2) 0.0092(2) 0.0003(3) S1 0.0683(11) 0.0581(9) 0.0409(7) -0.0045(7) 0.0072(7) -0.0035(9) S2 0.0840(14) 0.0730(12) 0.0424(8) -0.0048(8) 0.0022(8) 0.0004(11) P1 0.0944(17) 0.0827(15) 0.0494(10) 0.0102(9) -0.0013(10) -0.0314(13) P2 0.0839(15) 0.0617(12) 0.0645(11) -0.0142(9) -0.0069(10) -0.0087(11) P3 0.0993(17) 0.0741(13) 0.0452(9) -0.0022(9) 0.0208(10) 0.0002(12) P4 0.0803(14) 0.0621(11) 0.0502(9) -0.0063(8) 0.0145(9) -0.0117(10) C1 0.089(6) 0.059(4) 0.057(4) 0.000(3) 0.006(4) 0.005(4) C2 0.092(6) 0.069(5) 0.061(4) -0.016(4) 0.010(4) 0.008(5) N3 0.090(6) 0.094(6) 0.079(5) -0.034(4) -0.015(4) 0.023(5) C4 0.094(7) 0.081(6) 0.051(4) -0.016(4) -0.005(4) 0.012(5) O4 0.102(5) 0.106(5) 0.095(4) -0.043(4) -0.020(4) 0.035(4) N5 0.087(5) 0.072(4) 0.077(4) -0.028(4) -0.011(4) 0.019(4) C6 0.065(5) 0.069(5) 0.073(5) -0.014(4) 0.013(4) -0.001(4) C7 0.114(8) 0.093(7) 0.060(5) -0.021(4) 0.004(5) 0.021(6) C8 0.102(8) 0.106(8) 0.096(7) -0.035(6) 0.021(6) 0.001(7) C9 0.100(8) 0.083(7) 0.131(9) -0.041(6) 0.045(7) -0.014(6) C10 0.094(8) 0.066(6) 0.143(10) -0.007(6) 0.029(7) 0.011(5) C11 0.088(7) 0.075(6) 0.093(6) -0.007(5) 0.017(5) 0.016(5) C12 0.091(7) 0.083(6) 0.070(5) 0.011(4) -0.012(5) 0.018(5) C13 0.099(8) 0.118(8) 0.078(6) -0.011(6) -0.022(5) 0.028(7) N14 0.104(7) 0.100(6) 0.128(8) -0.024(6) -0.045(6) 0.019(6) C15 0.115(9) 0.090(7) 0.073(5) -0.007(5) -0.010(5) 0.000(6) O15 0.145(8) 0.101(6) 0.116(6) -0.036(5) -0.042(6) 0.014(5) N16 0.124(8) 0.086(6) 0.109(7) -0.017(5) -0.022(6) 0.020(6) C17 0.093(7) 0.094(7) 0.079(6) 0.014(5) 0.004(5) 0.005(6) C18 0.109(9) 0.134(11) 0.109(9) -0.027(8) -0.011(7) 0.007(8) C19 0.108(10) 0.205(18) 0.094(8) -0.015(10) 0.004(7) -0.004(11) C20 0.125(10) 0.190(14) 0.102(8) 0.046(9) 0.020(8) 0.021(11) C21 0.130(13) 0.139(13) 0.161(15) 0.054(11) 0.007(11) 0.004(10) C22 0.119(10) 0.103(8) 0.123(9) 0.030(7) 0.007(8) 0.014(8) C23 0.150(10) 0.085(6) 0.096(7) 0.031(5) -0.006(7) -0.035(7) C24 0.199(16) 0.087(7) 0.107(9) 0.023(6) 0.002(9) -0.065(9) C25 0.151(12) 0.062(6) 0.127(9) 0.001(6) -0.032(8) -0.034(7) C26 0.086(6) 0.128(9) 0.054(4) -0.006(5) 0.005(4) -0.046(7) C27 0.108(9) 0.134(11) 0.098(8) -0.032(8) 0.034(7) -0.032(8) C28 0.134(14) 0.22(2) 0.196(19) -0.063(17) 0.078(14) -0.006(15) C29 0.116(10) 0.207(15) 0.172(13) -0.062(12) 0.061(10) -0.027(11) C30 0.130(11) 0.230(15) 0.107(9) -0.021(10) 0.042(8) -0.054(11) C31 0.106(9) 0.210(14) 0.092(7) 0.025(8) 0.031(7) -0.031(9) C32 0.094(7) 0.097(7) 0.045(4) 0.020(4) -0.001(4) -0.025(5) C33 0.115(9) 0.133(9) 0.061(5) -0.003(5) 0.008(5) -0.040(8) C34 0.122(10) 0.170(13) 0.061(5) -0.017(7) 0.010(6) -0.049(10) C35 0.111(9) 0.164(11) 0.081(6) 0.013(7) -0.010(6) -0.032(8) C36 0.114(10) 0.162(14) 0.109(9) 0.005(9) -0.027(8) 0.027(10) C37 0.122(10) 0.102(8) 0.094(7) 0.005(6) -0.020(7) -0.019(8) C38 0.083(6) 0.086(6) 0.085(6) -0.035(5) -0.002(5) 0.001(5) C39 0.099(9) 0.137(11) 0.163(13) -0.070(10) 0.019(9) 0.013(8) C40 0.140(14) 0.198(18) 0.189(17) -0.119(15) 0.038(13) 0.022(13) C41 0.186(15) 0.237(16) 0.138(11) -0.091(12) 0.043(11) -0.003(13) C42 0.164(12) 0.215(15) 0.087(7) -0.045(9) 0.006(8) 0.009(12) C43 0.108(8) 0.159(11) 0.074(6) -0.050(7) -0.002(6) 0.016(9) C44 0.082(6) 0.100(7) 0.068(5) -0.025(5) 0.011(4) -0.014(6) C45 0.092(8) 0.114(9) 0.127(9) -0.042(8) 0.019(7) -0.027(7) C46 0.081(9) 0.193(18) 0.162(14) -0.052(13) 0.018(8) -0.038(10) C47 0.115(10) 0.192(14) 0.134(10) -0.053(10) 0.017(8) 0.009(10) C48 0.100(10) 0.155(14) 0.153(13) -0.027(11) 0.000(9) 0.021(10) C49 0.090(7) 0.102(8) 0.104(7) -0.019(6) 0.005(6) 0.012(6) C50 0.140(10) 0.108(8) 0.060(5) -0.002(5) 0.038(6) -0.023(7) C51 0.112(9) 0.120(9) 0.089(7) -0.012(6) 0.050(6) -0.033(7) C52 0.107(8) 0.097(7) 0.072(5) -0.018(5) 0.033(5) -0.028(6) C53 0.119(8) 0.099(7) 0.045(4) 0.000(4) 0.023(4) 0.012(6) C54 0.193(13) 0.107(8) 0.082(6) 0.008(6) 0.004(8) 0.034(9) C55 0.215(19) 0.114(10) 0.104(9) 0.038(8) -0.028(11) 0.020(11) C56 0.182(13) 0.172(12) 0.067(6) -0.003(7) -0.021(7) 0.038(11) C57 0.184(13) 0.153(12) 0.100(8) -0.032(8) -0.033(9) 0.020(11) C58 0.157(11) 0.110(8) 0.093(7) -0.026(6) -0.021(7) 0.023(8) C59 0.084(6) 0.084(5) 0.058(4) -0.011(4) 0.018(4) 0.007(5) C60 0.102(8) 0.136(10) 0.082(6) -0.021(7) 0.024(6) 0.020(8) C61 0.099(9) 0.150(12) 0.109(9) -0.044(8) 0.034(7) 0.023(9) C62 0.088(8) 0.133(11) 0.153(12) -0.062(10) 0.007(8) 0.027(8) C63 0.134(11) 0.075(7) 0.160(12) -0.015(7) 0.023(10) 0.026(7) C64 0.121(9) 0.089(7) 0.101(7) -0.016(6) 0.045(7) 0.011(6) C65 0.077(6) 0.081(5) 0.060(4) -0.007(4) 0.010(4) -0.004(5) C66 0.100(7) 0.079(6) 0.108(7) 0.002(6) -0.012(6) 0.003(6) C67 0.171(16) 0.087(8) 0.158(13) 0.011(8) -0.014(11) 0.045(9) C68 0.123(12) 0.155(14) 0.126(11) -0.002(10) -0.009(9) 0.063(11) C69 0.094(9) 0.186(17) 0.116(10) 0.003(11) 0.005(7) 0.022(11) C70 0.096(8) 0.152(12) 0.090(7) 0.012(7) 0.011(6) -0.029(8) C71 0.082(6) 0.057(4) 0.062(4) -0.013(3) 0.020(4) -0.025(4) C72 0.097(7) 0.092(6) 0.053(4) -0.015(4) 0.005(4) 0.005(5) C73 0.112(9) 0.136(10) 0.061(5) -0.035(6) 0.008(5) -0.002(7) C74 0.109(8) 0.116(9) 0.092(7) -0.057(7) 0.028(6) -0.026(7) C75 0.159(12) 0.063(6) 0.122(9) -0.028(6) 0.062(8) -0.035(7) C76 0.127(9) 0.068(6) 0.093(6) -0.009(5) 0.040(6) -0.012(6) S80A 0.062(7) 0.049(8) 0.072(9) -0.007(6) -0.008(6) -0.008(5) S80B 0.130(12) 0.095(9) 0.072(6) -0.014(6) -0.014(7) 0.040(8) S80C 0.132(15) 0.065(11) 0.114(13) -0.002(8) -0.029(10) 0.029(9) S90A 0.135(12) 0.124(13) 0.118(11) -0.002(9) -0.006(10) -0.036(10) S90B 0.154(13) 0.143(13) 0.136(14) 0.038(10) 0.031(10) 0.007(10) S90C 0.14(2) 0.060(12) 0.106(19) 0.015(11) 0.009(15) 0.024(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 P1 2.287(2) . ? Pd1 P2 2.301(2) . ? Pd1 S1 2.3863(19) . ? Pd1 S2 2.389(2) . ? Pd2 P4 2.287(2) . ? Pd2 P3 2.292(2) . ? Pd2 S2 2.373(2) . ? Pd2 S1 2.3743(18) . ? S1 C1 1.842(8) . ? S2 C12 1.819(9) . ? P1 C26 1.794(7) . ? P1 C32 1.813(5) . ? P1 C23 1.827(11) . ? P2 C25 1.794(11) . ? P2 C38 1.800(6) . ? P2 C44 1.819(6) . ? P3 C59 1.808(5) . ? P3 C53 1.823(5) . ? P3 C50 1.827(11) . ? P4 C52 1.813(10) . ? P4 C71 1.813(4) . ? P4 C65 1.824(6) . ? C1 C2 1.517(11) . ? C2 N3 1.440(12) . ? N3 C4 1.326(11) . ? C4 O4 1.227(11) . ? C4 N5 1.382(12) . ? N5 C6 1.380(8) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C12 C13 1.523(13) . ? C13 N14 1.457(14) . ? N14 C15 1.385(14) . ? C15 O15 1.199(13) . ? C15 N16 1.402(15) . ? N16 C17 1.405(11) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.521(17) . ? C24 C25 1.537(19) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C50 C51 1.514(17) . ? C51 C52 1.539(13) . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? S80A O83A 1.435(13) . ? S80A O82A 1.444(14) . ? S80A O81A 1.456(13) . ? S80A C80A 1.81(2) . ? C80A F83A 1.286(16) . ? C80A F82A 1.290(16) . ? C80A F81A 1.294(16) . ? S80B O83B 1.437(13) . ? S80B O82B 1.440(13) . ? S80B O81B 1.456(13) . ? S80B C80B 1.81(2) . ? C80B F83B 1.311(16) . ? C80B F82B 1.315(16) . ? C80B F81B 1.324(16) . ? S80C O82C 1.436(14) . ? S80C O81C 1.444(14) . ? S80C O83C 1.452(14) . ? S80C C80C 1.80(2) . ? C80C F82C 1.290(16) . ? C80C F83C 1.292(16) . ? C80C F81C 1.298(16) . ? S80D O82D 1.444(15) . ? S80D O83D 1.445(15) . ? S80D O81D 1.447(14) . ? S80D C80D 1.81(2) . ? C80D F81D 1.306(17) . ? C80D F82D 1.306(17) . ? C80D F83D 1.309(17) . ? S90A O93A 1.445(14) . ? S90A O91A 1.446(13) . ? S90A O92A 1.451(14) . ? S90A C90A 1.80(2) . ? C90A F91A 1.304(15) . ? C90A F92A 1.305(15) . ? C90A F93A 1.320(15) . ? S90B O92B 1.439(14) . ? S90B O91B 1.446(14) . ? S90B O93B 1.449(14) . ? S90B C90B 1.80(2) . ? C90B F92B 1.303(16) . ? C90B F93B 1.309(17) . ? C90B F91B 1.309(16) . ? S90C O91C 1.445(14) . ? S90C O92C 1.445(15) . ? S90C O93C 1.451(15) . ? S90C C90C 1.80(2) . ? C90C F91C 1.300(16) . ? C90C F93C 1.304(16) . ? C90C F92C 1.311(17) . ? O100 C101 1.373(19) . ? O100 C104 1.376(19) . ? C101 C102 1.452(19) . ? C102 C103 1.435(19) . ? C103 C104 1.432(19) . ? O105 C106 1.38(2) . ? O105 C109 1.40(2) . ? C106 C107 1.45(2) . ? C107 C108 1.451(19) . ? C108 C109 1.453(19) . ? O110 C114 1.380(19) . ? O110 C111 1.386(19) . ? C111 C112 1.455(19) . ? C112 C113 1.455(19) . ? C113 C114 1.462(19) . ? O115 C119 1.387(19) . ? O115 C116 1.389(19) . ? C116 C117 1.463(19) . ? C117 C118 1.447(19) . ? C118 C119 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 91.25(9) . . ? P1 Pd1 S1 91.70(7) . . ? P2 Pd1 S1 176.82(8) . . ? P1 Pd1 S2 175.75(9) . . ? P2 Pd1 S2 92.01(8) . . ? S1 Pd1 S2 84.99(7) . . ? P4 Pd2 P3 92.01(9) . . ? P4 Pd2 S2 174.53(8) . . ? P3 Pd2 S2 91.57(8) . . ? P4 Pd2 S1 90.58(7) . . ? P3 Pd2 S1 175.69(8) . . ? S2 Pd2 S1 85.60(7) . . ? C1 S1 Pd2 102.1(3) . . ? C1 S1 Pd1 107.6(3) . . ? Pd2 S1 Pd1 90.27(6) . . ? C12 S2 Pd2 104.9(3) . . ? C12 S2 Pd1 106.9(4) . . ? Pd2 S2 Pd1 90.23(6) . . ? C26 P1 C32 105.7(3) . . ? C26 P1 C23 105.5(6) . . ? C32 P1 C23 102.9(5) . . ? C26 P1 Pd1 112.5(3) . . ? C32 P1 Pd1 113.7(2) . . ? C23 P1 Pd1 115.5(4) . . ? C25 P2 C38 102.2(5) . . ? C25 P2 C44 106.3(6) . . ? C38 P2 C44 106.6(3) . . ? C25 P2 Pd1 116.1(4) . . ? C38 P2 Pd1 112.8(3) . . ? C44 P2 Pd1 112.0(2) . . ? C59 P3 C53 105.4(3) . . ? C59 P3 C50 105.7(5) . . ? C53 P3 C50 102.5(5) . . ? C59 P3 Pd2 112.1(2) . . ? C53 P3 Pd2 113.9(3) . . ? C50 P3 Pd2 116.2(3) . . ? C52 P4 C71 103.3(4) . . ? C52 P4 C65 106.0(5) . . ? C71 P4 C65 106.8(3) . . ? C52 P4 Pd2 116.3(4) . . ? C71 P4 Pd2 113.6(2) . . ? C65 P4 Pd2 110.1(2) . . ? C2 C1 S1 109.5(6) . . ? N3 C2 C1 109.5(7) . . ? C4 N3 C2 123.0(8) . . ? O4 C4 N3 122.3(9) . . ? O4 C4 N5 122.0(8) . . ? N3 C4 N5 115.6(8) . . ? C6 N5 C4 127.6(7) . . ? N5 C6 C7 124.0(5) . . ? N5 C6 C11 116.0(5) . . ? C7 C6 C11 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C6 120.0 . . ? C13 C12 S2 109.6(7) . . ? N14 C13 C12 108.0(9) . . ? C15 N14 C13 117.8(10) . . ? O15 C15 N14 121.4(12) . . ? O15 C15 N16 125.1(11) . . ? N14 C15 N16 113.5(9) . . ? C15 N16 C17 125.1(9) . . ? C18 C17 C22 120.0 . . ? C18 C17 N16 124.6(7) . . ? C22 C17 N16 115.4(7) . . ? C17 C18 C19 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C17 120.0 . . ? C24 C23 P1 113.9(9) . . ? C23 C24 C25 112.3(12) . . ? C24 C25 P2 114.3(9) . . ? C27 C26 C31 120.0 . . ? C27 C26 P1 118.7(5) . . ? C31 C26 P1 121.1(5) . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C26 120.0 . . ? C33 C32 C37 120.0 . . ? C33 C32 P1 122.2(4) . . ? C37 C32 P1 117.8(4) . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C32 120.0 . . ? C39 C38 C43 120.0 . . ? C39 C38 P2 118.2(4) . . ? C43 C38 P2 121.7(4) . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C38 120.0 . . ? C45 C44 C49 120.0 . . ? C45 C44 P2 120.9(4) . . ? C49 C44 P2 119.0(4) . . ? C46 C45 C44 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C47 C48 C49 120.0 . . ? C48 C49 C44 120.0 . . ? C51 C50 P3 115.0(8) . . ? C50 C51 C52 112.7(10) . . ? C51 C52 P4 115.3(7) . . ? C54 C53 C58 120.0 . . ? C54 C53 P3 119.7(4) . . ? C58 C53 P3 120.3(4) . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C58 120.0 . . ? C57 C58 C53 120.0 . . ? C60 C59 C64 120.0 . . ? C60 C59 P3 120.8(4) . . ? C64 C59 P3 119.2(4) . . ? C61 C60 C59 120.0 . . ? C60 C61 C62 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C59 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 P4 118.5(4) . . ? C70 C65 P4 121.5(4) . . ? C65 C66 C67 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C69 120.0 . . ? C70 C69 C68 120.0 . . ? C69 C70 C65 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P4 120.0(3) . . ? C76 C71 P4 120.0(3) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? O83A S80A O82A 117.7(12) . . ? O83A S80A O81A 117.1(11) . . ? O82A S80A O81A 115.3(11) . . ? O83A S80A C80A 100.1(11) . . ? O82A S80A C80A 100.7(12) . . ? O81A S80A C80A 101.0(10) . . ? F83A C80A F82A 108.5(16) . . ? F83A C80A F81A 108.7(16) . . ? F82A C80A F81A 108.5(17) . . ? F83A C80A S80A 110.7(15) . . ? F82A C80A S80A 110.1(15) . . ? F81A C80A S80A 110.3(15) . . ? O83B S80B O82B 118.6(15) . . ? O83B S80B O81B 111.4(15) . . ? O82B S80B O81B 112.7(15) . . ? O83B S80B C80B 99.6(14) . . ? O82B S80B C80B 101.7(14) . . ? O81B S80B C80B 111.5(14) . . ? F83B C80B F82B 108(2) . . ? F83B C80B F81B 102(2) . . ? F82B C80B F81B 105(2) . . ? F83B C80B S80B 118(2) . . ? F82B C80B S80B 108.0(19) . . ? F81B C80B S80B 114.6(19) . . ? O82C S80C O81C 113.5(19) . . ? O82C S80C O83C 118(2) . . ? O81C S80C O83C 114.3(19) . . ? O82C S80C C80C 101.5(17) . . ? O81C S80C C80C 107.6(17) . . ? O83C S80C C80C 99.5(17) . . ? F82C C80C F83C 109(2) . . ? F82C C80C F81C 111(2) . . ? F83C C80C F81C 105(2) . . ? F82C C80C S80C 105.7(19) . . ? F83C C80C S80C 114(2) . . ? F81C C80C S80C 113(2) . . ? O82D S80D O83D 115(2) . . ? O82D S80D O81D 113(2) . . ? O83D S80D O81D 115(2) . . ? O82D S80D C80D 103.2(19) . . ? O83D S80D C80D 101.2(19) . . ? O81D S80D C80D 108.1(18) . . ? F81D C80D F82D 108(3) . . ? F81D C80D F83D 103(3) . . ? F82D C80D F83D 106(3) . . ? F81D C80D S80D 115(2) . . ? F82D C80D S80D 110(2) . . ? F83D C80D S80D 114(2) . . ? O93A S90A O91A 116.4(18) . . ? O93A S90A O92A 112.3(18) . . ? O91A S90A O92A 111.5(15) . . ? O93A S90A C90A 102.6(15) . . ? O91A S90A C90A 109.8(13) . . ? O92A S90A C90A 103.0(13) . . ? F91A C90A F92A 109.9(19) . . ? F91A C90A F93A 101.8(17) . . ? F92A C90A F93A 108.2(19) . . ? F91A C90A S90A 115.6(15) . . ? F92A C90A S90A 109.7(16) . . ? F93A C90A S90A 111.2(15) . . ? O92B S90B O91B 117(2) . . ? O92B S90B O93B 113.6(19) . . ? O91B S90B O93B 112.5(18) . . ? O92B S90B C90B 102.2(17) . . ? O91B S90B C90B 109.4(16) . . ? O93B S90B C90B 100.7(16) . . ? F92B C90B F93B 108(2) . . ? F92B C90B F91B 107(2) . . ? F93B C90B F91B 104(2) . . ? F92B C90B S90B 110(2) . . ? F93B C90B S90B 112(2) . . ? F91B C90B S90B 115(2) . . ? O91C S90C O92C 114(2) . . ? O91C S90C O93C 117(2) . . ? O92C S90C O93C 113.9(19) . . ? O91C S90C C90C 106.7(17) . . ? O92C S90C C90C 104.2(18) . . ? O93C S90C C90C 98.3(16) . . ? F91C C90C F93C 108(2) . . ? F91C C90C F92C 104(2) . . ? F93C C90C F92C 107(3) . . ? F91C C90C S90C 115(2) . . ? F93C C90C S90C 115(2) . . ? F92C C90C S90C 107(2) . . ? C101 O100 C104 111(2) . . ? O100 C101 C102 105.6(19) . . ? C103 C102 C101 107.9(18) . . ? C104 C103 C102 105.7(18) . . ? O100 C104 C103 108.1(19) . . ? C106 O105 C109 110(2) . . ? O105 C106 C107 107(2) . . ? C108 C107 C106 106(2) . . ? C107 C108 C109 107.0(19) . . ? O105 C109 C108 106.7(19) . . ? C114 O110 C111 112.7(19) . . ? O110 C111 C112 105.5(19) . . ? C113 C112 C111 108(2) . . ? C112 C113 C114 104.9(19) . . ? O110 C114 C113 107.5(19) . . ? C119 O115 C116 113(2) . . ? O115 C116 C117 106(2) . . ? C118 C117 C116 107(2) . . ? C117 C118 C119 107(2) . . ? O115 C119 C118 106(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.499 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.083 #===END data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 276099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H84 Cl8 F9 N4 Na O12 P4 Pd2 S5' _chemical_formula_weight 2256.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' S S 0.1246 0.1234 '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' _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 13.819(4) _cell_length_b 15.492(3) _cell_length_c 23.828(4) _cell_angle_alpha 103.025(9) _cell_angle_beta 96.742(18) _cell_angle_gamma 99.811(18) _cell_volume 4832.6(19) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 4.80 _cell_measurement_theta_max 12.47 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.97 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4874 _exptl_absorpt_correction_T_max 0.8355 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 31.90 _diffrn_reflns_number 13058 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 22.50 _reflns_number_total 12438 _reflns_number_gt 8557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12438 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 1261 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.002 _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 Pd1 Pd 0.10623(4) 0.45031(3) 0.70773(2) 0.02444(15) Uani 1 1 d . . . Pd2 Pd 0.22778(4) 0.62687(3) 0.81781(2) 0.02768(15) Uani 1 1 d . . . S1 S 0.14394(13) 0.47654(11) 0.81096(7) 0.0301(4) Uani 1 1 d . . . S2 S 0.24532(13) 0.57091(11) 0.71928(7) 0.0280(4) Uani 1 1 d . . . P1 P -0.03399(13) 0.34374(12) 0.70226(7) 0.0286(4) Uani 1 1 d . . . P2 P 0.06893(13) 0.43580(11) 0.60904(7) 0.0274(4) Uani 1 1 d . . . P3 P 0.30214(15) 0.76886(12) 0.81437(8) 0.0350(4) Uani 1 1 d . . . P4 P 0.19861(16) 0.67379(13) 0.91123(8) 0.0403(5) Uani 1 1 d . . . C1 C 0.2440(6) 0.4185(5) 0.8290(3) 0.0377(17) Uani 1 1 d . . . H1A H 0.2801 0.4056 0.7956 0.045 Uiso 1 1 calc R . . H1B H 0.2919 0.4579 0.8630 0.045 Uiso 1 1 calc R . . C2 C 0.2007(6) 0.3302(5) 0.8433(3) 0.0436(19) Uani 1 1 d . . . H2A H 0.1580 0.3425 0.8735 0.052 Uiso 1 1 calc R . . H2B H 0.1587 0.2884 0.8079 0.052 Uiso 1 1 calc R . . N3 N 0.2788(6) 0.2878(5) 0.8641(3) 0.0524(18) Uani 1 1 d D . . H3 H 0.295(7) 0.297(6) 0.9030(7) 0.07(3) Uiso 1 1 d D . . C4 C 0.3249(6) 0.2379(5) 0.8263(4) 0.046(2) Uani 1 1 d . . . O4 O 0.2995(4) 0.2227(4) 0.7734(2) 0.0472(13) Uani 1 1 d . C . N5 N 0.4025(6) 0.2084(5) 0.8520(4) 0.064(2) Uani 1 1 d D . . H5 H 0.419(6) 0.242(5) 0.8891(13) 0.05(3) Uiso 1 1 d D . . C6 C 0.4230(4) 0.0830(4) 0.7735(2) 0.059(2) Uani 1 1 d G . . H6A H 0.3643 0.0864 0.7498 0.071 Uiso 1 1 calc R . . C7 C 0.4766(5) 0.0170(4) 0.7540(3) 0.069(3) Uani 1 1 d G . . H7A H 0.4545 -0.0246 0.7169 0.083 Uiso 1 1 calc R . . C8 C 0.5625(5) 0.0120(5) 0.7888(4) 0.094(4) Uani 1 1 d G . . H8A H 0.5991 -0.0331 0.7754 0.112 Uiso 1 1 calc R . . C9 C 0.5949(5) 0.0728(6) 0.8430(4) 0.111(5) Uani 1 1 d G . . H9A H 0.6536 0.0694 0.8668 0.134 Uiso 1 1 calc R . . C10 C 0.5413(5) 0.1388(5) 0.8625(3) 0.094(4) Uani 1 1 d G . . H10A H 0.5634 0.1804 0.8996 0.112 Uiso 1 1 calc R . . C11 C 0.4554(5) 0.1438(4) 0.8278(3) 0.060(2) Uani 1 1 d G . . C12 C 0.3614(5) 0.5283(5) 0.7265(3) 0.0333(16) Uani 1 1 d . . . H12A H 0.4086 0.5677 0.7608 0.040 Uiso 1 1 calc R . . H12B H 0.3473 0.4663 0.7322 0.040 Uiso 1 1 calc R . . C13 C 0.4063(6) 0.5275(6) 0.6718(4) 0.045(2) Uani 1 1 d . . . H13A H 0.3596 0.4865 0.6378 0.054 Uiso 1 1 calc R . . H13B H 0.4177 0.5891 0.6654 0.054 Uiso 1 1 calc R . . N14 N 0.5012(5) 0.4967(5) 0.6770(3) 0.0511(18) Uani 1 1 d D . . H14 H 0.559(3) 0.538(4) 0.685(4) 0.05(2) Uiso 1 1 d D . . C15 C 0.5034(6) 0.4104(6) 0.6731(4) 0.046(2) Uani 1 1 d . . . O15 O 0.4241(4) 0.3523(3) 0.6611(2) 0.0433(12) Uani 1 1 d . C . N16 N 0.5936(6) 0.3893(5) 0.6816(4) 0.067(2) Uani 1 1 d D . . H16 H 0.640(9) 0.441(6) 0.694(7) 0.17(7) Uiso 1 1 d D . . C17 C 0.5890(5) 0.2367(4) 0.6241(2) 0.071(3) Uani 1 1 d G . . H17A H 0.5652 0.2523 0.5894 0.085 Uiso 1 1 calc R . . C18 C 0.6043(6) 0.1496(4) 0.6216(3) 0.087(4) Uani 1 1 d G . . H18A H 0.5909 0.1057 0.5852 0.105 Uiso 1 1 calc R . . C19 C 0.6392(6) 0.1267(4) 0.6723(4) 0.098(4) Uani 1 1 d G . . H19A H 0.6497 0.0672 0.6706 0.118 Uiso 1 1 calc R . . C20 C 0.6588(5) 0.1910(5) 0.7255(3) 0.085(3) Uani 1 1 d G . . H20A H 0.6827 0.1754 0.7602 0.102 Uiso 1 1 calc R . . C21 C 0.6436(5) 0.2781(4) 0.7281(2) 0.070(3) Uani 1 1 d G . . H21A H 0.6570 0.3220 0.7644 0.084 Uiso 1 1 calc R . . C22 C 0.6087(4) 0.3009(3) 0.6773(3) 0.054(2) Uani 1 1 d G . . C23 C -0.1428(5) 0.3555(5) 0.6562(3) 0.0342(16) Uani 1 1 d . . . H23A H -0.1998 0.3086 0.6582 0.041 Uiso 1 1 calc R . . H23B H -0.1586 0.4152 0.6727 0.041 Uiso 1 1 calc R . . C24 C -0.1343(5) 0.3479(5) 0.5918(3) 0.0370(17) Uani 1 1 d . . . H24A H -0.1116 0.2914 0.5759 0.044 Uiso 1 1 calc R . . H24B H -0.2011 0.3437 0.5697 0.044 Uiso 1 1 calc R . . C25 C -0.0626(5) 0.4277(5) 0.5821(3) 0.0334(16) Uani 1 1 d . . . H25A H -0.0822 0.4843 0.6013 0.040 Uiso 1 1 calc R . . H25B H -0.0705 0.4238 0.5397 0.040 Uiso 1 1 calc R . . C26 C -0.1093(4) 0.4268(3) 0.7981(2) 0.046(2) Uani 1 1 d G . . H26A H -0.1063 0.4758 0.7801 0.055 Uiso 1 1 calc R . . C27 C -0.1444(4) 0.4332(3) 0.8509(2) 0.058(2) Uani 1 1 d G . . H27A H -0.1654 0.4865 0.8690 0.069 Uiso 1 1 calc R . . C28 C -0.1488(5) 0.3615(4) 0.87732(18) 0.064(3) Uani 1 1 d G . . H28A H -0.1728 0.3659 0.9134 0.076 Uiso 1 1 calc R . . C29 C -0.1180(5) 0.2835(3) 0.8509(2) 0.066(3) Uani 1 1 d G . . H29A H -0.1210 0.2346 0.8690 0.079 Uiso 1 1 calc R . . C30 C -0.0829(4) 0.2772(3) 0.7981(2) 0.0455(19) Uani 1 1 d G . . H30A H -0.0619 0.2238 0.7801 0.055 Uiso 1 1 calc R . . C31 C -0.0785(4) 0.3488(3) 0.77173(16) 0.0348(17) Uani 1 1 d G . . C32 C -0.0968(3) 0.1590(3) 0.6483(2) 0.050(2) Uani 1 1 d G . . H32A H -0.1623 0.1705 0.6439 0.060 Uiso 1 1 calc R . . C33 C -0.0812(4) 0.0719(3) 0.6276(3) 0.063(3) Uani 1 1 d G . . H33A H -0.1360 0.0240 0.6090 0.075 Uiso 1 1 calc R . . C34 C 0.0145(4) 0.0550(2) 0.6341(3) 0.065(3) Uani 1 1 d G . . H34A H 0.0252 -0.0044 0.6199 0.078 Uiso 1 1 calc R . . C35 C 0.0947(3) 0.1252(3) 0.6613(3) 0.063(3) Uani 1 1 d G . . H35A H 0.1602 0.1136 0.6657 0.076 Uiso 1 1 calc R . . C36 C 0.0791(3) 0.2122(3) 0.6820(2) 0.0449(19) Uani 1 1 d G . . H36A H 0.1339 0.2602 0.7006 0.054 Uiso 1 1 calc R . . C37 C -0.0166(3) 0.2291(2) 0.6755(2) 0.0313(16) Uani 1 1 d G . . C38 C 0.0508(3) 0.2899(4) 0.5120(2) 0.054(2) Uani 1 1 d G . . H38A H -0.0078 0.3073 0.4972 0.065 Uiso 1 1 calc R . . C39 C 0.0816(4) 0.2160(4) 0.47972(19) 0.069(3) Uani 1 1 d G . . H39A H 0.0441 0.1828 0.4429 0.083 Uiso 1 1 calc R . . C40 C 0.1673(5) 0.1905(3) 0.5014(2) 0.066(3) Uani 1 1 d G . . H40A H 0.1884 0.1400 0.4793 0.079 Uiso 1 1 calc R . . C41 C 0.2222(4) 0.2390(4) 0.5553(2) 0.069(3) Uani 1 1 d G . . H41A H 0.2807 0.2216 0.5701 0.083 Uiso 1 1 calc R . . C42 C 0.1913(4) 0.3129(4) 0.58758(17) 0.049(2) Uani 1 1 d G . . H42A H 0.2288 0.3461 0.6244 0.059 Uiso 1 1 calc R . . C43 C 0.1056(4) 0.3384(3) 0.56593(18) 0.0320(16) Uani 1 1 d G . . C44 C 0.2074(3) 0.5280(2) 0.55476(19) 0.0355(17) Uani 1 1 d G . . H44A H 0.2241 0.4712 0.5400 0.043 Uiso 1 1 calc R . . C45 C 0.2598(3) 0.6058(3) 0.5438(2) 0.048(2) Uani 1 1 d G . . H45A H 0.3123 0.6021 0.5215 0.057 Uiso 1 1 calc R . . C46 C 0.2353(4) 0.6890(3) 0.5654(2) 0.052(2) Uani 1 1 d G . . H46A H 0.2711 0.7422 0.5580 0.062 Uiso 1 1 calc R . . C47 C 0.1585(4) 0.6945(2) 0.5980(2) 0.048(2) Uani 1 1 d G . . H47A H 0.1418 0.7514 0.6128 0.058 Uiso 1 1 calc R . . C48 C 0.1061(3) 0.6167(3) 0.60897(19) 0.0395(18) Uani 1 1 d G . . H48A H 0.0536 0.6205 0.6312 0.047 Uiso 1 1 calc R . . C49 C 0.1305(3) 0.5335(2) 0.58734(19) 0.0312(16) Uani 1 1 d G . . C50 C 0.2835(8) 0.7745(6) 0.9581(3) 0.056(2) Uani 1 1 d . . . H50A H 0.2583 0.7919 0.9954 0.067 Uiso 1 1 calc R . . H50B H 0.3495 0.7596 0.9670 0.067 Uiso 1 1 calc R . . C51 C 0.2959(8) 0.8552(5) 0.9309(4) 0.063(3) Uani 1 1 d . . . H51A H 0.2295 0.8614 0.9135 0.076 Uiso 1 1 calc R . . H51B H 0.3250 0.9110 0.9619 0.076 Uiso 1 1 calc R . . C52 C 0.3618(7) 0.8460(6) 0.8841(3) 0.053(2) Uani 1 1 d . . . H52A H 0.4212 0.8247 0.8987 0.064 Uiso 1 1 calc R . . H52B H 0.3849 0.9066 0.8777 0.064 Uiso 1 1 calc R . . C53 C 0.2979(3) 0.5770(4) 0.9751(2) 0.056(2) Uani 1 1 d G . . H53A H 0.3564 0.6177 0.9730 0.067 Uiso 1 1 calc R . . C54 C 0.3049(4) 0.5070(4) 1.0020(3) 0.073(3) Uani 1 1 d G . . H54A H 0.3683 0.4998 1.0184 0.088 Uiso 1 1 calc R . . C55 C 0.2193(5) 0.4475(3) 1.0050(2) 0.064(3) Uani 1 1 d G . . H55A H 0.2242 0.3997 1.0234 0.076 Uiso 1 1 calc R . . C56 C 0.1267(4) 0.4581(3) 0.9811(2) 0.056(2) Uani 1 1 d G . . H56A H 0.0682 0.4174 0.9832 0.067 Uiso 1 1 calc R . . C57 C 0.1196(3) 0.5280(3) 0.9542(2) 0.0426(19) Uani 1 1 d G . . H57A H 0.0563 0.5352 0.9379 0.051 Uiso 1 1 calc R . . C58 C 0.2052(4) 0.5875(3) 0.9512(2) 0.0430(19) Uani 1 1 d G . . C59 C 0.0458(5) 0.7324(5) 0.96616(19) 0.076(3) Uani 1 1 d G . . H59A H 0.0914 0.7440 1.0014 0.091 Uiso 1 1 calc R . . C60 C -0.0491(5) 0.7503(5) 0.9678(3) 0.094(4) Uani 1 1 d G . . H60A H -0.0685 0.7741 1.0042 0.113 Uiso 1 1 calc R . . C61 C -0.1158(4) 0.7333(5) 0.9163(3) 0.080(3) Uani 1 1 d G . . H61A H -0.1807 0.7455 0.9174 0.096 Uiso 1 1 calc R . . C62 C -0.0874(4) 0.6984(5) 0.8631(3) 0.074(3) Uani 1 1 d G . . H62A H -0.1330 0.6867 0.8278 0.088 Uiso 1 1 calc R . . C63 C 0.0075(4) 0.6804(4) 0.86142(19) 0.059(2) Uani 1 1 d G . . H63A H 0.0269 0.6566 0.8251 0.071 Uiso 1 1 calc R . . C64 C 0.0742(3) 0.6974(4) 0.9130(2) 0.045(2) Uani 1 1 d G . . C65 C 0.2369(4) 0.9160(3) 0.7862(3) 0.067(3) Uani 1 1 d G . . H65A H 0.3007 0.9497 0.8056 0.081 Uiso 1 1 calc R . . C66 C 0.1686(5) 0.9588(3) 0.7615(3) 0.081(3) Uani 1 1 d G . . H66A H 0.1858 1.0217 0.7641 0.097 Uiso 1 1 calc R . . C67 C 0.0753(4) 0.9094(4) 0.7331(3) 0.079(3) Uani 1 1 d G . . H67A H 0.0287 0.9386 0.7162 0.094 Uiso 1 1 calc R . . C68 C 0.0503(3) 0.8172(4) 0.7293(3) 0.066(3) Uani 1 1 d G . . H68A H -0.0135 0.7835 0.7099 0.079 Uiso 1 1 calc R . . C69 C 0.1185(4) 0.7745(3) 0.7539(3) 0.053(2) Uani 1 1 d G . . H69A H 0.1014 0.7115 0.7513 0.063 Uiso 1 1 calc R . . C70 C 0.2119(3) 0.8238(3) 0.7824(2) 0.0364(17) Uani 1 1 d G . . C71 C 0.3885(3) 0.7834(3) 0.71516(19) 0.0416(18) Uani 1 1 d G . . H71A H 0.3270 0.7952 0.6997 0.050 Uiso 1 1 calc R . . C72 C 0.4650(4) 0.7805(4) 0.68214(17) 0.053(2) Uani 1 1 d G . . H72A H 0.4557 0.7905 0.6441 0.064 Uiso 1 1 calc R . . C73 C 0.5550(3) 0.7632(4) 0.7047(2) 0.055(2) Uani 1 1 d G . . H73A H 0.6072 0.7613 0.6822 0.066 Uiso 1 1 calc R . . C74 C 0.5686(3) 0.7486(4) 0.7603(2) 0.058(2) Uani 1 1 d G . . H74A H 0.6301 0.7367 0.7757 0.070 Uiso 1 1 calc R . . C75 C 0.4922(3) 0.7514(4) 0.79334(17) 0.0452(19) Uani 1 1 d G . . H75A H 0.5014 0.7415 0.8313 0.054 Uiso 1 1 calc R . . C76 C 0.4021(3) 0.7688(3) 0.77076(17) 0.0339(17) Uani 1 1 d G . . Na Na 0.3908(5) 0.2101(4) 0.6877(3) 0.126(2) Uani 1 1 d . . . S80 S 0.8004(6) 0.6171(5) 0.6947(3) 0.080(4) Uani 0.661(10) 1 d PD A 1 O80A O 0.8934(8) 0.5921(11) 0.6958(7) 0.070(5) Uani 0.661(10) 1 d PDU A 1 O80B O 0.8072(9) 0.7136(6) 0.7171(6) 0.082(4) Uani 0.661(10) 1 d PDU A 1 O80C O 0.7275(7) 0.5648(7) 0.7169(5) 0.074(3) Uani 0.661(10) 1 d PDU A 1 C80 C 0.7512(9) 0.5975(8) 0.6191(6) 0.082(5) Uani 0.661(10) 1 d PD A 1 F80A F 0.6649(8) 0.6239(8) 0.6122(5) 0.111(4) Uani 0.661(10) 1 d PDU A 1 F80B F 0.7361(8) 0.5096(7) 0.5945(5) 0.119(4) Uani 0.661(10) 1 d PDU A 1 F80C F 0.8152(10) 0.6403(10) 0.5912(6) 0.134(5) Uani 0.661(10) 1 d PDU A 1 S80A S 0.8053(9) 0.6269(8) 0.6932(3) 0.029(3) Uiso 0.339(10) 1 d PD A 2 O80D O 0.9004(14) 0.605(2) 0.7001(12) 0.067(9) Uiso 0.339(10) 1 d PDU A 2 O80E O 0.7241(16) 0.5518(13) 0.6811(10) 0.107(8) Uiso 0.339(10) 1 d PDU A 2 O80F O 0.794(2) 0.7035(13) 0.7357(8) 0.074(7) Uiso 0.339(10) 1 d PDU A 2 C80A C 0.7976(12) 0.6622(11) 0.6260(7) 0.053(7) Uiso 0.339(10) 1 d PD A 2 F80D F 0.7095(13) 0.6821(16) 0.6111(9) 0.117(7) Uiso 0.339(10) 1 d PDU A 2 F80E F 0.8655(15) 0.7352(13) 0.6305(9) 0.137(8) Uiso 0.339(10) 1 d PDU A 2 F80F F 0.8088(19) 0.5967(14) 0.5818(7) 0.108(8) Uiso 0.339(10) 1 d PDU A 2 S81 S 0.4141(7) 0.2514(4) 1.0148(2) 0.0614(16) Uani 0.632(14) 1 d PD B 1 O81A O 0.4742(11) 0.2730(9) 0.9711(5) 0.103(5) Uani 0.632(14) 1 d PDU B 1 O81B O 0.4694(13) 0.2781(8) 1.0703(4) 0.105(5) Uani 0.632(14) 1 d PDU B 1 O81C O 0.3232(12) 0.2778(12) 1.0047(8) 0.144(6) Uani 0.632(14) 1 d PDU B 1 C81 C 0.3883(11) 0.1307(10) 0.9957(5) 0.100(8) Uani 0.632(14) 1 d PD B 1 F81A F 0.3361(16) 0.0961(9) 1.0320(7) 0.158(6) Uani 0.632(14) 1 d PDU B 1 F81B F 0.3373(14) 0.0947(10) 0.9417(5) 0.142(7) Uani 0.632(14) 1 d PDU B 1 F81C F 0.4719(10) 0.0986(7) 0.9979(6) 0.120(5) Uani 0.632(14) 1 d PDU B 1 S81A S 0.3779(9) 0.2320(7) 1.0164(5) 0.064(4) Uiso 0.368(14) 1 d PD B 2 O81D O 0.4665(14) 0.2574(15) 0.9933(11) 0.083(7) Uiso 0.368(14) 1 d PDU B 2 O81E O 0.383(2) 0.2591(14) 1.0758(7) 0.109(7) Uiso 0.368(14) 1 d PDU B 2 O81F O 0.2909(13) 0.2479(12) 0.9829(8) 0.066(5) Uiso 0.368(14) 1 d PDU B 2 C81A C 0.3564(14) 0.1105(12) 0.9986(8) 0.107(17) Uiso 0.368(14) 1 d PD B 2 F81D F 0.2728(15) 0.0774(12) 1.0164(9) 0.112(7) Uiso 0.368(14) 1 d PDU B 2 F81E F 0.3471(18) 0.0763(14) 0.9414(7) 0.091(7) Uiso 0.368(14) 1 d PDU B 2 F81F F 0.4302(16) 0.0831(13) 1.0251(11) 0.116(7) Uiso 0.368(14) 1 d PDU B 2 S82 S 0.3332(4) -0.0171(3) 0.5799(2) 0.0555(14) Uani 0.589(9) 1 d PD C 1 O82A O 0.3638(9) -0.0877(8) 0.6037(6) 0.074(4) Uani 0.589(9) 1 d PDU C 1 O82B O 0.3862(11) 0.0072(10) 0.5366(7) 0.122(5) Uani 0.589(9) 1 d PDU C 1 O82C O 0.3144(8) 0.0561(7) 0.6227(5) 0.075(4) Uani 0.589(9) 1 d PDU C 1 C82 C 0.2101(11) -0.0694(7) 0.5407(5) 0.127(14) Uani 0.589(9) 1 d PD C 1 F82A F 0.1690(11) -0.0105(9) 0.5191(6) 0.114(5) Uani 0.589(9) 1 d PDU C 1 F82B F 0.1558(8) -0.0983(8) 0.5782(6) 0.116(4) Uani 0.589(9) 1 d PDU C 1 F82C F 0.2146(10) -0.1381(7) 0.4971(5) 0.107(5) Uani 0.589(9) 1 d PDU C 1 S82A S 0.2992(6) -0.0306(5) 0.5968(3) 0.054(2) Uiso 0.411(9) 1 d PD C 2 O82D O 0.3737(15) -0.0844(14) 0.5833(9) 0.085(7) Uiso 0.411(9) 1 d PDU C 2 O82E O 0.2495(14) -0.0346(13) 0.6371(7) 0.099(6) Uiso 0.411(9) 1 d PDU C 2 O82F O 0.3519(13) 0.0682(10) 0.5963(8) 0.082(5) Uiso 0.411(9) 1 d PDU C 2 C82A C 0.2179(11) -0.0555(10) 0.5277(7) 0.049(7) Uiso 0.411(9) 1 d PD C 2 F82D F 0.1494(13) -0.0043(15) 0.5321(9) 0.108(7) Uiso 0.411(9) 1 d PDU C 2 F82E F 0.2656(12) -0.0401(12) 0.4855(5) 0.108(6) Uiso 0.411(9) 1 d PDU C 2 F82F F 0.1708(13) -0.1414(10) 0.5144(7) 0.097(6) Uiso 0.411(9) 1 d PDU C 2 C90 C 0.4279(10) 0.1386(11) 0.4550(7) 0.119(5) Uani 1 1 d U . . H90A H 0.4027 0.1185 0.4882 0.143 Uiso 1 1 calc R . . H90B H 0.4837 0.1085 0.4455 0.143 Uiso 1 1 calc R . . Cl1 Cl 0.3322(3) 0.1070(3) 0.39415(18) 0.1157(12) Uani 1 1 d . . . Cl2 Cl 0.4704(4) 0.2551(4) 0.47504(19) 0.1442(17) Uani 1 1 d . . . C91 C 0.8389(13) 0.9190(11) 0.7959(8) 0.135(6) Uani 1 1 d U . . H91A H 0.8083 0.8593 0.7690 0.162 Uiso 1 1 calc R . . H91B H 0.9104 0.9194 0.8068 0.162 Uiso 1 1 calc R . . Cl3 Cl 0.7864(4) 0.9280(4) 0.8568(2) 0.1535(19) Uani 1 1 d . . . Cl4 Cl 0.8299(4) 0.9998(4) 0.7585(2) 0.1498(18) Uani 1 1 d . . . C92 C 0.4306(16) 0.4637(12) 1.1396(7) 0.137(6) Uani 1 1 d U D 1 H92A H 0.3962 0.4412 1.0987 0.164 Uiso 1 1 calc R D 1 H92B H 0.4873 0.4330 1.1438 0.164 Uiso 1 1 calc R D 1 Cl5 Cl 0.3556(4) 0.4373(3) 1.1816(3) 0.1188(16) Uani 0.77 1 d PU D 1 Cl6 Cl 0.4780(4) 0.5838(3) 1.1541(3) 0.1536(18) Uani 0.97 1 d PU D 1 Cl6' Cl 0.522(2) 0.4521(19) 1.1107(13) 0.195(8) Uiso 0.26 1 d PU E 2 C93 C 0.880(3) 0.934(2) 1.0924(16) 0.271(16) Uani 1 1 d U . . H93A H 0.8200 0.9412 1.1106 0.325 Uiso 0.65(2) 1 calc PR F 1 H93B H 0.8569 0.8950 1.0524 0.325 Uiso 0.65(2) 1 calc PR F 1 H93C H 0.8473 0.9694 1.1199 0.325 Uiso 0.35(2) 1 d PR F 2 H93D H 0.8294 0.8887 1.0655 0.325 Uiso 0.35(2) 1 d PR F 2 Cl7 Cl 0.9455(7) 0.8800(5) 1.1294(4) 0.216(3) Uani 1 1 d . F . Cl8 Cl 0.9344(8) 1.0383(11) 1.0861(8) 0.191(6) Uani 0.65(2) 1 d PU F 1 Cl8' Cl 0.938(3) 0.990(3) 1.0469(19) 0.251(10) Uiso 0.35(2) 1 d PU F 2 O95 O 0.4532(17) 0.4514(14) 0.5273(9) 0.111(6) Uiso 0.54 1 d PU G 1 O96 O 0.507(4) 0.510(3) 0.5269(17) 0.129(11) Uiso 0.26 1 d PU . 2 O97 O 0.429(4) 0.412(4) 0.527(3) 0.114(9) Uiso 0.20 1 d PU H 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 Pd1 0.0243(3) 0.0266(3) 0.0223(3) 0.0069(2) 0.0037(2) 0.0042(2) Pd2 0.0298(3) 0.0288(3) 0.0248(3) 0.0073(2) 0.0062(2) 0.0049(2) S1 0.0316(10) 0.0337(9) 0.0258(8) 0.0105(7) 0.0048(7) 0.0045(8) S2 0.0264(9) 0.0312(9) 0.0260(8) 0.0074(7) 0.0054(7) 0.0039(7) P1 0.0261(10) 0.0313(9) 0.0278(9) 0.0084(7) 0.0059(7) 0.0019(8) P2 0.0275(10) 0.0305(9) 0.0239(9) 0.0078(7) 0.0038(7) 0.0038(8) P3 0.0367(11) 0.0303(10) 0.0358(10) 0.0068(8) 0.0077(8) 0.0019(8) P4 0.0493(13) 0.0421(11) 0.0304(10) 0.0081(8) 0.0128(9) 0.0091(10) C1 0.040(4) 0.034(4) 0.040(4) 0.012(3) 0.000(3) 0.010(3) C2 0.059(5) 0.047(4) 0.033(4) 0.016(3) 0.017(4) 0.021(4) N3 0.075(5) 0.061(4) 0.037(4) 0.027(3) 0.011(4) 0.036(4) C4 0.043(5) 0.040(4) 0.062(6) 0.025(4) 0.007(4) 0.014(4) O4 0.046(3) 0.056(3) 0.042(3) 0.013(3) 0.005(3) 0.016(3) N5 0.071(6) 0.060(5) 0.061(5) 0.009(4) -0.009(4) 0.032(4) C6 0.056(6) 0.044(5) 0.080(7) 0.021(5) 0.012(5) 0.008(4) C7 0.073(7) 0.037(5) 0.101(8) 0.018(5) 0.025(6) 0.015(5) C8 0.083(9) 0.070(7) 0.140(12) 0.028(8) 0.027(8) 0.040(7) C9 0.083(9) 0.111(11) 0.144(13) 0.024(10) -0.005(9) 0.056(9) C10 0.094(9) 0.101(9) 0.086(8) 0.007(7) -0.010(7) 0.059(8) C11 0.064(6) 0.055(5) 0.069(6) 0.028(5) 0.005(5) 0.023(5) C12 0.022(4) 0.041(4) 0.038(4) 0.009(3) 0.006(3) 0.010(3) C13 0.039(5) 0.049(5) 0.062(5) 0.026(4) 0.027(4) 0.016(4) N14 0.030(4) 0.042(4) 0.088(5) 0.022(4) 0.026(4) 0.007(3) C15 0.035(5) 0.050(5) 0.053(5) 0.009(4) 0.014(4) 0.011(4) O15 0.028(3) 0.040(3) 0.061(3) 0.014(2) 0.006(2) 0.005(3) N16 0.033(4) 0.047(5) 0.119(7) 0.012(4) 0.017(4) 0.011(4) C17 0.049(6) 0.085(8) 0.073(7) 0.003(6) 0.008(5) 0.021(5) C18 0.077(8) 0.051(6) 0.116(10) -0.013(6) 0.021(7) 0.009(6) C19 0.058(7) 0.092(9) 0.157(14) 0.039(10) 0.019(8) 0.037(7) C20 0.052(7) 0.088(8) 0.125(11) 0.049(8) 0.019(7) 0.010(6) C21 0.046(6) 0.060(6) 0.099(8) 0.017(5) 0.014(5) -0.003(5) C22 0.026(4) 0.055(5) 0.081(7) 0.014(5) 0.013(4) 0.012(4) C23 0.019(4) 0.039(4) 0.042(4) 0.010(3) 0.001(3) 0.000(3) C24 0.023(4) 0.046(4) 0.039(4) 0.008(3) -0.001(3) 0.005(3) C25 0.028(4) 0.042(4) 0.029(4) 0.011(3) -0.003(3) 0.007(3) C26 0.044(5) 0.048(5) 0.036(4) -0.005(4) 0.008(4) 0.005(4) C27 0.052(6) 0.066(6) 0.052(5) 0.000(4) 0.015(4) 0.017(5) C28 0.071(7) 0.081(7) 0.040(5) 0.010(5) 0.026(5) 0.012(5) C29 0.083(7) 0.071(6) 0.044(5) 0.025(5) 0.018(5) -0.002(6) C30 0.053(5) 0.047(5) 0.040(4) 0.011(4) 0.014(4) 0.015(4) C31 0.025(4) 0.048(4) 0.028(4) 0.008(3) 0.006(3) -0.002(3) C32 0.045(5) 0.042(5) 0.055(5) 0.006(4) 0.002(4) -0.001(4) C33 0.083(7) 0.034(5) 0.056(5) 0.000(4) 0.000(5) -0.004(5) C34 0.088(8) 0.036(5) 0.071(6) 0.008(4) 0.018(6) 0.019(5) C35 0.055(6) 0.046(5) 0.096(7) 0.017(5) 0.026(5) 0.017(5) C36 0.045(5) 0.036(4) 0.051(5) 0.005(4) 0.007(4) 0.006(4) C37 0.029(4) 0.034(4) 0.031(4) 0.006(3) 0.010(3) 0.005(3) C38 0.047(5) 0.061(5) 0.046(5) -0.004(4) -0.007(4) 0.019(4) C39 0.072(7) 0.066(6) 0.047(5) -0.021(5) 0.009(5) 0.002(5) C40 0.095(8) 0.049(5) 0.060(6) 0.006(4) 0.034(6) 0.028(5) C41 0.088(8) 0.076(7) 0.056(6) 0.015(5) 0.017(5) 0.049(6) C42 0.060(6) 0.067(6) 0.030(4) 0.013(4) 0.012(4) 0.034(5) C43 0.042(4) 0.027(4) 0.023(3) 0.003(3) 0.004(3) 0.002(3) C44 0.044(5) 0.039(4) 0.025(4) 0.012(3) 0.007(3) 0.005(4) C45 0.042(5) 0.064(6) 0.039(4) 0.030(4) 0.000(4) 0.000(4) C46 0.048(5) 0.048(5) 0.055(5) 0.028(4) -0.011(4) -0.010(4) C47 0.056(5) 0.041(5) 0.048(5) 0.021(4) -0.008(4) 0.010(4) C48 0.046(5) 0.035(4) 0.038(4) 0.012(3) -0.001(3) 0.011(4) C49 0.036(4) 0.029(4) 0.028(4) 0.013(3) -0.006(3) 0.003(3) C50 0.074(6) 0.051(5) 0.036(4) 0.004(4) 0.010(4) 0.002(5) C51 0.092(7) 0.037(5) 0.045(5) -0.008(4) 0.014(5) -0.008(5) C52 0.063(6) 0.043(5) 0.041(5) 0.001(4) 0.005(4) -0.012(4) C53 0.057(6) 0.071(6) 0.043(5) 0.020(4) 0.010(4) 0.013(5) C54 0.075(7) 0.102(8) 0.055(6) 0.041(6) 0.004(5) 0.028(7) C55 0.101(9) 0.066(6) 0.038(5) 0.026(4) 0.019(5) 0.036(6) C56 0.081(7) 0.056(5) 0.040(5) 0.016(4) 0.032(5) 0.019(5) C57 0.055(5) 0.043(4) 0.034(4) 0.010(3) 0.017(4) 0.015(4) C58 0.060(6) 0.051(5) 0.022(4) 0.011(3) 0.009(4) 0.017(4) C59 0.090(8) 0.085(7) 0.072(7) 0.021(6) 0.045(6) 0.050(7) C60 0.129(12) 0.106(9) 0.080(8) 0.030(7) 0.069(8) 0.066(9) C61 0.073(7) 0.073(7) 0.125(10) 0.050(7) 0.053(8) 0.039(6) C62 0.060(7) 0.088(8) 0.088(8) 0.036(6) 0.022(6) 0.030(6) C63 0.055(6) 0.071(6) 0.063(6) 0.019(5) 0.023(5) 0.031(5) C64 0.056(5) 0.041(4) 0.051(5) 0.020(4) 0.028(4) 0.019(4) C65 0.053(6) 0.045(5) 0.107(8) 0.029(5) 0.017(5) 0.006(5) C66 0.068(7) 0.055(6) 0.141(11) 0.055(7) 0.028(7) 0.026(6) C67 0.053(6) 0.092(8) 0.129(10) 0.076(7) 0.041(6) 0.036(6) C68 0.044(5) 0.069(6) 0.095(8) 0.040(6) 0.009(5) 0.014(5) C69 0.041(5) 0.045(5) 0.081(6) 0.031(4) 0.011(4) 0.012(4) C70 0.034(4) 0.035(4) 0.049(4) 0.017(3) 0.021(4) 0.010(3) C71 0.040(5) 0.043(4) 0.043(4) 0.018(3) 0.006(4) 0.003(4) C72 0.073(7) 0.043(5) 0.054(5) 0.027(4) 0.032(5) 0.007(4) C73 0.045(5) 0.057(5) 0.073(6) 0.028(5) 0.025(5) 0.013(4) C74 0.034(5) 0.052(5) 0.088(7) 0.019(5) 0.007(5) 0.008(4) C75 0.034(5) 0.046(5) 0.055(5) 0.020(4) 0.001(4) 0.003(4) C76 0.036(4) 0.026(4) 0.036(4) 0.010(3) 0.001(3) -0.002(3) Na 0.135(5) 0.099(4) 0.137(5) 0.018(3) 0.039(4) 0.009(4) S80 0.054(4) 0.051(4) 0.150(8) 0.039(3) 0.047(3) 0.013(2) O80A 0.048(6) 0.063(8) 0.099(9) 0.012(6) 0.009(5) 0.024(5) O80B 0.063(7) 0.062(7) 0.120(10) 0.004(7) 0.027(7) 0.023(5) O80C 0.052(6) 0.074(6) 0.085(8) 0.022(6) 0.009(5) -0.022(5) C80 0.067(11) 0.100(14) 0.093(13) 0.046(11) 0.015(10) 0.026(11) F80A 0.103(8) 0.121(9) 0.117(8) 0.024(7) -0.007(6) 0.074(7) F80B 0.102(8) 0.126(9) 0.111(8) -0.023(7) -0.010(6) 0.067(7) F80C 0.166(11) 0.147(11) 0.115(9) 0.075(8) 0.038(8) 0.035(10) S81 0.065(4) 0.065(3) 0.062(3) 0.028(2) 0.003(3) 0.023(3) O81A 0.130(10) 0.103(9) 0.052(7) 0.016(7) 0.002(7) -0.029(8) O81B 0.172(13) 0.079(7) 0.058(7) 0.015(6) -0.028(7) 0.045(8) O81C 0.125(12) 0.131(11) 0.170(13) 0.026(11) -0.037(11) 0.065(10) C81 0.095(16) 0.105(16) 0.093(16) 0.052(13) -0.041(12) 0.007(14) F81A 0.204(14) 0.140(10) 0.130(10) 0.056(8) 0.063(10) -0.022(11) F81B 0.170(13) 0.110(10) 0.107(9) 0.016(7) -0.038(9) -0.020(10) F81C 0.144(10) 0.082(7) 0.115(9) 0.000(6) -0.030(9) 0.042(7) S82 0.056(3) 0.033(2) 0.068(3) 0.0032(19) 0.008(3) -0.0024(19) O82A 0.071(8) 0.075(7) 0.085(9) 0.037(7) -0.004(7) 0.032(6) O82B 0.112(11) 0.115(10) 0.143(12) 0.049(9) 0.057(9) -0.016(9) O82C 0.061(7) 0.053(6) 0.084(8) -0.022(6) 0.003(6) -0.006(5) C82 0.25(4) 0.017(9) 0.090(16) 0.008(10) -0.044(19) 0.030(14) F82A 0.139(11) 0.089(8) 0.113(9) 0.028(7) -0.050(9) 0.063(8) F82B 0.078(8) 0.088(8) 0.193(12) 0.065(8) 0.029(8) 0.003(6) F82C 0.138(11) 0.071(7) 0.078(7) -0.020(6) -0.040(8) 0.018(7) C90 0.076(8) 0.159(12) 0.150(12) 0.088(10) 0.030(8) 0.026(8) Cl1 0.117(3) 0.111(3) 0.129(3) 0.032(2) 0.060(2) 0.021(2) Cl2 0.151(4) 0.179(4) 0.098(3) 0.047(3) 0.023(3) 0.002(3) C91 0.121(11) 0.103(10) 0.188(14) 0.029(9) 0.072(10) 0.016(9) Cl3 0.137(4) 0.209(5) 0.161(4) 0.092(4) 0.046(3) 0.085(4) Cl4 0.123(3) 0.194(5) 0.165(4) 0.089(4) 0.028(3) 0.058(3) C92 0.179(14) 0.145(12) 0.097(9) 0.042(9) 0.021(10) 0.044(11) Cl5 0.120(4) 0.098(3) 0.136(4) 0.040(3) 0.000(3) 0.016(3) Cl6 0.125(4) 0.121(3) 0.197(5) 0.031(3) 0.012(3) -0.001(3) C93 0.26(2) 0.28(2) 0.28(2) 0.059(17) 0.027(17) 0.109(18) Cl7 0.245(8) 0.146(5) 0.252(8) 0.042(5) 0.029(7) 0.041(5) Cl8 0.161(8) 0.214(10) 0.223(13) 0.070(9) 0.023(7) 0.093(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 Pd1 P1 2.2916(19) . ? Pd1 P2 2.2987(17) . ? Pd1 S1 2.3799(17) . ? Pd1 S2 2.3835(18) . ? Pd2 P4 2.286(2) . ? Pd2 P3 2.2874(19) . ? Pd2 S2 2.3684(17) . ? Pd2 S1 2.3786(18) . ? S1 C1 1.834(7) . ? S2 C12 1.840(7) . ? P1 C37 1.813(4) . ? P1 C23 1.816(7) . ? P1 C31 1.823(3) . ? P2 C43 1.809(4) . ? P2 C49 1.817(3) . ? P2 C25 1.829(7) . ? P3 C70 1.815(4) . ? P3 C52 1.821(8) . ? P3 C76 1.824(4) . ? P4 C58 1.815(4) . ? P4 C64 1.822(5) . ? P4 C50 1.828(9) . ? C1 C2 1.523(10) . ? C2 N3 1.451(10) . ? N3 C4 1.343(11) . ? C4 O4 1.225(10) . ? C4 N5 1.369(11) . ? O4 Na 2.511(8) . ? N5 C11 1.398(9) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C12 C13 1.506(10) . ? C13 N14 1.471(10) . ? N14 C15 1.325(11) . ? C15 O15 1.253(9) . ? C15 N16 1.346(11) . ? O15 Na 2.413(8) . ? N16 C22 1.403(9) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.533(10) . ? C24 C25 1.526(10) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C50 C51 1.527(12) . ? C51 C52 1.517(13) . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? Na O82C 2.509(11) . ? Na O82F 2.650(18) . ? S80 O80A 1.404(9) . ? S80 O80C 1.409(9) . ? S80 O80B 1.452(9) . ? S80 C80 1.789(14) . ? C80 F80B 1.326(12) . ? C80 F80A 1.329(11) . ? C80 F80C 1.341(11) . ? S80A O80D 1.414(12) . ? S80A O80F 1.419(12) . ? S80A O80E 1.422(13) . ? S80A C80A 1.802(18) . ? C80A F80E 1.315(13) . ? C80A F80F 1.333(13) . ? C80A F80D 1.334(13) . ? S81 O81B 1.382(11) . ? S81 O81C 1.397(13) . ? S81 O81A 1.468(13) . ? S81 C81 1.782(15) . ? C81 F81C 1.335(12) . ? C81 F81A 1.335(12) . ? C81 F81B 1.338(12) . ? S81A O81E 1.373(19) . ? S81A O81D 1.430(19) . ? S81A O81F 1.453(19) . ? S81A C81A 1.80(2) . ? C81A F81F 1.318(13) . ? C81A F81E 1.328(14) . ? C81A F81D 1.336(14) . ? S82 O82B 1.416(14) . ? S82 O82C 1.425(11) . ? S82 O82A 1.441(11) . ? S82 C82 1.800(15) . ? C82 F82A 1.319(12) . ? C82 F82C 1.325(11) . ? C82 F82B 1.336(13) . ? S82A O82E 1.251(16) . ? S82A O82D 1.451(17) . ? S82A O82F 1.583(16) . ? S82A C82A 1.804(16) . ? C82A F82E 1.310(13) . ? C82A F82F 1.328(13) . ? C82A F82D 1.332(13) . ? C90 Cl2 1.737(17) . ? C90 Cl1 1.761(15) . ? C91 Cl3 1.687(16) . ? C91 Cl4 1.705(17) . ? C92 Cl5 1.590(18) . ? C92 Cl6 1.802(18) . ? C93 Cl7 1.65(3) . ? C93 Cl8 1.70(4) . ? C93 Cl8' 1.72(4) . ? O96 O96 1.23(8) 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 P1 Pd1 P2 89.65(7) . . ? P1 Pd1 S1 92.37(6) . . ? P2 Pd1 S1 175.84(7) . . ? P1 Pd1 S2 174.65(7) . . ? P2 Pd1 S2 92.82(6) . . ? S1 Pd1 S2 84.88(6) . . ? P4 Pd2 P3 93.68(7) . . ? P4 Pd2 S2 175.49(7) . . ? P3 Pd2 S2 89.70(6) . . ? P4 Pd2 S1 91.21(7) . . ? P3 Pd2 S1 174.08(7) . . ? S2 Pd2 S1 85.24(6) . . ? C1 S1 Pd2 104.2(2) . . ? C1 S1 Pd1 109.2(2) . . ? Pd2 S1 Pd1 90.14(6) . . ? C12 S2 Pd2 102.5(2) . . ? C12 S2 Pd1 109.7(2) . . ? Pd2 S2 Pd1 90.30(6) . . ? C37 P1 C23 106.7(3) . . ? C37 P1 C31 106.7(2) . . ? C23 P1 C31 101.7(3) . . ? C37 P1 Pd1 112.66(17) . . ? C23 P1 Pd1 114.4(2) . . ? C31 P1 Pd1 113.81(18) . . ? C43 P2 C49 106.3(2) . . ? C43 P2 C25 106.8(3) . . ? C49 P2 C25 103.2(3) . . ? C43 P2 Pd1 112.73(16) . . ? C49 P2 Pd1 112.26(16) . . ? C25 P2 Pd1 114.7(2) . . ? C70 P3 C52 106.5(4) . . ? C70 P3 C76 106.9(2) . . ? C52 P3 C76 103.2(3) . . ? C70 P3 Pd2 110.39(17) . . ? C52 P3 Pd2 116.0(3) . . ? C76 P3 Pd2 113.13(18) . . ? C58 P4 C64 105.4(3) . . ? C58 P4 C50 104.2(3) . . ? C64 P4 C50 105.7(4) . . ? C58 P4 Pd2 111.83(19) . . ? C64 P4 Pd2 111.86(19) . . ? C50 P4 Pd2 116.9(3) . . ? C2 C1 S1 110.0(5) . . ? N3 C2 C1 111.3(7) . . ? C4 N3 C2 120.6(6) . . ? O4 C4 N3 121.6(7) . . ? O4 C4 N5 124.0(8) . . ? N3 C4 N5 114.3(8) . . ? C4 O4 Na 134.4(6) . . ? C4 N5 C11 129.8(8) . . ? C7 C6 C11 120.0 . . ? C8 C7 C6 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C6 120.0 . . ? C10 C11 N5 116.5(5) . . ? C6 C11 N5 123.4(5) . . ? C13 C12 S2 108.8(5) . . ? N14 C13 C12 110.2(6) . . ? C15 N14 C13 121.2(7) . . ? O15 C15 N14 120.2(7) . . ? O15 C15 N16 122.7(8) . . ? N14 C15 N16 117.0(8) . . ? C15 O15 Na 128.4(5) . . ? C15 N16 C22 123.9(7) . . ? C18 C17 C22 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C21 C22 N16 118.4(6) . . ? C17 C22 N16 121.6(6) . . ? C24 C23 P1 116.2(5) . . ? C25 C24 C23 113.2(6) . . ? C24 C25 P2 115.6(5) . . ? C27 C26 C31 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 P1 121.8(3) . . ? C26 C31 P1 118.2(3) . . ? C33 C32 C37 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 P1 118.8(3) . . ? C32 C37 P1 121.2(3) . . ? C39 C38 C43 120.0 . . ? C40 C39 C38 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 P2 118.5(3) . . ? C38 C43 P2 121.5(3) . . ? C45 C44 C49 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 P2 118.4(2) . . ? C44 C49 P2 121.3(2) . . ? C51 C50 P4 113.5(6) . . ? C52 C51 C50 112.7(8) . . ? C51 C52 P3 114.6(6) . . ? C54 C53 C58 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C57 C56 C55 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C53 120.0 . . ? C57 C58 P4 120.7(3) . . ? C53 C58 P4 119.1(3) . . ? C60 C59 C64 120.0 . . ? C59 C60 C61 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 P4 120.3(3) . . ? C59 C64 P4 119.7(3) . . ? C66 C65 C70 120.0 . . ? C65 C66 C67 120.0 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C70 C69 C68 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 P3 120.5(3) . . ? C65 C70 P3 119.5(3) . . ? C72 C71 C76 120.0 . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 P3 118.9(3) . . ? C71 C76 P3 121.1(3) . . ? O15 Na O82C 128.1(5) . . ? O15 Na O4 111.0(3) . . ? O82C Na O4 104.6(4) . . ? O15 Na O82F 112.9(5) . . ? O82C Na O82F 19.6(4) . . ? O4 Na O82F 124.2(5) . . ? O80A S80 O80C 116.5(8) . . ? O80A S80 O80B 113.3(8) . . ? O80C S80 O80B 112.3(8) . . ? O80A S80 C80 105.3(7) . . ? O80C S80 C80 104.5(7) . . ? O80B S80 C80 103.2(7) . . ? F80B C80 F80A 108.3(10) . . ? F80B C80 F80C 107.7(11) . . ? F80A C80 F80C 109.4(10) . . ? F80B C80 S80 108.6(8) . . ? F80A C80 S80 111.1(9) . . ? F80C C80 S80 111.4(9) . . ? O80D S80A O80F 114.6(11) . . ? O80D S80A O80E 114.6(12) . . ? O80F S80A O80E 114.5(11) . . ? O80D S80A C80A 104.0(10) . . ? O80F S80A C80A 104.3(10) . . ? O80E S80A C80A 102.9(9) . . ? F80E C80A F80F 109.2(13) . . ? F80E C80A F80D 106.8(13) . . ? F80F C80A F80D 106.2(13) . . ? F80E C80A S80A 111.1(12) . . ? F80F C80A S80A 111.0(12) . . ? F80D C80A S80A 112.2(12) . . ? O81B S81 O81C 119.7(9) . . ? O81B S81 O81A 111.5(9) . . ? O81C S81 O81A 108.7(8) . . ? O81B S81 C81 106.2(6) . . ? O81C S81 C81 106.8(9) . . ? O81A S81 C81 102.5(7) . . ? F81C C81 F81A 105.8(11) . . ? F81C C81 F81B 106.7(12) . . ? F81A C81 F81B 107.0(12) . . ? F81C C81 S81 111.4(10) . . ? F81A C81 S81 112.5(10) . . ? F81B C81 S81 113.0(10) . . ? O81E S81A O81D 116.8(14) . . ? O81E S81A O81F 114.6(13) . . ? O81D S81A O81F 111.7(13) . . ? O81E S81A C81A 105.8(11) . . ? O81D S81A C81A 103.8(11) . . ? O81F S81A C81A 102.0(10) . . ? F81F C81A F81E 108.8(14) . . ? F81F C81A F81D 107.9(14) . . ? F81E C81A F81D 108.3(14) . . ? F81F C81A S81A 110.6(12) . . ? F81E C81A S81A 111.1(13) . . ? F81D C81A S81A 110.1(12) . . ? O82B S82 O82C 115.9(8) . . ? O82B S82 O82A 115.5(9) . . ? O82C S82 O82A 113.8(9) . . ? O82B S82 C82 103.9(8) . . ? O82C S82 C82 102.1(6) . . ? O82A S82 C82 103.2(7) . . ? S82 O82C Na 143.9(8) . . ? F82A C82 F82C 108.7(11) . . ? F82A C82 F82B 109.6(12) . . ? F82C C82 F82B 110.4(11) . . ? F82A C82 S82 110.4(9) . . ? F82C C82 S82 109.9(10) . . ? F82B C82 S82 107.8(9) . . ? O82E S82A O82D 124.1(12) . . ? O82E S82A O82F 114.9(11) . . ? O82D S82A O82F 103.8(11) . . ? O82E S82A C82A 110.4(10) . . ? O82D S82A C82A 102.7(9) . . ? O82F S82A C82A 96.9(8) . . ? S82A O82F Na 124.7(10) . . ? F82E C82A F82F 109.7(12) . . ? F82E C82A F82D 107.9(13) . . ? F82F C82A F82D 107.7(12) . . ? F82E C82A S82A 112.7(11) . . ? F82F C82A S82A 109.1(11) . . ? F82D C82A S82A 109.7(11) . . ? Cl2 C90 Cl1 110.6(8) . . ? Cl3 C91 Cl4 117.0(10) . . ? Cl5 C92 Cl6 113.5(11) . . ? Cl7 C93 Cl8 119(2) . . ? Cl7 C93 Cl8' 118(2) . . ? Cl8 C93 Cl8' 36.4(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.694 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.098 #===END