# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Jose M. Vila' 'Alberto Fernandez' 'Jesus J. Fernandez' 'Margarita Lopez-Torres' 'Roberto Mosteiro' 'Antonio Suarez' 'Digna Vazquez-Garcia' _publ_contact_author_name 'Dr Jose M. Vila' _publ_contact_author_address ; Inorganic Chemistry University of Santiago Departamento de Química Inorgánica, Santiago de Compostela 15782 SPAIN ; _publ_contact_author_email 'QIDEPORT@USC.ES' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Nucleophilic addition of 1,3-dicarbonyl compounds as a route to functionalized cyclopalladated complexes with chelated 1,1-bis(diphenylphosphino)ethene ; data_2 _database_code_CSD 190097 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H42 F6 N O2 P3 Pd' _chemical_formula_weight 894.07 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' 'P' 'P' 0.1023 0.0942 '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 16.9482(3) _cell_length_b 17.54900(10) _cell_length_c 18.0086(3) _cell_angle_alpha 61.7800(10) _cell_angle_beta 64.0650(10) _cell_angle_gamma 66.1710(10) _cell_volume 4110.71(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8583 _exptl_absorpt_correction_T_max 0.9113 _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 ? _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 22085 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14094 _reflns_number_gt 9254 _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^)+(0.0864P)^2^+9.2605P] 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 14094 _refine_ls_number_parameters 973 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.089 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4008(5) 0.1274(5) 0.9766(5) 0.0475(16) Uani 1 1 d . . . C2 C 0.4661(5) 0.1019(5) 1.0150(6) 0.059(2) Uani 1 1 d . . . C3 C 0.4493(6) 0.0572(6) 1.1051(6) 0.064(2) Uani 1 1 d . . . H3 H 0.4941 0.0383 1.1311 0.077 Uiso 1 1 calc R . . C4 C 0.3652(6) 0.0412(6) 1.1556(5) 0.062(2) Uani 1 1 d . . . C5 C 0.2970(5) 0.0679(5) 1.1191(5) 0.0540(18) Uani 1 1 d . . . H5 H 0.2408 0.0559 1.1550 0.065 Uiso 1 1 calc R . . C6 C 0.3138(5) 0.1129(5) 1.0279(5) 0.0478(16) Uani 1 1 d . . . C7 C 0.6173(6) 0.0995(7) 0.9943(8) 0.096(3) Uani 1 1 d . . . H7A H 0.6693 0.1182 0.9473 0.115 Uiso 1 1 calc R . . H7B H 0.6333 0.0359 1.0241 0.115 Uiso 1 1 calc R . . H7C H 0.5966 0.1285 1.0356 0.115 Uiso 1 1 calc R . . C8 C 0.2721(8) -0.0178(9) 1.3035(6) 0.112(4) Uani 1 1 d . . . H8A H 0.2771 -0.0526 1.3621 0.134 Uiso 1 1 calc R . . H8B H 0.2491 -0.0478 1.2875 0.134 Uiso 1 1 calc R . . H8C H 0.2316 0.0397 1.3019 0.134 Uiso 1 1 calc R . . C9 C 0.4158(5) 0.1673(5) 0.8825(5) 0.0578(19) Uani 1 1 d . . . H9 H 0.4716 0.1792 0.8443 0.069 Uiso 1 1 calc R . . C10 C 0.3674(8) 0.2237(7) 0.7540(5) 0.091(3) Uani 1 1 d . . . H10 H 0.3111 0.2170 0.7576 0.109 Uiso 1 1 calc R . . C11 C 0.3483(13) 0.3165(8) 0.7127(7) 0.173(8) Uani 1 1 d . . . H11A H 0.3849 0.3386 0.7233 0.207 Uiso 1 1 calc R . . H11B H 0.2853 0.3411 0.7403 0.207 Uiso 1 1 calc R . . C12 C 0.3649(11) 0.3510(8) 0.6140(7) 0.144(6) Uani 1 1 d . . . H12A H 0.3077 0.3664 0.6040 0.172 Uiso 1 1 calc R . . H12B H 0.3844 0.4056 0.5874 0.172 Uiso 1 1 calc R . . C13 C 0.4303(13) 0.2918(11) 0.5682(7) 0.173(8) Uani 1 1 d . . . H13A H 0.4135 0.3070 0.5170 0.208 Uiso 1 1 calc R . . H13B H 0.4882 0.3057 0.5461 0.208 Uiso 1 1 calc R . . C14 C 0.4443(13) 0.2021(9) 0.6103(7) 0.159(7) Uani 1 1 d . . . H14A H 0.5070 0.1751 0.5841 0.190 Uiso 1 1 calc R . . H14B H 0.4069 0.1825 0.5980 0.190 Uiso 1 1 calc R . . C15 C 0.4253(11) 0.1644(8) 0.7116(7) 0.147(6) Uani 1 1 d . . . H15A H 0.4000 0.1136 0.7369 0.177 Uiso 1 1 calc R . . H15B H 0.4825 0.1427 0.7236 0.177 Uiso 1 1 calc R . . C16 C 0.0532(5) 0.1347(5) 0.9841(5) 0.0573(19) Uani 1 1 d . . . C17 C -0.0076(5) 0.0983(6) 0.9977(6) 0.072(2) Uani 1 1 d . . . H17A H -0.0319 0.0599 1.0540 0.086 Uiso 1 1 calc R . . H17B H -0.0267 0.1106 0.9511 0.086 Uiso 1 1 calc R . . C18 C 0.0994(5) 0.0183(6) 1.1510(5) 0.061(2) Uani 1 1 d . . . C19 C 0.1347(6) -0.0585(6) 1.1321(6) 0.076(2) Uani 1 1 d . . . H19 H 0.1590 -0.0551 1.0736 0.091 Uiso 1 1 calc R . . C20 C 0.1339(8) -0.1422(7) 1.2011(8) 0.098(3) Uani 1 1 d . . . H20 H 0.1573 -0.1946 1.1894 0.118 Uiso 1 1 calc R . . C21 C 0.0974(8) -0.1438(8) 1.2868(8) 0.113(4) Uani 1 1 d . . . H21 H 0.0967 -0.1987 1.3332 0.136 Uiso 1 1 calc R . . C22 C 0.0627(9) -0.0692(8) 1.3058(7) 0.112(4) Uani 1 1 d . . . H22 H 0.0388 -0.0729 1.3644 0.135 Uiso 1 1 calc R . . C23 C 0.0627(7) 0.0136(7) 1.2377(6) 0.085(3) Uani 1 1 d . . . H23 H 0.0381 0.0655 1.2505 0.102 Uiso 1 1 calc R . . C24 C 0.0336(5) 0.2100(5) 1.1059(5) 0.0566(19) Uani 1 1 d . . . C25 C 0.0719(7) 0.2512(8) 1.1252(7) 0.092(3) Uani 1 1 d . . . H25 H 0.1345 0.2382 1.1104 0.111 Uiso 1 1 calc R . . C26 C 0.0171(9) 0.3122(9) 1.1668(10) 0.127(5) Uani 1 1 d . . . H26 H 0.0426 0.3395 1.1812 0.152 Uiso 1 1 calc R . . C27 C -0.0749(9) 0.3320(8) 1.1866(8) 0.113(4) Uani 1 1 d . . . H27 H -0.1116 0.3743 1.2129 0.136 Uiso 1 1 calc R . . C28 C -0.1130(7) 0.2918(8) 1.1687(8) 0.100(3) Uani 1 1 d . . . H28 H -0.1757 0.3054 1.1834 0.120 Uiso 1 1 calc R . . C29 C -0.0590(6) 0.2301(7) 1.1284(7) 0.087(3) Uani 1 1 d . . . H29 H -0.0855 0.2018 1.1163 0.105 Uiso 1 1 calc R . . C30 C 0.1781(7) 0.0662(7) 0.8127(8) 0.093(3) Uani 1 1 d . . . H30 H 0.1906 0.0281 0.8659 0.111 Uiso 1 1 calc R . . C31 C 0.1947(9) 0.0312(10) 0.7500(11) 0.126(5) Uani 1 1 d . . . H31 H 0.2181 -0.0297 0.7613 0.152 Uiso 1 1 calc R . . C32 C 0.1762(11) 0.0871(13) 0.6726(10) 0.135(5) Uani 1 1 d . . . H32 H 0.1834 0.0637 0.6326 0.162 Uiso 1 1 calc R . . C33 C 0.1472(12) 0.1771(13) 0.6528(9) 0.150(6) Uani 1 1 d . . . H33 H 0.1393 0.2150 0.5977 0.180 Uiso 1 1 calc R . . C34 C 0.1292(9) 0.2130(8) 0.7162(7) 0.107(4) Uani 1 1 d . . . H34 H 0.1077 0.2742 0.7038 0.128 Uiso 1 1 calc R . . C35 C 0.1438(6) 0.1558(6) 0.7964(6) 0.067(2) Uani 1 1 d . . . C36 C 0.0597(5) 0.3108(5) 0.8524(5) 0.060(2) Uani 1 1 d . . . C37 C -0.0241(8) 0.3364(8) 0.8454(9) 0.115(4) Uani 1 1 d . . . H37 H -0.0497 0.2941 0.8533 0.138 Uiso 1 1 calc R . . C38 C -0.0725(9) 0.4256(9) 0.8266(10) 0.127(5) Uani 1 1 d . . . H38 H -0.1308 0.4410 0.8237 0.152 Uiso 1 1 calc R . . C39 C -0.0407(10) 0.4865(9) 0.8133(11) 0.141(6) Uani 1 1 d . . . H39 H -0.0725 0.5461 0.7960 0.170 Uiso 1 1 calc R . . C40 C 0.0405(11) 0.4625(10) 0.8248(16) 0.205(10) Uani 1 1 d . . . H40 H 0.0625 0.5057 0.8204 0.246 Uiso 1 1 calc R . . C41 C 0.0932(8) 0.3732(7) 0.8436(10) 0.121(5) Uani 1 1 d . . . H41 H 0.1499 0.3580 0.8497 0.145 Uiso 1 1 calc R . . C42 C 0.3387(5) 0.7528(5) 0.6109(5) 0.059(2) Uani 1 1 d . . . C43 C 0.2637(6) 0.7798(6) 0.5824(6) 0.073(2) Uani 1 1 d . . . C44 C 0.2277(6) 0.7186(7) 0.5897(5) 0.069(2) Uani 1 1 d . . . H44 H 0.1787 0.7371 0.5694 0.083 Uiso 1 1 calc R . . C45 C 0.2651(6) 0.6293(7) 0.6276(5) 0.067(2) Uani 1 1 d . . . C46 C 0.3388(5) 0.6001(6) 0.6593(5) 0.063(2) Uani 1 1 d . . . H46 H 0.3624 0.5394 0.6858 0.075 Uiso 1 1 calc R . . C47 C 0.3757(5) 0.6618(5) 0.6509(5) 0.0548(18) Uani 1 1 d . . . C48 C 0.1417(7) 0.9052(9) 0.5389(10) 0.141(6) Uani 1 1 d . . . H48A H 0.1286 0.9692 0.5133 0.169 Uiso 1 1 calc R . . H48B H 0.0986 0.8873 0.5965 0.169 Uiso 1 1 calc R . . H48C H 0.1380 0.8826 0.5017 0.169 Uiso 1 1 calc R . . C49 C 0.1679(8) 0.5833(9) 0.5990(9) 0.126(5) Uani 1 1 d . . . H49A H 0.1542 0.5297 0.6114 0.152 Uiso 1 1 calc R . . H49B H 0.1899 0.6128 0.5361 0.152 Uiso 1 1 calc R . . H49C H 0.1141 0.6222 0.6234 0.152 Uiso 1 1 calc R . . C50 C 0.3810(6) 0.8129(6) 0.6012(6) 0.078(3) Uani 1 1 d . . . H50 H 0.3576 0.8741 0.5768 0.094 Uiso 1 1 calc R . . C51 C 0.4939(8) 0.8469(7) 0.6198(10) 0.110(4) Uani 1 1 d . . . H51 H 0.4706 0.9015 0.5754 0.132 Uiso 1 1 calc R . . C52 C 0.5901(7) 0.8350(7) 0.5756(6) 0.087(3) Uani 1 1 d . . . H52A H 0.6020 0.8397 0.5159 0.104 Uiso 1 1 calc R . . H52B H 0.6207 0.7751 0.6062 0.104 Uiso 1 1 calc R . . C53 C 0.6303(10) 0.9000(9) 0.5701(10) 0.128(5) Uani 1 1 d . . . H53A H 0.6943 0.8731 0.5635 0.154 Uiso 1 1 calc R . . H53B H 0.6251 0.9524 0.5172 0.154 Uiso 1 1 calc R . . C54 C 0.5913(15) 0.9274(15) 0.6423(15) 0.201(10) Uani 1 1 d . . . H54A H 0.6057 0.9835 0.6225 0.242 Uiso 1 1 calc R . . H54B H 0.6220 0.8841 0.6860 0.242 Uiso 1 1 calc R . . C55 C 0.4941(13) 0.9402(9) 0.6881(11) 0.147(6) Uani 1 1 d . . . H55A H 0.4632 1.0002 0.6578 0.177 Uiso 1 1 calc R . . H55B H 0.4829 0.9350 0.7478 0.177 Uiso 1 1 calc R . . C56 C 0.4538(11) 0.8729(11) 0.6932(10) 0.147(6) Uani 1 1 d . . . H56A H 0.4596 0.8201 0.7456 0.176 Uiso 1 1 calc R . . H56B H 0.3897 0.8991 0.6999 0.176 Uiso 1 1 calc R . . C57 C 0.5604(5) 0.4980(5) 0.8278(5) 0.0546(18) Uani 1 1 d . . . C58 C 0.5585(6) 0.4580(6) 0.9101(6) 0.076(3) Uani 1 1 d . . . H58A H 0.5170 0.4239 0.9506 0.091 Uiso 1 1 calc R . . H58B H 0.5987 0.4636 0.9286 0.091 Uiso 1 1 calc R . . C59 C 0.7153(6) 0.5401(5) 0.6736(5) 0.0588(19) Uani 1 1 d . . . C60 C 0.7469(7) 0.5867(8) 0.5862(6) 0.095(3) Uani 1 1 d . . . H60 H 0.7140 0.6441 0.5611 0.114 Uiso 1 1 calc R . . C61 C 0.8283(10) 0.5497(11) 0.5334(9) 0.126(5) Uani 1 1 d . . . H61 H 0.8506 0.5832 0.4740 0.151 Uiso 1 1 calc R . . C62 C 0.8748(9) 0.4656(12) 0.5684(10) 0.118(4) Uani 1 1 d . . . H62 H 0.9286 0.4409 0.5326 0.142 Uiso 1 1 calc R . . C63 C 0.8440(8) 0.4170(9) 0.6546(11) 0.118(4) Uani 1 1 d . . . H63 H 0.8760 0.3586 0.6782 0.142 Uiso 1 1 calc R . . C64 C 0.7623(7) 0.4553(7) 0.7094(8) 0.093(3) Uani 1 1 d . . . H64 H 0.7411 0.4226 0.7694 0.111 Uiso 1 1 calc R . . C65 C 0.6381(5) 0.6383(5) 0.7933(4) 0.0493(17) Uani 1 1 d . . . C66 C 0.5677(6) 0.6713(5) 0.8575(5) 0.061(2) Uani 1 1 d . . . H66 H 0.5098 0.6649 0.8744 0.074 Uiso 1 1 calc R . . C67 C 0.5841(6) 0.7129(6) 0.8955(6) 0.069(2) Uani 1 1 d . . . H67 H 0.5377 0.7334 0.9392 0.083 Uiso 1 1 calc R . . C68 C 0.6702(7) 0.7242(6) 0.8685(6) 0.071(2) Uani 1 1 d . . . H68 H 0.6813 0.7525 0.8942 0.085 Uiso 1 1 calc R . . C69 C 0.7378(6) 0.6944(6) 0.8053(6) 0.071(2) Uani 1 1 d . . . H69 H 0.7950 0.7032 0.7869 0.085 Uiso 1 1 calc R . . C70 C 0.7226(5) 0.6511(5) 0.7677(5) 0.059(2) Uani 1 1 d . . . H70 H 0.7698 0.6302 0.7247 0.071 Uiso 1 1 calc R . . C71 C 0.5529(5) 0.4145(5) 0.7240(5) 0.0551(18) Uani 1 1 d . . . C72 C 0.5908(6) 0.3287(6) 0.7712(6) 0.077(2) Uani 1 1 d . . . H72 H 0.5830 0.3130 0.8306 0.092 Uiso 1 1 calc R . . C73 C 0.6408(7) 0.2645(7) 0.7314(8) 0.090(3) Uani 1 1 d . . . H73 H 0.6659 0.2063 0.7636 0.108 Uiso 1 1 calc R . . C74 C 0.6517(8) 0.2901(9) 0.6429(9) 0.106(4) Uani 1 1 d . . . H74 H 0.6849 0.2487 0.6149 0.127 Uiso 1 1 calc R . . C75 C 0.6144(8) 0.3753(8) 0.5962(7) 0.099(3) Uani 1 1 d . . . H75 H 0.6227 0.3916 0.5365 0.119 Uiso 1 1 calc R . . C76 C 0.5648(6) 0.4373(6) 0.6359(6) 0.074(2) Uani 1 1 d . . . H76 H 0.5390 0.4950 0.6034 0.088 Uiso 1 1 calc R . . C77 C 0.3621(6) 0.3947(6) 0.8705(5) 0.063(2) Uani 1 1 d . . . C78 C 0.3866(5) 0.4686(5) 0.8567(5) 0.0534(18) Uani 1 1 d . . . H78 H 0.4421 0.4797 0.8167 0.064 Uiso 1 1 calc R . . C79 C 0.3290(6) 0.5244(6) 0.9019(6) 0.078(3) Uani 1 1 d . . . H79 H 0.3462 0.5727 0.8931 0.094 Uiso 1 1 calc R . . C80 C 0.2213(7) 0.4379(7) 0.9732(7) 0.087(3) Uani 1 1 d . . . H80 H 0.1653 0.4275 1.0125 0.104 Uiso 1 1 calc R . . C81 C 0.2456(7) 0.5104(7) 0.9602(7) 0.094(3) Uani 1 1 d . . . H81 H 0.2064 0.5491 0.9902 0.113 Uiso 1 1 calc R . . C82 C 0.2780(6) 0.3819(7) 0.9297(6) 0.076(3) Uani 1 1 d . . . H82 H 0.2603 0.3334 0.9395 0.091 Uiso 1 1 calc R . . N1 N 0.3526(5) 0.1865(4) 0.8514(4) 0.0591(16) Uani 1 1 d . . . N2 N 0.4515(5) 0.7839(4) 0.6257(5) 0.0677(18) Uani 1 1 d . . . O1 O 0.5470(4) 0.1228(4) 0.9585(4) 0.0817(18) Uani 1 1 d . . . O2 O 0.3568(5) -0.0071(5) 1.2442(4) 0.092(2) Uani 1 1 d . . . O3 O 0.2306(5) 0.8706(5) 0.5469(5) 0.109(2) Uani 1 1 d . . . O4 O 0.2362(4) 0.5611(5) 0.6381(5) 0.0883(19) Uani 1 1 d . . . F1 F -0.0122(12) 0.1945(14) 1.4530(11) 0.359(12) Uani 1 1 d . . . F2 F 0.0897(6) 0.1363(7) 1.5130(5) 0.186(4) Uani 1 1 d . . . F3 F 0.0075(11) 0.2647(9) 1.4991(7) 0.283(8) Uani 1 1 d . . . F4 F 0.1512(8) 0.2464(8) 1.4254(8) 0.218(5) Uani 1 1 d . . . F5 F 0.0534(6) 0.3023(8) 1.3559(6) 0.230(6) Uani 1 1 d . . . F6 F 0.1379(10) 0.1725(7) 1.3691(7) 0.232(6) Uani 1 1 d . . . F7 F 0.2347(10) 0.6711(9) 1.0360(8) 0.376(12) Uani 1 1 d D . . F11 F 0.3556(6) 0.6991(8) 0.9145(8) 0.290(8) Uani 1 1 d D . . F10 F 0.3176(11) 0.8449(7) 0.9028(8) 0.360(13) Uani 1 1 d D . . F9 F 0.2159(7) 0.7877(8) 0.9056(9) 0.326(10) Uani 1 1 d D . . F8 F 0.1925(8) 0.8182(10) 1.0251(10) 0.394(14) Uani 1 1 d D . . F12 F 0.3331(7) 0.7324(5) 1.0337(7) 0.234(6) Uani 1 1 d D . . P1 P 0.10446(13) 0.12484(13) 1.05915(13) 0.0519(5) Uani 1 1 d . . . P2 P 0.12665(14) 0.19627(14) 0.87982(14) 0.0560(5) Uani 1 1 d . . . P3 P 0.0683(2) 0.2200(3) 1.4338(2) 0.1203(13) Uani 1 1 d . . . P4 P 0.49068(14) 0.49872(13) 0.77417(12) 0.0507(5) Uani 1 1 d . . . P5 P 0.60918(14) 0.59096(13) 0.74096(12) 0.0519(5) Uani 1 1 d . . . P6 P 0.2721(2) 0.7604(2) 0.9700(3) 0.1158(13) Uani 1 1 d D . . Pd1 Pd 0.23379(4) 0.15550(4) 0.95173(3) 0.04694(17) Uani 1 1 d . . . Pd2 Pd 0.48244(4) 0.64301(4) 0.68728(4) 0.04988(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(4) 0.046(4) 0.055(4) -0.021(3) -0.014(4) -0.014(3) C2 0.048(4) 0.061(5) 0.080(6) -0.038(4) -0.016(4) -0.014(4) C3 0.060(5) 0.070(6) 0.084(6) -0.037(5) -0.038(5) -0.009(4) C4 0.072(6) 0.063(5) 0.064(5) -0.025(4) -0.028(5) -0.017(4) C5 0.053(4) 0.057(5) 0.053(4) -0.017(4) -0.018(4) -0.015(4) C6 0.051(4) 0.044(4) 0.050(4) -0.019(3) -0.016(3) -0.010(3) C7 0.056(5) 0.107(8) 0.154(10) -0.060(7) -0.047(6) -0.016(5) C8 0.127(10) 0.145(11) 0.053(6) -0.004(6) -0.030(7) -0.061(9) C9 0.053(5) 0.056(5) 0.057(5) -0.023(4) -0.001(4) -0.021(4) C10 0.122(9) 0.092(8) 0.043(5) -0.016(5) -0.008(5) -0.041(7) C11 0.31(2) 0.073(8) 0.053(6) -0.021(6) -0.063(10) 0.028(10) C12 0.217(16) 0.090(9) 0.057(6) -0.015(6) -0.039(8) 0.007(9) C13 0.27(2) 0.148(14) 0.051(7) -0.034(8) -0.037(10) -0.017(14) C14 0.28(2) 0.084(9) 0.065(7) -0.027(6) -0.055(10) 0.007(10) C15 0.259(18) 0.075(8) 0.060(6) -0.032(6) -0.061(9) 0.025(9) C16 0.054(5) 0.059(5) 0.060(5) -0.018(4) -0.018(4) -0.018(4) C17 0.059(5) 0.079(6) 0.089(6) -0.033(5) -0.023(5) -0.025(5) C18 0.045(4) 0.063(5) 0.064(5) -0.015(4) -0.009(4) -0.022(4) C19 0.069(6) 0.070(6) 0.072(6) -0.015(5) -0.021(5) -0.015(5) C20 0.101(8) 0.064(7) 0.113(9) -0.018(6) -0.032(7) -0.024(6) C21 0.100(9) 0.085(9) 0.092(9) 0.005(7) -0.005(7) -0.038(7) C22 0.128(10) 0.086(8) 0.075(7) -0.018(6) 0.008(7) -0.039(8) C23 0.093(7) 0.076(7) 0.055(5) -0.011(5) 0.001(5) -0.034(6) C24 0.055(5) 0.059(5) 0.055(4) -0.021(4) -0.015(4) -0.015(4) C25 0.079(7) 0.114(9) 0.105(8) -0.064(7) -0.004(6) -0.040(6) C26 0.094(9) 0.152(12) 0.183(13) -0.125(11) -0.003(9) -0.041(8) C27 0.107(10) 0.103(9) 0.126(10) -0.075(8) 0.009(8) -0.032(8) C28 0.060(6) 0.112(9) 0.120(9) -0.060(8) -0.012(6) -0.008(6) C29 0.059(6) 0.100(8) 0.125(8) -0.064(7) -0.030(6) -0.009(5) C30 0.093(7) 0.087(8) 0.109(8) -0.060(7) -0.034(6) 0.001(6) C31 0.114(10) 0.135(12) 0.152(13) -0.098(11) -0.029(10) -0.007(9) C32 0.164(14) 0.176(16) 0.112(11) -0.086(12) -0.038(10) -0.048(13) C33 0.220(18) 0.173(16) 0.102(10) -0.045(10) -0.080(11) -0.061(14) C34 0.157(11) 0.109(9) 0.082(7) -0.032(6) -0.064(8) -0.031(8) C35 0.062(5) 0.084(7) 0.065(5) -0.029(5) -0.020(4) -0.023(5) C36 0.059(5) 0.061(5) 0.055(5) -0.016(4) -0.020(4) -0.013(4) C37 0.093(8) 0.077(8) 0.190(13) -0.022(8) -0.088(9) -0.016(6) C38 0.098(9) 0.089(9) 0.182(14) -0.026(9) -0.082(10) 0.002(8) C39 0.104(11) 0.078(9) 0.216(17) -0.035(10) -0.066(11) -0.001(8) C40 0.126(13) 0.086(10) 0.41(3) -0.111(15) -0.095(17) 0.001(9) C41 0.081(7) 0.066(7) 0.229(15) -0.061(8) -0.068(9) 0.001(6) C42 0.053(5) 0.058(5) 0.053(4) -0.013(4) -0.018(4) -0.011(4) C43 0.059(5) 0.065(6) 0.073(6) -0.011(5) -0.027(5) -0.004(4) C44 0.054(5) 0.093(7) 0.056(5) -0.028(5) -0.025(4) -0.003(5) C45 0.062(5) 0.086(7) 0.061(5) -0.039(5) -0.012(4) -0.017(5) C46 0.058(5) 0.073(6) 0.063(5) -0.026(4) -0.022(4) -0.017(4) C47 0.049(4) 0.064(5) 0.050(4) -0.024(4) -0.012(4) -0.012(4) C48 0.069(7) 0.127(11) 0.162(12) -0.014(9) -0.051(8) 0.006(7) C49 0.097(8) 0.162(13) 0.182(13) -0.083(10) -0.082(9) -0.020(8) C50 0.071(6) 0.055(5) 0.086(6) -0.013(5) -0.027(5) -0.008(5) C51 0.108(9) 0.064(7) 0.174(12) -0.060(8) -0.035(9) -0.024(6) C52 0.100(8) 0.095(7) 0.074(6) -0.006(5) -0.036(6) -0.052(6) C53 0.142(12) 0.099(9) 0.169(13) -0.010(9) -0.085(11) -0.060(9) C54 0.22(2) 0.28(3) 0.24(2) -0.15(2) -0.045(18) -0.14(2) C55 0.219(18) 0.101(10) 0.183(15) -0.066(10) -0.094(15) -0.042(12) C56 0.155(13) 0.190(16) 0.153(12) -0.111(12) -0.014(11) -0.073(12) C57 0.062(5) 0.051(4) 0.054(4) -0.014(4) -0.023(4) -0.018(4) C58 0.088(7) 0.067(6) 0.070(6) -0.003(4) -0.037(5) -0.029(5) C59 0.068(5) 0.058(5) 0.056(5) -0.022(4) -0.018(4) -0.021(4) C60 0.089(7) 0.106(8) 0.063(6) -0.033(6) -0.008(6) -0.013(6) C61 0.124(11) 0.139(13) 0.086(8) -0.046(9) -0.010(8) -0.023(10) C62 0.089(9) 0.149(13) 0.126(11) -0.091(11) 0.007(9) -0.032(9) C63 0.075(8) 0.087(8) 0.176(14) -0.066(9) -0.026(9) 0.005(6) C64 0.076(7) 0.083(8) 0.104(8) -0.034(6) -0.017(6) -0.017(6) C65 0.058(5) 0.044(4) 0.045(4) -0.011(3) -0.020(4) -0.015(3) C66 0.061(5) 0.058(5) 0.063(5) -0.019(4) -0.019(4) -0.017(4) C67 0.075(6) 0.068(6) 0.068(5) -0.036(5) -0.014(5) -0.017(5) C68 0.092(7) 0.059(5) 0.077(6) -0.025(5) -0.038(5) -0.020(5) C69 0.066(6) 0.075(6) 0.083(6) -0.021(5) -0.031(5) -0.027(5) C70 0.052(5) 0.071(5) 0.062(5) -0.027(4) -0.014(4) -0.023(4) C71 0.056(5) 0.055(5) 0.056(4) -0.020(4) -0.015(4) -0.018(4) C72 0.074(6) 0.075(6) 0.078(6) -0.035(5) -0.021(5) -0.010(5) C73 0.086(7) 0.071(7) 0.115(9) -0.043(6) -0.032(7) -0.007(5) C74 0.104(9) 0.111(10) 0.110(9) -0.075(8) 0.000(7) -0.028(7) C75 0.125(10) 0.098(9) 0.071(6) -0.043(6) -0.015(7) -0.024(7) C76 0.074(6) 0.078(6) 0.058(5) -0.027(5) -0.005(5) -0.023(5) C77 0.074(6) 0.065(5) 0.066(5) -0.023(4) -0.027(5) -0.028(4) C78 0.050(4) 0.052(5) 0.054(4) -0.014(4) -0.015(4) -0.016(4) C79 0.069(6) 0.072(6) 0.092(7) -0.038(5) -0.003(5) -0.029(5) C80 0.059(6) 0.089(7) 0.089(7) -0.028(6) -0.004(5) -0.024(5) C81 0.071(6) 0.097(8) 0.105(8) -0.059(7) 0.010(6) -0.025(6) C82 0.072(6) 0.080(6) 0.077(6) -0.020(5) -0.010(5) -0.045(5) N1 0.065(4) 0.065(4) 0.044(3) -0.016(3) -0.012(3) -0.023(3) N2 0.069(5) 0.053(4) 0.082(5) -0.020(4) -0.027(4) -0.016(4) O1 0.055(3) 0.104(5) 0.102(5) -0.045(4) -0.017(3) -0.032(3) O2 0.099(5) 0.117(6) 0.059(4) -0.014(4) -0.042(4) -0.028(4) O3 0.085(5) 0.085(5) 0.130(6) -0.001(4) -0.058(5) -0.014(4) O4 0.077(4) 0.102(5) 0.122(5) -0.056(4) -0.045(4) -0.019(4) F1 0.330(18) 0.50(3) 0.321(18) 0.058(18) -0.187(16) -0.32(2) F2 0.148(7) 0.182(9) 0.125(6) 0.029(6) -0.045(6) -0.046(7) F3 0.276(16) 0.220(13) 0.148(9) -0.060(9) 0.032(10) 0.013(11) F4 0.182(10) 0.242(13) 0.216(10) -0.022(9) -0.064(9) -0.111(9) F5 0.145(8) 0.225(11) 0.113(6) 0.035(6) -0.028(6) 0.015(7) F6 0.301(15) 0.171(10) 0.153(8) -0.075(7) -0.034(10) -0.013(10) F7 0.44(3) 0.43(3) 0.37(2) -0.11(2) -0.05(2) -0.33(3) F11 0.174(11) 0.327(18) 0.45(2) -0.275(18) -0.108(13) 0.035(11) F10 0.65(4) 0.232(14) 0.40(2) 0.046(14) -0.39(2) -0.23(2) F9 0.281(15) 0.320(18) 0.61(3) -0.28(2) -0.328(19) 0.056(13) F8 0.272(17) 0.50(3) 0.60(3) -0.48(3) -0.21(2) 0.147(18) F12 0.315(14) 0.104(7) 0.383(16) -0.046(8) -0.252(14) -0.035(8) P1 0.0477(11) 0.0547(12) 0.0528(11) -0.0164(9) -0.0153(9) -0.0159(9) P2 0.0573(12) 0.0591(13) 0.0582(12) -0.0181(10) -0.0254(10) -0.0157(10) P3 0.075(2) 0.149(3) 0.078(2) 0.001(2) -0.0209(17) -0.028(2) P4 0.0559(12) 0.0520(11) 0.0484(10) -0.0160(9) -0.0155(9) -0.0205(9) P5 0.0562(12) 0.0541(12) 0.0490(11) -0.0127(9) -0.0197(9) -0.0201(10) P6 0.0664(17) 0.096(2) 0.219(4) -0.089(3) -0.057(2) 0.0024(16) Pd1 0.0481(3) 0.0504(3) 0.0454(3) -0.0145(2) -0.0162(3) -0.0162(3) Pd2 0.0554(4) 0.0499(3) 0.0483(3) -0.0145(3) -0.0193(3) -0.0167(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.370(10) . ? C1 C6 1.408(9) . ? C1 C9 1.439(10) . ? C2 O1 1.372(9) . ? C2 C3 1.380(11) . ? C3 C4 1.374(11) . ? C4 O2 1.380(10) . ? C4 C5 1.386(10) . ? C5 C6 1.397(10) . ? C6 Pd1 2.029(7) . ? C7 O1 1.425(10) . ? C8 O2 1.386(12) . ? C9 N1 1.277(10) . ? C10 C15 1.380(14) . ? C10 C11 1.395(14) . ? C10 N1 1.493(10) . ? C11 C12 1.512(13) . ? C12 C13 1.438(17) . ? C13 C14 1.354(17) . ? C14 C15 1.544(14) . ? C16 C17 1.301(10) . ? C16 P1 1.816(8) . ? C16 P2 1.834(8) . ? C18 C19 1.376(12) . ? C18 C23 1.380(12) . ? C18 P1 1.822(8) . ? C19 C20 1.405(13) . ? C20 C21 1.380(16) . ? C21 C22 1.342(16) . ? C22 C23 1.389(14) . ? C24 C25 1.370(11) . ? C24 C29 1.371(11) . ? C24 P1 1.800(8) . ? C25 C26 1.385(14) . ? C26 C27 1.368(16) . ? C27 C28 1.334(15) . ? C28 C29 1.379(14) . ? C30 C35 1.368(13) . ? C30 C31 1.404(15) . ? C31 C32 1.357(19) . ? C32 C33 1.36(2) . ? C33 C34 1.418(17) . ? C34 C35 1.377(13) . ? C35 P2 1.818(9) . ? C36 C41 1.344(12) . ? C36 C37 1.350(12) . ? C36 P2 1.811(8) . ? C37 C38 1.395(16) . ? C38 C39 1.265(16) . ? C39 C40 1.348(19) . ? C40 C41 1.414(17) . ? C42 C43 1.400(11) . ? C42 C47 1.401(11) . ? C42 C50 1.408(12) . ? C43 C44 1.366(12) . ? C43 O3 1.376(11) . ? C44 C45 1.373(12) . ? C45 O4 1.373(10) . ? C45 C46 1.407(11) . ? C46 C47 1.377(10) . ? C47 Pd2 2.039(7) . ? C48 O3 1.424(12) . ? C49 O4 1.441(11) . ? C50 N2 1.280(11) . ? C51 C56 1.397(16) . ? C51 C52 1.442(14) . ? C51 N2 1.487(11) . ? C52 C53 1.495(14) . ? C53 C54 1.39(2) . ? C54 C55 1.46(2) . ? C55 C56 1.538(17) . ? C57 C58 1.297(10) . ? C57 P4 1.818(7) . ? C57 P5 1.827(7) . ? C59 C60 1.354(12) . ? C59 C64 1.360(12) . ? C59 P5 1.822(8) . ? C60 C61 1.394(16) . ? C61 C62 1.345(18) . ? C62 C63 1.345(18) . ? C63 C64 1.423(15) . ? C65 C70 1.377(10) . ? C65 C66 1.401(10) . ? C65 P5 1.815(7) . ? C66 C67 1.371(11) . ? C67 C68 1.389(12) . ? C68 C69 1.350(12) . ? C69 C70 1.378(11) . ? C71 C72 1.374(11) . ? C71 C76 1.380(11) . ? C71 P4 1.812(8) . ? C72 C73 1.401(13) . ? C73 C74 1.381(15) . ? C74 C75 1.362(15) . ? C75 C76 1.369(13) . ? C77 C82 1.386(11) . ? C77 C78 1.400(10) . ? C78 C79 1.363(11) . ? C78 P4 1.821(8) . ? C79 C81 1.379(12) . ? C80 C82 1.345(13) . ? C80 C81 1.377(13) . ? N1 Pd1 2.094(6) . ? N2 Pd2 2.118(7) . ? F1 P3 1.454(10) . ? F2 P3 1.538(8) . ? F3 P3 1.490(12) . ? F4 P3 1.576(10) . ? F5 P3 1.488(8) . ? F6 P3 1.537(11) . ? F7 P6 1.629(9) . ? F11 P6 1.645(8) . ? F10 P6 1.634(9) . ? F9 P6 1.597(8) . ? F8 P6 1.584(8) . ? F12 P6 1.650(7) . ? P1 Pd1 2.257(2) . ? P2 Pd1 2.370(2) . ? P4 Pd2 2.245(2) . ? P5 Pd2 2.404(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 C2 C1 C6 121.3(7) . . ? C2 C1 C9 123.6(7) . . ? C6 C1 C9 115.0(6) . . ? C1 C2 O1 116.0(7) . . ? C1 C2 C3 120.5(7) . . ? O1 C2 C3 123.5(7) . . ? C4 C3 C2 118.6(7) . . ? C3 C4 O2 113.9(7) . . ? C3 C4 C5 122.3(7) . . ? O2 C4 C5 123.7(8) . . ? C4 C5 C6 119.2(7) . . ? C5 C6 C1 117.9(7) . . ? C5 C6 Pd1 130.0(6) . . ? C1 C6 Pd1 111.9(5) . . ? N1 C9 C1 120.1(7) . . ? C15 C10 C11 124.7(9) . . ? C15 C10 N1 114.4(9) . . ? C11 C10 N1 117.3(8) . . ? C10 C11 C12 115.3(10) . . ? C13 C12 C11 116.6(11) . . ? C14 C13 C12 120.6(12) . . ? C13 C14 C15 117.9(11) . . ? C10 C15 C14 115.4(10) . . ? C17 C16 P1 131.0(7) . . ? C17 C16 P2 129.9(7) . . ? P1 C16 P2 98.4(4) . . ? C19 C18 C23 120.1(8) . . ? C19 C18 P1 118.4(7) . . ? C23 C18 P1 121.4(7) . . ? C18 C19 C20 120.2(10) . . ? C21 C20 C19 117.7(11) . . ? C22 C21 C20 122.5(11) . . ? C21 C22 C23 119.9(11) . . ? C18 C23 C22 119.6(10) . . ? C25 C24 C29 119.2(8) . . ? C25 C24 P1 119.7(7) . . ? C29 C24 P1 120.9(7) . . ? C24 C25 C26 119.9(10) . . ? C27 C26 C25 119.4(11) . . ? C28 C27 C26 121.3(11) . . ? C27 C28 C29 119.6(10) . . ? C24 C29 C28 120.6(9) . . ? C35 C30 C31 120.6(12) . . ? C32 C31 C30 119.5(13) . . ? C31 C32 C33 120.8(13) . . ? C32 C33 C34 120.0(13) . . ? C35 C34 C33 119.0(12) . . ? C30 C35 C34 119.9(9) . . ? C30 C35 P2 118.0(7) . . ? C34 C35 P2 122.0(8) . . ? C41 C36 C37 118.0(9) . . ? C41 C36 P2 118.0(7) . . ? C37 C36 P2 123.8(7) . . ? C36 C37 C38 120.5(11) . . ? C39 C38 C37 122.8(13) . . ? C38 C39 C40 118.0(14) . . ? C39 C40 C41 121.7(14) . . ? C36 C41 C40 118.6(11) . . ? C43 C42 C47 119.8(8) . . ? C43 C42 C50 123.5(8) . . ? C47 C42 C50 116.7(7) . . ? C44 C43 O3 123.7(8) . . ? C44 C43 C42 121.1(8) . . ? O3 C43 C42 115.2(9) . . ? C43 C44 C45 119.0(8) . . ? C44 C45 O4 124.9(8) . . ? C44 C45 C46 121.2(8) . . ? O4 C45 C46 113.8(8) . . ? C47 C46 C45 119.8(8) . . ? C46 C47 C42 119.0(7) . . ? C46 C47 Pd2 129.9(6) . . ? C42 C47 Pd2 111.0(6) . . ? N2 C50 C42 120.4(8) . . ? C56 C51 C52 120.4(11) . . ? C56 C51 N2 113.2(11) . . ? C52 C51 N2 116.6(9) . . ? C51 C52 C53 115.2(11) . . ? C54 C53 C52 115.4(13) . . ? C53 C54 C55 120.7(14) . . ? C54 C55 C56 113.5(13) . . ? C51 C56 C55 114.7(12) . . ? C58 C57 P4 129.2(7) . . ? C58 C57 P5 130.1(6) . . ? P4 C57 P5 98.9(4) . . ? C60 C59 C64 119.4(9) . . ? C60 C59 P5 119.6(7) . . ? C64 C59 P5 121.0(7) . . ? C59 C60 C61 120.7(11) . . ? C62 C61 C60 120.1(12) . . ? C63 C62 C61 120.5(12) . . ? C62 C63 C64 119.6(12) . . ? C59 C64 C63 119.5(11) . . ? C70 C65 C66 118.6(7) . . ? C70 C65 P5 123.8(6) . . ? C66 C65 P5 117.3(6) . . ? C67 C66 C65 120.2(8) . . ? C66 C67 C68 119.7(8) . . ? C69 C68 C67 120.3(8) . . ? C68 C69 C70 120.4(8) . . ? C69 C70 C65 120.7(8) . . ? C72 C71 C76 119.0(8) . . ? C72 C71 P4 121.4(6) . . ? C76 C71 P4 119.5(6) . . ? C71 C72 C73 121.1(9) . . ? C74 C73 C72 118.1(10) . . ? C75 C74 C73 120.6(10) . . ? C74 C75 C76 120.9(10) . . ? C75 C76 C71 120.2(10) . . ? C82 C77 C78 117.7(8) . . ? C79 C78 C77 120.0(8) . . ? C79 C78 P4 117.5(6) . . ? C77 C78 P4 122.4(6) . . ? C78 C79 C81 121.1(8) . . ? C82 C80 C81 120.6(9) . . ? C79 C81 C80 118.8(9) . . ? C80 C82 C77 121.8(8) . . ? C9 N1 C10 121.4(7) . . ? C9 N1 Pd1 112.0(5) . . ? C10 N1 Pd1 126.6(6) . . ? C50 N2 C51 120.8(8) . . ? C50 N2 Pd2 111.0(6) . . ? C51 N2 Pd2 127.8(7) . . ? C2 O1 C7 118.9(7) . . ? C4 O2 C8 119.1(7) . . ? C43 O3 C48 119.4(9) . . ? C45 O4 C49 118.3(8) . . ? C24 P1 C16 106.7(4) . . ? C24 P1 C18 106.3(4) . . ? C16 P1 C18 109.1(4) . . ? C24 P1 Pd1 115.1(3) . . ? C16 P1 Pd1 94.1(2) . . ? C18 P1 Pd1 123.6(3) . . ? C36 P2 C35 108.3(4) . . ? C36 P2 C16 104.5(4) . . ? C35 P2 C16 107.3(4) . . ? C36 P2 Pd1 117.3(3) . . ? C35 P2 Pd1 125.0(3) . . ? C16 P2 Pd1 90.0(2) . . ? F1 P3 F5 95.5(8) . . ? F1 P3 F3 83.7(11) . . ? F5 P3 F3 93.9(7) . . ? F1 P3 F6 100.6(12) . . ? F5 P3 F6 88.4(6) . . ? F3 P3 F6 175.0(10) . . ? F1 P3 F2 88.5(7) . . ? F5 P3 F2 176.1(7) . . ? F3 P3 F2 86.6(6) . . ? F6 P3 F2 90.9(6) . . ? F1 P3 F4 172.8(10) . . ? F5 P3 F4 88.9(7) . . ? F3 P3 F4 90.4(10) . . ? F6 P3 F4 85.2(7) . . ? F2 P3 F4 87.2(6) . . ? C71 P4 C57 107.9(4) . . ? C71 P4 C78 108.1(3) . . ? C57 P4 C78 109.6(3) . . ? C71 P4 Pd2 118.9(3) . . ? C57 P4 Pd2 92.8(2) . . ? C78 P4 Pd2 117.8(3) . . ? C65 P5 C59 107.0(3) . . ? C65 P5 C57 107.6(3) . . ? C59 P5 C57 105.2(4) . . ? C65 P5 Pd2 130.1(3) . . ? C59 P5 Pd2 114.3(3) . . ? C57 P5 Pd2 87.6(2) . . ? F8 P6 F9 92.1(5) . . ? F8 P6 F7 92.3(6) . . ? F9 P6 F7 92.0(4) . . ? F8 P6 F10 91.4(5) . . ? F9 P6 F10 90.4(5) . . ? F7 P6 F10 175.5(6) . . ? F8 P6 F11 178.8(6) . . ? F9 P6 F11 89.0(5) . . ? F7 P6 F11 87.2(5) . . ? F10 P6 F11 89.0(5) . . ? F8 P6 F12 89.4(5) . . ? F9 P6 F12 178.2(6) . . ? F7 P6 F12 89.1(5) . . ? F10 P6 F12 88.5(4) . . ? F11 P6 F12 89.5(4) . . ? C6 Pd1 N1 81.0(3) . . ? C6 Pd1 P1 99.4(2) . . ? N1 Pd1 P1 178.9(2) . . ? C6 Pd1 P2 172.6(2) . . ? N1 Pd1 P2 106.30(19) . . ? P1 Pd1 P2 73.27(7) . . ? C47 Pd2 N2 80.7(3) . . ? C47 Pd2 P4 96.2(2) . . ? N2 Pd2 P4 168.8(2) . . ? C47 Pd2 P5 169.0(2) . . ? N2 Pd2 P5 110.3(2) . . ? P4 Pd2 P5 73.06(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 -177.4(6) . . . . ? C9 C1 C2 O1 4.9(11) . . . . ? C6 C1 C2 C3 3.1(11) . . . . ? C9 C1 C2 C3 -174.6(7) . . . . ? C1 C2 C3 C4 -1.8(12) . . . . ? O1 C2 C3 C4 178.8(7) . . . . ? C2 C3 C4 O2 177.3(7) . . . . ? C2 C3 C4 C5 0.4(12) . . . . ? C3 C4 C5 C6 -0.3(12) . . . . ? O2 C4 C5 C6 -176.9(7) . . . . ? C4 C5 C6 C1 1.5(11) . . . . ? C4 C5 C6 Pd1 176.4(6) . . . . ? C2 C1 C6 C5 -2.9(10) . . . . ? C9 C1 C6 C5 174.9(7) . . . . ? C2 C1 C6 Pd1 -178.7(6) . . . . ? C9 C1 C6 Pd1 -0.9(8) . . . . ? C2 C1 C9 N1 177.4(7) . . . . ? C6 C1 C9 N1 -0.3(10) . . . . ? C15 C10 C11 C12 23(3) . . . . ? N1 C10 C11 C12 179.6(13) . . . . ? C10 C11 C12 C13 -25(3) . . . . ? C11 C12 C13 C14 29(3) . . . . ? C12 C13 C14 C15 -27(3) . . . . ? C11 C10 C15 C14 -20(2) . . . . ? N1 C10 C15 C14 -178.1(13) . . . . ? C13 C14 C15 C10 22(3) . . . . ? C23 C18 C19 C20 -0.4(14) . . . . ? P1 C18 C19 C20 178.5(7) . . . . ? C18 C19 C20 C21 -0.2(15) . . . . ? C19 C20 C21 C22 0.4(19) . . . . ? C20 C21 C22 C23 0(2) . . . . ? C19 C18 C23 C22 0.9(15) . . . . ? P1 C18 C23 C22 -178.0(9) . . . . ? C21 C22 C23 C18 -0.8(19) . . . . ? C29 C24 C25 C26 0.0(16) . . . . ? P1 C24 C25 C26 -175.5(10) . . . . ? C24 C25 C26 C27 -1(2) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? C25 C24 C29 C28 0.9(16) . . . . ? P1 C24 C29 C28 176.3(9) . . . . ? C27 C28 C29 C24 -0.4(19) . . . . ? C35 C30 C31 C32 0(2) . . . . ? C30 C31 C32 C33 4(2) . . . . ? C31 C32 C33 C34 -5(3) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C31 C30 C35 C34 -3.0(16) . . . . ? C31 C30 C35 P2 -178.6(9) . . . . ? C33 C34 C35 C30 2.1(17) . . . . ? C33 C34 C35 P2 177.6(10) . . . . ? C41 C36 C37 C38 2.2(19) . . . . ? P2 C36 C37 C38 178.1(10) . . . . ? C36 C37 C38 C39 2(2) . . . . ? C37 C38 C39 C40 -5(3) . . . . ? C38 C39 C40 C41 6(3) . . . . ? C37 C36 C41 C40 -2(2) . . . . ? P2 C36 C41 C40 -178.1(14) . . . . ? C39 C40 C41 C36 -2(3) . . . . ? C47 C42 C43 C44 -2.7(13) . . . . ? C50 C42 C43 C44 177.0(9) . . . . ? C47 C42 C43 O3 177.8(7) . . . . ? C50 C42 C43 O3 -2.6(13) . . . . ? O3 C43 C44 C45 -179.0(8) . . . . ? C42 C43 C44 C45 1.5(13) . . . . ? C43 C44 C45 O4 -179.3(8) . . . . ? C43 C44 C45 C46 0.5(12) . . . . ? C44 C45 C46 C47 -1.3(12) . . . . ? O4 C45 C46 C47 178.5(7) . . . . ? C45 C46 C47 C42 0.1(11) . . . . ? C45 C46 C47 Pd2 -178.9(6) . . . . ? C43 C42 C47 C46 1.8(11) . . . . ? C50 C42 C47 C46 -177.8(8) . . . . ? C43 C42 C47 Pd2 -179.0(6) . . . . ? C50 C42 C47 Pd2 1.4(9) . . . . ? C43 C42 C50 N2 -177.4(9) . . . . ? C47 C42 C50 N2 2.2(13) . . . . ? C56 C51 C52 C53 -36.8(17) . . . . ? N2 C51 C52 C53 179.4(10) . . . . ? C51 C52 C53 C54 34.2(19) . . . . ? C52 C53 C54 C55 -36(3) . . . . ? C53 C54 C55 C56 36(3) . . . . ? C52 C51 C56 C55 37(2) . . . . ? N2 C51 C56 C55 -178.3(12) . . . . ? C54 C55 C56 C51 -34(2) . . . . ? C64 C59 C60 C61 -2.0(16) . . . . ? P5 C59 C60 C61 179.4(10) . . . . ? C59 C60 C61 C62 2(2) . . . . ? C60 C61 C62 C63 -1(2) . . . . ? C61 C62 C63 C64 -1(2) . . . . ? C60 C59 C64 C63 0.1(15) . . . . ? P5 C59 C64 C63 178.8(8) . . . . ? C62 C63 C64 C59 1.3(18) . . . . ? C70 C65 C66 C67 -1.9(11) . . . . ? P5 C65 C66 C67 -175.9(6) . . . . ? C65 C66 C67 C68 1.6(13) . . . . ? C66 C67 C68 C69 -0.1(13) . . . . ? C67 C68 C69 C70 -1.1(13) . . . . ? C68 C69 C70 C65 0.7(13) . . . . ? C66 C65 C70 C69 0.7(12) . . . . ? P5 C65 C70 C69 174.4(6) . . . . ? C76 C71 C72 C73 -0.1(13) . . . . ? P4 C71 C72 C73 -178.4(7) . . . . ? C71 C72 C73 C74 0.6(15) . . . . ? C72 C73 C74 C75 -0.3(17) . . . . ? C73 C74 C75 C76 -0.4(19) . . . . ? C74 C75 C76 C71 1.0(17) . . . . ? C72 C71 C76 C75 -0.7(13) . . . . ? P4 C71 C76 C75 177.6(8) . . . . ? C82 C77 C78 C79 1.0(12) . . . . ? C82 C77 C78 P4 -174.7(6) . . . . ? C77 C78 C79 C81 -1.2(14) . . . . ? P4 C78 C79 C81 174.7(8) . . . . ? C78 C79 C81 C80 0.8(16) . . . . ? C82 C80 C81 C79 -0.1(17) . . . . ? C81 C80 C82 C77 0.0(16) . . . . ? C78 C77 C82 C80 -0.4(14) . . . . ? C1 C9 N1 C10 -176.9(7) . . . . ? C1 C9 N1 Pd1 1.3(9) . . . . ? C15 C10 N1 C9 68.8(14) . . . . ? C11 C10 N1 C9 -90.6(15) . . . . ? C15 C10 N1 Pd1 -109.1(12) . . . . ? C11 C10 N1 Pd1 91.4(13) . . . . ? C42 C50 N2 C51 -177.0(9) . . . . ? C42 C50 N2 Pd2 -4.4(11) . . . . ? C56 C51 N2 C50 84.9(15) . . . . ? C52 C51 N2 C50 -128.8(11) . . . . ? C56 C51 N2 Pd2 -86.4(13) . . . . ? C52 C51 N2 Pd2 60.0(14) . . . . ? C1 C2 O1 C7 178.9(7) . . . . ? C3 C2 O1 C7 -1.6(12) . . . . ? C3 C4 O2 C8 171.9(9) . . . . ? C5 C4 O2 C8 -11.2(13) . . . . ? C44 C43 O3 C48 17.9(15) . . . . ? C42 C43 O3 C48 -162.6(10) . . . . ? C44 C45 O4 C49 6.7(13) . . . . ? C46 C45 O4 C49 -173.1(9) . . . . ? C25 C24 P1 C16 -145.8(7) . . . . ? C29 C24 P1 C16 38.8(9) . . . . ? C25 C24 P1 C18 97.9(8) . . . . ? C29 C24 P1 C18 -77.5(8) . . . . ? C25 C24 P1 Pd1 -42.9(8) . . . . ? C29 C24 P1 Pd1 141.8(7) . . . . ? C17 C16 P1 C24 -88.9(9) . . . . ? P2 C16 P1 C24 100.1(4) . . . . ? C17 C16 P1 C18 25.5(10) . . . . ? P2 C16 P1 C18 -145.5(4) . . . . ? C17 C16 P1 Pd1 153.3(8) . . . . ? P2 C16 P1 Pd1 -17.7(3) . . . . ? C19 C18 P1 C24 168.7(7) . . . . ? C23 C18 P1 C24 -12.4(8) . . . . ? C19 C18 P1 C16 54.0(8) . . . . ? C23 C18 P1 C16 -127.1(8) . . . . ? C19 C18 P1 Pd1 -54.7(8) . . . . ? C23 C18 P1 Pd1 124.1(7) . . . . ? C41 C36 P2 C35 -124.7(9) . . . . ? C37 C36 P2 C35 59.4(10) . . . . ? C41 C36 P2 C16 121.2(9) . . . . ? C37 C36 P2 C16 -54.7(10) . . . . ? C41 C36 P2 Pd1 23.5(10) . . . . ? C37 C36 P2 Pd1 -152.4(9) . . . . ? C30 C35 P2 C36 -168.1(7) . . . . ? C34 C35 P2 C36 16.3(10) . . . . ? C30 C35 P2 C16 -55.9(8) . . . . ? C34 C35 P2 C16 128.5(9) . . . . ? C30 C35 P2 Pd1 46.6(9) . . . . ? C34 C35 P2 Pd1 -128.9(8) . . . . ? C17 C16 P2 C36 87.4(9) . . . . ? P1 C16 P2 C36 -101.5(4) . . . . ? C17 C16 P2 C35 -27.5(10) . . . . ? P1 C16 P2 C35 143.7(4) . . . . ? C17 C16 P2 Pd1 -154.3(8) . . . . ? P1 C16 P2 Pd1 16.8(3) . . . . ? C72 C71 P4 C57 50.4(8) . . . . ? C76 C71 P4 C57 -127.9(7) . . . . ? C72 C71 P4 C78 -68.0(8) . . . . ? C76 C71 P4 C78 113.7(7) . . . . ? C72 C71 P4 Pd2 154.2(6) . . . . ? C76 C71 P4 Pd2 -24.1(8) . . . . ? C58 C57 P4 C71 -96.6(9) . . . . ? P5 C57 P4 C71 97.7(4) . . . . ? C58 C57 P4 C78 20.9(10) . . . . ? P5 C57 P4 C78 -144.8(4) . . . . ? C58 C57 P4 Pd2 141.7(9) . . . . ? P5 C57 P4 Pd2 -23.9(3) . . . . ? C79 C78 P4 C71 -179.3(7) . . . . ? C77 C78 P4 C71 -3.4(8) . . . . ? C79 C78 P4 C57 63.4(8) . . . . ? C77 C78 P4 C57 -120.8(7) . . . . ? C79 C78 P4 Pd2 -40.9(8) . . . . ? C77 C78 P4 Pd2 135.0(6) . . . . ? C70 C65 P5 C59 14.3(7) . . . . ? C66 C65 P5 C59 -172.0(6) . . . . ? C70 C65 P5 C57 126.9(7) . . . . ? C66 C65 P5 C57 -59.4(7) . . . . ? C70 C65 P5 Pd2 -131.0(6) . . . . ? C66 C65 P5 Pd2 42.7(7) . . . . ? C60 C59 P5 C65 -96.0(8) . . . . ? C64 C59 P5 C65 85.4(8) . . . . ? C60 C59 P5 C57 149.7(8) . . . . ? C64 C59 P5 C57 -28.9(8) . . . . ? C60 C59 P5 Pd2 55.4(8) . . . . ? C64 C59 P5 Pd2 -123.2(7) . . . . ? C58 C57 P5 C65 -11.7(10) . . . . ? P4 C57 P5 C65 153.8(3) . . . . ? C58 C57 P5 C59 102.2(9) . . . . ? P4 C57 P5 C59 -92.3(4) . . . . ? C58 C57 P5 Pd2 -143.2(9) . . . . ? P4 C57 P5 Pd2 22.3(3) . . . . ? C5 C6 Pd1 N1 -174.0(7) . . . . ? C1 C6 Pd1 N1 1.2(5) . . . . ? C5 C6 Pd1 P1 7.0(7) . . . . ? C1 C6 Pd1 P1 -177.9(5) . . . . ? C5 C6 Pd1 P2 -3(2) . . . . ? C1 C6 Pd1 P2 171.8(12) . . . . ? C9 N1 Pd1 C6 -1.4(6) . . . . ? C10 N1 Pd1 C6 176.8(7) . . . . ? C9 N1 Pd1 P1 115(10) . . . . ? C10 N1 Pd1 P1 -67(10) . . . . ? C9 N1 Pd1 P2 179.9(5) . . . . ? C10 N1 Pd1 P2 -2.0(7) . . . . ? C24 P1 Pd1 C6 84.8(3) . . . . ? C16 P1 Pd1 C6 -164.5(3) . . . . ? C18 P1 Pd1 C6 -48.4(4) . . . . ? C24 P1 Pd1 N1 -31(10) . . . . ? C16 P1 Pd1 N1 80(10) . . . . ? C18 P1 Pd1 N1 -164(10) . . . . ? C24 P1 Pd1 P2 -96.6(3) . . . . ? C16 P1 Pd1 P2 14.1(3) . . . . ? C18 P1 Pd1 P2 130.3(4) . . . . ? C36 P2 Pd1 C6 103.1(16) . . . . ? C35 P2 Pd1 C6 -114.5(16) . . . . ? C16 P2 Pd1 C6 -3.3(16) . . . . ? C36 P2 Pd1 N1 -86.6(4) . . . . ? C35 P2 Pd1 N1 55.9(4) . . . . ? C16 P2 Pd1 N1 167.1(3) . . . . ? C36 P2 Pd1 P1 92.4(3) . . . . ? C35 P2 Pd1 P1 -125.1(4) . . . . ? C16 P2 Pd1 P1 -13.9(3) . . . . ? C46 C47 Pd2 N2 176.4(7) . . . . ? C42 C47 Pd2 N2 -2.7(5) . . . . ? C46 C47 Pd2 P4 -14.5(7) . . . . ? C42 C47 Pd2 P4 166.4(5) . . . . ? C46 C47 Pd2 P5 -2.4(17) . . . . ? C42 C47 Pd2 P5 178.5(8) . . . . ? C50 N2 Pd2 C47 3.9(7) . . . . ? C51 N2 Pd2 C47 175.8(9) . . . . ? C50 N2 Pd2 P4 -70.6(13) . . . . ? C51 N2 Pd2 P4 101.3(12) . . . . ? C50 N2 Pd2 P5 -176.4(6) . . . . ? C51 N2 Pd2 P5 -4.5(9) . . . . ? C71 P4 Pd2 C47 84.0(4) . . . . ? C57 P4 Pd2 C47 -163.8(3) . . . . ? C78 P4 Pd2 C47 -49.9(3) . . . . ? C71 P4 Pd2 N2 157.0(11) . . . . ? C57 P4 Pd2 N2 -90.8(11) . . . . ? C78 P4 Pd2 N2 23.1(11) . . . . ? C71 P4 Pd2 P5 -93.6(3) . . . . ? C57 P4 Pd2 P5 18.6(3) . . . . ? C78 P4 Pd2 P5 132.5(3) . . . . ? C65 P5 Pd2 C47 -142.2(11) . . . . ? C59 P5 Pd2 C47 74.5(11) . . . . ? C57 P5 Pd2 C47 -31.0(11) . . . . ? C65 P5 Pd2 N2 39.0(4) . . . . ? C59 P5 Pd2 N2 -104.2(4) . . . . ? C57 P5 Pd2 N2 150.2(3) . . . . ? C65 P5 Pd2 P4 -129.7(3) . . . . ? C59 P5 Pd2 P4 87.1(3) . . . . ? C57 P5 Pd2 P4 -18.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.121 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.114 #===END data_7 _database_code_CSD 190098 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 F6 N O5 P3 Pd' _chemical_formula_weight 1038.23 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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.0537(2) _cell_length_b 9.7220(3) _cell_length_c 23.33850(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.6610(10) _cell_angle_gamma 90.00 _cell_volume 4776.70(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8075 _exptl_absorpt_correction_T_max 0.8965 _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 ? _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 24120 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8399 _reflns_number_gt 5249 _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^)+(0.1149P)^2^+8.1276P] 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 8399 _refine_ls_number_parameters 614 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.873 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4116(3) 0.1605(6) 0.4422(3) 0.0436(14) Uani 1 1 d . . . C2 C 0.4711(3) 0.1969(7) 0.4641(3) 0.0502(16) Uani 1 1 d . . . C3 C 0.5261(3) 0.1339(7) 0.4438(3) 0.0514(16) Uani 1 1 d . . . H3 H 0.5660 0.1579 0.4580 0.062 Uiso 1 1 calc R . . C4 C 0.5191(3) 0.0359(7) 0.4024(3) 0.0536(16) Uani 1 1 d . . . C5 C 0.4593(3) -0.0010(7) 0.3796(3) 0.0538(17) Uani 1 1 d . . . H5 H 0.4563 -0.0678 0.3512 0.065 Uiso 1 1 calc R . . C6 C 0.4056(3) 0.0617(6) 0.3995(3) 0.0430(14) Uani 1 1 d . . . C7 C 0.5312(3) 0.3357(9) 0.5298(4) 0.080(3) Uani 1 1 d . . . H7A H 0.5243 0.4057 0.5581 0.096 Uiso 1 1 calc R . . H7B H 0.5582 0.3710 0.5004 0.096 Uiso 1 1 calc R . . H7C H 0.5510 0.2575 0.5476 0.096 Uiso 1 1 calc R . . C8 C 0.6305(3) -0.0042(10) 0.3993(4) 0.090(3) Uani 1 1 d . . . H8A H 0.6604 -0.0613 0.3797 0.108 Uiso 1 1 calc R . . H8B H 0.6335 -0.0215 0.4398 0.108 Uiso 1 1 calc R . . H8C H 0.6399 0.0907 0.3920 0.108 Uiso 1 1 calc R . . C9 C 0.3529(3) 0.2198(6) 0.4623(3) 0.0486(16) Uani 1 1 d . . . H9 H 0.3534 0.2845 0.4917 0.058 Uiso 1 1 calc R . . C10 C 0.2413(3) 0.2339(7) 0.4656(3) 0.0514(16) Uani 1 1 d . . . H10 H 0.2527 0.3019 0.4949 0.062 Uiso 1 1 calc R . . C11 C 0.1984(3) 0.3039(8) 0.4217(3) 0.0626(19) Uani 1 1 d . . . H11A H 0.1890 0.2406 0.3906 0.075 Uiso 1 1 calc R . . H11B H 0.2199 0.3832 0.4059 0.075 Uiso 1 1 calc R . . C12 C 0.1365(4) 0.3496(9) 0.4494(4) 0.082(3) Uani 1 1 d . . . H12A H 0.1457 0.4212 0.4773 0.098 Uiso 1 1 calc R . . H12B H 0.1086 0.3883 0.4203 0.098 Uiso 1 1 calc R . . C13 C 0.1033(4) 0.2331(10) 0.4785(4) 0.085(3) Uani 1 1 d . . . H13A H 0.0898 0.1661 0.4501 0.102 Uiso 1 1 calc R . . H13B H 0.0657 0.2676 0.4974 0.102 Uiso 1 1 calc R . . C14 C 0.1462(4) 0.1644(11) 0.5221(3) 0.087(3) Uani 1 1 d . . . H14A H 0.1245 0.0861 0.5386 0.104 Uiso 1 1 calc R . . H14B H 0.1561 0.2286 0.5528 0.104 Uiso 1 1 calc R . . C15 C 0.2074(3) 0.1166(9) 0.4947(3) 0.067(2) Uani 1 1 d . . . H15A H 0.2351 0.0771 0.5238 0.080 Uiso 1 1 calc R . . H15B H 0.1978 0.0455 0.4667 0.080 Uiso 1 1 calc R . . C16 C 0.2452(3) -0.1411(7) 0.2859(3) 0.0477(15) Uani 1 1 d . . . H16 H 0.2362 -0.2155 0.3130 0.057 Uiso 1 1 calc R . . C17 C 0.2203(3) -0.1949(8) 0.2289(3) 0.067(2) Uani 1 1 d . . . H17A H 0.2454 -0.2740 0.2178 0.081 Uiso 1 1 calc R . . H17B H 0.2258 -0.1244 0.2000 0.081 Uiso 1 1 calc R . . C18 C 0.1498(3) -0.2367(9) 0.2304(3) 0.070(2) Uani 1 1 d . . . H18 H 0.1258 -0.1568 0.2437 0.084 Uiso 1 1 calc R . . C19 C 0.1356(5) -0.3539(11) 0.2699(4) 0.087(3) Uani 1 1 d . . . C45 C 0.4069(4) 0.1353(10) 0.1445(3) 0.084(3) Uani 1 1 d . . . H45 H 0.4220 0.1856 0.1137 0.101 Uiso 1 1 calc R . . C20 C 0.0694(5) -0.3908(13) 0.2773(5) 0.125(4) Uani 1 1 d D . . H20A H 0.0468 -0.3679 0.2421 0.150 Uiso 1 1 calc R . . H20B H 0.0524 -0.3329 0.3072 0.150 Uiso 1 1 calc R . . C46 C 0.4106(4) 0.1878(8) 0.1983(3) 0.073(2) Uani 1 1 d . . . H46 H 0.4282 0.2744 0.2042 0.087 Uiso 1 1 calc R . . C21 C 0.0534(7) -0.5446(17) 0.2926(6) 0.231(11) Uani 1 1 d D . . H21A H 0.0084 -0.5538 0.2979 0.277 Uiso 1 1 calc R . . H21B H 0.0754 -0.5701 0.3272 0.277 Uiso 1 1 calc R . . H21C H 0.0665 -0.6036 0.2619 0.277 Uiso 1 1 calc R . . C22 C 0.0768(6) -0.1954(13) 0.0857(5) 0.125(4) Uani 1 1 d D . . H22A H 0.1089 -0.2354 0.0613 0.150 Uiso 1 1 calc R . . H22B H 0.0400 -0.2553 0.0867 0.150 Uiso 1 1 calc R . . C41 C 0.4139(4) -0.3185(8) 0.2686(4) 0.080(2) Uani 1 1 d . . . H41 H 0.4275 -0.2644 0.2383 0.096 Uiso 1 1 calc R . . C42 C 0.3620(3) -0.0152(7) 0.2370(3) 0.0498(16) Uani 1 1 d . . . C23 C 0.0594(8) -0.0516(16) 0.0672(8) 0.224(9) Uani 1 1 d D . . H23A H 0.0426 -0.0536 0.0288 0.269 Uiso 1 1 calc R . . H23B H 0.0966 0.0055 0.0685 0.269 Uiso 1 1 calc R . . H23C H 0.0281 -0.0151 0.0926 0.269 Uiso 1 1 calc R . . C24 C 0.1387(3) -0.0304(7) 0.3498(3) 0.0532(16) Uani 1 1 d . . . C25 C 0.1359(3) -0.1337(9) 0.3900(3) 0.070(2) Uani 1 1 d . . . H25 H 0.1732 -0.1778 0.4011 0.084 Uiso 1 1 calc R . . C26 C 0.0798(5) -0.1735(11) 0.4141(4) 0.095(3) Uani 1 1 d . . . H26 H 0.0791 -0.2436 0.4413 0.114 Uiso 1 1 calc R . . C27 C 0.0249(4) -0.1087(14) 0.3978(5) 0.109(4) Uani 1 1 d . . . H27 H -0.0135 -0.1357 0.4136 0.131 Uiso 1 1 calc R . . C28 C 0.0260(4) -0.0060(13) 0.3590(5) 0.102(3) Uani 1 1 d . . . H28 H -0.0117 0.0374 0.3483 0.123 Uiso 1 1 calc R . . C29 C 0.0822(3) 0.0349(9) 0.3354(3) 0.070(2) Uani 1 1 d . . . H29 H 0.0825 0.1074 0.3095 0.084 Uiso 1 1 calc R . . C30 C 0.2070(3) 0.1448(7) 0.2673(3) 0.0548(17) Uani 1 1 d . . . C31 C 0.1658(4) 0.1313(9) 0.2205(3) 0.082(2) Uani 1 1 d . . . H31 H 0.1381 0.0569 0.2184 0.098 Uiso 1 1 calc R . . C32 C 0.1660(6) 0.2269(12) 0.1780(4) 0.106(3) Uani 1 1 d . . . H32 H 0.1386 0.2173 0.1467 0.128 Uiso 1 1 calc R . . C33 C 0.2063(6) 0.3373(12) 0.1811(4) 0.107(4) Uani 1 1 d . . . H33 H 0.2071 0.4008 0.1513 0.128 Uiso 1 1 calc R . . C34 C 0.2454(5) 0.3546(9) 0.2275(4) 0.087(3) Uani 1 1 d . . . H34 H 0.2719 0.4310 0.2299 0.105 Uiso 1 1 calc R . . C35 C 0.2455(4) 0.2590(7) 0.2703(3) 0.0636(19) Uani 1 1 d . . . H35 H 0.2720 0.2712 0.3021 0.076 Uiso 1 1 calc R . . C36 C 0.3685(3) -0.2686(6) 0.3055(3) 0.0482(16) Uani 1 1 d . . . C37 C 0.3503(4) -0.3500(8) 0.3501(3) 0.069(2) Uani 1 1 d . . . H37 H 0.3205 -0.3175 0.3759 0.083 Uiso 1 1 calc R . . C38 C 0.3757(5) -0.4816(8) 0.3571(4) 0.082(3) Uani 1 1 d . . . H38 H 0.3627 -0.5364 0.3875 0.098 Uiso 1 1 calc R . . C39 C 0.4191(5) -0.5295(9) 0.3202(5) 0.091(3) Uani 1 1 d . . . H39 H 0.4353 -0.6180 0.3244 0.110 Uiso 1 1 calc R . . C40 C 0.4390(5) -0.4483(9) 0.2766(5) 0.101(3) Uani 1 1 d . . . H40 H 0.4700 -0.4805 0.2519 0.121 Uiso 1 1 calc R . . C43 C 0.3586(4) -0.0662(9) 0.1816(3) 0.078(2) Uani 1 1 d . . . H43 H 0.3410 -0.1526 0.1754 0.093 Uiso 1 1 calc R . . C44 C 0.3806(5) 0.0073(11) 0.1359(4) 0.097(3) Uani 1 1 d . . . H44 H 0.3777 -0.0292 0.0992 0.116 Uiso 1 1 calc R . . C47 C 0.3882(3) 0.1134(7) 0.2446(3) 0.0573(17) Uani 1 1 d . . . H47 H 0.3910 0.1508 0.2812 0.069 Uiso 1 1 calc R . . C48 C 0.1259(4) -0.2710(11) 0.1716(4) 0.077(2) Uani 1 1 d . . . N1 N 0.3010(2) 0.1829(5) 0.4397(2) 0.0436(12) Uani 1 1 d . . . O1 O 0.4718(2) 0.2956(5) 0.5052(2) 0.0716(15) Uani 1 1 d . . . O2 O 0.5684(2) -0.0345(5) 0.3796(2) 0.0765(16) Uani 1 1 d . . . O3 O 0.1770(3) -0.4152(7) 0.2961(3) 0.098(2) Uani 1 1 d . . . O4 O 0.1269(3) -0.3843(7) 0.1519(3) 0.102(2) Uani 1 1 d . . . O5 O 0.1022(4) -0.1640(9) 0.1448(4) 0.146(3) Uani 1 1 d . . . F3 F 0.2370(4) -0.4323(6) 0.5516(3) 0.150(3) Uani 1 1 d . A . F6 F 0.2941(4) -0.2017(7) 0.4768(3) 0.164(3) Uani 1 1 d . A . F1 F 0.3305(8) -0.298(2) 0.5451(13) 0.128(9) Uani 0.50(3) 1 d P A 1 F2 F 0.2423(12) -0.201(2) 0.5574(13) 0.143(10) Uani 0.50(3) 1 d P A 1 F4 F 0.1985(11) -0.328(3) 0.4911(13) 0.179(14) Uani 0.50(3) 1 d P A 1 F5 F 0.294(2) -0.4268(19) 0.4776(15) 0.183(16) Uani 0.50(3) 1 d P A 1 F1' F 0.2955(16) -0.2758(17) 0.5735(7) 0.146(12) Uani 0.50(3) 1 d PD A 2 F2' F 0.2073(10) -0.211(2) 0.5231(11) 0.143(12) Uani 0.50(3) 1 d PD A 2 F4' F 0.2330(11) -0.3606(16) 0.4530(7) 0.113(8) Uani 0.50(3) 1 d PD A 2 F5' F 0.3208(8) -0.427(2) 0.5013(10) 0.136(10) Uani 0.50(3) 1 d PD A 2 P1 P 0.33037(7) -0.10214(17) 0.29845(7) 0.0422(4) Uani 1 1 d . . . P2 P 0.21569(8) 0.01551(17) 0.32231(7) 0.0445(4) Uani 1 1 d . . . P3 P 0.26511(12) -0.3173(3) 0.51494(11) 0.0791(7) Uani 1 1 d D . . Pd1 Pd 0.31366(2) 0.04017(5) 0.373160(19) 0.03994(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(4) 0.041(3) 0.041(3) -0.006(3) 0.001(3) 0.001(3) C2 0.056(4) 0.050(4) 0.045(4) -0.014(3) -0.002(3) -0.004(3) C3 0.040(3) 0.061(4) 0.053(4) -0.005(3) -0.005(3) -0.003(3) C4 0.046(4) 0.058(4) 0.057(4) -0.010(3) -0.001(3) 0.005(3) C5 0.056(4) 0.052(4) 0.054(4) -0.011(3) 0.000(3) 0.001(3) C6 0.040(3) 0.047(4) 0.041(3) 0.000(3) -0.001(3) 0.001(3) C7 0.063(5) 0.099(6) 0.078(6) -0.038(5) -0.014(4) -0.019(5) C8 0.051(5) 0.113(7) 0.107(7) -0.032(6) 0.001(5) 0.014(5) C9 0.063(4) 0.047(4) 0.035(3) -0.011(3) 0.003(3) -0.001(3) C10 0.053(4) 0.055(4) 0.047(4) -0.009(3) 0.003(3) 0.008(3) C11 0.065(4) 0.067(5) 0.056(4) 0.001(4) 0.007(3) 0.019(4) C12 0.066(5) 0.103(7) 0.075(6) -0.013(5) -0.002(4) 0.041(5) C13 0.060(5) 0.125(8) 0.069(6) -0.014(5) 0.013(4) 0.009(5) C14 0.066(5) 0.137(8) 0.058(5) 0.008(5) 0.021(4) 0.011(5) C15 0.058(4) 0.094(6) 0.049(4) 0.003(4) 0.004(3) 0.011(4) C16 0.046(3) 0.053(4) 0.044(4) -0.004(3) -0.001(3) -0.002(3) C17 0.058(4) 0.084(5) 0.059(5) -0.022(4) 0.000(4) -0.007(4) C18 0.052(4) 0.082(6) 0.076(5) -0.018(5) -0.006(4) -0.007(4) C19 0.090(7) 0.114(8) 0.058(5) -0.020(5) -0.007(5) 0.000(6) C45 0.092(6) 0.109(7) 0.052(5) 0.018(5) 0.015(4) -0.017(6) C20 0.071(7) 0.195(13) 0.109(9) -0.057(9) -0.015(6) -0.005(8) C46 0.086(6) 0.075(5) 0.058(5) 0.009(4) 0.015(4) -0.022(4) C21 0.115(11) 0.41(3) 0.169(15) 0.171(18) -0.004(10) -0.055(15) C22 0.131(10) 0.121(10) 0.122(10) 0.014(8) -0.025(8) -0.010(8) C41 0.074(5) 0.067(5) 0.101(7) -0.008(5) 0.028(5) 0.006(4) C42 0.047(4) 0.063(4) 0.040(3) -0.007(3) 0.009(3) -0.010(3) C23 0.167(16) 0.32(3) 0.186(19) 0.035(18) -0.021(14) -0.036(17) C24 0.046(4) 0.071(5) 0.043(4) -0.002(3) 0.001(3) 0.009(3) C25 0.056(4) 0.102(6) 0.053(4) 0.015(4) 0.007(3) -0.005(4) C26 0.084(6) 0.134(9) 0.066(6) 0.023(6) 0.011(5) -0.014(6) C27 0.060(6) 0.183(12) 0.084(7) -0.015(8) 0.018(5) -0.025(7) C28 0.043(5) 0.173(11) 0.090(7) -0.024(7) -0.008(5) 0.016(6) C29 0.056(4) 0.099(6) 0.056(4) -0.011(4) -0.006(4) 0.022(4) C30 0.073(5) 0.058(4) 0.034(3) -0.003(3) 0.003(3) 0.009(4) C31 0.100(6) 0.090(6) 0.055(5) 0.013(4) -0.014(4) 0.006(5) C32 0.156(10) 0.113(8) 0.050(5) 0.025(5) -0.019(6) 0.009(8) C33 0.159(11) 0.097(8) 0.064(6) 0.037(6) 0.014(7) 0.040(7) C34 0.114(7) 0.058(5) 0.091(7) 0.016(5) 0.024(6) 0.013(5) C35 0.084(5) 0.056(4) 0.051(4) 0.004(3) 0.011(4) 0.013(4) C36 0.039(3) 0.046(4) 0.059(4) -0.014(3) -0.009(3) -0.006(3) C37 0.073(5) 0.069(5) 0.066(5) 0.001(4) 0.000(4) 0.013(4) C38 0.096(7) 0.058(5) 0.092(7) 0.013(5) -0.017(5) 0.003(5) C39 0.085(6) 0.057(5) 0.132(9) -0.024(6) -0.019(6) 0.005(5) C40 0.083(6) 0.065(6) 0.155(10) -0.024(6) 0.020(7) 0.026(5) C43 0.100(6) 0.086(6) 0.048(4) -0.020(4) 0.017(4) -0.035(5) C44 0.117(8) 0.132(8) 0.042(4) -0.006(5) 0.015(5) -0.032(7) C47 0.062(4) 0.062(4) 0.048(4) -0.002(3) 0.012(3) -0.008(4) C48 0.061(5) 0.096(7) 0.075(6) -0.017(5) -0.012(4) -0.001(5) N1 0.044(3) 0.047(3) 0.040(3) -0.007(2) 0.003(2) 0.000(2) O1 0.050(3) 0.088(4) 0.077(4) -0.043(3) -0.004(2) 0.000(3) O2 0.045(3) 0.086(4) 0.099(4) -0.045(3) -0.003(3) 0.010(3) O3 0.114(5) 0.085(4) 0.095(5) 0.000(4) -0.013(4) -0.018(4) O4 0.121(5) 0.097(5) 0.087(4) -0.027(4) -0.028(4) 0.000(4) O5 0.132(7) 0.134(7) 0.172(8) -0.054(6) -0.062(6) 0.011(5) F3 0.164(6) 0.114(5) 0.173(7) 0.058(5) 0.051(5) -0.007(4) F6 0.235(8) 0.103(5) 0.154(6) 0.045(4) 0.073(6) -0.014(5) F1 0.103(11) 0.107(13) 0.17(2) 0.008(14) -0.010(11) -0.019(9) F2 0.138(18) 0.106(12) 0.19(2) 0.007(14) 0.065(16) 0.015(13) F4 0.132(16) 0.27(3) 0.13(2) 0.08(2) -0.058(17) -0.02(2) F5 0.28(4) 0.068(11) 0.20(3) -0.018(12) 0.11(3) -0.003(16) F1' 0.26(3) 0.090(10) 0.089(11) -0.023(9) -0.061(15) 0.000(16) F2' 0.128(19) 0.115(15) 0.19(2) 0.060(16) 0.050(15) 0.068(15) F4' 0.148(15) 0.122(12) 0.067(9) 0.015(7) -0.027(10) -0.014(10) F5' 0.097(10) 0.140(18) 0.17(2) 0.000(13) 0.004(10) 0.049(10) P1 0.0416(8) 0.0445(9) 0.0405(9) -0.0063(7) 0.0021(7) -0.0057(7) P2 0.0464(9) 0.0520(10) 0.0350(8) -0.0005(7) -0.0030(7) 0.0036(8) P3 0.0815(16) 0.0762(15) 0.0793(16) 0.0141(13) -0.0033(13) -0.0018(13) Pd1 0.0421(3) 0.0437(3) 0.0340(3) -0.0044(2) 0.00086(18) 0.0004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.388(8) . ? C1 C2 1.393(8) . ? C1 C9 1.449(8) . ? C2 O1 1.356(7) . ? C2 C3 1.398(9) . ? C3 C4 1.364(9) . ? C4 O2 1.357(8) . ? C4 C5 1.407(9) . ? C5 C6 1.370(9) . ? C6 Pd1 2.035(6) . ? C7 O1 1.425(8) . ? C8 O2 1.411(9) . ? C9 N1 1.261(8) . ? C10 N1 1.485(8) . ? C10 C15 1.511(10) . ? C10 C11 1.518(9) . ? C11 C12 1.527(9) . ? C12 C13 1.499(12) . ? C13 C14 1.509(11) . ? C14 C15 1.518(10) . ? C16 C17 1.517(9) . ? C16 P2 1.854(6) . ? C16 P1 1.853(6) . ? C17 C18 1.538(9) . ? C18 C48 1.493(11) . ? C18 C19 1.499(13) . ? C19 O3 1.215(10) . ? C19 C20 1.451(13) . ? C45 C46 1.357(11) . ? C45 C44 1.376(12) . ? C20 C21 1.575(9) . ? C46 C47 1.385(9) . ? C22 C23 1.505(9) . ? C22 O5 1.507(13) . ? C41 C36 1.381(10) . ? C41 C40 1.381(11) . ? C42 C47 1.377(9) . ? C42 C43 1.384(9) . ? C42 P1 1.800(6) . ? C24 C25 1.377(10) . ? C24 C29 1.385(9) . ? C24 P2 1.807(7) . ? C25 C26 1.370(10) . ? C26 C27 1.367(13) . ? C27 C28 1.348(15) . ? C28 C29 1.371(12) . ? C30 C35 1.376(10) . ? C30 C31 1.393(10) . ? C30 P2 1.804(7) . ? C31 C32 1.360(12) . ? C32 C33 1.370(14) . ? C33 C34 1.363(14) . ? C34 C35 1.365(10) . ? C36 C37 1.365(10) . ? C36 P1 1.813(7) . ? C37 C38 1.397(10) . ? C38 C39 1.346(13) . ? C39 C40 1.357(14) . ? C43 C44 1.368(11) . ? C48 O4 1.194(10) . ? C48 O5 1.310(11) . ? N1 Pd1 2.102(5) . ? F3 P3 1.531(6) . ? F6 P3 1.562(6) . ? F1 P3 1.549(18) . ? F2 P3 1.579(19) . ? F4 P3 1.506(16) . ? F5 P3 1.51(2) . ? F1' P3 1.556(12) . ? F2' P3 1.609(12) . ? F4' P3 1.644(11) . ? F5' P3 1.618(14) . ? P1 Pd1 2.2566(16) . ? P2 Pd1 2.3799(16) . ? 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 C6 C1 C2 120.9(6) . . ? C6 C1 C9 116.0(5) . . ? C2 C1 C9 123.1(5) . . ? O1 C2 C1 116.2(6) . . ? O1 C2 C3 123.2(6) . . ? C1 C2 C3 120.6(5) . . ? C4 C3 C2 117.6(6) . . ? O2 C4 C3 123.6(6) . . ? O2 C4 C5 114.1(6) . . ? C3 C4 C5 122.3(6) . . ? C6 C5 C4 119.8(6) . . ? C5 C6 C1 118.8(6) . . ? C5 C6 Pd1 129.6(5) . . ? C1 C6 Pd1 111.5(4) . . ? N1 C9 C1 119.3(5) . . ? N1 C10 C15 109.7(5) . . ? N1 C10 C11 112.0(5) . . ? C15 C10 C11 111.2(6) . . ? C10 C11 C12 110.4(6) . . ? C13 C12 C11 112.1(7) . . ? C12 C13 C14 111.2(7) . . ? C13 C14 C15 110.8(6) . . ? C10 C15 C14 111.4(7) . . ? C17 C16 P2 124.8(5) . . ? C17 C16 P1 122.2(5) . . ? P2 C16 P1 95.1(3) . . ? C16 C17 C18 113.3(6) . . ? C48 C18 C19 109.2(7) . . ? C48 C18 C17 110.8(7) . . ? C19 C18 C17 114.5(7) . . ? O3 C19 C20 120.2(10) . . ? O3 C19 C18 122.3(9) . . ? C20 C19 C18 117.4(10) . . ? C46 C45 C44 119.6(8) . . ? C19 C20 C21 118.1(10) . . ? C45 C46 C47 120.5(8) . . ? C23 C22 O5 99.0(11) . . ? C36 C41 C40 120.2(9) . . ? C47 C42 C43 117.5(6) . . ? C47 C42 P1 118.4(5) . . ? C43 C42 P1 124.0(5) . . ? C25 C24 C29 117.1(7) . . ? C25 C24 P2 117.9(5) . . ? C29 C24 P2 124.9(6) . . ? C26 C25 C24 122.0(8) . . ? C25 C26 C27 119.0(9) . . ? C28 C27 C26 120.6(9) . . ? C27 C28 C29 120.4(9) . . ? C28 C29 C24 120.9(9) . . ? C35 C30 C31 118.4(7) . . ? C35 C30 P2 118.1(5) . . ? C31 C30 P2 123.4(6) . . ? C32 C31 C30 120.1(9) . . ? C31 C32 C33 120.3(9) . . ? C34 C33 C32 120.5(9) . . ? C33 C34 C35 119.5(9) . . ? C34 C35 C30 121.1(8) . . ? C37 C36 C41 118.3(7) . . ? C37 C36 P1 117.3(5) . . ? C41 C36 P1 124.4(6) . . ? C36 C37 C38 120.7(8) . . ? C39 C38 C37 120.2(9) . . ? C38 C39 C40 119.8(9) . . ? C39 C40 C41 120.8(9) . . ? C44 C43 C42 121.7(8) . . ? C43 C44 C45 119.8(8) . . ? C42 C47 C46 120.8(7) . . ? O4 C48 O5 123.8(9) . . ? O4 C48 C18 123.6(9) . . ? O5 C48 C18 112.6(9) . . ? C9 N1 C10 117.9(5) . . ? C9 N1 Pd1 112.4(4) . . ? C10 N1 Pd1 129.5(4) . . ? C2 O1 C7 118.7(5) . . ? C4 O2 C8 118.5(6) . . ? C48 O5 C22 114.0(8) . . ? C42 P1 C36 108.9(3) . . ? C42 P1 C16 109.7(3) . . ? C36 P1 C16 105.0(3) . . ? C42 P1 Pd1 113.0(2) . . ? C36 P1 Pd1 123.3(2) . . ? C16 P1 Pd1 95.0(2) . . ? C30 P2 C24 109.9(3) . . ? C30 P2 C16 106.1(3) . . ? C24 P2 C16 105.4(3) . . ? C30 P2 Pd1 111.4(2) . . ? C24 P2 Pd1 128.7(2) . . ? C16 P2 Pd1 91.04(19) . . ? F4 P3 F5 96.7(16) . . ? F4 P3 F1' 135.7(12) . . ? F5 P3 F1' 121.7(15) . . ? F4 P3 F3 77.9(9) . . ? F5 P3 F3 88.2(10) . . ? F1' P3 F3 81.7(10) . . ? F4 P3 F1 173.9(13) . . ? F5 P3 F1 89.1(14) . . ? F1' P3 F1 38.3(8) . . ? F3 P3 F1 100.4(8) . . ? F4 P3 F6 102.1(9) . . ? F5 P3 F6 90.9(9) . . ? F1' P3 F6 98.9(10) . . ? F3 P3 F6 179.1(5) . . ? F1 P3 F6 79.7(8) . . ? F4 P3 F2' 52.2(11) . . ? F5 P3 F2' 146.3(15) . . ? F1' P3 F2' 92.0(8) . . ? F3 P3 F2' 96.0(7) . . ? F1 P3 F2' 122.6(10) . . ? F6 P3 F2' 84.7(7) . . ? F4 P3 F2 89.7(12) . . ? F5 P3 F2 173.6(16) . . ? F1' P3 F2 52.3(9) . . ? F3 P3 F2 92.7(8) . . ? F1 P3 F2 84.5(10) . . ? F6 P3 F2 88.2(8) . . ? F2' P3 F2 39.9(8) . . ? F4 P3 F4' 44.3(10) . . ? F5 P3 F4' 58.4(15) . . ? F1' P3 F4' 179.8(9) . . ? F3 P3 F4' 98.5(7) . . ? F1 P3 F4' 141.6(9) . . ? F6 P3 F4' 80.9(7) . . ? F2' P3 F4' 87.9(8) . . ? F2 P3 F4' 127.6(11) . . ? F4 P3 F5' 123.6(14) . . ? F5 P3 F5' 28.8(17) . . ? F1' P3 F5' 92.9(9) . . ? F3 P3 F5' 85.1(9) . . ? F1 P3 F5' 61.7(10) . . ? F6 P3 F5' 94.1(9) . . ? F2' P3 F5' 175.1(10) . . ? F2 P3 F5' 145.0(11) . . ? F4' P3 F5' 87.1(7) . . ? C6 Pd1 N1 80.7(2) . . ? C6 Pd1 P1 98.05(17) . . ? N1 Pd1 P1 176.29(14) . . ? C6 Pd1 P2 167.65(17) . . ? N1 Pd1 P2 108.54(14) . . ? P1 Pd1 P2 72.24(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 179.3(6) . . . . ? C9 C1 C2 O1 -1.8(10) . . . . ? C6 C1 C2 C3 -0.4(10) . . . . ? C9 C1 C2 C3 178.5(6) . . . . ? O1 C2 C3 C4 180.0(6) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C2 C3 C4 O2 -179.0(7) . . . . ? C2 C3 C4 C5 0.8(11) . . . . ? O2 C4 C5 C6 179.3(6) . . . . ? C3 C4 C5 C6 -0.5(11) . . . . ? C4 C5 C6 C1 -0.3(10) . . . . ? C4 C5 C6 Pd1 176.3(5) . . . . ? C2 C1 C6 C5 0.8(9) . . . . ? C9 C1 C6 C5 -178.3(6) . . . . ? C2 C1 C6 Pd1 -176.5(5) . . . . ? C9 C1 C6 Pd1 4.5(7) . . . . ? C6 C1 C9 N1 -2.0(9) . . . . ? C2 C1 C9 N1 179.0(6) . . . . ? N1 C10 C11 C12 177.7(6) . . . . ? C15 C10 C11 C12 54.7(8) . . . . ? C10 C11 C12 C13 -55.0(9) . . . . ? C11 C12 C13 C14 55.7(10) . . . . ? C12 C13 C14 C15 -55.7(10) . . . . ? N1 C10 C15 C14 179.6(6) . . . . ? C11 C10 C15 C14 -56.0(8) . . . . ? C13 C14 C15 C10 56.1(10) . . . . ? P2 C16 C17 C18 -62.6(9) . . . . ? P1 C16 C17 C18 172.9(5) . . . . ? C16 C17 C18 C48 172.5(7) . . . . ? C16 C17 C18 C19 -63.6(9) . . . . ? C48 C18 C19 O3 120.8(9) . . . . ? C17 C18 C19 O3 -3.9(12) . . . . ? C48 C18 C19 C20 -60.6(10) . . . . ? C17 C18 C19 C20 174.7(8) . . . . ? O3 C19 C20 C21 -29.7(15) . . . . ? C18 C19 C20 C21 151.7(11) . . . . ? C44 C45 C46 C47 0.2(14) . . . . ? C29 C24 C25 C26 1.6(12) . . . . ? P2 C24 C25 C26 178.6(7) . . . . ? C24 C25 C26 C27 0.0(14) . . . . ? C25 C26 C27 C28 -0.8(17) . . . . ? C26 C27 C28 C29 0.0(17) . . . . ? C27 C28 C29 C24 1.6(15) . . . . ? C25 C24 C29 C28 -2.4(12) . . . . ? P2 C24 C29 C28 -179.1(7) . . . . ? C35 C30 C31 C32 2.6(12) . . . . ? P2 C30 C31 C32 -173.9(7) . . . . ? C30 C31 C32 C33 -0.4(16) . . . . ? C31 C32 C33 C34 -1.8(17) . . . . ? C32 C33 C34 C35 1.8(15) . . . . ? C33 C34 C35 C30 0.4(13) . . . . ? C31 C30 C35 C34 -2.6(11) . . . . ? P2 C30 C35 C34 174.0(6) . . . . ? C40 C41 C36 C37 0.8(12) . . . . ? C40 C41 C36 P1 -178.2(7) . . . . ? C41 C36 C37 C38 -1.5(11) . . . . ? P1 C36 C37 C38 177.6(6) . . . . ? C36 C37 C38 C39 0.4(12) . . . . ? C37 C38 C39 C40 1.4(14) . . . . ? C38 C39 C40 C41 -2.1(16) . . . . ? C36 C41 C40 C39 1.0(15) . . . . ? C47 C42 C43 C44 0.3(13) . . . . ? P1 C42 C43 C44 176.6(7) . . . . ? C42 C43 C44 C45 0.0(15) . . . . ? C46 C45 C44 C43 -0.3(15) . . . . ? C43 C42 C47 C46 -0.4(11) . . . . ? P1 C42 C47 C46 -176.9(6) . . . . ? C45 C46 C47 C42 0.2(12) . . . . ? C19 C18 C48 O4 -35.5(12) . . . . ? C17 C18 C48 O4 91.4(11) . . . . ? C19 C18 C48 O5 142.7(9) . . . . ? C17 C18 C48 O5 -90.4(10) . . . . ? C1 C9 N1 C10 173.4(5) . . . . ? C1 C9 N1 Pd1 -1.6(7) . . . . ? C15 C10 N1 C9 -109.7(7) . . . . ? C11 C10 N1 C9 126.4(6) . . . . ? C15 C10 N1 Pd1 64.3(7) . . . . ? C11 C10 N1 Pd1 -59.7(7) . . . . ? C1 C2 O1 C7 179.1(7) . . . . ? C3 C2 O1 C7 -1.2(10) . . . . ? C3 C4 O2 C8 -0.6(11) . . . . ? C5 C4 O2 C8 179.5(7) . . . . ? O4 C48 O5 C22 -0.9(15) . . . . ? C18 C48 O5 C22 -179.2(8) . . . . ? C23 C22 O5 C48 -175.6(11) . . . . ? C47 C42 P1 C36 -124.2(5) . . . . ? C43 C42 P1 C36 59.5(7) . . . . ? C47 C42 P1 C16 121.4(5) . . . . ? C43 C42 P1 C16 -54.9(8) . . . . ? C47 C42 P1 Pd1 16.7(6) . . . . ? C43 C42 P1 Pd1 -159.6(6) . . . . ? C37 C36 P1 C42 -179.8(5) . . . . ? C41 C36 P1 C42 -0.7(7) . . . . ? C37 C36 P1 C16 -62.4(6) . . . . ? C41 C36 P1 C16 116.7(6) . . . . ? C37 C36 P1 Pd1 44.2(6) . . . . ? C41 C36 P1 Pd1 -136.7(6) . . . . ? C17 C16 P1 C42 42.3(7) . . . . ? P2 C16 P1 C42 -94.8(3) . . . . ? C17 C16 P1 C36 -74.6(6) . . . . ? P2 C16 P1 C36 148.3(3) . . . . ? C17 C16 P1 Pd1 158.9(6) . . . . ? P2 C16 P1 Pd1 21.8(2) . . . . ? C35 C30 P2 C24 131.7(6) . . . . ? C31 C30 P2 C24 -51.8(7) . . . . ? C35 C30 P2 C16 -114.7(6) . . . . ? C31 C30 P2 C16 61.7(7) . . . . ? C35 C30 P2 Pd1 -17.0(6) . . . . ? C31 C30 P2 Pd1 159.4(6) . . . . ? C25 C24 P2 C30 176.5(6) . . . . ? C29 C24 P2 C30 -6.8(7) . . . . ? C25 C24 P2 C16 62.5(6) . . . . ? C29 C24 P2 C16 -120.8(6) . . . . ? C25 C24 P2 Pd1 -41.7(7) . . . . ? C29 C24 P2 Pd1 135.0(5) . . . . ? C17 C16 P2 C30 -43.4(6) . . . . ? P1 C16 P2 C30 92.1(3) . . . . ? C17 C16 P2 C24 73.2(6) . . . . ? P1 C16 P2 C24 -151.3(3) . . . . ? C17 C16 P2 Pd1 -156.0(6) . . . . ? P1 C16 P2 Pd1 -20.5(2) . . . . ? C5 C6 Pd1 N1 179.1(6) . . . . ? C1 C6 Pd1 N1 -4.0(4) . . . . ? C5 C6 Pd1 P1 -4.4(6) . . . . ? C1 C6 Pd1 P1 172.5(4) . . . . ? C5 C6 Pd1 P2 -41.8(12) . . . . ? C1 C6 Pd1 P2 135.1(7) . . . . ? C9 N1 Pd1 C6 3.1(5) . . . . ? C10 N1 Pd1 C6 -171.2(5) . . . . ? C9 N1 Pd1 P1 -67(2) . . . . ? C10 N1 Pd1 P1 119(2) . . . . ? C9 N1 Pd1 P2 -168.4(4) . . . . ? C10 N1 Pd1 P2 17.3(5) . . . . ? C42 P1 Pd1 C6 -75.9(3) . . . . ? C36 P1 Pd1 C6 58.6(3) . . . . ? C16 P1 Pd1 C6 170.2(3) . . . . ? C42 P1 Pd1 N1 -6(2) . . . . ? C36 P1 Pd1 N1 128(2) . . . . ? C16 P1 Pd1 N1 -120(2) . . . . ? C42 P1 Pd1 P2 96.3(2) . . . . ? C36 P1 Pd1 P2 -129.3(3) . . . . ? C16 P1 Pd1 P2 -17.6(2) . . . . ? C30 P2 Pd1 C6 -51.1(8) . . . . ? C24 P2 Pd1 C6 167.5(8) . . . . ? C16 P2 Pd1 C6 56.7(8) . . . . ? C30 P2 Pd1 N1 85.9(3) . . . . ? C24 P2 Pd1 N1 -55.5(3) . . . . ? C16 P2 Pd1 N1 -166.3(3) . . . . ? C30 P2 Pd1 P1 -90.3(2) . . . . ? C24 P2 Pd1 P1 128.4(3) . . . . ? C16 P2 Pd1 P1 17.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.857 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.088