# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nicholas Bruno' _publ_contact_author_email sbuchwal@MIT.EDU loop_ _publ_author_name 'Nicholas Bruno' 'Stephen Buchwald' 'Matthew Tudge' data_x12053 _database_code_depnum_ccdc_archive 'CCDC 891252' #TrackingRef '- 2L1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H59 Cl N P Pd' _chemical_formula_weight 786.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.1656(13) _cell_length_b 13.4105(18) _cell_length_c 15.503(2) _cell_angle_alpha 97.346(3) _cell_angle_beta 101.171(3) _cell_angle_gamma 101.772(3) _cell_volume 1998.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9695 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 31.07 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8890 _exptl_absorpt_correction_T_max 0.9821 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus sealed tube' _diffrn_radiation_monochromator 'Incoatech ImuS multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 126595 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12138 _reflns_number_gt 11484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0258P)^2^+1.0480P] 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 12138 _refine_ls_number_parameters 454 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.60469(3) 0.647223(19) 0.964998(18) 0.01707(5) Uani 1 1 d . . . Pd1 Pd 0.744270(7) 0.561634(6) 0.885782(5) 0.01153(2) Uani 1 1 d . . . P1 P 0.85319(3) 0.692677(19) 0.825268(17) 0.01081(5) Uani 1 1 d . . . C1 C 0.82903(10) 0.65143(8) 0.70292(7) 0.01237(17) Uani 1 1 d . . . H1 H 0.9064 0.6182 0.6947 0.015 Uiso 1 1 calc R . . C2 C 0.69434(11) 0.56747(8) 0.66466(7) 0.01548(18) Uani 1 1 d . . . H2A H 0.6930 0.5102 0.6992 0.019 Uiso 1 1 calc R . . H2B H 0.6144 0.5972 0.6708 0.019 Uiso 1 1 calc R . . C3 C 0.68183(11) 0.52538(9) 0.56636(8) 0.0187(2) Uani 1 1 d . . . H3A H 0.7577 0.4907 0.5608 0.022 Uiso 1 1 calc R . . H3B H 0.5934 0.4733 0.5430 0.022 Uiso 1 1 calc R . . C4 C 0.68792(12) 0.61170(9) 0.51084(7) 0.0201(2) Uani 1 1 d . . . H4A H 0.6831 0.5827 0.4480 0.024 Uiso 1 1 calc R . . H4B H 0.6079 0.6428 0.5123 0.024 Uiso 1 1 calc R . . C5 C 0.82122(11) 0.69458(9) 0.54757(7) 0.0189(2) Uani 1 1 d . . . H5A H 0.8224 0.7513 0.5125 0.023 Uiso 1 1 calc R . . H5B H 0.9009 0.6646 0.5415 0.023 Uiso 1 1 calc R . . C6 C 0.83435(11) 0.73796(8) 0.64609(7) 0.01500(18) Uani 1 1 d . . . H6A H 0.7584 0.7726 0.6515 0.018 Uiso 1 1 calc R . . H6B H 0.9227 0.7903 0.6689 0.018 Uiso 1 1 calc R . . C7 C 0.79570(10) 0.81531(8) 0.83498(7) 0.01276(17) Uani 1 1 d . . . H7 H 0.8436 0.8592 0.7975 0.015 Uiso 1 1 calc R . . C8 C 0.83392(11) 0.87848(8) 0.92999(7) 0.01462(18) Uani 1 1 d . . . H8A H 0.7866 0.8388 0.9694 0.018 Uiso 1 1 calc R . . H8B H 0.9346 0.8917 0.9541 0.018 Uiso 1 1 calc R . . C9 C 0.79126(11) 0.98162(8) 0.92872(8) 0.01707(19) Uani 1 1 d . . . H9A H 0.8124 1.0201 0.9906 0.020 Uiso 1 1 calc R . . H9B H 0.8457 1.0238 0.8941 0.020 Uiso 1 1 calc R . . C10 C 0.63785(11) 0.96596(9) 0.88755(8) 0.0206(2) Uani 1 1 d . . . H10A H 0.5831 0.9313 0.9263 0.025 Uiso 1 1 calc R . . H10B H 0.6159 1.0341 0.8841 0.025 Uiso 1 1 calc R . . C11 C 0.59804(11) 0.90072(8) 0.79435(8) 0.0186(2) Uani 1 1 d . . . H11A H 0.6442 0.9390 0.7537 0.022 Uiso 1 1 calc R . . H11B H 0.4971 0.8877 0.7711 0.022 Uiso 1 1 calc R . . C12 C 0.63979(10) 0.79742(8) 0.79610(7) 0.01450(18) Uani 1 1 d . . . H12A H 0.6160 0.7574 0.7347 0.017 Uiso 1 1 calc R . . H12B H 0.5879 0.7566 0.8329 0.017 Uiso 1 1 calc R . . C21 C 1.03760(10) 0.73312(7) 0.88101(7) 0.01161(16) Uani 1 1 d . . . C22 C 1.15556(10) 0.75951(7) 0.84565(7) 0.01152(16) Uani 1 1 d . . . C23 C 1.28617(10) 0.77836(8) 0.90320(7) 0.01435(18) Uani 1 1 d . . . H23 H 1.3657 0.7918 0.8790 0.017 Uiso 1 1 calc R . . C24 C 1.30334(11) 0.77815(8) 0.99398(7) 0.01557(18) Uani 1 1 d . . . H24 H 1.3931 0.7912 1.0313 0.019 Uiso 1 1 calc R . . C25 C 1.18736(11) 0.75859(8) 1.02975(7) 0.01575(18) Uani 1 1 d . . . H25 H 1.1972 0.7619 1.0923 0.019 Uiso 1 1 calc R . . C26 C 1.05725(11) 0.73426(8) 0.97356(7) 0.01403(18) Uani 1 1 d . . . H26 H 0.9787 0.7178 0.9983 0.017 Uiso 1 1 calc R . . C31 C 1.16001(10) 0.77621(8) 0.75223(7) 0.01192(17) Uani 1 1 d . . . C32 C 1.16777(10) 0.87719(8) 0.73316(7) 0.01345(17) Uani 1 1 d . . . C37 C 1.15733(11) 0.96591(8) 0.80165(7) 0.01492(18) Uani 1 1 d . . . H37 H 1.1166 0.9350 0.8487 0.018 Uiso 1 1 calc R . . C38 C 1.30050(12) 1.03409(9) 0.84708(8) 0.0210(2) Uani 1 1 d . . . H38A H 1.3562 0.9928 0.8790 0.032 Uiso 1 1 calc R . . H38B H 1.2912 1.0916 0.8895 0.032 Uiso 1 1 calc R . . H38C H 1.3458 1.0615 0.8018 0.032 Uiso 1 1 calc R . . C39 C 1.06342(12) 1.03237(9) 0.76148(8) 0.0205(2) Uani 1 1 d . . . H39A H 1.1063 1.0701 0.7200 0.031 Uiso 1 1 calc R . . H39B H 1.0500 1.0818 0.8094 0.031 Uiso 1 1 calc R . . H39C H 0.9739 0.9877 0.7293 0.031 Uiso 1 1 calc R . . C33 C 1.18692(11) 0.89618(8) 0.64956(7) 0.01695(19) Uani 1 1 d . . . H33 H 1.1925 0.9640 0.6365 0.020 Uiso 1 1 calc R . . C34 C 1.19811(12) 0.81801(9) 0.58455(7) 0.01775(19) Uani 1 1 d . . . C40 C 1.21676(15) 0.83937(10) 0.49326(8) 0.0254(2) Uani 1 1 d . . . H40 H 1.2148 0.7719 0.4565 0.030 Uiso 1 1 calc R . . C41 C 1.3554(2) 0.91046(14) 0.50000(11) 0.0464(4) Uani 1 1 d . . . H41A H 1.3668 0.9202 0.4401 0.070 Uiso 1 1 calc R . . H41B H 1.4286 0.8799 0.5285 0.070 Uiso 1 1 calc R . . H41C H 1.3610 0.9775 0.5358 0.070 Uiso 1 1 calc R . . C42 C 1.0991(2) 0.88136(18) 0.44463(11) 0.0511(5) Uani 1 1 d . . . H42A H 1.0108 0.8323 0.4392 0.077 Uiso 1 1 calc R . . H42B H 1.1126 0.8905 0.3850 0.077 Uiso 1 1 calc R . . H42C H 1.0986 0.9481 0.4786 0.077 Uiso 1 1 calc R . . C35 C 1.19228(11) 0.71958(8) 0.60544(7) 0.01650(19) Uani 1 1 d . . . H35 H 1.2010 0.6662 0.5619 0.020 Uiso 1 1 calc R . . C36 C 1.17402(10) 0.69675(8) 0.68842(7) 0.01314(17) Uani 1 1 d . . . C43 C 1.17468(11) 0.58875(8) 0.70864(7) 0.01478(18) Uani 1 1 d . . . H43 H 1.1328 0.5807 0.7614 0.018 Uiso 1 1 calc R . . C44 C 1.32279(12) 0.57592(9) 0.73397(9) 0.0250(2) Uani 1 1 d . . . H44A H 1.3685 0.5882 0.6849 0.038 Uiso 1 1 calc R . . H44B H 1.3214 0.5055 0.7454 0.038 Uiso 1 1 calc R . . H44C H 1.3733 0.6258 0.7879 0.038 Uiso 1 1 calc R . . C45 C 1.09099(12) 0.50206(9) 0.63163(8) 0.0190(2) Uani 1 1 d . . . H45A H 0.9968 0.5112 0.6142 0.029 Uiso 1 1 calc R . . H45B H 1.0881 0.4350 0.6509 0.029 Uiso 1 1 calc R . . H45C H 1.1345 0.5045 0.5805 0.029 Uiso 1 1 calc R . . N1 N 0.62858(10) 0.42076(7) 0.90931(6) 0.01531(16) Uani 1 1 d D . . H1A H 0.5706(15) 0.4309(12) 0.9423(10) 0.018 Uiso 1 1 d D . . H1B H 0.6856(15) 0.3894(11) 0.9380(10) 0.018 Uiso 1 1 d D . . C51 C 0.55908(11) 0.35997(8) 0.82262(7) 0.01575(19) Uani 1 1 d . . . C52 C 0.41637(12) 0.32595(9) 0.80068(8) 0.0194(2) Uani 1 1 d . . . H52 H 0.3642 0.3408 0.8433 0.023 Uiso 1 1 calc R . . C53 C 0.35002(13) 0.27009(9) 0.71615(9) 0.0231(2) Uani 1 1 d . . . H53 H 0.2523 0.2478 0.7006 0.028 Uiso 1 1 calc R . . C54 C 0.42646(14) 0.24683(9) 0.65441(8) 0.0239(2) Uani 1 1 d . . . H54 H 0.3812 0.2080 0.5969 0.029 Uiso 1 1 calc R . . C55 C 0.56881(13) 0.28048(9) 0.67695(8) 0.0208(2) Uani 1 1 d . . . H55 H 0.6204 0.2641 0.6344 0.025 Uiso 1 1 calc R . . C56 C 0.63836(12) 0.33799(8) 0.76079(7) 0.01658(19) Uani 1 1 d . . . C57 C 0.79095(11) 0.37169(8) 0.78711(7) 0.01619(19) Uani 1 1 d . . . C58 C 0.86812(13) 0.30140(9) 0.76275(8) 0.0202(2) Uani 1 1 d . . . H58 H 0.8226 0.2387 0.7227 0.024 Uiso 1 1 calc R . . C59 C 1.00960(13) 0.32183(9) 0.79602(9) 0.0231(2) Uani 1 1 d . . . H59 H 1.0607 0.2740 0.7784 0.028 Uiso 1 1 calc R . . C60 C 1.07563(12) 0.41282(9) 0.85532(9) 0.0217(2) Uani 1 1 d . . . H60 H 1.1716 0.4260 0.8809 0.026 Uiso 1 1 calc R . . C61 C 1.00070(12) 0.48505(9) 0.87735(8) 0.0179(2) Uani 1 1 d . . . H61 H 1.0475 0.5476 0.9172 0.022 Uiso 1 1 calc R . . C62 C 0.85874(11) 0.46797(8) 0.84238(7) 0.01498(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 Cl1 0.01966(11) 0.01510(10) 0.02174(12) 0.00532(9) 0.01307(9) 0.00675(9) Pd1 0.01256(4) 0.01066(4) 0.01439(4) 0.00428(3) 0.00725(3) 0.00427(3) P1 0.01047(10) 0.01065(10) 0.01260(11) 0.00319(8) 0.00442(8) 0.00296(8) C1 0.0117(4) 0.0130(4) 0.0128(4) 0.0030(3) 0.0035(3) 0.0026(3) C2 0.0132(4) 0.0139(4) 0.0181(5) 0.0028(4) 0.0030(4) 0.0008(3) C3 0.0162(5) 0.0178(5) 0.0185(5) -0.0008(4) 0.0001(4) 0.0021(4) C4 0.0175(5) 0.0244(5) 0.0151(5) 0.0022(4) 0.0001(4) 0.0020(4) C5 0.0165(5) 0.0253(5) 0.0138(5) 0.0054(4) 0.0033(4) 0.0013(4) C6 0.0140(4) 0.0160(4) 0.0141(4) 0.0049(4) 0.0025(3) 0.0007(3) C7 0.0118(4) 0.0113(4) 0.0161(4) 0.0031(3) 0.0042(3) 0.0033(3) C8 0.0137(4) 0.0136(4) 0.0161(4) 0.0007(3) 0.0032(3) 0.0036(3) C9 0.0146(4) 0.0132(4) 0.0225(5) -0.0001(4) 0.0036(4) 0.0038(4) C10 0.0153(5) 0.0170(5) 0.0285(6) -0.0019(4) 0.0032(4) 0.0069(4) C11 0.0157(4) 0.0161(5) 0.0241(5) 0.0029(4) 0.0019(4) 0.0068(4) C12 0.0122(4) 0.0136(4) 0.0177(5) 0.0020(3) 0.0030(3) 0.0038(3) C21 0.0124(4) 0.0109(4) 0.0128(4) 0.0031(3) 0.0038(3) 0.0041(3) C22 0.0121(4) 0.0103(4) 0.0130(4) 0.0024(3) 0.0038(3) 0.0032(3) C23 0.0123(4) 0.0138(4) 0.0172(5) 0.0036(3) 0.0032(3) 0.0033(3) C24 0.0160(4) 0.0134(4) 0.0166(5) 0.0027(4) 0.0001(4) 0.0049(4) C25 0.0208(5) 0.0150(4) 0.0128(4) 0.0034(3) 0.0029(4) 0.0074(4) C26 0.0168(4) 0.0145(4) 0.0136(4) 0.0047(3) 0.0060(3) 0.0061(4) C31 0.0101(4) 0.0137(4) 0.0127(4) 0.0037(3) 0.0039(3) 0.0023(3) C32 0.0129(4) 0.0139(4) 0.0149(4) 0.0041(3) 0.0050(3) 0.0033(3) C37 0.0170(4) 0.0128(4) 0.0173(5) 0.0042(4) 0.0069(4) 0.0048(4) C38 0.0199(5) 0.0180(5) 0.0235(5) 0.0003(4) 0.0048(4) 0.0029(4) C39 0.0217(5) 0.0167(5) 0.0271(6) 0.0081(4) 0.0085(4) 0.0080(4) C33 0.0197(5) 0.0161(5) 0.0177(5) 0.0070(4) 0.0078(4) 0.0042(4) C34 0.0200(5) 0.0195(5) 0.0161(5) 0.0061(4) 0.0089(4) 0.0036(4) C40 0.0375(7) 0.0249(6) 0.0192(5) 0.0080(4) 0.0160(5) 0.0076(5) C41 0.0553(10) 0.0432(9) 0.0361(8) 0.0011(7) 0.0291(8) -0.0132(8) C42 0.0686(12) 0.0794(14) 0.0280(7) 0.0284(8) 0.0228(8) 0.0457(11) C35 0.0178(5) 0.0172(5) 0.0157(5) 0.0026(4) 0.0076(4) 0.0036(4) C36 0.0113(4) 0.0138(4) 0.0148(4) 0.0027(3) 0.0047(3) 0.0023(3) C43 0.0160(4) 0.0127(4) 0.0159(4) 0.0021(3) 0.0048(4) 0.0031(3) C44 0.0185(5) 0.0191(5) 0.0350(7) 0.0024(5) -0.0010(5) 0.0071(4) C45 0.0190(5) 0.0154(5) 0.0211(5) -0.0008(4) 0.0041(4) 0.0033(4) N1 0.0187(4) 0.0131(4) 0.0182(4) 0.0052(3) 0.0106(3) 0.0054(3) C51 0.0206(5) 0.0112(4) 0.0190(5) 0.0058(4) 0.0098(4) 0.0047(4) C52 0.0204(5) 0.0162(5) 0.0252(5) 0.0068(4) 0.0108(4) 0.0048(4) C53 0.0215(5) 0.0199(5) 0.0279(6) 0.0065(4) 0.0062(4) 0.0027(4) C54 0.0292(6) 0.0193(5) 0.0218(5) 0.0033(4) 0.0052(5) 0.0032(4) C55 0.0277(6) 0.0174(5) 0.0196(5) 0.0037(4) 0.0101(4) 0.0057(4) C56 0.0215(5) 0.0125(4) 0.0199(5) 0.0060(4) 0.0107(4) 0.0057(4) C57 0.0209(5) 0.0151(4) 0.0181(5) 0.0068(4) 0.0119(4) 0.0073(4) C58 0.0281(6) 0.0161(5) 0.0234(5) 0.0060(4) 0.0160(4) 0.0098(4) C59 0.0283(6) 0.0208(5) 0.0311(6) 0.0112(5) 0.0191(5) 0.0149(5) C60 0.0210(5) 0.0224(5) 0.0304(6) 0.0126(5) 0.0136(4) 0.0121(4) C61 0.0189(5) 0.0169(5) 0.0234(5) 0.0089(4) 0.0101(4) 0.0081(4) C62 0.0181(5) 0.0147(4) 0.0177(5) 0.0072(4) 0.0106(4) 0.0074(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Pd1 2.4121(3) . ? Pd1 C62 2.0170(10) . ? Pd1 N1 2.1263(9) . ? Pd1 P1 2.2857(3) . ? P1 C21 1.8419(10) . ? P1 C7 1.8526(10) . ? P1 C1 1.8600(11) . ? C1 C2 1.5427(14) . ? C1 C6 1.5428(14) . ? C1 H1 1.0000 . ? C2 C3 1.5275(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5267(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5233(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.5333(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5373(14) . ? C7 C12 1.5396(14) . ? C7 H7 1.0000 . ? C8 C9 1.5330(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.5264(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5240(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.5314(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C21 C26 1.4076(14) . ? C21 C22 1.4124(13) . ? C22 C23 1.4032(14) . ? C22 C31 1.5013(14) . ? C23 C24 1.3846(15) . ? C23 H23 0.9500 . ? C24 C25 1.3895(15) . ? C24 H24 0.9500 . ? C25 C26 1.3854(15) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.4077(14) . ? C31 C32 1.4125(14) . ? C32 C33 1.3943(14) . ? C32 C37 1.5254(15) . ? C37 C38 1.5315(16) . ? C37 C39 1.5336(15) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C33 C34 1.3966(15) . ? C33 H33 0.9500 . ? C34 C35 1.3913(15) . ? C34 C40 1.5188(16) . ? C40 C41 1.509(2) . ? C40 C42 1.533(2) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C35 C36 1.3974(14) . ? C35 H35 0.9500 . ? C36 C43 1.5217(14) . ? C43 C44 1.5311(16) . ? C43 C45 1.5325(15) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? N1 C51 1.4446(15) . ? N1 H1A 0.872(13) . ? N1 H1B 0.871(13) . ? C51 C52 1.3884(16) . ? C51 C56 1.4067(15) . ? C52 C53 1.3905(17) . ? C52 H52 0.9500 . ? C53 C54 1.3886(18) . ? C53 H53 0.9500 . ? C54 C55 1.3845(18) . ? C54 H54 0.9500 . ? C55 C56 1.3961(16) . ? C55 H55 0.9500 . ? C56 C57 1.4827(16) . ? C57 C58 1.4043(15) . ? C57 C62 1.4147(15) . ? C58 C59 1.3875(18) . ? C58 H58 0.9500 . ? C59 C60 1.3873(18) . ? C59 H59 0.9500 . ? C60 C61 1.3973(15) . ? C60 H60 0.9500 . ? C61 C62 1.3997(15) . ? C61 H61 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C62 Pd1 N1 82.41(4) . . ? C62 Pd1 P1 90.81(3) . . ? N1 Pd1 P1 166.04(3) . . ? C62 Pd1 Cl1 166.02(3) . . ? N1 Pd1 Cl1 86.65(3) . . ? P1 Pd1 Cl1 101.681(13) . . ? C21 P1 C7 103.33(5) . . ? C21 P1 C1 111.18(5) . . ? C7 P1 C1 104.00(5) . . ? C21 P1 Pd1 110.14(3) . . ? C7 P1 Pd1 117.65(3) . . ? C1 P1 Pd1 110.24(3) . . ? C2 C1 C6 109.33(8) . . ? C2 C1 P1 110.97(7) . . ? C6 C1 P1 116.43(7) . . ? C2 C1 H1 106.5 . . ? C6 C1 H1 106.5 . . ? P1 C1 H1 106.5 . . ? C3 C2 C1 111.03(9) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 111.33(9) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 110.21(9) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.84(9) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C1 111.20(9) . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C12 109.91(8) . . ? C8 C7 P1 114.65(7) . . ? C12 C7 P1 111.67(7) . . ? C8 C7 H7 106.7 . . ? C12 C7 H7 106.7 . . ? P1 C7 H7 106.7 . . ? C9 C8 C7 110.01(9) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 111.90(9) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.29(9) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.84(9) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C7 110.66(8) . . ? C11 C12 H12A 109.5 . . ? C7 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C26 C21 C22 118.08(9) . . ? C26 C21 P1 111.23(7) . . ? C22 C21 P1 130.67(8) . . ? C23 C22 C21 118.51(9) . . ? C23 C22 C31 113.87(9) . . ? C21 C22 C31 127.53(9) . . ? C24 C23 C22 122.40(10) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 119.05(10) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 119.56(10) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C21 122.18(10) . . ? C25 C26 H26 118.9 . . ? C21 C26 H26 118.9 . . ? C36 C31 C32 120.43(9) . . ? C36 C31 C22 120.85(9) . . ? C32 C31 C22 118.23(9) . . ? C33 C32 C31 118.86(10) . . ? C33 C32 C37 119.26(9) . . ? C31 C32 C37 121.88(9) . . ? C32 C37 C38 110.85(9) . . ? C32 C37 C39 112.86(9) . . ? C38 C37 C39 109.95(9) . . ? C32 C37 H37 107.7 . . ? C38 C37 H37 107.7 . . ? C39 C37 H37 107.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C32 C33 C34 121.68(10) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 118.37(10) . . ? C35 C34 C40 120.49(10) . . ? C33 C34 C40 121.14(10) . . ? C41 C40 C34 111.09(12) . . ? C41 C40 C42 111.38(14) . . ? C34 C40 C42 112.18(11) . . ? C41 C40 H40 107.3 . . ? C34 C40 H40 107.3 . . ? C42 C40 H40 107.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C34 C35 C36 122.13(10) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C35 C36 C31 118.51(9) . . ? C35 C36 C43 119.62(9) . . ? C31 C36 C43 121.83(9) . . ? C36 C43 C44 110.48(9) . . ? C36 C43 C45 113.57(9) . . ? C44 C43 C45 109.35(9) . . ? C36 C43 H43 107.7 . . ? C44 C43 H43 107.7 . . ? C45 C43 H43 107.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 N1 Pd1 106.45(6) . . ? C51 N1 H1A 111.8(10) . . ? Pd1 N1 H1A 112.3(10) . . ? C51 N1 H1B 110.6(10) . . ? Pd1 N1 H1B 108.4(10) . . ? H1A N1 H1B 107.3(14) . . ? C52 C51 C56 121.00(11) . . ? C52 C51 N1 120.20(10) . . ? C56 C51 N1 118.79(10) . . ? C51 C52 C53 119.81(11) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 120.09(11) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 119.77(11) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 121.53(11) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? C55 C56 C51 117.79(11) . . ? C55 C56 C57 122.24(10) . . ? C51 C56 C57 119.91(10) . . ? C58 C57 C62 119.84(10) . . ? C58 C57 C56 118.25(10) . . ? C62 C57 C56 121.66(9) . . ? C59 C58 C57 121.23(11) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C60 C59 C58 119.32(10) . . ? C60 C59 H59 120.3 . . ? C58 C59 H59 120.3 . . ? C59 C60 C61 119.88(11) . . ? C59 C60 H60 120.1 . . ? C61 C60 H60 120.1 . . ? C60 C61 C62 121.93(11) . . ? C60 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C61 C62 C57 117.55(10) . . ? C61 C62 Pd1 122.45(8) . . ? C57 C62 Pd1 118.95(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Cl1 0.872(13) 2.637(14) 3.4080(10) 148.1(13) 2_667 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.850 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.054 # Attachment '- 2L13.cif' data_x12094 _database_code_depnum_ccdc_archive 'CCDC 891253' #TrackingRef '- 2L13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57.50 H45 Cl4 N P2 Pd' _chemical_formula_weight 1060.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5500(18) _cell_length_b 13.7601(17) _cell_length_c 23.806(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.469(3) _cell_angle_gamma 90.00 _cell_volume 4751.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9551 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 32.17 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7605 _exptl_absorpt_correction_T_max 0.8397 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus sealed tube' _diffrn_radiation_monochromator 'Incoatech ImuS multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 420406 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 32.03 _reflns_number_total 16548 _reflns_number_gt 14420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0392P)^2^+4.0122P] 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 16548 _refine_ls_number_parameters 838 _refine_ls_number_restraints 1187 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.64100(2) 1.01981(2) 0.876300(16) 0.02190(7) Uani 1 1 d . . . P1 P 0.47763(2) 0.78269(2) 0.775588(15) 0.01596(6) Uani 1 1 d D . . C1 C 0.39475(9) 0.80600(10) 0.71506(6) 0.0183(2) Uani 1 1 d D . . C2 C 0.41678(12) 0.87500(12) 0.67530(7) 0.0262(3) Uani 1 1 d D . . H2 H 0.4735 0.9092 0.6802 0.031 Uiso 1 1 calc R . . C3 C 0.35587(15) 0.89385(14) 0.62850(8) 0.0360(4) Uani 1 1 d D . . H3 H 0.3703 0.9426 0.6023 0.043 Uiso 1 1 calc R . . C4 C 0.27449(13) 0.84210(13) 0.61993(7) 0.0329(4) Uani 1 1 d D . . H4 H 0.2326 0.8561 0.5884 0.040 Uiso 1 1 calc R . . C5 C 0.25426(11) 0.76969(12) 0.65758(7) 0.0263(3) Uani 1 1 d D . . H5 H 0.1996 0.7322 0.6509 0.032 Uiso 1 1 calc R . . C6 C 0.31380(10) 0.75179(11) 0.70508(6) 0.0210(3) Uani 1 1 d D . . H6 H 0.2994 0.7024 0.7309 0.025 Uiso 1 1 calc R . . C7 C 0.55095(9) 0.69320(10) 0.74531(6) 0.0182(2) Uani 1 1 d . . . C8 C 0.51160(11) 0.60856(11) 0.72200(7) 0.0258(3) Uani 1 1 d . . . H8 H 0.4473 0.5976 0.7228 0.031 Uiso 1 1 calc R . . C9 C 0.56630(13) 0.54034(13) 0.69757(8) 0.0325(4) Uani 1 1 d . . . H9 H 0.5396 0.4821 0.6823 0.039 Uiso 1 1 calc R . . C10 C 0.66029(12) 0.55720(12) 0.69546(8) 0.0296(3) Uani 1 1 d . . . H10 H 0.6978 0.5103 0.6789 0.036 Uiso 1 1 calc R . . C11 C 0.69907(11) 0.64211(12) 0.71742(7) 0.0255(3) Uani 1 1 d . . . H11 H 0.7630 0.6539 0.7153 0.031 Uiso 1 1 calc R . . C12 C 0.64490(10) 0.71025(11) 0.74253(6) 0.0218(3) Uani 1 1 d . . . H12 H 0.6719 0.7683 0.7578 0.026 Uiso 1 1 calc R . . C31 C 0.40976(9) 0.72363(10) 0.82748(6) 0.0171(2) Uani 1 1 d . . . C32 C 0.32475(10) 0.77170(11) 0.83416(6) 0.0197(2) Uani 1 1 d . . . H32 H 0.3069 0.8247 0.8101 0.024 Uiso 1 1 calc R . . C33 C 0.26831(10) 0.74341(11) 0.87427(6) 0.0219(3) Uani 1 1 d . . . H33 H 0.2113 0.7758 0.8773 0.026 Uiso 1 1 calc R . . C34 C 0.29417(10) 0.66640(11) 0.91120(6) 0.0201(2) Uani 1 1 d . . . C35 C 0.23615(11) 0.63799(12) 0.95354(7) 0.0251(3) Uani 1 1 d . . . H35 H 0.1775 0.6678 0.9551 0.030 Uiso 1 1 calc R . . C36 C 0.26387(11) 0.56796(13) 0.99211(7) 0.0267(3) Uani 1 1 d . . . H36 H 0.2248 0.5494 1.0204 0.032 Uiso 1 1 calc R . . C37 C 0.35027(11) 0.52379(11) 0.98954(6) 0.0246(3) Uani 1 1 d . . . H37 H 0.3701 0.4766 1.0170 0.030 Uiso 1 1 calc R . . C38 C 0.40689(10) 0.54761(11) 0.94792(6) 0.0215(3) Uani 1 1 d . . . H38 H 0.4643 0.5152 0.9464 0.026 Uiso 1 1 calc R . . C39 C 0.38075(10) 0.62002(10) 0.90724(6) 0.0182(2) Uani 1 1 d . . . C40 C 0.43956(9) 0.64985(10) 0.86430(6) 0.0167(2) Uani 1 1 d . . . C41 C 0.61278(9) 0.65475(10) 0.87946(6) 0.0177(2) Uani 1 1 d . A . C42 C 0.69996(10) 0.60747(10) 0.88018(6) 0.0197(2) Uani 1 1 d . . . H42 H 0.7542 0.6424 0.8924 0.024 Uiso 1 1 calc R . . C43 C 0.70711(10) 0.51288(11) 0.86372(6) 0.0214(3) Uani 1 1 d . . . H43 H 0.7661 0.4831 0.8645 0.026 Uiso 1 1 calc R . . C44 C 0.62787(10) 0.45896(11) 0.84561(6) 0.0205(3) Uani 1 1 d . . . C45 C 0.63479(11) 0.36101(11) 0.82692(7) 0.0257(3) Uani 1 1 d . . . H45 H 0.6936 0.3310 0.8271 0.031 Uiso 1 1 calc R . . C46 C 0.55748(12) 0.30958(12) 0.80864(8) 0.0287(3) Uani 1 1 d . . . H46 H 0.5627 0.2444 0.7962 0.034 Uiso 1 1 calc R . . C47 C 0.47015(11) 0.35406(11) 0.80847(7) 0.0256(3) Uani 1 1 d . . . H47 H 0.4167 0.3186 0.7953 0.031 Uiso 1 1 calc R . . C48 C 0.46108(10) 0.44803(11) 0.82713(6) 0.0215(3) Uani 1 1 d . . . H48 H 0.4014 0.4760 0.8274 0.026 Uiso 1 1 calc R . . C49 C 0.53967(10) 0.50376(10) 0.84596(6) 0.0184(2) Uani 1 1 d . . . C50 C 0.53289(9) 0.60311(10) 0.86316(6) 0.0170(2) Uani 1 1 d . . . P2 P 0.60911(3) 0.78563(3) 0.895622(16) 0.01882(7) Uani 1 1 d DU . . C13 C 0.7255(4) 0.8107(4) 0.9268(4) 0.0202(11) Uani 0.58(3) 1 d PDU A 1 C14 C 0.7498(5) 0.8095(7) 0.9845(3) 0.0294(12) Uani 0.58(3) 1 d PDU A 1 H14 H 0.7041 0.7994 1.0104 0.035 Uiso 0.58(3) 1 calc PR A 1 C15 C 0.8420(6) 0.8234(7) 1.0042(4) 0.0437(16) Uani 0.58(3) 1 d PDU A 1 H15 H 0.8591 0.8222 1.0435 0.052 Uiso 0.58(3) 1 calc PR A 1 C16 C 0.9082(5) 0.8387(8) 0.9667(5) 0.0442(18) Uani 0.58(3) 1 d PDU A 1 H16 H 0.9704 0.8494 0.9805 0.053 Uiso 0.58(3) 1 calc PR A 1 C17 C 0.8850(5) 0.8387(9) 0.9094(5) 0.0354(15) Uani 0.58(3) 1 d PDU A 1 H17 H 0.9312 0.8467 0.8837 0.043 Uiso 0.58(3) 1 calc PR A 1 C18 C 0.7930(6) 0.8267(11) 0.8898(4) 0.0272(15) Uani 0.58(3) 1 d PDU A 1 H18 H 0.7762 0.8296 0.8504 0.033 Uiso 0.58(3) 1 calc PR A 1 C13A C 0.7310(7) 0.8074(6) 0.9172(7) 0.030(2) Uani 0.42(3) 1 d PDU A 2 C14A C 0.7642(10) 0.8115(13) 0.9736(7) 0.047(3) Uani 0.42(3) 1 d PDU A 2 H14A H 0.7227 0.8078 1.0024 0.056 Uiso 0.42(3) 1 calc PR A 2 C15A C 0.8598(11) 0.8212(12) 0.9877(9) 0.065(3) Uani 0.42(3) 1 d PDU A 2 H15A H 0.8825 0.8236 1.0262 0.078 Uiso 0.42(3) 1 calc PR A 2 C16A C 0.9191(8) 0.8270(10) 0.9468(10) 0.054(3) Uani 0.42(3) 1 d PDU A 2 H16A H 0.9837 0.8289 0.9566 0.065 Uiso 0.42(3) 1 calc PR A 2 C17A C 0.8864(8) 0.8302(9) 0.8914(9) 0.038(2) Uani 0.42(3) 1 d PDU A 2 H17A H 0.9279 0.8391 0.8630 0.046 Uiso 0.42(3) 1 calc PR A 2 C18A C 0.7920(7) 0.8204(13) 0.8765(7) 0.0251(19) Uani 0.42(3) 1 d PDU A 2 H18A H 0.7699 0.8226 0.8380 0.030 Uiso 0.42(3) 1 calc PR A 2 C19 C 0.53855(11) 0.79027(11) 0.95501(6) 0.0228(3) Uani 1 1 d D A . C20 C 0.47027(11) 0.86058(12) 0.95646(7) 0.0261(3) Uani 1 1 d D . . H20 H 0.4633 0.9083 0.9276 0.031 Uiso 1 1 calc R A . C21 C 0.41201(14) 0.86114(14) 1.00016(8) 0.0339(4) Uani 1 1 d D A . H21 H 0.3658 0.9097 1.0012 0.041 Uiso 1 1 calc R . . C22 C 0.42118(17) 0.79131(14) 1.04202(8) 0.0401(4) Uani 1 1 d D . . H22 H 0.3806 0.7915 1.0714 0.048 Uiso 1 1 calc R A . C23 C 0.48893(17) 0.72148(14) 1.04136(8) 0.0407(5) Uani 1 1 d D A . H23 H 0.4953 0.6739 1.0703 0.049 Uiso 1 1 calc R . . C24 C 0.54798(14) 0.72098(12) 0.99808(7) 0.0321(4) Uani 1 1 d D . . H24 H 0.5951 0.6732 0.9978 0.039 Uiso 1 1 calc R A . Pd1 Pd 0.556273(7) 0.899851(7) 0.824466(4) 0.01627(3) Uani 1 1 d DU A . C51 C 0.5150(3) 1.0077(3) 0.76923(17) 0.0196(3) Uani 0.778(3) 1 d PDU A 1 C52 C 0.5831(4) 1.0398(3) 0.73473(17) 0.0197(6) Uani 0.778(3) 1 d PDU A 1 H52 H 0.6432 1.0125 0.7395 0.024 Uiso 0.778(3) 1 calc PR A 1 C53 C 0.5644(5) 1.1107(4) 0.6938(2) 0.0267(8) Uani 0.778(3) 1 d PDU A 1 H53 H 0.6115 1.1314 0.6711 0.032 Uiso 0.778(3) 1 calc PR A 1 C54 C 0.4767(7) 1.1514(8) 0.6862(4) 0.0309(4) Uani 0.778(3) 1 d PDU A 1 H54 H 0.4628 1.1977 0.6572 0.037 Uiso 0.778(3) 1 calc PR A 1 C55 C 0.4101(5) 1.1237(5) 0.7214(3) 0.0256(9) Uani 0.778(3) 1 d PDU A 1 H55 H 0.3512 1.1536 0.7174 0.031 Uiso 0.778(3) 1 calc PR A 1 C56 C 0.4277(3) 1.0524(4) 0.7631(2) 0.0206(7) Uani 0.778(3) 1 d PDU A 1 C57 C 0.34879(15) 1.02641(16) 0.79691(10) 0.0202(4) Uani 0.778(3) 1 d PDU A 1 C58 C 0.26708(15) 0.99051(15) 0.76990(12) 0.0228(4) Uani 0.778(3) 1 d PDU A 1 H58 H 0.2637 0.9805 0.7303 0.027 Uiso 0.778(3) 1 calc PR A 1 C59 C 0.19032(13) 0.96882(15) 0.79921(10) 0.0256(4) Uani 0.778(3) 1 d PDU A 1 H59 H 0.1357 0.9437 0.7800 0.031 Uiso 0.778(3) 1 calc PR A 1 C60 C 0.19523(17) 0.98460(19) 0.85687(11) 0.0275(5) Uani 0.778(3) 1 d PDU A 1 H60 H 0.1436 0.9698 0.8774 0.033 Uiso 0.778(3) 1 calc PR A 1 C61 C 0.27458(18) 1.0216(2) 0.88490(12) 0.0274(5) Uani 0.778(3) 1 d PDU A 1 H61 H 0.2770 1.0317 0.9245 0.033 Uiso 0.778(3) 1 calc PR A 1 C62 C 0.35201(15) 1.04440(14) 0.85512(9) 0.0228(4) Uani 0.778(3) 1 d PDU A 1 N1 N 0.42510(15) 1.09274(16) 0.88261(9) 0.0269(4) Uani 0.778(3) 1 d PDU A 1 H1A H 0.4274(18) 1.091(2) 0.9204(6) 0.032 Uiso 0.778(3) 1 d PD A 1 H1B H 0.4785(11) 1.088(2) 0.8678(11) 0.032 Uiso 0.778(3) 1 d PD A 1 C51A C 0.5185(11) 1.0074(9) 0.7686(6) 0.0196(3) Uani 0.222(3) 1 d PDU A 2 C52A C 0.5789(14) 1.0292(14) 0.7275(7) 0.0197(6) Uani 0.222(3) 1 d PDU A 2 H52A H 0.6348 0.9937 0.7271 0.024 Uiso 0.222(3) 1 calc PR A 2 C53A C 0.560(2) 1.1012(18) 0.6870(10) 0.0267(8) Uani 0.222(3) 1 d PDU A 2 H53A H 0.6023 1.1153 0.6597 0.032 Uiso 0.222(3) 1 calc PR A 2 C54A C 0.477(2) 1.152(3) 0.6876(14) 0.0309(4) Uani 0.222(3) 1 d PDU A 2 H54A H 0.4630 1.2023 0.6610 0.037 Uiso 0.222(3) 1 calc PR A 2 C55A C 0.415(2) 1.129(2) 0.7271(11) 0.0256(9) Uani 0.222(3) 1 d PDU A 2 H55A H 0.3583 1.1633 0.7261 0.031 Uiso 0.222(3) 1 calc PR A 2 C56A C 0.4344(13) 1.0582(14) 0.7683(8) 0.0206(7) Uani 0.222(3) 1 d PDU A 2 C57A C 0.3699(5) 1.0452(5) 0.8145(3) 0.0181(13) Uani 0.222(3) 1 d PDU A 2 C58A C 0.4003(5) 1.0617(6) 0.8697(3) 0.0196(13) Uani 0.222(3) 1 d PDU A 2 H58A H 0.4631 1.0786 0.8784 0.023 Uiso 0.222(3) 1 calc PR A 2 C59A C 0.3430(5) 1.0545(6) 0.9132(3) 0.0273(15) Uani 0.222(3) 1 d PDU A 2 H59A H 0.3657 1.0683 0.9509 0.033 Uiso 0.222(3) 1 calc PR A 2 C60A C 0.2527(7) 1.0272(8) 0.9011(4) 0.031(2) Uani 0.222(3) 1 d PDU A 2 H60A H 0.2127 1.0205 0.9305 0.038 Uiso 0.222(3) 1 calc PR A 2 C61A C 0.2207(6) 1.0096(6) 0.8462(4) 0.0280(16) Uani 0.222(3) 1 d PDU A 2 H61A H 0.1581 0.9912 0.8382 0.034 Uiso 0.222(3) 1 calc PR A 2 C62A C 0.2791(4) 1.0181(5) 0.8008(3) 0.0207(13) Uani 0.222(3) 1 d PDU A 2 N1A N 0.2426(5) 1.0021(5) 0.7462(3) 0.0251(14) Uani 0.222(3) 1 d PDU A 2 H1C H 0.284(2) 0.991(6) 0.7208(13) 0.030 Uiso 0.222(3) 1 d PD A 2 H1D H 0.192(4) 0.964(5) 0.7425(15) 0.030 Uiso 0.222(3) 1 d PD A 2 C1S C 0.6875(3) 0.6883(4) 0.56482(19) 0.0559(10) Uani 0.577(5) 1 d PDU B 1 H1S1 H 0.7311 0.7250 0.5429 0.067 Uiso 0.577(5) 1 calc PR B 1 H1S2 H 0.7221 0.6642 0.5995 0.067 Uiso 0.577(5) 1 calc PR B 1 Cl2 Cl 0.6452(2) 0.5908(2) 0.52566(19) 0.1319(17) Uani 0.577(5) 1 d PDU B 1 Cl3 Cl 0.60016(15) 0.7663(2) 0.58326(12) 0.0815(7) Uani 0.577(5) 1 d PDU B 1 C1T C 0.6433(5) 0.6245(6) 0.5633(3) 0.0653(18) Uani 0.423(5) 1 d PDU B 2 H1T1 H 0.5990 0.5745 0.5740 0.078 Uiso 0.423(5) 1 calc PR B 2 H1T2 H 0.7027 0.6118 0.5852 0.078 Uiso 0.423(5) 1 calc PR B 2 Cl2A Cl 0.65937(11) 0.61107(14) 0.49271(9) 0.0503(6) Uani 0.423(5) 1 d PDU B 2 Cl3A Cl 0.6039(4) 0.7356(4) 0.58244(13) 0.1263(19) Uani 0.423(5) 1 d PDU B 2 C2S C 0.5337(11) 1.0665(11) 0.4896(4) 0.086(3) Uani 0.2758(16) 1 d PDU C -1 H2S1 H 0.5966 1.0719 0.4767 0.104 Uiso 0.2758(16) 1 calc PR C -1 H2S2 H 0.4988 1.1254 0.4771 0.104 Uiso 0.2758(16) 1 calc PR C -1 Cl4 Cl 0.54056(19) 1.0594(3) 0.56346(11) 0.0527(7) Uani 0.2758(16) 1 d PDU C -1 Cl5 Cl 0.4782(4) 0.9617(6) 0.4590(2) 0.0747(15) Uani 0.2758(16) 1 d PDU C -1 C2T C 0.518(2) 0.9463(15) 0.5193(12) 0.092(4) Uani 0.120(2) 1 d PDU D -2 H2T1 H 0.5061 0.9248 0.5577 0.110 Uiso 0.120(2) 1 calc PR D -2 H2T2 H 0.5781 0.9173 0.5110 0.110 Uiso 0.120(2) 1 calc PR D -2 Cl5A Cl 0.4350(5) 0.8951(6) 0.4735(3) 0.067(2) Uani 0.120(2) 1 d PDU D -2 Cl4A Cl 0.5336(12) 1.0699(12) 0.5219(9) 0.108(4) Uani 0.120(2) 1 d PDU D -2 C2U C 0.510(3) 1.012(2) 0.4821(8) 0.092(4) Uani 0.104(2) 1 d PDU E -3 H2U1 H 0.4731 0.9539 0.4708 0.110 Uiso 0.104(2) 1 calc PR E -3 H2U2 H 0.5704 1.0054 0.4656 0.110 Uiso 0.104(2) 1 calc PR E -3 Cl4B Cl 0.4539(12) 1.1150(13) 0.4526(7) 0.148(4) Uani 0.104(2) 1 d PDU E -3 Cl5B Cl 0.5302(16) 1.0114(17) 0.5555(6) 0.098(3) Uani 0.104(2) 1 d PDU E -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 Cl1 0.01892(14) 0.01824(14) 0.02807(16) -0.00403(12) -0.00128(12) -0.00205(11) P1 0.01523(14) 0.01480(14) 0.01762(15) 0.00023(11) -0.00028(11) -0.00017(11) C1 0.0186(6) 0.0177(6) 0.0183(6) -0.0001(5) -0.0008(5) 0.0010(5) C2 0.0316(8) 0.0249(7) 0.0213(7) 0.0028(5) -0.0022(6) -0.0064(6) C3 0.0509(11) 0.0308(8) 0.0244(8) 0.0077(6) -0.0090(7) -0.0070(8) C4 0.0393(9) 0.0315(8) 0.0256(8) 0.0008(6) -0.0131(7) 0.0010(7) C5 0.0243(7) 0.0264(7) 0.0269(7) -0.0050(6) -0.0057(6) 0.0011(6) C6 0.0198(6) 0.0202(6) 0.0225(6) -0.0010(5) -0.0009(5) 0.0001(5) C7 0.0175(6) 0.0180(6) 0.0190(6) 0.0003(5) 0.0009(4) 0.0002(5) C8 0.0214(6) 0.0237(7) 0.0329(8) -0.0084(6) 0.0056(6) -0.0028(5) C9 0.0317(8) 0.0254(7) 0.0417(9) -0.0131(7) 0.0110(7) -0.0026(6) C10 0.0291(8) 0.0254(7) 0.0355(8) -0.0037(6) 0.0101(6) 0.0053(6) C11 0.0190(6) 0.0278(7) 0.0301(7) 0.0020(6) 0.0043(5) 0.0040(5) C12 0.0173(6) 0.0227(6) 0.0250(7) 0.0004(5) 0.0004(5) 0.0002(5) C31 0.0161(5) 0.0173(6) 0.0177(6) -0.0007(4) -0.0004(4) -0.0007(4) C32 0.0181(6) 0.0201(6) 0.0207(6) 0.0013(5) -0.0005(5) 0.0022(5) C33 0.0176(6) 0.0255(7) 0.0226(6) 0.0007(5) 0.0006(5) 0.0037(5) C34 0.0192(6) 0.0217(6) 0.0194(6) -0.0006(5) 0.0009(5) -0.0002(5) C35 0.0223(7) 0.0287(7) 0.0247(7) 0.0012(6) 0.0052(5) 0.0008(6) C36 0.0279(7) 0.0293(8) 0.0234(7) 0.0035(6) 0.0060(6) -0.0010(6) C37 0.0299(7) 0.0229(7) 0.0211(6) 0.0037(5) 0.0018(5) 0.0005(6) C38 0.0239(6) 0.0197(6) 0.0205(6) 0.0017(5) 0.0000(5) 0.0006(5) C39 0.0192(6) 0.0172(6) 0.0178(6) -0.0003(4) -0.0006(5) -0.0008(5) C40 0.0161(5) 0.0157(5) 0.0180(6) -0.0011(4) -0.0015(4) -0.0004(4) C41 0.0183(6) 0.0161(5) 0.0184(6) 0.0012(4) -0.0009(4) 0.0005(4) C42 0.0174(6) 0.0203(6) 0.0212(6) 0.0019(5) -0.0002(5) -0.0003(5) C43 0.0189(6) 0.0220(6) 0.0233(6) 0.0018(5) 0.0019(5) 0.0034(5) C44 0.0217(6) 0.0187(6) 0.0212(6) -0.0003(5) 0.0016(5) 0.0022(5) C45 0.0274(7) 0.0206(7) 0.0291(7) -0.0036(6) 0.0019(6) 0.0051(5) C46 0.0337(8) 0.0188(6) 0.0336(8) -0.0062(6) 0.0024(6) 0.0018(6) C47 0.0278(7) 0.0209(7) 0.0277(7) -0.0038(5) -0.0004(6) -0.0028(5) C48 0.0210(6) 0.0194(6) 0.0236(6) -0.0015(5) -0.0014(5) -0.0008(5) C49 0.0199(6) 0.0162(6) 0.0189(6) -0.0001(4) 0.0003(5) 0.0006(5) C50 0.0167(5) 0.0159(5) 0.0182(6) 0.0009(4) -0.0004(4) 0.0007(4) P2 0.01802(15) 0.01566(15) 0.02193(16) 0.00015(12) -0.00382(12) -0.00045(12) C13 0.0160(16) 0.0149(18) 0.029(2) -0.0014(13) -0.0052(14) -0.0014(13) C14 0.0231(19) 0.038(2) 0.025(2) 0.0018(18) -0.0118(16) -0.0048(17) C15 0.033(2) 0.059(3) 0.036(3) 0.007(2) -0.014(2) -0.010(2) C16 0.025(2) 0.056(4) 0.050(4) 0.007(3) -0.014(2) -0.011(2) C17 0.0187(16) 0.037(3) 0.049(3) 0.013(3) -0.004(2) -0.0064(16) C18 0.0249(19) 0.024(3) 0.031(3) 0.005(3) -0.0071(18) -0.0029(15) C13A 0.031(4) 0.021(3) 0.035(5) -0.003(2) -0.014(3) 0.001(2) C14A 0.041(4) 0.057(5) 0.042(5) -0.005(4) -0.003(3) -0.005(4) C15A 0.044(5) 0.096(6) 0.050(6) -0.005(6) -0.029(4) -0.009(5) C16A 0.026(3) 0.060(4) 0.073(8) -0.005(5) -0.018(4) -0.005(3) C17A 0.026(3) 0.021(2) 0.064(6) 0.005(4) -0.013(4) -0.0023(18) C18A 0.017(2) 0.016(2) 0.040(5) 0.002(4) -0.007(3) -0.0040(16) C19 0.0294(7) 0.0188(6) 0.0194(6) -0.0026(5) -0.0020(5) -0.0016(5) C20 0.0300(7) 0.0246(7) 0.0234(7) -0.0013(5) 0.0000(6) 0.0016(6) C21 0.0404(9) 0.0332(9) 0.0290(8) -0.0046(7) 0.0077(7) 0.0028(7) C22 0.0627(13) 0.0319(9) 0.0274(8) -0.0066(7) 0.0155(8) -0.0067(9) C23 0.0763(15) 0.0243(8) 0.0224(8) -0.0009(6) 0.0096(8) -0.0017(9) C24 0.0526(11) 0.0206(7) 0.0228(7) -0.0016(6) 0.0000(7) 0.0039(7) Pd1 0.01509(5) 0.01364(5) 0.01981(5) -0.00016(3) -0.00037(3) -0.00031(3) C51 0.0203(7) 0.0151(5) 0.0231(6) -0.0002(5) -0.0006(5) -0.0011(5) C52 0.0196(8) 0.0158(13) 0.0235(14) -0.0025(9) -0.0007(10) -0.0024(8) C53 0.0268(11) 0.0244(16) 0.0293(17) 0.0053(13) 0.0042(13) -0.0024(10) C54 0.0303(8) 0.0279(8) 0.0342(10) 0.0118(7) 0.0005(7) 0.0025(6) C55 0.0230(11) 0.0219(12) 0.0312(17) 0.0046(13) -0.0023(11) 0.0033(9) C56 0.0197(10) 0.0167(9) 0.0253(13) 0.0008(9) 0.0003(10) 0.0009(8) C57 0.0188(10) 0.0160(9) 0.0254(11) -0.0014(8) -0.0007(8) 0.0019(7) C58 0.0192(9) 0.0203(9) 0.0279(12) 0.0002(9) -0.0048(8) 0.0021(7) C59 0.0167(8) 0.0214(9) 0.0377(11) 0.0003(7) -0.0036(7) 0.0022(6) C60 0.0194(11) 0.0251(12) 0.0380(12) 0.0013(9) 0.0027(9) 0.0027(8) C61 0.0245(12) 0.0299(11) 0.0279(12) -0.0020(10) 0.0026(9) 0.0033(10) C62 0.0191(9) 0.0207(8) 0.0280(10) -0.0024(7) -0.0018(8) 0.0031(7) N1 0.0197(9) 0.0305(11) 0.0299(10) -0.0070(8) -0.0022(7) 0.0010(8) C51A 0.0203(7) 0.0151(5) 0.0231(6) -0.0002(5) -0.0006(5) -0.0011(5) C52A 0.0196(8) 0.0158(13) 0.0235(14) -0.0025(9) -0.0007(10) -0.0024(8) C53A 0.0268(11) 0.0244(16) 0.0293(17) 0.0053(13) 0.0042(13) -0.0024(10) C54A 0.0303(8) 0.0279(8) 0.0342(10) 0.0118(7) 0.0005(7) 0.0025(6) C55A 0.0230(11) 0.0219(12) 0.0312(17) 0.0046(13) -0.0023(11) 0.0033(9) C56A 0.0197(10) 0.0167(9) 0.0253(13) 0.0008(9) 0.0003(10) 0.0009(8) C57A 0.017(3) 0.014(3) 0.023(4) -0.003(2) -0.003(2) 0.000(2) C58A 0.014(4) 0.021(3) 0.023(3) -0.002(3) -0.004(3) 0.001(3) C59A 0.029(3) 0.029(3) 0.025(3) 0.001(3) 0.004(2) 0.008(3) C60A 0.034(4) 0.025(4) 0.037(5) 0.010(4) 0.013(4) 0.006(3) C61A 0.018(3) 0.016(3) 0.052(4) 0.011(3) 0.011(3) 0.004(3) C62A 0.014(3) 0.017(3) 0.030(3) 0.000(3) -0.006(2) 0.001(2) N1A 0.020(3) 0.022(3) 0.033(4) -0.005(3) -0.004(3) -0.004(2) C1S 0.051(2) 0.066(3) 0.051(2) 0.0194(17) 0.0069(17) 0.0207(18) Cl2 0.1050(17) 0.138(2) 0.141(3) -0.059(2) -0.068(2) 0.0664(16) Cl3 0.0662(10) 0.0850(14) 0.0955(15) 0.0198(10) 0.0188(9) 0.0307(9) C1T 0.053(3) 0.097(4) 0.046(2) -0.017(4) 0.006(3) 0.004(4) Cl2A 0.0332(7) 0.0724(10) 0.0461(9) 0.0120(7) 0.0075(6) 0.0114(6) Cl3A 0.215(5) 0.114(3) 0.0434(12) -0.0056(13) -0.0300(17) 0.070(3) C2S 0.090(6) 0.138(6) 0.029(2) -0.034(5) -0.010(5) -0.008(5) Cl4 0.0482(12) 0.0762(19) 0.0341(12) -0.0006(11) 0.0054(9) -0.0151(12) Cl5 0.056(2) 0.110(4) 0.059(3) -0.030(3) 0.008(2) 0.009(2) C2T 0.084(7) 0.129(6) 0.061(7) -0.021(7) -0.007(6) -0.007(7) Cl5A 0.073(4) 0.090(5) 0.035(3) -0.007(3) -0.007(3) 0.016(3) Cl4A 0.098(6) 0.129(6) 0.095(7) -0.037(6) -0.002(6) -0.007(5) C2U 0.083(7) 0.126(7) 0.066(5) -0.038(7) 0.000(7) -0.012(7) Cl4B 0.139(8) 0.184(9) 0.120(7) 0.007(7) -0.001(7) 0.028(7) Cl5B 0.082(6) 0.148(8) 0.065(5) -0.030(5) 0.008(5) -0.021(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 Cl1 Pd1 2.3516(4) . ? P1 C7 1.8148(14) . ? P1 C31 1.8309(14) . ? P1 C1 1.8338(14) . ? P1 Pd1 2.2483(4) . ? C1 C2 1.395(2) . ? C1 C6 1.3989(19) . ? C2 C3 1.393(2) . ? C2 H2 0.9500 . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(2) . ? C4 H4 0.9500 . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.3936(19) . ? C7 C8 1.394(2) . ? C8 C9 1.387(2) . ? C8 H8 0.9500 . ? C9 C10 1.392(2) . ? C9 H9 0.9500 . ? C10 C11 1.382(2) . ? C10 H10 0.9500 . ? C11 C12 1.390(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C31 C40 1.3885(19) . ? C31 C32 1.4224(19) . ? C32 C33 1.364(2) . ? C32 H32 0.9500 . ? C33 C34 1.409(2) . ? C33 H33 0.9500 . ? C34 C35 1.419(2) . ? C34 C39 1.422(2) . ? C35 C36 1.370(2) . ? C35 H35 0.9500 . ? C36 C37 1.402(2) . ? C36 H36 0.9500 . ? C37 C38 1.377(2) . ? C37 H37 0.9500 . ? C38 C39 1.421(2) . ? C38 H38 0.9500 . ? C39 C40 1.4429(19) . ? C40 C50 1.5047(19) . ? C41 C50 1.3915(19) . ? C41 C42 1.4245(19) . ? C41 P2 1.8432(14) . ? C42 C43 1.366(2) . ? C42 H42 0.9500 . ? C43 C44 1.410(2) . ? C43 H43 0.9500 . ? C44 C49 1.424(2) . ? C44 C45 1.425(2) . ? C45 C46 1.371(2) . ? C45 H45 0.9500 . ? C46 C47 1.410(2) . ? C46 H46 0.9500 . ? C47 C48 1.377(2) . ? C47 H47 0.9500 . ? C48 C49 1.420(2) . ? C48 H48 0.9500 . ? C49 C50 1.4327(19) . ? P2 C19 1.8119(16) . ? P2 C13 1.828(6) . ? P2 C13A 1.832(10) . ? P2 Pd1 2.3933(4) . ? C13 C18 1.387(7) . ? C13 C14 1.393(7) . ? C14 C15 1.399(7) . ? C14 H14 0.9500 . ? C15 C16 1.381(7) . ? C15 H15 0.9500 . ? C16 C17 1.378(7) . ? C16 H16 0.9500 . ? C17 C18 1.394(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C13A C18A 1.376(10) . ? C13A C14A 1.391(10) . ? C14A C15A 1.411(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.354(10) . ? C15A H15A 0.9500 . ? C16A C17A 1.367(9) . ? C16A H16A 0.9500 . ? C17A C18A 1.397(10) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19 C20 1.389(2) . ? C19 C24 1.399(2) . ? C20 C21 1.392(2) . ? C20 H20 0.9500 . ? C21 C22 1.383(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(3) . ? C22 H22 0.9500 . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Pd1 C51A 2.036(13) . ? Pd1 C51 2.041(4) . ? C51 C52 1.406(4) . ? C51 C56 1.409(4) . ? C52 C53 1.390(4) . ? C52 H52 0.9500 . ? C53 C54 1.392(5) . ? C53 H53 0.9500 . ? C54 C55 1.383(5) . ? C54 H54 0.9500 . ? C55 C56 1.404(4) . ? C55 H55 0.9500 . ? C56 C57 1.497(4) . ? C57 C58 1.397(3) . ? C57 C62 1.405(3) . ? C58 C59 1.394(3) . ? C58 H58 0.9500 . ? C59 C60 1.386(3) . ? C59 H59 0.9500 . ? C60 C61 1.385(3) . ? C60 H60 0.9500 . ? C61 C62 1.412(4) . ? C61 H61 0.9500 . ? C62 N1 1.376(3) . ? N1 H1A 0.897(15) . ? N1 H1B 0.881(15) . ? C51A C52A 1.399(14) . ? C51A C56A 1.409(13) . ? C52A C53A 1.395(15) . ? C52A H52A 0.9500 . ? C53A C54A 1.395(15) . ? C53A H53A 0.9500 . ? C54A C55A 1.384(15) . ? C54A H54A 0.9500 . ? C55A C56A 1.399(14) . ? C55A H55A 0.9500 . ? C56A C57A 1.510(13) . ? C57A C58A 1.374(10) . ? C57A C62A 1.387(8) . ? C58A C59A 1.382(9) . ? C58A H58A 0.9500 . ? C59A C60A 1.376(11) . ? C59A H59A 0.9500 . ? C60A C61A 1.374(12) . ? C60A H60A 0.9500 . ? C61A C62A 1.432(10) . ? C61A H61A 0.9500 . ? C62A N1A 1.382(9) . ? N1A H1C 0.898(19) . ? N1A H1D 0.894(19) . ? C1S Cl2 1.721(6) . ? C1S Cl3 1.746(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C1T Cl3A 1.707(8) . ? C1T Cl2A 1.724(6) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2S Cl4 1.756(10) . ? C2S Cl5 1.781(11) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C2T Cl4A 1.716(14) . ? C2T Cl5A 1.717(14) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C2U Cl5B 1.747(14) . ? C2U Cl4B 1.757(15) . ? C2U H2U1 0.9900 . ? C2U H2U2 0.9900 . ? 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 C7 P1 C31 109.36(6) . . ? C7 P1 C1 100.23(6) . . ? C31 P1 C1 104.57(6) . . ? C7 P1 Pd1 113.63(5) . . ? C31 P1 Pd1 104.39(5) . . ? C1 P1 Pd1 123.93(5) . . ? C2 C1 C6 118.85(13) . . ? C2 C1 P1 118.70(11) . . ? C6 C1 P1 122.25(11) . . ? C3 C2 C1 120.25(15) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.41(16) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.78(15) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.15(15) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.41(14) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 119.72(13) . . ? C12 C7 P1 120.92(11) . . ? C8 C7 P1 119.28(11) . . ? C9 C8 C7 120.07(15) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.98(16) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.03(15) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.30(14) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.88(14) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C40 C31 C32 120.07(13) . . ? C40 C31 P1 126.31(10) . . ? C32 C31 P1 112.85(10) . . ? C33 C32 C31 121.45(13) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 120.36(13) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 120.37(14) . . ? C33 C34 C39 119.41(13) . . ? C35 C34 C39 120.17(13) . . ? C36 C35 C34 120.63(14) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.60(14) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 121.14(14) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.95(14) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C38 C39 C34 117.46(13) . . ? C38 C39 C40 122.72(13) . . ? C34 C39 C40 119.78(13) . . ? C31 C40 C39 118.81(12) . . ? C31 C40 C50 122.62(12) . . ? C39 C40 C50 118.49(12) . . ? C50 C41 C42 119.60(13) . . ? C50 C41 P2 121.33(10) . . ? C42 C41 P2 118.94(10) . . ? C43 C42 C41 121.30(13) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 120.70(13) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C49 119.08(13) . . ? C43 C44 C45 121.14(14) . . ? C49 C44 C45 119.78(14) . . ? C46 C45 C44 120.73(14) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 119.59(15) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C48 C47 C46 121.04(15) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 120.92(14) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C44 117.91(13) . . ? C48 C49 C50 122.26(13) . . ? C44 C49 C50 119.79(13) . . ? C41 C50 C49 119.49(12) . . ? C41 C50 C40 120.81(12) . . ? C49 C50 C40 119.69(12) . . ? C19 P2 C13 103.9(3) . . ? C19 P2 C13A 111.7(5) . . ? C13 P2 C13A 7.9(7) . . ? C19 P2 C41 102.98(7) . . ? C13 P2 C41 103.2(2) . . ? C13A P2 C41 100.1(3) . . ? C19 P2 Pd1 111.03(5) . . ? C13 P2 Pd1 113.6(2) . . ? C13A P2 Pd1 110.0(4) . . ? C41 P2 Pd1 120.46(5) . . ? C18 C13 C14 119.5(5) . . ? C18 C13 P2 116.8(6) . . ? C14 C13 P2 123.7(6) . . ? C13 C14 C15 119.5(6) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.7(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.2(6) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C13 C18 C17 120.9(6) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18A C13A C14A 118.6(8) . . ? C18A C13A P2 119.2(8) . . ? C14A C13A P2 122.2(8) . . ? C13A C14A C15A 119.8(8) . . ? C13A C14A H14A 120.1 . . ? C15A C14A H14A 120.1 . . ? C16A C15A C14A 120.4(8) . . ? C16A C15A H15A 119.8 . . ? C14A C15A H15A 119.8 . . ? C15A C16A C17A 120.1(8) . . ? C15A C16A H16A 120.0 . . ? C17A C16A H16A 120.0 . . ? C16A C17A C18A 120.2(9) . . ? C16A C17A H17A 119.9 . . ? C18A C17A H17A 119.9 . . ? C13A C18A C17A 120.6(9) . . ? C13A C18A H18A 119.7 . . ? C17A C18A H18A 119.7 . . ? C20 C19 C24 119.07(15) . . ? C20 C19 P2 119.59(12) . . ? C24 C19 P2 121.25(13) . . ? C19 C20 C21 120.05(16) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.28(18) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.35(18) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.70(17) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C19 120.54(17) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C51A Pd1 C51 1.5(7) . . ? C51A Pd1 P1 94.7(3) . . ? C51 Pd1 P1 94.33(10) . . ? C51A Pd1 Cl1 86.3(3) . . ? C51 Pd1 Cl1 86.77(10) . . ? P1 Pd1 Cl1 178.721(13) . . ? C51A Pd1 P2 174.2(3) . . ? C51 Pd1 P2 174.43(10) . . ? P1 Pd1 P2 91.026(16) . . ? Cl1 Pd1 P2 87.889(16) . . ? C52 C51 C56 118.1(4) . . ? C52 C51 Pd1 114.8(3) . . ? C56 C51 Pd1 127.0(3) . . ? C53 C52 C51 121.5(4) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 120.1(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.2(5) . . ? C55 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C54 C55 C56 121.5(5) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? C55 C56 C51 119.5(4) . . ? C55 C56 C57 116.2(4) . . ? C51 C56 C57 124.3(4) . . ? C58 C57 C62 118.6(2) . . ? C58 C57 C56 119.9(3) . . ? C62 C57 C56 121.4(3) . . ? C59 C58 C57 122.1(2) . . ? C59 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? C60 C59 C58 118.7(2) . . ? C60 C59 H59 120.6 . . ? C58 C59 H59 120.6 . . ? C61 C60 C59 120.8(3) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 120.5(3) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? N1 C62 C57 121.3(2) . . ? N1 C62 C61 119.1(2) . . ? C57 C62 C61 119.3(2) . . ? C62 N1 H1A 115.4(17) . . ? C62 N1 H1B 116.4(17) . . ? H1A N1 H1B 116(3) . . ? C52A C51A C56A 118.9(13) . . ? C52A C51A Pd1 117.4(12) . . ? C56A C51A Pd1 123.7(12) . . ? C53A C52A C51A 122.3(16) . . ? C53A C52A H52A 118.9 . . ? C51A C52A H52A 118.9 . . ? C52A C53A C54A 118.3(18) . . ? C52A C53A H53A 120.9 . . ? C54A C53A H53A 120.9 . . ? C55A C54A C53A 120.1(19) . . ? C55A C54A H54A 119.9 . . ? C53A C54A H54A 119.9 . . ? C54A C55A C56A 121.9(18) . . ? C54A C55A H55A 119.0 . . ? C56A C55A H55A 119.0 . . ? C55A C56A C51A 118.4(14) . . ? C55A C56A C57A 119.5(14) . . ? C51A C56A C57A 121.7(13) . . ? C58A C57A C62A 119.9(7) . . ? C58A C57A C56A 120.4(11) . . ? C62A C57A C56A 119.7(11) . . ? C57A C58A C59A 122.6(8) . . ? C57A C58A H58A 118.7 . . ? C59A C58A H58A 118.7 . . ? H1A C58A H58A 60.4 . . ? H1B C58A H58A 15.0 . . ? C60A C59A C58A 118.9(8) . . ? C60A C59A H59A 120.6 . . ? C58A C59A H59A 120.6 . . ? H1A C59A H59A 63.5 . . ? C61A C60A C59A 119.7(9) . . ? C61A C60A H60A 120.1 . . ? C59A C60A H60A 120.1 . . ? C60A C61A C62A 121.8(8) . . ? C60A C61A H61A 119.1 . . ? C62A C61A H61A 119.1 . . ? N1A C62A C57A 123.5(6) . . ? N1A C62A C61A 119.4(6) . . ? C57A C62A C61A 117.1(7) . . ? C62A N1A H1C 116(2) . . ? C62A N1A H1D 116(2) . . ? H1C N1A H1D 115(4) . . ? Cl2 C1S Cl3 112.3(3) . . ? Cl2 C1S H1S1 109.2 . . ? Cl3 C1S H1S1 109.2 . . ? Cl2 C1S H1S2 109.2 . . ? Cl3 C1S H1S2 109.2 . . ? H1S1 C1S H1S2 107.9 . . ? Cl3A C1T Cl2A 115.5(5) . . ? Cl3A C1T H1T1 108.4 . . ? Cl2A C1T H1T1 108.4 . . ? Cl3A C1T H1T2 108.4 . . ? Cl2A C1T H1T2 108.4 . . ? H1T1 C1T H1T2 107.5 . . ? Cl4 C2S Cl5 110.6(8) . . ? Cl4 C2S H2S1 109.5 . . ? Cl5 C2S H2S1 109.5 . . ? Cl4 C2S H2S2 109.5 . . ? Cl5 C2S H2S2 109.5 . . ? H2S1 C2S H2S2 108.1 . . ? Cl4A C2T Cl5A 120.8(14) . . ? Cl4A C2T H2T1 107.1 . . ? Cl5A C2T H2T1 107.1 . . ? Cl4A C2T H2T2 107.1 . . ? Cl5A C2T H2T2 107.1 . . ? H2T1 C2T H2T2 106.8 . . ? Cl5B C2U Cl4B 116.1(13) . . ? Cl5B C2U H2U1 108.3 . . ? Cl4B C2U H2U1 108.3 . . ? Cl5B C2U H2U2 108.3 . . ? Cl4B C2U H2U2 108.3 . . ? H2U1 C2U H2U2 107.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B Cl1 0.881(15) 2.54(2) 3.312(2) 147(2) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.944 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.074 # Attachment '- 6a.cif' data_12044 _database_code_depnum_ccdc_archive 'CCDC 891254' #TrackingRef '- 6a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H72 N O4 P Pd S' _chemical_formula_weight 920.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3071(10) _cell_length_b 13.5653(11) _cell_length_c 14.7831(12) _cell_angle_alpha 102.4550(10) _cell_angle_beta 94.4810(10) _cell_angle_gamma 98.6540(10) _cell_volume 2366.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9654 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 30.99 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8489 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 68495 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 30.51 _reflns_number_total 14378 _reflns_number_gt 12798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0348P)^2^+1.5870P] 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 14378 _refine_ls_number_parameters 599 _refine_ls_number_restraints 269 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.042 _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 0.296114(9) 0.378035(8) 0.917300(8) 0.01042(3) Uani 1 1 d . . . O1 O 0.29946(9) 0.39207(8) 1.06749(8) 0.0155(2) Uani 1 1 d . . . S1 S 0.39618(3) 0.45044(3) 1.13398(3) 0.01532(8) Uani 1 1 d . . . O2 O 0.48796(10) 0.39550(10) 1.13217(11) 0.0279(3) Uani 1 1 d . . . O3 O 0.42332(11) 0.55545(9) 1.12545(9) 0.0248(3) Uani 1 1 d . . . C71 C 0.34857(19) 0.45657(17) 1.24449(13) 0.0328(5) Uani 1 1 d . . . H71A H 0.4086 0.4923 1.2934 0.049 Uiso 1 1 calc R . . H71B H 0.3246 0.3870 1.2523 0.049 Uiso 1 1 calc R . . H71C H 0.2862 0.4938 1.2490 0.049 Uiso 1 1 calc R . . P1 P 0.25115(3) 0.20351(3) 0.87261(3) 0.00980(7) Uani 1 1 d . . . C1 C 0.22309(12) 0.13738(11) 0.96775(11) 0.0126(3) Uani 1 1 d . . . H1 H 0.1958 0.0633 0.9382 0.015 Uiso 1 1 calc R . . C2 C 0.13202(13) 0.17740(12) 1.02398(11) 0.0162(3) Uani 1 1 d . . . H2A H 0.1546 0.2518 1.0512 0.019 Uiso 1 1 calc R . . H2B H 0.0627 0.1673 0.9818 0.019 Uiso 1 1 calc R . . C3 C 0.11126(15) 0.12132(15) 1.10217(13) 0.0240(4) Uani 1 1 d . . . H3A H 0.0551 0.1506 1.1391 0.029 Uiso 1 1 calc R . . H3B H 0.0819 0.0480 1.0746 0.029 Uiso 1 1 calc R . . C4 C 0.21791(16) 0.13104(16) 1.16623(13) 0.0268(4) Uani 1 1 d . . . H4A H 0.2440 0.2039 1.1978 0.032 Uiso 1 1 calc R . . H4B H 0.2030 0.0922 1.2148 0.032 Uiso 1 1 calc R . . C5 C 0.30741(15) 0.09017(13) 1.11108(12) 0.0219(3) Uani 1 1 d . . . H5A H 0.2842 0.0157 1.0847 0.026 Uiso 1 1 calc R . . H5B H 0.3765 0.1002 1.1535 0.026 Uiso 1 1 calc R . . C6 C 0.32968(13) 0.14405(12) 1.03210(11) 0.0155(3) Uani 1 1 d . . . H6A H 0.3843 0.1121 0.9951 0.019 Uiso 1 1 calc R . . H6B H 0.3619 0.2169 1.0588 0.019 Uiso 1 1 calc R . . C7 C 0.12383(12) 0.16780(11) 0.78783(11) 0.0118(3) Uani 1 1 d . . . H7 H 0.1483 0.1674 0.7248 0.014 Uiso 1 1 calc R . . C8 C 0.05068(12) 0.06332(11) 0.78016(11) 0.0138(3) Uani 1 1 d . . . H8A H 0.0959 0.0084 0.7680 0.017 Uiso 1 1 calc R . . H8B H 0.0192 0.0622 0.8396 0.017 Uiso 1 1 calc R . . C9 C -0.04304(13) 0.04437(13) 0.70074(12) 0.0184(3) Uani 1 1 d . . . H9A H -0.0110 0.0425 0.6411 0.022 Uiso 1 1 calc R . . H9B H -0.0895 -0.0232 0.6961 0.022 Uiso 1 1 calc R . . C10 C -0.11521(13) 0.12722(14) 0.71579(14) 0.0227(4) Uani 1 1 d . . . H10A H -0.1538 0.1245 0.7717 0.027 Uiso 1 1 calc R . . H10B H -0.1718 0.1149 0.6614 0.027 Uiso 1 1 calc R . . C11 C -0.04424(14) 0.23294(14) 0.72859(13) 0.0216(3) Uani 1 1 d . . . H11A H -0.0910 0.2863 0.7433 0.026 Uiso 1 1 calc R . . H11B H -0.0132 0.2384 0.6697 0.026 Uiso 1 1 calc R . . C12 C 0.05026(13) 0.25105(12) 0.80717(12) 0.0156(3) Uani 1 1 d . . . H12A H 0.0192 0.2504 0.8669 0.019 Uiso 1 1 calc R . . H12B H 0.0958 0.3193 0.8131 0.019 Uiso 1 1 calc R . . C21 C 0.37034(12) 0.14769(11) 0.82883(11) 0.0109(3) Uani 1 1 d . . . C22 C 0.37459(12) 0.05086(11) 0.77135(11) 0.0115(3) Uani 1 1 d . . . C23 C 0.47843(13) 0.02428(12) 0.75550(12) 0.0157(3) Uani 1 1 d . . . H23 H 0.4818 -0.0403 0.7162 0.019 Uiso 1 1 calc R . . C24 C 0.57629(13) 0.08936(13) 0.79534(13) 0.0182(3) Uani 1 1 d . . . H24 H 0.6454 0.0692 0.7835 0.022 Uiso 1 1 calc R . . C25 C 0.57273(13) 0.18397(12) 0.85252(12) 0.0180(3) Uani 1 1 d . . . H25 H 0.6393 0.2290 0.8806 0.022 Uiso 1 1 calc R . . C26 C 0.47090(12) 0.21229(12) 0.86833(11) 0.0147(3) Uani 1 1 d . . . H26 H 0.4690 0.2775 0.9072 0.018 Uiso 1 1 calc R . . C31 C 0.27701(12) -0.02781(11) 0.72105(11) 0.0121(3) Uani 1 1 d . . . C32 C 0.23097(12) -0.02124(11) 0.63270(11) 0.0128(3) Uani 1 1 d . . . C37 C 0.28043(13) 0.06275(12) 0.58646(11) 0.0155(3) Uani 1 1 d . . . H37 H 0.3207 0.1212 0.6369 0.019 Uiso 1 1 calc R . . C38 C 0.36535(16) 0.02338(16) 0.52356(14) 0.0273(4) Uani 1 1 d . . . H38A H 0.4224 0.0010 0.5605 0.041 Uiso 1 1 calc R . . H38B H 0.3997 0.0785 0.4964 0.041 Uiso 1 1 calc R . . H38C H 0.3282 -0.0345 0.4736 0.041 Uiso 1 1 calc R . . C39 C 0.19570(14) 0.10408(13) 0.53039(12) 0.0198(3) Uani 1 1 d . . . H39A H 0.1595 0.0498 0.4769 0.030 Uiso 1 1 calc R . . H39B H 0.2331 0.1618 0.5081 0.030 Uiso 1 1 calc R . . H39C H 0.1400 0.1272 0.5701 0.030 Uiso 1 1 calc R . . C33 C 0.14284(13) -0.09655(11) 0.58531(11) 0.0144(3) Uani 1 1 d . . . H33 H 0.1110 -0.0917 0.5261 0.017 Uiso 1 1 calc R . . C34 C 0.10014(13) -0.17867(11) 0.62209(12) 0.0156(3) Uani 1 1 d DU A . C40 C 0.00253(14) -0.25777(12) 0.56879(12) 0.0193(3) Uani 1 1 d DU . . H40A H -0.0350 -0.2254 0.5232 0.023 Uiso 0.60(3) 1 calc PR A 1 H40B H -0.0227 -0.2350 0.5119 0.023 Uiso 0.40(3) 1 calc PR A 2 C41 C 0.0457(8) -0.3509(6) 0.5114(8) 0.0373(17) Uani 0.60(3) 1 d PDU A 1 H41A H -0.0171 -0.4018 0.4769 0.056 Uiso 0.60(3) 1 calc PR A 1 H41B H 0.0879 -0.3816 0.5536 0.056 Uiso 0.60(3) 1 calc PR A 1 H41C H 0.0937 -0.3280 0.4673 0.056 Uiso 0.60(3) 1 calc PR A 1 C42 C -0.0820(9) -0.2889(11) 0.6298(7) 0.046(2) Uani 0.60(3) 1 d PDU A 1 H42A H -0.1424 -0.3397 0.5916 0.069 Uiso 0.60(3) 1 calc PR A 1 H42B H -0.1113 -0.2286 0.6605 0.069 Uiso 0.60(3) 1 calc PR A 1 H42C H -0.0473 -0.3186 0.6771 0.069 Uiso 0.60(3) 1 calc PR A 1 C41A C 0.0297(8) -0.3648(6) 0.5377(8) 0.0206(16) Uani 0.40(3) 1 d PDU A 2 H41D H -0.0365 -0.4115 0.5038 0.031 Uiso 0.40(3) 1 calc PR A 2 H41E H 0.0544 -0.3888 0.5925 0.031 Uiso 0.40(3) 1 calc PR A 2 H41F H 0.0886 -0.3631 0.4968 0.031 Uiso 0.40(3) 1 calc PR A 2 C42A C -0.0963(10) -0.2659(9) 0.6283(10) 0.0229(16) Uani 0.40(3) 1 d PDU A 2 H42D H -0.1578 -0.3172 0.5922 0.034 Uiso 0.40(3) 1 calc PR A 2 H42E H -0.1202 -0.1993 0.6447 0.034 Uiso 0.40(3) 1 calc PR A 2 H42F H -0.0728 -0.2865 0.6854 0.034 Uiso 0.40(3) 1 calc PR A 2 C35 C 0.15022(13) -0.18620(11) 0.70734(12) 0.0157(3) Uani 1 1 d . . . H35 H 0.1241 -0.2435 0.7318 0.019 Uiso 1 1 calc R A . C36 C 0.23802(12) -0.11207(11) 0.75846(11) 0.0131(3) Uani 1 1 d . A . C43 C 0.28901(13) -0.12603(12) 0.85101(11) 0.0154(3) Uani 1 1 d . . . H43 H 0.3344 -0.0589 0.8852 0.018 Uiso 1 1 calc R A . C44 C 0.36621(15) -0.20565(14) 0.83579(14) 0.0242(4) Uani 1 1 d . A . H44A H 0.3239 -0.2719 0.8011 0.036 Uiso 1 1 calc R . . H44B H 0.3986 -0.2126 0.8963 0.036 Uiso 1 1 calc R . . H44C H 0.4254 -0.1833 0.8002 0.036 Uiso 1 1 calc R . . C45 C 0.20207(14) -0.15754(13) 0.91322(12) 0.0202(3) Uani 1 1 d . A . H45A H 0.1512 -0.1081 0.9218 0.030 Uiso 1 1 calc R . . H45B H 0.2391 -0.1588 0.9740 0.030 Uiso 1 1 calc R . . H45C H 0.1605 -0.2259 0.8835 0.030 Uiso 1 1 calc R . . N1 N 0.31139(12) 0.53956(10) 0.94494(10) 0.0156(3) Uani 1 1 d D . . H1A H 0.3613(15) 0.5611(15) 0.9123(14) 0.019 Uiso 1 1 d D . . H1B H 0.3333(17) 0.5645(15) 1.0039(11) 0.019 Uiso 1 1 d D . . C51 C 0.20239(13) 0.55415(11) 0.91580(12) 0.0161(3) Uani 1 1 d . . . C52 C 0.13601(15) 0.59757(12) 0.97972(13) 0.0204(3) Uani 1 1 d . . . H52 H 0.1638 0.6212 1.0438 0.025 Uiso 1 1 calc R . . C53 C 0.02849(15) 0.60621(13) 0.94935(14) 0.0239(4) Uani 1 1 d . . . H53 H -0.0177 0.6343 0.9930 0.029 Uiso 1 1 calc R . . C54 C -0.01118(15) 0.57389(14) 0.85557(14) 0.0240(4) Uani 1 1 d . . . H54 H -0.0835 0.5821 0.8347 0.029 Uiso 1 1 calc R . . C55 C 0.05499(14) 0.52944(13) 0.79211(13) 0.0205(3) Uani 1 1 d . . . H55 H 0.0272 0.5073 0.7279 0.025 Uiso 1 1 calc R . . C56 C 0.16196(13) 0.51675(12) 0.82113(12) 0.0158(3) Uani 1 1 d . . . C57 C 0.23058(13) 0.46118(12) 0.75664(11) 0.0152(3) Uani 1 1 d . . . C58 C 0.23485(14) 0.47931(13) 0.66726(12) 0.0204(3) Uani 1 1 d . . . H58 H 0.1934 0.5270 0.6491 0.024 Uiso 1 1 calc R . . C59 C 0.29809(15) 0.42944(14) 0.60444(12) 0.0222(3) Uani 1 1 d . . . H59 H 0.2990 0.4420 0.5437 0.027 Uiso 1 1 calc R . . C60 C 0.35991(14) 0.36095(13) 0.63136(12) 0.0193(3) Uani 1 1 d . . . H60 H 0.4038 0.3266 0.5891 0.023 Uiso 1 1 calc R . . C61 C 0.35758(13) 0.34264(12) 0.72043(11) 0.0155(3) Uani 1 1 d . . . H61 H 0.4014 0.2965 0.7384 0.019 Uiso 1 1 calc R . . C62 C 0.29262(12) 0.39015(11) 0.78416(11) 0.0128(3) Uani 1 1 d . . . C2S C 0.3587(9) 0.7422(9) 0.3497(5) 0.071(3) Uani 0.559(4) 1 d PDU B 1 H2S1 H 0.2858 0.7298 0.3134 0.106 Uiso 0.559(4) 1 calc PR B 1 H2S2 H 0.4051 0.6964 0.3174 0.106 Uiso 0.559(4) 1 calc PR B 1 H2S3 H 0.3938 0.8136 0.3563 0.106 Uiso 0.559(4) 1 calc PR B 1 C1S C 0.3456(4) 0.7218(3) 0.4445(3) 0.0373(9) Uani 0.559(4) 1 d PDU B 1 H1S1 H 0.2980 0.7679 0.4763 0.045 Uiso 0.559(4) 1 calc PR B 1 H1S2 H 0.3075 0.6504 0.4370 0.045 Uiso 0.559(4) 1 calc PR B 1 O1S O 0.4475(3) 0.7365(3) 0.5017(2) 0.0464(9) Uani 0.559(4) 1 d PDU B 1 C3S C 0.4412(5) 0.7191(5) 0.5945(3) 0.0557(13) Uani 0.559(4) 1 d PDU B 1 H3S1 H 0.4120 0.6463 0.5920 0.067 Uiso 0.559(4) 1 calc PR B 1 H3S2 H 0.3935 0.7626 0.6293 0.067 Uiso 0.559(4) 1 calc PR B 1 C4S C 0.5593(5) 0.7483(5) 0.6382(3) 0.0512(13) Uani 0.559(4) 1 d PDU B 1 H4S1 H 0.5638 0.7385 0.7021 0.077 Uiso 0.559(4) 1 calc PR B 1 H4S2 H 0.5863 0.8204 0.6394 0.077 Uiso 0.559(4) 1 calc PR B 1 H4S3 H 0.6050 0.7051 0.6017 0.077 Uiso 0.559(4) 1 calc PR B 1 C2T C 0.3575(5) 0.7413(5) 0.3521(4) 0.0176(13) Uani 0.441(4) 1 d PDU B 2 H2T1 H 0.3112 0.7656 0.3074 0.026 Uiso 0.441(4) 1 calc PR B 2 H2T2 H 0.3954 0.6886 0.3183 0.026 Uiso 0.441(4) 1 calc PR B 2 H2T3 H 0.4125 0.7988 0.3886 0.026 Uiso 0.441(4) 1 calc PR B 2 C1T C 0.2856(4) 0.6964(4) 0.4169(3) 0.0288(10) Uani 0.441(4) 1 d PDU B 2 H1T1 H 0.2467 0.7495 0.4503 0.035 Uiso 0.441(4) 1 calc PR B 2 H1T2 H 0.2292 0.6392 0.3798 0.035 Uiso 0.441(4) 1 calc PR B 2 O1T O 0.3538(3) 0.6576(3) 0.4869(3) 0.0437(10) Uani 0.441(4) 1 d PDU B 2 C3T C 0.4276(5) 0.7389(4) 0.5603(4) 0.0363(11) Uani 0.441(4) 1 d PDU B 2 H3T1 H 0.3809 0.7786 0.6004 0.044 Uiso 0.441(4) 1 calc PR B 2 H3T2 H 0.4717 0.7866 0.5295 0.044 Uiso 0.441(4) 1 calc PR B 2 C4T C 0.5067(5) 0.6972(5) 0.6219(4) 0.0375(13) Uani 0.441(4) 1 d PDU B 2 H4T1 H 0.5515 0.7543 0.6685 0.056 Uiso 0.441(4) 1 calc PR B 2 H4T2 H 0.5553 0.6600 0.5832 0.056 Uiso 0.441(4) 1 calc PR B 2 H4T3 H 0.4639 0.6507 0.6536 0.056 Uiso 0.441(4) 1 calc PR B 2 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 0.01066(5) 0.00808(5) 0.01183(6) 0.00203(4) -0.00125(4) 0.00112(4) O1 0.0153(5) 0.0152(5) 0.0134(5) 0.0017(4) -0.0012(4) -0.0014(4) S1 0.01569(17) 0.01345(16) 0.01495(18) 0.00300(13) -0.00238(14) -0.00087(13) O2 0.0168(6) 0.0229(6) 0.0430(8) 0.0070(6) -0.0020(6) 0.0038(5) O3 0.0299(7) 0.0139(5) 0.0253(7) 0.0040(5) -0.0107(5) -0.0046(5) C71 0.0399(11) 0.0364(11) 0.0163(9) 0.0016(8) 0.0021(8) -0.0040(9) P1 0.00845(15) 0.00861(15) 0.01199(17) 0.00241(13) -0.00036(13) 0.00112(12) C1 0.0129(6) 0.0112(6) 0.0142(7) 0.0043(5) 0.0006(5) 0.0021(5) C2 0.0138(7) 0.0188(7) 0.0168(8) 0.0058(6) 0.0027(6) 0.0020(6) C3 0.0215(8) 0.0316(9) 0.0195(8) 0.0112(7) 0.0041(7) -0.0017(7) C4 0.0269(9) 0.0382(10) 0.0168(8) 0.0133(8) 0.0028(7) 0.0001(8) C5 0.0256(8) 0.0214(8) 0.0199(8) 0.0109(7) -0.0036(7) 0.0017(7) C6 0.0160(7) 0.0156(7) 0.0160(7) 0.0063(6) -0.0007(6) 0.0032(6) C7 0.0094(6) 0.0115(6) 0.0137(7) 0.0031(5) -0.0005(5) 0.0003(5) C8 0.0106(6) 0.0128(6) 0.0164(7) 0.0016(5) 0.0007(5) -0.0004(5) C9 0.0121(7) 0.0190(7) 0.0199(8) -0.0003(6) -0.0017(6) -0.0018(6) C10 0.0093(7) 0.0259(8) 0.0295(10) 0.0021(7) -0.0042(6) 0.0015(6) C11 0.0135(7) 0.0242(8) 0.0277(9) 0.0076(7) -0.0039(6) 0.0058(6) C12 0.0115(6) 0.0138(7) 0.0215(8) 0.0040(6) -0.0012(6) 0.0036(5) C21 0.0093(6) 0.0105(6) 0.0137(7) 0.0048(5) 0.0005(5) 0.0018(5) C22 0.0110(6) 0.0104(6) 0.0139(7) 0.0047(5) 0.0006(5) 0.0018(5) C23 0.0130(7) 0.0133(7) 0.0221(8) 0.0048(6) 0.0031(6) 0.0042(5) C24 0.0105(6) 0.0183(7) 0.0289(9) 0.0102(7) 0.0038(6) 0.0049(6) C25 0.0091(6) 0.0171(7) 0.0275(9) 0.0076(6) -0.0013(6) -0.0001(6) C26 0.0124(6) 0.0118(6) 0.0192(8) 0.0037(6) -0.0006(6) 0.0010(5) C31 0.0113(6) 0.0092(6) 0.0154(7) 0.0012(5) 0.0018(5) 0.0025(5) C32 0.0131(6) 0.0102(6) 0.0154(7) 0.0023(5) 0.0026(5) 0.0031(5) C37 0.0167(7) 0.0148(7) 0.0148(7) 0.0049(6) 0.0006(6) 0.0007(6) C38 0.0263(9) 0.0330(10) 0.0293(10) 0.0151(8) 0.0136(8) 0.0092(8) C39 0.0233(8) 0.0194(7) 0.0177(8) 0.0075(6) 0.0001(6) 0.0034(6) C33 0.0159(7) 0.0126(6) 0.0136(7) 0.0012(5) -0.0006(6) 0.0025(5) C34 0.0156(7) 0.0109(6) 0.0183(8) 0.0006(5) -0.0011(6) 0.0016(5) C40 0.0196(7) 0.0133(7) 0.0218(8) 0.0029(6) -0.0073(6) -0.0008(6) C41 0.041(3) 0.017(2) 0.044(4) -0.004(2) -0.019(2) 0.002(2) C42 0.034(3) 0.055(6) 0.035(3) 0.011(3) -0.010(2) -0.029(3) C41A 0.021(3) 0.010(2) 0.028(4) 0.000(2) -0.002(2) 0.0005(19) C42A 0.022(3) 0.019(3) 0.025(3) 0.004(2) 0.000(2) 0.000(2) C35 0.0159(7) 0.0101(6) 0.0201(8) 0.0036(6) -0.0009(6) -0.0002(5) C36 0.0124(6) 0.0101(6) 0.0170(7) 0.0032(5) 0.0005(5) 0.0029(5) C43 0.0156(7) 0.0124(6) 0.0178(8) 0.0059(6) -0.0025(6) -0.0001(5) C44 0.0215(8) 0.0220(8) 0.0321(10) 0.0109(7) -0.0004(7) 0.0081(7) C45 0.0213(8) 0.0183(7) 0.0207(8) 0.0085(6) -0.0006(6) -0.0016(6) N1 0.0183(6) 0.0107(6) 0.0167(7) 0.0028(5) -0.0029(5) 0.0017(5) C51 0.0179(7) 0.0091(6) 0.0221(8) 0.0061(6) 0.0004(6) 0.0022(5) C52 0.0264(8) 0.0125(7) 0.0229(9) 0.0044(6) 0.0042(7) 0.0035(6) C53 0.0250(9) 0.0163(7) 0.0338(10) 0.0069(7) 0.0109(7) 0.0080(7) C54 0.0169(7) 0.0202(8) 0.0376(11) 0.0102(7) 0.0037(7) 0.0067(6) C55 0.0190(8) 0.0180(7) 0.0259(9) 0.0081(6) -0.0013(7) 0.0047(6) C56 0.0160(7) 0.0119(6) 0.0207(8) 0.0064(6) 0.0009(6) 0.0027(5) C57 0.0145(7) 0.0139(7) 0.0169(7) 0.0050(6) -0.0018(6) 0.0014(5) C58 0.0213(8) 0.0218(8) 0.0197(8) 0.0088(6) -0.0015(6) 0.0049(6) C59 0.0252(8) 0.0251(8) 0.0168(8) 0.0082(7) -0.0001(7) 0.0019(7) C60 0.0207(8) 0.0190(7) 0.0166(8) 0.0027(6) 0.0024(6) 0.0005(6) C61 0.0151(7) 0.0141(7) 0.0170(8) 0.0043(6) -0.0004(6) 0.0018(6) C62 0.0118(6) 0.0111(6) 0.0143(7) 0.0035(5) -0.0019(5) -0.0008(5) C2S 0.076(7) 0.098(7) 0.062(5) 0.044(5) 0.026(4) 0.045(6) C1S 0.032(2) 0.037(2) 0.040(2) -0.0013(17) 0.0079(16) 0.0107(17) O1S 0.0483(17) 0.0477(17) 0.0472(19) 0.0127(15) 0.0114(14) 0.0154(14) C3S 0.092(3) 0.051(3) 0.029(2) 0.009(2) 0.015(2) 0.027(3) C4S 0.066(3) 0.056(3) 0.031(2) -0.005(2) 0.018(2) 0.024(3) C2T 0.014(3) 0.013(2) 0.027(3) 0.003(2) 0.005(2) 0.008(2) C1T 0.031(2) 0.029(2) 0.031(2) 0.0127(18) 0.0133(18) 0.0093(19) O1T 0.048(2) 0.0390(19) 0.045(2) 0.0117(15) 0.0060(16) 0.0074(16) C3T 0.057(3) 0.036(3) 0.018(3) 0.0048(19) 0.011(2) 0.013(2) C4T 0.038(3) 0.053(4) 0.025(3) 0.003(2) 0.007(2) 0.029(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 Pd1 C62 2.0078(15) . ? Pd1 N1 2.1169(13) . ? Pd1 O1 2.1838(11) . ? Pd1 P1 2.2851(4) . ? O1 S1 1.4858(11) . ? S1 O2 1.4428(14) . ? S1 O3 1.4482(12) . ? S1 C71 1.768(2) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? P1 C21 1.8481(15) . ? P1 C1 1.8518(15) . ? P1 C7 1.8610(15) . ? C1 C6 1.538(2) . ? C1 C2 1.541(2) . ? C1 H1 1.0000 . ? C2 C3 1.532(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.529(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.537(2) . ? C7 C12 1.545(2) . ? C7 H7 1.0000 . ? C8 C9 1.531(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.525(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.528(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.530(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C21 C26 1.407(2) . ? C21 C22 1.413(2) . ? C22 C23 1.403(2) . ? C22 C31 1.506(2) . ? C23 C24 1.386(2) . ? C23 H23 0.9500 . ? C24 C25 1.385(2) . ? C24 H24 0.9500 . ? C25 C26 1.387(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.409(2) . ? C31 C36 1.411(2) . ? C32 C33 1.396(2) . ? C32 C37 1.526(2) . ? C37 C39 1.526(2) . ? C37 C38 1.532(2) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C33 C34 1.394(2) . ? C33 H33 0.9500 . ? C34 C35 1.390(2) . ? C34 C40 1.521(2) . ? C40 C42 1.501(7) . ? C40 C41A 1.521(7) . ? C40 C41 1.552(7) . ? C40 C42A 1.560(9) . ? C40 H40A 1.0000 . ? C40 H40B 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C35 C36 1.403(2) . ? C35 H35 0.9500 . ? C36 C43 1.522(2) . ? C43 C44 1.535(2) . ? C43 C45 1.536(2) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? N1 C51 1.432(2) . ? N1 H1A 0.865(15) . ? N1 H1B 0.870(15) . ? C51 C52 1.390(2) . ? C51 C56 1.404(2) . ? C52 C53 1.394(3) . ? C52 H52 0.9500 . ? C53 C54 1.386(3) . ? C53 H53 0.9500 . ? C54 C55 1.389(3) . ? C54 H54 0.9500 . ? C55 C56 1.400(2) . ? C55 H55 0.9500 . ? C56 C57 1.483(2) . ? C57 C58 1.399(2) . ? C57 C62 1.421(2) . ? C58 C59 1.388(3) . ? C58 H58 0.9500 . ? C59 C60 1.388(3) . ? C59 H59 0.9500 . ? C60 C61 1.393(2) . ? C60 H60 0.9500 . ? C61 C62 1.397(2) . ? C61 H61 0.9500 . ? C2S C1S 1.502(6) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C1S O1S 1.419(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? O1S C3S 1.448(5) . ? C3S C4S 1.503(6) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C2T C1T 1.515(5) . ? C2T H2T1 0.9800 . ? C2T H2T2 0.9800 . ? C2T H2T3 0.9800 . ? C1T O1T 1.512(5) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? O1T C3T 1.498(5) . ? C3T C4T 1.532(6) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9800 . ? C4T H4T2 0.9800 . ? C4T H4T3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C62 Pd1 N1 83.20(6) . . ? C62 Pd1 O1 170.51(5) . . ? N1 Pd1 O1 87.36(5) . . ? C62 Pd1 P1 91.69(4) . . ? N1 Pd1 P1 170.00(4) . . ? O1 Pd1 P1 97.49(3) . . ? S1 O1 Pd1 121.88(6) . . ? O2 S1 O3 115.09(8) . . ? O2 S1 O1 112.06(8) . . ? O3 S1 O1 112.19(7) . . ? O2 S1 C71 106.62(10) . . ? O3 S1 C71 106.10(9) . . ? O1 S1 C71 103.78(9) . . ? S1 C71 H71A 109.5 . . ? S1 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? S1 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C21 P1 C1 101.00(7) . . ? C21 P1 C7 114.02(7) . . ? C1 P1 C7 106.54(7) . . ? C21 P1 Pd1 110.48(5) . . ? C1 P1 Pd1 115.49(5) . . ? C7 P1 Pd1 109.21(5) . . ? C6 C1 C2 111.06(13) . . ? C6 C1 P1 111.06(10) . . ? C2 C1 P1 112.40(10) . . ? C6 C1 H1 107.3 . . ? C2 C1 H1 107.3 . . ? P1 C1 H1 107.3 . . ? C3 C2 C1 110.98(14) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 110.95(14) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 110.82(15) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 111.66(14) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 111.50(13) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C12 107.93(12) . . ? C8 C7 P1 117.99(11) . . ? C12 C7 P1 110.26(10) . . ? C8 C7 H7 106.7 . . ? C12 C7 H7 106.7 . . ? P1 C7 H7 106.7 . . ? C9 C8 C7 109.80(13) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 111.89(14) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 110.22(13) . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 111.02(14) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C7 111.07(13) . . ? C11 C12 H12A 109.4 . . ? C7 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C7 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C26 C21 C22 118.17(14) . . ? C26 C21 P1 111.07(11) . . ? C22 C21 P1 130.48(11) . . ? C23 C22 C21 118.60(13) . . ? C23 C22 C31 115.08(13) . . ? C21 C22 C31 126.29(13) . . ? C24 C23 C22 122.05(15) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C25 C24 C23 119.65(15) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.25(14) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C21 122.26(15) . . ? C25 C26 H26 118.9 . . ? C21 C26 H26 118.9 . . ? C32 C31 C36 120.21(13) . . ? C32 C31 C22 119.36(13) . . ? C36 C31 C22 120.22(13) . . ? C33 C32 C31 118.88(14) . . ? C33 C32 C37 120.11(14) . . ? C31 C32 C37 120.91(13) . . ? C32 C37 C39 114.56(13) . . ? C32 C37 C38 109.56(13) . . ? C39 C37 C38 109.52(14) . . ? C32 C37 H37 107.7 . . ? C39 C37 H37 107.7 . . ? C38 C37 H37 107.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C33 C32 122.07(15) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C35 C34 C33 118.04(14) . . ? C35 C34 C40 121.74(14) . . ? C33 C34 C40 120.22(15) . . ? C42 C40 C41A 94.4(5) . . ? C42 C40 C34 113.3(4) . . ? C41A C40 C34 113.8(4) . . ? C42 C40 C41 112.4(4) . . ? C41A C40 C41 19.0(3) . . ? C34 C40 C41 109.4(4) . . ? C42 C40 C42A 14.2(7) . . ? C41A C40 C42A 107.5(5) . . ? C34 C40 C42A 111.3(6) . . ? C41 C40 C42A 124.6(6) . . ? C42 C40 H40A 107.1 . . ? C41A C40 H40A 120.5 . . ? C34 C40 H40A 107.1 . . ? C41 C40 H40A 107.1 . . ? C42A C40 H40A 95.1 . . ? C42 C40 H40B 118.7 . . ? C41A C40 H40B 108.0 . . ? C34 C40 H40B 108.0 . . ? C41 C40 H40B 93.0 . . ? C42A C40 H40B 108.0 . . ? H40A C40 H40B 15.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C41A H41D 109.5 . . ? C40 C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40 C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40 C42A H42D 109.5 . . ? C40 C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40 C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C34 C35 C36 122.22(14) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C35 C36 C31 118.47(14) . . ? C35 C36 C43 119.13(13) . . ? C31 C36 C43 122.39(13) . . ? C36 C43 C44 111.10(14) . . ? C36 C43 C45 112.94(13) . . ? C44 C43 C45 109.01(13) . . ? C36 C43 H43 107.9 . . ? C44 C43 H43 107.9 . . ? C45 C43 H43 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 N1 Pd1 102.91(9) . . ? C51 N1 H1A 113.7(14) . . ? Pd1 N1 H1A 107.1(14) . . ? C51 N1 H1B 114.4(14) . . ? Pd1 N1 H1B 108.6(14) . . ? H1A N1 H1B 109.5(19) . . ? C52 C51 C56 120.97(16) . . ? C52 C51 N1 121.31(16) . . ? C56 C51 N1 117.59(15) . . ? C51 C52 C53 119.69(17) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C54 C53 C52 120.16(17) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 119.93(17) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 121.09(17) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C55 C56 C51 118.07(16) . . ? C55 C56 C57 122.27(15) . . ? C51 C56 C57 119.59(14) . . ? C58 C57 C62 119.35(15) . . ? C58 C57 C56 119.47(14) . . ? C62 C57 C56 121.18(14) . . ? C59 C58 C57 121.66(16) . . ? C59 C58 H58 119.2 . . ? C57 C58 H58 119.2 . . ? C60 C59 C58 119.23(16) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C61 119.95(16) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C62 121.87(15) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C61 C62 C57 117.92(14) . . ? C61 C62 Pd1 124.02(11) . . ? C57 C62 Pd1 117.60(12) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O1S C1S C2S 113.4(5) . . ? O1S C1S H1S1 108.9 . . ? C2S C1S H1S1 108.9 . . ? O1S C1S H1S2 108.9 . . ? C2S C1S H1S2 108.9 . . ? H1S1 C1S H1S2 107.7 . . ? C1S O1S C3S 116.5(4) . . ? O1S C3S C4S 103.3(4) . . ? O1S C3S H3S1 111.1 . . ? C4S C3S H3S1 111.1 . . ? O1S C3S H3S2 111.1 . . ? C4S C3S H3S2 111.1 . . ? H3S1 C3S H3S2 109.1 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C1T C2T H2T1 109.5 . . ? C1T C2T H2T2 109.5 . . ? H2T1 C2T H2T2 109.5 . . ? C1T C2T H2T3 109.5 . . ? H2T1 C2T H2T3 109.5 . . ? H2T2 C2T H2T3 109.5 . . ? O1T C1T C2T 111.3(4) . . ? O1T C1T H1T1 109.4 . . ? C2T C1T H1T1 109.4 . . ? O1T C1T H1T2 109.4 . . ? C2T C1T H1T2 109.4 . . ? H1T1 C1T H1T2 108.0 . . ? C3T O1T C1T 115.3(4) . . ? O1T C3T C4T 114.0(5) . . ? O1T C3T H3T1 108.8 . . ? C4T C3T H3T1 108.8 . . ? O1T C3T H3T2 108.8 . . ? C4T C3T H3T2 108.8 . . ? H3T1 C3T H3T2 107.7 . . ? C3T C4T H4T1 109.5 . . ? C3T C4T H4T2 109.5 . . ? H4T1 C4T H4T2 109.5 . . ? C3T C4T H4T3 109.5 . . ? H4T1 C4T H4T3 109.5 . . ? H4T2 C4T H4T3 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O2 0.865(15) 2.062(16) 2.897(2) 162.0(19) 2_667 N1 H1B O3 0.870(15) 2.073(17) 2.8554(19) 149.4(19) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.102 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.076 # Attachment '- 6b.cif' data_x12064 _database_code_depnum_ccdc_archive 'CCDC 891255' #TrackingRef '- 6b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H55 N P Pd, C H3 O3 S, 2(C H2 Cl2)' _chemical_formula_sum 'C44 H62 Cl4 N O3 P Pd S' _chemical_formula_weight 964.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.8288(9) _cell_length_b 13.3096(11) _cell_length_c 17.3470(15) _cell_angle_alpha 110.420(2) _cell_angle_beta 93.341(2) _cell_angle_gamma 103.421(2) _cell_volume 2252.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 31.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8307 _exptl_absorpt_correction_T_max 0.8427 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus sealed tube' _diffrn_radiation_monochromator 'Incoatech ImuS multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 221977 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 31.30 _reflns_number_total 14723 _reflns_number_gt 13934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0274P)^2^+1.5674P] 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 14723 _refine_ls_number_parameters 515 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 0.158420(7) 0.419511(7) 0.233983(5) 0.01037(2) Uani 1 1 d . . . P1 P 0.11264(3) 0.27899(2) 0.286708(17) 0.01149(5) Uani 1 1 d . . . C1 C 0.00593(11) 0.14611(10) 0.20437(7) 0.0164(2) Uani 1 1 d . . . C2 C 0.08490(14) 0.10901(12) 0.13448(9) 0.0277(3) Uani 1 1 d . . . H2A H 0.0299 0.0462 0.0871 0.042 Uiso 1 1 calc R . . H2B H 0.1559 0.0860 0.1547 0.042 Uiso 1 1 calc R . . H2C H 0.1194 0.1710 0.1169 0.042 Uiso 1 1 calc R . . C3 C -0.04179(13) 0.04851(11) 0.23288(9) 0.0226(2) Uani 1 1 d . . . H3A H -0.0916 -0.0170 0.1853 0.034 Uiso 1 1 calc R . . H3B H -0.0962 0.0691 0.2758 0.034 Uiso 1 1 calc R . . H3C H 0.0320 0.0313 0.2557 0.034 Uiso 1 1 calc R . . C4 C -0.11025(12) 0.17177(11) 0.16768(8) 0.0223(2) Uani 1 1 d . . . H4A H -0.0802 0.2283 0.1439 0.033 Uiso 1 1 calc R . . H4B H -0.1604 0.1996 0.2117 0.033 Uiso 1 1 calc R . . H4C H -0.1642 0.1037 0.1240 0.033 Uiso 1 1 calc R . . C5 C 0.05072(11) 0.30355(10) 0.38998(7) 0.01509(19) Uani 1 1 d . . . C6 C -0.09246(11) 0.30029(11) 0.37760(8) 0.0186(2) Uani 1 1 d . . . H6A H -0.1434 0.2237 0.3456 0.028 Uiso 1 1 calc R . . H6B H -0.1044 0.3481 0.3474 0.028 Uiso 1 1 calc R . . H6C H -0.1207 0.3270 0.4320 0.028 Uiso 1 1 calc R . . C7 C 0.06393(13) 0.22214(11) 0.43286(8) 0.0205(2) Uani 1 1 d . . . H7A H 0.0238 0.2397 0.4834 0.031 Uiso 1 1 calc R . . H7B H 0.1551 0.2292 0.4476 0.031 Uiso 1 1 calc R . . H7C H 0.0212 0.1458 0.3949 0.031 Uiso 1 1 calc R . . C8 C 0.12982(12) 0.41948(10) 0.45001(7) 0.0173(2) Uani 1 1 d . . . H8A H 0.0896 0.4423 0.5002 0.026 Uiso 1 1 calc R . . H8B H 0.1330 0.4731 0.4228 0.026 Uiso 1 1 calc R . . H8C H 0.2173 0.4169 0.4653 0.026 Uiso 1 1 calc R . . C11 C 0.27065(10) 0.25493(9) 0.30325(7) 0.01210(18) Uani 1 1 d . . . C12 C 0.28708(11) 0.17120(9) 0.33155(7) 0.01463(19) Uani 1 1 d . . . H12 H 0.2135 0.1219 0.3384 0.018 Uiso 1 1 calc R . . C13 C 0.40800(12) 0.15866(10) 0.34973(7) 0.0162(2) Uani 1 1 d . . . H13 H 0.4168 0.1016 0.3689 0.019 Uiso 1 1 calc R . . C14 C 0.51592(11) 0.23042(10) 0.33954(7) 0.0159(2) Uani 1 1 d . . . H14 H 0.5993 0.2246 0.3539 0.019 Uiso 1 1 calc R . . C15 C 0.50152(11) 0.31054(9) 0.30828(7) 0.01420(19) Uani 1 1 d . . . H15 H 0.5756 0.3578 0.3000 0.017 Uiso 1 1 calc R . . C16 C 0.38001(10) 0.32343(9) 0.28864(6) 0.01146(17) Uani 1 1 d . . . C21 C 0.38111(10) 0.40798(9) 0.24882(7) 0.01158(17) Uani 1 1 d . . . C22 C 0.39951(10) 0.37771(9) 0.16357(7) 0.01298(18) Uani 1 1 d . . . C27 C 0.38533(11) 0.25772(9) 0.10735(7) 0.01509(19) Uani 1 1 d . . . H27 H 0.3413 0.2086 0.1356 0.018 Uiso 1 1 calc R . . C28 C 0.51781(12) 0.23743(11) 0.09508(8) 0.0205(2) Uani 1 1 d . . . H28A H 0.5629 0.2847 0.0674 0.031 Uiso 1 1 calc R . . H28B H 0.5073 0.1590 0.0606 0.031 Uiso 1 1 calc R . . H28C H 0.5679 0.2556 0.1494 0.031 Uiso 1 1 calc R . . C29 C 0.30437(13) 0.22433(11) 0.02231(8) 0.0205(2) Uani 1 1 d . . . H29A H 0.2212 0.2406 0.0303 0.031 Uiso 1 1 calc R . . H29B H 0.2906 0.1445 -0.0090 0.031 Uiso 1 1 calc R . . H29C H 0.3496 0.2666 -0.0087 0.031 Uiso 1 1 calc R . . C23 C 0.44560(11) 0.46139(10) 0.13320(7) 0.01471(19) Uani 1 1 d . . . H23 H 0.4576 0.4406 0.0765 0.018 Uiso 1 1 calc R . . C24 C 0.47479(10) 0.57435(10) 0.18290(7) 0.01463(19) Uani 1 1 d . . . C30 C 0.53101(12) 0.66050(10) 0.14640(8) 0.0180(2) Uani 1 1 d . . . H30 H 0.5771 0.6244 0.1007 0.022 Uiso 1 1 calc R . . C31 C 0.62850(17) 0.76270(14) 0.20841(11) 0.0379(4) Uani 1 1 d . . . H31A H 0.6729 0.8079 0.1790 0.057 Uiso 1 1 calc R . . H31B H 0.6912 0.7395 0.2366 0.057 Uiso 1 1 calc R . . H31C H 0.5844 0.8067 0.2496 0.057 Uiso 1 1 calc R . . C32 C 0.42436(13) 0.69222(13) 0.10696(9) 0.0257(3) Uani 1 1 d . . . H32A H 0.3690 0.6259 0.0624 0.039 Uiso 1 1 calc R . . H32B H 0.4621 0.7477 0.0838 0.039 Uiso 1 1 calc R . . H32C H 0.3732 0.7235 0.1493 0.039 Uiso 1 1 calc R . . C25 C 0.45103(11) 0.60351(9) 0.26491(7) 0.01459(19) Uani 1 1 d . . . H25 H 0.4643 0.6799 0.2983 0.018 Uiso 1 1 calc R . . C26 C 0.40812(10) 0.52320(9) 0.29949(7) 0.01257(18) Uani 1 1 d . . . C33 C 0.40714(11) 0.56096(9) 0.39266(7) 0.01409(19) Uani 1 1 d . . . H33 H 0.3576 0.4959 0.4044 0.017 Uiso 1 1 calc R . . C34 C 0.34178(12) 0.65514(10) 0.42524(8) 0.0197(2) Uani 1 1 d . . . H34A H 0.3954 0.7234 0.4220 0.030 Uiso 1 1 calc R . . H34B H 0.3306 0.6679 0.4832 0.030 Uiso 1 1 calc R . . H34C H 0.2576 0.6343 0.3913 0.030 Uiso 1 1 calc R . . C35 C 0.54491(12) 0.59631(11) 0.43894(8) 0.0200(2) Uani 1 1 d . . . H35A H 0.5831 0.5336 0.4201 0.030 Uiso 1 1 calc R . . H35B H 0.5432 0.6189 0.4989 0.030 Uiso 1 1 calc R . . H35C H 0.5963 0.6590 0.4273 0.030 Uiso 1 1 calc R . . N1 N 0.17052(9) 0.50911(8) 0.15404(6) 0.01293(16) Uani 1 1 d D . . H1A H 0.1550(16) 0.5731(12) 0.1815(10) 0.016 Uiso 1 1 d D . . H1B H 0.2508(13) 0.5257(14) 0.1443(10) 0.016 Uiso 1 1 d D . . C41 C -0.01067(10) 0.45840(9) 0.24104(7) 0.01301(18) Uani 1 1 d . . . C42 C -0.04146(11) 0.51865(10) 0.31715(7) 0.0159(2) Uani 1 1 d . . . H42 H 0.0145 0.5358 0.3669 0.019 Uiso 1 1 calc R . . C43 C -0.15338(12) 0.55443(11) 0.32169(8) 0.0188(2) Uani 1 1 d . . . H43 H -0.1734 0.5949 0.3742 0.023 Uiso 1 1 calc R . . C44 C -0.23491(11) 0.53074(11) 0.24948(8) 0.0200(2) Uani 1 1 d . . . H44 H -0.3135 0.5511 0.2523 0.024 Uiso 1 1 calc R . . C45 C -0.20092(11) 0.47700(10) 0.17284(8) 0.0175(2) Uani 1 1 d . . . H45 H -0.2553 0.4636 0.1233 0.021 Uiso 1 1 calc R . . C46 C -0.08792(10) 0.44216(9) 0.16721(7) 0.01371(18) Uani 1 1 d . . . C47 C -0.04618(11) 0.39925(9) 0.08513(7) 0.01401(19) Uani 1 1 d . . . C48 C 0.08311(11) 0.43799(9) 0.07881(7) 0.01350(18) Uani 1 1 d . . . C49 C 0.12602(12) 0.40616(10) 0.00224(7) 0.0175(2) Uani 1 1 d . . . H49 H 0.2135 0.4345 -0.0016 0.021 Uiso 1 1 calc R . . C50 C 0.04075(13) 0.33273(11) -0.06892(8) 0.0211(2) Uani 1 1 d . . . H50 H 0.0701 0.3107 -0.1213 0.025 Uiso 1 1 calc R . . C51 C -0.08718(13) 0.29168(11) -0.06342(8) 0.0209(2) Uani 1 1 d . . . H51 H -0.1451 0.2404 -0.1117 0.025 Uiso 1 1 calc R . . C52 C -0.13010(12) 0.32605(10) 0.01317(7) 0.0179(2) Uani 1 1 d . . . H52 H -0.2181 0.2991 0.0164 0.021 Uiso 1 1 calc R . . S1 S 0.22585(3) 0.84246(2) 0.308619(18) 0.01673(5) Uani 1 1 d . . . O1 O 0.21501(12) 0.72622(8) 0.26041(7) 0.0302(2) Uani 1 1 d . . . O2 O 0.19988(11) 0.90357(8) 0.25752(6) 0.0271(2) Uani 1 1 d . . . O3 O 0.34687(10) 0.89709(9) 0.36565(6) 0.0277(2) Uani 1 1 d . . . C61 C 0.10386(16) 0.84153(16) 0.37153(11) 0.0379(4) Uani 1 1 d . . . H61A H 0.0204 0.8016 0.3362 0.057 Uiso 1 1 calc R . . H61B H 0.1037 0.9183 0.4041 0.057 Uiso 1 1 calc R . . H61C H 0.1197 0.8042 0.4094 0.057 Uiso 1 1 calc R . . C1S C 0.35739(15) 0.04218(12) 0.55659(9) 0.0268(3) Uani 1 1 d DU . . H1S1 H 0.3707 0.0092 0.4980 0.032 Uiso 1 1 calc R . . H1S2 H 0.4408 0.0917 0.5898 0.032 Uiso 1 1 calc R . . Cl1S Cl 0.24491(5) 0.12072(4) 0.56248(3) 0.04654(11) Uani 1 1 d DU . . Cl2S Cl 0.30339(4) -0.06444(4) 0.59424(3) 0.04027(9) Uani 1 1 d DU . . C2S C 0.40236(14) 1.00040(13) 0.15370(9) 0.0282(3) Uani 1 1 d DU . . H2S1 H 0.3595 0.9523 0.1823 0.034 Uiso 1 1 calc R . . H2S2 H 0.3939 1.0764 0.1830 0.034 Uiso 1 1 calc R . . Cl3S Cl 0.56675(4) 1.00416(3) 0.15930(3) 0.03608(8) Uani 1 1 d DU . . Cl4S Cl 0.32515(4) 0.94920(3) 0.04978(2) 0.03010(7) Uani 1 1 d DU . . 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 0.00900(4) 0.01237(4) 0.01099(4) 0.00524(3) 0.00072(2) 0.00406(3) P1 0.01017(11) 0.01319(12) 0.01251(11) 0.00598(9) 0.00225(9) 0.00379(9) C1 0.0136(5) 0.0162(5) 0.0174(5) 0.0054(4) 0.0021(4) 0.0015(4) C2 0.0220(6) 0.0278(7) 0.0204(6) -0.0019(5) 0.0053(5) -0.0010(5) C3 0.0226(6) 0.0161(5) 0.0274(6) 0.0090(5) 0.0009(5) 0.0013(4) C4 0.0179(5) 0.0204(6) 0.0245(6) 0.0082(5) -0.0056(4) 0.0000(4) C5 0.0146(5) 0.0189(5) 0.0152(5) 0.0090(4) 0.0049(4) 0.0063(4) C6 0.0142(5) 0.0223(5) 0.0220(5) 0.0102(4) 0.0067(4) 0.0064(4) C7 0.0241(6) 0.0252(6) 0.0198(5) 0.0143(5) 0.0083(4) 0.0103(5) C8 0.0172(5) 0.0211(5) 0.0145(5) 0.0066(4) 0.0029(4) 0.0068(4) C11 0.0118(4) 0.0126(4) 0.0132(4) 0.0052(4) 0.0023(3) 0.0050(4) C12 0.0157(5) 0.0136(5) 0.0168(5) 0.0073(4) 0.0033(4) 0.0053(4) C13 0.0190(5) 0.0155(5) 0.0177(5) 0.0080(4) 0.0023(4) 0.0084(4) C14 0.0152(5) 0.0167(5) 0.0178(5) 0.0070(4) 0.0007(4) 0.0077(4) C15 0.0123(4) 0.0149(5) 0.0166(5) 0.0067(4) 0.0017(4) 0.0049(4) C16 0.0120(4) 0.0111(4) 0.0120(4) 0.0043(3) 0.0014(3) 0.0042(3) C21 0.0097(4) 0.0124(4) 0.0138(4) 0.0060(4) 0.0009(3) 0.0035(3) C22 0.0110(4) 0.0144(4) 0.0145(4) 0.0063(4) 0.0017(3) 0.0040(4) C27 0.0172(5) 0.0143(5) 0.0145(5) 0.0053(4) 0.0041(4) 0.0053(4) C28 0.0206(5) 0.0206(5) 0.0230(6) 0.0079(5) 0.0084(4) 0.0097(4) C29 0.0240(6) 0.0200(5) 0.0154(5) 0.0052(4) 0.0019(4) 0.0047(5) C23 0.0126(4) 0.0184(5) 0.0155(5) 0.0088(4) 0.0023(4) 0.0046(4) C24 0.0107(4) 0.0161(5) 0.0189(5) 0.0102(4) -0.0006(4) 0.0019(4) C30 0.0168(5) 0.0188(5) 0.0210(5) 0.0123(4) 0.0012(4) 0.0022(4) C31 0.0392(8) 0.0324(8) 0.0356(8) 0.0228(7) -0.0132(7) -0.0134(7) C32 0.0196(6) 0.0332(7) 0.0339(7) 0.0258(6) 0.0017(5) 0.0049(5) C25 0.0126(4) 0.0133(4) 0.0177(5) 0.0066(4) -0.0011(4) 0.0028(4) C26 0.0103(4) 0.0133(4) 0.0146(4) 0.0056(4) 0.0003(3) 0.0041(4) C33 0.0145(5) 0.0137(4) 0.0135(4) 0.0039(4) 0.0006(4) 0.0049(4) C34 0.0215(5) 0.0175(5) 0.0191(5) 0.0035(4) 0.0028(4) 0.0086(4) C35 0.0170(5) 0.0226(6) 0.0174(5) 0.0048(4) -0.0023(4) 0.0053(4) N1 0.0108(4) 0.0145(4) 0.0138(4) 0.0063(3) -0.0003(3) 0.0028(3) C41 0.0102(4) 0.0152(5) 0.0153(5) 0.0069(4) 0.0014(3) 0.0048(4) C42 0.0138(5) 0.0202(5) 0.0156(5) 0.0071(4) 0.0016(4) 0.0074(4) C43 0.0170(5) 0.0241(6) 0.0187(5) 0.0082(4) 0.0052(4) 0.0107(4) C44 0.0132(5) 0.0271(6) 0.0241(6) 0.0113(5) 0.0035(4) 0.0105(4) C45 0.0116(5) 0.0225(5) 0.0200(5) 0.0097(4) -0.0006(4) 0.0055(4) C46 0.0107(4) 0.0153(5) 0.0152(5) 0.0065(4) -0.0002(4) 0.0030(4) C47 0.0137(5) 0.0148(5) 0.0138(5) 0.0060(4) -0.0010(4) 0.0042(4) C48 0.0138(5) 0.0139(4) 0.0130(4) 0.0058(4) -0.0009(4) 0.0036(4) C49 0.0183(5) 0.0202(5) 0.0154(5) 0.0081(4) 0.0023(4) 0.0055(4) C50 0.0271(6) 0.0233(6) 0.0131(5) 0.0064(4) 0.0017(4) 0.0076(5) C51 0.0248(6) 0.0199(5) 0.0142(5) 0.0042(4) -0.0039(4) 0.0036(5) C52 0.0164(5) 0.0179(5) 0.0170(5) 0.0060(4) -0.0032(4) 0.0026(4) S1 0.02091(13) 0.01349(12) 0.01404(12) 0.00406(9) 0.00196(10) 0.00322(10) O1 0.0416(6) 0.0154(4) 0.0280(5) 0.0017(4) -0.0016(4) 0.0090(4) O2 0.0361(6) 0.0219(4) 0.0254(5) 0.0126(4) 0.0001(4) 0.0068(4) O3 0.0258(5) 0.0292(5) 0.0220(5) 0.0076(4) -0.0031(4) 0.0008(4) C61 0.0302(8) 0.0468(9) 0.0298(7) 0.0093(7) 0.0130(6) 0.0032(7) C1S 0.0301(7) 0.0251(6) 0.0226(6) 0.0101(5) 0.0005(5) 0.0012(5) Cl1S 0.0651(3) 0.02852(18) 0.0453(2) 0.01163(17) -0.0119(2) 0.01966(19) Cl2S 0.0433(2) 0.0376(2) 0.0556(3) 0.03343(19) 0.00938(19) 0.01471(17) C2S 0.0289(7) 0.0299(7) 0.0272(6) 0.0102(5) 0.0116(5) 0.0095(6) Cl3S 0.03129(18) 0.03246(18) 0.0467(2) 0.01391(16) 0.00807(16) 0.01346(15) Cl4S 0.03390(17) 0.02145(14) 0.02783(16) 0.00141(12) 0.00788(13) 0.00554(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 C41 2.0143(11) . ? Pd1 N1 2.1131(10) . ? Pd1 P1 2.3230(3) . ? Pd1 C21 2.4561(10) . ? P1 C11 1.8369(11) . ? P1 C5 1.8971(11) . ? P1 C1 1.8973(12) . ? C1 C2 1.5310(18) . ? C1 C4 1.5370(17) . ? C1 C3 1.5381(17) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.5363(17) . ? C5 C7 1.5393(16) . ? C5 C6 1.5412(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.4064(15) . ? C11 C16 1.4117(15) . ? C12 C13 1.3899(16) . ? C12 H12 0.9500 . ? C13 C14 1.3902(17) . ? C13 H13 0.9500 . ? C14 C15 1.3880(15) . ? C14 H14 0.9500 . ? C15 C16 1.4035(15) . ? C15 H15 0.9500 . ? C16 C21 1.5103(15) . ? C21 C26 1.4252(15) . ? C21 C22 1.4299(15) . ? C22 C23 1.3960(15) . ? C22 C27 1.5190(16) . ? C27 C28 1.5335(17) . ? C27 C29 1.5341(17) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C23 C24 1.3953(16) . ? C23 H23 0.9500 . ? C24 C25 1.3944(16) . ? C24 C30 1.5212(16) . ? C30 C31 1.5171(19) . ? C30 C32 1.5218(17) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C25 C26 1.4027(15) . ? C25 H25 0.9500 . ? C26 C33 1.5174(16) . ? C33 C34 1.5349(16) . ? C33 C35 1.5370(16) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N1 C48 1.4398(14) . ? N1 H1A 0.879(13) . ? N1 H1B 0.888(13) . ? C41 C42 1.3906(16) . ? C41 C46 1.4088(15) . ? C42 C43 1.3981(16) . ? C42 H42 0.9500 . ? C43 C44 1.3837(17) . ? C43 H43 0.9500 . ? C44 C45 1.3894(17) . ? C44 H44 0.9500 . ? C45 C46 1.4027(15) . ? C45 H45 0.9500 . ? C46 C47 1.4783(16) . ? C47 C52 1.3933(15) . ? C47 C48 1.4000(16) . ? C48 C49 1.3894(16) . ? C49 C50 1.3921(17) . ? C49 H49 0.9500 . ? C50 C51 1.3882(19) . ? C50 H50 0.9500 . ? C51 C52 1.3917(18) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? S1 O2 1.4514(10) . ? S1 O1 1.4520(10) . ? S1 O3 1.4593(11) . ? S1 C61 1.7624(16) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C1S Cl2S 1.7573(15) . ? C1S Cl1S 1.7657(16) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S Cl4S 1.7652(16) . ? C2S Cl3S 1.7652(16) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? 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 C41 Pd1 N1 79.86(4) . . ? C41 Pd1 P1 98.21(3) . . ? N1 Pd1 P1 163.32(3) . . ? C41 Pd1 C21 168.51(4) . . ? N1 Pd1 C21 99.71(4) . . ? P1 Pd1 C21 85.46(3) . . ? C11 P1 C5 105.26(5) . . ? C11 P1 C1 107.10(5) . . ? C5 P1 C1 109.76(5) . . ? C11 P1 Pd1 102.53(4) . . ? C5 P1 Pd1 120.83(4) . . ? C1 P1 Pd1 110.20(4) . . ? C2 C1 C4 107.49(11) . . ? C2 C1 C3 107.98(11) . . ? C4 C1 C3 109.19(10) . . ? C2 C1 P1 106.62(8) . . ? C4 C1 P1 109.30(8) . . ? C3 C1 P1 115.92(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 106.29(10) . . ? C8 C5 C6 110.22(10) . . ? C7 C5 C6 107.77(10) . . ? C8 C5 P1 106.72(8) . . ? C7 C5 P1 116.64(8) . . ? C6 C5 P1 109.10(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C11 C16 118.49(10) . . ? C12 C11 P1 122.09(8) . . ? C16 C11 P1 119.42(8) . . ? C13 C12 C11 121.79(10) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 119.34(10) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.81(10) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.54(10) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 118.87(10) . . ? C15 C16 C21 114.47(9) . . ? C11 C16 C21 126.57(9) . . ? C26 C21 C22 118.52(10) . . ? C26 C21 C16 120.02(9) . . ? C22 C21 C16 117.95(9) . . ? C26 C21 Pd1 83.92(6) . . ? C22 C21 Pd1 99.11(7) . . ? C16 C21 Pd1 105.52(7) . . ? C23 C22 C21 119.23(10) . . ? C23 C22 C27 118.37(10) . . ? C21 C22 C27 122.02(10) . . ? C22 C27 C28 110.34(10) . . ? C22 C27 C29 112.88(10) . . ? C28 C27 C29 109.63(10) . . ? C22 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C23 C22 122.55(10) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C25 C24 C23 118.00(10) . . ? C25 C24 C30 122.58(11) . . ? C23 C24 C30 119.41(10) . . ? C31 C30 C24 113.47(11) . . ? C31 C30 C32 111.31(12) . . ? C24 C30 C32 110.49(10) . . ? C31 C30 H30 107.1 . . ? C24 C30 H30 107.1 . . ? C32 C30 H30 107.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C24 C25 C26 121.88(10) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 119.66(10) . . ? C25 C26 C33 118.96(10) . . ? C21 C26 C33 120.95(10) . . ? C26 C33 C34 112.67(9) . . ? C26 C33 C35 110.04(9) . . ? C34 C33 C35 110.58(10) . . ? C26 C33 H33 107.8 . . ? C34 C33 H33 107.8 . . ? C35 C33 H33 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C48 N1 Pd1 106.54(7) . . ? C48 N1 H1A 116.3(11) . . ? Pd1 N1 H1A 107.2(11) . . ? C48 N1 H1B 111.6(11) . . ? Pd1 N1 H1B 109.1(11) . . ? H1A N1 H1B 105.9(15) . . ? C42 C41 C46 118.97(10) . . ? C42 C41 Pd1 120.90(8) . . ? C46 C41 Pd1 119.13(8) . . ? C41 C42 C43 121.16(11) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 119.83(11) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 119.48(11) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C44 C45 C46 121.29(11) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C41 118.89(10) . . ? C45 C46 C47 119.53(10) . . ? C41 C46 C47 121.32(10) . . ? C52 C47 C48 118.44(11) . . ? C52 C47 C46 123.26(10) . . ? C48 C47 C46 118.24(10) . . ? C49 C48 C47 120.72(10) . . ? C49 C48 N1 121.13(10) . . ? C47 C48 N1 118.13(10) . . ? C48 C49 C50 119.96(11) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 120.01(11) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 119.68(11) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C51 C52 C47 121.14(11) . . ? C51 C52 H52 119.4 . . ? C47 C52 H52 119.4 . . ? O2 S1 O1 113.01(6) . . ? O2 S1 O3 112.95(6) . . ? O1 S1 O3 112.15(7) . . ? O2 S1 C61 106.38(8) . . ? O1 S1 C61 105.52(8) . . ? O3 S1 C61 106.11(8) . . ? S1 C61 H61A 109.5 . . ? S1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? S1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Cl2S C1S Cl1S 110.80(8) . . ? Cl2S C1S H1S1 109.5 . . ? Cl1S C1S H1S1 109.5 . . ? Cl2S C1S H1S2 109.5 . . ? Cl1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 108.1 . . ? Cl4S C2S Cl3S 111.85(8) . . ? Cl4S C2S H2S1 109.2 . . ? Cl3S C2S H2S1 109.2 . . ? Cl4S C2S H2S2 109.2 . . ? Cl3S C2S H2S2 109.2 . . ? H2S1 C2S H2S2 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.879(13) 1.946(14) 2.7415(14) 149.9(15) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.903 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.063 # Attachment '- 6c.cif' data_x12062 _database_code_depnum_ccdc_archive 'CCDC 891256' #TrackingRef '- 6c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H66 N O5 P Pd S' _chemical_formula_weight 906.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5569(6) _cell_length_b 17.0797(7) _cell_length_c 16.7243(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.2220(10) _cell_angle_gamma 90.00 _cell_volume 4431.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9670 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 31.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8527 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus sealed tube' _diffrn_radiation_monochromator 'Incoatech ImuS multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 211874 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 31.00 _reflns_number_total 14118 _reflns_number_gt 12119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0274P)^2^+2.6220P] 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 14118 _refine_ls_number_parameters 529 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.729223(5) 0.747412(5) 0.991553(5) 0.01009(3) Uani 1 1 d . . . P1 P 0.702551(18) 0.827496(17) 0.884448(18) 0.01062(6) Uani 1 1 d . . . C1 C 0.75127(7) 0.92456(7) 0.90334(7) 0.0122(2) Uani 1 1 d . . . H1 H 0.7348 0.9589 0.8562 0.015 Uiso 1 1 calc R . . C2 C 0.71906(8) 0.96284(7) 0.97817(8) 0.0154(2) Uani 1 1 d . . . H2A H 0.7342 0.9293 1.0254 0.018 Uiso 1 1 calc R . . H2B H 0.6555 0.9676 0.9719 0.018 Uiso 1 1 calc R . . C3 C 0.75914(8) 1.04407(7) 0.99192(9) 0.0189(2) Uani 1 1 d . . . H3A H 0.7394 1.0789 0.9470 0.023 Uiso 1 1 calc R . . H3B H 0.7393 1.0666 1.0419 0.023 Uiso 1 1 calc R . . C4 C 0.85751(8) 1.04040(8) 0.99818(9) 0.0200(3) Uani 1 1 d . . . H4A H 0.8777 1.0116 1.0474 0.024 Uiso 1 1 calc R . . H4B H 0.8812 1.0942 1.0023 0.024 Uiso 1 1 calc R . . C5 C 0.89068(8) 0.99961(7) 0.92507(8) 0.0172(2) Uani 1 1 d . . . H5A H 0.8769 1.0320 0.8768 0.021 Uiso 1 1 calc R . . H5B H 0.9541 0.9942 0.9326 0.021 Uiso 1 1 calc R . . C6 C 0.85005(7) 0.91871(7) 0.91259(8) 0.0149(2) Uani 1 1 d . . . H6A H 0.8676 0.8849 0.9590 0.018 Uiso 1 1 calc R . . H6B H 0.8711 0.8944 0.8640 0.018 Uiso 1 1 calc R . . C7 C 0.74034(8) 0.79598(7) 0.78726(7) 0.0141(2) Uani 1 1 d . . . H7 H 0.7978 0.7715 0.8013 0.017 Uiso 1 1 calc R . . C8 C 0.68441(10) 0.72916(9) 0.75149(9) 0.0259(3) Uani 1 1 d . . . H8A H 0.6759 0.6896 0.7935 0.031 Uiso 1 1 calc R . . H8B H 0.6271 0.7498 0.7322 0.031 Uiso 1 1 calc R . . C9 C 0.72673(12) 0.69060(9) 0.68192(10) 0.0324(4) Uani 1 1 d . . . H9A H 0.7799 0.6634 0.7029 0.039 Uiso 1 1 calc R . . H9B H 0.6871 0.6508 0.6569 0.039 Uiso 1 1 calc R . . C0 C 0.74920(10) 0.74905(9) 0.61866(9) 0.0243(3) Uani 1 1 d . . . H0A H 0.6955 0.7702 0.5915 0.029 Uiso 1 1 calc R . . H0B H 0.7817 0.7222 0.5779 0.029 Uiso 1 1 calc R . . C11 C 0.80307(8) 0.81605(8) 0.65530(8) 0.0190(2) Uani 1 1 d . . . H11A H 0.8139 0.8547 0.6131 0.023 Uiso 1 1 calc R . . H11B H 0.8594 0.7956 0.6775 0.023 Uiso 1 1 calc R . . C12 C 0.75702(9) 0.85623(8) 0.72203(8) 0.0187(2) Uani 1 1 d . . . H12A H 0.7017 0.8787 0.6997 0.022 Uiso 1 1 calc R . . H12B H 0.7931 0.8994 0.7454 0.022 Uiso 1 1 calc R . . C21 C 0.58568(7) 0.83850(6) 0.87415(7) 0.0116(2) Uani 1 1 d . . . C22 C 0.54314(8) 0.88347(7) 0.81268(7) 0.0133(2) Uani 1 1 d . . . O1 O 0.59442(6) 0.93098(5) 0.77085(6) 0.01767(18) Uani 1 1 d . . . C27 C 0.55440(9) 0.97032(9) 0.70221(9) 0.0250(3) Uani 1 1 d . . . H27A H 0.5306 0.9315 0.6635 0.038 Uiso 1 1 calc R . . H27B H 0.5973 1.0024 0.6773 0.038 Uiso 1 1 calc R . . H27C H 0.5079 1.0040 0.7189 0.038 Uiso 1 1 calc R . . C23 C 0.45449(8) 0.87902(7) 0.79723(8) 0.0155(2) Uani 1 1 d . . . H23 H 0.4265 0.9081 0.7545 0.019 Uiso 1 1 calc R . . C24 C 0.40694(8) 0.83148(7) 0.84504(8) 0.0162(2) Uani 1 1 d . . . H24 H 0.3464 0.8271 0.8337 0.019 Uiso 1 1 calc R . . C25 C 0.44659(7) 0.79036(7) 0.90901(7) 0.0140(2) Uani 1 1 d . . . O2 O 0.40244(6) 0.74437(5) 0.95923(6) 0.01826(18) Uani 1 1 d . . . C28 C 0.31691(8) 0.72195(8) 0.93054(8) 0.0197(2) Uani 1 1 d . . . H28A H 0.2785 0.7673 0.9320 0.029 Uiso 1 1 calc R . . H28B H 0.2964 0.6803 0.9647 0.029 Uiso 1 1 calc R . . H28C H 0.3174 0.7029 0.8753 0.029 Uiso 1 1 calc R . . C26 C 0.53662(7) 0.79403(7) 0.92519(7) 0.0116(2) Uani 1 1 d . . . C31 C 0.57273(7) 0.75063(6) 0.99864(7) 0.0115(2) Uani 1 1 d . . . C32 C 0.58565(7) 0.66822(7) 0.99551(7) 0.0122(2) Uani 1 1 d . . . C37 C 0.57935(8) 0.62381(7) 0.91648(7) 0.0152(2) Uani 1 1 d . . . H37 H 0.5771 0.6629 0.8719 0.018 Uiso 1 1 calc R . . C38 C 0.65681(9) 0.57008(8) 0.90749(9) 0.0228(3) Uani 1 1 d . . . H38A H 0.7101 0.6009 0.9137 0.034 Uiso 1 1 calc R . . H38B H 0.6518 0.5457 0.8543 0.034 Uiso 1 1 calc R . . H38C H 0.6581 0.5293 0.9487 0.034 Uiso 1 1 calc R . . C39 C 0.49609(10) 0.57584(9) 0.90883(9) 0.0247(3) Uani 1 1 d . . . H39A H 0.4966 0.5377 0.9526 0.037 Uiso 1 1 calc R . . H39B H 0.4918 0.5483 0.8573 0.037 Uiso 1 1 calc R . . H39C H 0.4465 0.6109 0.9117 0.037 Uiso 1 1 calc R . . C33 C 0.59482(7) 0.62529(7) 1.06698(7) 0.0135(2) Uani 1 1 d . . . H33 H 0.6063 0.5708 1.0646 0.016 Uiso 1 1 calc R . . C34 C 0.58759(7) 0.66004(7) 1.14134(7) 0.0130(2) Uani 1 1 d . . . C40 C 0.59353(8) 0.61017(7) 1.21692(7) 0.0149(2) Uani 1 1 d . . . H40 H 0.5995 0.5545 1.1998 0.018 Uiso 1 1 calc R . . C41 C 0.51110(9) 0.61575(9) 1.26086(9) 0.0250(3) Uani 1 1 d . . . H41A H 0.5163 0.5822 1.3085 0.037 Uiso 1 1 calc R . . H41B H 0.4620 0.5985 1.2252 0.037 Uiso 1 1 calc R . . H41C H 0.5022 0.6701 1.2771 0.037 Uiso 1 1 calc R . . C42 C 0.67234(9) 0.62961(10) 1.27328(9) 0.0272(3) Uani 1 1 d . . . H42A H 0.7248 0.6215 1.2453 0.041 Uiso 1 1 calc R . . H42B H 0.6735 0.5954 1.3204 0.041 Uiso 1 1 calc R . . H42C H 0.6693 0.6844 1.2903 0.041 Uiso 1 1 calc R . . C35 C 0.57531(7) 0.74120(7) 1.14430(7) 0.0133(2) Uani 1 1 d . . . H35 H 0.5720 0.7657 1.1950 0.016 Uiso 1 1 calc R . . C36 C 0.56785(7) 0.78710(7) 1.07519(7) 0.0121(2) Uani 1 1 d . . . C43 C 0.54600(8) 0.87346(7) 1.08283(8) 0.0153(2) Uani 1 1 d . . . H43 H 0.5518 0.8988 1.0296 0.018 Uiso 1 1 calc R . . C44 C 0.45221(9) 0.88290(9) 1.10390(10) 0.0245(3) Uani 1 1 d . . . H44A H 0.4137 0.8585 1.0621 0.037 Uiso 1 1 calc R . . H44B H 0.4384 0.9387 1.1076 0.037 Uiso 1 1 calc R . . H44C H 0.4446 0.8575 1.1555 0.037 Uiso 1 1 calc R . . C45 C 0.60587(8) 0.91615(7) 1.14506(8) 0.0182(2) Uani 1 1 d . . . H45A H 0.5948 0.8979 1.1989 0.027 Uiso 1 1 calc R . . H45B H 0.5952 0.9726 1.1412 0.027 Uiso 1 1 calc R . . H45C H 0.6660 0.9053 1.1349 0.027 Uiso 1 1 calc R . . C51 C 0.85369(7) 0.72977(7) 0.96990(8) 0.0133(2) Uani 1 1 d . . . C52 C 0.87612(8) 0.68705(7) 0.90334(8) 0.0166(2) Uani 1 1 d . . . H52 H 0.8320 0.6677 0.8663 0.020 Uiso 1 1 calc R . . C53 C 0.96233(9) 0.67225(8) 0.89032(9) 0.0211(3) Uani 1 1 d . . . H53 H 0.9764 0.6439 0.8442 0.025 Uiso 1 1 calc R . . C54 C 1.02723(9) 0.69894(8) 0.94457(9) 0.0233(3) Uani 1 1 d . . . H54 H 1.0860 0.6907 0.9350 0.028 Uiso 1 1 calc R . . C55 C 1.00579(8) 0.73778(8) 1.01295(9) 0.0197(3) Uani 1 1 d . . . H55 H 1.0503 0.7544 1.0511 0.024 Uiso 1 1 calc R . . C57 C 0.89946(7) 0.79471(7) 1.10063(7) 0.0137(2) Uani 1 1 d . . . C58 C 0.82615(7) 0.77441(7) 1.13983(7) 0.0131(2) Uani 1 1 d . . . N1 N 0.77375(6) 0.71037(6) 1.10793(6) 0.01330(19) Uani 1 1 d D . . H1A H 0.8019(10) 0.6643(8) 1.1081(10) 0.016 Uiso 1 1 d D . . H1B H 0.7287(9) 0.7056(9) 1.1357(9) 0.016 Uiso 1 1 d D . . C59 C 0.80240(8) 0.81692(7) 1.20543(8) 0.0168(2) Uani 1 1 d . . . H59 H 0.7520 0.8029 1.2309 0.020 Uiso 1 1 calc R . . C60 C 0.85219(9) 0.88005(8) 1.23398(8) 0.0210(3) Uani 1 1 d . . . H60 H 0.8354 0.9098 1.2782 0.025 Uiso 1 1 calc R . . C61 C 0.92669(9) 0.89923(8) 1.19731(8) 0.0225(3) Uani 1 1 d . . . H61 H 0.9618 0.9414 1.2174 0.027 Uiso 1 1 calc R . . C62 C 0.94985(8) 0.85699(8) 1.13147(8) 0.0182(2) Uani 1 1 d . . . H62 H 1.0009 0.8706 1.1069 0.022 Uiso 1 1 calc R . . C66 C 0.91969(8) 0.75310(7) 1.02713(8) 0.0138(2) Uani 1 1 d . . . S1 S 0.18712(2) 0.518759(17) 0.892657(19) 0.01567(6) Uani 1 1 d . . . O3 O 0.14863(7) 0.58378(6) 0.84716(6) 0.0240(2) Uani 1 1 d . . . O4 O 0.27974(6) 0.52568(6) 0.90856(7) 0.0261(2) Uani 1 1 d . . . O5 O 0.16106(7) 0.44251(6) 0.85929(7) 0.0279(2) Uani 1 1 d . . . C71 C 0.14347(11) 0.52156(10) 0.98758(9) 0.0297(3) Uani 1 1 d . . . H71A H 0.1637 0.4760 1.0192 0.045 Uiso 1 1 calc R . . H71B H 0.0804 0.5206 0.9802 0.045 Uiso 1 1 calc R . . H71C H 0.1622 0.5696 1.0158 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01021(4) 0.01034(4) 0.00947(5) 0.00060(3) -0.00104(3) -0.00015(3) P1 0.01148(12) 0.01092(12) 0.00933(14) 0.00014(10) -0.00006(10) -0.00074(9) C1 0.0133(5) 0.0113(5) 0.0121(5) -0.0001(4) 0.0010(4) -0.0018(4) C2 0.0177(5) 0.0144(5) 0.0146(6) -0.0025(4) 0.0040(4) -0.0027(4) C3 0.0201(6) 0.0144(5) 0.0225(7) -0.0048(5) 0.0042(5) -0.0019(4) C4 0.0197(6) 0.0162(5) 0.0237(7) -0.0047(5) -0.0014(5) -0.0037(4) C5 0.0138(5) 0.0145(5) 0.0231(7) -0.0002(5) 0.0006(5) -0.0024(4) C6 0.0125(5) 0.0131(5) 0.0191(6) -0.0011(4) 0.0014(4) -0.0013(4) C7 0.0159(5) 0.0147(5) 0.0118(6) -0.0012(4) 0.0023(4) -0.0014(4) C8 0.0325(7) 0.0262(7) 0.0203(7) -0.0105(5) 0.0113(6) -0.0157(6) C9 0.0472(9) 0.0260(7) 0.0264(8) -0.0147(6) 0.0189(7) -0.0179(6) C0 0.0247(6) 0.0332(7) 0.0155(7) -0.0088(5) 0.0052(5) -0.0085(5) C11 0.0214(6) 0.0227(6) 0.0134(6) -0.0022(5) 0.0048(5) -0.0033(5) C12 0.0250(6) 0.0181(6) 0.0134(6) 0.0004(4) 0.0048(5) 0.0000(5) C21 0.0122(5) 0.0116(5) 0.0108(5) 0.0001(4) -0.0008(4) -0.0004(4) C22 0.0151(5) 0.0132(5) 0.0115(6) 0.0016(4) 0.0004(4) 0.0005(4) O1 0.0169(4) 0.0205(4) 0.0156(5) 0.0097(3) 0.0008(3) 0.0008(3) C27 0.0232(6) 0.0304(7) 0.0216(7) 0.0166(6) 0.0024(5) 0.0045(5) C23 0.0162(5) 0.0171(5) 0.0127(6) 0.0031(4) -0.0021(4) 0.0011(4) C24 0.0132(5) 0.0202(6) 0.0147(6) 0.0027(4) -0.0029(4) -0.0001(4) C25 0.0132(5) 0.0164(5) 0.0122(6) 0.0023(4) -0.0008(4) -0.0030(4) O2 0.0137(4) 0.0246(5) 0.0159(5) 0.0072(3) -0.0027(3) -0.0070(3) C28 0.0144(5) 0.0273(6) 0.0169(6) 0.0013(5) -0.0011(4) -0.0069(5) C26 0.0136(5) 0.0114(5) 0.0095(5) 0.0009(4) -0.0019(4) -0.0003(4) C31 0.0103(4) 0.0127(5) 0.0112(5) 0.0018(4) -0.0010(4) -0.0016(4) C32 0.0122(5) 0.0123(5) 0.0116(5) 0.0012(4) -0.0020(4) -0.0023(4) C37 0.0216(6) 0.0121(5) 0.0115(6) 0.0006(4) -0.0027(4) -0.0031(4) C38 0.0298(7) 0.0183(6) 0.0197(7) -0.0051(5) -0.0017(5) 0.0029(5) C39 0.0296(7) 0.0248(7) 0.0182(7) 0.0012(5) -0.0075(5) -0.0123(5) C33 0.0135(5) 0.0126(5) 0.0140(6) 0.0021(4) -0.0023(4) -0.0023(4) C34 0.0104(4) 0.0157(5) 0.0127(6) 0.0037(4) -0.0015(4) -0.0019(4) C40 0.0152(5) 0.0170(5) 0.0122(6) 0.0043(4) -0.0008(4) -0.0014(4) C41 0.0224(6) 0.0283(7) 0.0254(7) 0.0130(6) 0.0090(5) 0.0040(5) C42 0.0248(7) 0.0378(8) 0.0176(7) 0.0117(6) -0.0084(5) -0.0101(6) C35 0.0130(5) 0.0164(5) 0.0105(5) 0.0007(4) 0.0001(4) -0.0007(4) C36 0.0105(5) 0.0136(5) 0.0120(6) 0.0011(4) -0.0003(4) -0.0012(4) C43 0.0178(5) 0.0141(5) 0.0138(6) 0.0012(4) 0.0001(4) 0.0024(4) C44 0.0183(6) 0.0247(6) 0.0303(8) -0.0021(6) 0.0008(5) 0.0060(5) C45 0.0228(6) 0.0164(5) 0.0153(6) -0.0021(4) 0.0001(5) -0.0003(4) C51 0.0134(5) 0.0111(5) 0.0154(6) 0.0009(4) 0.0001(4) 0.0016(4) C52 0.0196(5) 0.0135(5) 0.0167(6) -0.0013(4) 0.0014(5) 0.0022(4) C53 0.0233(6) 0.0168(6) 0.0238(7) -0.0025(5) 0.0071(5) 0.0051(5) C54 0.0164(6) 0.0228(6) 0.0314(8) -0.0003(5) 0.0064(5) 0.0056(5) C55 0.0135(5) 0.0213(6) 0.0242(7) 0.0003(5) 0.0001(5) 0.0015(4) C57 0.0133(5) 0.0138(5) 0.0136(6) 0.0009(4) -0.0020(4) -0.0001(4) C58 0.0138(5) 0.0126(5) 0.0122(6) 0.0021(4) -0.0036(4) -0.0010(4) N1 0.0119(4) 0.0141(4) 0.0135(5) 0.0022(4) -0.0013(4) -0.0021(3) C59 0.0185(5) 0.0193(6) 0.0124(6) 0.0015(4) -0.0004(4) -0.0001(4) C60 0.0283(7) 0.0206(6) 0.0139(6) -0.0029(5) -0.0001(5) -0.0022(5) C61 0.0291(7) 0.0197(6) 0.0180(7) -0.0031(5) -0.0025(5) -0.0083(5) C62 0.0182(5) 0.0190(6) 0.0170(6) 0.0005(5) -0.0013(5) -0.0058(4) C66 0.0124(5) 0.0128(5) 0.0159(6) 0.0009(4) -0.0001(4) 0.0004(4) S1 0.01769(13) 0.01489(13) 0.01406(15) 0.00037(10) -0.00129(11) 0.00290(10) O3 0.0323(5) 0.0220(5) 0.0175(5) 0.0041(4) 0.0002(4) 0.0116(4) O4 0.0188(4) 0.0269(5) 0.0321(6) 0.0059(4) -0.0014(4) -0.0007(4) O5 0.0343(6) 0.0184(5) 0.0288(6) -0.0045(4) -0.0117(4) 0.0011(4) C71 0.0353(8) 0.0352(8) 0.0194(7) 0.0070(6) 0.0077(6) 0.0086(6) _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 C51 2.0185(12) . ? Pd1 N1 2.1143(11) . ? Pd1 P1 2.2677(3) . ? Pd1 C31 2.4467(11) . ? Pd1 C32 2.6162(11) . ? P1 C21 1.8233(11) . ? P1 C1 1.8404(12) . ? P1 C7 1.8487(12) . ? C1 C2 1.5288(16) . ? C1 C6 1.5364(16) . ? C1 H1 1.0000 . ? C2 C3 1.5314(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5275(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5295(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.5275(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5300(18) . ? C7 C12 1.5356(17) . ? C7 H7 1.0000 . ? C8 C9 1.5277(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C0 1.514(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C0 C11 1.5204(19) . ? C0 H0A 0.9900 . ? C0 H0B 0.9900 . ? C11 C12 1.5321(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C21 C26 1.4085(16) . ? C21 C22 1.4087(16) . ? C22 O1 1.3662(14) . ? C22 C23 1.3865(16) . ? O1 C27 1.4323(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C23 C24 1.3904(17) . ? C23 H23 0.9500 . ? C24 C25 1.3860(17) . ? C24 H24 0.9500 . ? C25 O2 1.3707(14) . ? C25 C26 1.4082(16) . ? O2 C28 1.4329(15) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26 C31 1.5075(16) . ? C31 C32 1.4232(15) . ? C31 C36 1.4308(17) . ? C32 C33 1.4006(16) . ? C32 C37 1.5207(17) . ? C37 C39 1.5301(18) . ? C37 C38 1.5309(18) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C33 C34 1.3899(17) . ? C33 H33 0.9500 . ? C34 C35 1.4006(16) . ? C34 C40 1.5215(17) . ? C40 C42 1.5270(18) . ? C40 C41 1.5271(17) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C35 C36 1.3944(16) . ? C35 H35 0.9500 . ? C36 C43 1.5213(16) . ? C43 C45 1.5295(18) . ? C43 C44 1.5346(18) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C51 C52 1.3967(17) . ? C51 C66 1.4087(17) . ? C52 C53 1.3974(17) . ? C52 H52 0.9500 . ? C53 C54 1.384(2) . ? C53 H53 0.9500 . ? C54 C55 1.384(2) . ? C54 H54 0.9500 . ? C55 C66 1.4021(17) . ? C55 H55 0.9500 . ? C57 C62 1.3974(17) . ? C57 C58 1.4003(16) . ? C57 C66 1.4737(17) . ? C58 C59 1.3881(17) . ? C58 N1 1.4426(15) . ? N1 H1A 0.901(13) . ? N1 H1B 0.873(13) . ? C59 C60 1.3915(18) . ? C59 H59 0.9500 . ? C60 C61 1.3898(19) . ? C60 H60 0.9500 . ? C61 C62 1.3861(19) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? S1 O3 1.4504(10) . ? S1 O4 1.4506(10) . ? S1 O5 1.4624(10) . ? S1 C71 1.7727(15) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C51 Pd1 N1 82.35(5) . . ? C51 Pd1 P1 94.04(4) . . ? N1 Pd1 P1 159.42(3) . . ? C51 Pd1 C31 169.45(4) . . ? N1 Pd1 C31 102.82(4) . . ? P1 Pd1 C31 84.25(3) . . ? C51 Pd1 C32 139.41(4) . . ? N1 Pd1 C32 92.55(4) . . ? P1 Pd1 C32 103.00(3) . . ? C31 Pd1 C32 32.43(4) . . ? C21 P1 C1 108.58(5) . . ? C21 P1 C7 109.05(6) . . ? C1 P1 C7 105.04(5) . . ? C21 P1 Pd1 105.07(4) . . ? C1 P1 Pd1 111.02(4) . . ? C7 P1 Pd1 117.86(4) . . ? C2 C1 C6 109.33(10) . . ? C2 C1 P1 111.72(8) . . ? C6 C1 P1 110.79(8) . . ? C2 C1 H1 108.3 . . ? C6 C1 H1 108.3 . . ? P1 C1 H1 108.3 . . ? C1 C2 C3 110.86(10) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.58(10) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.05(11) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 111.14(10) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 110.84(9) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 110.06(11) . . ? C8 C7 P1 110.63(8) . . ? C12 C7 P1 120.72(8) . . ? C8 C7 H7 104.6 . . ? C12 C7 H7 104.6 . . ? P1 C7 H7 104.6 . . ? C9 C8 C7 110.78(11) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C0 C9 C8 112.49(13) . . ? C0 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C0 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C0 C11 111.31(12) . . ? C9 C0 H0A 109.4 . . ? C11 C0 H0A 109.4 . . ? C9 C0 H0B 109.4 . . ? C11 C0 H0B 109.4 . . ? H0A C0 H0B 108.0 . . ? C0 C11 C12 110.93(11) . . ? C0 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C0 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C7 109.26(10) . . ? C11 C12 H12A 109.8 . . ? C7 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C7 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C26 C21 C22 119.33(10) . . ? C26 C21 P1 117.92(9) . . ? C22 C21 P1 122.46(9) . . ? O1 C22 C23 123.19(11) . . ? O1 C22 C21 115.91(10) . . ? C23 C22 C21 120.90(11) . . ? C22 O1 C27 116.96(10) . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C23 C24 119.27(11) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.96(11) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? O2 C25 C24 123.28(11) . . ? O2 C25 C26 116.35(10) . . ? C24 C25 C26 120.37(11) . . ? C25 O2 C28 116.28(10) . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C26 C21 118.90(10) . . ? C25 C26 C31 116.13(10) . . ? C21 C26 C31 124.95(10) . . ? C32 C31 C36 118.71(11) . . ? C32 C31 C26 120.10(11) . . ? C36 C31 C26 118.29(10) . . ? C32 C31 Pd1 80.35(7) . . ? C36 C31 Pd1 99.88(7) . . ? C26 C31 Pd1 106.50(7) . . ? C33 C32 C31 119.48(11) . . ? C33 C32 C37 118.46(10) . . ? C31 C32 C37 121.67(11) . . ? C33 C32 Pd1 104.99(7) . . ? C31 C32 Pd1 67.22(6) . . ? C37 C32 Pd1 103.67(7) . . ? C32 C37 C39 109.86(11) . . ? C32 C37 C38 112.56(10) . . ? C39 C37 C38 109.78(11) . . ? C32 C37 H37 108.2 . . ? C39 C37 H37 108.2 . . ? C38 C37 H37 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C33 C32 122.02(11) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 118.33(11) . . ? C33 C34 C40 120.01(11) . . ? C35 C34 C40 121.66(11) . . ? C34 C40 C42 112.83(10) . . ? C34 C40 C41 111.29(10) . . ? C42 C40 C41 110.72(12) . . ? C34 C40 H40 107.2 . . ? C42 C40 H40 107.2 . . ? C41 C40 H40 107.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C36 C35 C34 122.03(11) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C31 119.36(10) . . ? C35 C36 C43 118.75(11) . . ? C31 C36 C43 121.62(10) . . ? C36 C43 C45 113.00(10) . . ? C36 C43 C44 110.07(10) . . ? C45 C43 C44 109.60(11) . . ? C36 C43 H43 108.0 . . ? C45 C43 H43 108.0 . . ? C44 C43 H43 108.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C52 C51 C66 118.49(11) . . ? C52 C51 Pd1 121.35(9) . . ? C66 C51 Pd1 119.78(9) . . ? C51 C52 C53 121.17(12) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C54 C53 C52 120.04(12) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 119.40(12) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C66 121.38(13) . . ? C54 C55 H55 119.3 . . ? C66 C55 H55 119.3 . . ? C62 C57 C58 118.03(11) . . ? C62 C57 C66 121.76(11) . . ? C58 C57 C66 120.16(11) . . ? C59 C58 C57 120.92(11) . . ? C59 C58 N1 120.85(11) . . ? C57 C58 N1 118.17(11) . . ? C58 N1 Pd1 104.56(7) . . ? C58 N1 H1A 113.6(10) . . ? Pd1 N1 H1A 113.0(10) . . ? C58 N1 H1B 109.2(11) . . ? Pd1 N1 H1B 107.2(11) . . ? H1A N1 H1B 109.0(15) . . ? C58 C59 C60 120.18(12) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C61 C60 C59 119.50(12) . . ? C61 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C62 C61 C60 120.13(12) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C61 C62 C57 121.19(12) . . ? C61 C62 H62 119.4 . . ? C57 C62 H62 119.4 . . ? C55 C66 C51 119.33(12) . . ? C55 C66 C57 119.77(11) . . ? C51 C66 C57 120.89(10) . . ? O3 S1 O4 113.57(6) . . ? O3 S1 O5 112.93(6) . . ? O4 S1 O5 112.72(6) . . ? O3 S1 C71 106.18(7) . . ? O4 S1 C71 105.93(7) . . ? O5 S1 C71 104.60(8) . . ? S1 C71 H71A 109.5 . . ? S1 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? S1 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.901(13) 1.977(13) 2.8399(14) 159.8(14) 3_667 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.567 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.064 # Attachment '- 6n.cif' data_x12061 _database_code_depnum_ccdc_archive 'CCDC 891257' #TrackingRef '- 6n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C56 H42 N P2 Pd) (C H3 S O3) 3.5(C H2 Cl2)' _chemical_formula_sum 'C60.50 H52 Cl7 N O3 P2 Pd S' _chemical_formula_weight 1289.58 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9763(14) _cell_length_b 20.426(2) _cell_length_c 21.290(2) _cell_angle_alpha 75.424(2) _cell_angle_beta 85.472(2) _cell_angle_gamma 76.307(2) _cell_volume 5713.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 31.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7972 _exptl_absorpt_correction_T_max 0.9615 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus sealed tube' _diffrn_radiation_monochromator 'Incoatech ImuS multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 370048 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 31.00 _reflns_number_total 36383 _reflns_number_gt 30210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0434P)^2^+8.3609P] 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 36383 _refine_ls_number_parameters 1552 _refine_ls_number_restraints 828 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.900969(11) 0.237664(8) -0.027737(7) 0.01441(3) Uani 1 1 d . . . P1 P 0.91510(4) 0.34858(3) -0.04166(3) 0.01499(9) Uani 1 1 d . . . P2 P 0.88153(4) 0.22092(3) 0.08598(3) 0.01631(9) Uani 1 1 d . . . C1 C 0.97581(15) 0.38464(11) -0.11779(10) 0.0174(4) Uani 1 1 d . . . C2 C 0.94319(16) 0.45212(12) -0.15477(11) 0.0219(4) Uani 1 1 d . . . H2 H 0.8895 0.4827 -0.1394 0.026 Uiso 1 1 calc R . . C3 C 0.98896(18) 0.47497(13) -0.21420(12) 0.0264(5) Uani 1 1 d . . . H3 H 0.9672 0.5214 -0.2387 0.032 Uiso 1 1 calc R . . C4 C 1.06586(18) 0.43046(14) -0.23767(11) 0.0271(5) Uani 1 1 d . . . H4 H 1.0956 0.4459 -0.2787 0.033 Uiso 1 1 calc R . . C5 C 1.09941(16) 0.36328(13) -0.20122(11) 0.0233(4) Uani 1 1 d . . . H5 H 1.1528 0.3329 -0.2171 0.028 Uiso 1 1 calc R . . C6 C 1.05519(15) 0.34035(12) -0.14166(11) 0.0195(4) Uani 1 1 d . . . H6 H 1.0788 0.2943 -0.1168 0.023 Uiso 1 1 calc R . . C7 C 0.79709(14) 0.40873(11) -0.03995(10) 0.0163(3) Uani 1 1 d . . . C8 C 0.78985(16) 0.47745(11) -0.03747(11) 0.0198(4) Uani 1 1 d . . . H8 H 0.8477 0.4930 -0.0340 0.024 Uiso 1 1 calc R . . C9 C 0.69832(17) 0.52303(12) -0.04009(11) 0.0228(4) Uani 1 1 d . . . H9 H 0.6937 0.5699 -0.0391 0.027 Uiso 1 1 calc R . . C10 C 0.61341(17) 0.50018(12) -0.04410(12) 0.0245(4) Uani 1 1 d . . . H10 H 0.5509 0.5316 -0.0464 0.029 Uiso 1 1 calc R . . C11 C 0.61990(16) 0.43150(12) -0.04477(12) 0.0235(4) Uani 1 1 d . . . H11 H 0.5616 0.4157 -0.0464 0.028 Uiso 1 1 calc R . . C12 C 0.71142(15) 0.38558(11) -0.04301(10) 0.0187(4) Uani 1 1 d . . . H12 H 0.7157 0.3387 -0.0439 0.022 Uiso 1 1 calc R . . C21 C 0.98924(14) 0.35553(11) 0.02262(10) 0.0168(4) Uani 1 1 d . . . C22 C 0.95430(14) 0.35308(11) 0.08604(10) 0.0170(4) Uani 1 1 d . . . C23 C 1.02087(15) 0.34648(11) 0.13628(10) 0.0185(4) Uani 1 1 d . . . C24 C 0.98965(16) 0.34005(12) 0.20207(11) 0.0211(4) Uani 1 1 d . . . H24 H 0.9216 0.3444 0.2130 0.025 Uiso 1 1 calc R . . C25 C 1.05597(17) 0.32765(13) 0.25032(11) 0.0241(4) Uani 1 1 d . . . H25 H 1.0337 0.3220 0.2943 0.029 Uiso 1 1 calc R . . C26 C 1.15692(17) 0.32320(13) 0.23494(12) 0.0265(5) Uani 1 1 d . . . H26 H 1.2023 0.3155 0.2684 0.032 Uiso 1 1 calc R . . C27 C 1.18951(17) 0.32991(13) 0.17203(12) 0.0259(5) Uani 1 1 d . . . H27 H 1.2576 0.3272 0.1620 0.031 Uiso 1 1 calc R . . C28 C 1.12290(15) 0.34092(12) 0.12118(11) 0.0207(4) Uani 1 1 d . . . C29 C 1.15601(16) 0.34435(12) 0.05634(11) 0.0226(4) Uani 1 1 d . . . H29 H 1.2240 0.3411 0.0457 0.027 Uiso 1 1 calc R . . C30 C 1.09110(15) 0.35229(12) 0.00859(11) 0.0195(4) Uani 1 1 d . . . H30 H 1.1147 0.3557 -0.0349 0.023 Uiso 1 1 calc R . . C31 C 0.81031(15) 0.29667(11) 0.11294(10) 0.0176(4) Uani 1 1 d . . . C32 C 0.84829(14) 0.35490(11) 0.10514(10) 0.0173(4) Uani 1 1 d . . . C33 C 0.78732(15) 0.41760(11) 0.11774(10) 0.0183(4) Uani 1 1 d . . . C34 C 0.82372(17) 0.47826(12) 0.11230(11) 0.0220(4) Uani 1 1 d . . . H34 H 0.8908 0.4777 0.1003 0.026 Uiso 1 1 calc R . . C35 C 0.76282(18) 0.53757(12) 0.12414(11) 0.0248(4) Uani 1 1 d . . . H35 H 0.7883 0.5775 0.1209 0.030 Uiso 1 1 calc R . . C36 C 0.66257(18) 0.53959(13) 0.14113(11) 0.0260(5) Uani 1 1 d . . . H36 H 0.6210 0.5809 0.1491 0.031 Uiso 1 1 calc R . . C37 C 0.62523(17) 0.48252(12) 0.14613(11) 0.0244(4) Uani 1 1 d . . . H37 H 0.5575 0.4846 0.1570 0.029 Uiso 1 1 calc R . . C38 C 0.68646(15) 0.41990(12) 0.13529(10) 0.0202(4) Uani 1 1 d . . . C39 C 0.65008(15) 0.35951(12) 0.14306(11) 0.0212(4) Uani 1 1 d . . . H39 H 0.5831 0.3605 0.1557 0.025 Uiso 1 1 calc R . . C40 C 0.70973(15) 0.29943(12) 0.13266(10) 0.0197(4) Uani 1 1 d . . . H40 H 0.6839 0.2592 0.1386 0.024 Uiso 1 1 calc R . . C41 C 0.99845(15) 0.19171(11) 0.12656(11) 0.0204(4) Uani 1 1 d . . . C42 C 1.00651(18) 0.18370(13) 0.19321(12) 0.0274(5) Uani 1 1 d . . . H42 H 0.9493 0.1959 0.2188 0.033 Uiso 1 1 calc R . . C43 C 1.0977(2) 0.15799(15) 0.22224(14) 0.0367(6) Uani 1 1 d . . . H43 H 1.1033 0.1529 0.2675 0.044 Uiso 1 1 calc R . . C44 C 1.1807(2) 0.13979(17) 0.18432(16) 0.0431(8) Uani 1 1 d . . . H44 H 1.2431 0.1212 0.2042 0.052 Uiso 1 1 calc R . . C45 C 1.17395(18) 0.14825(15) 0.11855(15) 0.0342(6) Uani 1 1 d . . . H45 H 1.2314 0.1363 0.0931 0.041 Uiso 1 1 calc R . . C46 C 1.08289(16) 0.17434(12) 0.08941(12) 0.0233(4) Uani 1 1 d . . . H46 H 1.0781 0.1804 0.0439 0.028 Uiso 1 1 calc R . . C47 C 0.81503(16) 0.15244(11) 0.11874(10) 0.0197(4) Uani 1 1 d . . . C48 C 0.84165(18) 0.09988(13) 0.17410(12) 0.0269(5) Uani 1 1 d . . . H48 H 0.8957 0.0995 0.1987 0.032 Uiso 1 1 calc R . . C49 C 0.7893(2) 0.04755(14) 0.19370(13) 0.0342(6) Uani 1 1 d . . . H49 H 0.8079 0.0116 0.2316 0.041 Uiso 1 1 calc R . . C50 C 0.7104(2) 0.04793(14) 0.15821(14) 0.0319(5) Uani 1 1 d . . . H50 H 0.6750 0.0122 0.1718 0.038 Uiso 1 1 calc R . . C51 C 0.68274(18) 0.10026(13) 0.10289(13) 0.0272(5) Uani 1 1 d . . . H51 H 0.6282 0.1007 0.0787 0.033 Uiso 1 1 calc R . . C52 C 0.73524(16) 0.15197(12) 0.08302(11) 0.0230(4) Uani 1 1 d . . . H52 H 0.7169 0.1875 0.0448 0.028 Uiso 1 1 calc R . . N1 N 0.90626(14) 0.13225(9) -0.02337(9) 0.0189(3) Uani 1 1 d D . . H1A H 0.886(2) 0.1082(13) 0.0140(10) 0.023 Uiso 1 1 d D . . H1B H 0.8649(18) 0.1342(15) -0.0541(12) 0.023 Uiso 1 1 d D . . C61 C 0.92082(15) 0.24083(11) -0.12461(10) 0.0173(4) Uani 1 1 d . . . C62 C 0.86425(16) 0.29109(12) -0.17251(11) 0.0212(4) Uani 1 1 d . . . H62 H 0.8141 0.3263 -0.1603 0.025 Uiso 1 1 calc R . . C63 C 0.87934(19) 0.29102(13) -0.23783(12) 0.0274(5) Uani 1 1 d . . . H63 H 0.8398 0.3259 -0.2697 0.033 Uiso 1 1 calc R . . C64 C 0.9525(2) 0.23980(15) -0.25646(12) 0.0306(5) Uani 1 1 d . . . H64 H 0.9641 0.2401 -0.3011 0.037 Uiso 1 1 calc R . . C65 C 1.00804(18) 0.18834(13) -0.20946(11) 0.0261(5) Uani 1 1 d . . . H65 H 1.0574 0.1530 -0.2222 0.031 Uiso 1 1 calc R . . C66 C 0.99282(15) 0.18742(11) -0.14346(10) 0.0190(4) Uani 1 1 d . . . C67 C 1.05209(16) 0.13082(11) -0.09418(11) 0.0208(4) Uani 1 1 d . . . C68 C 1.00852(16) 0.10322(11) -0.03526(11) 0.0204(4) Uani 1 1 d . . . C69 C 1.06271(19) 0.05183(12) 0.01286(13) 0.0274(5) Uani 1 1 d . . . H69 H 1.0316 0.0341 0.0528 0.033 Uiso 1 1 calc R . . C70 C 1.1629(2) 0.02637(13) 0.00236(15) 0.0341(6) Uani 1 1 d . . . H70 H 1.2006 -0.0086 0.0351 0.041 Uiso 1 1 calc R . . C71 C 1.20647(19) 0.05231(14) -0.05579(16) 0.0345(6) Uani 1 1 d . . . H71 H 1.2746 0.0349 -0.0632 0.041 Uiso 1 1 calc R . . C72 C 1.15229(18) 0.10349(13) -0.10382(14) 0.0286(5) Uani 1 1 d . . . H72 H 1.1837 0.1203 -0.1439 0.034 Uiso 1 1 calc R . . S1 S 0.65234(4) 0.18425(3) -0.08948(3) 0.01842(9) Uani 1 1 d . . . O1 O 0.67153(13) 0.24180(9) -0.06780(9) 0.0256(3) Uani 1 1 d . . . O2 O 0.74164(12) 0.13157(9) -0.09577(8) 0.0249(3) Uani 1 1 d . . . O3 O 0.57519(12) 0.15409(9) -0.05121(8) 0.0255(3) Uani 1 1 d . . . C81 C 0.60666(19) 0.21938(13) -0.16885(12) 0.0281(5) Uani 1 1 d . . . H81A H 0.5476 0.2563 -0.1681 0.042 Uiso 1 1 calc R . . H81B H 0.5900 0.1828 -0.1852 0.042 Uiso 1 1 calc R . . H81C H 0.6571 0.2385 -0.1973 0.042 Uiso 1 1 calc R . . Pd2 Pd 0.413781(11) 0.241205(9) 0.471214(8) 0.01794(4) Uani 1 1 d . . . P3 P 0.50732(4) 0.25385(3) 0.37351(3) 0.01646(9) Uani 1 1 d . . . P4 P 0.41053(4) 0.35010(3) 0.47895(3) 0.01766(10) Uani 1 1 d . . . C101 C 0.64020(15) 0.23353(11) 0.37798(11) 0.0207(4) Uani 1 1 d . . . C102 C 0.69831(18) 0.25475(13) 0.32394(13) 0.0284(5) Uani 1 1 d . . . H102 H 0.6684 0.2816 0.2843 0.034 Uiso 1 1 calc R . . C103 C 0.80026(19) 0.23655(16) 0.32831(17) 0.0393(7) Uani 1 1 d . . . H103 H 0.8400 0.2516 0.2917 0.047 Uiso 1 1 calc R . . C104 C 0.8442(2) 0.19668(19) 0.3857(2) 0.0496(9) Uani 1 1 d . . . H104 H 0.9139 0.1841 0.3884 0.060 Uiso 1 1 calc R . . C105 C 0.7870(2) 0.17550(19) 0.43833(18) 0.0477(8) Uani 1 1 d . . . H105 H 0.8175 0.1478 0.4775 0.057 Uiso 1 1 calc R . . C106 C 0.68450(19) 0.19369(14) 0.43567(13) 0.0310(5) Uani 1 1 d . . . H106 H 0.6454 0.1791 0.4728 0.037 Uiso 1 1 calc R . . C107 C 0.48080(16) 0.19595(11) 0.32844(10) 0.0195(4) Uani 1 1 d . . . C108 C 0.55238(18) 0.15502(14) 0.29635(13) 0.0286(5) Uani 1 1 d . . . H108 H 0.6194 0.1576 0.2959 0.034 Uiso 1 1 calc R . . C109 C 0.5250(2) 0.11048(17) 0.26507(16) 0.0397(7) Uani 1 1 d . . . H109 H 0.5737 0.0824 0.2435 0.048 Uiso 1 1 calc R . . C110 C 0.4275(2) 0.10655(16) 0.26502(15) 0.0378(6) Uani 1 1 d . . . H110 H 0.4096 0.0761 0.2432 0.045 Uiso 1 1 calc R . . C111 C 0.35611(19) 0.14682(14) 0.29667(13) 0.0290(5) Uani 1 1 d . . . H111 H 0.2891 0.1443 0.2964 0.035 Uiso 1 1 calc R . . C112 C 0.38246(16) 0.19087(12) 0.32880(11) 0.0218(4) Uani 1 1 d . . . H112 H 0.3335 0.2178 0.3512 0.026 Uiso 1 1 calc R . . C121 C 0.47265(15) 0.34045(11) 0.31991(10) 0.0180(4) Uani 1 1 d . . . C122 C 0.49545(15) 0.39720(11) 0.33463(10) 0.0178(4) Uani 1 1 d . . . C123 C 0.45675(15) 0.46565(11) 0.29599(10) 0.0189(4) Uani 1 1 d . . . C124 C 0.47987(16) 0.52597(12) 0.30670(11) 0.0224(4) Uani 1 1 d . . . H124 H 0.5230 0.5216 0.3406 0.027 Uiso 1 1 calc R . . C125 C 0.44074(17) 0.59042(12) 0.26879(13) 0.0263(5) Uani 1 1 d . . . H125 H 0.4575 0.6301 0.2764 0.032 Uiso 1 1 calc R . . C126 C 0.37581(18) 0.59849(13) 0.21856(13) 0.0279(5) Uani 1 1 d . . . H126 H 0.3497 0.6433 0.1922 0.034 Uiso 1 1 calc R . . C127 C 0.35057(17) 0.54169(13) 0.20792(12) 0.0249(4) Uani 1 1 d . . . H127 H 0.3050 0.5475 0.1750 0.030 Uiso 1 1 calc R . . C128 C 0.39124(15) 0.47429(12) 0.24517(10) 0.0199(4) Uani 1 1 d . . . C129 C 0.37043(16) 0.41514(12) 0.23131(11) 0.0219(4) Uani 1 1 d . . . H129 H 0.3278 0.4207 0.1968 0.026 Uiso 1 1 calc R . . C130 C 0.41067(16) 0.35025(12) 0.26680(11) 0.0209(4) Uani 1 1 d . . . H130 H 0.3972 0.3110 0.2560 0.025 Uiso 1 1 calc R . . C131 C 0.52952(15) 0.37304(11) 0.45442(10) 0.0176(4) Uani 1 1 d . . . C132 C 0.56111(15) 0.38900(11) 0.38996(10) 0.0170(4) Uani 1 1 d . . . C133 C 0.66025(15) 0.39812(11) 0.37502(10) 0.0183(4) Uani 1 1 d . . . C134 C 0.69653(16) 0.41601(12) 0.31044(11) 0.0210(4) Uani 1 1 d . . . H134 H 0.6539 0.4236 0.2754 0.025 Uiso 1 1 calc R . . C135 C 0.79165(17) 0.42260(12) 0.29748(12) 0.0234(4) Uani 1 1 d . . . H135 H 0.8140 0.4354 0.2538 0.028 Uiso 1 1 calc R . . C136 C 0.85692(17) 0.41044(12) 0.34870(12) 0.0253(4) Uani 1 1 d . . . H136 H 0.9234 0.4138 0.3394 0.030 Uiso 1 1 calc R . . C137 C 0.82435(16) 0.39392(12) 0.41154(12) 0.0230(4) Uani 1 1 d . . . H137 H 0.8684 0.3862 0.4458 0.028 Uiso 1 1 calc R . . C138 C 0.72542(15) 0.38804(11) 0.42639(11) 0.0195(4) Uani 1 1 d . . . C139 C 0.69006(16) 0.37309(12) 0.49097(11) 0.0216(4) Uani 1 1 d . . . H139 H 0.7327 0.3674 0.5255 0.026 Uiso 1 1 calc R . . C140 C 0.59471(16) 0.36671(12) 0.50453(10) 0.0212(4) Uani 1 1 d . . . H140 H 0.5718 0.3579 0.5484 0.025 Uiso 1 1 calc R . . C141 C 0.38793(16) 0.36174(12) 0.56139(11) 0.0207(4) Uani 1 1 d . . . C142 C 0.43370(16) 0.30798(12) 0.61224(11) 0.0220(4) Uani 1 1 d . . . H142 H 0.4797 0.2692 0.6026 0.026 Uiso 1 1 calc R . . C143 C 0.41277(18) 0.31068(14) 0.67622(11) 0.0260(5) Uani 1 1 d . . . H143 H 0.4441 0.2739 0.7103 0.031 Uiso 1 1 calc R . . C144 C 0.34547(19) 0.36753(14) 0.69054(12) 0.0281(5) Uani 1 1 d . . . H144 H 0.3304 0.3693 0.7345 0.034 Uiso 1 1 calc R . . C145 C 0.30081(19) 0.42116(14) 0.64106(12) 0.0281(5) Uani 1 1 d . . . H145 H 0.2557 0.4602 0.6510 0.034 Uiso 1 1 calc R . . C146 C 0.32146(17) 0.41851(12) 0.57630(12) 0.0238(4) Uani 1 1 d . . . H146 H 0.2901 0.4555 0.5424 0.029 Uiso 1 1 calc R . . C147 C 0.31764(15) 0.41639(12) 0.42981(11) 0.0199(4) Uani 1 1 d . . . C148 C 0.31606(17) 0.48694(12) 0.41882(11) 0.0235(4) Uani 1 1 d . . . H148 H 0.3646 0.5014 0.4375 0.028 Uiso 1 1 calc R . . C149 C 0.24369(18) 0.53599(13) 0.38070(12) 0.0278(5) Uani 1 1 d . . . H149 H 0.2427 0.5840 0.3735 0.033 Uiso 1 1 calc R . . C150 C 0.17273(19) 0.51511(15) 0.35302(14) 0.0335(6) Uani 1 1 d . . . H150 H 0.1235 0.5487 0.3267 0.040 Uiso 1 1 calc R . . C151 C 0.17415(18) 0.44507(15) 0.36404(13) 0.0319(5) Uani 1 1 d . . . H151 H 0.1255 0.4309 0.3452 0.038 Uiso 1 1 calc R . . C152 C 0.24585(17) 0.39529(13) 0.40239(12) 0.0256(4) Uani 1 1 d . . . H152 H 0.2461 0.3474 0.4099 0.031 Uiso 1 1 calc R . . N2 N 0.41696(15) 0.13506(11) 0.47869(10) 0.0230(4) Uani 1 1 d D . . H2A H 0.441(2) 0.1186(15) 0.4441(11) 0.028 Uiso 1 1 d D . . H2B H 0.3558(14) 0.1304(16) 0.4883(15) 0.028 Uiso 1 1 d D . . C161 C 0.33401(19) 0.22150(14) 0.55620(12) 0.0288(5) Uani 1 1 d . . . C162 C 0.2444(2) 0.26336(18) 0.56938(15) 0.0382(7) Uani 1 1 d . . . H162 H 0.2143 0.3020 0.5365 0.046 Uiso 1 1 calc R . . C163 C 0.1982(3) 0.2495(2) 0.63006(17) 0.0534(10) Uani 1 1 d . . . H163 H 0.1372 0.2786 0.6385 0.064 Uiso 1 1 calc R . . C164 C 0.2413(3) 0.1932(2) 0.67790(17) 0.0642(12) Uani 1 1 d . . . H164 H 0.2113 0.1847 0.7199 0.077 Uiso 1 1 calc R . . C165 C 0.3285(3) 0.1488(2) 0.66490(15) 0.0538(10) Uani 1 1 d . . . H165 H 0.3565 0.1093 0.6977 0.065 Uiso 1 1 calc R . . C166 C 0.3755(2) 0.16178(16) 0.60387(12) 0.0361(6) Uani 1 1 d . . . C167 C 0.4666(2) 0.11298(15) 0.59109(13) 0.0348(6) Uani 1 1 d . . . C168 C 0.48513(19) 0.09791(13) 0.52974(12) 0.0272(5) Uani 1 1 d . . . C169 C 0.5691(2) 0.05143(14) 0.51665(15) 0.0345(6) Uani 1 1 d . . . H169 H 0.5792 0.0418 0.4749 0.041 Uiso 1 1 calc R . . C170 C 0.6387(3) 0.01878(16) 0.56438(19) 0.0499(9) Uani 1 1 d . . . H170 H 0.6962 -0.0135 0.5556 0.060 Uiso 1 1 calc R . . C171 C 0.6234(3) 0.03369(18) 0.62448(19) 0.0583(11) Uani 1 1 d . . . H171 H 0.6712 0.0122 0.6571 0.070 Uiso 1 1 calc R . . C172 C 0.5388(3) 0.07983(18) 0.63776(16) 0.0493(9) Uani 1 1 d . . . H172 H 0.5295 0.0892 0.6796 0.059 Uiso 1 1 calc R . . S2 S 0.14372(4) 0.19469(3) 0.42517(3) 0.02506(11) Uani 1 1 d . . . O4 O 0.09801(15) 0.17642(12) 0.37535(10) 0.0390(5) Uani 1 1 d . . . O5 O 0.18023(15) 0.25737(11) 0.40184(11) 0.0375(4) Uani 1 1 d . . . O6 O 0.21722(13) 0.13666(10) 0.46116(10) 0.0325(4) Uani 1 1 d . . . C181 C 0.0489(2) 0.21356(19) 0.48236(15) 0.0423(7) Uani 1 1 d . . . H18A H -0.0040 0.2515 0.4608 0.063 Uiso 1 1 calc R . . H18B H 0.0755 0.2275 0.5170 0.063 Uiso 1 1 calc R . . H18C H 0.0227 0.1722 0.5010 0.063 Uiso 1 1 calc R . . C1S C 0.4111(2) -0.01169(14) 0.10034(13) 0.0330(5) Uani 1 1 d DU . . H1S1 H 0.4103 -0.0457 0.0746 0.040 Uiso 1 1 calc R . . H1S2 H 0.3439 0.0018 0.1185 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.44485(6) 0.06228(4) 0.04961(4) 0.04245(16) Uani 1 1 d DU . . Cl2 Cl 0.49542(6) -0.05044(4) 0.16472(4) 0.04085(15) Uani 1 1 d DU . . C2S C 0.35081(18) 0.18338(15) 0.90989(13) 0.0331(5) Uani 1 1 d DU . . H2S1 H 0.3517 0.1333 0.9185 0.040 Uiso 1 1 calc R . . H2S2 H 0.4161 0.1878 0.9210 0.040 Uiso 1 1 calc R . . Cl3 Cl 0.32987(6) 0.22210(6) 0.82652(4) 0.0574(2) Uani 1 1 d DU . . Cl4 Cl 0.25974(5) 0.22216(4) 0.95950(4) 0.04194(16) Uani 1 1 d DU . . C3S C 0.8433(2) 0.09388(16) 0.77587(15) 0.0363(6) Uani 1 1 d DU . . H3S1 H 0.8684 0.1221 0.7359 0.044 Uiso 1 1 calc R . . H3S2 H 0.8238 0.1233 0.8073 0.044 Uiso 1 1 calc R . . Cl5 Cl 0.93736(7) 0.02289(5) 0.80863(4) 0.05135(19) Uani 1 1 d DU . . Cl6 Cl 0.73891(6) 0.06855(5) 0.75706(4) 0.04747(18) Uani 1 1 d DU . . C4S C 0.7340(6) 0.2110(7) 0.6077(6) 0.0356(18) Uani 0.554(10) 1 d PDU A 1 H4S1 H 0.6940 0.2255 0.5682 0.043 Uiso 0.554(10) 1 calc PR A 1 H4S2 H 0.7317 0.1624 0.6293 0.043 Uiso 0.554(10) 1 calc PR A 1 Cl7 Cl 0.68645(16) 0.26503(17) 0.66025(10) 0.0319(5) Uani 0.554(10) 1 d PDU A 1 Cl8 Cl 0.85644(13) 0.2167(3) 0.58668(15) 0.0565(10) Uani 0.554(10) 1 d PDU A 1 C4T C 0.7287(9) 0.2026(13) 0.6059(11) 0.053(4) Uani 0.446(10) 1 d PDU A 2 H4T1 H 0.7065 0.2295 0.5619 0.063 Uiso 0.446(10) 1 calc PR A 2 H4T2 H 0.6955 0.1633 0.6188 0.063 Uiso 0.446(10) 1 calc PR A 2 Cl7A Cl 0.6953(5) 0.2548(4) 0.6595(3) 0.095(2) Uani 0.446(10) 1 d PDU A 2 Cl8A Cl 0.8563(2) 0.1701(6) 0.60349(19) 0.088(2) Uani 0.446(10) 1 d PDU A 2 C5S C 0.5069(7) 0.2648(5) 0.0375(3) 0.0320(19) Uani 0.51(2) 1 d PDU B 1 H5S1 H 0.5733 0.2750 0.0310 0.038 Uiso 0.51(2) 1 calc PR B 1 H5S2 H 0.5124 0.2175 0.0316 0.038 Uiso 0.51(2) 1 calc PR B 1 Cl9 Cl 0.4639(5) 0.2681(5) 0.1162(3) 0.0548(12) Uani 0.51(2) 1 d PDU B 1 Cl10 Cl 0.4277(3) 0.32445(18) -0.0197(2) 0.0327(11) Uani 0.51(2) 1 d PDU B 1 C5T C 0.4721(12) 0.2497(5) 0.0394(4) 0.044(2) Uani 0.49(2) 1 d PDU B 2 H5T1 H 0.4415 0.2121 0.0350 0.052 Uiso 0.49(2) 1 calc PR B 2 H5T2 H 0.5438 0.2348 0.0314 0.052 Uiso 0.49(2) 1 calc PR B 2 Cl9A Cl 0.4547(7) 0.2571(6) 0.1169(3) 0.0658(16) Uani 0.49(2) 1 d PDU B 2 Cl11 Cl 0.4259(4) 0.3243(3) -0.0225(3) 0.0426(14) Uani 0.49(2) 1 d PDU B 2 C6S C 0.1743(4) 0.0696(3) 0.6016(2) 0.0451(12) Uani 0.675(7) 1 d PDU C 1 H6S1 H 0.2055 0.1099 0.5890 0.054 Uiso 0.675(7) 1 calc PR C 1 H6S2 H 0.1424 0.0669 0.5627 0.054 Uiso 0.675(7) 1 calc PR C 1 Cl12 Cl 0.2671(3) -0.0065(2) 0.6259(2) 0.0943(13) Uani 0.675(7) 1 d PDU C 1 Cl13 Cl 0.08423(10) 0.08377(10) 0.66075(8) 0.0504(5) Uani 0.675(7) 1 d PDU C 1 C6T C 0.1709(7) 0.0228(11) 0.5882(6) 0.082(4) Uani 0.325(7) 1 d PDU C 2 H6T1 H 0.1593 -0.0133 0.5680 0.098 Uiso 0.325(7) 1 calc PR C 2 H6T2 H 0.1711 0.0655 0.5538 0.098 Uiso 0.325(7) 1 calc PR C 2 Cl14 Cl 0.2816(4) -0.0053(3) 0.6271(3) 0.0469(12) Uani 0.325(7) 1 d PDU C 2 Cl15 Cl 0.0800(4) 0.0390(8) 0.6455(3) 0.151(5) Uani 0.325(7) 1 d PDU C 2 C7S C 0.9678(7) -0.0308(4) 0.5946(5) 0.066(2) Uani 0.384(2) 1 d PDU D -1 H7S1 H 0.9524 -0.0758 0.5949 0.080 Uiso 0.384(2) 1 calc PR D -1 H7S2 H 1.0238 -0.0406 0.6238 0.080 Uiso 0.384(2) 1 calc PR D -1 Cl16 Cl 0.8697(2) 0.0184(2) 0.6243(3) 0.0898(13) Uani 0.384(2) 1 d PDU D -1 Cl17 Cl 1.0033(3) 0.0064(2) 0.51697(18) 0.0920(12) Uani 0.384(2) 1 d PDU D -1 C7T C 0.9127(14) -0.0335(9) 0.638(2) 0.066(2) Uani 0.116(2) 1 d PDU A -2 H7T1 H 0.8974 -0.0604 0.6088 0.080 Uiso 0.116(2) 1 calc PR D -2 H7T2 H 0.8701 -0.0410 0.6772 0.080 Uiso 0.116(2) 1 calc PR D -2 Cl18 Cl 0.8855(7) 0.0525(5) 0.5995(5) 0.063(3) Uani 0.116(2) 1 d PDU A -2 Cl19 Cl 1.0351(5) -0.0647(3) 0.6601(3) 0.0401(16) Uani 0.116(2) 1 d PDU A -2 C8S C 0.0278(14) 0.4870(7) 0.5126(8) 0.086(3) Uani 0.3516(18) 1 d PDU E -1 H8S1 H 0.0940 0.4875 0.4925 0.103 Uiso 0.3516(18) 1 calc PR E -1 H8S2 H 0.0230 0.5061 0.5515 0.103 Uiso 0.3516(18) 1 calc PR E -1 Cl20 Cl 0.0122(3) 0.4009(3) 0.5360(2) 0.0804(12) Uani 0.3516(18) 1 d PDU E -1 Cl21 Cl -0.0638(3) 0.5399(3) 0.4563(3) 0.0916(13) Uani 0.3516(18) 1 d PDU E -1 C8T C 0.045(4) 0.526(2) 0.493(4) 0.086(3) Uani 0.071(3) 1 d PDU F -2 H8T1 H 0.0504 0.5444 0.5311 0.103 Uiso 0.071(3) 1 calc PR F -2 H8T2 H 0.1116 0.5169 0.4727 0.103 Uiso 0.071(3) 1 calc PR F -2 Cl22 Cl 0.010(3) 0.4465(14) 0.5211(13) 0.108(6) Uani 0.071(3) 1 d PDU F -2 Cl23 Cl -0.0334(15) 0.5889(13) 0.4378(12) 0.094(6) Uani 0.071(3) 1 d PDU F -2 C8U C -0.037(3) 0.6103(16) 0.485(3) 0.086(3) Uani 0.077(3) 1 d PDU G -3 H8U1 H -0.0991 0.6141 0.4640 0.103 Uiso 0.077(3) 1 calc PR G -3 H8U2 H -0.0531 0.6309 0.5232 0.103 Uiso 0.077(3) 1 calc PR G -3 Cl24 Cl 0.022(2) 0.5229(13) 0.5112(15) 0.112(7) Uani 0.077(3) 1 d PDU G -3 Cl25 Cl 0.0380(14) 0.6558(10) 0.4309(7) 0.096(5) Uani 0.077(3) 1 d PDU G -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 0.01312(6) 0.01571(7) 0.01432(7) -0.00358(5) -0.00056(5) -0.00300(5) P1 0.0128(2) 0.0163(2) 0.0157(2) -0.00389(18) -0.00030(17) -0.00298(17) P2 0.0133(2) 0.0196(2) 0.0154(2) -0.00391(19) -0.00087(17) -0.00260(18) C1 0.0161(8) 0.0216(9) 0.0158(9) -0.0047(7) -0.0005(7) -0.0067(7) C2 0.0216(10) 0.0221(10) 0.0202(10) -0.0026(8) 0.0010(8) -0.0048(8) C3 0.0287(11) 0.0263(11) 0.0216(10) 0.0018(9) -0.0009(9) -0.0092(9) C4 0.0273(11) 0.0370(13) 0.0187(10) -0.0045(9) 0.0036(8) -0.0140(10) C5 0.0178(9) 0.0317(12) 0.0222(10) -0.0082(9) 0.0029(8) -0.0079(8) C6 0.0164(9) 0.0234(10) 0.0200(9) -0.0058(8) -0.0004(7) -0.0062(7) C7 0.0132(8) 0.0185(9) 0.0162(9) -0.0038(7) 0.0004(7) -0.0023(7) C8 0.0193(9) 0.0197(9) 0.0211(10) -0.0059(8) -0.0002(7) -0.0050(7) C9 0.0230(10) 0.0195(10) 0.0249(11) -0.0061(8) 0.0026(8) -0.0027(8) C10 0.0187(10) 0.0252(11) 0.0256(11) -0.0050(9) 0.0015(8) 0.0008(8) C11 0.0150(9) 0.0267(11) 0.0274(11) -0.0050(9) 0.0005(8) -0.0039(8) C12 0.0162(9) 0.0204(9) 0.0197(9) -0.0040(8) 0.0005(7) -0.0052(7) C21 0.0133(8) 0.0181(9) 0.0199(9) -0.0062(7) 0.0003(7) -0.0037(7) C22 0.0129(8) 0.0193(9) 0.0198(9) -0.0068(7) -0.0005(7) -0.0032(7) C23 0.0146(8) 0.0223(10) 0.0203(9) -0.0085(8) -0.0002(7) -0.0040(7) C24 0.0179(9) 0.0260(10) 0.0204(10) -0.0094(8) -0.0006(7) -0.0024(8) C25 0.0224(10) 0.0289(11) 0.0217(10) -0.0110(9) -0.0038(8) -0.0011(8) C26 0.0219(10) 0.0329(12) 0.0267(11) -0.0126(10) -0.0072(8) -0.0023(9) C27 0.0166(9) 0.0354(12) 0.0298(12) -0.0150(10) -0.0044(8) -0.0045(9) C28 0.0149(9) 0.0260(10) 0.0242(10) -0.0105(8) -0.0028(7) -0.0050(8) C29 0.0138(9) 0.0310(11) 0.0269(11) -0.0117(9) 0.0013(8) -0.0079(8) C30 0.0152(9) 0.0259(10) 0.0202(9) -0.0085(8) 0.0023(7) -0.0077(8) C31 0.0148(8) 0.0227(10) 0.0141(8) -0.0045(7) -0.0008(7) -0.0015(7) C32 0.0133(8) 0.0233(10) 0.0147(8) -0.0057(7) -0.0001(7) -0.0021(7) C33 0.0161(9) 0.0235(10) 0.0146(9) -0.0055(7) -0.0003(7) -0.0021(7) C34 0.0212(10) 0.0253(10) 0.0197(10) -0.0077(8) -0.0003(8) -0.0034(8) C35 0.0280(11) 0.0244(11) 0.0214(10) -0.0077(9) 0.0000(8) -0.0026(9) C36 0.0257(11) 0.0263(11) 0.0224(10) -0.0078(9) 0.0018(8) 0.0026(9) C37 0.0194(10) 0.0281(11) 0.0208(10) -0.0054(9) 0.0002(8) 0.0031(8) C38 0.0160(9) 0.0261(10) 0.0162(9) -0.0057(8) -0.0007(7) 0.0002(8) C39 0.0136(8) 0.0285(11) 0.0192(9) -0.0047(8) 0.0012(7) -0.0016(8) C40 0.0161(9) 0.0247(10) 0.0181(9) -0.0047(8) 0.0005(7) -0.0052(8) C41 0.0171(9) 0.0226(10) 0.0217(10) -0.0082(8) -0.0044(7) -0.0006(7) C42 0.0269(11) 0.0306(12) 0.0235(11) -0.0111(9) -0.0057(9) 0.0021(9) C43 0.0371(14) 0.0419(15) 0.0303(13) -0.0180(12) -0.0164(11) 0.0080(11) C44 0.0277(13) 0.0535(18) 0.0496(17) -0.0278(15) -0.0206(12) 0.0110(12) C45 0.0177(10) 0.0433(15) 0.0452(15) -0.0243(13) -0.0081(10) 0.0033(10) C46 0.0168(9) 0.0279(11) 0.0270(11) -0.0120(9) -0.0035(8) -0.0018(8) C47 0.0187(9) 0.0211(9) 0.0183(9) -0.0040(8) 0.0018(7) -0.0038(7) C48 0.0277(11) 0.0274(11) 0.0220(11) -0.0007(9) -0.0017(9) -0.0046(9) C49 0.0409(14) 0.0283(12) 0.0276(12) 0.0022(10) 0.0040(11) -0.0075(11) C50 0.0317(12) 0.0281(12) 0.0362(14) -0.0069(10) 0.0121(10) -0.0120(10) C51 0.0210(10) 0.0291(12) 0.0336(12) -0.0107(10) 0.0054(9) -0.0085(9) C52 0.0200(10) 0.0249(10) 0.0235(10) -0.0043(8) 0.0002(8) -0.0057(8) N1 0.0206(8) 0.0174(8) 0.0183(8) -0.0023(7) 0.0000(6) -0.0062(7) C61 0.0159(8) 0.0192(9) 0.0180(9) -0.0051(7) -0.0010(7) -0.0056(7) C62 0.0200(9) 0.0224(10) 0.0210(10) -0.0027(8) -0.0032(8) -0.0063(8) C63 0.0314(12) 0.0312(12) 0.0198(10) -0.0003(9) -0.0071(9) -0.0114(10) C64 0.0366(13) 0.0425(14) 0.0175(10) -0.0080(10) 0.0031(9) -0.0186(11) C65 0.0271(11) 0.0338(12) 0.0217(10) -0.0125(9) 0.0055(8) -0.0109(9) C66 0.0182(9) 0.0219(10) 0.0189(9) -0.0068(8) 0.0009(7) -0.0066(7) C67 0.0181(9) 0.0194(9) 0.0271(11) -0.0104(8) -0.0033(8) -0.0025(7) C68 0.0196(9) 0.0163(9) 0.0272(11) -0.0076(8) -0.0058(8) -0.0032(7) C69 0.0328(12) 0.0182(10) 0.0329(12) -0.0047(9) -0.0135(10) -0.0062(9) C70 0.0324(13) 0.0194(11) 0.0515(17) -0.0093(11) -0.0211(12) -0.0004(9) C71 0.0214(11) 0.0272(12) 0.0574(18) -0.0185(12) -0.0102(11) 0.0018(9) C72 0.0209(10) 0.0281(12) 0.0397(14) -0.0165(10) -0.0011(9) -0.0023(9) S1 0.0173(2) 0.0183(2) 0.0198(2) -0.00319(18) -0.00266(17) -0.00505(18) O1 0.0266(8) 0.0241(8) 0.0299(9) -0.0110(7) -0.0001(7) -0.0084(6) O2 0.0207(7) 0.0235(8) 0.0296(9) -0.0075(7) -0.0026(6) -0.0012(6) O3 0.0222(8) 0.0271(8) 0.0277(8) -0.0034(7) 0.0014(6) -0.0107(6) C81 0.0337(12) 0.0261(11) 0.0237(11) -0.0007(9) -0.0069(9) -0.0085(9) Pd2 0.01666(7) 0.02241(8) 0.01664(7) -0.00686(6) 0.00196(5) -0.00646(6) P3 0.0137(2) 0.0200(2) 0.0158(2) -0.00529(19) -0.00018(17) -0.00302(18) P4 0.0143(2) 0.0221(2) 0.0177(2) -0.0071(2) 0.00092(18) -0.00441(19) C101 0.0151(9) 0.0213(10) 0.0269(11) -0.0081(8) -0.0006(8) -0.0037(7) C102 0.0220(11) 0.0277(11) 0.0353(13) -0.0103(10) 0.0073(9) -0.0052(9) C103 0.0208(11) 0.0398(15) 0.064(2) -0.0253(14) 0.0160(12) -0.0116(10) C104 0.0161(11) 0.061(2) 0.081(3) -0.0368(19) -0.0051(13) -0.0044(12) C105 0.0266(13) 0.062(2) 0.0521(19) -0.0171(16) -0.0185(13) 0.0038(13) C106 0.0240(11) 0.0353(13) 0.0327(13) -0.0070(11) -0.0091(9) -0.0030(10) C107 0.0190(9) 0.0223(10) 0.0167(9) -0.0051(8) -0.0019(7) -0.0028(8) C108 0.0215(10) 0.0358(13) 0.0317(12) -0.0176(10) 0.0022(9) -0.0033(9) C109 0.0318(13) 0.0492(17) 0.0471(17) -0.0339(14) 0.0043(12) -0.0047(12) C110 0.0358(14) 0.0457(16) 0.0409(15) -0.0270(13) -0.0023(11) -0.0085(12) C111 0.0249(11) 0.0362(13) 0.0306(12) -0.0142(10) -0.0047(9) -0.0080(10) C112 0.0193(9) 0.0259(10) 0.0214(10) -0.0082(8) -0.0012(8) -0.0042(8) C121 0.0158(9) 0.0208(9) 0.0162(9) -0.0038(7) 0.0011(7) -0.0030(7) C122 0.0147(8) 0.0240(10) 0.0147(9) -0.0052(7) 0.0001(7) -0.0043(7) C123 0.0162(9) 0.0222(10) 0.0170(9) -0.0031(8) 0.0002(7) -0.0040(7) C124 0.0195(9) 0.0236(10) 0.0243(10) -0.0049(8) -0.0031(8) -0.0053(8) C125 0.0225(10) 0.0224(10) 0.0335(12) -0.0044(9) -0.0038(9) -0.0060(8) C126 0.0227(11) 0.0228(11) 0.0341(13) 0.0015(9) -0.0066(9) -0.0039(8) C127 0.0190(10) 0.0279(11) 0.0250(11) -0.0005(9) -0.0060(8) -0.0042(8) C128 0.0159(9) 0.0244(10) 0.0182(9) -0.0026(8) -0.0014(7) -0.0043(7) C129 0.0195(9) 0.0271(11) 0.0196(10) -0.0042(8) -0.0035(8) -0.0065(8) C130 0.0201(9) 0.0244(10) 0.0192(10) -0.0061(8) -0.0017(7) -0.0056(8) C131 0.0149(8) 0.0210(9) 0.0181(9) -0.0066(7) -0.0004(7) -0.0040(7) C132 0.0152(8) 0.0192(9) 0.0172(9) -0.0051(7) -0.0017(7) -0.0038(7) C133 0.0151(8) 0.0192(9) 0.0205(9) -0.0052(8) -0.0004(7) -0.0034(7) C134 0.0201(9) 0.0228(10) 0.0202(10) -0.0061(8) 0.0013(7) -0.0046(8) C135 0.0229(10) 0.0235(10) 0.0238(10) -0.0068(8) 0.0059(8) -0.0062(8) C136 0.0174(9) 0.0270(11) 0.0324(12) -0.0092(9) 0.0039(8) -0.0058(8) C137 0.0155(9) 0.0264(11) 0.0271(11) -0.0060(9) -0.0011(8) -0.0052(8) C138 0.0152(9) 0.0213(10) 0.0218(10) -0.0043(8) -0.0012(7) -0.0043(7) C139 0.0189(9) 0.0268(11) 0.0202(10) -0.0050(8) -0.0040(7) -0.0069(8) C140 0.0199(9) 0.0283(11) 0.0162(9) -0.0052(8) -0.0008(7) -0.0070(8) C141 0.0186(9) 0.0275(11) 0.0194(9) -0.0096(8) 0.0031(7) -0.0087(8) C142 0.0206(10) 0.0287(11) 0.0199(10) -0.0092(8) 0.0006(8) -0.0084(8) C143 0.0252(11) 0.0355(12) 0.0203(10) -0.0075(9) 0.0015(8) -0.0126(9) C144 0.0301(12) 0.0403(13) 0.0221(11) -0.0164(10) 0.0082(9) -0.0170(10) C145 0.0279(11) 0.0325(12) 0.0284(12) -0.0157(10) 0.0094(9) -0.0097(10) C146 0.0218(10) 0.0268(11) 0.0241(11) -0.0091(9) 0.0041(8) -0.0068(8) C147 0.0146(8) 0.0245(10) 0.0202(10) -0.0069(8) 0.0000(7) -0.0024(7) C148 0.0218(10) 0.0269(11) 0.0224(10) -0.0073(9) -0.0006(8) -0.0052(8) C149 0.0259(11) 0.0272(11) 0.0287(12) -0.0061(9) -0.0025(9) -0.0031(9) C150 0.0254(12) 0.0384(14) 0.0334(13) -0.0066(11) -0.0103(10) 0.0002(10) C151 0.0215(11) 0.0406(14) 0.0349(13) -0.0089(11) -0.0087(9) -0.0067(10) C152 0.0198(10) 0.0312(12) 0.0286(11) -0.0108(9) -0.0027(8) -0.0066(9) N2 0.0234(9) 0.0254(9) 0.0220(9) -0.0069(7) -0.0001(7) -0.0083(7) C161 0.0331(12) 0.0399(13) 0.0226(11) -0.0139(10) 0.0084(9) -0.0222(11) C162 0.0321(13) 0.0575(18) 0.0401(15) -0.0293(14) 0.0167(11) -0.0262(13) C163 0.0517(19) 0.082(3) 0.0482(19) -0.0400(19) 0.0308(16) -0.0421(19) C164 0.082(3) 0.100(3) 0.0363(17) -0.035(2) 0.0360(18) -0.064(3) C165 0.083(3) 0.069(2) 0.0241(14) -0.0131(14) 0.0132(15) -0.048(2) C166 0.0530(17) 0.0454(15) 0.0204(11) -0.0103(11) 0.0067(11) -0.0313(14) C167 0.0528(17) 0.0330(13) 0.0236(12) -0.0004(10) -0.0070(11) -0.0241(12) C168 0.0326(12) 0.0244(11) 0.0273(11) -0.0026(9) -0.0049(9) -0.0144(9) C169 0.0366(14) 0.0253(12) 0.0441(15) -0.0057(11) -0.0120(12) -0.0108(10) C170 0.0484(18) 0.0292(14) 0.072(2) -0.0053(15) -0.0296(17) -0.0064(13) C171 0.076(3) 0.0380(17) 0.059(2) 0.0067(15) -0.043(2) -0.0160(17) C172 0.079(2) 0.0425(17) 0.0311(15) 0.0036(13) -0.0210(15) -0.0288(17) S2 0.0187(2) 0.0332(3) 0.0260(3) -0.0105(2) -0.0004(2) -0.0077(2) O4 0.0362(10) 0.0530(13) 0.0353(10) -0.0186(9) -0.0085(8) -0.0133(9) O5 0.0339(10) 0.0356(10) 0.0460(12) -0.0118(9) 0.0041(9) -0.0131(8) O6 0.0225(8) 0.0389(10) 0.0349(10) -0.0071(8) -0.0025(7) -0.0058(7) C181 0.0264(13) 0.063(2) 0.0395(16) -0.0205(15) 0.0091(11) -0.0079(13) C1S 0.0333(13) 0.0338(13) 0.0334(13) -0.0039(10) -0.0009(10) -0.0148(11) Cl1 0.0474(4) 0.0317(3) 0.0472(4) 0.0026(3) -0.0066(3) -0.0179(3) Cl2 0.0399(4) 0.0448(4) 0.0368(3) -0.0021(3) -0.0051(3) -0.0144(3) C2S 0.0210(11) 0.0396(14) 0.0329(13) -0.0021(11) -0.0019(9) -0.0019(10) Cl3 0.0338(4) 0.0781(6) 0.0374(4) 0.0169(4) -0.0011(3) -0.0007(4) Cl4 0.0278(3) 0.0492(4) 0.0520(4) -0.0230(3) -0.0030(3) -0.0025(3) C3S 0.0296(13) 0.0421(15) 0.0378(14) -0.0111(12) -0.0024(11) -0.0073(11) Cl5 0.0489(4) 0.0475(4) 0.0503(5) -0.0041(4) -0.0121(4) -0.0012(3) Cl6 0.0412(4) 0.0606(5) 0.0451(4) -0.0088(4) -0.0040(3) -0.0232(4) C4S 0.032(3) 0.044(4) 0.022(4) -0.004(3) 0.001(3) 0.002(3) Cl7 0.0297(8) 0.0476(10) 0.0144(8) -0.0066(6) -0.0032(5) -0.0012(6) Cl8 0.0299(7) 0.092(2) 0.0437(11) -0.0219(13) 0.0046(6) -0.0018(9) C4T 0.041(4) 0.072(9) 0.050(7) -0.019(6) -0.012(5) -0.011(5) Cl7A 0.121(4) 0.090(3) 0.061(3) -0.025(2) -0.023(2) 0.016(3) Cl8A 0.0475(13) 0.158(7) 0.0432(15) -0.028(3) 0.0030(10) 0.007(2) C5S 0.029(4) 0.034(4) 0.028(2) -0.011(2) 0.000(2) 0.005(3) Cl9 0.0254(11) 0.110(3) 0.0448(18) -0.045(2) 0.0087(10) -0.0218(15) Cl10 0.0176(15) 0.0165(14) 0.058(2) -0.0003(12) 0.0061(13) -0.0030(11) C5T 0.048(6) 0.035(4) 0.048(3) -0.018(3) -0.014(4) 0.003(3) Cl9A 0.042(3) 0.101(3) 0.0382(17) -0.0059(19) 0.0108(15) -0.001(2) Cl11 0.039(3) 0.047(3) 0.0397(19) -0.0127(16) -0.0066(16) -0.0013(18) C6S 0.047(3) 0.060(3) 0.026(2) -0.004(2) 0.0058(17) -0.017(2) Cl12 0.089(2) 0.104(2) 0.0614(18) -0.0189(16) 0.0116(15) 0.0278(16) Cl13 0.0308(6) 0.0683(11) 0.0436(7) -0.0101(6) -0.0018(5) 0.0020(5) C6T 0.049(5) 0.130(12) 0.050(6) 0.012(7) -0.009(4) -0.023(7) Cl14 0.0423(16) 0.067(3) 0.037(2) -0.0042(17) -0.0054(13) -0.0320(19) Cl15 0.054(2) 0.262(12) 0.076(3) 0.009(5) -0.003(2) 0.030(4) C7S 0.059(4) 0.028(3) 0.117(6) -0.021(4) -0.010(4) -0.012(3) Cl16 0.0558(17) 0.081(2) 0.149(4) -0.056(3) -0.0028(19) -0.0151(16) Cl17 0.107(3) 0.100(3) 0.079(2) -0.030(2) -0.026(2) -0.024(2) C7T 0.059(4) 0.028(3) 0.117(6) -0.021(4) -0.010(4) -0.012(3) Cl18 0.047(4) 0.044(4) 0.083(6) 0.015(4) -0.004(4) -0.015(3) Cl19 0.053(3) 0.023(2) 0.044(3) -0.001(2) -0.007(3) -0.013(2) C8S 0.080(7) 0.117(5) 0.086(6) -0.063(5) -0.016(5) -0.024(5) Cl20 0.0492(18) 0.092(2) 0.100(3) -0.047(2) -0.0152(18) 0.0156(17) Cl21 0.0499(19) 0.102(3) 0.118(4) -0.035(2) 0.013(2) -0.0031(19) C8T 0.080(7) 0.117(5) 0.086(6) -0.063(5) -0.016(5) -0.024(5) Cl22 0.127(14) 0.099(8) 0.108(12) -0.069(8) 0.036(11) -0.011(9) Cl23 0.062(9) 0.123(11) 0.114(12) -0.047(8) -0.022(8) -0.031(8) C8U 0.080(7) 0.117(5) 0.086(6) -0.063(5) -0.016(5) -0.024(5) Cl24 0.083(11) 0.127(8) 0.123(13) -0.036(10) 0.006(10) -0.016(9) Cl25 0.086(9) 0.119(10) 0.052(7) -0.017(7) -0.004(6) 0.035(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 C61 2.046(2) . ? Pd1 N1 2.1156(18) . ? Pd1 P1 2.2637(6) . ? Pd1 P2 2.3613(6) . ? P1 C7 1.812(2) . ? P1 C21 1.832(2) . ? P1 C1 1.835(2) . ? P2 C41 1.810(2) . ? P2 C47 1.825(2) . ? P2 C31 1.828(2) . ? C1 C2 1.393(3) . ? C1 C6 1.405(3) . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.397(3) . ? C7 C12 1.399(3) . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C21 C22 1.392(3) . ? C21 C30 1.421(3) . ? C22 C23 1.433(3) . ? C22 C32 1.500(3) . ? C23 C24 1.417(3) . ? C23 C28 1.421(3) . ? C24 C25 1.374(3) . ? C24 H24 0.9500 . ? C25 C26 1.410(3) . ? C25 H25 0.9500 . ? C26 C27 1.364(3) . ? C26 H26 0.9500 . ? C27 C28 1.424(3) . ? C27 H27 0.9500 . ? C28 C29 1.411(3) . ? C29 C30 1.369(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 C40 1.427(3) . ? C32 C33 1.435(3) . ? C33 C38 1.422(3) . ? C33 C34 1.423(3) . ? C34 C35 1.374(3) . ? C34 H34 0.9500 . ? C35 C36 1.413(3) . ? C35 H35 0.9500 . ? C36 C37 1.363(4) . ? C36 H36 0.9500 . ? C37 C38 1.422(3) . ? C37 H37 0.9500 . ? C38 C39 1.410(3) . ? C39 C40 1.369(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.393(3) . ? C41 C42 1.397(3) . ? C42 C43 1.387(3) . ? C42 H42 0.9500 . ? C43 C44 1.392(4) . ? C43 H43 0.9500 . ? C44 C45 1.375(4) . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.387(3) . ? C47 C52 1.402(3) . ? C48 C49 1.397(4) . ? C48 H48 0.9500 . ? C49 C50 1.382(4) . ? C49 H49 0.9500 . ? C50 C51 1.386(4) . ? C50 H50 0.9500 . ? C51 C52 1.388(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? N1 C68 1.441(3) . ? N1 H1A 0.885(17) . ? N1 H1B 0.895(17) . ? C61 C62 1.391(3) . ? C61 C66 1.415(3) . ? C62 C63 1.390(3) . ? C62 H62 0.9500 . ? C63 C64 1.391(4) . ? C63 H63 0.9500 . ? C64 C65 1.384(4) . ? C64 H64 0.9500 . ? C65 C66 1.400(3) . ? C65 H65 0.9500 . ? C66 C67 1.482(3) . ? C67 C68 1.396(3) . ? C67 C72 1.399(3) . ? C68 C69 1.389(3) . ? C69 C70 1.394(4) . ? C69 H69 0.9500 . ? C70 C71 1.374(4) . ? C70 H70 0.9500 . ? C71 C72 1.386(4) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? S1 O1 1.4520(17) . ? S1 O3 1.4593(17) . ? S1 O2 1.4642(17) . ? S1 C81 1.767(2) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? Pd2 C161 2.051(2) . ? Pd2 N2 2.124(2) . ? Pd2 P4 2.2611(6) . ? Pd2 P3 2.3586(6) . ? P3 C101 1.809(2) . ? P3 C107 1.814(2) . ? P3 C121 1.825(2) . ? P4 C147 1.812(2) . ? P4 C141 1.823(2) . ? P4 C131 1.835(2) . ? C101 C106 1.390(3) . ? C101 C102 1.392(3) . ? C102 C103 1.389(4) . ? C102 H102 0.9500 . ? C103 C104 1.383(5) . ? C103 H103 0.9500 . ? C104 C105 1.364(5) . ? C104 H104 0.9500 . ? C105 C106 1.394(4) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C108 1.396(3) . ? C107 C112 1.402(3) . ? C108 C109 1.389(4) . ? C108 H108 0.9500 . ? C109 C110 1.383(4) . ? C109 H109 0.9500 . ? C110 C111 1.382(4) . ? C110 H110 0.9500 . ? C111 C112 1.385(3) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C121 C122 1.385(3) . ? C121 C130 1.424(3) . ? C122 C123 1.434(3) . ? C122 C132 1.502(3) . ? C123 C124 1.420(3) . ? C123 C128 1.423(3) . ? C124 C125 1.370(3) . ? C124 H124 0.9500 . ? C125 C126 1.410(3) . ? C125 H125 0.9500 . ? C126 C127 1.364(3) . ? C126 H126 0.9500 . ? C127 C128 1.414(3) . ? C127 H127 0.9500 . ? C128 C129 1.411(3) . ? C129 C130 1.362(3) . ? C129 H129 0.9500 . ? C130 H130 0.9500 . ? C131 C132 1.390(3) . ? C131 C140 1.419(3) . ? C132 C133 1.442(3) . ? C133 C134 1.416(3) . ? C133 C138 1.422(3) . ? C134 C135 1.367(3) . ? C134 H134 0.9500 . ? C135 C136 1.413(3) . ? C135 H135 0.9500 . ? C136 C137 1.364(3) . ? C136 H136 0.9500 . ? C137 C138 1.420(3) . ? C137 H137 0.9500 . ? C138 C139 1.407(3) . ? C139 C140 1.371(3) . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C141 C146 1.392(3) . ? C141 C142 1.402(3) . ? C142 C143 1.382(3) . ? C142 H142 0.9500 . ? C143 C144 1.394(4) . ? C143 H143 0.9500 . ? C144 C145 1.378(4) . ? C144 H144 0.9500 . ? C145 C146 1.398(3) . ? C145 H145 0.9500 . ? C146 H146 0.9500 . ? C147 C148 1.396(3) . ? C147 C152 1.399(3) . ? C148 C149 1.388(3) . ? C148 H148 0.9500 . ? C149 C150 1.390(4) . ? C149 H149 0.9500 . ? C150 C151 1.386(4) . ? C150 H150 0.9500 . ? C151 C152 1.390(3) . ? C151 H151 0.9500 . ? C152 H152 0.9500 . ? N2 C168 1.439(3) . ? N2 H2A 0.895(17) . ? N2 H2B 0.885(17) . ? C161 C162 1.392(4) . ? C161 C166 1.411(4) . ? C162 C163 1.392(4) . ? C162 H162 0.9500 . ? C163 C164 1.379(6) . ? C163 H163 0.9500 . ? C164 C165 1.391(6) . ? C164 H164 0.9500 . ? C165 C166 1.402(4) . ? C165 H165 0.9500 . ? C166 C167 1.473(5) . ? C167 C172 1.400(4) . ? C167 C168 1.407(4) . ? C168 C169 1.382(4) . ? C169 C170 1.390(4) . ? C169 H169 0.9500 . ? C170 C171 1.378(6) . ? C170 H170 0.9500 . ? C171 C172 1.386(6) . ? C171 H171 0.9500 . ? C172 H172 0.9500 . ? S2 O4 1.4463(19) . ? S2 O5 1.448(2) . ? S2 O6 1.462(2) . ? S2 C181 1.768(3) . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C1S Cl1 1.763(3) . ? C1S Cl2 1.778(3) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S Cl4 1.759(3) . ? C2S Cl3 1.768(3) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S Cl5 1.747(3) . ? C3S Cl6 1.763(3) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S Cl7 1.752(8) . ? C4S Cl8 1.758(9) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C4T Cl7A 1.719(12) . ? C4T Cl8A 1.750(12) . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? Cl8A Cl18 2.361(15) . ? C5S Cl10 1.738(7) . ? C5S Cl9 1.746(7) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C5T Cl9A 1.687(9) . ? C5T Cl11 1.770(10) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6S Cl13 1.736(5) . ? C6S Cl12 1.764(6) . ? C6S H6S1 0.9900 . ? C6S H6S2 0.9900 . ? C6T Cl14 1.718(10) . ? C6T Cl15 1.725(11) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7S Cl16 1.679(9) . ? C7S Cl17 1.725(10) . ? C7S H7S1 0.9900 . ? C7S H7S2 0.9900 . ? C7T Cl18 1.705(14) . ? C7T Cl19 1.737(14) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8S Cl20 1.765(13) . ? C8S Cl21 1.783(12) . ? C8S H8S1 0.9900 . ? C8S H8S2 0.9900 . ? C8T Cl23 1.742(15) . ? C8T Cl22 1.749(15) . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? C8U Cl25 1.738(15) . ? C8U Cl24 1.745(15) . ? C8U H8U1 0.9900 . ? C8U H8U2 0.9900 . ? 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 C61 Pd1 N1 81.26(8) . . ? C61 Pd1 P1 93.15(6) . . ? N1 Pd1 P1 171.72(5) . . ? C61 Pd1 P2 173.85(6) . . ? N1 Pd1 P2 92.68(5) . . ? P1 Pd1 P2 92.761(19) . . ? C7 P1 C21 107.33(9) . . ? C7 P1 C1 105.26(10) . . ? C21 P1 C1 105.00(9) . . ? C7 P1 Pd1 112.77(7) . . ? C21 P1 Pd1 110.46(7) . . ? C1 P1 Pd1 115.40(7) . . ? C41 P2 C47 105.34(10) . . ? C41 P2 C31 108.66(10) . . ? C47 P2 C31 105.25(10) . . ? C41 P2 Pd1 112.19(8) . . ? C47 P2 Pd1 110.09(7) . . ? C31 P2 Pd1 114.69(7) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 P1 123.19(16) . . ? C6 C1 P1 117.97(16) . . ? C1 C2 C3 120.3(2) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 119.62(19) . . ? C8 C7 P1 121.90(15) . . ? C12 C7 P1 118.46(16) . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.1(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.8(2) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C22 C21 C30 119.03(19) . . ? C22 C21 P1 123.15(15) . . ? C30 C21 P1 117.07(15) . . ? C21 C22 C23 120.09(18) . . ? C21 C22 C32 122.38(18) . . ? C23 C22 C32 117.50(18) . . ? C24 C23 C28 118.18(19) . . ? C24 C23 C22 122.07(19) . . ? C28 C23 C22 119.58(19) . . ? C25 C24 C23 121.2(2) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.9(2) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C23 119.05(19) . . ? C29 C28 C27 121.6(2) . . ? C23 C28 C27 119.3(2) . . ? C30 C29 C28 120.65(19) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C21 121.5(2) . . ? C29 C30 H30 119.2 . . ? C21 C30 H30 119.2 . . ? C32 C31 C40 119.73(19) . . ? C32 C31 P2 120.32(15) . . ? C40 C31 P2 119.24(16) . . ? C31 C32 C33 120.18(18) . . ? C31 C32 C22 120.94(18) . . ? C33 C32 C22 118.84(18) . . ? C38 C33 C34 118.54(19) . . ? C38 C33 C32 119.1(2) . . ? C34 C33 C32 122.32(19) . . ? C35 C34 C33 120.6(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.5(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.8(2) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 121.5(2) . . ? C39 C38 C33 119.22(19) . . ? C37 C38 C33 119.3(2) . . ? C40 C39 C38 121.0(2) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C31 120.6(2) . . ? C39 C40 H40 119.7 . . ? C31 C40 H40 119.7 . . ? C46 C41 C42 119.4(2) . . ? C46 C41 P2 117.74(17) . . ? C42 C41 P2 122.82(17) . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.2(2) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 121.0(2) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 119.8(2) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 120.2(2) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C48 C47 C52 119.0(2) . . ? C48 C47 P2 124.19(18) . . ? C52 C47 P2 116.75(17) . . ? C47 C48 C49 120.2(2) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 120.2(2) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 120.2(2) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 119.6(2) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C51 C52 C47 120.8(2) . . ? C51 C52 H52 119.6 . . ? C47 C52 H52 119.6 . . ? C68 N1 Pd1 104.28(13) . . ? C68 N1 H1A 109.5(19) . . ? Pd1 N1 H1A 115.5(19) . . ? C68 N1 H1B 115.6(19) . . ? Pd1 N1 H1B 103.8(18) . . ? H1A N1 H1B 108(3) . . ? C62 C61 C66 118.4(2) . . ? C62 C61 Pd1 123.30(16) . . ? C66 C61 Pd1 118.19(15) . . ? C63 C62 C61 121.6(2) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C62 C63 C64 119.9(2) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C65 C64 C63 119.5(2) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C64 C65 C66 121.2(2) . . ? C64 C65 H65 119.4 . . ? C66 C65 H65 119.4 . . ? C65 C66 C61 119.4(2) . . ? C65 C66 C67 119.9(2) . . ? C61 C66 C67 120.70(19) . . ? C68 C67 C72 117.5(2) . . ? C68 C67 C66 120.10(19) . . ? C72 C67 C66 122.4(2) . . ? C69 C68 C67 121.6(2) . . ? C69 C68 N1 119.9(2) . . ? C67 C68 N1 118.40(19) . . ? C68 C69 C70 119.7(3) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C71 C70 C69 119.4(2) . . ? C71 C70 H70 120.3 . . ? C69 C70 H70 120.3 . . ? C70 C71 C72 120.9(2) . . ? C70 C71 H71 119.6 . . ? C72 C71 H71 119.6 . . ? C71 C72 C67 121.0(3) . . ? C71 C72 H72 119.5 . . ? C67 C72 H72 119.5 . . ? O1 S1 O3 113.03(10) . . ? O1 S1 O2 113.13(10) . . ? O3 S1 O2 112.20(10) . . ? O1 S1 C81 106.19(11) . . ? O3 S1 C81 105.95(11) . . ? O2 S1 C81 105.57(12) . . ? S1 C81 H81A 109.5 . . ? S1 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? S1 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C161 Pd2 N2 81.18(9) . . ? C161 Pd2 P4 91.90(7) . . ? N2 Pd2 P4 171.80(6) . . ? C161 Pd2 P3 175.14(7) . . ? N2 Pd2 P3 93.97(6) . . ? P4 Pd2 P3 92.92(2) . . ? C101 P3 C107 104.89(10) . . ? C101 P3 C121 106.30(10) . . ? C107 P3 C121 104.95(10) . . ? C101 P3 Pd2 118.50(8) . . ? C107 P3 Pd2 108.19(7) . . ? C121 P3 Pd2 112.92(7) . . ? C147 P4 C141 105.76(10) . . ? C147 P4 C131 107.04(10) . . ? C141 P4 C131 104.78(10) . . ? C147 P4 Pd2 113.86(7) . . ? C141 P4 Pd2 113.53(8) . . ? C131 P4 Pd2 111.22(7) . . ? C106 C101 C102 119.9(2) . . ? C106 C101 P3 119.09(18) . . ? C102 C101 P3 121.01(18) . . ? C103 C102 C101 119.7(3) . . ? C103 C102 H102 120.2 . . ? C101 C102 H102 120.2 . . ? C104 C103 C102 120.3(3) . . ? C104 C103 H103 119.8 . . ? C102 C103 H103 119.8 . . ? C105 C104 C103 119.7(3) . . ? C105 C104 H104 120.1 . . ? C103 C104 H104 120.1 . . ? C104 C105 C106 121.2(3) . . ? C104 C105 H105 119.4 . . ? C106 C105 H105 119.4 . . ? C101 C106 C105 119.1(3) . . ? C101 C106 H106 120.4 . . ? C105 C106 H106 120.4 . . ? C108 C107 C112 119.2(2) . . ? C108 C107 P3 123.98(17) . . ? C112 C107 P3 116.76(16) . . ? C109 C108 C107 119.6(2) . . ? C109 C108 H108 120.2 . . ? C107 C108 H108 120.2 . . ? C110 C109 C108 120.7(2) . . ? C110 C109 H109 119.6 . . ? C108 C109 H109 119.6 . . ? C111 C110 C109 120.1(2) . . ? C111 C110 H110 119.9 . . ? C109 C110 H110 119.9 . . ? C110 C111 C112 119.8(2) . . ? C110 C111 H111 120.1 . . ? C112 C111 H111 120.1 . . ? C111 C112 C107 120.5(2) . . ? C111 C112 H112 119.7 . . ? C107 C112 H112 119.7 . . ? C122 C121 C130 120.0(2) . . ? C122 C121 P3 121.09(16) . . ? C130 C121 P3 118.47(16) . . ? C121 C122 C123 119.70(19) . . ? C121 C122 C132 121.58(19) . . ? C123 C122 C132 118.71(18) . . ? C124 C123 C128 118.0(2) . . ? C124 C123 C122 122.83(19) . . ? C128 C123 C122 119.17(19) . . ? C125 C124 C123 120.8(2) . . ? C125 C124 H124 119.6 . . ? C123 C124 H124 119.6 . . ? C124 C125 C126 120.8(2) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? C127 C126 C125 119.8(2) . . ? C127 C126 H126 120.1 . . ? C125 C126 H126 120.1 . . ? C126 C127 C128 120.9(2) . . ? C126 C127 H127 119.5 . . ? C128 C127 H127 119.5 . . ? C129 C128 C127 121.0(2) . . ? C129 C128 C123 119.4(2) . . ? C127 C128 C123 119.6(2) . . ? C130 C129 C128 120.8(2) . . ? C130 C129 H129 119.6 . . ? C128 C129 H129 119.6 . . ? C129 C130 C121 120.9(2) . . ? C129 C130 H130 119.6 . . ? C121 C130 H130 119.6 . . ? C132 C131 C140 119.69(19) . . ? C132 C131 P4 122.70(15) . . ? C140 C131 P4 117.27(16) . . ? C131 C132 C133 119.39(18) . . ? C131 C132 C122 122.34(18) . . ? C133 C132 C122 118.27(18) . . ? C134 C133 C138 118.02(19) . . ? C134 C133 C132 122.37(19) . . ? C138 C133 C132 119.61(19) . . ? C135 C134 C133 121.3(2) . . ? C135 C134 H134 119.3 . . ? C133 C134 H134 119.3 . . ? C134 C135 C136 120.4(2) . . ? C134 C135 H135 119.8 . . ? C136 C135 H135 119.8 . . ? C137 C136 C135 120.0(2) . . ? C137 C136 H136 120.0 . . ? C135 C136 H136 120.0 . . ? C136 C137 C138 120.8(2) . . ? C136 C137 H137 119.6 . . ? C138 C137 H137 119.6 . . ? C139 C138 C137 121.4(2) . . ? C139 C138 C133 119.17(19) . . ? C137 C138 C133 119.5(2) . . ? C140 C139 C138 120.7(2) . . ? C140 C139 H139 119.7 . . ? C138 C139 H139 119.7 . . ? C139 C140 C131 121.4(2) . . ? C139 C140 H140 119.3 . . ? C131 C140 H140 119.3 . . ? C146 C141 C142 118.9(2) . . ? C146 C141 P4 123.00(18) . . ? C142 C141 P4 117.91(17) . . ? C143 C142 C141 120.9(2) . . ? C143 C142 H142 119.6 . . ? C141 C142 H142 119.6 . . ? C142 C143 C144 119.7(2) . . ? C142 C143 H143 120.1 . . ? C144 C143 H143 120.1 . . ? C145 C144 C143 120.1(2) . . ? C145 C144 H144 120.0 . . ? C143 C144 H144 120.0 . . ? C144 C145 C146 120.4(2) . . ? C144 C145 H145 119.8 . . ? C146 C145 H145 119.8 . . ? C141 C146 C145 120.1(2) . . ? C141 C146 H146 120.0 . . ? C145 C146 H146 120.0 . . ? C148 C147 C152 119.8(2) . . ? C148 C147 P4 122.03(17) . . ? C152 C147 P4 118.21(18) . . ? C149 C148 C147 120.1(2) . . ? C149 C148 H148 119.9 . . ? C147 C148 H148 119.9 . . ? C148 C149 C150 120.2(2) . . ? C148 C149 H149 119.9 . . ? C150 C149 H149 119.9 . . ? C151 C150 C149 119.7(2) . . ? C151 C150 H150 120.2 . . ? C149 C150 H150 120.2 . . ? C150 C151 C152 120.8(2) . . ? C150 C151 H151 119.6 . . ? C152 C151 H151 119.6 . . ? C151 C152 C147 119.4(2) . . ? C151 C152 H152 120.3 . . ? C147 C152 H152 120.3 . . ? C168 N2 Pd2 104.32(14) . . ? C168 N2 H2A 105(2) . . ? Pd2 N2 H2A 116(2) . . ? C168 N2 H2B 114(2) . . ? Pd2 N2 H2B 106(2) . . ? H2A N2 H2B 112(3) . . ? C162 C161 C166 119.3(2) . . ? C162 C161 Pd2 124.4(2) . . ? C166 C161 Pd2 116.3(2) . . ? C161 C162 C163 121.0(3) . . ? C161 C162 H162 119.5 . . ? C163 C162 H162 119.5 . . ? C164 C163 C162 119.7(4) . . ? C164 C163 H163 120.1 . . ? C162 C163 H163 120.1 . . ? C163 C164 C165 120.2(3) . . ? C163 C164 H164 119.9 . . ? C165 C164 H164 119.9 . . ? C164 C165 C166 120.7(4) . . ? C164 C165 H165 119.7 . . ? C166 C165 H165 119.7 . . ? C165 C166 C161 118.9(3) . . ? C165 C166 C167 119.4(3) . . ? C161 C166 C167 121.7(2) . . ? C172 C167 C168 116.6(3) . . ? C172 C167 C166 123.0(3) . . ? C168 C167 C166 120.4(2) . . ? C169 C168 C167 121.8(3) . . ? C169 C168 N2 119.6(2) . . ? C167 C168 N2 118.5(2) . . ? C168 C169 C170 120.1(3) . . ? C168 C169 H169 119.9 . . ? C170 C169 H169 119.9 . . ? C171 C170 C169 119.3(3) . . ? C171 C170 H170 120.3 . . ? C169 C170 H170 120.3 . . ? C170 C171 C172 120.5(3) . . ? C170 C171 H171 119.7 . . ? C172 C171 H171 119.7 . . ? C171 C172 C167 121.7(3) . . ? C171 C172 H172 119.2 . . ? C167 C172 H172 119.2 . . ? O4 S2 O5 113.31(13) . . ? O4 S2 O6 112.76(13) . . ? O5 S2 O6 112.80(12) . . ? O4 S2 C181 105.84(14) . . ? O5 S2 C181 105.81(15) . . ? O6 S2 C181 105.47(14) . . ? S2 C181 H18A 109.5 . . ? S2 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? S2 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? Cl1 C1S Cl2 110.55(14) . . ? Cl1 C1S H1S1 109.5 . . ? Cl2 C1S H1S1 109.5 . . ? Cl1 C1S H1S2 109.5 . . ? Cl2 C1S H1S2 109.5 . . ? H1S1 C1S H1S2 108.1 . . ? Cl4 C2S Cl3 111.86(14) . . ? Cl4 C2S H2S1 109.2 . . ? Cl3 C2S H2S1 109.2 . . ? Cl4 C2S H2S2 109.2 . . ? Cl3 C2S H2S2 109.2 . . ? H2S1 C2S H2S2 107.9 . . ? Cl5 C3S Cl6 112.41(17) . . ? Cl5 C3S H3S1 109.1 . . ? Cl6 C3S H3S1 109.1 . . ? Cl5 C3S H3S2 109.1 . . ? Cl6 C3S H3S2 109.1 . . ? H3S1 C3S H3S2 107.9 . . ? Cl7 C4S Cl8 108.9(6) . . ? Cl7 C4S H4S1 109.9 . . ? Cl8 C4S H4S1 109.9 . . ? Cl7 C4S H4S2 109.9 . . ? Cl8 C4S H4S2 109.9 . . ? H4S1 C4S H4S2 108.3 . . ? Cl7A C4T Cl8A 111.8(9) . . ? Cl7A C4T H4T1 109.3 . . ? Cl8A C4T H4T1 109.3 . . ? Cl7A C4T H4T2 109.3 . . ? Cl8A C4T H4T2 109.3 . . ? H4T1 C4T H4T2 107.9 . . ? C4T Cl8A Cl18 108.0(8) . . ? Cl10 C5S Cl9 110.8(5) . . ? Cl10 C5S H5S1 109.5 . . ? Cl9 C5S H5S1 109.5 . . ? Cl10 C5S H5S2 109.5 . . ? Cl9 C5S H5S2 109.5 . . ? H5S1 C5S H5S2 108.1 . . ? Cl9A C5T Cl11 117.4(6) . . ? Cl9A C5T H5T1 108.0 . . ? Cl11 C5T H5T1 108.0 . . ? Cl9A C5T H5T2 108.0 . . ? Cl11 C5T H5T2 108.0 . . ? H5T1 C5T H5T2 107.2 . . ? Cl13 C6S Cl12 114.2(3) . . ? Cl13 C6S H6S1 108.7 . . ? Cl12 C6S H6S1 108.7 . . ? Cl13 C6S H6S2 108.7 . . ? Cl12 C6S H6S2 108.7 . . ? H6S1 C6S H6S2 107.6 . . ? Cl14 C6T Cl15 107.6(7) . . ? Cl14 C6T H6T1 110.2 . . ? Cl15 C6T H6T1 110.2 . . ? Cl14 C6T H6T2 110.2 . . ? Cl15 C6T H6T2 110.2 . . ? H6T1 C6T H6T2 108.5 . . ? Cl16 C7S Cl17 114.1(6) . . ? Cl16 C7S H7S1 108.7 . . ? Cl17 C7S H7S1 108.7 . . ? Cl16 C7S H7S2 108.7 . . ? Cl17 C7S H7S2 108.7 . . ? H7S1 C7S H7S2 107.6 . . ? Cl18 C7T Cl19 113.3(11) . . ? Cl18 C7T H7T1 108.9 . . ? Cl19 C7T H7T1 108.9 . . ? Cl18 C7T H7T2 108.9 . . ? Cl19 C7T H7T2 108.9 . . ? H7T1 C7T H7T2 107.7 . . ? C7T Cl18 Cl8A 150.0(16) . . ? Cl20 C8S Cl21 110.5(8) . . ? Cl20 C8S H8S1 109.6 . . ? Cl21 C8S H8S1 109.6 . . ? Cl20 C8S H8S2 109.6 . . ? Cl21 C8S H8S2 109.6 . . ? H8S1 C8S H8S2 108.1 . . ? Cl23 C8T Cl22 116(2) . . ? Cl23 C8T H8T1 108.4 . . ? Cl22 C8T H8T1 108.4 . . ? Cl23 C8T H8T2 108.4 . . ? Cl22 C8T H8T2 108.4 . . ? H8T1 C8T H8T2 107.5 . . ? Cl25 C8U Cl24 110.9(17) . . ? Cl25 C8U H8U1 109.5 . . ? Cl24 C8U H8U1 109.5 . . ? Cl25 C8U H8U2 109.5 . . ? Cl24 C8U H8U2 109.5 . . ? H8U1 C8U H8U2 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O2 0.895(17) 2.017(19) 2.873(2) 160(3) . N1 H1B S1 0.895(17) 2.99(2) 3.736(2) 141(2) . N2 H2B O6 0.885(17) 2.03(2) 2.837(3) 151(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.593 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.092