Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Ramon Vilar' 'D. Mingos' 'Gareth R. Owen' 'Andrew White' 'David J. Williams' 'Anna M. Williamson' _publ_contact_author_name 'Dr Ramon Vilar' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Technology and Medicine South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email R.VILAR@IMPERIAL.AC.UK _publ_section_title ; Synthesis and Structural Characterisation of the Palladium Cluster Compounds [Pd3(u-SO2)2(u-PPh2py)(PBz3)2] and [Pd4(u-SO2)2(u3-S)(CNR)(PBz3)3] (R=tBu, 2,6-dimethylphenyl and cyclohexyl) ; data_Compound_5 _database_code_CSD 204856 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H76 N2 O4 P4 S2 Cl6 Pd3' _chemical_formula_weight 1837.32 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 13.9578(11) _cell_length_b 14.4750(12) _cell_length_c 20.1575(15) _cell_angle_alpha 95.190(9) _cell_angle_beta 100.051(8) _cell_angle_gamma 97.313(7) _cell_volume 3950.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 11.28 _cell_measurement_theta_max 27.99 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method ? _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 8.971 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.3205 _exptl_absorpt_correction_T_max 0.4395 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12271 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 59.99 _reflns_number_total 11712 _reflns_number_observed 9349 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 718 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+6.6648P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10994 _refine_ls_number_parameters 798 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_obs 0.0526 _refine_ls_wR_factor_all 0.1424 _refine_ls_wR_factor_obs 0.1235 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.79852(3) 0.67013(3) 0.72052(2) 0.02525(14) Uani 1 d . . Pd2 Pd 0.68457(3) 0.61383(3) 0.80706(2) 0.02821(14) Uani 1 d . . Pd3 Pd 0.71574(3) 0.78118(3) 0.63680(2) 0.02783(14) Uani 1 d . . S1 S 0.64095(11) 0.56948(10) 0.69792(7) 0.0282(3) Uani 1 d . . S2 S 0.77559(12) 0.83155(10) 0.74447(7) 0.0309(3) Uani 1 d . . P1 P 0.90758(11) 0.64701(11) 0.81510(8) 0.0297(3) Uani 1 d . . P2 P 0.85712(12) 0.64286(11) 0.62062(8) 0.0314(3) Uani 1 d . . P3 P 0.54498(12) 0.54688(12) 0.83795(8) 0.0338(4) Uani 1 d . . P4 P 0.65948(12) 0.91561(11) 0.60876(8) 0.0323(3) Uani 1 d . . O1 O 0.6436(4) 0.4707(3) 0.6773(3) 0.0436(11) Uani 1 d . . O2 O 0.5488(4) 0.5980(4) 0.6659(3) 0.0439(12) Uani 1 d . . O3 O 0.7017(4) 0.8584(4) 0.7837(3) 0.0456(12) Uani 1 d . . O4 O 0.8651(4) 0.9028(4) 0.7575(2) 0.0432(11) Uani 1 d . . N1 N 0.7846(4) 0.6922(4) 0.8963(3) 0.0340(12) Uani 1 d . . C2 C 0.7565(6) 0.7317(6) 0.9500(4) 0.045(2) Uani 1 d . . H2A H 0.6891(6) 0.7228(6) 0.9517(4) 0.054 Uiso 1 calc R . C3 C 0.8206(6) 0.7853(6) 1.0037(4) 0.049(2) Uani 1 d . . H3A H 0.7972(6) 0.8143(6) 1.0401(4) 0.058 Uiso 1 calc R . C4 C 0.9209(6) 0.7953(6) 1.0023(4) 0.053(2) Uani 1 d . . H4A H 0.9671(6) 0.8294(6) 1.0386(4) 0.064 Uiso 1 calc R . C5 C 0.9508(6) 0.7544(6) 0.9466(4) 0.046(2) Uani 1 d . . H5A H 1.0180(6) 0.7605(6) 0.9446(4) 0.055 Uiso 1 calc R . C6 C 0.8822(5) 0.7041(5) 0.8938(3) 0.0317(13) Uani 1 d . . N7 N 0.6848(4) 0.6684(4) 0.5525(3) 0.0318(11) Uani 1 d . . C8 C 0.6005(6) 0.6497(5) 0.5058(4) 0.043(2) Uani 1 d . . H8A H 0.5534(6) 0.6905(5) 0.5072(4) 0.052 Uiso 1 calc R . C9 C 0.5802(6) 0.5742(6) 0.4564(4) 0.051(2) Uani 1 d . . H9A H 0.5208(6) 0.5634(6) 0.4247(4) 0.062 Uiso 1 calc R . C10 C 0.6495(8) 0.5151(7) 0.4551(4) 0.061(2) Uani 1 d . . H10A H 0.6375(8) 0.4625(7) 0.4222(4) 0.074 Uiso 1 calc R . C11 C 0.7370(7) 0.5324(6) 0.5017(4) 0.050(2) Uani 1 d . . H11A H 0.7849(7) 0.4924(6) 0.5007(4) 0.060 Uiso 1 calc R . C12 C 0.7525(5) 0.6098(5) 0.5498(3) 0.039(2) Uani 1 d . . C13 C 0.9806(4) 0.5147(3) 0.8963(2) 0.046(2) Uani 1 d G . H13A H 1.0157(4) 0.5665(3) 0.9260(2) 0.055 Uiso 1 calc R . C14 C 0.9914(4) 0.4242(3) 0.9111(2) 0.058(2) Uani 1 d G . H14A H 1.0338(6) 0.4149(5) 0.9508(3) 0.069 Uiso 1 calc R . C15 C 0.9395(4) 0.3476(2) 0.8672(3) 0.055(2) Uani 1 d G . H15A H 0.9468(6) 0.2864(3) 0.8772(4) 0.066 Uiso 1 calc R . C16 C 0.8767(4) 0.3615(3) 0.8086(3) 0.067(3) Uani 1 d G . H16A H 0.8416(6) 0.3097(3) 0.7789(4) 0.080 Uiso 1 calc R . C17 C 0.8659(4) 0.4520(3) 0.7938(2) 0.056(2) Uani 1 d G . H17A H 0.8235(6) 0.4614(4) 0.7541(3) 0.068 Uiso 1 calc R . C18 C 0.9178(4) 0.5286(2) 0.8377(2) 0.0324(13) Uani 1 d G . C19 C 1.1028(3) 0.6390(3) 0.8010(3) 0.051(2) Uani 1 d G . H19A H 1.0850(3) 0.5736(3) 0.7950(3) 0.061 Uiso 1 calc R . C20 C 1.1974(3) 0.6781(4) 0.7966(4) 0.067(3) Uani 1 d G . H20A H 1.2436(4) 0.6391(5) 0.7876(5) 0.081 Uiso 1 calc R . C21 C 1.2237(3) 0.7750(4) 0.8055(4) 0.065(2) Uani 1 d G . H21A H 1.2876(3) 0.8014(5) 0.8025(5) 0.078 Uiso 1 calc R . C22 C 1.1553(4) 0.8327(3) 0.8187(4) 0.069(3) Uani 1 d G . H22A H 1.1731(5) 0.8982(3) 0.8247(5) 0.082 Uiso 1 calc R . C23 C 1.0607(3) 0.7936(3) 0.8231(3) 0.060(2) Uani 1 d G . H23A H 1.0145(5) 0.8327(4) 0.8321(5) 0.072 Uiso 1 calc R . C24 C 1.0344(3) 0.6968(3) 0.8143(3) 0.0342(14) Uani 1 d G . C25 C 0.8871(3) 0.4582(3) 0.6258(3) 0.060(2) Uani 1 d G . H25A H 0.8194(3) 0.4473(3) 0.6263(3) 0.072 Uiso 1 calc R . C26 C 0.9429(5) 0.3855(3) 0.6330(4) 0.072(3) Uani 1 d G . H26A H 0.9129(6) 0.3254(3) 0.6384(5) 0.086 Uiso 1 calc R . C27 C 1.0430(4) 0.4016(4) 0.6323(3) 0.069(3) Uani 1 d G . H27A H 1.0807(6) 0.3524(5) 0.6372(5) 0.083 Uiso 1 calc R . C28 C 1.0874(3) 0.4905(4) 0.6244(3) 0.067(3) Uani 1 d G . H28A H 1.1551(3) 0.5014(6) 0.6239(5) 0.081 Uiso 1 calc R . C29 C 1.0316(3) 0.5632(3) 0.6172(3) 0.055(2) Uani 1 d G . H29A H 1.0616(5) 0.6233(4) 0.6119(5) 0.066 Uiso 1 calc R . C30 C 0.9315(3) 0.5471(3) 0.6179(3) 0.039(2) Uani 1 d G . C31 C 0.9508(5) 0.7256(4) 0.5236(2) 0.064(3) Uani 1 d G . H31A H 0.9281(5) 0.6686(4) 0.4957(2) 0.077 Uiso 1 calc R . C32 C 1.0050(5) 0.7985(5) 0.4997(2) 0.077(3) Uani 1 d G . H32A H 1.0189(8) 0.7908(7) 0.4558(3) 0.092 Uiso 1 calc R . C33 C 1.0387(5) 0.8828(4) 0.5409(4) 0.072(3) Uani 1 d G . H33A H 1.0753(7) 0.9321(5) 0.5248(5) 0.087 Uiso 1 calc R . C34 C 1.0181(5) 0.8941(3) 0.6060(4) 0.098(5) Uani 1 d G . H34A H 1.0409(8) 0.9511(4) 0.6338(5) 0.118 Uiso 1 calc R . C35 C 0.9639(5) 0.8212(4) 0.6298(3) 0.074(3) Uani 1 d G . H35A H 0.9500(7) 0.8289(6) 0.6738(3) 0.089 Uiso 1 calc R . C36 C 0.9303(4) 0.7370(3) 0.5886(2) 0.0364(14) Uani 1 d G . C37 C 0.4778(6) 0.4451(6) 0.7784(4) 0.046(2) Uani 1 d . . H37A H 0.4633(6) 0.4655(6) 0.7331(4) 0.055 Uiso 1 calc R . H37B H 0.5215(6) 0.3975(6) 0.7762(4) 0.055 Uiso 1 calc R . C38 C 0.2937(4) 0.4313(4) 0.7722(3) 0.057(2) Uani 1 d G . H38A H 0.2924(4) 0.4801(4) 0.7444(3) 0.068 Uiso 1 calc R . C39 C 0.2074(3) 0.3914(4) 0.7903(3) 0.064(2) Uani 1 d G . H39A H 0.1478(3) 0.4132(6) 0.7747(5) 0.077 Uiso 1 calc R . C40 C 0.2092(3) 0.3194(4) 0.8314(3) 0.066(3) Uani 1 d G . H40A H 0.1508(4) 0.2924(6) 0.8436(5) 0.079 Uiso 1 calc R . C41 C 0.2974(4) 0.2872(4) 0.8544(3) 0.068(3) Uani 1 d G . H41A H 0.2986(6) 0.2384(5) 0.8822(4) 0.081 Uiso 1 calc R . C42 C 0.3837(3) 0.3271(4) 0.8363(3) 0.055(2) Uani 1 d G . H42A H 0.4433(4) 0.3053(5) 0.8519(4) 0.066 Uiso 1 calc R . C43 C 0.3818(3) 0.3992(4) 0.7952(3) 0.044(2) Uani 1 d G . C44 C 0.5521(5) 0.5111(5) 0.9235(3) 0.0387(15) Uani 1 d . . H44A H 0.5551(5) 0.5674(5) 0.9551(3) 0.046 Uiso 1 calc R . H44B H 0.4907(5) 0.4705(5) 0.9244(3) 0.046 Uiso 1 calc R . C45 C 0.6514(4) 0.3776(4) 0.9160(2) 0.056(2) Uani 1 d G . H45A H 0.6137(4) 0.3557(4) 0.8727(2) 0.067 Uiso 1 calc R . C46 C 0.7222(4) 0.3268(4) 0.9457(3) 0.070(3) Uani 1 d G . H46A H 0.7324(6) 0.2707(5) 0.9226(4) 0.084 Uiso 1 calc R . C47 C 0.7778(4) 0.3592(4) 1.0096(3) 0.072(3) Uani 1 d G . H47A H 0.8257(6) 0.3249(6) 1.0297(4) 0.087 Uiso 1 calc R . C48 C 0.7626(4) 0.4422(5) 1.0439(2) 0.067(3) Uani 1 d G . H48A H 0.8003(6) 0.4641(6) 1.0871(3) 0.080 Uiso 1 calc R . C49 C 0.6919(4) 0.4930(3) 1.0141(2) 0.052(2) Uani 1 d G . H49A H 0.6816(6) 0.5492(4) 1.0373(3) 0.062 Uiso 1 calc R . C50 C 0.6362(3) 0.4606(3) 0.9502(2) 0.042(2) Uani 1 d G . C51 C 0.4497(5) 0.6238(6) 0.8371(4) 0.041(2) Uani 1 d . . H51A H 0.4272(5) 0.6361(6) 0.7904(4) 0.049 Uiso 1 calc R . H51B H 0.3933(5) 0.5910(6) 0.8527(4) 0.049 Uiso 1 calc R . C52 C 0.4655(5) 0.7296(4) 0.9465(3) 0.058(2) Uani 1 d G . H52A H 0.4306(5) 0.6807(4) 0.9641(3) 0.070 Uiso 1 calc R . C53 C 0.4983(6) 0.8155(4) 0.9858(3) 0.077(3) Uani 1 d G . H53A H 0.4855(8) 0.8246(6) 1.0300(3) 0.092 Uiso 1 calc R . C54 C 0.5498(6) 0.8879(4) 0.9597(3) 0.083(3) Uani 1 d G . H54A H 0.5720(8) 0.9459(4) 0.9863(5) 0.100 Uiso 1 calc R . C55 C 0.5687(5) 0.8744(3) 0.8943(3) 0.071(3) Uani 1 d G . H55A H 0.6036(7) 0.9233(4) 0.8767(5) 0.085 Uiso 1 calc R . C56 C 0.5359(4) 0.7885(4) 0.8550(2) 0.055(2) Uani 1 d G . H56A H 0.5487(7) 0.7794(5) 0.8108(3) 0.066 Uiso 1 calc R . C57 C 0.4843(4) 0.7162(3) 0.8811(2) 0.045(2) Uani 1 d G . C58 C 0.5721(5) 0.9538(5) 0.6594(4) 0.041(2) Uani 1 d . . H58A H 0.6036(5) 0.9607(5) 0.7074(4) 0.049 Uiso 1 calc R . H58B H 0.5587(5) 1.0160(5) 0.6482(4) 0.049 Uiso 1 calc R . C59 C 0.4717(3) 0.7964(3) 0.6622(3) 0.047(2) Uani 1 d G . H59A H 0.5307(3) 0.7712(3) 0.6722(3) 0.056 Uiso 1 calc R . C60 C 0.3821(4) 0.7404(3) 0.6591(3) 0.054(2) Uani 1 d G . H60A H 0.3804(5) 0.6773(3) 0.6669(4) 0.064 Uiso 1 calc R . C61 C 0.2949(3) 0.7778(4) 0.6444(3) 0.067(3) Uani 1 d G . H61A H 0.2343(3) 0.7399(5) 0.6423(5) 0.080 Uiso 1 calc R . C62 C 0.2974(3) 0.8712(4) 0.6329(3) 0.067(3) Uani 1 d G . H62A H 0.2384(3) 0.8965(6) 0.6229(5) 0.080 Uiso 1 calc R . C63 C 0.3870(4) 0.9273(3) 0.6360(3) 0.049(2) Uani 1 d G . H63A H 0.3887(5) 0.9904(3) 0.6281(4) 0.059 Uiso 1 calc R . C64 C 0.4742(3) 0.8899(3) 0.6507(3) 0.041(2) Uani 1 d G . C65 C 0.7593(5) 1.0181(5) 0.6289(4) 0.040(2) Uani 1 d . . H65A H 0.7896(5) 1.0211(5) 0.6769(4) 0.048 Uiso 1 calc R . H65B H 0.8098(5) 1.0061(5) 0.6024(4) 0.048 Uiso 1 calc R . C66 C 0.7099(4) 1.1712(3) 0.6689(2) 0.045(2) Uani 1 d G . H66A H 0.7139(4) 1.1519(3) 0.7124(2) 0.054 Uiso 1 calc R . C67 C 0.6826(4) 1.2581(3) 0.6569(2) 0.048(2) Uani 1 d G . H67A H 0.6682(6) 1.2976(4) 0.6923(3) 0.058 Uiso 1 calc R . C68 C 0.6767(4) 1.2867(3) 0.5924(2) 0.051(2) Uani 1 d G . H68A H 0.6582(6) 1.3455(3) 0.5843(3) 0.061 Uiso 1 calc R . C69 C 0.6980(5) 1.2282(3) 0.5400(2) 0.057(2) Uani 1 d G . H69A H 0.6939(7) 1.2475(5) 0.4964(2) 0.068 Uiso 1 calc R . C70 C 0.7252(4) 1.1413(3) 0.5520(2) 0.049(2) Uani 1 d G . H70A H 0.7396(6) 1.1018(4) 0.5166(2) 0.059 Uiso 1 calc R . C71 C 0.7312(4) 1.1128(2) 0.6164(2) 0.0392(15) Uani 1 d G . C72 C 0.5947(5) 0.9215(5) 0.5229(4) 0.0381(15) Uani 1 d . . H72A H 0.5265(5) 0.8919(5) 0.5191(4) 0.046 Uiso 1 calc R . H72B H 0.5930(5) 0.9877(5) 0.5168(4) 0.046 Uiso 1 calc R . C73 C 0.7362(3) 0.8837(5) 0.4640(2) 0.059(2) Uani 1 d G . H73A H 0.7817(3) 0.9150(5) 0.5018(2) 0.070 Uiso 1 calc R . C74 C 0.7692(3) 0.8447(6) 0.4081(3) 0.077(3) Uani 1 d G . H74A H 0.8369(4) 0.8497(8) 0.4081(4) 0.092 Uiso 1 calc R . C75 C 0.7019(5) 0.7984(6) 0.3523(2) 0.083(3) Uani 1 d G . H75A H 0.7241(7) 0.7720(8) 0.3145(3) 0.100 Uiso 1 calc R . C76 C 0.6016(5) 0.7910(5) 0.3524(2) 0.072(3) Uani 1 d G . H76A H 0.5561(6) 0.7597(7) 0.3147(3) 0.087 Uiso 1 calc R . C77 C 0.5687(3) 0.8300(4) 0.4083(3) 0.057(2) Uani 1 d G . H77A H 0.5009(3) 0.8250(7) 0.4084(4) 0.068 Uiso 1 calc R . C78 C 0.6360(3) 0.8763(4) 0.4642(2) 0.042(2) Uani 1 d G . C80 C 0.8346(11) 0.0070(8) 0.9067(6) 0.086(4) Uani 1 d . . H80A H 0.8973(11) -0.0118(8) 0.8994(6) 0.103 Uiso 1 calc R . H80B H 0.7829(11) -0.0467(8) 0.8905(6) 0.103 Uiso 1 calc R . Cl1 Cl 0.8100(4) 0.0998(3) 0.8612(2) 0.1133(12) Uani 1 d . . Cl2 Cl 0.8405(5) 0.0384(3) 0.9933(2) 0.141(2) Uani 1 d . . C90 C 0.0029(17) 0.0834(15) 0.7556(8) 0.115(7) Uani 0.75 d PU 1 H90A H -0.0087(17) 0.0191(15) 0.7329(8) 0.137 Uiso 0.75 calc PR 1 H90B H -0.0603(17) 0.0955(15) 0.7666(8) 0.137 Uiso 0.75 calc PR 1 Cl3 Cl 0.0205(6) 0.1502(4) 0.6951(3) 0.109(2) Uani 0.75 d P 1 Cl4 Cl 0.0769(3) 0.0776(3) 0.8333(2) 0.0854(10) Uani 0.75 d P 1 C90' C 0.0775(30) 0.1318(25) 0.7053(18) 0.047(8) Uiso 0.25 d P 2 H90C H 0.1274(30) 0.1841(25) 0.7013(18) 0.056 Uiso 0.25 calc PR 2 H90D H 0.0642(30) 0.0858(25) 0.6648(18) 0.056 Uiso 0.25 calc PR 2 Cl3' Cl -0.0063(15) 0.1596(13) 0.7238(10) 0.103(5) Uiso 0.25 d P 2 Cl4' Cl 0.1066(15) 0.0715(14) 0.7990(11) 0.117(5) Uiso 0.25 d P 2 C100 C 0.4279(19) 0.0429(20) 0.7966(12) 0.175(11) Uani 1 d . . H10B H 0.4428(19) -0.0199(20) 0.7839(12) 0.210 Uiso 0.70 calc PR 1 H10C H 0.3880(19) 0.0620(20) 0.7566(12) 0.210 Uiso 0.70 calc PR 1 H10D H 0.4438(19) -0.0153(20) 0.8117(12) 0.210 Uiso 0.30 d PR 2 H10E H 0.4136(19) 0.0325(20) 0.7480(12) 0.210 Uiso 0.30 d PR 2 Cl5 Cl 0.5347(4) 0.1174(4) 0.8169(3) 0.1275(14) Uani 1 d . . Cl6 Cl 0.3582(4) 0.0361(4) 0.8598(4) 0.118(2) Uani 0.70 d P 1 Cl6' Cl 0.3350(13) 0.0546(12) 0.8129(9) 0.118(4) Uiso 0.30 d P 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 0.0243(2) 0.0279(2) 0.0226(2) 0.0039(2) 0.0013(2) 0.0041(2) Pd2 0.0256(2) 0.0327(2) 0.0237(2) 0.0007(2) 0.0028(2) -0.0009(2) Pd3 0.0316(2) 0.0252(2) 0.0242(2) 0.0030(2) -0.0014(2) 0.0038(2) S1 0.0279(7) 0.0292(7) 0.0246(7) 0.0022(5) 0.0004(5) -0.0001(6) S2 0.0361(8) 0.0272(7) 0.0269(7) 0.0010(6) 0.0023(6) 0.0021(6) P1 0.0264(7) 0.0338(8) 0.0270(7) 0.0042(6) 0.0001(6) 0.0043(6) P2 0.0327(8) 0.0331(8) 0.0273(7) 0.0017(6) 0.0054(6) 0.0026(6) P3 0.0277(8) 0.0442(9) 0.0271(8) 0.0034(7) 0.0040(6) -0.0021(7) P4 0.0344(8) 0.0280(8) 0.0332(8) 0.0061(6) 0.0002(6) 0.0061(6) O1 0.046(3) 0.031(2) 0.049(3) -0.009(2) 0.005(2) 0.002(2) O2 0.029(2) 0.048(3) 0.049(3) 0.012(2) -0.009(2) 0.004(2) O3 0.046(3) 0.050(3) 0.042(3) 0.000(2) 0.015(2) 0.010(2) O4 0.046(3) 0.038(3) 0.039(3) -0.003(2) -0.001(2) -0.003(2) N1 0.033(3) 0.041(3) 0.027(3) 0.000(2) 0.004(2) 0.003(2) C2 0.041(4) 0.048(4) 0.043(4) 0.002(3) 0.010(3) -0.005(3) C3 0.050(4) 0.053(4) 0.038(4) -0.005(3) 0.009(3) -0.003(4) C4 0.048(4) 0.059(5) 0.041(4) -0.012(4) -0.007(3) -0.005(4) C5 0.034(4) 0.054(4) 0.041(4) -0.004(3) -0.004(3) -0.001(3) C6 0.035(3) 0.034(3) 0.024(3) 0.001(2) 0.002(2) 0.008(3) N7 0.036(3) 0.029(3) 0.025(2) 0.000(2) -0.003(2) -0.001(2) C8 0.042(4) 0.044(4) 0.036(4) 0.001(3) -0.008(3) -0.005(3) C9 0.052(4) 0.054(5) 0.036(4) -0.002(3) -0.010(3) -0.008(4) C10 0.072(6) 0.056(5) 0.044(4) -0.021(4) 0.001(4) -0.009(4) C11 0.059(5) 0.047(4) 0.041(4) -0.009(3) 0.007(3) 0.007(4) C12 0.043(4) 0.039(4) 0.030(3) 0.003(3) 0.007(3) -0.004(3) C13 0.054(4) 0.044(4) 0.035(4) 0.005(3) 0.003(3) -0.002(3) C14 0.075(6) 0.051(5) 0.046(4) 0.025(4) -0.005(4) 0.012(4) C15 0.063(5) 0.042(4) 0.061(5) 0.020(4) 0.000(4) 0.008(4) C16 0.063(6) 0.038(4) 0.086(7) 0.007(4) -0.017(5) 0.005(4) C17 0.053(5) 0.056(5) 0.050(4) -0.002(4) -0.016(4) 0.013(4) C18 0.029(3) 0.037(3) 0.030(3) 0.006(3) -0.003(2) 0.009(3) C19 0.037(4) 0.061(5) 0.062(5) 0.016(4) 0.020(3) 0.016(4) C20 0.036(4) 0.083(7) 0.088(7) 0.009(5) 0.023(4) 0.014(4) C21 0.035(4) 0.085(7) 0.074(6) 0.018(5) 0.008(4) -0.001(4) C22 0.050(5) 0.061(6) 0.089(7) 0.016(5) 0.007(5) -0.009(4) C23 0.038(4) 0.052(5) 0.091(7) 0.017(5) 0.012(4) 0.001(4) C24 0.029(3) 0.042(4) 0.030(3) 0.009(3) -0.001(2) 0.004(3) C25 0.056(5) 0.048(5) 0.078(6) 0.002(4) 0.022(4) 0.012(4) C26 0.089(7) 0.046(5) 0.088(7) 0.015(5) 0.025(6) 0.025(5) C27 0.085(7) 0.074(7) 0.054(5) 0.002(5) 0.011(5) 0.042(6) C28 0.049(5) 0.095(8) 0.062(5) 0.006(5) 0.014(4) 0.027(5) C29 0.047(4) 0.064(5) 0.056(5) 0.009(4) 0.012(4) 0.012(4) C30 0.047(4) 0.046(4) 0.029(3) 0.002(3) 0.012(3) 0.013(3) C31 0.077(6) 0.064(6) 0.040(4) 0.008(4) 0.004(4) -0.023(5) C32 0.085(7) 0.088(8) 0.049(5) 0.026(5) 0.011(5) -0.026(6) C33 0.057(5) 0.060(6) 0.114(9) 0.039(6) 0.038(6) 0.009(4) C34 0.098(9) 0.047(5) 0.156(13) -0.020(6) 0.081(9) -0.024(6) C35 0.062(6) 0.067(6) 0.091(7) -0.024(5) 0.046(5) -0.019(5) C36 0.033(3) 0.037(4) 0.040(4) 0.006(3) 0.012(3) 0.002(3) C37 0.041(4) 0.053(4) 0.034(4) -0.002(3) 0.002(3) -0.012(3) C38 0.050(5) 0.051(5) 0.059(5) 0.008(4) -0.012(4) -0.007(4) C39 0.034(4) 0.068(6) 0.082(6) -0.009(5) 0.002(4) 0.000(4) C40 0.048(5) 0.064(6) 0.083(6) -0.007(5) 0.029(5) -0.014(4) C41 0.075(7) 0.051(5) 0.078(6) 0.012(5) 0.031(5) -0.011(5) C42 0.056(5) 0.049(5) 0.064(5) 0.011(4) 0.019(4) 0.007(4) C43 0.038(4) 0.046(4) 0.045(4) 0.004(3) 0.005(3) -0.001(3) C44 0.039(4) 0.047(4) 0.032(3) 0.007(3) 0.013(3) 0.003(3) C45 0.042(4) 0.071(6) 0.050(4) -0.008(4) 0.002(3) 0.015(4) C46 0.055(5) 0.073(6) 0.080(7) -0.012(5) 0.008(5) 0.022(5) C47 0.042(5) 0.094(8) 0.081(7) 0.015(6) -0.001(4) 0.027(5) C48 0.046(5) 0.095(7) 0.059(5) 0.011(5) -0.005(4) 0.024(5) C49 0.044(4) 0.064(5) 0.044(4) 0.000(4) 0.001(3) 0.006(4) C50 0.035(4) 0.056(4) 0.035(3) 0.007(3) 0.008(3) 0.003(3) C51 0.028(3) 0.053(4) 0.041(4) 0.008(3) 0.005(3) 0.004(3) C52 0.056(5) 0.061(5) 0.063(5) 0.012(4) 0.027(4) 0.006(4) C53 0.086(7) 0.079(7) 0.068(6) -0.015(5) 0.037(6) 0.006(6) C54 0.094(8) 0.054(6) 0.104(9) -0.006(6) 0.035(7) 0.012(5) C55 0.074(6) 0.057(6) 0.090(7) 0.009(5) 0.032(6) 0.012(5) C56 0.051(5) 0.059(5) 0.061(5) 0.014(4) 0.024(4) 0.005(4) C57 0.040(4) 0.054(4) 0.044(4) 0.009(3) 0.011(3) 0.014(3) C58 0.041(4) 0.037(4) 0.044(4) 0.002(3) 0.008(3) 0.009(3) C59 0.045(4) 0.048(4) 0.045(4) 0.001(3) 0.005(3) 0.002(3) C60 0.057(5) 0.056(5) 0.044(4) 0.012(4) 0.006(4) -0.007(4) C61 0.039(4) 0.095(8) 0.063(5) 0.017(5) 0.009(4) -0.003(5) C62 0.040(4) 0.101(8) 0.065(6) 0.027(5) 0.010(4) 0.021(5) C63 0.045(4) 0.064(5) 0.042(4) 0.015(4) 0.009(3) 0.020(4) C64 0.044(4) 0.045(4) 0.033(3) 0.004(3) 0.004(3) 0.004(3) C65 0.040(4) 0.029(3) 0.046(4) 0.004(3) -0.002(3) 0.003(3) C66 0.050(4) 0.037(4) 0.042(4) 0.003(3) -0.001(3) 0.001(3) C67 0.049(4) 0.031(4) 0.056(5) -0.010(3) -0.003(3) 0.006(3) C68 0.058(5) 0.034(4) 0.057(5) 0.006(3) -0.002(4) 0.007(3) C69 0.073(6) 0.044(4) 0.056(5) 0.018(4) 0.014(4) 0.009(4) C70 0.058(5) 0.040(4) 0.051(4) 0.011(3) 0.011(4) 0.008(3) C71 0.043(4) 0.031(3) 0.038(4) 0.002(3) -0.001(3) 0.000(3) C72 0.036(3) 0.037(4) 0.039(4) 0.013(3) -0.007(3) 0.013(3) C73 0.055(5) 0.077(6) 0.037(4) -0.003(4) -0.002(3) 0.007(4) C74 0.073(6) 0.115(9) 0.046(5) 0.000(5) 0.015(5) 0.029(6) C75 0.110(10) 0.092(8) 0.047(5) -0.004(5) 0.013(6) 0.030(7) C76 0.088(7) 0.073(6) 0.045(5) 0.000(4) -0.007(5) 0.002(5) C77 0.062(5) 0.059(5) 0.039(4) 0.002(4) -0.012(4) 0.003(4) C78 0.043(4) 0.042(4) 0.035(4) 0.010(3) -0.005(3) 0.001(3) C80 0.116(10) 0.056(6) 0.073(7) -0.021(5) 0.014(6) -0.005(6) Cl1 0.154(4) 0.075(2) 0.116(3) 0.004(2) 0.030(2) 0.032(2) Cl2 0.214(5) 0.109(3) 0.081(2) -0.026(2) 0.041(3) -0.045(3) C90 0.144(13) 0.115(12) 0.056(8) 0.025(8) -0.007(8) -0.064(11) Cl3 0.121(5) 0.088(3) 0.113(4) 0.018(3) 0.026(4) -0.010(3) Cl4 0.082(2) 0.077(2) 0.083(2) -0.014(2) 0.002(2) -0.007(2) C100 0.175(23) 0.192(24) 0.120(16) -0.056(16) -0.001(15) -0.018(19) Cl5 0.125(3) 0.134(3) 0.132(3) 0.001(3) 0.050(3) 0.028(3) Cl6 0.096(3) 0.086(3) 0.154(6) 0.001(3) -0.005(3) -0.007(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 P1 2.301(2) . ? Pd1 P2 2.322(2) . ? Pd1 S2 2.416(2) . ? Pd1 S1 2.425(2) . ? Pd1 Pd3 2.6552(6) . ? Pd1 Pd2 2.6708(6) . ? Pd2 S1 2.1910(15) . ? Pd2 N1 2.197(5) . ? Pd2 P3 2.275(2) . ? Pd3 N7 2.191(5) . ? Pd3 S2 2.206(2) . ? Pd3 P4 2.271(2) . ? S1 O1 1.460(5) . ? S1 O2 1.461(5) . ? S2 O3 1.473(5) . ? S2 O4 1.483(5) . ? P1 C24 1.828(4) . ? P1 C18 1.829(4) . ? P1 C6 1.833(6) . ? P2 C36 1.830(4) . ? P2 C12 1.837(7) . ? P2 C30 1.837(4) . ? P3 C44 1.834(7) . ? P3 C51 1.838(7) . ? P3 C37 1.851(7) . ? P4 C72 1.822(6) . ? P4 C58 1.828(7) . ? P4 C65 1.864(7) . ? N1 C2 1.320(10) . ? N1 C6 1.362(9) . ? C2 C3 1.381(11) . ? C3 C4 1.395(12) . ? C4 C5 1.375(12) . ? C5 C6 1.380(10) . ? N7 C8 1.352(9) . ? N7 C12 1.353(10) . ? C8 C9 1.376(12) . ? C9 C10 1.373(14) . ? C10 C11 1.385(13) . ? C11 C12 1.381(11) . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C25 C26 1.39 . ? C25 C30 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C29 C30 1.39 . ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? C37 C43 1.524(8) . ? C38 C39 1.39 . ? C38 C43 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C42 C43 1.39 . ? C44 C50 1.507(8) . ? C45 C46 1.39 . ? C45 C50 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C48 C49 1.39 . ? C49 C50 1.39 . ? C51 C57 1.510(9) . ? C52 C53 1.39 . ? C52 C57 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C56 C57 1.39 . ? C58 C64 1.523(8) . ? C59 C60 1.39 . ? C59 C64 1.39 . ? C60 C61 1.39 . ? C61 C62 1.39 . ? C62 C63 1.39 . ? C63 C64 1.39 . ? C65 C71 1.504(8) . ? C66 C67 1.39 . ? C66 C71 1.39 . ? C67 C68 1.39 . ? C68 C69 1.39 . ? C69 C70 1.39 . ? C70 C71 1.39 . ? C72 C78 1.535(8) . ? C73 C74 1.39 . ? C73 C78 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? C76 C77 1.39 . ? C77 C78 1.39 . ? C80 Cl1 1.731(14) . ? C80 Cl2 1.749(12) . ? C90 Cl3 1.65(2) . ? C90 Cl4 1.73(2) . ? C90' Cl3' 1.38(4) . ? C90' Cl4' 2.15(4) . ? C100 Cl6' 1.42(3) . ? C100 Cl5 1.69(2) . ? C100 Cl6 1.74(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 112.91(6) . . ? P1 Pd1 S2 102.73(6) . . ? P2 Pd1 S2 112.58(6) . . ? P1 Pd1 S1 116.04(6) . . ? P2 Pd1 S1 102.88(6) . . ? S2 Pd1 S1 110.02(6) . . ? P1 Pd1 Pd3 151.51(5) . . ? P2 Pd1 Pd3 74.37(4) . . ? S2 Pd1 Pd3 51.31(4) . . ? S1 Pd1 Pd3 87.26(4) . . ? P1 Pd1 Pd2 75.62(4) . . ? P2 Pd1 Pd2 150.19(5) . . ? S2 Pd1 Pd2 91.91(4) . . ? S1 Pd1 Pd2 50.65(4) . . ? Pd3 Pd1 Pd2 112.43(2) . . ? S1 Pd2 N1 152.7(2) . . ? S1 Pd2 P3 97.31(6) . . ? N1 Pd2 P3 109.80(15) . . ? S1 Pd2 Pd1 58.86(4) . . ? N1 Pd2 Pd1 93.87(15) . . ? P3 Pd2 Pd1 155.79(4) . . ? N7 Pd3 S2 149.91(15) . . ? N7 Pd3 P4 113.60(15) . . ? S2 Pd3 P4 96.45(6) . . ? N7 Pd3 Pd1 91.19(14) . . ? S2 Pd3 Pd1 58.73(4) . . ? P4 Pd3 Pd1 155.13(5) . . ? O1 S1 O2 111.0(3) . . ? O1 S1 Pd2 115.2(2) . . ? O2 S1 Pd2 114.9(2) . . ? O1 S1 Pd1 115.5(2) . . ? O2 S1 Pd1 124.0(2) . . ? Pd2 S1 Pd1 70.49(4) . . ? O3 S2 O4 111.9(3) . . ? O3 S2 Pd3 114.4(2) . . ? O4 S2 Pd3 115.5(2) . . ? O3 S2 Pd1 122.0(2) . . ? O4 S2 Pd1 116.8(2) . . ? Pd3 S2 Pd1 69.96(4) . . ? C24 P1 C18 103.6(2) . . ? C24 P1 C6 103.9(3) . . ? C18 P1 C6 101.0(3) . . ? C24 P1 Pd1 113.1(2) . . ? C18 P1 Pd1 120.53(15) . . ? C6 P1 Pd1 112.8(2) . . ? C36 P2 C12 101.5(3) . . ? C36 P2 C30 102.7(2) . . ? C12 P2 C30 105.6(3) . . ? C36 P2 Pd1 120.9(2) . . ? C12 P2 Pd1 109.2(2) . . ? C30 P2 Pd1 115.3(2) . . ? C44 P3 C51 100.5(3) . . ? C44 P3 C37 106.6(4) . . ? C51 P3 C37 101.0(4) . . ? C44 P3 Pd2 119.0(2) . . ? C51 P3 Pd2 113.8(2) . . ? C37 P3 Pd2 113.8(3) . . ? C72 P4 C58 101.6(3) . . ? C72 P4 C65 106.6(3) . . ? C58 P4 C65 101.0(3) . . ? C72 P4 Pd3 120.0(2) . . ? C58 P4 Pd3 113.9(2) . . ? C65 P4 Pd3 111.7(2) . . ? C2 N1 C6 118.5(6) . . ? C2 N1 Pd2 124.8(5) . . ? C6 N1 Pd2 116.6(4) . . ? N1 C2 C3 123.7(7) . . ? C2 C3 C4 118.1(7) . . ? C5 C4 C3 118.5(7) . . ? C4 C5 C6 120.2(7) . . ? N1 C6 C5 121.0(6) . . ? N1 C6 P1 112.6(5) . . ? C5 C6 P1 126.4(6) . . ? C8 N7 C12 117.8(6) . . ? C8 N7 Pd3 124.8(5) . . ? C12 N7 Pd3 117.3(4) . . ? N7 C8 C9 123.4(8) . . ? C10 C9 C8 117.7(7) . . ? C9 C10 C11 120.5(7) . . ? C12 C11 C10 118.6(8) . . ? N7 C12 C11 122.0(7) . . ? N7 C12 P2 110.9(5) . . ? C11 C12 P2 126.9(6) . . ? C14 C13 C18 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 P1 119.3(2) . . ? C13 C18 P1 120.6(2) . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 P1 119.3(3) . . ? C19 C24 P1 120.6(3) . . ? C26 C25 C30 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 P2 122.2(3) . . ? C25 C30 P2 117.3(3) . . ? C32 C31 C36 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 P2 119.2(3) . . ? C31 C36 P2 120.8(3) . . ? C43 C37 P3 116.2(5) . . ? C39 C38 C43 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 C37 119.4(5) . . ? C38 C43 C37 120.6(5) . . ? C50 C44 P3 117.8(4) . . ? C46 C45 C50 120.0 . . ? C47 C46 C45 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 C44 118.3(4) . . ? C45 C50 C44 121.3(4) . . ? C57 C51 P3 113.6(5) . . ? C53 C52 C57 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 C51 118.7(4) . . ? C52 C57 C51 121.3(4) . . ? C64 C58 P4 116.2(5) . . ? C60 C59 C64 120.0 . . ? C61 C60 C59 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 C58 119.4(4) . . ? C59 C64 C58 120.4(4) . . ? C71 C65 P4 117.3(5) . . ? C67 C66 C71 120.0 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C70 C69 C68 120.0 . . ? C69 C70 C71 120.0 . . ? C70 C71 C66 120.0 . . ? C70 C71 C65 119.8(4) . . ? C66 C71 C65 120.2(4) . . ? C78 C72 P4 117.3(4) . . ? C74 C73 C78 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C77 120.0 . . ? C78 C77 C76 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 C72 117.4(4) . . ? C73 C78 C72 122.6(4) . . ? Cl1 C80 Cl2 110.7(7) . . ? Cl3 C90 Cl4 130.3(11) . . ? Cl3' C90' Cl4' 89.0(19) . . ? Cl6' C100 Cl5 128.8(18) . . ? Cl5 C100 Cl6 115.6(11) . . ? _refine_diff_density_max 0.926 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.114 #===END data_Compound_6 _database_code_CSD 204857 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C92.25 H105.25 N O7 P4 S3 Cl0.75 Pd4' _chemical_formula_weight 2012.27 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 13.7471(9) _cell_length_b 15.2582(10) _cell_length_c 23.473(3) _cell_angle_alpha 72.388(5) _cell_angle_beta 85.513(8) _cell_angle_gamma 86.122(5) _cell_volume 4673.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.57 _cell_measurement_theta_max 22.48 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method ? _exptl_crystal_F_000 2053 _exptl_absorpt_coefficient_mu 7.984 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2460 _exptl_absorpt_correction_T_max 0.7042 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14431 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 59.99 _reflns_number_total 13762 _reflns_number_observed 10552 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 923 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+5.7033P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12839 _refine_ls_number_parameters 922 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_obs 0.0536 _refine_ls_wR_factor_all 0.1400 _refine_ls_wR_factor_obs 0.1208 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.111 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.22738(4) 0.73211(3) 0.26898(2) 0.03252(14) Uani 1 d . . Pd2 Pd 0.11051(4) 0.63801(3) 0.21543(2) 0.03103(13) Uani 1 d . . Pd3 Pd 0.27454(4) 0.54736(3) 0.28386(2) 0.03033(13) Uani 1 d . . Pd4 Pd 0.29875(4) 0.69992(3) 0.16608(2) 0.03174(13) Uani 1 d . . S1 S 0.38172(13) 0.67124(12) 0.25642(8) 0.0358(4) Uani 1 d . . S2 S 0.15705(13) 0.73887(12) 0.12419(8) 0.0355(4) Uani 1 d . . S3 S 0.12352(13) 0.50429(13) 0.29580(8) 0.0399(4) Uani 1 d . . P1 P 0.28254(15) 0.80696(12) 0.32959(8) 0.0352(4) Uani 1 d . . P2 P -0.02422(13) 0.59213(13) 0.17859(8) 0.0328(4) Uani 1 d . . P3 P 0.34355(14) 0.41182(12) 0.33890(8) 0.0331(4) Uani 1 d . . P4 P 0.39011(14) 0.72002(13) 0.07757(9) 0.0364(4) Uani 1 d . . O1 O 0.1313(4) 0.8367(4) 0.1134(3) 0.0500(14) Uani 1 d . . O2 O 0.1385(4) 0.7056(4) 0.0736(2) 0.0438(12) Uani 1 d . . O3 O 0.0772(4) 0.5009(5) 0.3553(3) 0.060(2) Uani 1 d . . O4 O 0.1046(4) 0.4213(4) 0.2784(3) 0.054(2) Uani 1 d . . C1 C 0.0943(6) 0.7897(6) 0.2610(4) 0.049(2) Uani 1 d . . N2 N 0.0240(6) 0.8357(5) 0.2537(4) 0.056(2) Uani 1 d . . C3 C -0.0609(8) 0.8994(8) 0.2407(6) 0.071(3) Uani 1 d . . C4 C -0.0241(12) 0.9902(9) 0.2077(8) 0.118(6) Uani 1 d . . H4A H 0.0190(12) 1.0089(9) 0.2323(8) 0.177 Uiso 1 calc R . H4B H -0.0786(12) 1.0348(9) 0.1980(8) 0.177 Uiso 1 calc R . H4C H 0.0116(12) 0.9868(9) 0.1710(8) 0.177 Uiso 1 calc R . C5 C -0.1283(8) 0.8614(9) 0.2087(7) 0.089(4) Uani 1 d . . H5A H -0.1483(8) 0.8016(9) 0.2340(7) 0.133 Uiso 1 calc R . H5B H -0.0952(8) 0.8548(9) 0.1720(7) 0.133 Uiso 1 calc R . H5C H -0.1854(8) 0.9028(9) 0.1990(7) 0.133 Uiso 1 calc R . C6 C -0.1104(11) 0.8993(11) 0.3021(7) 0.113(5) Uani 1 d . . H6A H -0.1339(11) 0.8386(11) 0.3228(7) 0.170 Uiso 1 calc R . H6B H -0.1650(11) 0.9443(11) 0.2962(7) 0.170 Uiso 1 calc R . H6C H -0.0635(11) 0.9149(11) 0.3259(7) 0.170 Uiso 1 calc R . C7 C 0.3583(6) 0.9025(5) 0.2879(4) 0.043(2) Uani 1 d . . H7A H 0.3798(6) 0.9328(5) 0.3157(4) 0.052 Uiso 1 calc R . H7B H 0.4166(6) 0.8780(5) 0.2700(4) 0.052 Uiso 1 calc R . C8 C 0.2904(5) 0.9534(3) 0.1862(3) 0.059(3) Uani 1 d G . H8A H 0.3127(5) 0.8963(3) 0.1814(3) 0.071 Uiso 1 calc R . C9 C 0.2427(6) 1.0181(5) 0.1406(2) 0.087(4) Uani 1 d G . H9A H 0.2328(9) 1.0047(6) 0.1050(3) 0.105 Uiso 1 calc R . C10 C 0.2097(6) 1.1025(4) 0.1477(3) 0.089(4) Uani 1 d G . H10A H 0.1774(8) 1.1462(5) 0.1168(4) 0.107 Uiso 1 calc R . C11 C 0.2244(5) 1.1222(3) 0.2003(3) 0.076(3) Uani 1 d G . H11A H 0.2021(7) 1.1793(4) 0.2051(5) 0.091 Uiso 1 calc R . C12 C 0.2721(5) 1.0575(4) 0.2459(2) 0.057(2) Uani 1 d G . H12A H 0.2821(7) 1.0709(5) 0.2815(3) 0.069 Uiso 1 calc R . C13 C 0.3051(4) 0.9731(3) 0.2388(2) 0.043(2) Uani 1 d G . C14 C 0.1896(7) 0.8620(6) 0.3701(4) 0.050(2) Uani 1 d . . H14A H 0.2236(7) 0.8895(6) 0.3952(4) 0.060 Uiso 1 calc R . H14B H 0.1569(7) 0.9126(6) 0.3404(4) 0.060 Uiso 1 calc R . C15 C 0.0542(8) 0.8422(5) 0.4480(4) 0.119(6) Uani 1 d G . H15A H 0.0678(8) 0.9009(5) 0.4497(4) 0.143 Uiso 1 calc R . C16 C -0.0225(8) 0.7951(7) 0.4838(4) 0.168(10) Uani 1 d G . H16A H -0.0608(11) 0.8219(10) 0.5096(6) 0.202 Uiso 1 calc R . C17 C -0.0426(6) 0.7082(7) 0.4813(4) 0.121(6) Uani 1 d G . H17A H -0.0944(8) 0.6764(9) 0.5055(6) 0.145 Uiso 1 calc R . C18 C 0.0141(6) 0.6686(5) 0.4431(3) 0.077(3) Uani 1 d G . H18A H 0.0005(9) 0.6099(5) 0.4415(5) 0.093 Uiso 1 calc R . C19 C 0.0908(5) 0.7157(4) 0.4074(3) 0.058(2) Uani 1 d G . H19A H 0.1290(7) 0.6889(6) 0.3815(4) 0.070 Uiso 1 calc R . C20 C 0.1108(5) 0.8025(4) 0.4098(3) 0.060(2) Uani 1 d G . C21 C 0.3596(7) 0.7312(5) 0.3878(3) 0.048(2) Uani 1 d D . H21A H 0.3173(7) 0.6867(5) 0.4160(3) 0.057 Uiso 0.75 calc PR 1 H21B H 0.4063(7) 0.6964(5) 0.3683(3) 0.057 Uiso 0.75 calc PR 1 H21C H 0.4217(7) 0.7209(5) 0.3686(3) 0.057 Uiso 0.25 d PR 2 H21D H 0.3296(7) 0.6729(5) 0.4023(3) 0.057 Uiso 0.25 d PR 2 C22 C 0.3792(7) 0.7771(6) 0.4798(3) 0.073(4) Uani 0.75 d PGDU 1 H22A H 0.3174(7) 0.7543(6) 0.4946(3) 0.088 Uiso 0.75 calc PR 1 C23 C 0.4334(9) 0.8131(7) 0.5143(3) 0.088(5) Uani 0.75 d PGU 1 H23A H 0.4083(12) 0.8146(11) 0.5525(4) 0.106 Uiso 0.75 calc PR 1 C24 C 0.5248(9) 0.8467(7) 0.4925(5) 0.098(6) Uani 0.75 d PGU 1 H24A H 0.5615(11) 0.8711(10) 0.5158(6) 0.117 Uiso 0.75 calc PR 1 C25 C 0.5620(6) 0.8444(7) 0.4362(5) 0.094(6) Uani 0.75 d PGU 1 H25A H 0.6238(7) 0.8672(9) 0.4214(7) 0.113 Uiso 0.75 calc PR 1 C26 C 0.5078(6) 0.8084(6) 0.4016(4) 0.075(5) Uani 0.75 d PGD 1 H26A H 0.5329(8) 0.8068(9) 0.3635(4) 0.090 Uiso 0.75 calc PR 1 C27 C 0.4164(6) 0.7747(5) 0.4235(3) 0.050(3) Uani 0.75 d PGD 1 C22' C 0.3054(17) 0.7631(22) 0.4904(5) 0.080(13) Uiso 0.25 d PGD 2 H22B H 0.2442(17) 0.7403(22) 0.4886(5) 0.096 Uiso 0.25 calc PR 2 C23' C 0.3218(19) 0.7988(21) 0.5365(5) 0.110(19) Uiso 0.25 d PG 2 H23B H 0.2717(20) 0.8001(28) 0.5659(6) 0.132 Uiso 0.25 calc PR 2 C24' C 0.4122(22) 0.8325(17) 0.5391(5) 0.120(24) Uiso 0.25 d PG 2 H24B H 0.4233(27) 0.8567(19) 0.5703(6) 0.144 Uiso 0.25 calc PR 2 C25' C 0.4863(21) 0.8305(23) 0.4956(6) 0.052(10) Uiso 0.25 d PG 2 H25B H 0.5475(24) 0.8533(31) 0.4974(7) 0.063 Uiso 0.25 calc PR 2 C26' C 0.4699(16) 0.7948(19) 0.4495(5) 0.144(29) Uiso 0.25 d PGD 2 H26B H 0.5199(15) 0.7935(26) 0.4201(6) 0.173 Uiso 0.25 calc PR 2 C27' C 0.3794(16) 0.7611(14) 0.4469(4) 0.079(17) Uiso 0.25 d PGD 2 C28 C 0.3642(6) 0.8302(6) 0.0200(3) 0.048(2) Uani 1 d G . H28A H 0.2937(7) 0.8443(13) 0.0227(4) 0.057 Uiso 1 calc R . H28B H 0.3963(12) 0.8783(8) 0.0303(4) 0.057 Uiso 1 calc R . C29 C 0.3279(4) 0.8130(4) -0.0778(3) 0.058(2) Uani 1 d G . H29A H 0.2667(4) 0.7918(4) -0.0603(3) 0.070 Uiso 1 calc R . C30 C 0.3526(5) 0.8197(5) -0.1375(3) 0.070(3) Uani 1 d G . H30A H 0.3080(7) 0.8031(7) -0.1604(3) 0.083 Uiso 1 calc R . C31 C 0.4431(6) 0.8511(5) -0.1633(2) 0.076(3) Uani 1 d G . H31A H 0.4598(8) 0.8557(7) -0.2037(2) 0.091 Uiso 1 calc R . C32 C 0.5090(4) 0.8757(5) -0.1294(3) 0.074(3) Uani 1 d G . H32A H 0.5702(5) 0.8969(7) -0.1469(4) 0.089 Uiso 1 calc R . C33 C 0.4843(4) 0.8689(4) -0.0697(3) 0.060(2) Uani 1 d G . H33A H 0.5289(5) 0.8855(6) -0.0468(4) 0.072 Uiso 1 calc R . C34 C 0.3938(4) 0.8375(4) -0.0439(2) 0.047(2) Uani 1 d G . C35 C 0.5232(6) 0.7074(6) 0.0784(4) 0.052(2) Uani 1 d . . H35A H 0.5401(6) 0.6502(6) 0.1095(4) 0.063 Uiso 1 calc R . H35B H 0.5489(6) 0.7002(6) 0.0399(4) 0.063 Uiso 1 calc R . C36 C 0.6473(5) 0.8295(5) 0.0480(3) 0.080(4) Uani 1 d G . H36A H 0.6642(5) 0.8114(5) 0.0135(3) 0.096 Uiso 1 calc R . C37 C 0.6943(5) 0.9011(5) 0.0577(4) 0.101(5) Uani 1 d GU . H37A H 0.7430(7) 0.9315(8) 0.0297(5) 0.122 Uiso 1 calc R . C38 C 0.6692(6) 0.9279(4) 0.1087(4) 0.092(4) Uani 1 d GU . H38A H 0.7010(8) 0.9763(6) 0.1152(6) 0.110 Uiso 1 calc R . C39 C 0.5972(6) 0.8830(5) 0.1501(4) 0.096(4) Uani 1 d G . H39A H 0.5803(9) 0.9011(8) 0.1846(4) 0.115 Uiso 1 calc R . C40 C 0.5502(5) 0.8113(5) 0.1404(3) 0.079(3) Uani 1 d G . H40A H 0.5015(7) 0.7810(7) 0.1684(4) 0.095 Uiso 1 calc R . C41 C 0.5753(4) 0.7846(4) 0.0894(3) 0.053(2) Uani 1 d G . C42 C 0.3628(6) 0.6344(5) 0.0409(3) 0.040(2) Uani 1 d . . H42A H 0.2967(6) 0.6479(5) 0.0267(3) 0.047 Uiso 1 calc R . H42B H 0.4084(6) 0.6403(5) 0.0058(3) 0.047 Uiso 1 calc R . C43 C 0.4487(3) 0.4773(3) 0.0739(2) 0.047(2) Uani 1 d G . H43A H 0.5008(3) 0.5004(3) 0.0462(2) 0.056 Uiso 1 calc R . C44 C 0.4502(3) 0.3849(3) 0.1072(2) 0.055(2) Uani 1 d G . H44A H 0.5034(4) 0.3454(4) 0.1019(4) 0.065 Uiso 1 calc R . C45 C 0.3730(4) 0.3507(2) 0.1481(2) 0.049(2) Uani 1 d G . H45A H 0.3741(5) 0.2882(3) 0.1706(3) 0.058 Uiso 1 calc R . C46 C 0.2944(3) 0.4091(3) 0.1558(2) 0.045(2) Uani 1 d G . H46A H 0.2422(4) 0.3860(4) 0.1835(3) 0.054 Uiso 1 calc R . C47 C 0.2928(3) 0.5016(3) 0.1226(2) 0.040(2) Uani 1 d G . H47A H 0.2396(4) 0.5410(4) 0.1278(3) 0.049 Uiso 1 calc R . C48 C 0.3700(4) 0.5357(2) 0.0816(2) 0.036(2) Uani 1 d G . C49 C -0.0961(5) 0.6850(5) 0.1267(3) 0.038(2) Uani 1 d . . H49A H -0.1487(5) 0.7072(5) 0.1503(3) 0.046 Uiso 1 calc R . H49B H -0.0535(5) 0.7364(5) 0.1083(3) 0.046 Uiso 1 calc R . C50 C -0.0976(3) 0.6861(4) 0.0192(2) 0.045(2) Uani 1 d G . H50A H -0.0403(3) 0.7192(4) 0.0111(2) 0.054 Uiso 1 calc R . C51 C -0.1386(4) 0.6636(4) -0.0266(2) 0.053(2) Uani 1 d G . H51A H -0.1090(5) 0.6815(6) -0.0656(2) 0.064 Uiso 1 calc R . C52 C -0.2234(4) 0.6148(4) -0.0147(2) 0.057(2) Uani 1 d G . H52A H -0.2511(5) 0.5996(6) -0.0456(3) 0.068 Uiso 1 calc R . C53 C -0.2672(3) 0.5884(4) 0.0430(2) 0.053(2) Uani 1 d G . H53A H -0.3245(4) 0.5554(6) 0.0511(3) 0.063 Uiso 1 calc R . C54 C -0.2262(3) 0.6109(4) 0.0887(2) 0.049(2) Uani 1 d G . H54A H -0.2558(5) 0.5931(6) 0.1277(2) 0.059 Uiso 1 calc R . C55 C -0.1414(3) 0.6598(4) 0.0768(2) 0.038(2) Uani 1 d G . C56 C 0.0274(5) 0.5138(5) 0.1370(3) 0.036(2) Uani 1 d . . H56A H 0.0415(5) 0.5516(5) 0.0957(3) 0.043 Uiso 1 calc R . H56B H 0.0906(5) 0.4896(5) 0.1534(3) 0.043 Uiso 1 calc R . C57 C -0.0716(4) 0.4335(3) 0.0821(2) 0.045(2) Uani 1 d G . H57A H -0.0748(4) 0.4886(3) 0.0504(2) 0.054 Uiso 1 calc R . C58 C -0.1112(4) 0.3549(4) 0.0772(2) 0.058(2) Uani 1 d G . H58A H -0.1413(6) 0.3568(5) 0.0422(3) 0.070 Uiso 1 calc R . C59 C -0.1065(5) 0.2734(3) 0.1240(3) 0.069(3) Uani 1 d G . H59A H -0.1333(7) 0.2203(4) 0.1207(4) 0.083 Uiso 1 calc R . C60 C -0.0621(5) 0.2706(3) 0.1758(3) 0.068(3) Uani 1 d G . H60A H -0.0589(8) 0.2155(4) 0.2075(3) 0.081 Uiso 1 calc R . C61 C -0.0224(5) 0.3492(3) 0.1807(2) 0.053(2) Uani 1 d G . H61A H 0.0076(7) 0.3473(5) 0.2157(2) 0.064 Uiso 1 calc R . C62 C -0.0272(4) 0.4307(3) 0.1339(2) 0.037(2) Uani 1 d G . C63 C -0.1171(5) 0.5276(5) 0.2327(4) 0.039(2) Uani 1 d . . H63A H -0.1619(5) 0.5036(5) 0.2112(4) 0.047 Uiso 1 calc R . H63B H -0.0847(5) 0.4748(5) 0.2609(4) 0.047 Uiso 1 calc R . C64 C -0.1345(3) 0.6055(4) 0.3137(2) 0.050(2) Uani 1 d G . H64A H -0.0691(3) 0.5874(4) 0.3219(2) 0.060 Uiso 1 calc R . C65 C -0.1894(4) 0.6545(5) 0.3471(2) 0.063(2) Uani 1 d G . H65A H -0.1612(6) 0.6695(7) 0.3780(3) 0.076 Uiso 1 calc R . C66 C -0.2862(4) 0.6812(5) 0.3351(3) 0.064(3) Uani 1 d G . H66A H -0.3234(5) 0.7143(7) 0.3577(4) 0.077 Uiso 1 calc R . C67 C -0.3280(3) 0.6589(5) 0.2895(3) 0.071(3) Uani 1 d G . H67A H -0.3935(3) 0.6770(7) 0.2813(4) 0.086 Uiso 1 calc R . C68 C -0.2731(4) 0.6100(5) 0.2560(2) 0.061(3) Uani 1 d G . H68A H -0.3014(5) 0.5949(7) 0.2252(3) 0.073 Uiso 1 calc R . C69 C -0.1763(3) 0.5832(4) 0.2681(2) 0.041(2) Uani 1 d G . C70 C 0.3260(7) 0.3200(4) 0.3055(3) 0.044(2) Uani 1 d D . H70A H 0.2620(7) 0.3317(4) 0.2882(3) 0.052 Uiso 0.55 calc PR 1 H70B H 0.3754(7) 0.3254(4) 0.2723(3) 0.052 Uiso 0.55 calc PR 1 H70C H 0.3595(7) 0.3360(4) 0.2665(3) 0.052 Uiso 0.45 d PR 2 H70D H 0.2577(7) 0.3206(4) 0.2996(3) 0.052 Uiso 0.45 d PR 2 C71 C 0.2495(8) 0.1793(7) 0.3790(6) 0.052(4) Uani 0.55 d PGD 1 H71A H 0.1897(8) 0.2133(7) 0.3781(6) 0.062 Uiso 0.55 calc PR 1 C72 C 0.2562(11) 0.0875(7) 0.4134(5) 0.068(6) Uani 0.55 d PG 1 H72A H 0.2010(13) 0.0594(10) 0.4359(7) 0.082 Uiso 0.55 calc PR 1 C73 C 0.3447(12) 0.0373(5) 0.4147(6) 0.066(6) Uani 0.55 d PG 1 H73A H 0.3493(15) -0.0247(5) 0.4380(8) 0.080 Uiso 0.55 calc PR 1 C74 C 0.4265(10) 0.0789(6) 0.3815(6) 0.063(6) Uani 0.55 d PG 1 H74A H 0.4863(11) 0.0450(9) 0.3824(9) 0.075 Uiso 0.55 calc PR 1 C75 C 0.4197(8) 0.1707(7) 0.3471(6) 0.053(4) Uani 0.55 d PGD 1 H75A H 0.4750(9) 0.1988(10) 0.3247(8) 0.063 Uiso 0.55 calc PR 1 C76 C 0.3313(9) 0.2209(5) 0.3458(5) 0.041(4) Uani 0.55 d PGD 1 C71' C 0.2869(11) 0.1687(11) 0.3798(9) 0.060(7) Uiso 0.45 d PGD 2 H71B H 0.2253(11) 0.1953(11) 0.3868(9) 0.072 Uiso 0.45 calc PR 2 C72' C 0.3099(14) 0.0772(10) 0.4102(8) 0.071(9) Uiso 0.45 d PG 2 H72B H 0.2637(18) 0.0419(14) 0.4379(12) 0.086 Uiso 0.45 calc PR 2 C73' C 0.4011(15) 0.0378(9) 0.3998(9) 0.075(9) Uiso 0.45 d PG 2 H73B H 0.4166(21) -0.0241(10) 0.4204(13) 0.089 Uiso 0.45 calc PR 2 C74' C 0.4694(12) 0.0899(11) 0.3590(10) 0.090(11) Uiso 0.45 d PG 2 H74B H 0.5311(15) 0.0633(16) 0.3519(14) 0.108 Uiso 0.45 calc PR 2 C75' C 0.4464(12) 0.1814(11) 0.3285(10) 0.067(8) Uiso 0.45 d PGD 2 H75B H 0.4926(15) 0.2167(15) 0.3008(13) 0.081 Uiso 0.45 calc PR 2 C76' C 0.3552(12) 0.2208(9) 0.3389(9) 0.056(8) Uiso 0.45 d PGD 2 C77 C 0.4745(6) 0.4077(6) 0.3509(4) 0.046(2) Uani 1 d . . H77A H 0.4875(6) 0.4626(6) 0.3621(4) 0.056 Uiso 1 calc R . H77B H 0.4882(6) 0.3542(6) 0.3853(4) 0.056 Uiso 1 calc R . C78 C 0.6284(4) 0.3433(4) 0.3129(2) 0.078(3) Uani 1 d G . H78A H 0.6379(4) 0.3079(4) 0.3527(2) 0.093 Uiso 1 calc R . C79 C 0.6962(4) 0.3361(5) 0.2673(3) 0.087(4) Uani 1 d G . H79A H 0.7516(5) 0.2959(6) 0.2761(4) 0.104 Uiso 1 calc R . C80 C 0.6822(4) 0.3884(5) 0.2085(3) 0.065(3) Uani 1 d G . H80A H 0.7281(5) 0.3835(7) 0.1776(3) 0.078 Uiso 1 calc R . C81 C 0.6003(4) 0.4478(4) 0.1954(2) 0.056(2) Uani 1 d G . H81A H 0.5908(6) 0.4831(6) 0.1556(2) 0.067 Uiso 1 calc R . C82 C 0.5324(3) 0.4550(4) 0.2410(2) 0.047(2) Uani 1 d G . H82A H 0.4770(4) 0.4951(5) 0.2321(3) 0.056 Uiso 1 calc R . C83 C 0.5464(4) 0.4027(4) 0.2998(2) 0.042(2) Uani 1 d G . C84 C 0.2883(6) 0.3674(5) 0.4159(3) 0.040(2) Uani 1 d . . H84A H 0.2181(6) 0.3627(5) 0.4136(3) 0.048 Uiso 1 calc R . H84B H 0.3160(6) 0.3051(5) 0.4339(3) 0.048 Uiso 1 calc R . C85 C 0.3827(4) 0.4048(4) 0.4922(2) 0.054(2) Uani 1 d G . H85A H 0.4296(4) 0.3587(4) 0.4885(2) 0.064 Uiso 1 calc R . C86 C 0.3938(4) 0.4532(4) 0.5326(2) 0.063(3) Uani 1 d G . H86A H 0.4481(5) 0.4399(6) 0.5563(3) 0.075 Uiso 1 calc R . C87 C 0.3245(5) 0.5213(4) 0.5381(2) 0.061(3) Uani 1 d G . H87A H 0.3319(7) 0.5541(6) 0.5655(3) 0.073 Uiso 1 calc R . C88 C 0.2441(4) 0.5411(4) 0.5031(3) 0.066(3) Uani 1 d G . H88A H 0.1973(6) 0.5871(5) 0.5068(4) 0.079 Uiso 1 calc R . C89 C 0.2331(4) 0.4927(4) 0.4627(2) 0.052(2) Uani 1 d G . H89A H 0.1788(5) 0.5060(6) 0.4390(3) 0.062 Uiso 1 calc R . C90 C 0.3024(4) 0.4245(3) 0.4572(2) 0.043(2) Uani 1 d G . O100 O -0.0358(9) 0.3093(6) 0.3556(5) 0.117(4) Uani 1 d . . C101 C -0.1084(13) 0.3491(10) 0.3887(7) 0.115(5) Uani 1 d . . H10B H -0.1276(13) 0.3032(10) 0.4258(7) 0.173 Uiso 1 d R . H10C H -0.1649(13) 0.3708(10) 0.3651(7) 0.173 Uiso 1 d R . H10D H -0.0816(13) 0.4005(10) 0.3975(7) 0.173 Uiso 1 d R . O105 O 0.0209(15) 1.1025(12) 0.3356(8) 0.184(7) Uani 1 d . . C106 C -0.0626(26) 1.1474(19) 0.3371(16) 0.108(10) Uani 0.50 d PU 1 H10E H -0.0900(26) 1.1579(19) 0.2986(16) 0.162 Uiso 0.50 d PR 1 H10F H -0.0507(26) 1.2061(19) 0.3428(16) 0.162 Uiso 0.50 d PR 1 H10G H -0.1081(26) 1.1144(19) 0.3687(16) 0.162 Uiso 0.50 d PR 1 C107 C 0.0030(26) 1.1241(21) 0.3862(15) 0.108(10) Uani 0.50 d P 2 H10H H 0.0628(26) 1.1161(21) 0.4069(15) 0.162 Uiso 0.50 d PR 2 H10I H -0.0459(26) 1.0849(21) 0.4116(15) 0.162 Uiso 0.50 d PR 2 H10J H -0.0208(26) 1.1879(21) 0.3767(15) 0.162 Uiso 0.50 d PR 2 O110 O -0.2104(26) 1.0995(20) 0.3493(16) 0.176(11) Uani 0.50 d PU 1 C111 C -0.3078(29) 1.0484(29) 0.3236(20) 0.155(15) Uani 0.50 d PU 1 H11B H -0.3065(29) 0.9823(29) 0.3423(20) 0.232 Uiso 0.50 d PR 1 H11C H -0.3072(29) 1.0615(29) 0.2805(20) 0.232 Uiso 0.50 d PR 1 H11D H -0.3667(29) 1.0762(29) 0.3377(20) 0.232 Uiso 0.50 d PR 1 O115 O -0.1405(28) 1.0487(22) 0.4492(13) 0.176(11) Uani 0.50 d PU 2 C116 C -0.2477(33) 1.0750(31) 0.4224(20) 0.158(16) Uani 0.50 d PU 2 H11E H -0.2757(33) 1.1352(31) 0.4017(20) 0.238 Uiso 0.50 d PR 2 H11F H -0.2954(33) 1.0413(31) 0.4523(20) 0.238 Uiso 0.50 d PR 2 H11G H -0.2295(33) 1.0413(31) 0.3939(20) 0.238 Uiso 0.50 d PR 2 C120 C 0.9683(35) 1.0317(31) -0.0090(22) 0.074(11) Uiso 0.25 d P . Cl1 Cl 1.0627(9) 1.0735(6) 0.0009(6) 0.159(4) Uani 0.50 d PU . Cl2 Cl 0.9004(10) 1.0571(9) 0.0486(6) 0.090(3) Uiso 0.25 d P . 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 0.0351(3) 0.0302(3) 0.0355(3) -0.0144(2) -0.0052(2) 0.0014(2) Pd2 0.0292(2) 0.0333(3) 0.0311(3) -0.0100(2) -0.0021(2) -0.0029(2) Pd3 0.0311(3) 0.0265(2) 0.0319(3) -0.0065(2) -0.0021(2) -0.0006(2) Pd4 0.0318(3) 0.0331(3) 0.0311(3) -0.0104(2) -0.0005(2) -0.0045(2) S1 0.0333(8) 0.0355(9) 0.0404(10) -0.0134(7) -0.0047(7) -0.0025(7) S2 0.0370(9) 0.0338(9) 0.0340(9) -0.0071(7) -0.0041(7) -0.0029(7) S3 0.0340(9) 0.0437(10) 0.0356(10) -0.0015(8) -0.0028(7) -0.0052(8) P1 0.0479(10) 0.0276(8) 0.0322(9) -0.0114(7) -0.0058(8) -0.0018(8) P2 0.0296(8) 0.0366(9) 0.0334(9) -0.0119(8) -0.0017(7) -0.0030(7) P3 0.0387(9) 0.0288(9) 0.0285(9) -0.0044(7) -0.0004(7) 0.0002(7) P4 0.0348(9) 0.0357(9) 0.0377(10) -0.0095(8) 0.0021(8) -0.0058(7) O1 0.058(3) 0.035(3) 0.054(4) -0.009(3) -0.012(3) 0.007(3) O2 0.044(3) 0.054(3) 0.032(3) -0.010(2) -0.002(2) -0.005(3) O3 0.046(3) 0.085(5) 0.035(3) -0.001(3) 0.005(3) 0.000(3) O4 0.054(3) 0.038(3) 0.066(4) -0.003(3) -0.015(3) -0.011(3) C1 0.045(5) 0.053(5) 0.051(5) -0.018(4) -0.005(4) -0.002(4) N2 0.049(4) 0.052(4) 0.071(5) -0.026(4) -0.013(4) 0.011(4) C3 0.058(6) 0.068(6) 0.100(9) -0.046(6) -0.019(6) 0.025(5) C4 0.112(12) 0.059(7) 0.172(17) -0.010(9) -0.044(12) 0.003(7) C5 0.060(6) 0.095(9) 0.118(11) -0.039(8) -0.035(7) 0.021(6) C6 0.095(10) 0.126(13) 0.128(13) -0.067(11) 0.017(9) 0.040(9) C7 0.052(4) 0.031(4) 0.047(5) -0.010(3) -0.008(4) -0.017(3) C8 0.088(7) 0.037(4) 0.048(5) -0.002(4) -0.016(5) -0.016(5) C9 0.124(11) 0.072(7) 0.060(7) 0.002(6) -0.025(7) -0.041(7) C10 0.095(9) 0.059(7) 0.089(9) 0.025(6) -0.038(7) -0.019(6) C11 0.078(7) 0.037(5) 0.096(9) 0.005(5) -0.013(7) -0.002(5) C12 0.070(6) 0.037(4) 0.064(6) -0.014(4) -0.004(5) -0.008(4) C13 0.049(4) 0.031(4) 0.045(5) -0.005(3) -0.003(4) -0.007(3) C14 0.066(5) 0.043(4) 0.043(5) -0.018(4) 0.003(4) -0.001(4) C15 0.177(17) 0.105(11) 0.075(9) -0.043(8) 0.070(10) -0.024(11) C16 0.196(22) 0.170(19) 0.151(18) -0.086(16) 0.114(17) -0.058(17) C17 0.122(13) 0.137(14) 0.086(10) -0.015(10) 0.051(10) -0.029(11) C18 0.074(7) 0.099(9) 0.051(6) -0.011(6) 0.006(5) -0.017(6) C19 0.059(5) 0.060(6) 0.047(5) -0.004(4) 0.003(4) -0.006(4) C20 0.080(7) 0.064(6) 0.031(4) -0.009(4) 0.001(4) 0.000(5) C21 0.073(6) 0.028(4) 0.042(5) -0.007(3) -0.020(4) 0.008(4) C22 0.135(12) 0.044(6) 0.047(7) -0.020(6) -0.027(8) 0.014(7) C23 0.149(15) 0.067(9) 0.046(7) -0.018(7) -0.031(9) 0.038(10) C24 0.115(10) 0.076(8) 0.105(10) -0.025(7) -0.034(8) -0.008(8) C25 0.107(11) 0.051(7) 0.128(13) -0.018(8) -0.070(10) -0.001(7) C26 0.095(11) 0.038(6) 0.096(11) -0.014(7) -0.062(10) 0.004(7) C27 0.094(10) 0.019(5) 0.037(6) -0.004(4) -0.032(7) 0.013(5) C28 0.044(4) 0.042(4) 0.046(5) 0.001(4) 0.001(4) -0.002(4) C29 0.061(6) 0.052(5) 0.054(6) -0.002(4) -0.001(5) -0.007(4) C30 0.096(8) 0.062(6) 0.048(6) -0.010(5) -0.014(6) -0.002(6) C31 0.108(9) 0.060(6) 0.049(6) -0.006(5) 0.013(6) 0.002(6) C32 0.090(8) 0.058(6) 0.064(7) -0.011(5) 0.034(6) -0.014(6) C33 0.062(6) 0.048(5) 0.057(6) 0.000(4) 0.010(5) -0.015(4) C34 0.050(5) 0.033(4) 0.052(5) -0.004(4) 0.005(4) -0.004(3) C35 0.042(4) 0.048(5) 0.064(6) -0.016(4) 0.013(4) -0.007(4) C36 0.055(6) 0.077(7) 0.090(9) 0.008(6) -0.001(6) -0.022(6) C37 0.083(8) 0.086(8) 0.115(10) 0.011(7) -0.019(8) -0.039(7) C38 0.085(8) 0.057(6) 0.124(10) 0.003(6) -0.047(8) -0.025(6) C39 0.104(10) 0.078(8) 0.120(11) -0.041(8) -0.030(9) -0.024(8) C40 0.069(7) 0.089(8) 0.087(8) -0.028(7) -0.009(6) -0.036(6) C41 0.037(4) 0.049(5) 0.064(6) -0.002(4) -0.008(4) -0.005(4) C42 0.047(4) 0.041(4) 0.033(4) -0.017(3) 0.010(3) -0.008(3) C43 0.042(4) 0.058(5) 0.041(5) -0.018(4) 0.003(4) -0.006(4) C44 0.060(5) 0.056(5) 0.048(5) -0.017(4) -0.002(4) 0.002(4) C45 0.056(5) 0.048(5) 0.040(5) -0.011(4) -0.007(4) 0.003(4) C46 0.055(5) 0.049(4) 0.033(4) -0.014(3) -0.003(4) -0.010(4) C47 0.048(4) 0.040(4) 0.035(4) -0.013(3) 0.000(3) -0.002(3) C48 0.044(4) 0.037(4) 0.027(4) -0.009(3) 0.001(3) -0.009(3) C49 0.035(4) 0.042(4) 0.041(4) -0.018(3) -0.006(3) 0.001(3) C50 0.042(4) 0.045(4) 0.047(5) -0.016(4) -0.001(4) 0.008(3) C51 0.063(5) 0.058(5) 0.037(5) -0.014(4) -0.002(4) 0.013(4) C52 0.056(5) 0.076(6) 0.051(5) -0.036(5) -0.019(4) 0.013(5) C53 0.032(4) 0.081(6) 0.056(5) -0.036(5) -0.008(4) 0.000(4) C54 0.036(4) 0.061(5) 0.059(5) -0.029(4) -0.008(4) 0.002(4) C55 0.035(4) 0.041(4) 0.041(4) -0.018(3) -0.002(3) 0.006(3) C56 0.034(4) 0.033(4) 0.043(4) -0.014(3) -0.002(3) -0.005(3) C57 0.040(4) 0.045(4) 0.055(5) -0.023(4) 0.000(4) 0.002(3) C58 0.050(5) 0.065(6) 0.075(7) -0.041(5) -0.013(5) -0.002(4) C59 0.080(7) 0.058(6) 0.080(7) -0.032(6) -0.010(6) -0.017(5) C60 0.089(7) 0.037(5) 0.072(7) -0.008(4) 0.002(6) -0.016(5) C61 0.066(6) 0.038(4) 0.051(5) -0.007(4) -0.007(4) -0.001(4) C62 0.031(3) 0.040(4) 0.044(4) -0.021(3) -0.004(3) 0.001(3) C63 0.032(4) 0.044(4) 0.043(4) -0.015(3) 0.003(3) -0.008(3) C64 0.050(5) 0.061(5) 0.041(5) -0.016(4) -0.003(4) -0.002(4) C65 0.063(6) 0.074(6) 0.057(6) -0.030(5) 0.004(5) 0.003(5) C66 0.050(5) 0.088(7) 0.054(6) -0.028(5) 0.013(4) 0.012(5) C67 0.037(5) 0.102(8) 0.080(8) -0.039(7) 0.004(5) 0.008(5) C68 0.033(4) 0.095(7) 0.064(6) -0.038(6) 0.003(4) -0.002(4) C69 0.032(4) 0.047(4) 0.042(4) -0.012(4) 0.008(3) -0.004(3) C70 0.069(5) 0.030(4) 0.032(4) -0.009(3) -0.006(4) 0.005(4) C71 0.056(11) 0.041(9) 0.058(11) -0.018(7) 0.013(9) -0.001(8) C72 0.104(19) 0.044(10) 0.060(12) -0.019(8) 0.003(11) -0.027(11) C73 0.104(18) 0.045(10) 0.064(12) -0.030(9) -0.057(13) 0.022(11) C74 0.092(16) 0.032(9) 0.068(13) -0.014(9) -0.037(14) 0.012(10) C75 0.078(13) 0.038(9) 0.047(11) -0.019(7) -0.024(10) 0.023(8) C76 0.071(11) 0.020(7) 0.033(8) -0.009(6) -0.013(8) 0.001(7) C77 0.045(4) 0.060(5) 0.031(4) -0.010(4) -0.006(3) 0.010(4) C78 0.051(6) 0.086(8) 0.067(7) 0.010(6) 0.011(5) 0.024(5) C79 0.057(6) 0.084(8) 0.099(10) -0.009(7) 0.021(6) 0.022(6) C80 0.055(5) 0.078(7) 0.066(7) -0.031(5) 0.022(5) -0.014(5) C81 0.044(5) 0.066(6) 0.055(6) -0.019(5) 0.002(4) -0.003(4) C82 0.043(4) 0.053(5) 0.041(5) -0.009(4) 0.001(4) 0.002(4) C83 0.037(4) 0.042(4) 0.047(5) -0.013(4) 0.000(3) 0.002(3) C84 0.053(4) 0.033(4) 0.030(4) -0.004(3) 0.005(3) -0.008(3) C85 0.064(6) 0.057(5) 0.038(5) -0.010(4) -0.001(4) -0.007(4) C86 0.076(7) 0.076(7) 0.037(5) -0.013(5) -0.009(5) -0.017(5) C87 0.092(7) 0.052(5) 0.040(5) -0.016(4) -0.002(5) -0.009(5) C88 0.094(8) 0.051(5) 0.046(5) -0.012(4) -0.001(5) 0.016(5) C89 0.065(5) 0.051(5) 0.039(5) -0.014(4) -0.006(4) 0.002(4) C90 0.051(4) 0.040(4) 0.032(4) -0.003(3) 0.006(3) -0.009(4) O100 0.159(10) 0.076(6) 0.111(8) -0.027(5) 0.056(7) -0.052(6) C101 0.138(14) 0.092(10) 0.104(12) -0.017(9) 0.038(11) -0.026(10) O105 0.225(19) 0.185(15) 0.166(15) -0.091(13) -0.032(14) 0.018(14) C106 0.124(22) 0.071(15) 0.137(24) -0.035(16) -0.062(20) 0.014(15) C107 0.124(26) 0.092(20) 0.106(24) -0.034(18) 0.004(20) 0.014(18) O110 0.193(20) 0.141(16) 0.219(20) -0.095(15) -0.026(16) 0.029(14) C111 0.129(20) 0.147(21) 0.166(22) -0.026(17) 0.007(17) 0.027(16) O115 0.215(20) 0.166(18) 0.136(17) -0.026(14) 0.001(16) -0.037(16) C116 0.152(22) 0.169(22) 0.126(21) -0.008(16) 0.022(17) -0.009(17) Cl1 0.175(9) 0.087(5) 0.190(10) 0.015(5) -0.074(8) -0.030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.972(9) . ? Pd1 P1 2.274(2) . ? Pd1 S1 2.292(2) . ? Pd1 Pd4 2.7056(8) . ? Pd1 Pd3 2.7715(7) . ? Pd1 Pd2 2.8184(7) . ? Pd2 S2 2.300(2) . ? Pd2 S3 2.330(2) . ? Pd2 P2 2.337(2) . ? Pd2 Pd4 2.8514(7) . ? Pd2 Pd3 2.8946(7) . ? Pd3 S3 2.192(2) . ? Pd3 P3 2.271(2) . ? Pd3 S1 2.377(2) . ? Pd3 Pd4 3.0397(8) . ? Pd4 S2 2.214(2) . ? Pd4 P4 2.290(2) . ? Pd4 S1 2.396(2) . ? S2 O1 1.460(6) . ? S2 O2 1.471(5) . ? S3 O3 1.477(6) . ? S3 O4 1.488(6) . ? P1 C7 1.830(7) . ? P1 C14 1.841(9) . ? P1 C21 1.851(8) . ? P2 C56 1.835(7) . ? P2 C63 1.837(8) . ? P2 C49 1.850(8) . ? P3 C70 1.837(7) . ? P3 C77 1.838(8) . ? P3 C84 1.848(7) . ? P4 C35 1.827(9) . ? P4 C42 1.840(7) . ? P4 C28 1.844(8) . ? C1 N2 1.148(11) . ? N2 C3 1.457(12) . ? C3 C4 1.47(2) . ? C3 C5 1.486(15) . ? C3 C6 1.55(2) . ? C7 C13 1.515(9) . ? C8 C9 1.39 . ? C8 C13 1.39 . ? C9 C10 1.39 . ? C10 C11 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C14 C20 1.527(10) . ? C15 C16 1.39 . ? C15 C20 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C21 C27 1.504(8) . ? C21 C27' 1.633(10) . ? C22 C23 1.39 . ? C22 C27 1.39 . ? C23 C24 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C22' C23' 1.39 . ? C22' C27' 1.39 . ? C23' C24' 1.39 . ? C24' C25' 1.39 . ? C25' C26' 1.39 . ? C26' C27' 1.39 . ? C28 C34 1.495(9) . ? C29 C30 1.39 . ? C29 C34 1.39 . ? C30 C31 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C35 C41 1.514(9) . ? C36 C37 1.39 . ? C36 C41 1.39 . ? C37 C38 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C42 C48 1.523(8) . ? C43 C44 1.39 . ? C43 C48 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C49 C55 1.526(7) . ? C50 C51 1.39 . ? C50 C55 1.39 . ? C51 C52 1.39 . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C56 C62 1.540(7) . ? C57 C58 1.39 . ? C57 C62 1.39 . ? C58 C59 1.39 . ? C59 C60 1.39 . ? C60 C61 1.39 . ? C61 C62 1.39 . ? C63 C69 1.516(8) . ? C64 C65 1.39 . ? C64 C69 1.39 . ? C65 C66 1.39 . ? C66 C67 1.39 . ? C67 C68 1.39 . ? C68 C69 1.39 . ? C70 C76' 1.522(11) . ? C70 C76 1.523(9) . ? C71 C72 1.39 . ? C71 C76 1.39 . ? C72 C73 1.39 . ? C73 C74 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? C71' C72' 1.39 . ? C71' C76' 1.39 . ? C72' C73' 1.39 . ? C73' C74' 1.39 . ? C74' C75' 1.39 . ? C75' C76' 1.39 . ? C77 C83 1.511(9) . ? C78 C79 1.39 . ? C78 C83 1.39 . ? C79 C80 1.39 . ? C80 C81 1.39 . ? C81 C82 1.39 . ? C82 C83 1.39 . ? C84 C90 1.517(8) . ? C85 C86 1.39 . ? C85 C90 1.39 . ? C86 C87 1.39 . ? C87 C88 1.39 . ? C88 C89 1.39 . ? C89 C90 1.39 . ? O100 C101 1.43(2) . ? O105 C106 1.30(3) . ? O105 C107 1.33(3) . ? O110 C111 1.82(5) . ? O115 C116 1.63(5) . ? C120 C120 1.25(9) 2_775 ? C120 Cl1 1.55(5) . ? C120 Cl1 1.64(5) 2_775 ? C120 Cl2 1.71(5) . ? Cl1 C120 1.64(5) 2_775 ? Cl1 Cl2 2.41(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 98.3(2) . . ? C1 Pd1 S1 167.7(3) . . ? P1 Pd1 S1 90.42(7) . . ? C1 Pd1 Pd4 111.3(3) . . ? P1 Pd1 Pd4 134.11(6) . . ? S1 Pd1 Pd4 56.56(5) . . ? C1 Pd1 Pd3 125.2(2) . . ? P1 Pd1 Pd3 121.84(5) . . ? S1 Pd1 Pd3 55.02(4) . . ? Pd4 Pd1 Pd3 67.41(2) . . ? C1 Pd1 Pd2 69.5(2) . . ? P1 Pd1 Pd2 163.63(6) . . ? S1 Pd1 Pd2 103.43(5) . . ? Pd4 Pd1 Pd2 62.11(2) . . ? Pd3 Pd1 Pd2 62.37(2) . . ? S2 Pd2 S3 155.37(7) . . ? S2 Pd2 P2 93.37(6) . . ? S3 Pd2 P2 94.62(7) . . ? S2 Pd2 Pd1 88.02(5) . . ? S3 Pd2 Pd1 91.54(5) . . ? P2 Pd2 Pd1 161.80(5) . . ? S2 Pd2 Pd4 49.51(5) . . ? S3 Pd2 Pd4 110.95(5) . . ? P2 Pd2 Pd4 134.89(5) . . ? Pd1 Pd2 Pd4 57.00(2) . . ? S2 Pd2 Pd3 113.03(5) . . ? S3 Pd2 Pd3 48.12(5) . . ? P2 Pd2 Pd3 136.35(5) . . ? Pd1 Pd2 Pd3 58.02(2) . . ? Pd4 Pd2 Pd3 63.87(2) . . ? S3 Pd3 P3 97.18(7) . . ? S3 Pd3 S1 147.37(7) . . ? P3 Pd3 S1 113.88(7) . . ? S3 Pd3 Pd1 95.86(6) . . ? P3 Pd3 Pd1 149.02(5) . . ? S1 Pd3 Pd1 52.18(5) . . ? S3 Pd3 Pd2 52.33(5) . . ? P3 Pd3 Pd2 146.36(5) . . ? S1 Pd3 Pd2 99.06(5) . . ? Pd1 Pd3 Pd2 59.61(2) . . ? S3 Pd3 Pd4 108.68(5) . . ? P3 Pd3 Pd4 142.82(5) . . ? S1 Pd3 Pd4 50.71(4) . . ? Pd1 Pd3 Pd4 55.26(2) . . ? Pd2 Pd3 Pd4 57.37(2) . . ? S2 Pd4 P4 95.17(7) . . ? S2 Pd4 S1 145.32(7) . . ? P4 Pd4 S1 118.59(7) . . ? S2 Pd4 Pd1 92.68(5) . . ? P4 Pd4 Pd1 158.52(5) . . ? S1 Pd4 Pd1 52.97(5) . . ? S2 Pd4 Pd2 52.17(5) . . ? P4 Pd4 Pd2 137.89(5) . . ? S1 Pd4 Pd2 99.81(5) . . ? Pd1 Pd4 Pd2 60.89(2) . . ? S2 Pd4 Pd3 110.58(5) . . ? P4 Pd4 Pd3 136.32(5) . . ? S1 Pd4 Pd3 50.17(4) . . ? Pd1 Pd4 Pd3 57.33(2) . . ? Pd2 Pd4 Pd3 58.75(2) . . ? Pd1 S1 Pd3 72.80(5) . . ? Pd1 S1 Pd4 70.47(5) . . ? Pd3 S1 Pd4 79.12(5) . . ? O1 S2 O2 113.0(3) . . ? O1 S2 Pd4 111.6(2) . . ? O2 S2 Pd4 118.6(2) . . ? O1 S2 Pd2 118.5(3) . . ? O2 S2 Pd2 112.8(2) . . ? Pd4 S2 Pd2 78.32(6) . . ? O3 S3 O4 111.9(4) . . ? O3 S3 Pd3 113.0(3) . . ? O4 S3 Pd3 117.0(3) . . ? O3 S3 Pd2 120.5(3) . . ? O4 S3 Pd2 111.5(3) . . ? Pd3 S3 Pd2 79.55(6) . . ? C7 P1 C14 103.0(4) . . ? C7 P1 C21 105.8(4) . . ? C14 P1 C21 105.5(4) . . ? C7 P1 Pd1 112.0(3) . . ? C14 P1 Pd1 116.9(3) . . ? C21 P1 Pd1 112.7(2) . . ? C56 P2 C63 105.8(3) . . ? C56 P2 C49 107.7(3) . . ? C63 P2 C49 103.7(4) . . ? C56 P2 Pd2 104.8(2) . . ? C63 P2 Pd2 118.2(3) . . ? C49 P2 Pd2 115.9(2) . . ? C70 P3 C77 106.5(4) . . ? C70 P3 C84 103.6(3) . . ? C77 P3 C84 102.7(4) . . ? C70 P3 Pd3 110.5(2) . . ? C77 P3 Pd3 117.8(3) . . ? C84 P3 Pd3 114.5(3) . . ? C35 P4 C42 101.9(4) . . ? C35 P4 C28 105.4(4) . . ? C42 P4 C28 102.8(4) . . ? C35 P4 Pd4 119.3(3) . . ? C42 P4 Pd4 111.1(2) . . ? C28 P4 Pd4 114.5(3) . . ? N2 C1 Pd1 169.5(8) . . ? C1 N2 C3 175.5(11) . . ? N2 C3 C4 106.8(10) . . ? N2 C3 C5 107.6(8) . . ? C4 C3 C5 115.8(12) . . ? N2 C3 C6 105.9(10) . . ? C4 C3 C6 111.3(12) . . ? C5 C3 C6 108.8(12) . . ? C13 C7 P1 112.8(5) . . ? C9 C8 C13 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 C7 120.5(5) . . ? C8 C13 C7 119.5(5) . . ? C20 C14 P1 118.1(6) . . ? C16 C15 C20 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 C14 124.1(5) . . ? C15 C20 C14 115.8(5) . . ? C27 C21 P1 118.4(5) . . ? C27' C21 P1 120.1(8) . . ? C23 C22 C27 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 C21 120.3(6) . . ? C22 C27 C21 119.6(6) . . ? C23' C22' C27' 120.0 . . ? C22' C23' C24' 120.0 . . ? C23' C24' C25' 120.0 . . ? C26' C25' C24' 120.0 . . ? C27' C26' C25' 120.0 . . ? C26' C27' C22' 120.0 . . ? C26' C27' C21 118.1(8) . . ? C22' C27' C21 121.5(8) . . ? C34 C28 P4 118.2(6) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 C28 121.6(5) . . ? C29 C34 C28 118.4(5) . . ? C41 C35 P4 117.0(6) . . ? C37 C36 C41 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 C35 120.1(5) . . ? C36 C41 C35 119.9(5) . . ? C48 C42 P4 113.5(5) . . ? C44 C43 C48 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 C42 119.5(4) . . ? C43 C48 C42 120.1(4) . . ? C55 C49 P2 116.3(5) . . ? C51 C50 C55 120.0 . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 C49 120.4(4) . . ? C50 C55 C49 119.6(4) . . ? C62 C56 P2 122.3(5) . . ? C58 C57 C62 120.0 . . ? C57 C58 C59 120.0 . . ? C60 C59 C58 120.0 . . ? C61 C60 C59 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C57 120.0 . . ? C61 C62 C56 119.2(4) . . ? C57 C62 C56 120.4(4) . . ? C69 C63 P2 114.5(5) . . ? C65 C64 C69 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C67 120.0 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C68 C69 C64 120.0 . . ? C68 C69 C63 120.0(4) . . ? C64 C69 C63 119.9(4) . . ? C76' C70 P3 119.6(11) . . ? C76 C70 P3 117.9(7) . . ? C72 C71 C76 120.0 . . ? C71 C72 C73 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 C70 118.3(7) . . ? C71 C76 C70 121.7(7) . . ? C72' C71' C76' 120.0 . . ? C71' C72' C73' 120.0 . . ? C74' C73' C72' 120.0 . . ? C73' C74' C75' 120.0 . . ? C74' C75' C76' 120.0 . . ? C75' C76' C71' 120.0 . . ? C75' C76' C70 121.8(9) . . ? C71' C76' C70 118.2(9) . . ? C83 C77 P3 118.0(5) . . ? C79 C78 C83 120.0 . . ? C78 C79 C80 120.0 . . ? C79 C80 C81 120.0 . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C82 C83 C78 120.0 . . ? C82 C83 C77 121.9(5) . . ? C78 C83 C77 118.1(5) . . ? C90 C84 P3 115.6(5) . . ? C86 C85 C90 120.0 . . ? C87 C86 C85 120.0 . . ? C86 C87 C88 120.0 . . ? C89 C88 C87 120.0 . . ? C88 C89 C90 120.0 . . ? C89 C90 C85 120.0 . . ? C89 C90 C84 120.6(5) . . ? C85 C90 C84 119.3(5) . . ? C120 C120 Cl1 70.8(41) 2_775 . ? C120 C120 Cl1 63.0(38) 2_775 2_775 ? Cl1 C120 Cl1 133.8(31) . 2_775 ? C120 C120 Cl2 112.4(55) 2_775 . ? Cl1 C120 Cl2 95.3(26) . . ? Cl1 C120 Cl2 101.8(27) 2_775 . ? C120 Cl1 C120 46.2(31) . 2_775 ? C120 Cl1 Cl2 44.9(19) . . ? C120 Cl1 Cl2 72.6(18) 2_775 . ? C120 Cl2 Cl1 39.8(16) . . ? _refine_diff_density_max 1.071 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.111 #===END data_Compound_7 _database_code_CSD 204858 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C92.50 H101 N O5.50 P4 S3 Pd4' _chemical_formula_weight 1960.40 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 13.822(3) _cell_length_b 15.464(4) _cell_length_c 23.567(7) _cell_angle_alpha 71.32(2) _cell_angle_beta 85.57(2) _cell_angle_gamma 87.920(14) _cell_volume 4757.3(20) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 11.11 _cell_measurement_theta_max 27.83 _exptl_crystal_description rhombs _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method ? _exptl_crystal_F_000 1998 _exptl_absorpt_coefficient_mu 7.628 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0465 _exptl_absorpt_correction_T_max 0.4643 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14632 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 60.00 _reflns_number_total 13957 _reflns_number_observed 8535 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1596 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00134(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12361 _refine_ls_number_parameters 901 _refine_ls_number_restraints 148 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_obs 0.0890 _refine_ls_wR_factor_all 0.2663 _refine_ls_wR_factor_obs 0.2158 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.078 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.76751(9) 0.76845(6) 0.23250(4) 0.0633(3) Uani 1 d . . Pd2 Pd 0.88484(8) 0.86134(6) 0.28604(4) 0.0616(3) Uani 1 d . . Pd3 Pd 0.69633(8) 0.79664(6) 0.33630(4) 0.0628(3) Uani 1 d . . Pd4 Pd 0.72260(8) 0.95066(6) 0.21710(4) 0.0627(3) Uani 1 d . . S1 S 0.6137(3) 0.8244(2) 0.2461(2) 0.0687(9) Uani 1 d . . S2 S 0.8743(3) 0.9948(2) 0.2048(2) 0.0723(9) Uani 1 d . . O1 O 0.9200(10) 0.9994(9) 0.1455(5) 0.101(4) Uani 1 d . . O2 O 0.8929(9) 1.0770(6) 0.2215(5) 0.092(3) Uani 1 d . . S3 S 0.8359(3) 0.7602(2) 0.37851(13) 0.0651(8) Uani 1 d . . O3 O 0.8594(10) 0.6621(6) 0.3926(5) 0.091(3) Uani 1 d . . O4 O 0.8557(9) 0.7941(7) 0.4295(4) 0.084(3) Uani 1 d . . P1 P 0.7135(3) 0.6930(2) 0.17204(15) 0.0670(10) Uani 1 d . . P2 P 1.0219(3) 0.9064(2) 0.3220(2) 0.0655(9) Uani 1 d . . P3 P 0.6031(3) 0.7778(2) 0.4244(2) 0.0685(9) Uani 1 d . . P4 P 0.6580(3) 1.0856(2) 0.1609(2) 0.0674(9) Uani 1 d . . C1 C 0.9006(13) 0.7244(11) 0.2364(7) 0.076(4) Uani 1 d . . N1 N 0.9733(15) 0.6865(11) 0.2409(8) 0.113(6) Uani 1 d . . C2 C 1.0835(35) 0.6444(31) 0.2425(21) 0.229(10) Uani 1 d U . H2A H 1.1378(35) 0.6838(31) 0.2418(21) 0.275 Uiso 1 calc R . C3 C 1.0824(33) 0.6021(31) 0.1962(20) 0.234(11) Uani 1 d U . H3A H 1.0649(33) 0.6455(31) 0.1584(20) 0.281 Uiso 1 calc R . H3B H 1.0384(33) 0.5510(31) 0.2077(20) 0.281 Uiso 1 calc R . C4 C 1.1941(35) 0.5690(32) 0.1927(21) 0.251(11) Uani 1 d U . H4A H 1.2394(35) 0.6117(32) 0.1981(21) 0.301 Uiso 1 calc R . H4B H 1.2129(35) 0.5539(32) 0.1564(21) 0.301 Uiso 1 calc R . C5 C 1.1765(35) 0.4787(32) 0.2523(21) 0.246(11) Uani 1 d U . H5A H 1.1153(35) 0.4504(32) 0.2516(21) 0.296 Uiso 1 calc R . H5B H 1.2284(35) 0.4343(32) 0.2540(21) 0.296 Uiso 1 calc R . C6 C 1.1751(35) 0.5123(33) 0.3045(21) 0.248(11) Uani 1 d U . H6A H 1.2213(35) 0.5609(33) 0.2982(21) 0.298 Uiso 1 calc R . H6B H 1.1874(35) 0.4636(33) 0.3413(21) 0.298 Uiso 1 calc R . C7 C 1.0607(34) 0.5504(32) 0.3048(21) 0.248(11) Uani 1 d U . H7A H 1.0403(34) 0.5663(32) 0.3405(21) 0.297 Uiso 1 calc R . H7B H 1.0150(34) 0.5089(32) 0.2984(21) 0.297 Uiso 1 calc R . C8 C 0.8044(13) 0.6467(9) 0.1283(7) 0.082(4) Uani 1 d D . H8A H 0.8347(13) 0.5943(9) 0.1561(7) 0.098 Uiso 0.65 calc PR 1 H8B H 0.7698(13) 0.6240(9) 0.1017(7) 0.098 Uiso 0.65 calc PR 1 H8C H 0.7726(13) 0.6049(9) 0.1134(7) 0.098 Uiso 0.35 d PR 2 H8D H 0.8503(13) 0.6120(9) 0.1556(7) 0.098 Uiso 0.35 d PR 2 C9 C 0.9012(19) 0.7962(14) 0.0892(9) 0.075(9) Uani 0.65 d PG 1 H9A H 0.8599(19) 0.8227(14) 0.1122(9) 0.090 Uiso 0.65 calc PR 1 C10 C 0.9787(23) 0.8452(14) 0.0539(12) 0.145(35) Uani 0.65 d PG 1 H10A H 0.9893(32) 0.9046(16) 0.0533(18) 0.174 Uiso 0.65 calc PR 1 C11 C 1.0405(19) 0.8056(21) 0.0196(12) 0.160(17) Uani 0.65 d PG 1 H11A H 1.0923(25) 0.8384(28) -0.0040(17) 0.192 Uiso 0.65 calc PR 1 C12 C 1.0247(19) 0.7168(22) 0.0206(12) 0.168(20) Uani 0.65 d PG 1 H12A H 1.0660(25) 0.6903(29) -0.0024(16) 0.201 Uiso 0.65 calc PR 1 C13 C 0.9472(21) 0.6677(16) 0.0559(12) 0.140(16) Uani 0.65 d PG 1 H13A H 0.9367(31) 0.6084(18) 0.0565(18) 0.168 Uiso 0.65 calc PR 1 C14 C 0.8855(18) 0.7074(15) 0.0902(10) 0.091(10) Uani 0.65 d PG 1 C9' C 0.9160(50) 0.7810(46) 0.0919(24) 0.117(33) Uiso 0.35 d PGD 2 H9'A H 0.9108(50) 0.7815(46) 0.1314(24) 0.140 Uiso 0.35 calc PR 2 C10' C 0.9732(49) 0.8451(39) 0.0486(35) 0.122(48) Uiso 0.35 d PGD 2 H10B H 1.0061(67) 0.8885(50) 0.0591(48) 0.146 Uiso 0.35 calc PR 2 C11' C 0.9810(40) 0.8444(36) -0.0104(30) 0.174(37) Uiso 0.35 d PGD 2 H11B H 1.0193(47) 0.8873(44) -0.0394(39) 0.209 Uiso 0.35 calc PR 2 C12' C 0.9318(49) 0.7795(46) -0.0261(24) 0.190(39) Uiso 0.35 d PGD 2 H12B H 0.9370(69) 0.7790(65) -0.0656(25) 0.228 Uiso 0.35 calc PR 2 C13' C 0.8746(41) 0.7154(38) 0.0172(32) 0.152(29) Uiso 0.35 d PGD 2 H13B H 0.8417(56) 0.6720(49) 0.0067(44) 0.182 Uiso 0.35 calc PR 2 C14' C 0.8668(31) 0.7162(35) 0.0762(28) 0.114(29) Uiso 0.35 d PGD 2 C15 C 0.6293(15) 0.7652(10) 0.1176(7) 0.091(6) Uani 1 d . . H15A H 0.5852(15) 0.7959(10) 0.1391(7) 0.109 Uiso 0.60 calc PR 1 H15B H 0.6677(15) 0.8121(10) 0.0879(7) 0.109 Uiso 0.60 calc PR 1 H15C H 0.6620(15) 0.8206(10) 0.0948(7) 0.109 Uiso 0.40 d PR 2 H15D H 0.5736(15) 0.7812(10) 0.1392(7) 0.109 Uiso 0.40 d PR 2 C16 C 0.6001(16) 0.7196(15) 0.0256(9) 0.081(8) Uani 0.60 d PG 1 H16A H 0.6603(16) 0.7444(15) 0.0093(9) 0.097 Uiso 0.60 calc PR 1 C17 C 0.5438(19) 0.6830(16) -0.0073(8) 0.099(11) Uani 0.60 d PG 1 H17A H 0.5663(25) 0.6833(24) -0.0455(9) 0.119 Uiso 0.60 calc PR 1 C18 C 0.4539(18) 0.6460(19) 0.0171(11) 0.110(11) Uani 0.60 d PG 1 H18A H 0.4163(24) 0.6215(27) -0.0049(15) 0.132 Uiso 0.60 calc PR 1 C19 C 0.4203(16) 0.6456(20) 0.0743(12) 0.106(11) Uani 0.60 d PG 1 H19A H 0.3602(19) 0.6208(28) 0.0906(16) 0.127 Uiso 0.60 calc PR 1 C20 C 0.4766(19) 0.6822(19) 0.1072(9) 0.098(11) Uani 0.60 d PG 1 H20A H 0.4541(25) 0.6819(27) 0.1455(10) 0.118 Uiso 0.60 calc PR 1 C21 C 0.5665(18) 0.7192(16) 0.0828(9) 0.063(8) Uani 0.60 d PG 1 C16' C 0.6442(26) 0.7213(34) 0.0227(20) 0.096(17) Uiso 0.40 d PG 2 H16B H 0.7059(26) 0.7458(34) 0.0116(20) 0.115 Uiso 0.40 calc PR 2 C17' C 0.5983(29) 0.6860(29) -0.0154(15) 0.088(15) Uiso 0.40 d PG 2 H17B H 0.6294(40) 0.6869(43) -0.0520(18) 0.106 Uiso 0.40 calc PR 2 C18' C 0.5061(31) 0.6495(34) 0.0012(20) 0.104(21) Uiso 0.40 d PG 2 H18B H 0.4754(42) 0.6259(52) -0.0243(27) 0.125 Uiso 0.40 calc PR 2 C19' C 0.4597(28) 0.6482(36) 0.0559(22) 0.146(30) Uiso 0.40 d PG 2 H19B H 0.3979(33) 0.6238(52) 0.0670(31) 0.175 Uiso 0.40 calc PR 2 C20' C 0.5055(34) 0.6835(36) 0.0940(17) 0.080(14) Uiso 0.40 d PG 2 H20B H 0.4744(46) 0.6827(51) 0.1306(20) 0.096 Uiso 0.40 calc PR 2 C21' C 0.5977(34) 0.7201(38) 0.0774(19) 0.083(17) Uiso 0.40 d PG 2 C22 C 0.6458(13) 0.5918(9) 0.2158(6) 0.080(5) Uani 1 d . . H22A H 0.5890(13) 0.6105(9) 0.2360(6) 0.096 Uiso 1 calc R . H22B H 0.6236(13) 0.5622(9) 0.1887(6) 0.096 Uiso 1 calc R . C23 C 0.7393(11) 0.4457(7) 0.2509(5) 0.113(7) Uani 1 d G . H23A H 0.7266(11) 0.4344(7) 0.2158(5) 0.136 Uiso 1 calc R . C24 C 0.7947(11) 0.3840(6) 0.2928(7) 0.144(10) Uani 1 d G . H24A H 0.8190(15) 0.3312(9) 0.2857(10) 0.173 Uiso 1 calc R . C25 C 0.8137(12) 0.4010(8) 0.3453(7) 0.163(13) Uani 1 d G . H25A H 0.8507(16) 0.3596(11) 0.3733(9) 0.196 Uiso 1 calc R . C26 C 0.7773(13) 0.4798(8) 0.3559(5) 0.157(13) Uani 1 d G . H26A H 0.7900(18) 0.4912(12) 0.3910(6) 0.189 Uiso 1 calc R . C27 C 0.7219(10) 0.5416(6) 0.3140(4) 0.106(7) Uani 1 d G . H27A H 0.6975(15) 0.5943(8) 0.3211(6) 0.127 Uiso 1 calc R . C28 C 0.7029(9) 0.5245(6) 0.2615(4) 0.079(4) Uani 1 d G . C29 C 1.1146(12) 0.9708(10) 0.2662(8) 0.081(4) Uani 1 d . . H29A H 1.0830(12) 1.0212(10) 0.2375(8) 0.098 Uiso 1 calc R . H29B H 1.1586(12) 0.9966(10) 0.2864(8) 0.098 Uiso 1 calc R . C30 C 1.1357(8) 0.9003(8) 0.1831(5) 0.094(5) Uani 1 d G . H30A H 1.0736(8) 0.9218(8) 0.1727(5) 0.113 Uiso 1 calc R . C31 C 1.1892(10) 0.8524(9) 0.1503(5) 0.107(6) Uani 1 d G . H31A H 1.1629(13) 0.8419(13) 0.1180(6) 0.128 Uiso 1 calc R . C32 C 1.2819(9) 0.8203(9) 0.1658(6) 0.094(5) Uani 1 d G . H32A H 1.3177(12) 0.7883(12) 0.1438(8) 0.113 Uiso 1 calc R . C33 C 1.3211(7) 0.8361(10) 0.2141(6) 0.134(9) Uani 1 d G . H33A H 1.3831(9) 0.8147(14) 0.2244(9) 0.161 Uiso 1 calc R . C34 C 1.2676(9) 0.8840(10) 0.2469(5) 0.101(6) Uani 1 d G . H34A H 1.2938(12) 0.8946(14) 0.2792(7) 0.122 Uiso 1 calc R . C35 C 1.1749(9) 0.9161(8) 0.2314(5) 0.091(5) Uani 1 d G . C36 C 1.0908(11) 0.8150(9) 0.3757(6) 0.070(4) Uani 1 d . . H36A H 1.0475(11) 0.7644(9) 0.3947(6) 0.084 Uiso 1 calc R . H36B H 1.1421(11) 0.7933(9) 0.3530(6) 0.084 Uiso 1 calc R . C37 C 1.0930(7) 0.8100(7) 0.4824(5) 0.096(5) Uani 1 d G . H37A H 1.0365(7) 0.7760(7) 0.4906(5) 0.115 Uiso 1 calc R . C38 C 1.1347(9) 0.8305(9) 0.5282(4) 0.093(5) Uani 1 d G . H38A H 1.1061(13) 0.8102(12) 0.5672(4) 0.112 Uiso 1 calc R . C39 C 1.2192(9) 0.8813(9) 0.5160(5) 0.107(6) Uani 1 d G . H39A H 1.2471(13) 0.8950(13) 0.5467(6) 0.129 Uiso 1 calc R . C40 C 1.2619(8) 0.9116(9) 0.4578(6) 0.109(6) Uani 1 d G . H40A H 1.3184(10) 0.9456(12) 0.4495(8) 0.131 Uiso 1 calc R . C41 C 1.2202(9) 0.8911(8) 0.4119(4) 0.094(5) Uani 1 d G . H41A H 1.2488(12) 0.9113(12) 0.3730(5) 0.113 Uiso 1 calc R . C42 C 1.1357(8) 0.8403(8) 0.4242(4) 0.089(5) Uani 1 d G . C43 C 0.9723(12) 0.9830(9) 0.3642(7) 0.075(4) Uani 1 d . . H43A H 0.9108(12) 1.0068(9) 0.3480(7) 0.090 Uiso 1 calc R . H43B H 0.9576(12) 0.9449(9) 0.4053(7) 0.090 Uiso 1 calc R . C44 C 1.0728(9) 1.0631(6) 0.4187(4) 0.088(5) Uani 1 d G . H44A H 1.0730(9) 1.0094(6) 0.4510(4) 0.106 Uiso 1 calc R . C45 C 1.1155(9) 1.1411(9) 0.4222(6) 0.114(7) Uani 1 d G . H45A H 1.1443(14) 1.1396(12) 0.4569(7) 0.137 Uiso 1 calc R . C46 C 1.1151(10) 1.2213(7) 0.3738(7) 0.124(8) Uani 1 d G . H46A H 1.1437(14) 1.2735(9) 0.3762(9) 0.149 Uiso 1 calc R . C47 C 1.0720(11) 1.2236(6) 0.3220(6) 0.121(8) Uani 1 d G . H47A H 1.0718(16) 1.2772(7) 0.2897(7) 0.145 Uiso 1 calc R . C48 C 1.0293(10) 1.1456(7) 0.3185(4) 0.103(6) Uani 1 d G . H48A H 1.0005(14) 1.1471(10) 0.2838(5) 0.123 Uiso 1 calc R . C49 C 1.0297(8) 1.0654(5) 0.3669(5) 0.075(4) Uani 1 d G . C50 C 0.4716(11) 0.7888(11) 0.4236(8) 0.079(4) Uani 1 d . . H50A H 0.4471(11) 0.7988(11) 0.4607(8) 0.095 Uiso 1 calc R . H50B H 0.4567(11) 0.8434(11) 0.3910(8) 0.095 Uiso 1 calc R . C51 C 0.4434(9) 0.6724(9) 0.3720(6) 0.113(7) Uani 1 d G . H51A H 0.4964(9) 0.6954(9) 0.3453(6) 0.135 Uiso 1 calc R . C52 C 0.3920(13) 0.5997(9) 0.3674(7) 0.139(9) Uani 1 d G . H52A H 0.4107(17) 0.5739(14) 0.3375(9) 0.167 Uiso 1 calc R . C53 C 0.3128(12) 0.5653(8) 0.4074(8) 0.139(10) Uani 1 d G . H53A H 0.2784(16) 0.5166(11) 0.4042(11) 0.167 Uiso 1 calc R . C54 C 0.2849(9) 0.6038(10) 0.4520(7) 0.148(11) Uani 1 d G . H54A H 0.2319(11) 0.5808(14) 0.4788(9) 0.178 Uiso 1 calc R . C55 C 0.3362(9) 0.6766(9) 0.4567(5) 0.112(7) Uani 1 d G . H55A H 0.3175(14) 0.7023(13) 0.4866(7) 0.134 Uiso 1 calc R . C56 C 0.4155(9) 0.7109(7) 0.4167(6) 0.084(5) Uani 1 d G . C57 C 0.6259(14) 0.6665(10) 0.4824(8) 0.089(5) Uani 1 d . . H57A H 0.5917(14) 0.6196(10) 0.4731(8) 0.106 Uiso 1 calc R . H57B H 0.6947(14) 0.6524(10) 0.4798(8) 0.106 Uiso 1 calc R . C58 C 0.5022(8) 0.6336(8) 0.5713(5) 0.098(5) Uani 1 d G . H58A H 0.4588(8) 0.6183(8) 0.5478(5) 0.117 Uiso 1 calc R . C59 C 0.4740(9) 0.6280(8) 0.6302(6) 0.120(8) Uani 1 d G . H59A H 0.4119(10) 0.6089(12) 0.6463(8) 0.144 Uiso 1 calc R . C60 C 0.5388(12) 0.6509(9) 0.6652(4) 0.124(9) Uani 1 d G . H60A H 0.5200(16) 0.6471(12) 0.7047(4) 0.149 Uiso 1 calc R . C61 C 0.6317(11) 0.6794(9) 0.6413(5) 0.103(6) Uani 1 d G . H61A H 0.6751(14) 0.6947(12) 0.6647(7) 0.124 Uiso 1 calc R . C62 C 0.6599(7) 0.6850(8) 0.5823(5) 0.099(5) Uani 1 d G . H62A H 0.7220(8) 0.7041(12) 0.5663(7) 0.118 Uiso 1 calc R . C63 C 0.5951(9) 0.6622(7) 0.5473(4) 0.077(4) Uani 1 d G . C64 C 0.6311(13) 0.8628(10) 0.4597(6) 0.077(4) Uani 1 d . . H64A H 0.5856(13) 0.8562(10) 0.4942(6) 0.092 Uiso 1 calc R . H64B H 0.6956(13) 0.8498(10) 0.4742(6) 0.092 Uiso 1 calc R . C65 C 0.5508(6) 1.0180(6) 0.4258(4) 0.075(4) Uani 1 d G . H65A H 0.4982(6) 0.9948(6) 0.4528(4) 0.090 Uiso 1 calc R . C66 C 0.5527(7) 1.1100(6) 0.3921(5) 0.093(5) Uani 1 d G . H66A H 0.5014(9) 1.1484(8) 0.3965(7) 0.112 Uiso 1 calc R . C67 C 0.6314(8) 1.1447(4) 0.3517(4) 0.079(4) Uani 1 d G . H67A H 0.6327(11) 1.2062(4) 0.3291(6) 0.095 Uiso 1 calc R . C68 C 0.7082(7) 1.0873(6) 0.3450(4) 0.074(4) Uani 1 d G . H68A H 0.7608(8) 1.1105(8) 0.3180(5) 0.088 Uiso 1 calc R . C69 C 0.7063(6) 0.9953(5) 0.3788(4) 0.072(4) Uani 1 d G . H69A H 0.7576(8) 0.9569(7) 0.3743(6) 0.086 Uiso 1 calc R . C70 C 0.6276(7) 0.9607(4) 0.4192(4) 0.072(4) Uani 1 d G . C71 C 0.7139(13) 1.1311(8) 0.0831(6) 0.078(4) Uani 1 d . . H71A H 0.6904(13) 1.1931(8) 0.0655(6) 0.093 Uiso 1 calc R . H71B H 0.7836(13) 1.1340(8) 0.0851(6) 0.093 Uiso 1 calc R . C72 C 0.6168(8) 1.1008(7) 0.0057(5) 0.090(5) Uani 1 d G . H72A H 0.5744(8) 1.1475(7) 0.0085(5) 0.108 Uiso 1 calc R . C73 C 0.6020(8) 1.0543(8) -0.0345(5) 0.098(5) Uani 1 d G . H73A H 0.5497(10) 1.0700(11) -0.0586(6) 0.117 Uiso 1 calc R . C74 C 0.6653(10) 0.9844(7) -0.0387(4) 0.105(7) Uani 1 d G . H74A H 0.6554(14) 0.9533(10) -0.0656(6) 0.127 Uiso 1 calc R . C75 C 0.7434(9) 0.9609(6) -0.0028(5) 0.110(7) Uani 1 d G . H75A H 0.7858(12) 0.9141(9) -0.0056(7) 0.132 Uiso 1 calc R . C76 C 0.7582(7) 1.0074(6) 0.0374(4) 0.085(5) Uani 1 d G . H76A H 0.8105(9) 0.9917(10) 0.0615(6) 0.102 Uiso 1 calc R . C77 C 0.6949(8) 1.0773(6) 0.0416(4) 0.072(4) Uani 1 d G . C78 C 0.5276(14) 1.0895(11) 0.1474(7) 0.087(5) Uani 1 d . . H78A H 0.5164(14) 1.1421(11) 0.1127(7) 0.104 Uiso 1 calc R . H78B H 0.5134(14) 1.0356(11) 0.1371(7) 0.104 Uiso 1 calc R . C79 C 0.4670(9) 1.0409(8) 0.2574(5) 0.102(6) Uani 1 d G . H79A H 0.5191(9) 1.0001(8) 0.2662(5) 0.122 Uiso 1 calc R . C80 C 0.4009(11) 1.0481(9) 0.3033(4) 0.111(6) Uani 1 d G . H80A H 0.4087(15) 1.0123(13) 0.3427(4) 0.134 Uiso 1 calc R . C81 C 0.3230(10) 1.1090(10) 0.2901(6) 0.112(7) Uani 1 d G . H81A H 0.2787(13) 1.1139(14) 0.3208(8) 0.134 Uiso 1 calc R . C82 C 0.3112(9) 1.1626(9) 0.2312(7) 0.139(9) Uani 1 d G . H82A H 0.2591(12) 1.2033(12) 0.2224(10) 0.167 Uiso 1 calc R . C83 C 0.3774(11) 1.1553(8) 0.1853(5) 0.129(9) Uani 1 d G . H83A H 0.3695(15) 1.1912(12) 0.1459(6) 0.155 Uiso 1 calc R . C84 C 0.4552(9) 1.0945(8) 0.1985(4) 0.085(4) Uani 1 d G . C85 C 0.6790(14) 1.1767(8) 0.1932(6) 0.080(5) Uani 1 d . . H85A H 0.6473(14) 1.1592(8) 0.2334(6) 0.096 Uiso 0.60 calc PR 1 H85B H 0.7481(14) 1.1783(8) 0.1974(6) 0.096 Uiso 0.60 calc PR 1 H85C H 0.7423(14) 1.1662(8) 0.2085(6) 0.096 Uiso 0.40 d PR 2 H85D H 0.6328(14) 1.1701(8) 0.2269(6) 0.096 Uiso 0.40 d PR 2 C86 C 0.5567(23) 1.3115(13) 0.1717(15) 0.113(13) Uani 0.60 d PG 1 H86A H 0.5103(23) 1.2755(13) 0.1988(15) 0.136 Uiso 0.60 calc PR 1 C87 C 0.5372(19) 1.4033(13) 0.1430(13) 0.116(13) Uani 0.60 d PG 1 H87A H 0.4777(21) 1.4287(18) 0.1509(18) 0.140 Uiso 0.60 calc PR 1 C88 C 0.6066(22) 1.4571(10) 0.1024(10) 0.087(8) Uani 0.60 d PG 1 H88A H 0.5935(28) 1.5185(11) 0.0832(14) 0.104 Uiso 0.60 calc PR 1 C89 C 0.6955(20) 1.4191(12) 0.0906(11) 0.159(20) Uani 0.60 d PGU 1 H89A H 0.7419(25) 1.4551(17) 0.0635(16) 0.191 Uiso 0.60 calc PR 1 C90 C 0.7150(18) 1.3273(14) 0.1194(13) 0.099(12) Uani 0.60 d PG 1 H90A H 0.7744(19) 1.3018(19) 0.1115(18) 0.119 Uiso 0.60 calc PR 1 C91 C 0.6456(23) 1.2735(11) 0.1599(14) 0.093(16) Uani 0.60 d PG 1 C86' C 0.5838(32) 1.3238(28) 0.1555(22) 0.093(16) Uiso 0.40 d PG 2 H86B H 0.5290(32) 1.2954(28) 0.1783(22) 0.112 Uiso 0.40 calc PR 2 C87' C 0.5789(25) 1.4150(27) 0.1205(21) 0.120(24) Uiso 0.40 d PG 2 H87B H 0.5210(29) 1.4477(37) 0.1199(32) 0.144 Uiso 0.40 calc PR 2 C88' C 0.6607(29) 1.4574(19) 0.0863(16) 0.071(11) Uiso 0.40 d PG 2 H88B H 0.6575(40) 1.5185(20) 0.0628(23) 0.085 Uiso 0.40 calc PR 2 C89' C 0.7473(25) 1.4086(26) 0.0871(19) 0.132(24) Uiso 0.40 d PG 2 H89B H 0.8021(30) 1.4370(37) 0.0642(29) 0.159 Uiso 0.40 calc PR 2 C90' C 0.7522(29) 1.3174(26) 0.1221(22) 0.095(18) Uiso 0.40 d PG 2 H90B H 0.8101(35) 1.2847(36) 0.1227(33) 0.115 Uiso 0.40 calc PR 2 C91' C 0.6704(39) 1.2749(20) 0.1563(20) 0.060(12) Uiso 0.40 d PG 2 O100 O 0.9653(32) 0.8019(24) -0.1435(17) 0.206(16) Uani 0.65 d P 1 H100 H 1.0086(32) 0.8397(24) -0.1519(17) 0.310 Uiso 0.65 d PR 1 C101 C 0.8836(50) 0.8370(36) -0.1125(25) 0.232(34) Uani 0.65 d P 1 H10C H 0.8995(50) 0.8368(36) -0.0735(25) 0.348 Uiso 0.65 d PR 1 H10D H 0.8295(50) 0.7977(36) -0.1084(25) 0.348 Uiso 0.65 d PR 1 H10E H 0.8668(50) 0.8980(36) -0.1362(25) 0.348 Uiso 0.65 d PR 1 O102 O 0.9139(41) 0.6015(37) 0.5302(25) 0.223(21) Uani 0.50 d PU -1 H102 H 0.9270(41) 0.6129(37) 0.5603(25) 0.334 Uiso 0.50 d PR -1 C103 C 0.9734(67) 0.5386(57) 0.5074(43) 0.234(38) Uani 0.50 d PU -1 H10F H 1.0341(67) 0.5599(57) 0.5148(43) 0.351 Uiso 0.50 d PR -1 H10G H 0.9722(67) 0.5462(57) 0.4654(43) 0.351 Uiso 0.50 d PR -1 H10H H 0.9663(67) 0.4752(57) 0.5302(43) 0.351 Uiso 0.50 d PR -1 O104 O 0.9766(57) 0.6026(50) -0.1079(35) 0.207(28) Uiso 0.35 d P . H104 H 0.9275(57) 0.5762(50) -0.1103(35) 0.310 Uiso 0.35 d PR . C105 C 1.0138(71) 0.6389(64) -0.1560(44) 0.175(35) Uiso 0.35 d P . H10I H 1.0510(71) 0.5964(64) -0.1711(44) 0.262 Uiso 0.35 d PR . H10J H 1.0554(71) 0.6864(64) -0.1544(44) 0.262 Uiso 0.35 d PR . H10K H 0.9630(71) 0.6652(64) -0.1820(44) 0.262 Uiso 0.35 d PR . 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 0.0738(8) 0.0547(4) 0.0642(5) -0.0225(4) -0.0067(5) -0.0003(4) Pd2 0.0665(7) 0.0566(4) 0.0605(5) -0.0165(4) -0.0060(5) -0.0026(4) Pd3 0.0691(8) 0.0601(4) 0.0590(5) -0.0185(4) -0.0027(5) -0.0049(5) Pd4 0.0699(8) 0.0522(4) 0.0631(5) -0.0139(4) -0.0062(5) -0.0002(4) S1 0.070(3) 0.066(2) 0.071(2) -0.0208(13) -0.011(2) -0.007(2) S2 0.065(3) 0.070(2) 0.073(2) -0.0095(14) -0.007(2) -0.005(2) O1 0.094(10) 0.122(8) 0.076(7) -0.018(6) 0.001(7) 0.007(7) O2 0.095(9) 0.063(5) 0.114(8) -0.019(5) -0.021(7) -0.013(5) S3 0.075(3) 0.0635(15) 0.0520(15) -0.0121(12) -0.003(2) -0.006(2) O3 0.107(10) 0.061(5) 0.093(7) -0.009(5) -0.009(7) 0.010(6) O4 0.094(9) 0.091(6) 0.068(6) -0.022(5) -0.026(6) -0.010(6) P1 0.090(3) 0.0552(14) 0.058(2) -0.0207(12) -0.007(2) -0.005(2) P2 0.059(2) 0.0619(15) 0.076(2) -0.0220(14) -0.004(2) -0.003(2) P3 0.072(3) 0.063(2) 0.067(2) -0.0182(14) 0.003(2) -0.008(2) P4 0.080(3) 0.0576(15) 0.060(2) -0.0125(13) -0.006(2) 0.003(2) C1 0.070(12) 0.087(9) 0.066(8) -0.020(7) -0.003(8) 0.013(8) N1 0.126(16) 0.104(10) 0.116(12) -0.045(9) -0.033(11) 0.044(11) C2 0.232(12) 0.226(12) 0.233(12) -0.077(8) -0.013(8) 0.010(8) C3 0.232(13) 0.238(12) 0.234(12) -0.079(8) -0.014(8) 0.014(8) C4 0.251(13) 0.250(12) 0.249(13) -0.077(8) -0.012(8) 0.002(8) C5 0.252(13) 0.243(12) 0.246(13) -0.080(8) -0.018(8) 0.004(8) C6 0.249(13) 0.248(12) 0.245(13) -0.077(8) -0.018(8) 0.008(8) C7 0.242(13) 0.249(12) 0.247(12) -0.074(8) -0.013(8) 0.011(8) C8 0.100(14) 0.071(7) 0.075(9) -0.028(7) 0.013(9) -0.010(8) C9 0.073(19) 0.078(13) 0.054(12) 0.010(10) -0.011(11) -0.009(13) C10 0.159(54) 0.119(34) 0.138(42) -0.024(22) 0.066(34) -0.071(32) C11 0.127(41) 0.207(49) 0.132(34) -0.038(33) 0.024(30) -0.036(36) C12 0.170(46) 0.206(45) 0.170(40) -0.134(39) 0.057(35) -0.019(37) C13 0.170(40) 0.153(28) 0.119(25) -0.090(24) 0.083(28) -0.056(28) C14 0.110(25) 0.080(15) 0.094(18) -0.040(13) 0.001(19) -0.032(15) C15 0.140(17) 0.075(7) 0.075(9) -0.037(7) -0.063(10) 0.018(9) C16 0.089(27) 0.077(14) 0.078(18) -0.024(11) -0.016(17) -0.006(16) C17 0.118(35) 0.107(23) 0.082(19) -0.036(16) -0.051(21) 0.031(26) C18 0.131(37) 0.118(24) 0.094(23) -0.051(19) -0.002(25) -0.003(25) C19 0.049(20) 0.122(24) 0.154(33) -0.052(23) -0.018(21) -0.002(17) C20 0.066(24) 0.145(30) 0.092(22) -0.049(21) -0.009(19) 0.002(22) C21 0.091(25) 0.053(11) 0.055(12) -0.025(9) -0.019(14) -0.001(16) C22 0.107(14) 0.067(7) 0.069(8) -0.023(6) -0.015(9) -0.017(8) C23 0.105(17) 0.079(10) 0.139(17) -0.017(10) 0.013(14) -0.006(11) C24 0.181(28) 0.066(9) 0.179(24) -0.019(12) -0.064(21) 0.000(13) C25 0.186(30) 0.104(15) 0.169(24) 0.018(15) -0.100(23) 0.010(16) C26 0.231(34) 0.086(12) 0.135(19) 0.014(12) -0.090(21) -0.024(16) C27 0.154(20) 0.066(7) 0.080(10) 0.011(7) -0.037(12) -0.033(10) C28 0.097(13) 0.058(6) 0.080(9) -0.019(6) -0.007(9) -0.005(7) C29 0.073(12) 0.075(8) 0.097(11) -0.029(7) -0.006(9) -0.007(8) C30 0.087(14) 0.102(11) 0.107(13) -0.055(10) 0.004(11) 0.006(10) C31 0.095(16) 0.127(14) 0.111(14) -0.060(12) 0.013(12) 0.001(13) C32 0.075(14) 0.113(12) 0.091(11) -0.034(10) 0.015(10) 0.021(10) C33 0.083(17) 0.160(20) 0.168(24) -0.073(19) 0.027(16) 0.015(15) C34 0.063(12) 0.151(16) 0.107(13) -0.067(13) -0.007(10) 0.007(12) C35 0.092(15) 0.093(10) 0.088(11) -0.033(8) 0.007(10) 0.000(10) C36 0.062(10) 0.079(7) 0.070(8) -0.026(6) -0.017(7) 0.016(7) C37 0.099(15) 0.103(11) 0.091(12) -0.038(9) -0.021(11) 0.030(11) C38 0.076(13) 0.120(13) 0.084(11) -0.038(9) 0.006(9) 0.017(11) C39 0.114(18) 0.122(14) 0.095(13) -0.048(11) -0.013(12) 0.006(13) C40 0.070(13) 0.152(17) 0.119(16) -0.058(13) -0.029(12) -0.007(12) C41 0.084(14) 0.109(11) 0.098(12) -0.042(10) -0.005(10) -0.018(10) C42 0.105(15) 0.086(9) 0.086(11) -0.041(8) -0.017(10) 0.020(10) C43 0.074(11) 0.076(7) 0.091(10) -0.046(7) -0.011(8) -0.012(8) C44 0.089(14) 0.091(9) 0.091(11) -0.036(8) -0.018(10) 0.014(9) C45 0.101(16) 0.120(14) 0.156(19) -0.090(15) -0.028(14) 0.010(13) C46 0.121(19) 0.095(12) 0.170(22) -0.058(14) -0.011(16) -0.040(13) C47 0.140(21) 0.076(9) 0.144(18) -0.031(11) 0.002(16) -0.024(12) C48 0.114(17) 0.089(10) 0.113(14) -0.047(10) 0.007(12) -0.012(11) C49 0.074(11) 0.066(7) 0.087(9) -0.026(6) -0.002(8) -0.005(7) C50 0.048(10) 0.094(9) 0.093(10) -0.029(8) 0.003(8) 0.002(8) C51 0.121(19) 0.103(12) 0.122(15) -0.047(11) 0.010(13) -0.040(12) C52 0.121(21) 0.133(17) 0.185(26) -0.079(18) -0.003(19) -0.039(16) C53 0.151(26) 0.108(14) 0.149(22) -0.018(14) -0.046(20) -0.036(16) C54 0.111(21) 0.109(14) 0.189(27) 0.014(16) -0.040(19) -0.051(15) C55 0.075(14) 0.116(13) 0.130(16) -0.017(12) -0.002(12) -0.025(11) C56 0.070(12) 0.079(8) 0.100(11) -0.018(8) -0.023(9) -0.015(8) C57 0.088(14) 0.073(8) 0.097(11) -0.018(7) 0.008(10) -0.010(8) C58 0.103(16) 0.086(9) 0.086(11) -0.003(8) -0.005(11) -0.003(10) C59 0.170(24) 0.106(12) 0.072(11) -0.017(9) 0.035(13) -0.032(14) C60 0.168(26) 0.096(11) 0.086(13) -0.007(10) 0.030(15) 0.016(14) C61 0.121(19) 0.109(12) 0.070(10) -0.015(9) -0.021(11) 0.024(12) C62 0.090(15) 0.114(12) 0.078(10) -0.013(9) -0.003(10) 0.000(11) C63 0.072(12) 0.073(7) 0.073(9) -0.005(6) 0.004(8) -0.001(8) C64 0.088(12) 0.084(8) 0.061(7) -0.027(6) -0.008(8) -0.004(8) C65 0.078(12) 0.087(8) 0.061(8) -0.026(6) -0.005(7) 0.007(8) C66 0.093(15) 0.089(9) 0.097(12) -0.028(9) -0.027(11) 0.027(10) C67 0.090(13) 0.073(7) 0.070(8) -0.016(6) -0.006(8) -0.002(8) C68 0.090(12) 0.066(7) 0.066(8) -0.022(6) 0.001(8) -0.007(8) C69 0.068(11) 0.068(7) 0.075(8) -0.018(6) 0.006(8) -0.010(7) C70 0.088(12) 0.068(7) 0.065(8) -0.026(6) -0.007(8) -0.006(8) C71 0.088(12) 0.061(6) 0.068(8) -0.001(6) 0.011(8) 0.000(7) C72 0.109(16) 0.082(8) 0.073(9) -0.018(7) -0.009(10) 0.018(9) C73 0.100(15) 0.112(12) 0.079(10) -0.028(9) -0.009(10) 0.000(11) C74 0.159(21) 0.082(9) 0.072(9) -0.013(7) -0.030(12) -0.011(12) C75 0.174(23) 0.076(8) 0.077(10) -0.026(8) -0.001(13) 0.019(12) C76 0.100(14) 0.078(8) 0.067(8) -0.007(7) -0.012(9) 0.006(9) C77 0.085(12) 0.066(7) 0.053(7) -0.003(5) -0.001(7) -0.009(7) C78 0.100(14) 0.091(9) 0.071(9) -0.025(7) -0.028(9) 0.015(9) C79 0.118(18) 0.108(11) 0.074(10) -0.025(9) 0.000(11) 0.013(12) C80 0.093(16) 0.137(16) 0.109(15) -0.042(13) -0.016(13) -0.018(13) C81 0.113(19) 0.103(12) 0.116(15) -0.033(11) 0.005(14) -0.020(13) C82 0.121(22) 0.106(14) 0.168(24) -0.017(15) 0.000(19) 0.023(14) C83 0.114(20) 0.117(14) 0.119(16) 0.005(12) 0.003(14) 0.053(14) C84 0.089(13) 0.083(8) 0.076(9) -0.018(7) -0.004(9) 0.003(9) C85 0.122(15) 0.054(6) 0.068(8) -0.025(6) -0.017(9) 0.020(8) C86 0.133(38) 0.085(18) 0.128(33) -0.045(19) -0.020(28) 0.045(22) C87 0.160(37) 0.071(15) 0.144(31) -0.070(19) -0.027(30) 0.039(21) C88 0.090(25) 0.079(16) 0.079(16) -0.014(13) 0.021(17) 0.009(17) C89 0.297(59) 0.053(13) 0.147(32) -0.051(17) -0.078(36) 0.049(26) C90 0.113(30) 0.099(21) 0.113(25) -0.061(19) -0.053(24) -0.002(20) C91 0.110(40) 0.068(16) 0.099(25) -0.020(13) -0.035(23) -0.002(19) O100 0.234(44) 0.171(28) 0.204(36) -0.049(25) 0.044(32) -0.099(29) C101 0.300(89) 0.163(43) 0.170(50) 0.012(36) 0.070(54) 0.039(50) O102 0.221(23) 0.224(23) 0.220(23) -0.065(12) -0.016(10) -0.003(10) C103 0.234(39) 0.232(39) 0.234(39) -0.074(15) -0.013(11) 0.000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.94(2) . ? Pd1 P1 2.289(3) . ? Pd1 S1 2.304(4) . ? Pd1 Pd3 2.724(2) . ? Pd1 Pd4 2.7766(13) . ? Pd1 Pd2 2.8165(14) . ? Pd2 S3 2.306(3) . ? Pd2 S2 2.332(3) . ? Pd2 P2 2.348(4) . ? Pd2 Pd3 2.854(2) . ? Pd2 Pd4 2.912(2) . ? Pd3 S3 2.210(4) . ? Pd3 P3 2.298(4) . ? Pd3 S1 2.400(4) . ? Pd3 Pd4 3.052(2) . ? Pd4 S2 2.197(4) . ? Pd4 P4 2.276(3) . ? Pd4 S1 2.397(3) . ? S2 O1 1.470(13) . ? S2 O2 1.482(10) . ? S3 O3 1.476(10) . ? S3 O4 1.502(10) . ? P1 C22 1.819(14) . ? P1 C8 1.83(2) . ? P1 C15 1.862(14) . ? P2 C29 1.83(2) . ? P2 C36 1.857(13) . ? P2 C43 1.858(14) . ? P3 C50 1.82(2) . ? P3 C64 1.831(13) . ? P3 C57 1.86(2) . ? P4 C85 1.844(12) . ? P4 C78 1.85(2) . ? P4 C71 1.857(14) . ? C1 N1 1.14(2) . ? N1 C2 1.63(4) . ? C2 C3 1.44(5) . ? C2 C7 1.72(5) . ? C3 C4 1.61(5) . ? C4 C5 1.64(5) . ? C5 C6 1.48(5) . ? C6 C7 1.67(5) . ? C8 C14 1.52(2) . ? C8 C14' 1.57(5) . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C10 C11 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C9' C10' 1.39 . ? C9' C14' 1.39 . ? C10' C11' 1.39 . ? C11' C12' 1.39 . ? C12' C13' 1.39 . ? C13' C14' 1.39 . ? C15 C21' 1.44(3) . ? C15 C21 1.57(2) . ? C16 C17 1.39 . ? C16 C21 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C16' C17' 1.39 . ? C16' C21' 1.39 . ? C17' C18' 1.39 . ? C18' C19' 1.39 . ? C19' C20' 1.39 . ? C20' C21' 1.39 . ? C22 C28 1.49(2) . ? C23 C24 1.39 . ? C23 C28 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C29 C35 1.54(2) . ? C30 C31 1.39 . ? C30 C35 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C36 C42 1.502(15) . ? C37 C38 1.39 . ? C37 C42 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C43 C49 1.545(14) . ? C44 C45 1.39 . ? C44 C49 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C48 C49 1.39 . ? C50 C56 1.51(2) . ? C51 C52 1.39 . ? C51 C56 1.39 . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C57 C63 1.54(2) . ? C58 C59 1.39 . ? C58 C63 1.39 . ? C59 C60 1.39 . ? C60 C61 1.39 . ? C61 C62 1.39 . ? C62 C63 1.39 . ? C64 C70 1.51(2) . ? C65 C66 1.39 . ? C65 C70 1.39 . ? C66 C67 1.39 . ? C67 C68 1.39 . ? C68 C69 1.39 . ? C69 C70 1.39 . ? C71 C77 1.52(2) . ? C72 C73 1.39 . ? C72 C77 1.39 . ? C73 C74 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? C76 C77 1.39 . ? C78 C84 1.52(2) . ? C79 C80 1.39 . ? C79 C84 1.39 . ? C80 C81 1.39 . ? C81 C82 1.39 . ? C82 C83 1.39 . ? C83 C84 1.39 . ? C85 C91' 1.50(3) . ? C85 C91 1.52(2) . ? C86 C87 1.39 . ? C86 C91 1.39 . ? C87 C88 1.39 . ? C88 C89 1.39 . ? C89 C90 1.39 . ? C90 C91 1.39 . ? C86' C87' 1.39 . ? C86' C91' 1.39 . ? C87' C88' 1.39 . ? C88' C89' 1.39 . ? C89' C90' 1.39 . ? C90' C91' 1.39 . ? O100 C101 1.48(6) . ? O102 C103 1.46(8) . ? O104 C105 1.18(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 99.1(5) . . ? C1 Pd1 S1 168.5(5) . . ? P1 Pd1 S1 91.21(14) . . ? C1 Pd1 Pd3 112.3(4) . . ? P1 Pd1 Pd3 134.55(12) . . ? S1 Pd1 Pd3 56.27(9) . . ? C1 Pd1 Pd4 121.2(5) . . ? P1 Pd1 Pd4 122.52(10) . . ? S1 Pd1 Pd4 55.36(8) . . ? Pd3 Pd1 Pd4 67.40(4) . . ? C1 Pd1 Pd2 67.0(5) . . ? P1 Pd1 Pd2 163.15(12) . . ? S1 Pd1 Pd2 103.63(9) . . ? Pd3 Pd1 Pd2 61.98(4) . . ? Pd4 Pd1 Pd2 62.74(4) . . ? S3 Pd2 S2 154.87(15) . . ? S3 Pd2 P2 93.31(13) . . ? S2 Pd2 P2 95.03(13) . . ? S3 Pd2 Pd1 88.74(9) . . ? S2 Pd2 Pd1 91.09(10) . . ? P2 Pd2 Pd1 160.75(10) . . ? S3 Pd2 Pd3 49.33(10) . . ? S2 Pd2 Pd3 110.90(11) . . ? P2 Pd2 Pd3 135.37(11) . . ? Pd1 Pd2 Pd3 57.43(4) . . ? S3 Pd2 Pd4 112.83(11) . . ? S2 Pd2 Pd4 48.00(10) . . ? P2 Pd2 Pd4 136.97(9) . . ? Pd1 Pd2 Pd4 57.96(4) . . ? Pd3 Pd2 Pd4 63.92(4) . . ? S3 Pd3 P3 95.74(14) . . ? S3 Pd3 S1 145.84(14) . . ? P3 Pd3 S1 117.7(2) . . ? S3 Pd3 Pd1 93.12(10) . . ? P3 Pd3 Pd1 159.63(10) . . ? S1 Pd3 Pd1 52.98(10) . . ? S3 Pd3 Pd2 52.31(9) . . ? P3 Pd3 Pd2 137.96(11) . . ? S1 Pd3 Pd2 100.07(10) . . ? Pd1 Pd3 Pd2 60.59(4) . . ? S3 Pd3 Pd4 110.85(9) . . ? P3 Pd3 Pd4 134.58(10) . . ? S1 Pd3 Pd4 50.44(8) . . ? Pd1 Pd3 Pd4 57.12(4) . . ? Pd2 Pd3 Pd4 58.96(4) . . ? S2 Pd4 P4 96.93(14) . . ? S2 Pd4 S1 146.61(14) . . ? P4 Pd4 S1 114.88(14) . . ? S2 Pd4 Pd1 95.09(10) . . ? P4 Pd4 Pd1 149.17(10) . . ? S1 Pd4 Pd1 52.27(10) . . ? S2 Pd4 Pd2 52.06(9) . . ? P4 Pd4 Pd2 145.94(11) . . ? S1 Pd4 Pd2 98.56(9) . . ? Pd1 Pd4 Pd2 59.30(4) . . ? S2 Pd4 Pd3 108.18(10) . . ? P4 Pd4 Pd3 143.50(11) . . ? S1 Pd4 Pd3 50.53(9) . . ? Pd1 Pd4 Pd3 55.49(4) . . ? Pd2 Pd4 Pd3 57.12(4) . . ? Pd1 S1 Pd4 72.37(12) . . ? Pd1 S1 Pd3 70.75(11) . . ? Pd4 S1 Pd3 79.03(11) . . ? O1 S2 O2 112.6(8) . . ? O1 S2 Pd4 112.7(6) . . ? O2 S2 Pd4 115.9(6) . . ? O1 S2 Pd2 120.3(5) . . ? O2 S2 Pd2 111.8(5) . . ? Pd4 S2 Pd2 79.95(12) . . ? O3 S3 O4 111.3(6) . . ? O3 S3 Pd3 112.1(5) . . ? O4 S3 Pd3 119.0(5) . . ? O3 S3 Pd2 120.1(5) . . ? O4 S3 Pd2 112.6(4) . . ? Pd3 S3 Pd2 78.35(11) . . ? C22 P1 C8 102.3(7) . . ? C22 P1 C15 106.2(8) . . ? C8 P1 C15 106.4(8) . . ? C22 P1 Pd1 111.2(5) . . ? C8 P1 Pd1 117.9(6) . . ? C15 P1 Pd1 111.9(4) . . ? C29 P2 C36 104.5(8) . . ? C29 P2 C43 106.9(7) . . ? C36 P2 C43 106.1(7) . . ? C29 P2 Pd2 117.4(6) . . ? C36 P2 Pd2 116.8(5) . . ? C43 P2 Pd2 104.3(5) . . ? C50 P3 C64 101.5(8) . . ? C50 P3 C57 105.1(8) . . ? C64 P3 C57 104.2(7) . . ? C50 P3 Pd3 120.0(6) . . ? C64 P3 Pd3 111.7(5) . . ? C57 P3 Pd3 112.8(6) . . ? C85 P4 C78 107.3(8) . . ? C85 P4 C71 103.2(7) . . ? C78 P4 C71 101.5(8) . . ? C85 P4 Pd4 110.6(5) . . ? C78 P4 Pd4 118.1(5) . . ? C71 P4 Pd4 114.7(5) . . ? N1 C1 Pd1 170.3(16) . . ? C1 N1 C2 172.8(25) . . ? C3 C2 N1 100.2(35) . . ? C3 C2 C7 99.6(36) . . ? N1 C2 C7 96.1(31) . . ? C2 C3 C4 100.7(38) . . ? C3 C4 C5 92.7(35) . . ? C6 C5 C4 105.8(38) . . ? C5 C6 C7 99.2(38) . . ? C6 C7 C2 93.6(33) . . ? C14 C8 P1 119.9(11) . . ? C14' C8 P1 117.9(18) . . ? C10 C9 C14 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 C8 115.6(15) . . ? C9 C14 C8 124.4(15) . . ? C10' C9' C14' 120.0 . . ? C11' C10' C9' 120.0 . . ? C12' C11' C10' 120.0 . . ? C11' C12' C13' 120.0 . . ? C14' C13' C12' 120.0 . . ? C13' C14' C9' 120.0 . . ? C13' C14' C8 123.8(48) . . ? C9' C14' C8 116.2(48) . . ? C21' C15 P1 112.6(23) . . ? C21 C15 P1 119.1(13) . . ? C17 C16 C21 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 C15 121.1(16) . . ? C16 C21 C15 118.8(16) . . ? C17' C16' C21' 120.0 . . ? C16' C17' C18' 120.0 . . ? C19' C18' C17' 120.0 . . ? C20' C19' C18' 120.0 . . ? C19' C20' C21' 120.0 . . ? C20' C21' C16' 120.0 . . ? C20' C21' C15 113.1(32) . . ? C16' C21' C15 126.3(32) . . ? C28 C22 P1 113.8(11) . . ? C24 C23 C28 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 C22 120.1(9) . . ? C23 C28 C22 119.8(9) . . ? C35 C29 P2 115.7(10) . . ? C31 C30 C35 120.0 . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 C29 121.2(10) . . ? C30 C35 C29 118.8(10) . . ? C42 C36 P2 116.7(9) . . ? C38 C37 C42 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 C36 121.0(10) . . ? C37 C42 C36 119.0(10) . . ? C49 C43 P2 121.9(11) . . ? C45 C44 C49 120.0 . . ? C46 C45 C44 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 C43 118.6(9) . . ? C44 C49 C43 121.1(9) . . ? C56 C50 P3 118.3(11) . . ? C52 C51 C56 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 C50 119.0(10) . . ? C51 C56 C50 120.9(10) . . ? C63 C57 P3 115.3(11) . . ? C59 C58 C63 120.0 . . ? C58 C59 C60 120.0 . . ? C61 C60 C59 120.0 . . ? C62 C61 C60 120.0 . . ? C63 C62 C61 120.0 . . ? C62 C63 C58 120.0 . . ? C62 C63 C57 120.5(10) . . ? C58 C63 C57 119.5(10) . . ? C70 C64 P3 114.9(9) . . ? C66 C65 C70 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C69 120.0 . . ? C70 C69 C68 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 C64 119.2(9) . . ? C65 C70 C64 120.6(9) . . ? C77 C71 P4 115.7(9) . . ? C73 C72 C77 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C77 120.0 . . ? C76 C77 C72 120.0 . . ? C76 C77 C71 120.0(9) . . ? C72 C77 C71 119.9(9) . . ? C84 C78 P4 117.2(10) . . ? C80 C79 C84 120.0 . . ? C81 C80 C79 120.0 . . ? C82 C81 C80 120.0 . . ? C83 C82 C81 120.0 . . ? C82 C83 C84 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 C78 118.7(10) . . ? C79 C84 C78 121.2(10) . . ? C91' C85 P4 120.6(22) . . ? C91 C85 P4 118.4(16) . . ? C87 C86 C91 120.0 . . ? C88 C87 C86 120.0 . . ? C87 C88 C89 120.0 . . ? C88 C89 C90 120.0 . . ? C91 C90 C89 120.0 . . ? C90 C91 C86 120.0 . . ? C90 C91 C85 115.1(19) . . ? C86 C91 C85 124.6(18) . . ? C87' C86' C91' 120.0 . . ? C88' C87' C86' 120.0 . . ? C87' C88' C89' 120.0 . . ? C90' C89' C88' 120.0 . . ? C91' C90' C89' 120.0 . . ? C90' C91' C86' 120.0 . . ? C90' C91' C85 118.1(32) . . ? C86' C91' C85 121.9(32) . . ? _refine_diff_density_max 1.309 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.135 #===END data_Compound_8 _database_code_CSD 204859 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C94 H97 N O5 P4 Pd4 S3' _chemical_formula_weight 1966.39 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 15.8551(8) _cell_length_b 16.7489(9) _cell_length_c 18.9814(8) _cell_angle_alpha 83.375(5) _cell_angle_beta 67.888(5) _cell_angle_gamma 72.737(7) _cell_volume 4459.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 10.58 _cell_measurement_theta_max 28.04 _exptl_crystal_description rhombs _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 8.137 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0551 _exptl_absorpt_correction_T_max 0.4845 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13799 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 59.99 _reflns_number_total 13214 _reflns_number_observed 9944 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 955 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+166.4998P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12259 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 1300 _refine_ls_R_factor_all 0.1714 _refine_ls_R_factor_obs 0.1332 _refine_ls_wR_factor_all 0.3408 _refine_ls_wR_factor_obs 0.3034 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.072 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 1.38797(11) 1.32221(9) 0.81426(10) 0.0659(5) Uani 1 d . . Pd2 Pd 1.30416(9) 1.20488(11) 0.80187(8) 0.0657(5) Uani 1 d D . Pd3 Pd 1.49532(9) 1.20419(8) 0.70138(7) 0.0474(4) Uani 1 d . . Pd4 Pd 1.31618(12) 1.34275(13) 0.69922(10) 0.0840(6) Uani 1 d . . S1 S 1.4634(4) 1.3516(3) 0.6882(4) 0.084(2) Uani 1 d . . S2 S 1.1895(4) 1.3095(5) 0.7711(3) 0.093(2) Uani 1 d . . O1 O 1.1226(11) 1.3705(13) 0.8292(10) 0.110(7) Uani 1 d . . O2 O 1.1414(12) 1.2738(15) 0.7339(11) 0.129(8) Uani 1 d . . S3 S 1.4499(3) 1.1061(3) 0.7783(2) 0.0514(10) Uani 1 d . . O3 O 1.4915(8) 1.0858(8) 0.8381(6) 0.058(3) Uani 1 d . . O4 O 1.4549(10) 1.0309(9) 0.7428(7) 0.070(4) Uani 1 d . . P1 P 1.4446(4) 1.4115(5) 0.8530(6) 0.119(3) Uani 1 d . . P2 P 1.2204(5) 1.1080(6) 0.8215(3) 0.114(3) Uani 1 d D . P3 P 1.6343(3) 1.1152(3) 0.6279(2) 0.0485(10) Uani 1 d . . P4 P 1.2619(5) 1.4060(5) 0.6048(4) 0.095(2) Uani 1 d . . C1 C 1.3169(15) 1.2795(14) 0.9189(14) 0.074(6) Uani 1 d DU . N1 N 1.2878(16) 1.2626(11) 0.9784(12) 0.084(6) Uani 1 d . . C2 C 1.2433(17) 1.2356(18) 1.0554(15) 0.063(5) Uani 0.50 d PDU 4 C3 C 1.2774(20) 1.1488(19) 1.0724(17) 0.063(5) Uani 0.50 d PDU 4 C4 C 1.2342(21) 1.1262(21) 1.1506(19) 0.065(6) Uani 0.50 d PDU 4 H4A H 1.2526(21) 1.0698(21) 1.1664(19) 0.078 Uiso 0.50 calc PR 4 C5 C 1.1654(21) 1.1858(20) 1.2039(19) 0.066(6) Uani 0.50 d PDU 4 H5A H 1.1370(21) 1.1689(20) 1.2548(19) 0.079 Uiso 0.50 calc PR 4 C6 C 1.1381(19) 1.2684(20) 1.1840(17) 0.070(6) Uani 0.50 d PDU 4 H6A H 1.0925(19) 1.3080(20) 1.2213(17) 0.083 Uiso 0.50 calc PR 4 C7 C 1.1780(17) 1.2944(17) 1.1075(14) 0.057(5) Uani 0.50 d PDU 4 C8 C 1.3487(20) 1.0874(19) 1.0164(19) 0.059(7) Uani 0.50 d PDU 4 H8A H 1.4113(20) 1.0943(19) 1.0070(19) 0.089 Uiso 0.50 d PR 4 H8B H 1.3368(20) 1.0954(19) 0.9686(19) 0.089 Uiso 0.50 d PR 4 H8C H 1.3466(20) 1.0311(19) 1.0362(19) 0.089 Uiso 0.50 d PR 4 C9 C 1.1460(21) 1.3825(19) 1.0863(20) 0.057(7) Uani 0.50 d PDU 4 H9A H 1.0989(21) 1.4160(19) 1.1303(20) 0.085 Uiso 0.50 d PR 4 H9B H 1.1179(21) 1.3840(19) 1.0480(20) 0.085 Uiso 0.50 d PR 4 H9C H 1.2006(21) 1.4055(19) 1.0644(20) 0.085 Uiso 0.50 d PR 4 C2' C 1.2606(22) 1.2460(14) 1.0546(16) 0.074(6) Uani 0.50 d PDU 5 C3' C 1.3338(25) 1.2024(16) 1.0835(17) 0.081(6) Uani 0.50 d PDU 5 C4' C 1.2962(27) 1.1850(19) 1.1624(20) 0.079(6) Uani 0.50 d PDU 5 H4'A H 1.3381(27) 1.1564(19) 1.1878(20) 0.095 Uiso 0.50 calc PR 5 C5' C 1.1973(26) 1.2095(19) 1.2043(19) 0.082(7) Uani 0.50 d PDU 5 H5'A H 1.1749(26) 1.1952(19) 1.2567(19) 0.099 Uiso 0.50 calc PR 5 C6' C 1.1328(25) 1.2528(18) 1.1720(18) 0.080(6) Uani 0.50 d PDU 5 H6'A H 1.0672(25) 1.2697(18) 1.2018(18) 0.096 Uiso 0.50 calc PR 5 C7' C 1.1651(21) 1.2718(17) 1.0944(16) 0.083(7) Uani 0.50 d PDU 5 C8' C 1.4338(25) 1.1790(21) 1.0348(23) 0.087(9) Uani 0.50 d PDU 5 H8'1 H 1.4581(25) 1.2280(21) 1.0169(23) 0.131 Uiso 0.50 d PR 5 H8'2 H 1.4414(25) 1.1481(21) 0.9911(23) 0.131 Uiso 0.50 d PR 5 H8'3 H 1.4693(25) 1.1428(21) 1.0645(23) 0.131 Uiso 0.50 d PR 5 C9' C 1.1023(28) 1.3165(21) 1.0525(24) 0.103(10) Uani 0.50 d PDU 5 H9'1 H 1.0352(28) 1.3273(21) 1.0849(24) 0.154 Uiso 0.50 d PR 5 H9'2 H 1.1163(28) 1.2793(21) 1.0109(24) 0.154 Uiso 0.50 d PR 5 H9'3 H 1.1161(28) 1.3694(21) 1.0314(24) 0.154 Uiso 0.50 d PR 5 C10 C 1.3712(18) 1.5199(16) 0.8568(17) 0.108(9) Uani 1 d U . H10A H 1.4035(18) 1.5559(16) 0.8689(17) 0.130 Uiso 1 calc R . H10B H 1.3702(18) 1.5357(16) 0.8052(17) 0.130 Uiso 1 calc R . C11 C 1.2080(9) 1.5081(7) 0.8988(7) 0.056(5) Uani 1 d G . H11A H 1.2276(9) 1.4722(7) 0.8569(7) 0.067 Uiso 1 calc R . C12 C 1.1143(8) 1.5283(8) 0.9485(8) 0.075(6) Uani 1 d G . H12A H 1.0699(10) 1.5062(12) 0.9407(13) 0.090 Uiso 1 calc R . C13 C 1.0857(8) 1.5808(8) 1.0098(7) 0.075(7) Uani 1 d G . H13A H 1.0216(9) 1.5946(12) 1.0438(10) 0.090 Uiso 1 calc R . C14 C 1.1507(11) 1.6132(8) 1.0213(7) 0.084(7) Uani 1 d G . H14A H 1.1311(16) 1.6491(12) 1.0631(9) 0.101 Uiso 1 calc R . C15 C 1.2444(10) 1.5930(9) 0.9715(9) 0.104(8) Uani 1 d GU . H15A H 1.2888(13) 1.6152(14) 0.9794(14) 0.125 Uiso 1 calc R . C16 C 1.2730(7) 1.5405(8) 0.9103(8) 0.077(7) Uani 1 d G . C17 C 1.5664(18) 1.4123(15) 0.7965(15) 0.126(11) Uani 1 d DU . H17A H 1.6084(18) 1.3563(15) 0.8003(15) 0.151 Uiso 0.50 calc PR 1 H17B H 1.5722(18) 1.4213(15) 0.7426(15) 0.151 Uiso 0.50 calc PR 1 H17C H 1.5675(18) 1.4127(15) 0.7456(15) 0.151 Uiso 0.50 d PR 2 H17D H 1.6136(18) 1.3630(15) 0.8016(15) 0.151 Uiso 0.50 d PR 2 C18 C 1.5869(23) 1.5526(15) 0.7825(16) 0.070(12) Uani 0.50 d PGDU 1 H18A H 1.5550(23) 1.5643(15) 0.7474(16) 0.084 Uiso 0.50 calc PR 1 C19 C 1.6188(27) 1.6139(14) 0.8000(19) 0.086(14) Uani 0.50 d PGDU 1 H19A H 1.6087(38) 1.6675(16) 0.7769(27) 0.103 Uiso 0.50 calc PR 1 C20 C 1.6654(23) 1.5966(19) 0.8513(18) 0.064(12) Uani 0.50 d PGDU 1 H20A H 1.6872(30) 1.6385(23) 0.8633(23) 0.077 Uiso 0.50 calc PR 1 C21 C 1.6802(26) 1.5181(21) 0.8852(19) 0.096(20) Uani 0.50 d PGDU 1 H21A H 1.7121(37) 1.5064(29) 0.9203(27) 0.115 Uiso 0.50 calc PR 1 C22 C 1.6484(23) 1.4569(16) 0.8677(18) 0.080(14) Uani 0.50 d PGDU 1 H22A H 1.6585(34) 1.4032(18) 0.8909(25) 0.096 Uiso 0.50 calc PR 1 C23 C 1.6017(15) 1.4741(12) 0.8164(13) 0.157(41) Uani 0.50 d PGDU 1 C18' C 1.5643(28) 1.5619(17) 0.7705(23) 0.113(22) Uani 0.50 d PGDU 2 H18' H 1.5229(28) 1.5676(17) 0.7437(23) 0.136 Uiso 0.50 calc PR 2 C19' C 1.5927(34) 1.6303(16) 0.7781(28) 0.167(34) Uani 0.50 d PGDU 2 H19' H 1.5708(49) 1.6828(19) 0.7566(40) 0.200 Uiso 0.50 calc PR 2 C20' C 1.6533(26) 1.6221(18) 0.8173(23) 0.074(13) Uani 0.50 d PGDU 2 H20' H 1.6728(33) 1.6688(22) 0.8226(30) 0.088 Uiso 0.50 calc PR 2 C21' C 1.6855(26) 1.5454(22) 0.8489(25) 0.104(21) Uani 0.50 d PGD 2 H21' H 1.7269(38) 1.5397(30) 0.8757(36) 0.125 Uiso 0.50 calc PR 2 C22' C 1.6570(25) 1.4770(17) 0.8412(22) 0.155(32) Uani 0.50 d PGDU 2 H22' H 1.6790(39) 1.4246(21) 0.8628(33) 0.186 Uiso 0.50 calc PR 2 C23' C 1.5964(16) 1.4853(14) 0.8020(14) 0.096(20) Uani 0.50 d PGDU 2 C24 C 1.4496(16) 1.3875(13) 0.9506(14) 0.119(10) Uani 1 d DU . H24A H 1.4610(16) 1.4359(13) 0.9671(14) 0.143 Uiso 0.70 calc PR 1 H24B H 1.3862(16) 1.3836(13) 0.9854(14) 0.143 Uiso 0.70 calc PR 1 H24C H 1.3957(16) 1.3691(13) 0.9831(14) 0.143 Uiso 0.30 d PR 2 H24D H 1.4488(16) 1.4369(13) 0.9722(14) 0.143 Uiso 0.30 d PR 2 C25 C 1.5733(16) 1.3193(13) 1.0026(13) 0.078(12) Uani 0.70 d PGDU 1 H25A H 1.5632(16) 1.3718(13) 1.0233(13) 0.094 Uiso 0.70 calc PR 1 C26 C 1.6416(16) 1.2499(16) 1.0135(15) 0.113(22) Uani 0.70 d PGD 1 H26A H 1.6781(23) 1.2550(21) 1.0417(21) 0.136 Uiso 0.70 calc PR 1 C27 C 1.6563(14) 1.1731(13) 0.9832(15) 0.125(18) Uani 0.70 d PGD 1 H27A H 1.7030(19) 1.1257(16) 0.9907(20) 0.150 Uiso 0.70 calc PR 1 C28 C 1.6028(14) 1.1656(9) 0.9420(13) 0.086(10) Uani 0.70 d PGD 1 H28A H 1.6129(21) 1.1131(9) 0.9213(18) 0.103 Uiso 0.70 calc PR 1 C29 C 1.5345(12) 1.2350(9) 0.9311(10) 0.054(6) Uani 0.70 d PGDU 1 H29A H 1.4979(17) 1.2299(12) 0.9030(14) 0.065 Uiso 0.70 calc PR 1 C30 C 1.5197(11) 1.3118(9) 0.9614(9) 0.069(8) Uani 0.70 d PGDU 1 C25' C 1.5648(42) 1.3033(39) 1.0059(27) 0.165(74) Uiso 0.30 d PGD 2 H25' H 1.5309(42) 1.3356(39) 1.0510(27) 0.198 Uiso 0.30 calc PR 2 C26' C 1.6454(50) 1.2384(47) 1.0008(37) 0.165(87) Uiso 0.30 d PGD 2 H26' H 1.6667(70) 1.2263(66) 1.0425(47) 0.198 Uiso 0.30 calc PR 2 C27' C 1.6949(34) 1.1911(33) 0.9348(37) 0.158(55) Uiso 0.30 d PGD 2 H27' H 1.7500(41) 1.1468(40) 0.9313(47) 0.190 Uiso 0.30 calc PR 2 C28' C 1.6638(25) 1.2088(24) 0.8739(29) 0.065(17) Uiso 0.30 d PGD 2 H28' H 1.6976(36) 1.1765(34) 0.8288(34) 0.078 Uiso 0.30 calc PR 2 C29' C 1.5831(24) 1.2737(22) 0.8790(20) 0.072(19) Uiso 0.30 d PGD 2 H29' H 1.5618(40) 1.2857(38) 0.8374(24) 0.087 Uiso 0.30 calc PR 2 C30' C 1.5336(19) 1.3209(16) 0.9450(18) 0.611(350) Uiso 0.30 d PGD 2 C31 C 1.2472(14) 1.0671(13) 0.7304(11) 0.118(10) Uani 1 d DU . H31A H 1.2817(14) 1.1042(13) 0.6941(11) 0.142 Uiso 0.65 calc PR 1 H31B H 1.2953(14) 1.0130(13) 0.7281(11) 0.142 Uiso 0.65 calc PR 1 H31C H 1.3080(14) 1.0269(13) 0.7194(11) 0.142 Uiso 0.35 d PR 2 H31D H 1.2574(14) 1.1124(13) 0.6953(11) 0.142 Uiso 0.35 d PR 2 C32 C 1.1481(14) 0.9851(12) 0.7170(10) 0.052(7) Uani 0.65 d PGD 1 H32A H 1.1580(14) 0.9493(12) 0.7575(10) 0.063 Uiso 0.65 calc PR 1 C33 C 1.0923(15) 0.9718(14) 0.6803(13) 0.079(11) Uani 0.65 d PGD 1 H33A H 1.0640(22) 0.9269(18) 0.6958(18) 0.095 Uiso 0.65 calc PR 1 C34 C 1.0779(15) 1.0241(17) 0.6211(13) 0.088(13) Uani 0.65 d PGD 1 H34A H 1.0398(20) 1.0150(22) 0.5961(17) 0.105 Uiso 0.65 calc PR 1 C35 C 1.1194(18) 1.0898(15) 0.5985(12) 0.111(17) Uani 0.65 d PGD 1 H35A H 1.1095(26) 1.1255(19) 0.5580(15) 0.133 Uiso 0.65 calc PR 1 C36 C 1.1752(16) 1.1030(11) 0.6351(11) 0.126(21) Uani 0.65 d PGD 1 H36A H 1.2035(22) 1.1479(14) 0.6196(16) 0.152 Uiso 0.65 calc PR 1 C37 C 1.1896(10) 1.0507(11) 0.6943(9) 0.060(9) Uani 0.65 d PGD 1 C32' C 1.2030(22) 0.9427(15) 0.7239(19) 0.057(13) Uiso 0.35 d PGD 2 H32' H 1.2426(22) 0.9141(15) 0.7513(19) 0.068 Uiso 0.35 calc PR 2 C33' C 1.1543(28) 0.9001(18) 0.7014(24) 0.070(16) Uiso 0.35 d PGD 2 H33' H 1.1606(39) 0.8424(20) 0.7134(33) 0.084 Uiso 0.35 calc PR 2 C34' C 1.0964(28) 0.9418(26) 0.6614(25) 0.133(42) Uiso 0.35 d PGD 2 H34' H 1.0631(36) 0.9127(32) 0.6460(33) 0.160 Uiso 0.35 calc PR 2 C35' C 1.0871(31) 1.0261(26) 0.6439(28) 0.073(21) Uiso 0.35 d PGD 2 H35' H 1.0475(42) 1.0547(33) 0.6165(38) 0.088 Uiso 0.35 calc PR 2 C36' C 1.1358(26) 1.0687(19) 0.6664(23) 0.076(18) Uiso 0.35 d PGD 2 H36' H 1.1294(36) 1.1263(20) 0.6544(32) 0.091 Uiso 0.35 calc PR 2 C37' C 1.1937(15) 1.0270(15) 0.7064(13) 0.044(15) Uiso 0.35 d PGD 2 C38 C 1.2490(15) 1.0213(11) 0.8753(11) 0.101(8) Uani 1 d DU . H38A H 1.3167(15) 1.0122(11) 0.8670(11) 0.121 Uiso 0.50 calc PR 1 H38B H 1.2134(15) 1.0390(11) 0.9290(11) 0.121 Uiso 0.50 calc PR 1 H38C H 1.3146(15) 0.9934(11) 0.8494(11) 0.121 Uiso 0.50 d PR 2 H38D H 1.2134(15) 0.9854(11) 0.8720(11) 0.121 Uiso 0.50 d PR 2 C39 C 1.3141(17) 0.8749(15) 0.8294(17) 0.091(14) Uani 0.50 d PGDU 1 H39A H 1.3744(17) 0.8846(15) 0.8034(17) 0.109 Uiso 0.50 calc PR 1 C40 C 1.3017(23) 0.7970(14) 0.8252(20) 0.163(30) Uani 0.50 d PGDU 1 H40A H 1.3535(28) 0.7536(17) 0.7964(28) 0.196 Uiso 0.50 calc PR 1 C41 C 1.2135(26) 0.7828(15) 0.8632(19) 0.076(12) Uani 0.50 d PGDU 1 H41A H 1.2050(34) 0.7296(17) 0.8603(25) 0.091 Uiso 0.50 calc PR 1 C42 C 1.1377(21) 0.8464(20) 0.9053(22) 0.245(53) Uani 0.50 d PGDU 1 H42A H 1.0774(25) 0.8367(27) 0.9313(31) 0.294 Uiso 0.50 calc PR 1 C43 C 1.1501(17) 0.9242(17) 0.9095(18) 0.101(16) Uani 0.50 d PGDU 1 H43A H 1.0983(19) 0.9677(21) 0.9383(26) 0.122 Uiso 0.50 calc PR 1 C44 C 1.2383(16) 0.9385(12) 0.8715(12) 0.098(15) Uani 0.50 d PGDU 1 C39' C 1.1417(18) 1.0313(23) 1.0095(14) 0.110(18) Uani 0.50 d PGDU 2 H39B H 1.0926(18) 1.0259(23) 0.9949(14) 0.132 Uiso 0.50 calc PR 2 C40' C 1.1257(25) 1.0398(27) 1.0858(13) 0.137(24) Uani 0.50 d PGDU 2 H40B H 1.0656(29) 1.0402(38) 1.1234(16) 0.164 Uiso 0.50 calc PR 2 C41' C 1.1976(32) 1.0477(23) 1.1072(13) 0.155(28) Uani 0.50 d PGDU 2 H41B H 1.1867(40) 1.0535(30) 1.1593(14) 0.186 Uiso 0.50 calc PR 2 C42' C 1.2856(28) 1.0471(23) 1.0522(18) 0.113(18) Uani 0.50 d PGDU 2 H42B H 1.3348(34) 1.0525(32) 1.0668(24) 0.135 Uiso 0.50 calc PR 2 C43' C 1.3016(19) 1.0386(18) 0.9759(16) 0.097(17) Uani 0.50 d PGD 2 H43B H 1.3617(19) 1.0382(28) 0.9383(20) 0.117 Uiso 0.50 calc PR 2 C44' C 1.2297(16) 1.0307(12) 0.9546(11) 0.086(15) Uani 0.50 d PGD 2 C45 C 1.0961(13) 1.1477(15) 0.8583(10) 0.137(12) Uani 1 d DU . H45A H 1.0800(13) 1.1417(15) 0.9140(10) 0.165 Uiso 0.40 calc PR 1 H45B H 1.0857(13) 1.2085(15) 0.8480(10) 0.165 Uiso 0.40 calc PR 1 H45C H 1.0751(13) 1.1079(15) 0.8413(10) 0.165 Uiso 0.40 d PR 2 H45D H 1.0786(13) 1.1992(15) 0.8326(10) 0.165 Uiso 0.40 d PR 2 H45E H 1.0689(13) 1.1101(15) 0.8453(10) 0.165 Uiso 0.20 d PR 3 H45F H 1.0726(13) 1.2029(15) 0.8409(10) 0.165 Uiso 0.20 d PR 3 C46 C 0.9625(20) 1.1869(16) 0.8118(18) 0.107(22) Uiso 0.40 d PGD 1 H46A H 0.9734(20) 1.2401(16) 0.7965(18) 0.128 Uiso 0.40 calc PR 1 C47 C 0.8904(21) 1.1663(22) 0.7994(21) 0.070(14) Uiso 0.40 d PGD 1 H47A H 0.8521(29) 1.2055(27) 0.7757(29) 0.083 Uiso 0.40 calc PR 1 C48 C 0.8744(20) 1.0885(24) 0.8217(20) 0.139(31) Uiso 0.40 d PGD 1 H48A H 0.8252(24) 1.0744(30) 0.8132(26) 0.167 Uiso 0.40 calc PR 1 C49 C 0.9304(23) 1.0312(19) 0.8563(21) 0.073(14) Uiso 0.40 d PGD 1 H49A H 0.9195(32) 0.9780(22) 0.8716(29) 0.088 Uiso 0.40 calc PR 1 C50 C 1.0025(19) 1.0517(15) 0.8687(17) 0.070(14) Uiso 0.40 d PGD 1 H50A H 1.0408(26) 1.0125(18) 0.8925(24) 0.084 Uiso 0.40 calc PR 1 C51 C 1.0185(13) 1.1296(15) 0.8465(12) 0.081(16) Uiso 0.40 d PGD 1 C46' C 1.0672(15) 1.1917(17) 0.9846(11) 0.020(7) Uiso 0.40 d PGD 2 H46B H 1.1277(15) 1.2020(17) 0.9651(11) 0.023 Uiso 0.40 calc PR 2 C47' C 1.0108(20) 1.2067(21) 1.0608(11) 0.067(17) Uiso 0.40 d PGD 2 H47B H 1.0326(27) 1.2274(30) 1.0933(14) 0.080 Uiso 0.40 calc PR 2 C48' C 0.9223(19) 1.1916(21) 1.0894(10) 0.099(20) Uiso 0.40 d PGD 2 H48B H 0.8837(24) 1.2019(28) 1.1415(11) 0.119 Uiso 0.40 calc PR 2 C49' C 0.8903(15) 1.1614(23) 1.0418(14) 0.079(15) Uiso 0.40 d PGD 2 H49B H 0.8299(19) 1.1510(32) 1.0614(19) 0.094 Uiso 0.40 calc PR 2 C50' C 0.9468(15) 1.1463(19) 0.9656(13) 0.059(12) Uiso 0.40 d PGD 2 H50B H 0.9250(20) 1.1256(27) 0.9331(17) 0.071 Uiso 0.40 calc PR 2 C51' C 1.0353(12) 1.1614(12) 0.9370(9) 0.063(12) Uiso 0.40 d PGD 2 C46" C 1.0752(56) 1.0699(24) 0.9800(19) 0.158(73) Uiso 0.20 d PGD 3 H46C H 1.0885(56) 1.0198(24) 0.9541(19) 0.190 Uiso 0.20 calc PR 3 C47" C 1.0553(65) 1.0683(34) 1.0579(20) 0.106(43) Uiso 0.20 d PGD 3 H47C H 1.0551(95) 1.0171(39) 1.0853(28) 0.128 Uiso 0.20 calc PR 3 C48" C 1.0357(44) 1.1417(38) 1.0958(13) 0.071(28) Uiso 0.20 d PGD 3 H48C H 1.0222(55) 1.1406(48) 1.1491(14) 0.086 Uiso 0.20 calc PR 3 C49" C 1.0360(45) 1.2166(32) 1.0558(17) 0.026(15) Uiso 0.20 d PGD 3 H49C H 1.0227(69) 1.2667(37) 1.0818(25) 0.032 Uiso 0.20 calc PR 3 C50" C 1.0559(41) 1.2182(22) 0.9779(17) 0.099(50) Uiso 0.20 d PGD 3 H50C H 1.0561(68) 1.2694(22) 0.9506(24) 0.119 Uiso 0.20 calc PR 3 C51" C 1.0754(21) 1.1449(20) 0.9400(12) 0.171(83) Uiso 0.20 d PGD 3 C52 C 1.6174(13) 1.0415(10) 0.5743(10) 0.052(4) Uani 1 d . . H52A H 1.6804(13) 1.0054(10) 0.5443(10) 0.062 Uiso 1 calc R . H52B H 1.5820(13) 1.0051(10) 0.6108(10) 0.062 Uiso 1 calc R . C53 C 1.4670(8) 1.1018(8) 0.5471(6) 0.058(5) Uani 1 d G . H53A H 1.4320(8) 1.0964(8) 0.5996(6) 0.070 Uiso 1 calc R . C54 C 1.4199(9) 1.1316(9) 0.4966(9) 0.085(7) Uani 1 d G . H54A H 1.3527(9) 1.1465(14) 0.5147(13) 0.102 Uiso 1 calc R . C55 C 1.4712(13) 1.1394(9) 0.4198(8) 0.103(10) Uani 1 d G . H55A H 1.4390(17) 1.1598(14) 0.3853(11) 0.123 Uiso 1 calc R . C56 C 1.5695(13) 1.1175(10) 0.3934(5) 0.107(10) Uani 1 d G . H56A H 1.6045(17) 1.1229(14) 0.3409(5) 0.128 Uiso 1 calc R . C57 C 1.6166(9) 1.0878(9) 0.4439(6) 0.084(8) Uani 1 d G . H57A H 1.6839(9) 1.0728(13) 0.4259(9) 0.101 Uiso 1 calc R . C58 C 1.5654(8) 1.0799(8) 0.5207(5) 0.055(5) Uani 1 d G . C59 C 1.7256(13) 1.1551(11) 0.5543(11) 0.058(5) Uani 1 d . . H59A H 1.7805(13) 1.1068(11) 0.5315(11) 0.070 Uiso 1 calc R . H59B H 1.7006(13) 1.1807(11) 0.5139(11) 0.070 Uiso 1 calc R . C60 C 1.7088(8) 1.3014(8) 0.5861(10) 0.099(9) Uani 1 d G . H60A H 1.6504(8) 1.3187(8) 0.5782(10) 0.118 Uiso 1 calc R . C61 C 1.7422(10) 1.3596(6) 0.6068(10) 0.100(9) Uani 1 d G . H61A H 1.7065(13) 1.4166(7) 0.6129(14) 0.120 Uiso 1 calc R . C62 C 1.8277(11) 1.3342(8) 0.6184(8) 0.075(6) Uani 1 d G . H62A H 1.8505(15) 1.3740(11) 0.6325(12) 0.090 Uiso 1 calc R . C63 C 1.8800(9) 1.2507(9) 0.6095(9) 0.100(9) Uani 1 d G . H63A H 1.9384(11) 1.2334(13) 0.6174(14) 0.120 Uiso 1 calc R . C64 C 1.8466(9) 1.1925(6) 0.5888(9) 0.084(7) Uani 1 d G . H64A H 1.8823(12) 1.1355(7) 0.5827(13) 0.101 Uiso 1 calc R . C65 C 1.7611(9) 1.2179(7) 0.5772(8) 0.061(5) Uani 1 d G . C66 C 1.6960(13) 1.0457(10) 0.6873(11) 0.056(5) Uani 1 d . . H66A H 1.7250(13) 1.0790(10) 0.7065(11) 0.068 Uiso 1 calc R . H66B H 1.6479(13) 1.0280(10) 0.7320(11) 0.068 Uiso 1 calc R . C67 C 1.8677(8) 0.9658(6) 0.6192(7) 0.060(5) Uani 1 d G . H67A H 1.8866(8) 1.0137(6) 0.6218(7) 0.073 Uiso 1 calc R . C68 C 1.9352(7) 0.8933(8) 0.5847(9) 0.092(8) Uani 1 d G . H68A H 2.0003(7) 0.8918(12) 0.5637(12) 0.111 Uiso 1 calc R . C69 C 1.9074(10) 0.8231(7) 0.5809(9) 0.093(8) Uani 1 d G . H69A H 1.9536(12) 0.7736(8) 0.5573(12) 0.112 Uiso 1 calc R . C70 C 1.8121(11) 0.8254(6) 0.6115(8) 0.070(6) Uani 1 d G . H70A H 1.7932(14) 0.7774(7) 0.6089(12) 0.084 Uiso 1 calc R . C71 C 1.7446(7) 0.8978(7) 0.6460(7) 0.065(5) Uani 1 d G . H71A H 1.6795(8) 0.8994(10) 0.6670(11) 0.079 Uiso 1 calc R . C72 C 1.7724(7) 0.9680(5) 0.6498(6) 0.044(4) Uani 1 d G . C73 C 1.2449(21) 1.3262(16) 0.5544(15) 0.102(10) Uani 1 d . . H73A H 1.3082(21) 1.2901(16) 0.5250(15) 0.123 Uiso 1 calc R . H73B H 1.2111(21) 1.2905(16) 0.5932(15) 0.123 Uiso 1 calc R . C74 C 1.0952(10) 1.3654(9) 0.5235(6) 0.078(7) Uani 1 d G . H74A H 1.0618(10) 1.3486(9) 0.5732(6) 0.094 Uiso 1 calc R . C75 C 1.0479(8) 1.3975(9) 0.4735(8) 0.073(6) Uani 1 d G . H75A H 0.9821(8) 1.4025(13) 0.4891(11) 0.088 Uiso 1 calc R . C76 C 1.0967(10) 1.4221(9) 0.4007(7) 0.073(6) Uani 1 d G . H76A H 1.0644(13) 1.4440(12) 0.3665(10) 0.087 Uiso 1 calc R . C77 C 1.1929(10) 1.4146(9) 0.3779(6) 0.076(6) Uani 1 d G . H77A H 1.2263(13) 1.4315(13) 0.3281(7) 0.091 Uiso 1 calc R . C78 C 1.2403(7) 1.3826(9) 0.4279(7) 0.073(6) Uani 1 d G . H78A H 1.3060(8) 1.3775(13) 0.4123(11) 0.087 Uiso 1 calc R . C79 C 1.1914(10) 1.3580(8) 0.5007(7) 0.069(6) Uani 1 d G . C80 C 1.1448(18) 1.4815(16) 0.6357(16) 0.104(10) Uani 1 d . . H80A H 1.1223(18) 1.4922(16) 0.5924(16) 0.125 Uiso 1 calc R . H80B H 1.1008(18) 1.4553(16) 0.6767(16) 0.125 Uiso 1 calc R . C81 C 1.1348(12) 1.6331(11) 0.6167(7) 0.111(11) Uani 1 d G . H81A H 1.1374(12) 1.6291(11) 0.5664(7) 0.133 Uiso 1 calc R . C82 C 1.1281(12) 1.7094(9) 0.6436(8) 0.107(10) Uani 1 d G . H82A H 1.1261(17) 1.7574(11) 0.6117(11) 0.128 Uiso 1 calc R . C83 C 1.1244(11) 1.7153(7) 0.7172(9) 0.090(8) Uani 1 d G . H83A H 1.1199(17) 1.7675(8) 0.7355(12) 0.108 Uiso 1 calc R . C84 C 1.1275(11) 1.6450(9) 0.7639(7) 0.089(8) Uani 1 d G . H84A H 1.1249(17) 1.6491(13) 0.8142(7) 0.107 Uiso 1 calc R . C85 C 1.1342(11) 1.5688(8) 0.7370(8) 0.090(8) Uani 1 d G . H85A H 1.1362(16) 1.5207(9) 0.7689(11) 0.107 Uiso 1 calc R . C86 C 1.1379(11) 1.5628(9) 0.6634(9) 0.100(10) Uani 1 d G . C87 C 1.3277(18) 1.4704(14) 0.5333(14) 0.092(8) Uani 1 d . . H87A H 1.2902(18) 1.4969(14) 0.5010(14) 0.111 Uiso 1 calc R . H87B H 1.3312(18) 1.5158(14) 0.5602(14) 0.111 Uiso 1 calc R . C88 C 1.4729(11) 1.4742(6) 0.4198(10) 0.092(8) Uani 1 d G . H88A H 1.4393(11) 1.5296(6) 0.4119(10) 0.110 Uiso 1 calc R . C89 C 1.5653(11) 1.4405(8) 0.3709(9) 0.118(12) Uani 1 d G . H89A H 1.5948(15) 1.4728(12) 0.3297(13) 0.142 Uiso 1 calc R . C90 C 1.6145(8) 1.3593(9) 0.3824(8) 0.071(6) Uani 1 d G . H90A H 1.6776(9) 1.3363(12) 0.3490(11) 0.085 Uiso 1 calc R . C91 C 1.5713(10) 1.3120(7) 0.4427(9) 0.093(8) Uani 1 d G . H91A H 1.6049(14) 1.2565(8) 0.4505(12) 0.111 Uiso 1 calc R . C92 C 1.4789(11) 1.3457(8) 0.4915(8) 0.130(13) Uani 1 d G . H92A H 1.4494(14) 1.3133(12) 0.5328(10) 0.156 Uiso 1 calc R . C93 C 1.4297(9) 1.4268(8) 0.4801(8) 0.084(8) Uani 1 d G . O100 O 1.4852(24) 1.1277(13) 1.2221(15) 0.078(9) Uani 0.50 d P 1 H100 H 1.5348(24) 1.1425(13) 1.2114(15) 0.117 Uiso 0.50 d PR 1 C101 C 1.4606(30) 1.1307(23) 1.1590(26) 0.072(13) Uani 0.50 d P 1 H10C H 1.3994(30) 1.1189(23) 1.1726(26) 0.109 Uiso 0.50 d PR 1 H10D H 1.5097(30) 1.0896(23) 1.1217(26) 0.109 Uiso 0.50 d PR 1 H10E H 1.4568(30) 1.1870(23) 1.1371(26) 0.109 Uiso 0.50 d PR 1 O105 O 0.9685(31) 1.3177(37) 0.7239(28) 0.154(18) Uani 0.50 d PU . H105 H 1.0228(31) 1.2915(37) 0.7236(28) 0.231 Uiso 0.50 d PR . C106 C 0.9549(40) 1.3975(33) 0.7255(34) 0.102(17) Uani 0.50 d PU . H10F H 0.9380(40) 1.4204(33) 0.6812(34) 0.152 Uiso 0.50 d PR . H10G H 1.0153(40) 1.4069(33) 0.7197(34) 0.152 Uiso 0.50 d PR . H10H H 0.9054(40) 1.4254(33) 0.7717(34) 0.152 Uiso 0.50 d PR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0625(9) 0.0523(9) 0.0904(11) -0.0190(8) -0.0427(8) 0.0003(7) Pd2 0.0446(7) 0.1055(13) 0.0506(8) -0.0237(8) -0.0105(6) -0.0256(8) Pd3 0.0470(7) 0.0406(7) 0.0475(7) 0.0061(5) -0.0121(6) -0.0109(5) Pd4 0.0648(10) 0.0999(14) 0.0769(11) -0.0279(10) -0.0358(9) 0.0161(9) S1 0.082(4) 0.043(3) 0.123(5) 0.015(3) -0.048(4) -0.003(3) S2 0.053(3) 0.145(6) 0.079(4) -0.048(4) -0.029(3) 0.004(3) O1 0.062(9) 0.149(17) 0.102(13) -0.069(12) -0.023(9) 0.011(10) O2 0.087(12) 0.195(22) 0.124(15) -0.071(15) -0.064(11) -0.008(13) S3 0.052(2) 0.062(3) 0.041(2) -0.003(2) -0.009(2) -0.027(2) O3 0.059(7) 0.062(8) 0.040(6) 0.014(6) -0.005(6) -0.021(6) O4 0.078(9) 0.083(10) 0.048(7) -0.006(7) 0.007(6) -0.056(8) P1 0.055(3) 0.090(5) 0.203(9) -0.092(6) -0.016(4) -0.013(3) P2 0.095(5) 0.230(10) 0.043(3) -0.031(4) 0.010(3) -0.120(6) P3 0.050(2) 0.040(2) 0.046(2) 0.012(2) -0.012(2) -0.011(2) P4 0.088(4) 0.093(5) 0.095(5) -0.047(4) -0.053(4) 0.032(4) C1 0.089(13) 0.086(13) 0.068(12) -0.015(10) -0.051(11) -0.017(10) N1 0.135(18) 0.057(11) 0.084(14) -0.016(10) -0.080(14) -0.004(11) C2 0.076(10) 0.061(10) 0.076(10) 0.002(9) -0.045(9) -0.033(9) C3 0.072(10) 0.055(10) 0.080(10) 0.007(9) -0.035(9) -0.039(9) C4 0.076(10) 0.053(10) 0.081(10) 0.008(9) -0.034(9) -0.037(9) C5 0.075(10) 0.060(10) 0.082(10) 0.003(9) -0.038(9) -0.036(9) C6 0.077(10) 0.062(10) 0.086(10) 0.003(9) -0.035(9) -0.036(9) C7 0.068(10) 0.050(10) 0.085(10) 0.007(9) -0.038(9) -0.049(8) C8 0.070(13) 0.041(12) 0.080(14) 0.008(12) -0.024(12) -0.044(11) C9 0.067(13) 0.047(13) 0.069(14) 0.005(12) -0.028(12) -0.033(11) C2' 0.086(10) 0.061(10) 0.085(10) 0.005(9) -0.038(9) -0.027(9) C3' 0.085(10) 0.067(10) 0.090(11) 0.007(9) -0.028(9) -0.027(9) C4' 0.086(10) 0.065(10) 0.091(11) 0.011(9) -0.029(9) -0.034(9) C5' 0.087(11) 0.070(10) 0.090(11) 0.007(9) -0.031(10) -0.025(9) C6' 0.083(10) 0.064(10) 0.095(11) 0.008(9) -0.026(9) -0.031(9) C7' 0.083(10) 0.067(10) 0.096(11) 0.013(9) -0.029(10) -0.026(10) C8' 0.091(15) 0.071(14) 0.095(15) 0.025(14) -0.025(14) -0.036(13) C9' 0.099(15) 0.079(15) 0.106(16) 0.019(14) -0.017(15) -0.023(14) C10 0.089(14) 0.085(14) 0.132(16) -0.035(12) 0.008(12) -0.047(12) C11 0.064(12) 0.033(9) 0.064(12) 0.008(8) -0.028(10) -0.002(8) C12 0.070(14) 0.053(12) 0.103(18) 0.006(12) -0.036(13) -0.015(10) C13 0.073(14) 0.040(11) 0.065(13) 0.028(10) 0.001(11) 0.005(10) C14 0.098(18) 0.071(15) 0.067(14) -0.022(12) -0.025(13) 0.002(13) C15 0.090(14) 0.095(15) 0.129(16) -0.039(13) -0.036(12) -0.018(12) C16 0.064(12) 0.048(11) 0.109(18) -0.034(12) -0.007(12) -0.022(10) C17 0.122(13) 0.121(13) 0.135(14) -0.012(9) -0.038(9) -0.041(9) C18 0.061(14) 0.074(15) 0.073(15) 0.007(9) -0.020(10) -0.025(9) C19 0.082(16) 0.091(17) 0.088(16) -0.005(9) -0.027(10) -0.030(10) C20 0.056(17) 0.057(18) 0.068(19) 0.021(15) 0.006(13) -0.042(15) C21 0.091(25) 0.084(25) 0.110(27) -0.001(17) -0.021(17) -0.040(17) C22 0.077(16) 0.073(16) 0.085(16) 0.002(9) -0.016(10) -0.030(10) C23 0.157(42) 0.157(42) 0.158(41) -0.005(10) -0.055(17) -0.043(14) C18' 0.112(23) 0.122(24) 0.113(23) -0.006(10) -0.041(12) -0.039(11) C19' 0.163(35) 0.167(35) 0.166(35) 0.001(10) -0.058(15) -0.042(13) C20' 0.077(15) 0.079(16) 0.067(15) -0.004(9) -0.031(10) -0.018(9) C21' 0.064(33) 0.104(52) 0.138(60) -0.036(48) -0.018(35) -0.025(33) C22' 0.154(36) 0.148(36) 0.160(36) -0.019(19) -0.049(21) -0.042(20) C23' 0.080(24) 0.090(25) 0.110(26) -0.035(17) -0.008(16) -0.033(17) C24 0.122(17) 0.122(17) 0.135(17) -0.058(13) -0.058(14) -0.030(13) C25 0.075(17) 0.090(18) 0.090(19) -0.021(13) -0.022(13) -0.055(15) C26 0.105(34) 0.160(51) 0.124(36) -0.012(31) -0.051(26) -0.091(35) C27 0.077(25) 0.177(54) 0.146(42) 0.052(37) -0.075(29) -0.043(30) C28 0.095(24) 0.067(21) 0.125(30) 0.013(20) -0.073(23) -0.025(18) C29 0.071(13) 0.049(12) 0.052(12) 0.029(10) -0.025(10) -0.040(11) C30 0.065(14) 0.072(15) 0.084(15) -0.022(12) -0.041(12) -0.014(11) C31 0.122(13) 0.132(13) 0.110(13) -0.011(9) -0.039(9) -0.047(9) C32 0.075(19) 0.052(16) 0.032(13) 0.008(11) -0.010(13) -0.037(15) C33 0.080(24) 0.112(30) 0.076(23) 0.009(23) -0.033(19) -0.069(22) C34 0.091(27) 0.104(33) 0.101(31) -0.020(24) -0.057(25) -0.037(23) C35 0.124(36) 0.100(33) 0.118(36) -0.045(28) -0.073(31) 0.010(28) C36 0.154(44) 0.089(31) 0.068(26) -0.029(23) 0.049(28) -0.042(30) C37 0.048(17) 0.087(24) 0.061(20) -0.029(18) -0.015(15) -0.035(16) C38 0.100(11) 0.104(11) 0.106(11) -0.027(8) -0.021(8) -0.050(9) C39 0.091(20) 0.095(21) 0.097(21) 0.030(16) -0.032(15) -0.054(16) C40 0.165(31) 0.167(31) 0.156(31) 0.004(10) -0.063(14) -0.039(12) C41 0.089(19) 0.058(17) 0.080(19) -0.002(14) -0.013(15) -0.041(15) C42 0.251(56) 0.241(56) 0.245(56) 0.003(20) -0.087(27) -0.075(24) C43 0.109(23) 0.103(23) 0.102(23) 0.003(17) -0.037(17) -0.045(17) C44 0.109(22) 0.099(22) 0.100(22) 0.002(16) -0.031(16) -0.058(17) C39' 0.135(25) 0.104(24) 0.099(23) -0.010(17) -0.046(18) -0.037(18) C40' 0.148(29) 0.135(29) 0.129(29) 0.009(18) -0.046(19) -0.049(19) C41' 0.158(33) 0.157(33) 0.154(33) 0.003(19) -0.057(20) -0.049(20) C42' 0.120(24) 0.118(25) 0.103(24) 0.000(17) -0.055(18) -0.020(17) C43' 0.136(47) 0.046(25) 0.107(40) 0.017(25) -0.028(35) -0.046(28) C44' 0.086(32) 0.129(44) 0.054(25) 0.014(26) -0.012(23) -0.066(32) C45 0.133(14) 0.142(15) 0.140(15) 0.007(9) -0.046(10) -0.048(9) C52 0.063(11) 0.030(9) 0.054(10) 0.013(7) -0.019(9) -0.009(8) C53 0.074(13) 0.048(11) 0.053(11) 0.009(8) -0.026(10) -0.016(9) C54 0.111(19) 0.070(15) 0.095(18) 0.006(13) -0.066(16) -0.021(13) C55 0.197(32) 0.055(14) 0.083(18) 0.015(12) -0.100(21) -0.015(17) C56 0.180(30) 0.074(17) 0.047(13) 0.020(11) -0.049(17) -0.003(18) C57 0.109(18) 0.080(15) 0.021(9) 0.031(9) 0.004(10) -0.016(13) C58 0.089(14) 0.030(9) 0.036(9) 0.014(7) -0.018(9) -0.015(9) C59 0.060(11) 0.047(10) 0.063(12) 0.019(9) -0.014(9) -0.023(9) C60 0.064(14) 0.047(13) 0.177(28) 0.010(15) -0.034(16) -0.021(11) C61 0.067(15) 0.070(16) 0.138(24) 0.009(15) -0.018(15) -0.012(13) C62 0.084(15) 0.067(14) 0.066(13) 0.030(11) -0.009(11) -0.045(12) C63 0.066(14) 0.077(17) 0.139(24) 0.059(16) -0.033(15) -0.021(13) C64 0.080(15) 0.061(14) 0.112(19) 0.042(13) -0.038(14) -0.033(12) C65 0.051(11) 0.049(11) 0.058(11) 0.022(9) -0.001(9) -0.009(9) C66 0.067(12) 0.032(9) 0.069(12) 0.009(8) -0.030(10) -0.009(8) C67 0.067(12) 0.052(11) 0.062(12) 0.022(9) -0.025(10) -0.021(9) C68 0.067(14) 0.064(15) 0.115(20) -0.003(14) -0.008(14) -0.006(12) C69 0.122(22) 0.028(11) 0.126(22) -0.021(12) -0.054(18) 0.004(12) C70 0.104(17) 0.031(10) 0.089(15) 0.017(9) -0.057(14) -0.015(10) C71 0.070(13) 0.057(12) 0.070(13) 0.017(10) -0.033(11) -0.015(10) C72 0.067(11) 0.021(8) 0.043(9) 0.026(6) -0.020(8) -0.018(7) C73 0.136(23) 0.080(17) 0.089(17) -0.035(14) -0.069(17) 0.023(16) C74 0.080(15) 0.081(16) 0.062(13) -0.024(12) 0.001(12) -0.030(12) C75 0.082(14) 0.077(15) 0.077(15) -0.009(12) -0.030(12) -0.041(12) C76 0.102(17) 0.066(13) 0.055(12) 0.022(10) -0.024(12) -0.042(12) C77 0.084(15) 0.076(15) 0.057(12) -0.006(11) -0.008(11) -0.028(12) C78 0.072(13) 0.072(14) 0.069(14) -0.015(11) -0.024(11) -0.009(11) C79 0.117(18) 0.038(10) 0.035(10) -0.002(8) -0.020(11) -0.006(11) C80 0.094(17) 0.103(19) 0.119(20) -0.069(17) -0.072(16) 0.038(15) C81 0.092(18) 0.133(25) 0.106(20) -0.052(19) -0.070(17) 0.038(17) C82 0.124(22) 0.090(19) 0.089(18) -0.034(15) -0.069(17) 0.048(16) C83 0.100(18) 0.066(15) 0.089(17) -0.017(13) -0.054(15) 0.030(13) C84 0.091(16) 0.097(18) 0.075(15) -0.044(14) -0.046(13) 0.019(14) C85 0.082(15) 0.078(16) 0.100(18) -0.034(14) -0.049(14) 0.025(12) C86 0.088(16) 0.106(20) 0.108(19) -0.068(17) -0.074(15) 0.046(15) C87 0.115(20) 0.060(14) 0.079(16) 0.019(12) -0.037(15) 0.004(13) C88 0.111(20) 0.051(13) 0.123(21) 0.059(14) -0.058(17) -0.039(13) C89 0.086(18) 0.058(15) 0.179(30) 0.070(17) -0.040(19) -0.011(13) C90 0.086(15) 0.046(11) 0.092(16) 0.005(11) -0.045(13) -0.020(11) C91 0.119(20) 0.055(13) 0.074(15) -0.013(12) -0.038(15) 0.029(13) C92 0.136(26) 0.083(19) 0.100(21) 0.023(16) -0.023(19) 0.037(18) C93 0.096(16) 0.059(13) 0.106(18) -0.046(13) -0.078(15) 0.035(12) O100 0.150(28) 0.016(11) 0.071(18) 0.018(11) -0.056(19) -0.013(14) C101 0.081(28) 0.044(22) 0.111(35) 0.049(22) -0.044(26) -0.049(21) O105 0.121(26) 0.215(37) 0.166(30) -0.022(27) -0.112(24) -0.016(24) C106 0.111(29) 0.087(28) 0.136(32) 0.051(25) -0.097(26) -0.019(23) _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 C1 2.05(3) . ? Pd1 P1 2.264(6) . ? Pd1 S1 2.306(7) . ? Pd1 Pd2 2.752(2) . ? Pd1 Pd3 2.762(2) . ? Pd1 Pd4 2.766(2) . ? Pd2 P2 2.303(7) . ? Pd2 S2 2.321(7) . ? Pd2 S3 2.324(5) . ? Pd2 Pd4 2.847(3) . ? Pd2 Pd3 2.908(2) . ? Pd3 S3 2.169(5) . ? Pd3 P3 2.289(5) . ? Pd3 S1 2.372(5) . ? Pd3 Pd4 3.100(2) . ? Pd4 S2 2.152(7) . ? Pd4 P4 2.293(7) . ? Pd4 S1 2.313(7) . ? S2 O1 1.456(15) . ? S2 O2 1.49(2) . ? S3 O4 1.465(13) . ? S3 O3 1.476(13) . ? P1 C17 1.83(2) . ? P1 C10 1.84(3) . ? P1 C24 1.88(3) . ? P2 C38 1.73(2) . ? P2 C45 1.76(2) . ? P2 C31 1.79(2) . ? P3 C59 1.82(2) . ? P3 C52 1.82(2) . ? P3 C66 1.85(2) . ? P4 C80 1.83(2) . ? P4 C87 1.83(3) . ? P4 C73 1.87(2) . ? C1 N1 1.09(3) . ? N1 C2' 1.36(3) . ? N1 C2 1.45(3) . ? C2 C7 1.37(3) . ? C2 C3 1.44(4) . ? C3 C4 1.44(4) . ? C3 C8 1.46(4) . ? C4 C5 1.40(4) . ? C5 C6 1.37(4) . ? C6 C7 1.42(3) . ? C7 C9 1.47(4) . ? C2' C7' 1.37(4) . ? C2' C3' 1.44(4) . ? C3' C4' 1.42(4) . ? C3' C8' 1.46(4) . ? C4' C5' 1.42(4) . ? C5' C6' 1.37(4) . ? C6' C7' 1.40(3) . ? C7' C9' 1.48(4) . ? C10 C16 1.46(2) . ? C11 C12 1.39 . ? C11 C16 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C17 C23 1.45(2) . ? C17 C23' 1.46(2) . ? C18 C19 1.39 . ? C18 C23 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C18' C19' 1.39 . ? C18' C23' 1.39 . ? C19' C20' 1.39 . ? C20' C21' 1.39 . ? C21' C22' 1.39 . ? C22' C23' 1.39 . ? C24 C30' 1.44(2) . ? C24 C30 1.47(2) . ? C25 C26 1.39 . ? C25 C30 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C29 C30 1.39 . ? C25' C26' 1.39 . ? C25' C30' 1.39 . ? C26' C27' 1.39 . ? C27' C28' 1.39 . ? C28' C29' 1.39 . ? C29' C30' 1.39 . ? C31 C37 1.43(2) . ? C31 C37' 1.44(2) . ? C32 C33 1.39 . ? C32 C37 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? C36 C37 1.39 . ? C32' C33' 1.39 . ? C32' C37' 1.39 . ? C33' C34' 1.39 . ? C34' C35' 1.39 . ? C35' C36' 1.39 . ? C36' C37' 1.39 . ? C38 C44' 1.43(2) . ? C38 C44 1.46(2) . ? C39 C40 1.39 . ? C39 C44 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C42 C43 1.39 . ? C43 C44 1.39 . ? C39' C40' 1.39 . ? C39' C44' 1.39 . ? C40' C41' 1.39 . ? C41' C42' 1.39 . ? C42' C43' 1.39 . ? C43' C44' 1.39 . ? C45 C51' 1.44(2) . ? C45 C51 1.45(2) . ? C45 C51" 1.46(2) . ? C46 C47 1.39 . ? C46 C51 1.39 . ? C47 C48 1.39 . ? C48 C49 1.39 . ? C49 C50 1.39 . ? C50 C51 1.39 . ? C46' C47' 1.39 . ? C46' C51' 1.39 . ? C47' C48' 1.39 . ? C48' C49' 1.39 . ? C49' C50' 1.39 . ? C50' C51' 1.39 . ? C46" C47" 1.39 . ? C46" C51" 1.39 . ? C47" C48" 1.39 . ? C48" C49" 1.39 . ? C49" C50" 1.39 . ? C50" C51" 1.39 . ? C52 C58 1.51(2) . ? C53 C54 1.39 . ? C53 C58 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C56 C57 1.39 . ? C57 C58 1.39 . ? C59 C65 1.50(2) . ? C60 C61 1.39 . ? C60 C65 1.39 . ? C61 C62 1.39 . ? C62 C63 1.39 . ? C63 C64 1.39 . ? C64 C65 1.39 . ? C66 C72 1.52(2) . ? C67 C68 1.39 . ? C67 C72 1.39 . ? C68 C69 1.39 . ? C69 C70 1.39 . ? C70 C71 1.39 . ? C71 C72 1.39 . ? C73 C79 1.52(2) . ? C74 C75 1.39 . ? C74 C79 1.39 . ? C75 C76 1.39 . ? C76 C77 1.39 . ? C77 C78 1.39 . ? C78 C79 1.39 . ? C80 C86 1.47(3) . ? C81 C82 1.39 . ? C81 C86 1.39 . ? C82 C83 1.39 . ? C83 C84 1.39 . ? C84 C85 1.39 . ? C85 C86 1.39 . ? C87 C93 1.55(3) . ? C88 C89 1.39 . ? C88 C93 1.39 . ? C89 C90 1.39 . ? C90 C91 1.39 . ? C91 C92 1.39 . ? C92 C93 1.39 . ? O100 C101 1.38(5) . ? O105 C106 1.29(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 98.3(6) . . ? C1 Pd1 S1 170.0(5) . . ? P1 Pd1 S1 91.5(3) . . ? C1 Pd1 Pd2 68.7(5) . . ? P1 Pd1 Pd2 166.9(3) . . ? S1 Pd1 Pd2 101.5(2) . . ? C1 Pd1 Pd3 116.9(6) . . ? P1 Pd1 Pd3 124.7(2) . . ? S1 Pd1 Pd3 54.92(14) . . ? Pd2 Pd1 Pd3 63.65(5) . . ? C1 Pd1 Pd4 120.1(5) . . ? P1 Pd1 Pd4 128.8(3) . . ? S1 Pd1 Pd4 53.3(2) . . ? Pd2 Pd1 Pd4 62.13(7) . . ? Pd3 Pd1 Pd4 68.21(5) . . ? P2 Pd2 S2 92.6(3) . . ? P2 Pd2 S3 94.8(3) . . ? S2 Pd2 S3 155.9(2) . . ? P2 Pd2 Pd1 166.85(15) . . ? S2 Pd2 Pd1 90.2(2) . . ? S3 Pd2 Pd1 87.80(12) . . ? P2 Pd2 Pd4 130.5(2) . . ? S2 Pd2 Pd4 47.9(2) . . ? S3 Pd2 Pd4 112.12(12) . . ? Pd1 Pd2 Pd4 59.16(6) . . ? P2 Pd2 Pd3 131.5(2) . . ? S2 Pd2 Pd3 112.5(2) . . ? S3 Pd2 Pd3 47.38(11) . . ? Pd1 Pd2 Pd3 58.34(5) . . ? Pd4 Pd2 Pd3 65.16(5) . . ? S3 Pd3 P3 93.8(2) . . ? S3 Pd3 S1 142.5(2) . . ? P3 Pd3 S1 122.3(2) . . ? S3 Pd3 Pd1 90.71(12) . . ? P3 Pd3 Pd1 153.43(14) . . ? S1 Pd3 Pd1 52.7(2) . . ? S3 Pd3 Pd2 52.03(13) . . ? P3 Pd3 Pd2 140.91(13) . . ? S1 Pd3 Pd2 95.6(2) . . ? Pd1 Pd3 Pd2 58.01(5) . . ? S3 Pd3 Pd4 108.11(13) . . ? P3 Pd3 Pd4 144.77(13) . . ? S1 Pd3 Pd4 47.8(2) . . ? Pd1 Pd3 Pd4 55.94(5) . . ? Pd2 Pd3 Pd4 56.48(6) . . ? S2 Pd4 P4 97.0(3) . . ? S2 Pd4 S1 146.2(2) . . ? P4 Pd4 S1 116.3(3) . . ? S2 Pd4 Pd1 93.5(2) . . ? P4 Pd4 Pd1 159.7(2) . . ? S1 Pd4 Pd1 53.1(2) . . ? S2 Pd4 Pd2 53.1(2) . . ? P4 Pd4 Pd2 140.4(2) . . ? S1 Pd4 Pd2 98.6(2) . . ? Pd1 Pd4 Pd2 58.70(6) . . ? S2 Pd4 Pd3 110.9(2) . . ? P4 Pd4 Pd3 134.0(2) . . ? S1 Pd4 Pd3 49.40(13) . . ? Pd1 Pd4 Pd3 55.84(5) . . ? Pd2 Pd4 Pd3 58.36(5) . . ? Pd1 S1 Pd4 73.6(2) . . ? Pd1 S1 Pd3 72.4(2) . . ? Pd4 S1 Pd3 82.8(2) . . ? O1 S2 O2 112.2(10) . . ? O1 S2 Pd4 115.4(9) . . ? O2 S2 Pd4 117.5(9) . . ? O1 S2 Pd2 118.3(8) . . ? O2 S2 Pd2 110.8(9) . . ? Pd4 S2 Pd2 79.0(2) . . ? O4 S3 O3 112.0(8) . . ? O4 S3 Pd3 116.2(5) . . ? O3 S3 Pd3 113.5(5) . . ? O4 S3 Pd2 111.7(6) . . ? O3 S3 Pd2 119.7(5) . . ? Pd3 S3 Pd2 80.6(2) . . ? C17 P1 C10 106.7(12) . . ? C17 P1 C24 101.8(12) . . ? C10 P1 C24 105.7(12) . . ? C17 P1 Pd1 116.0(7) . . ? C10 P1 Pd1 112.1(10) . . ? C24 P1 Pd1 113.5(8) . . ? C38 P2 C45 106.9(10) . . ? C38 P2 C31 104.7(9) . . ? C45 P2 C31 104.9(8) . . ? C38 P2 Pd2 116.7(7) . . ? C45 P2 Pd2 115.6(8) . . ? C31 P2 Pd2 106.8(7) . . ? C59 P3 C52 101.6(9) . . ? C59 P3 C66 104.9(9) . . ? C52 P3 C66 102.8(8) . . ? C59 P3 Pd3 121.1(6) . . ? C52 P3 Pd3 113.3(6) . . ? C66 P3 Pd3 111.3(6) . . ? C80 P4 C87 98.9(13) . . ? C80 P4 C73 102.4(11) . . ? C87 P4 C73 108.3(13) . . ? C80 P4 Pd4 116.2(9) . . ? C87 P4 Pd4 119.6(9) . . ? C73 P4 Pd4 109.7(8) . . ? N1 C1 Pd1 168.0(18) . . ? C1 N1 C2' 171.8(26) . . ? C1 N1 C2 173.8(23) . . ? C7 C2 C3 124.9(27) . . ? C7 C2 N1 118.5(24) . . ? C3 C2 N1 116.5(24) . . ? C2 C3 C4 114.2(28) . . ? C2 C3 C8 124.0(25) . . ? C4 C3 C8 121.8(26) . . ? C5 C4 C3 121.2(30) . . ? C6 C5 C4 121.4(30) . . ? C5 C6 C7 120.0(29) . . ? C2 C7 C6 118.3(26) . . ? C2 C7 C9 122.1(25) . . ? C6 C7 C9 119.6(25) . . ? N1 C2' C7' 115.3(25) . . ? N1 C2' C3' 117.2(25) . . ? C7' C2' C3' 127.6(28) . . ? C4' C3' C2' 111.8(29) . . ? C4' C3' C8' 126.1(29) . . ? C2' C3' C8' 122.1(26) . . ? C5' C4' C3' 121.5(31) . . ? C6' C5' C4' 122.5(31) . . ? C5' C6' C7' 119.0(29) . . ? C2' C7' C6' 117.7(27) . . ? C2' C7' C9' 118.3(26) . . ? C6' C7' C9' 124.1(28) . . ? C16 C10 P1 118.4(17) . . ? C12 C11 C16 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 C10 120.4(14) . . ? C11 C16 C10 119.5(14) . . ? C23 C17 P1 117.0(13) . . ? C23' C17 P1 118.1(14) . . ? C19 C18 C23 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 C17 122.2(11) . . ? C18 C23 C17 117.8(11) . . ? C19' C18' C23' 120.0 . . ? C20' C19' C18' 120.0 . . ? C19' C20' C21' 120.0 . . ? C22' C21' C20' 120.0 . . ? C21' C22' C23' 120.0 . . ? C22' C23' C18' 120.0 . . ? C22' C23' C17 118.4(12) . . ? C18' C23' C17 121.5(12) . . ? C30' C24 P1 108.7(14) . . ? C30 C24 P1 118.6(12) . . ? C26 C25 C30 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 C24 122.2(10) . . ? C25 C30 C24 117.7(10) . . ? C26' C25' C30' 120.0 . . ? C27' C26' C25' 120.0 . . ? C26' C27' C28' 120.0 . . ? C29' C28' C27' 120.0 . . ? C30' C29' C28' 120.0 . . ? C29' C30' C25' 120.0 . . ? C29' C30' C24 120.0(12) . . ? C25' C30' C24 120.0(12) . . ? C37 C31 P2 132.7(12) . . ? C37' C31 P2 129.1(13) . . ? C33 C32 C37 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 C31 117.9(11) . . ? C32 C37 C31 122.1(11) . . ? C33' C32' C37' 120.0 . . ? C34' C33' C32' 120.0 . . ? C33' C34' C35' 120.0 . . ? C34' C35' C36' 120.0 . . ? C37' C36' C35' 120.0 . . ? C36' C37' C32' 120.0 . . ? C36' C37' C31 122.8(11) . . ? C32' C37' C31 117.2(11) . . ? C44' C38 P2 119.8(11) . . ? C44 C38 P2 127.1(12) . . ? C40 C39 C44 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 C38 119.0(11) . . ? C39 C44 C38 121.0(11) . . ? C40' C39' C44' 120.0 . . ? C41' C40' C39' 120.0 . . ? C40' C41' C42' 120.0 . . ? C43' C42' C41' 120.0 . . ? C42' C43' C44' 120.0 . . ? C43' C44' C39' 120.0 . . ? C43' C44' C38 118.5(11) . . ? C39' C44' C38 121.5(11) . . ? C51' C45 P2 127.4(12) . . ? C51 C45 P2 134.9(12) . . ? C51" C45 P2 102.1(13) . . ? C47 C46 C51 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 C45 118.3(11) . . ? C46 C51 C45 121.6(11) . . ? C47' C46' C51' 120.0 . . ? C48' C47' C46' 120.0 . . ? C47' C48' C49' 120.0 . . ? C48' C49' C50' 120.0 . . ? C51' C50' C49' 120.0 . . ? C50' C51' C46' 120.0 . . ? C50' C51' C45 122.2(10) . . ? C46' C51' C45 117.8(10) . . ? C47" C46" C51" 120.0 . . ? C48" C47" C46" 120.0 . . ? C49" C48" C47" 120.0 . . ? C48" C49" C50" 120.0 . . ? C51" C50" C49" 120.0 . . ? C50" C51" C46" 120.0 . . ? C50" C51" C45 119.3(12) . . ? C46" C51" C45 120.7(12) . . ? C58 C52 P3 115.8(11) . . ? C54 C53 C58 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C58 120.0 . . ? C57 C58 C53 120.0 . . ? C57 C58 C52 119.6(10) . . ? C53 C58 C52 120.3(10) . . ? C65 C59 P3 117.9(13) . . ? C61 C60 C65 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 C59 119.9(11) . . ? C60 C65 C59 120.1(11) . . ? C72 C66 P3 117.1(12) . . ? C68 C67 C72 120.0 . . ? C69 C68 C67 120.0 . . ? C68 C69 C70 120.0 . . ? C69 C70 C71 120.0 . . ? C72 C71 C70 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 C66 118.0(10) . . ? C67 C72 C66 122.0(10) . . ? C79 C73 P4 117.2(16) . . ? C75 C74 C79 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C77 120.0 . . ? C76 C77 C78 120.0 . . ? C79 C78 C77 120.0 . . ? C78 C79 C74 120.0 . . ? C78 C79 C73 118.3(16) . . ? C74 C79 C73 121.6(15) . . ? C86 C80 P4 116.9(17) . . ? C82 C81 C86 120.0 . . ? C83 C82 C81 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? C85 C86 C80 119.4(16) . . ? C81 C86 C80 120.6(16) . . ? C93 C87 P4 117.9(14) . . ? C89 C88 C93 120.0 . . ? C90 C89 C88 120.0 . . ? C89 C90 C91 120.0 . . ? C92 C91 C90 120.0 . . ? C93 C92 C91 120.0 . . ? C92 C93 C88 120.0 . . ? C92 C93 C87 123.4(12) . . ? C88 C93 C87 116.6(12) . . ? _refine_diff_density_max 3.211 _refine_diff_density_min -4.949 _refine_diff_density_rms 0.203 #===END