# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Paul Peringer' _publ_contact_author_email PAUL.PERINGER@UIBK.AC.AT loop_ _publ_author_name P.Peringer H.Kopacka C.Reitsamer W.Schuh S.Stallinger K.Wurst data_p143 _database_code_depnum_ccdc_archive 'CCDC 614361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.50 H68 Cl2 O P4 Pd' _chemical_formula_weight 1220.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2001(2) _cell_length_b 12.4004(2) _cell_length_c 24.4161(4) _cell_angle_alpha 84.068(1) _cell_angle_beta 82.649(1) _cell_angle_gamma 89.914(1) _cell_volume 3046.28(9) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 31104 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1266 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17938 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.50 _reflns_number_total 12411 _reflns_number_gt 10607 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Disorder of two toluene solvent, one in a general position with 1:1 position disorder with nearly overlying carbon atoms C12-C18: C12A-C18A. The other lies nearby an inversion centre and is disordered over 3 positions with 2:1:1 disorder. Once the inversion centre is in the middle of the 6-ring, C19-C22. The two other positions C19A-C22A and C21B have overlying parts and the inversion centre is in the middle of the axis C21A-C21A' and C21B-C21B. All carbon atoms were refined isotropically and the hydrogen atoms were omitted. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.6218P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'mixed; refined with bond reastraint at O1' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12411 _refine_ls_number_parameters 702 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.23868(2) 0.108171(15) 0.231151(8) 0.03348(7) Uani 1 1 d . . . P1 P 0.05864(7) 0.14706(5) 0.29303(3) 0.03461(15) Uani 1 1 d . . . P2 P 0.11345(6) -0.07837(5) 0.32213(3) 0.03023(14) Uani 1 1 d . . . P3 P 0.26973(6) -0.14967(5) 0.21965(3) 0.02845(14) Uani 1 1 d . . . P4 P 0.38813(6) 0.05004(5) 0.16175(3) 0.02939(14) Uani 1 1 d . . . Cl1 Cl 0.28942(12) 0.29182(6) 0.20246(4) 0.0790(3) Uani 1 1 d . . . Cl2 Cl 0.67223(9) -0.08298(9) 0.27824(4) 0.0701(3) Uani 1 1 d . . . O1 O 0.7246(3) -0.0820(3) 0.40156(12) 0.0803(8) Uani 1 1 d D . . H1O H 0.710(5) -0.071(4) 0.3677(10) 0.093(16) Uiso 1 1 d D . . C1 C 0.2047(2) -0.05329(19) 0.25900(10) 0.0310(5) Uani 1 1 d . . . C2 C -0.0205(2) 0.0176(2) 0.32274(11) 0.0364(6) Uani 1 1 d . . . H2A H -0.0631 0.0226 0.3607 0.044 Uiso 1 1 calc . . . H2B H -0.0870 -0.0037 0.3002 0.044 Uiso 1 1 calc . . . C3 C 0.4225(2) -0.09196(19) 0.18197(10) 0.0301(5) Uani 1 1 d . . . H3A H 0.4494 -0.1297 0.1491 0.036 Uiso 1 1 calc . . . H3B H 0.4934 -0.0978 0.2056 0.036 Uiso 1 1 calc . . . C4 C 0.7037(5) -0.1889(4) 0.42452(19) 0.0935(14) Uani 1 1 d . . . H4A H 0.7797 -0.2318 0.4128 0.140 Uiso 1 1 calc R . . H4B H 0.6255 -0.2178 0.4121 0.140 Uiso 1 1 calc R . . H4C H 0.6912 -0.1916 0.4647 0.140 Uiso 1 1 calc R . . C5 C 0.5999(4) -0.3519(3) 0.13600(16) 0.0609(9) Uani 1 1 d . . . C6 C 0.6181(4) -0.2789(3) 0.08823(17) 0.0684(10) Uani 1 1 d . . . H6 H 0.6723 -0.2173 0.0871 0.082 Uiso 1 1 calc . . . C7 C 0.5575(5) -0.2961(4) 0.04304(18) 0.0863(14) Uani 1 1 d . . . H7 H 0.5697 -0.2458 0.0112 0.104 Uiso 1 1 calc . . . C8 C 0.4795(6) -0.3856(5) 0.0437(2) 0.1002(18) Uani 1 1 d . . . H8 H 0.4390 -0.3972 0.0123 0.120 Uiso 1 1 calc . . . C9 C 0.4601(5) -0.4591(4) 0.0906(3) 0.0918(15) Uani 1 1 d . . . H9 H 0.4066 -0.5209 0.0910 0.110 Uiso 1 1 calc . . . C10 C 0.5187(4) -0.4423(3) 0.13641(19) 0.0720(11) Uani 1 1 d . . . H10 H 0.5040 -0.4920 0.1684 0.086 Uiso 1 1 calc . . . C11 C 0.6672(4) -0.3336(4) 0.18514(18) 0.0793(12) Uani 1 1 d . . . H11A H 0.7598 -0.3519 0.1779 0.119 Uiso 1 1 calc R . . H11B H 0.6258 -0.3789 0.2175 0.119 Uiso 1 1 calc R . . H11C H 0.6596 -0.2580 0.1919 0.119 Uiso 1 1 calc R . . C101 C -0.0698(3) 0.2291(2) 0.26484(13) 0.0497(8) Uani 1 1 d . . . C102 C -0.0418(5) 0.3388(3) 0.2503(2) 0.0875(14) Uani 1 1 d . . . H102 H 0.0412 0.3672 0.2546 0.105 Uiso 1 1 calc . . . C103 C -0.1359(7) 0.4062(4) 0.2293(3) 0.111(2) Uani 1 1 d . . . H103 H -0.1180 0.4807 0.2202 0.133 Uiso 1 1 calc . . . C104 C -0.2544(7) 0.3638(4) 0.2220(2) 0.114(2) Uani 1 1 d . . . H104 H -0.3171 0.4092 0.2066 0.137 Uiso 1 1 calc . . . C105 C -0.2843(5) 0.2557(4) 0.2367(2) 0.0987(18) Uani 1 1 d . . . H105 H -0.3677 0.2281 0.2323 0.118 Uiso 1 1 calc . . . C106 C -0.1908(4) 0.1877(3) 0.25811(16) 0.0665(11) Uani 1 1 d . . . H106 H -0.2103 0.1137 0.2680 0.080 Uiso 1 1 calc . . . C107 C 0.0869(3) 0.2133(2) 0.35365(11) 0.0350(6) Uani 1 1 d . . . C108 C 0.2126(3) 0.2403(2) 0.36310(13) 0.0438(7) Uani 1 1 d . . . H108 H 0.2859 0.2276 0.3372 0.053 Uiso 1 1 calc . . . C109 C 0.2301(3) 0.2862(3) 0.41118(15) 0.0568(8) Uani 1 1 d . . . H109 H 0.3158 0.3043 0.4178 0.068 Uiso 1 1 calc . . . C110 C 0.1234(4) 0.3057(3) 0.44915(14) 0.0580(9) Uani 1 1 d . . . H110 H 0.1363 0.3365 0.4817 0.070 Uiso 1 1 calc . . . C111 C -0.0016(3) 0.2802(3) 0.43960(14) 0.0570(8) Uani 1 1 d . . . H111 H -0.0747 0.2941 0.4654 0.068 Uiso 1 1 calc . . . C112 C -0.0203(3) 0.2341(3) 0.39227(13) 0.0486(7) Uani 1 1 d . . . H112 H -0.1063 0.2166 0.3859 0.058 Uiso 1 1 calc . . . C201 C 0.0461(3) -0.2144(2) 0.33837(12) 0.0378(6) Uani 1 1 d . . . C202 C 0.0969(3) -0.2880(2) 0.37708(14) 0.0502(7) Uani 1 1 d . . . H202 H 0.1619 -0.2657 0.3977 0.060 Uiso 1 1 calc . . . C203 C 0.0507(4) -0.3946(3) 0.38505(18) 0.0671(10) Uani 1 1 d . . . H203 H 0.0855 -0.4448 0.4108 0.080 Uiso 1 1 calc . . . C204 C -0.0450(4) -0.4270(3) 0.3556(2) 0.0715(11) Uani 1 1 d . . . H204 H -0.0750 -0.4995 0.3611 0.086 Uiso 1 1 calc . . . C205 C -0.0975(3) -0.3545(3) 0.31817(18) 0.0641(10) Uani 1 1 d . . . H205 H -0.1642 -0.3774 0.2986 0.077 Uiso 1 1 calc . . . C206 C -0.0528(3) -0.2478(2) 0.30909(14) 0.0473(7) Uani 1 1 d . . . H206 H -0.0888 -0.1983 0.2834 0.057 Uiso 1 1 calc . . . C207 C 0.1989(3) -0.0514(2) 0.37984(11) 0.0349(6) Uani 1 1 d . . . C208 C 0.3335(3) -0.0286(2) 0.37098(12) 0.0391(6) Uani 1 1 d . . . H208 H 0.3806 -0.0303 0.3354 0.047 Uiso 1 1 calc . . . C209 C 0.3985(3) -0.0034(3) 0.41452(15) 0.0555(8) Uani 1 1 d . . . H209 H 0.4899 0.0114 0.4087 0.067 Uiso 1 1 calc . . . C210 C 0.3283(4) -0.0002(3) 0.46664(15) 0.0622(9) Uani 1 1 d . . . H210 H 0.3720 0.0184 0.4960 0.075 Uiso 1 1 calc . . . C211 C 0.1964(4) -0.0238(3) 0.47592(13) 0.0624(9) Uani 1 1 d . . . H211 H 0.1500 -0.0223 0.5117 0.075 Uiso 1 1 calc . . . C212 C 0.1304(3) -0.0499(3) 0.43279(13) 0.0496(7) Uani 1 1 d . . . H212 H 0.0395 -0.0665 0.4393 0.059 Uiso 1 1 calc . . . C301 C 0.1708(3) -0.1847(2) 0.16717(11) 0.0348(6) Uani 1 1 d . . . C302 C 0.0461(3) -0.1418(2) 0.16618(13) 0.0453(7) Uani 1 1 d . . . H302 H 0.0137 -0.0947 0.1924 0.054 Uiso 1 1 calc . . . C303 C -0.0316(4) -0.1679(3) 0.12678(17) 0.0632(10) Uani 1 1 d . . . H303 H -0.1170 -0.1394 0.1265 0.076 Uiso 1 1 calc . . . C304 C 0.0172(4) -0.2359(3) 0.08790(16) 0.0651(10) Uani 1 1 d . . . H304 H -0.0353 -0.2532 0.0610 0.078 Uiso 1 1 calc . . . C305 C 0.1406(4) -0.2783(3) 0.08800(15) 0.0590(9) Uani 1 1 d . . . H305 H 0.1726 -0.3247 0.0614 0.071 Uiso 1 1 calc . . . C306 C 0.2189(3) -0.2528(2) 0.12744(13) 0.0467(7) Uani 1 1 d . . . H306 H 0.3043 -0.2814 0.1274 0.056 Uiso 1 1 calc . . . C307 C 0.3119(3) -0.2765(2) 0.25694(11) 0.0336(5) Uani 1 1 d . . . C308 C 0.4076(3) -0.2727(2) 0.29244(13) 0.0445(7) Uani 1 1 d . . . H308 H 0.4478 -0.2064 0.2965 0.053 Uiso 1 1 calc . . . C309 C 0.4432(3) -0.3675(3) 0.32184(16) 0.0611(9) Uani 1 1 d . . . H309 H 0.5080 -0.3653 0.3459 0.073 Uiso 1 1 calc . . . C310 C 0.3846(4) -0.4649(3) 0.31612(17) 0.0665(10) Uani 1 1 d . . . H310 H 0.4094 -0.5288 0.3362 0.080 Uiso 1 1 calc . . . C311 C 0.2901(4) -0.4687(2) 0.28116(17) 0.0628(9) Uani 1 1 d . . . H311 H 0.2504 -0.5354 0.2773 0.075 Uiso 1 1 calc . . . C312 C 0.2524(3) -0.3746(2) 0.25144(13) 0.0456(7) Uani 1 1 d . . . H312 H 0.1871 -0.3774 0.2277 0.055 Uiso 1 1 calc . . . C401 C 0.3103(2) 0.0499(2) 0.09855(10) 0.0321(5) Uani 1 1 d . . . C402 C 0.2000(3) 0.1116(3) 0.09139(13) 0.0511(8) Uani 1 1 d . . . H402 H 0.1662 0.1562 0.1186 0.061 Uiso 1 1 calc . . . C403 C 0.1387(3) 0.1081(4) 0.04407(15) 0.0676(11) Uani 1 1 d . . . H403 H 0.0639 0.1507 0.0394 0.081 Uiso 1 1 calc . . . C404 C 0.1861(3) 0.0434(3) 0.00430(13) 0.0582(9) Uani 1 1 d . . . H404 H 0.1430 0.0405 -0.0274 0.070 Uiso 1 1 calc . . . C405 C 0.2962(4) -0.0174(3) 0.01050(13) 0.0541(8) Uani 1 1 d . . . H405 H 0.3290 -0.0620 -0.0169 0.065 Uiso 1 1 calc . . . C406 C 0.3590(3) -0.0134(3) 0.05699(12) 0.0449(7) Uani 1 1 d . . . H406 H 0.4359 -0.0540 0.0606 0.054 Uiso 1 1 calc . . . C407 C 0.5484(3) 0.1132(2) 0.13652(10) 0.0342(5) Uani 1 1 d . . . C408 C 0.6667(3) 0.0624(2) 0.14476(12) 0.0421(6) Uani 1 1 d . . . H408 H 0.6663 -0.0067 0.1647 0.051 Uiso 1 1 calc . . . C409 C 0.7858(3) 0.1142(3) 0.12343(15) 0.0526(8) Uani 1 1 d . . . H409 H 0.8659 0.0795 0.1287 0.063 Uiso 1 1 calc . . . C410 C 0.7878(3) 0.2151(3) 0.09497(15) 0.0565(8) Uani 1 1 d . . . H410 H 0.8690 0.2489 0.0804 0.068 Uiso 1 1 calc . . . C411 C 0.6712(3) 0.2673(3) 0.08754(14) 0.0542(8) Uani 1 1 d . . . H411 H 0.6728 0.3374 0.0687 0.065 Uiso 1 1 calc . . . C412 C 0.5513(3) 0.2162(2) 0.10791(13) 0.0450(7) Uani 1 1 d . . . H412 H 0.4717 0.2514 0.1023 0.054 Uiso 1 1 calc . . . C12 C 0.3446(9) -0.4039(8) 0.5328(4) 0.086(3) Uiso 0.50 1 d PD . . C13 C 0.3755(11) -0.2932(8) 0.5159(5) 0.075(3) Uiso 0.50 1 d PD . . C14 C 0.3920(11) -0.2253(9) 0.5588(5) 0.096(3) Uiso 0.50 1 d PD . . C15 C 0.3931(13) -0.2556(9) 0.6125(5) 0.095(4) Uiso 0.50 1 d PD . . C16 C 0.3639(11) -0.3734(9) 0.6296(5) 0.097(3) Uiso 0.50 1 d PD . . C17 C 0.3458(10) -0.4259(8) 0.5911(4) 0.069(3) Uiso 0.50 1 d PD . . C18 C 0.3234(12) -0.4782(10) 0.4934(5) 0.105(3) Uiso 0.50 1 d PD . . C12A C 0.3737(9) -0.3315(7) 0.5756(4) 0.077(2) Uiso 0.50 1 d PD . . C13A C 0.3420(10) -0.4521(7) 0.5769(4) 0.071(3) Uiso 0.50 1 d PD . . C14A C 0.3261(12) -0.4942(10) 0.5318(5) 0.106(3) Uiso 0.50 1 d PD . . C15A C 0.3396(11) -0.4225(9) 0.4781(4) 0.089(3) Uiso 0.50 1 d PD . . C16A C 0.3705(10) -0.3195(8) 0.4809(5) 0.089(3) Uiso 0.50 1 d PD . . C17A C 0.3860(14) -0.2673(12) 0.5275(5) 0.096(4) Uiso 0.50 1 d PD . . C18A C 0.3870(15) -0.2902(12) 0.6288(5) 0.113(5) Uiso 0.50 1 d PD . . C19 C 0.0377(13) -0.5411(10) 0.0494(6) 0.097(3) Uiso 0.50 1 d PD . . C20 C 0.1351(10) -0.5472(9) 0.0007(6) 0.080(3) Uiso 0.50 1 d PD . . C21 C 0.0758(11) -0.4974(9) -0.0493(6) 0.075(2) Uiso 0.50 1 d PD . . C22 C 0.033(3) -0.561(3) 0.1032(7) 0.139(11) Uiso 0.25 1 d PD . . C19A C 0.052(2) -0.5310(19) 0.0185(12) 0.092(6) Uiso 0.25 1 d P . . C20A C 0.1034(10) -0.5220(8) -0.0255(6) 0.067(2) Uiso 0.50 1 d P . . C21B C 0.1397(17) -0.5735(15) 0.0335(10) 0.071(4) Uiso 0.25 1 d P . . C21A C 0.048(2) -0.4761(16) -0.0727(9) 0.071(5) Uiso 0.25 1 d P . . C22A C 0.0910(16) -0.5783(13) 0.0774(8) 0.129(4) Uiso 0.50 1 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 0.04680(13) 0.02381(11) 0.02929(11) -0.00622(7) -0.00012(8) 0.00211(8) P1 0.0409(4) 0.0301(3) 0.0341(4) -0.0086(3) -0.0054(3) 0.0078(3) P2 0.0296(3) 0.0276(3) 0.0337(3) -0.0049(3) -0.0034(3) 0.0002(2) P3 0.0310(3) 0.0239(3) 0.0319(3) -0.0063(2) -0.0072(3) 0.0015(2) P4 0.0350(3) 0.0274(3) 0.0261(3) -0.0050(2) -0.0033(3) 0.0015(2) Cl1 0.1253(9) 0.0260(4) 0.0746(6) -0.0070(4) 0.0311(6) -0.0052(4) Cl2 0.0592(5) 0.0880(7) 0.0664(6) 0.0091(5) -0.0337(4) -0.0214(5) O1 0.0781(19) 0.110(2) 0.0518(17) -0.0104(16) -0.0013(14) -0.0151(16) C1 0.0384(13) 0.0219(11) 0.0328(13) -0.0053(9) -0.0028(10) 0.0003(10) C2 0.0297(12) 0.0388(14) 0.0418(15) -0.0084(11) -0.0057(11) 0.0036(10) C3 0.0319(12) 0.0283(12) 0.0303(13) -0.0037(10) -0.0048(10) 0.0015(10) C4 0.112(4) 0.098(4) 0.062(3) -0.004(2) 0.016(3) 0.001(3) C5 0.059(2) 0.060(2) 0.065(2) -0.0127(17) -0.0052(17) 0.0269(17) C6 0.067(2) 0.067(2) 0.069(3) -0.0086(19) 0.0020(19) 0.0174(19) C7 0.101(3) 0.097(4) 0.062(3) -0.016(2) -0.005(2) 0.037(3) C8 0.120(4) 0.103(4) 0.093(4) -0.050(3) -0.045(3) 0.055(3) C9 0.084(3) 0.067(3) 0.137(5) -0.037(3) -0.038(3) 0.028(2) C10 0.065(2) 0.055(2) 0.094(3) -0.002(2) -0.009(2) 0.0194(18) C11 0.077(3) 0.083(3) 0.082(3) -0.018(2) -0.017(2) 0.021(2) C101 0.070(2) 0.0443(17) 0.0416(16) -0.0181(13) -0.0224(15) 0.0239(15) C102 0.106(3) 0.048(2) 0.114(4) 0.000(2) -0.041(3) 0.023(2) C103 0.157(5) 0.058(3) 0.132(5) -0.011(3) -0.073(4) 0.046(3) C104 0.168(5) 0.092(4) 0.110(4) -0.049(3) -0.097(4) 0.083(4) C105 0.115(4) 0.095(3) 0.114(4) -0.058(3) -0.084(3) 0.054(3) C106 0.076(2) 0.063(2) 0.075(2) -0.0332(19) -0.046(2) 0.0301(18) C107 0.0393(14) 0.0306(13) 0.0358(14) -0.0068(10) -0.0049(11) 0.0068(10) C108 0.0414(15) 0.0413(16) 0.0490(17) -0.0086(13) -0.0038(13) 0.0000(12) C109 0.0576(19) 0.058(2) 0.059(2) -0.0146(16) -0.0178(16) -0.0091(16) C110 0.079(2) 0.056(2) 0.0447(18) -0.0190(15) -0.0174(17) 0.0041(17) C111 0.063(2) 0.064(2) 0.0453(18) -0.0207(16) 0.0001(15) 0.0126(16) C112 0.0416(15) 0.0588(19) 0.0479(18) -0.0217(14) -0.0024(13) 0.0073(14) C201 0.0337(13) 0.0325(13) 0.0447(16) -0.0049(11) 0.0055(11) -0.0033(10) C202 0.0529(17) 0.0383(16) 0.0563(19) 0.0044(14) -0.0028(15) -0.0018(13) C203 0.071(2) 0.0405(18) 0.083(3) 0.0139(17) 0.003(2) -0.0020(16) C204 0.068(2) 0.0376(18) 0.102(3) -0.0027(19) 0.012(2) -0.0167(16) C205 0.054(2) 0.050(2) 0.088(3) -0.0171(19) -0.0006(18) -0.0162(16) C206 0.0426(15) 0.0420(16) 0.0564(19) -0.0073(14) -0.0019(14) -0.0070(12) C207 0.0378(13) 0.0327(13) 0.0354(14) -0.0054(11) -0.0073(11) 0.0039(10) C208 0.0390(14) 0.0413(15) 0.0385(15) -0.0086(12) -0.0073(11) 0.0036(11) C209 0.0497(18) 0.061(2) 0.063(2) -0.0195(17) -0.0233(16) 0.0066(15) C210 0.076(2) 0.069(2) 0.050(2) -0.0226(17) -0.0291(18) 0.0176(19) C211 0.075(2) 0.080(3) 0.0338(17) -0.0159(16) -0.0073(16) 0.0206(19) C212 0.0452(16) 0.063(2) 0.0390(16) -0.0068(14) 0.0017(13) 0.0091(14) C301 0.0385(13) 0.0302(13) 0.0383(14) -0.0061(11) -0.0126(11) -0.0017(10) C302 0.0453(16) 0.0408(16) 0.0535(18) -0.0106(13) -0.0163(13) 0.0029(12) C303 0.058(2) 0.059(2) 0.083(3) -0.0132(18) -0.0412(19) 0.0053(16) C304 0.080(2) 0.058(2) 0.068(2) -0.0151(18) -0.043(2) -0.0058(18) C305 0.079(2) 0.0510(19) 0.053(2) -0.0234(16) -0.0199(18) -0.0044(17) C306 0.0504(17) 0.0443(16) 0.0500(18) -0.0175(13) -0.0137(14) 0.0029(13) C307 0.0378(13) 0.0259(12) 0.0367(14) -0.0042(10) -0.0029(11) 0.0037(10) C308 0.0456(16) 0.0377(15) 0.0499(17) 0.0027(13) -0.0110(13) 0.0016(12) C309 0.060(2) 0.056(2) 0.065(2) 0.0154(17) -0.0185(17) 0.0078(16) C310 0.076(2) 0.0393(18) 0.079(3) 0.0189(17) -0.011(2) 0.0095(16) C311 0.084(2) 0.0249(15) 0.077(2) 0.0001(15) -0.005(2) -0.0015(15) C312 0.0535(17) 0.0333(14) 0.0505(17) -0.0066(12) -0.0067(14) -0.0023(12) C401 0.0342(13) 0.0340(13) 0.0280(13) -0.0015(10) -0.0046(10) 0.0009(10) C402 0.0500(17) 0.065(2) 0.0385(16) -0.0063(14) -0.0049(13) 0.0192(15) C403 0.0490(19) 0.104(3) 0.052(2) -0.001(2) -0.0186(16) 0.0266(19) C404 0.0570(19) 0.083(3) 0.0367(17) -0.0020(16) -0.0183(15) -0.0065(18) C405 0.070(2) 0.060(2) 0.0367(16) -0.0157(14) -0.0142(15) 0.0057(16) C406 0.0523(17) 0.0516(17) 0.0332(15) -0.0109(12) -0.0102(13) 0.0135(14) C407 0.0417(14) 0.0333(13) 0.0282(13) -0.0072(10) -0.0042(11) -0.0047(11) C408 0.0426(15) 0.0403(15) 0.0436(16) -0.0055(12) -0.0053(12) -0.0011(12) C409 0.0390(15) 0.0512(18) 0.068(2) -0.0131(16) -0.0021(14) -0.0036(13) C410 0.0464(17) 0.056(2) 0.065(2) -0.0133(16) 0.0065(15) -0.0171(15) C411 0.061(2) 0.0422(17) 0.056(2) 0.0022(14) -0.0005(16) -0.0133(14) C412 0.0473(16) 0.0405(16) 0.0462(17) 0.0013(13) -0.0068(13) -0.0043(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.062(2) . ? Pd1 P4 2.3028(7) . ? Pd1 P1 2.3078(7) . ? Pd1 Cl1 2.3507(8) . ? P1 C101 1.819(3) . ? P1 C107 1.819(3) . ? P1 C2 1.835(3) . ? P2 C1 1.695(3) . ? P2 C207 1.808(3) . ? P2 C201 1.808(3) . ? P2 C2 1.810(3) . ? P3 C1 1.692(2) . ? P3 C3 1.813(3) . ? P3 C307 1.813(3) . ? P3 C301 1.816(3) . ? P4 C407 1.820(3) . ? P4 C401 1.824(3) . ? P4 C3 1.825(2) . ? Cl2 H1O 2.29(2) . ? O1 H1O 0.855(19) . ? O1 C4 1.390(6) . ? C5 C10 1.393(6) . ? C5 C6 1.394(5) . ? C5 C11 1.493(5) . ? C6 C7 1.367(6) . ? C7 C8 1.364(8) . ? C8 C9 1.381(8) . ? C9 C10 1.369(7) . ? C101 C106 1.372(5) . ? C101 C102 1.391(5) . ? C102 C103 1.385(6) . ? C103 C104 1.358(8) . ? C104 C105 1.376(8) . ? C105 C106 1.389(5) . ? C107 C108 1.379(4) . ? C107 C112 1.392(4) . ? C108 C109 1.388(4) . ? C109 C110 1.375(5) . ? C110 C111 1.369(5) . ? C111 C112 1.375(4) . ? C201 C202 1.393(4) . ? C201 C206 1.395(4) . ? C202 C203 1.391(5) . ? C203 C204 1.367(6) . ? C204 C205 1.374(6) . ? C205 C206 1.388(4) . ? C207 C208 1.388(4) . ? C207 C212 1.390(4) . ? C208 C209 1.385(4) . ? C209 C210 1.383(5) . ? C210 C211 1.362(5) . ? C211 C212 1.385(5) . ? C301 C302 1.379(4) . ? C301 C306 1.393(4) . ? C302 C303 1.385(4) . ? C303 C304 1.380(5) . ? C304 C305 1.364(5) . ? C305 C306 1.388(4) . ? C307 C312 1.386(4) . ? C307 C308 1.390(4) . ? C308 C309 1.386(4) . ? C309 C310 1.376(5) . ? C310 C311 1.371(5) . ? C311 C312 1.389(4) . ? C401 C402 1.379(4) . ? C401 C406 1.389(4) . ? C402 C403 1.386(5) . ? C403 C404 1.364(5) . ? C404 C405 1.367(5) . ? C405 C406 1.378(4) . ? C407 C408 1.389(4) . ? C407 C412 1.389(4) . ? C408 C409 1.390(4) . ? C409 C410 1.365(5) . ? C410 C411 1.376(5) . ? C411 C412 1.388(4) . ? C12 C14A 1.139(14) . ? C12 C13A 1.174(13) . ? C12 C15A 1.384(13) . ? C12 C13 1.416(11) . ? C12 C17 1.424(11) . ? C12 C18 1.433(11) . ? C12 C12A 1.503(12) . ? C12 C16A 1.553(14) . ? C12 C17A 1.734(17) . ? C13 C16A 0.954(12) . ? C13 C14 1.437(13) . ? C13 C12A 1.483(15) . ? C13 C15A 1.988(15) . ? C14 C17A 0.978(13) . ? C14 C15 1.326(12) . ? C14 C12A 1.344(13) . ? C14 C18A 1.805(16) . ? C15 C18A 0.552(17) . ? C15 C12A 1.400(14) . ? C15 C16 1.497(13) . ? C16 C18A 1.056(15) . ? C16 C17 1.229(11) . ? C16 C12A 1.358(13) . ? C16 C13A 1.729(14) . ? C17 C13A 0.505(12) . ? C17 C12A 1.215(12) . ? C17 C14A 1.785(14) . ? C18 C15A 0.759(14) . ? C18 C14A 0.941(13) . ? C18 C16A 2.010(15) . ? C12A C17A 1.341(12) . ? C12A C18A 1.466(12) . ? C12A C13A 1.527(11) . ? C13A C14A 1.295(12) . ? C14A C15A 1.497(13) . ? C15A C16A 1.326(12) . ? C16A C17A 1.391(13) . ? C19 C19A 0.75(3) . ? C19 C22A 1.003(17) . ? C19 C21A 1.018(19) 2_545 ? C19 C21B 1.15(2) . ? C19 C21 1.252(16) 2_545 ? C19 C22 1.308(16) . ? C19 C20 1.456(13) . ? C19 C20A 1.773(18) 2_545 ? C19 C20A 1.856(15) . ? C20 C20A 0.789(11) . ? C20 C21B 0.840(18) . ? C20 C19A 0.93(3) . ? C20 C21 1.506(12) . ? C20 C22A 1.87(2) . ? C21 C21A 0.696(19) . ? C21 C20A 0.717(11) . ? C21 C19 1.252(16) 2_545 ? C21 C19A 1.48(3) 2_545 ? C21 C19A 1.65(3) . ? C21 C22 1.92(3) 2_545 ? C22 C22A 0.85(3) . ? C22 C21A 1.24(3) 2_545 ? C22 C21 1.92(3) 2_545 ? C22 C21B 1.92(3) . ? C19A C21B 1.12(3) . ? C19A C20A 1.13(3) . ? C19A C21 1.48(3) 2_545 ? C19A C21A 1.58(4) 2_545 ? C19A C22A 1.59(3) . ? C19A C19A 1.63(4) 2_545 ? C19A C20A 1.71(3) 2_545 ? C20A C21A 1.41(2) . ? C20A C21B 1.60(2) . ? C20A C19A 1.71(3) 2_545 ? C20A C19 1.773(18) 2_545 ? C21B C22A 1.12(2) . ? C21A C19 1.018(19) 2_545 ? C21A C22 1.24(3) 2_545 ? C21A C19A 1.58(4) 2_545 ? C21A C22A 1.58(3) 2_545 ? C22A C21A 1.58(3) 2_545 ? 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 P4 86.79(7) . . ? C1 Pd1 P1 87.61(7) . . ? P4 Pd1 P1 168.54(3) . . ? C1 Pd1 Cl1 176.31(8) . . ? P4 Pd1 Cl1 92.72(3) . . ? P1 Pd1 Cl1 93.50(3) . . ? C101 P1 C107 102.91(12) . . ? C101 P1 C2 106.22(14) . . ? C107 P1 C2 103.67(12) . . ? C101 P1 Pd1 116.70(11) . . ? C107 P1 Pd1 118.62(9) . . ? C2 P1 Pd1 107.41(9) . . ? C1 P2 C207 114.44(13) . . ? C1 P2 C201 115.38(12) . . ? C207 P2 C201 106.31(13) . . ? C1 P2 C2 105.91(12) . . ? C207 P2 C2 104.90(12) . . ? C201 P2 C2 109.36(12) . . ? C1 P3 C3 105.75(12) . . ? C1 P3 C307 116.21(12) . . ? C3 P3 C307 106.77(11) . . ? C1 P3 C301 115.00(12) . . ? C3 P3 C301 105.81(12) . . ? C307 P3 C301 106.52(12) . . ? C407 P4 C401 102.79(12) . . ? C407 P4 C3 105.48(12) . . ? C401 P4 C3 105.23(12) . . ? C407 P4 Pd1 125.03(8) . . ? C401 P4 Pd1 109.36(8) . . ? C3 P4 Pd1 107.37(8) . . ? H1O O1 C4 114(3) . . ? P3 C1 P2 124.86(15) . . ? P3 C1 Pd1 119.60(14) . . ? P2 C1 Pd1 115.53(12) . . ? P2 C2 P1 104.59(13) . . ? P3 C3 P4 105.98(12) . . ? C10 C5 C6 118.3(4) . . ? C10 C5 C11 121.2(4) . . ? C6 C5 C11 120.4(4) . . ? C7 C6 C5 120.5(4) . . ? C8 C7 C6 120.6(5) . . ? C7 C8 C9 119.9(5) . . ? C10 C9 C8 120.2(5) . . ? C9 C10 C5 120.5(4) . . ? C106 C101 C102 119.8(3) . . ? C106 C101 P1 123.1(3) . . ? C102 C101 P1 117.1(3) . . ? C103 C102 C101 120.1(5) . . ? C104 C103 C102 119.5(5) . . ? C103 C104 C105 121.2(4) . . ? C104 C105 C106 119.6(5) . . ? C101 C106 C105 119.7(4) . . ? C108 C107 C112 119.2(3) . . ? C108 C107 P1 121.5(2) . . ? C112 C107 P1 119.3(2) . . ? C107 C108 C109 119.6(3) . . ? C110 C109 C108 120.6(3) . . ? C111 C110 C109 120.0(3) . . ? C110 C111 C112 119.9(3) . . ? C111 C112 C107 120.7(3) . . ? C202 C201 C206 119.7(3) . . ? C202 C201 P2 121.0(2) . . ? C206 C201 P2 119.2(2) . . ? C203 C202 C201 119.5(3) . . ? C204 C203 C202 120.4(3) . . ? C203 C204 C205 120.5(3) . . ? C204 C205 C206 120.4(3) . . ? C205 C206 C201 119.5(3) . . ? C208 C207 C212 119.5(3) . . ? C208 C207 P2 119.7(2) . . ? C212 C207 P2 120.8(2) . . ? C209 C208 C207 120.1(3) . . ? C210 C209 C208 119.6(3) . . ? C211 C210 C209 120.8(3) . . ? C210 C211 C212 120.2(3) . . ? C211 C212 C207 119.9(3) . . ? C302 C301 C306 119.4(2) . . ? C302 C301 P3 119.3(2) . . ? C306 C301 P3 121.3(2) . . ? C301 C302 C303 120.4(3) . . ? C304 C303 C302 119.6(3) . . ? C305 C304 C303 120.8(3) . . ? C304 C305 C306 120.0(3) . . ? C305 C306 C301 119.9(3) . . ? C312 C307 C308 119.9(2) . . ? C312 C307 P3 122.8(2) . . ? C308 C307 P3 117.4(2) . . ? C309 C308 C307 119.5(3) . . ? C310 C309 C308 120.5(3) . . ? C311 C310 C309 120.0(3) . . ? C310 C311 C312 120.4(3) . . ? C307 C312 C311 119.6(3) . . ? C402 C401 C406 118.4(2) . . ? C402 C401 P4 120.6(2) . . ? C406 C401 P4 120.98(19) . . ? C401 C402 C403 120.1(3) . . ? C404 C403 C402 120.6(3) . . ? C403 C404 C405 119.9(3) . . ? C404 C405 C406 120.0(3) . . ? C405 C406 C401 120.8(3) . . ? C408 C407 C412 119.2(3) . . ? C408 C407 P4 122.6(2) . . ? C412 C407 P4 118.2(2) . . ? C407 C408 C409 119.7(3) . . ? C410 C409 C408 120.7(3) . . ? C409 C410 C411 120.2(3) . . ? C410 C411 C412 119.9(3) . . ? C411 C412 C407 120.3(3) . . ? C14A C12 C13A 68.0(8) . . ? C14A C12 C15A 72.0(8) . . ? C13A C12 C15A 139.9(10) . . ? C14A C12 C13 162.1(11) . . ? C13A C12 C13 129.1(10) . . ? C15A C12 C13 90.4(8) . . ? C14A C12 C17 87.5(9) . . ? C13A C12 C17 19.5(6) . . ? C15A C12 C17 159.5(10) . . ? C13 C12 C17 109.9(9) . . ? C14A C12 C18 40.9(7) . . ? C13A C12 C18 109.0(10) . . ? C15A C12 C18 31.2(6) . . ? C13 C12 C18 121.6(9) . . ? C17 C12 C18 128.4(10) . . ? C14A C12 C12A 136.2(10) . . ? C13A C12 C12A 68.3(7) . . ? C15A C12 C12A 151.1(9) . . ? C13 C12 C12A 60.9(7) . . ? C17 C12 C12A 49.0(6) . . ? C18 C12 C12A 175.9(10) . . ? C14A C12 C16A 125.2(10) . . ? C13A C12 C16A 165.1(10) . . ? C15A C12 C16A 53.3(6) . . ? C13 C12 C16A 37.1(5) . . ? C17 C12 C16A 146.8(9) . . ? C18 C12 C16A 84.5(8) . . ? C12A C12 C16A 97.9(8) . . ? C14A C12 C17A 173.4(11) . . ? C13A C12 C17A 116.5(9) . . ? C15A C12 C17A 103.0(8) . . ? C13 C12 C17A 12.6(6) . . ? C17 C12 C17A 97.3(7) . . ? C18 C12 C17A 134.2(9) . . ? C12A C12 C17A 48.3(5) . . ? C16A C12 C17A 49.7(6) . . ? C16A C13 C12 79.2(10) . . ? C16A C13 C14 163.7(13) . . ? C12 C13 C14 117.0(9) . . ? C16A C13 C12A 141.3(12) . . ? C12 C13 C12A 62.4(7) . . ? C14 C13 C12A 54.8(7) . . ? C16A C13 C15A 35.1(8) . . ? C12 C13 C15A 44.1(5) . . ? C14 C13 C15A 161.2(9) . . ? C12A C13 C15A 106.5(7) . . ? C17A C14 C15 131.6(14) . . ? C17A C14 C12A 68.5(10) . . ? C15 C14 C12A 63.2(8) . . ? C17A C14 C13 4.9(11) . . ? C15 C14 C13 127.6(10) . . ? C12A C14 C13 64.3(8) . . ? C17A C14 C18A 121.5(12) . . ? C15 C14 C18A 10.2(7) . . ? C12A C14 C18A 53.1(6) . . ? C13 C14 C18A 117.4(9) . . ? C18A C15 C14 145(2) . . ? C18A C15 C12A 86(2) . . ? C14 C15 C12A 59.0(8) . . ? C18A C15 C16 30.1(17) . . ? C14 C15 C16 114.6(10) . . ? C12A C15 C16 55.8(7) . . ? C18A C16 C17 129.4(13) . . ? C18A C16 C12A 73.6(9) . . ? C17 C16 C12A 55.8(7) . . ? C18A C16 C15 15.2(9) . . ? C17 C16 C15 114.2(10) . . ? C12A C16 C15 58.5(7) . . ? C18A C16 C13A 131.4(11) . . ? C17 C16 C13A 2.6(7) . . ? C12A C16 C13A 57.8(6) . . ? C15 C16 C13A 116.3(8) . . ? C13A C17 C12A 119(2) . . ? C13A C17 C16 171(2) . . ? C12A C17 C16 67.5(8) . . ? C13A C17 C12 51.0(17) . . ? C12A C17 C12 68.9(7) . . ? C16 C17 C12 136.4(11) . . ? C13A C17 C14A 11.8(17) . . ? C12A C17 C14A 108.4(8) . . ? C16 C17 C14A 175.7(10) . . ? C12 C17 C14A 39.6(5) . . ? C15A C18 C14A 123.1(17) . . ? C15A C18 C12 70.8(12) . . ? C14A C18 C12 52.5(9) . . ? C15A C18 C16A 20.6(11) . . ? C14A C18 C16A 102.6(11) . . ? C12 C18 C16A 50.3(6) . . ? C17 C12A C17A 137.0(10) . . ? C17 C12A C14 174.5(10) . . ? C17A C12A C14 42.7(7) . . ? C17 C12A C16 56.7(6) . . ? C17A C12A C16 166.1(10) . . ? C14 C12A C16 123.4(9) . . ? C17 C12A C15 122.4(9) . . ? C17A C12A C15 100.4(9) . . ? C14 C12A C15 57.8(6) . . ? C16 C12A C15 65.7(7) . . ? C17 C12A C18A 100.4(9) . . ? C17A C12A C18A 122.5(10) . . ? C14 C12A C18A 79.8(8) . . ? C16 C12A C18A 43.7(7) . . ? C15 C12A C18A 22.0(7) . . ? C17 C12A C13 118.8(8) . . ? C17A C12A C13 18.3(7) . . ? C14 C12A C13 60.9(7) . . ? C16 C12A C13 174.9(9) . . ? C15 C12A C13 118.6(9) . . ? C18A C12A C13 140.6(9) . . ? C17 C12A C12 62.1(6) . . ? C17A C12A C12 74.9(8) . . ? C14 C12A C12 117.3(9) . . ? C16 C12A C12 118.8(8) . . ? C15 C12A C12 173.9(9) . . ? C18A C12A C12 162.4(10) . . ? C13 C12A C12 56.6(6) . . ? C17 C12A C13A 16.8(6) . . ? C17A C12A C13A 120.4(10) . . ? C14 C12A C13A 162.7(9) . . ? C16 C12A C13A 73.4(7) . . ? C15 C12A C13A 139.1(9) . . ? C18A C12A C13A 117.1(9) . . ? C13 C12A C13A 102.2(7) . . ? C12 C12A C13A 45.6(5) . . ? C17 C13A C12 110(2) . . ? C17 C13A C14A 164(2) . . ? C12 C13A C14A 54.7(8) . . ? C17 C13A C12A 44.0(17) . . ? C12 C13A C12A 66.2(7) . . ? C14A C13A C12A 120.8(10) . . ? C17 C13A C16 6.3(17) . . ? C12 C13A C16 114.8(8) . . ? C14A C13A C16 169.5(10) . . ? C12A C13A C16 48.8(5) . . ? C18 C14A C12 86.6(12) . . ? C18 C14A C13A 143.8(15) . . ? C12 C14A C13A 57.3(8) . . ? C18 C14A C15A 25.2(8) . . ? C12 C14A C15A 61.6(8) . . ? C13A C14A C15A 118.8(11) . . ? C18 C14A C17 139.4(13) . . ? C12 C14A C17 52.9(7) . . ? C13A C14A C17 4.6(6) . . ? C15A C14A C17 114.4(9) . . ? C18 C15A C16A 147.8(16) . . ? C18 C15A C12 78.0(12) . . ? C16A C15A C12 69.9(8) . . ? C18 C15A C14A 31.8(10) . . ? C16A C15A C14A 116.1(10) . . ? C12 C15A C14A 46.4(6) . . ? C18 C15A C13 123.4(14) . . ? C16A C15A C13 24.4(6) . . ? C12 C15A C13 45.4(6) . . ? C14A C15A C13 91.8(8) . . ? C13 C16A C15A 120.5(13) . . ? C13 C16A C17A 8.5(10) . . ? C15A C16A C17A 128.8(11) . . ? C13 C16A C12 63.7(9) . . ? C15A C16A C12 56.8(7) . . ? C17A C16A C12 71.9(9) . . ? C13 C16A C18 108.9(10) . . ? C15A C16A C18 11.6(6) . . ? C17A C16A C18 117.2(9) . . ? C12 C16A C18 45.2(5) . . ? C14 C17A C12A 68.8(10) . . ? C14 C17A C16A 174.8(16) . . ? C12A C17A C16A 115.1(12) . . ? C14 C17A C12 125.2(13) . . ? C12A C17A C12 56.8(7) . . ? C16A C17A C12 58.4(7) . . ? C15 C18A C16 135(2) . . ? C15 C18A C12A 72.2(19) . . ? C16 C18A C12A 62.7(9) . . ? C15 C18A C14 25.1(18) . . ? C16 C18A C14 109.7(10) . . ? C12A C18A C14 47.1(6) . . ? C19A C19 C22A 131(3) . . ? C19A C19 C21A 126(3) . 2_545 ? C22A C19 C21A 103(2) . 2_545 ? C19A C19 C21B 69(2) . . ? C22A C19 C21B 62.2(15) . . ? C21A C19 C21B 165(2) 2_545 . ? C19A C19 C21 92(3) . 2_545 ? C22A C19 C21 136.9(19) . 2_545 ? C21A C19 C21 33.8(12) 2_545 2_545 ? C21B C19 C21 160.4(18) . 2_545 ? C19A C19 C22 171(3) . . ? C22A C19 C22 40.6(16) . . ? C21A C19 C22 63.2(19) 2_545 . ? C21B C19 C22 102.6(19) . . ? C21 C19 C22 96.9(18) 2_545 . ? C19A C19 C20 34(2) . . ? C22A C19 C20 97.3(15) . . ? C21A C19 C20 159.5(19) 2_545 . ? C21B C19 C20 35.2(10) . . ? C21 C19 C20 125.7(13) 2_545 . ? C22 C19 C20 137.2(18) . . ? C19A C19 C20A 73(2) . 2_545 ? C22A C19 C20A 156.0(17) . 2_545 ? C21A C19 C20A 52.8(14) 2_545 2_545 ? C21B C19 C20A 141.6(15) . 2_545 ? C21 C19 C20A 19.0(7) 2_545 2_545 ? C22 C19 C20A 115.8(18) . 2_545 ? C20 C19 C20A 106.7(9) . 2_545 ? C19A C19 C20A 10(2) . . ? C22A C19 C20A 121.1(15) . . ? C21A C19 C20A 135.6(18) 2_545 . ? C21B C19 C20A 58.9(12) . . ? C21 C19 C20A 101.9(10) 2_545 . ? C22 C19 C20A 160.8(18) . . ? C20 C19 C20A 23.9(5) . . ? C20A C19 C20A 82.8(7) 2_545 . ? C20A C20 C21B 159(2) . . ? C20A C20 C19A 81.5(19) . . ? C21B C20 C19A 78(2) . . ? C20A C20 C19 107.8(14) . . ? C21B C20 C19 52.0(14) . . ? C19A C20 C19 26.4(16) . . ? C20A C20 C21 0.9(10) . . ? C21B C20 C21 159.4(18) . . ? C19A C20 C21 81.6(18) . . ? C19 C20 C21 107.9(10) . . ? C20A C20 C22A 139.9(14) . . ? C21B C20 C22A 20.1(14) . . ? C19A C20 C22A 58.5(17) . . ? C19 C20 C22A 32.1(6) . . ? C21 C20 C22A 140.0(9) . . ? C21A C21 C20A 177(3) . . ? C21A C21 C19 54.4(19) . 2_545 ? C20A C21 C19 126.2(18) . 2_545 ? C21A C21 C19A 85(2) . 2_545 ? C20A C21 C19A 96.0(17) . 2_545 ? C19 C21 C19A 30.3(10) 2_545 2_545 ? C21A C21 C20 178(2) . . ? C20A C21 C20 1.0(11) . . ? C19 C21 C20 126.3(12) 2_545 . ? C19A C21 C20 96.1(13) 2_545 . ? C21A C21 C19A 147(2) . . ? C20A C21 C19A 33.8(14) . . ? C19 C21 C19A 92.4(12) 2_545 . ? C19A C21 C19A 62.2(15) 2_545 . ? C20 C21 C19A 33.9(9) . . ? C21A C21 C22 12(2) . 2_545 ? C20A C21 C22 167.9(17) . 2_545 ? C19 C21 C22 42.7(10) 2_545 2_545 ? C19A C21 C22 72.9(13) 2_545 2_545 ? C20 C21 C22 168.4(11) . 2_545 ? C19A C21 C22 134.8(12) . 2_545 ? C22A C22 C21A 97(2) . 2_545 ? C22A C22 C19 50.1(14) . . ? C21A C22 C19 47.0(12) 2_545 . ? C22A C22 C21 90(2) . 2_545 ? C21A C22 C21 6.6(11) 2_545 2_545 ? C19 C22 C21 40.5(11) . 2_545 ? C22A C22 C21B 14.7(17) . . ? C21A C22 C21B 82.7(13) 2_545 . ? C19 C22 C21B 35.8(10) . . ? C21 C22 C21B 76.2(9) 2_545 . ? C19 C19A C20 120(3) . . ? C19 C19A C21B 73(2) . . ? C20 C19A C21B 47.3(15) . . ? C19 C19A C20A 164(3) . . ? C20 C19A C20A 43.8(15) . . ? C21B C19A C20A 91(2) . . ? C19 C19A C21 58(2) . 2_545 ? C20 C19A C21 177(3) . 2_545 ? C21B C19A C21 131(3) . 2_545 ? C20A C19A C21 138(2) . 2_545 ? C19 C19A C21A 32(2) . 2_545 ? C20 C19A C21A 151(3) . 2_545 ? C21B C19A C21A 104(2) . 2_545 ? C20A C19A C21A 164(2) . 2_545 ? C21 C19A C21A 26.1(8) 2_545 2_545 ? C19 C19A C22A 28.5(17) . . ? C20 C19A C22A 91.7(19) . . ? C21B C19A C22A 44.6(14) . . ? C20A C19A C22A 135(2) . . ? C21 C19A C22A 86.0(19) 2_545 . ? C21A C19A C22A 59.9(16) 2_545 . ? C19 C19A C19A 121(4) . 2_545 ? C20 C19A C19A 118(3) . 2_545 ? C21B C19A C19A 165(4) . 2_545 ? C20A C19A C19A 75(2) . 2_545 ? C21 C19A C19A 64.0(17) 2_545 2_545 ? C21A C19A C19A 90(2) 2_545 2_545 ? C22A C19A C19A 150(3) . 2_545 ? C19 C19A C21 174(3) . . ? C20 C19A C21 64.5(18) . . ? C21B C19A C21 112(2) . . ? C20A C19A C21 20.7(8) . . ? C21 C19A C21 117.8(15) 2_545 . ? C21A C19A C21 143.8(17) 2_545 . ? C22A C19A C21 156(2) . . ? C19A C19A C21 53.8(16) 2_545 . ? C19 C19A C20A 82(3) . 2_545 ? C20 C19A C20A 158(3) . 2_545 ? C21B C19A C20A 155(3) . 2_545 ? C20A C19A C20A 113.9(18) . 2_545 ? C21 C19A C20A 24.6(6) 2_545 2_545 ? C21A C19A C20A 50.7(11) 2_545 2_545 ? C22A C19A C20A 111(2) . 2_545 ? C19A C19A C20A 39.4(13) 2_545 2_545 ? C21 C19A C20A 93.2(12) . 2_545 ? C21 C20A C20 178(2) . . ? C21 C20A C19A 126(2) . . ? C20 C20A C19A 54.7(14) . . ? C21 C20A C21A 1.4(14) . . ? C20 C20A C21A 179.2(16) . . ? C19A C20A C21A 125.8(17) . . ? C21 C20A C21B 169.7(17) . . ? C20 C20A C21B 10.8(11) . . ? C19A C20A C21B 44.3(13) . . ? C21A C20A C21B 169.8(12) . . ? C21 C20A C19A 59.4(15) . 2_545 ? C20 C20A C19A 120.8(16) . 2_545 ? C19A C20A C19A 66.1(18) . 2_545 ? C21A C20A C19A 59.7(13) . 2_545 ? C21B C20A C19A 110.4(14) . 2_545 ? C21 C20A C19 34.7(12) . 2_545 ? C20 C20A C19 145.5(13) . 2_545 ? C19A C20A C19 90.8(14) . 2_545 ? C21A C20A C19 35.0(8) . 2_545 ? C21B C20A C19 135.0(10) . 2_545 ? C19A C20A C19 24.7(8) 2_545 2_545 ? C21 C20A C19 131.9(15) . . ? C20 C20A C19 48.3(11) . . ? C19A C20A C19 6.5(14) . . ? C21A C20A C19 132.2(10) . . ? C21B C20A C19 37.9(7) . . ? C19A C20A C19 72.5(12) 2_545 . ? C19 C20A C19 97.2(7) 2_545 . ? C20 C21B C22A 145(2) . . ? C20 C21B C19A 54.6(18) . . ? C22A C21B C19A 91(2) . . ? C20 C21B C19 92.8(18) . . ? C22A C21B C19 52.4(13) . . ? C19A C21B C19 38.4(15) . . ? C20 C21B C20A 10.1(11) . . ? C22A C21B C20A 135.5(17) . . ? C19A C21B C20A 44.7(17) . . ? C19 C21B C20A 83.1(13) . . ? C20 C21B C22 134(2) . . ? C22A C21B C22 11.2(14) . . ? C19A C21B C22 80(2) . . ? C19 C21B C22 41.7(12) . . ? C20A C21B C22 124.6(14) . . ? C21 C21A C19 92(3) . 2_545 ? C21 C21A C22 161(3) . 2_545 ? C19 C21A C22 69.9(16) 2_545 2_545 ? C21 C21A C20A 1.4(15) . . ? C19 C21A C20A 92.2(18) 2_545 . ? C22 C21A C20A 161(2) 2_545 . ? C21 C21A C19A 69(2) . 2_545 ? C19 C21A C19A 22.6(13) 2_545 2_545 ? C22 C21A C19A 92.4(18) 2_545 2_545 ? C20A C21A C19A 69.6(12) . 2_545 ? C21 C21A C22A 130(3) . 2_545 ? C19 C21A C22A 38.0(12) 2_545 2_545 ? C22 C21A C22A 32.2(11) 2_545 2_545 ? C20A C21A C22A 130.2(16) . 2_545 ? C19A C21A C22A 60.6(13) 2_545 2_545 ? C22 C22A C19 89(2) . . ? C22 C22A C21B 154(3) . . ? C19 C22A C21B 65.4(16) . . ? C22 C22A C21A 51(2) . 2_545 ? C19 C22A C21A 38.7(12) . 2_545 ? C21B C22A C21A 104.1(17) . 2_545 ? C22 C22A C19A 110(3) . . ? C19 C22A C19A 20.8(13) . . ? C21B C22A C19A 44.6(14) . . ? C21A C22A C19A 59.5(16) 2_545 . ? C22 C22A C20 139(3) . . ? C19 C22A C20 50.6(12) . . ? C21B C22A C20 15.0(10) . . ? C21A C22A C20 89.3(12) 2_545 . ? C19A C22A C20 29.9(10) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.619 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.063 # Attachment '2.cif' data_p146c _database_code_depnum_ccdc_archive 'CCDC 614362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H51 Cl3 O3 P4 Pd' _chemical_formula_weight 1048.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2897(3) _cell_length_b 13.5853(6) _cell_length_c 19.9199(7) _cell_angle_alpha 86.390(2) _cell_angle_beta 89.649(2) _cell_angle_gamma 72.822(2) _cell_volume 2396.84(16) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 22632 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13389 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8354 _reflns_number_gt 6610 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Because of a slightly disorder of the water molecule O3 (disorder not solved), the hydrogen atoms could not be exact localized and were omitted. The hydrogen atom at methine C1 was localized and refined regulary with isotropic displacement parameters. Hydrogen atoms at O1 and O2 were found and refined with bond restraints (d=0.9 angs.). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.3976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'mixed; refined at C1 and O1,O2 (bond restr)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8354 _refine_ls_number_parameters 579 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.76635(3) 0.79673(2) 0.825836(12) 0.02313(8) Uani 1 1 d . . . P1 P 0.68429(9) 0.64954(7) 0.83048(4) 0.0231(2) Uani 1 1 d . . . P2 P 0.76424(9) 0.67331(7) 0.68951(4) 0.0234(2) Uani 1 1 d . . . P3 P 0.75316(9) 0.90789(7) 0.67828(4) 0.02242(19) Uani 1 1 d . . . P4 P 0.81903(9) 0.95337(7) 0.81362(4) 0.0240(2) Uani 1 1 d . . . Cl1 Cl 0.76207(13) 0.80647(8) 0.94203(4) 0.0471(3) Uani 1 1 d . . . Cl2 Cl 1.22471(10) 0.76040(8) 0.70472(5) 0.0428(2) Uani 1 1 d . . . Cl3 Cl 0.77947(13) 1.23180(9) 0.63797(5) 0.0544(3) Uani 1 1 d . . . O1 O 0.5574(4) 1.4348(3) 0.6969(2) 0.0701(10) Uani 1 1 d D . . H1OA H 0.610(6) 1.379(3) 0.677(3) 0.10(2) Uiso 1 1 d D . . H1OB H 0.515(5) 1.462(4) 0.6576(15) 0.074(18) Uiso 1 1 d D . . O2 O 0.3285(6) 1.5586(4) 0.6091(2) 0.1038(14) Uani 1 1 d D . . H2OA H 0.283(9) 1.620(4) 0.626(4) 0.20(4) Uiso 1 1 d D . . H2OB H 0.275(8) 1.584(6) 0.571(2) 0.16(3) Uiso 1 1 d D . . O3 O 0.2777(10) 1.5802(4) 0.4693(2) 0.209(4) Uani 1 1 d . . . C1 C 0.8067(4) 0.7824(3) 0.72245(16) 0.0240(7) Uani 1 1 d . . . H1 H 0.912(4) 0.767(3) 0.7211(16) 0.029(9) Uiso 1 1 d . . . C2 C 0.6273(3) 0.6407(3) 0.74344(16) 0.0256(8) Uani 1 1 d . . . H2A H 0.6244 0.5705 0.7365 0.031 Uiso 1 1 calc . . . H2B H 0.5269 0.6887 0.7337 0.031 Uiso 1 1 calc . . . C3 C 0.8652(3) 0.9696(3) 0.72456(16) 0.0246(7) Uani 1 1 d . . . H3A H 0.8404 1.0431 0.7101 0.030 Uiso 1 1 calc . . . H3B H 0.9728 0.9371 0.7174 0.030 Uiso 1 1 calc . . . C101 C 0.5236(4) 0.6424(3) 0.88154(17) 0.0285(8) Uani 1 1 d . . . C102 C 0.5327(4) 0.6477(3) 0.95060(19) 0.0445(10) Uani 1 1 d . . . H102 H 0.6178 0.6593 0.9699 0.053 Uiso 1 1 calc . . . C103 C 0.4170(5) 0.6359(4) 0.9911(2) 0.0575(13) Uani 1 1 d . . . H103 H 0.4237 0.6392 1.0379 0.069 Uiso 1 1 calc . . . C104 C 0.2923(5) 0.6195(4) 0.9631(2) 0.0603(13) Uani 1 1 d . . . H104 H 0.2130 0.6124 0.9907 0.072 Uiso 1 1 calc . . . C105 C 0.2834(5) 0.6134(4) 0.8951(2) 0.0595(13) Uani 1 1 d . . . H105 H 0.1982 0.6013 0.8762 0.071 Uiso 1 1 calc . . . C106 C 0.3984(4) 0.6248(3) 0.85372(18) 0.0409(10) Uani 1 1 d . . . H106 H 0.3913 0.6205 0.8070 0.049 Uiso 1 1 calc . . . C107 C 0.8221(3) 0.5275(3) 0.85649(16) 0.0259(8) Uani 1 1 d . . . C108 C 0.9393(4) 0.5268(3) 0.89918(18) 0.0337(9) Uani 1 1 d . . . H108 H 0.9510 0.5895 0.9118 0.040 Uiso 1 1 calc . . . C109 C 1.0397(4) 0.4341(3) 0.92348(18) 0.0385(9) Uani 1 1 d . . . H109 H 1.1186 0.4340 0.9528 0.046 Uiso 1 1 calc . . . C110 C 1.0237(4) 0.3432(3) 0.9047(2) 0.0468(11) Uani 1 1 d . . . H110 H 1.0922 0.2805 0.9210 0.056 Uiso 1 1 calc . . . C111 C 0.9083(5) 0.3422(3) 0.8622(2) 0.0507(11) Uani 1 1 d . . . H111 H 0.8984 0.2791 0.8493 0.061 Uiso 1 1 calc . . . C112 C 0.8068(4) 0.4343(3) 0.8383(2) 0.0411(10) Uani 1 1 d . . . H112 H 0.7271 0.4336 0.8096 0.049 Uiso 1 1 calc . . . C201 C 0.6975(4) 0.6893(3) 0.60420(17) 0.0300(8) Uani 1 1 d . . . C202 C 0.7988(5) 0.6579(3) 0.55282(19) 0.0449(10) Uani 1 1 d . . . H202 H 0.9026 0.6320 0.5624 0.054 Uiso 1 1 calc . . . C203 C 0.7454(6) 0.6649(4) 0.4866(2) 0.0618(13) Uani 1 1 d . . . H203 H 0.8130 0.6432 0.4515 0.074 Uiso 1 1 calc . . . C204 C 0.5937(6) 0.7039(4) 0.4734(2) 0.0618(14) Uani 1 1 d . . . H204 H 0.5577 0.7071 0.4291 0.074 Uiso 1 1 calc . . . C205 C 0.4944(5) 0.7380(4) 0.5235(2) 0.0603(13) Uani 1 1 d . . . H205 H 0.3913 0.7671 0.5132 0.072 Uiso 1 1 calc . . . C206 C 0.5445(4) 0.7302(3) 0.58962(19) 0.0427(10) Uani 1 1 d . . . H206 H 0.4756 0.7523 0.6243 0.051 Uiso 1 1 calc . . . C207 C 0.9296(4) 0.5644(3) 0.69837(16) 0.0263(8) Uani 1 1 d . . . C208 C 1.0575(4) 0.5656(3) 0.73310(19) 0.0361(9) Uani 1 1 d . . . H208 H 1.0666 0.6279 0.7477 0.043 Uiso 1 1 calc . . . C209 C 1.1727(4) 0.4740(3) 0.7463(2) 0.0470(11) Uani 1 1 d . . . H209 H 1.2596 0.4746 0.7700 0.056 Uiso 1 1 calc . . . C210 C 1.1599(5) 0.3836(3) 0.7250(2) 0.0508(11) Uani 1 1 d . . . H210 H 1.2370 0.3218 0.7350 0.061 Uiso 1 1 calc . . . C211 C 1.0357(5) 0.3824(3) 0.6892(2) 0.0502(11) Uani 1 1 d . . . H211 H 1.0294 0.3200 0.6733 0.060 Uiso 1 1 calc . . . C212 C 0.9199(4) 0.4716(3) 0.6761(2) 0.0395(9) Uani 1 1 d . . . H212 H 0.8340 0.4699 0.6520 0.047 Uiso 1 1 calc . . . C301 C 0.5593(3) 0.9783(3) 0.68690(16) 0.0243(7) Uani 1 1 d . . . C302 C 0.4564(4) 0.9341(3) 0.71675(19) 0.0369(9) Uani 1 1 d . . . H302 H 0.4872 0.8638 0.7314 0.044 Uiso 1 1 calc . . . C303 C 0.3088(4) 0.9925(3) 0.7252(2) 0.0453(10) Uani 1 1 d . . . H303 H 0.2395 0.9620 0.7456 0.054 Uiso 1 1 calc . . . C304 C 0.2638(4) 1.0943(3) 0.7038(2) 0.0451(10) Uani 1 1 d . . . H304 H 0.1635 1.1341 0.7097 0.054 Uiso 1 1 calc . . . C305 C 0.3649(5) 1.1394(3) 0.6734(2) 0.0448(10) Uani 1 1 d . . . H305 H 0.3328 1.2095 0.6583 0.054 Uiso 1 1 calc . . . C306 C 0.5131(4) 1.0819(3) 0.66515(18) 0.0333(9) Uani 1 1 d . . . H306 H 0.5821 1.1129 0.6449 0.040 Uiso 1 1 calc . . . C307 C 0.8055(4) 0.9086(3) 0.59129(16) 0.0258(8) Uani 1 1 d . . . C308 C 0.9550(4) 0.8608(3) 0.57588(18) 0.0419(10) Uani 1 1 d . . . H308 H 1.0252 0.8288 0.6102 0.050 Uiso 1 1 calc . . . C309 C 0.9994(4) 0.8608(4) 0.50947(19) 0.0485(11) Uani 1 1 d . . . H309 H 1.1000 0.8275 0.4987 0.058 Uiso 1 1 calc . . . C310 C 0.8990(4) 0.9084(4) 0.45966(18) 0.0470(11) Uani 1 1 d . . . H310 H 0.9306 0.9083 0.4147 0.056 Uiso 1 1 calc . . . C311 C 0.7519(5) 0.9568(4) 0.47475(18) 0.0497(11) Uani 1 1 d . . . H311 H 0.6833 0.9904 0.4402 0.060 Uiso 1 1 calc . . . C312 C 0.7041(4) 0.9563(3) 0.54057(18) 0.0408(10) Uani 1 1 d . . . H312 H 0.6027 0.9883 0.5507 0.049 Uiso 1 1 calc . . . C401 C 0.6636(4) 1.0659(3) 0.83077(16) 0.0264(8) Uani 1 1 d . . . C402 C 0.5550(5) 1.0568(3) 0.8768(2) 0.0485(11) Uani 1 1 d . . . H402 H 0.5560 0.9916 0.8962 0.058 Uiso 1 1 calc . . . C403 C 0.4446(5) 1.1452(4) 0.8940(3) 0.0647(14) Uani 1 1 d . . . H403 H 0.3719 1.1396 0.9259 0.078 Uiso 1 1 calc . . . C404 C 0.4401(5) 1.2398(3) 0.8652(2) 0.0516(11) Uani 1 1 d . . . H404 H 0.3647 1.2987 0.8775 0.062 Uiso 1 1 calc . . . C405 C 0.5436(4) 1.2495(3) 0.8190(2) 0.0435(10) Uani 1 1 d . . . H405 H 0.5389 1.3148 0.7988 0.052 Uiso 1 1 calc . . . C406 C 0.6566(4) 1.1626(3) 0.80164(18) 0.0357(9) Uani 1 1 d . . . H406 H 0.7288 1.1695 0.7699 0.043 Uiso 1 1 calc . . . C407 C 0.9772(4) 0.9656(3) 0.86172(16) 0.0278(8) Uani 1 1 d . . . C408 C 1.1117(4) 0.8881(3) 0.8612(2) 0.0489(11) Uani 1 1 d . . . H408 H 1.1216 0.8316 0.8348 0.059 Uiso 1 1 calc . . . C409 C 1.2327(4) 0.8936(4) 0.8998(2) 0.0566(12) Uani 1 1 d . . . H409 H 1.3248 0.8410 0.8990 0.068 Uiso 1 1 calc . . . C410 C 1.2193(5) 0.9744(4) 0.9390(2) 0.0513(11) Uani 1 1 d . . . H410 H 1.3019 0.9777 0.9648 0.062 Uiso 1 1 calc . . . C411 C 1.0846(5) 1.0512(3) 0.9405(2) 0.0525(11) Uani 1 1 d . . . H411 H 1.0747 1.1065 0.9680 0.063 Uiso 1 1 calc . . . C412 C 0.9635(4) 1.0476(3) 0.9017(2) 0.0419(10) Uani 1 1 d . . . H412 H 0.8719 1.1007 0.9025 0.050 Uiso 1 1 calc . . . 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 0.02758(14) 0.02303(15) 0.01966(14) -0.00205(10) -0.00157(10) -0.00868(11) P1 0.0238(4) 0.0235(5) 0.0221(5) 0.0004(4) -0.0021(4) -0.0076(4) P2 0.0252(4) 0.0223(5) 0.0221(4) -0.0031(4) -0.0016(4) -0.0057(4) P3 0.0239(4) 0.0220(5) 0.0210(4) -0.0014(4) -0.0015(4) -0.0062(4) P4 0.0265(5) 0.0247(5) 0.0227(5) -0.0041(4) 0.0012(4) -0.0101(4) Cl1 0.0782(7) 0.0510(6) 0.0217(5) -0.0037(4) -0.0004(5) -0.0335(6) Cl2 0.0337(5) 0.0441(6) 0.0495(6) -0.0019(5) -0.0084(4) -0.0100(4) Cl3 0.0665(7) 0.0471(7) 0.0524(7) -0.0045(5) 0.0170(5) -0.0211(6) O1 0.068(2) 0.058(2) 0.085(3) -0.022(2) -0.005(2) -0.0159(19) O2 0.159(4) 0.072(3) 0.071(3) 0.005(2) -0.008(3) -0.021(3) O3 0.469(11) 0.146(5) 0.083(3) 0.048(3) -0.105(5) -0.208(7) C1 0.0240(18) 0.0219(18) 0.0256(18) -0.0039(15) 0.0010(15) -0.0057(15) C2 0.0213(17) 0.0253(19) 0.0292(19) -0.0009(15) -0.0020(14) -0.0056(15) C3 0.0226(17) 0.0280(19) 0.0240(18) -0.0036(15) 0.0022(14) -0.0083(15) C101 0.0253(18) 0.029(2) 0.032(2) -0.0009(16) 0.0022(15) -0.0102(16) C102 0.042(2) 0.070(3) 0.030(2) -0.006(2) 0.0039(18) -0.030(2) C103 0.059(3) 0.095(4) 0.031(2) -0.009(2) 0.011(2) -0.040(3) C104 0.052(3) 0.092(4) 0.051(3) -0.009(3) 0.020(2) -0.043(3) C105 0.042(2) 0.091(4) 0.058(3) -0.006(3) 0.001(2) -0.038(3) C106 0.037(2) 0.061(3) 0.031(2) -0.003(2) 0.0010(17) -0.025(2) C107 0.0230(17) 0.030(2) 0.0248(18) 0.0008(15) 0.0016(14) -0.0080(15) C108 0.0283(19) 0.039(2) 0.035(2) -0.0007(17) -0.0018(16) -0.0110(17) C109 0.0263(19) 0.047(3) 0.036(2) 0.0081(19) -0.0065(16) -0.0031(18) C110 0.039(2) 0.038(3) 0.050(3) 0.013(2) -0.003(2) 0.0062(19) C111 0.064(3) 0.026(2) 0.060(3) 0.003(2) -0.006(2) -0.010(2) C112 0.045(2) 0.029(2) 0.048(2) 0.0053(18) -0.0154(19) -0.0105(18) C201 0.038(2) 0.030(2) 0.0246(19) -0.0027(16) -0.0036(16) -0.0148(17) C202 0.055(3) 0.047(3) 0.034(2) -0.0046(19) 0.003(2) -0.017(2) C203 0.093(4) 0.070(3) 0.026(2) -0.003(2) 0.010(2) -0.030(3) C204 0.092(4) 0.077(4) 0.031(2) 0.007(2) -0.017(3) -0.050(3) C205 0.062(3) 0.084(4) 0.046(3) 0.018(3) -0.026(2) -0.042(3) C206 0.040(2) 0.057(3) 0.033(2) 0.0036(19) -0.0078(18) -0.020(2) C207 0.0240(17) 0.027(2) 0.0262(18) -0.0045(15) 0.0028(14) -0.0050(15) C208 0.0290(19) 0.032(2) 0.047(2) -0.0078(18) 0.0005(17) -0.0086(17) C209 0.029(2) 0.046(3) 0.059(3) -0.009(2) -0.0131(19) 0.0016(19) C210 0.044(2) 0.038(3) 0.059(3) -0.012(2) -0.006(2) 0.007(2) C211 0.057(3) 0.028(2) 0.059(3) -0.015(2) -0.006(2) 0.001(2) C212 0.037(2) 0.029(2) 0.050(2) -0.0094(19) -0.0080(18) -0.0044(17) C301 0.0253(17) 0.0251(19) 0.0221(17) -0.0017(15) -0.0015(14) -0.0066(15) C302 0.034(2) 0.030(2) 0.048(2) -0.0009(18) 0.0032(18) -0.0103(17) C303 0.030(2) 0.040(3) 0.066(3) 0.000(2) 0.011(2) -0.0106(19) C304 0.030(2) 0.044(3) 0.052(3) -0.009(2) 0.0032(19) 0.0037(19) C305 0.050(3) 0.028(2) 0.047(2) -0.0005(19) 0.005(2) 0.0036(19) C306 0.036(2) 0.030(2) 0.032(2) -0.0026(17) 0.0053(16) -0.0075(17) C307 0.0285(18) 0.0242(19) 0.0244(18) -0.0016(15) 0.0009(15) -0.0071(15) C308 0.032(2) 0.060(3) 0.028(2) -0.0019(19) -0.0040(17) -0.0046(19) C309 0.031(2) 0.077(3) 0.034(2) -0.008(2) 0.0051(18) -0.010(2) C310 0.045(2) 0.074(3) 0.025(2) -0.005(2) 0.0060(18) -0.021(2) C311 0.046(2) 0.072(3) 0.023(2) 0.004(2) -0.0058(18) -0.007(2) C312 0.030(2) 0.059(3) 0.026(2) -0.0012(19) -0.0037(16) -0.0019(19) C401 0.0278(18) 0.026(2) 0.0280(19) -0.0050(15) -0.0015(15) -0.0106(15) C402 0.049(3) 0.034(2) 0.063(3) -0.006(2) 0.023(2) -0.013(2) C403 0.053(3) 0.057(3) 0.083(4) -0.015(3) 0.039(3) -0.013(2) C404 0.041(2) 0.038(3) 0.072(3) -0.019(2) 0.011(2) -0.003(2) C405 0.046(2) 0.029(2) 0.051(3) -0.0055(19) -0.001(2) -0.0046(19) C406 0.039(2) 0.032(2) 0.038(2) -0.0055(18) 0.0076(17) -0.0132(18) C407 0.0328(19) 0.031(2) 0.0222(18) -0.0006(15) 0.0003(15) -0.0137(17) C408 0.043(2) 0.049(3) 0.053(3) -0.019(2) -0.008(2) -0.007(2) C409 0.034(2) 0.068(3) 0.063(3) -0.009(3) -0.012(2) -0.006(2) C410 0.048(3) 0.066(3) 0.048(3) 0.007(2) -0.021(2) -0.031(2) C411 0.069(3) 0.045(3) 0.052(3) -0.005(2) -0.021(2) -0.030(2) C412 0.046(2) 0.033(2) 0.049(2) -0.0084(19) -0.0119(19) -0.0128(19) _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 2.102(3) . ? Pd1 P4 2.3185(9) . ? Pd1 Cl1 2.3260(9) . ? Pd1 P1 2.3376(9) . ? P1 C107 1.817(3) . ? P1 C101 1.824(3) . ? P1 C2 1.837(3) . ? P2 C201 1.791(3) . ? P2 C207 1.791(3) . ? P2 C2 1.796(3) . ? P2 C1 1.804(3) . ? P3 C301 1.786(3) . ? P3 C307 1.797(3) . ? P3 C1 1.801(3) . ? P3 C3 1.806(3) . ? P4 C407 1.813(3) . ? P4 C401 1.815(3) . ? P4 C3 1.838(3) . ? O1 H1OA 0.88(2) . ? O1 H1OB 0.887(19) . ? O2 H2OA 0.90(2) . ? O2 H2OB 0.91(2) . ? C1 H1 0.94(3) . ? C101 C106 1.381(5) . ? C101 C102 1.386(5) . ? C102 C103 1.380(5) . ? C103 C104 1.371(6) . ? C104 C105 1.368(6) . ? C105 C106 1.383(5) . ? C107 C108 1.383(5) . ? C107 C112 1.385(5) . ? C108 C109 1.388(5) . ? C109 C110 1.361(6) . ? C110 C111 1.374(6) . ? C111 C112 1.384(5) . ? C201 C202 1.386(5) . ? C201 C206 1.390(5) . ? C202 C203 1.399(6) . ? C203 C204 1.372(7) . ? C204 C205 1.363(7) . ? C205 C206 1.386(5) . ? C207 C208 1.383(5) . ? C207 C212 1.391(5) . ? C208 C209 1.392(5) . ? C209 C210 1.362(6) . ? C210 C211 1.365(6) . ? C211 C212 1.374(5) . ? C301 C302 1.383(5) . ? C301 C306 1.387(5) . ? C302 C303 1.382(5) . ? C303 C304 1.363(6) . ? C304 C305 1.382(6) . ? C305 C306 1.382(5) . ? C307 C312 1.377(5) . ? C307 C308 1.390(5) . ? C308 C309 1.383(5) . ? C309 C310 1.359(5) . ? C310 C311 1.371(5) . ? C311 C312 1.382(5) . ? C401 C406 1.387(5) . ? C401 C402 1.387(5) . ? C402 C403 1.390(6) . ? C403 C404 1.363(6) . ? C404 C405 1.356(6) . ? C405 C406 1.389(5) . ? C407 C408 1.376(5) . ? C407 C412 1.385(5) . ? C408 C409 1.389(5) . ? C409 C410 1.362(6) . ? C410 C411 1.373(6) . ? C411 C412 1.384(5) . ? 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 P4 87.66(9) . . ? C1 Pd1 Cl1 171.10(10) . . ? P4 Pd1 Cl1 89.92(3) . . ? C1 Pd1 P1 89.97(9) . . ? P4 Pd1 P1 172.58(3) . . ? Cl1 Pd1 P1 93.46(3) . . ? C107 P1 C101 101.04(15) . . ? C107 P1 C2 107.43(15) . . ? C101 P1 C2 105.20(15) . . ? C107 P1 Pd1 117.01(11) . . ? C101 P1 Pd1 120.98(12) . . ? C2 P1 Pd1 104.14(11) . . ? C201 P2 C207 109.29(16) . . ? C201 P2 C2 109.29(16) . . ? C207 P2 C2 105.33(16) . . ? C201 P2 C1 116.49(16) . . ? C207 P2 C1 108.19(16) . . ? C2 P2 C1 107.66(15) . . ? C301 P3 C307 110.36(15) . . ? C301 P3 C1 113.90(16) . . ? C307 P3 C1 114.82(15) . . ? C301 P3 C3 108.26(15) . . ? C307 P3 C3 109.07(15) . . ? C1 P3 C3 99.66(15) . . ? C407 P4 C401 105.11(15) . . ? C407 P4 C3 106.30(15) . . ? C401 P4 C3 106.33(15) . . ? C407 P4 Pd1 117.09(12) . . ? C401 P4 Pd1 115.34(11) . . ? C3 P4 Pd1 105.88(11) . . ? H1OA O1 H1OB 89(5) . . ? H2OA O2 H2OB 87(7) . . ? H1 C1 P3 100(2) . . ? H1 C1 P2 106(2) . . ? P3 C1 P2 121.93(19) . . ? H1 C1 Pd1 102(2) . . ? P3 C1 Pd1 110.18(16) . . ? P2 C1 Pd1 114.19(17) . . ? P2 C2 P1 107.12(16) . . ? P3 C3 P4 106.09(16) . . ? C106 C101 C102 119.4(3) . . ? C106 C101 P1 121.6(3) . . ? C102 C101 P1 118.8(3) . . ? C103 C102 C101 120.2(3) . . ? C104 C103 C102 120.1(4) . . ? C105 C104 C103 120.0(4) . . ? C104 C105 C106 120.7(4) . . ? C101 C106 C105 119.6(3) . . ? C108 C107 C112 119.0(3) . . ? C108 C107 P1 119.4(3) . . ? C112 C107 P1 121.5(3) . . ? C107 C108 C109 120.4(3) . . ? C110 C109 C108 119.8(3) . . ? C109 C110 C111 120.7(4) . . ? C110 C111 C112 119.9(4) . . ? C111 C112 C107 120.2(3) . . ? C202 C201 C206 120.0(3) . . ? C202 C201 P2 119.7(3) . . ? C206 C201 P2 120.3(3) . . ? C201 C202 C203 119.5(4) . . ? C204 C203 C202 119.5(4) . . ? C205 C204 C203 121.0(4) . . ? C204 C205 C206 120.4(4) . . ? C205 C206 C201 119.4(4) . . ? C208 C207 C212 119.1(3) . . ? C208 C207 P2 123.2(3) . . ? C212 C207 P2 117.2(3) . . ? C207 C208 C209 119.7(3) . . ? C210 C209 C208 120.2(4) . . ? C209 C210 C211 120.3(4) . . ? C210 C211 C212 120.5(4) . . ? C211 C212 C207 120.0(3) . . ? C302 C301 C306 119.5(3) . . ? C302 C301 P3 122.3(3) . . ? C306 C301 P3 118.1(3) . . ? C303 C302 C301 120.5(4) . . ? C304 C303 C302 119.8(4) . . ? C303 C304 C305 120.3(3) . . ? C306 C305 C304 120.3(4) . . ? C305 C306 C301 119.5(3) . . ? C312 C307 C308 119.8(3) . . ? C312 C307 P3 122.4(3) . . ? C308 C307 P3 117.8(3) . . ? C309 C308 C307 119.3(3) . . ? C310 C309 C308 120.6(3) . . ? C309 C310 C311 120.2(3) . . ? C310 C311 C312 120.3(4) . . ? C307 C312 C311 119.7(3) . . ? C406 C401 C402 119.1(3) . . ? C406 C401 P4 120.9(3) . . ? C402 C401 P4 119.9(3) . . ? C401 C402 C403 119.2(4) . . ? C404 C403 C402 120.9(4) . . ? C405 C404 C403 120.5(4) . . ? C404 C405 C406 119.8(4) . . ? C401 C406 C405 120.5(3) . . ? C408 C407 C412 119.4(3) . . ? C408 C407 P4 118.7(3) . . ? C412 C407 P4 121.7(3) . . ? C407 C408 C409 119.8(4) . . ? C410 C409 C408 120.7(4) . . ? C409 C410 C411 119.8(4) . . ? C410 C411 C412 120.3(4) . . ? C411 C412 C407 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.587 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.077 # Attachment '3.cif' data_p148 _database_code_depnum_ccdc_archive 'CCDC 614363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H51.50 Cl6.50 P4' _chemical_formula_weight 1078.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 15.2377(6) _cell_length_b 20.5124(7) _cell_length_c 8.7621(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2738.70(19) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 81370 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15158 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4284 _reflns_number_gt 3750 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Half a molecule lies in the asymmetric unit and will be completed by a twofold rotation axis. 3:1 occupation disorder with nearly overlying positions of solvent chloroform with occupation of 0.75 and toluene occupation of 0.25. Toluene were refined isotropically with bond restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+1.3875P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(10) _refine_ls_number_reflns 4284 _refine_ls_number_parameters 323 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.97042(7) 1.15092(5) 0.69868(12) 0.0617(3) Uani 1 1 d . . . P1 P 0.89723(6) 0.99554(4) 0.95014(10) 0.0411(2) Uani 1 1 d . . . P2 P 0.75499(7) 1.07686(5) 1.10161(13) 0.0514(3) Uani 1 1 d . . . C1 C 1.0000 1.0000 0.8485(5) 0.0403(11) Uani 1 2 d S . . H1A H 0.9970 1.0383 0.7819 0.048 Uiso 0.50 1 calc P . . H1B H 1.0030 0.9617 0.7819 0.048 Uiso 0.50 1 calc P . . C2 C 0.8695(2) 1.07422(18) 1.0270(4) 0.0463(9) Uani 1 1 d . . . H2A H 0.8763 1.1073 0.9471 0.056 Uiso 1 1 calc . . . H2B H 0.9104 1.0849 1.1098 0.056 Uiso 1 1 calc . . . C101 C 0.8162(2) 0.97498(17) 0.8114(5) 0.0446(8) Uani 1 1 d . . . C102 C 0.7550(3) 0.92674(19) 0.8379(5) 0.0582(10) Uani 1 1 d . . . H102 H 0.7571 0.9020 0.9281 0.070 Uiso 1 1 calc . . . C103 C 0.6905(3) 0.9152(2) 0.7301(7) 0.0763(14) Uani 1 1 d . . . H103 H 0.6482 0.8827 0.7476 0.092 Uiso 1 1 calc . . . C104 C 0.6879(3) 0.9508(3) 0.5990(6) 0.0732(14) Uani 1 1 d . . . H104 H 0.6442 0.9419 0.5262 0.088 Uiso 1 1 calc . . . C105 C 0.7477(3) 0.9992(3) 0.5709(5) 0.0699(12) Uani 1 1 d . . . H105 H 0.7440 1.0241 0.4811 0.084 Uiso 1 1 calc . . . C106 C 0.8138(3) 1.0110(2) 0.6768(5) 0.0570(10) Uani 1 1 d . . . H106 H 0.8565 1.0430 0.6575 0.068 Uiso 1 1 calc . . . C107 C 0.9049(2) 0.93506(17) 1.0957(4) 0.0453(8) Uani 1 1 d . . . C108 C 0.9183(3) 0.86978(18) 1.0525(5) 0.0516(9) Uani 1 1 d . . . H108 H 0.9187 0.8581 0.9488 0.062 Uiso 1 1 calc . . . C109 C 0.9310(3) 0.8227(2) 1.1647(5) 0.0619(11) Uani 1 1 d . . . H109 H 0.9400 0.7790 1.1367 0.074 Uiso 1 1 calc . . . C110 C 0.9306(3) 0.8397(2) 1.3161(6) 0.0663(12) Uani 1 1 d . . . H110 H 0.9398 0.8077 1.3911 0.080 Uiso 1 1 calc . . . C111 C 0.9165(3) 0.9039(2) 1.3589(5) 0.0665(12) Uani 1 1 d . . . H111 H 0.9168 0.9154 1.4627 0.080 Uiso 1 1 calc . . . C112 C 0.9023(3) 0.9505(2) 1.2495(4) 0.0595(11) Uani 1 1 d . . . H112 H 0.8905 0.9936 1.2794 0.071 Uiso 1 1 calc . . . C201 C 0.6907(3) 1.09858(19) 0.9350(5) 0.0556(10) Uani 1 1 d . . . C202 C 0.6111(3) 1.0668(2) 0.9161(7) 0.0833(15) Uani 1 1 d . . . H202 H 0.5940 1.0340 0.9850 0.100 Uiso 1 1 calc . . . C203 C 0.5572(4) 1.0834(3) 0.7962(11) 0.119(2) Uani 1 1 d . . . H203 H 0.5033 1.0618 0.7851 0.143 Uiso 1 1 calc . . . C204 C 0.5792(5) 1.1295(3) 0.6950(9) 0.110(2) Uani 1 1 d . . . H204 H 0.5409 1.1403 0.6149 0.132 Uiso 1 1 calc . . . C205 C 0.6583(4) 1.1606(3) 0.7096(7) 0.0866(15) Uani 1 1 d . . . H205 H 0.6747 1.1924 0.6379 0.104 Uiso 1 1 calc . . . C206 C 0.7144(3) 1.1455(3) 0.8290(6) 0.0711(13) Uani 1 1 d . . . H206 H 0.7685 1.1672 0.8381 0.085 Uiso 1 1 calc . . . C207 C 0.7585(3) 1.15332(18) 1.2080(5) 0.0513(9) Uani 1 1 d . . . C208 C 0.6942(3) 1.2004(2) 1.1920(6) 0.0694(12) Uani 1 1 d . . . H208 H 0.6510 1.1956 1.1162 0.083 Uiso 1 1 calc . . . C209 C 0.6928(4) 1.2547(2) 1.2870(6) 0.0755(14) Uani 1 1 d . . . H209 H 0.6479 1.2858 1.2762 0.091 Uiso 1 1 calc . . . C210 C 0.7552(4) 1.2632(2) 1.3942(6) 0.0744(13) Uani 1 1 d . . . H210 H 0.7537 1.3002 1.4576 0.089 Uiso 1 1 calc . . . C211 C 0.8215(4) 1.2176(2) 1.4113(6) 0.0751(13) Uani 1 1 d . . . H211 H 0.8662 1.2242 1.4837 0.090 Uiso 1 1 calc . . . C212 C 0.8215(3) 1.1629(2) 1.3220(5) 0.0649(12) Uani 1 1 d . . . H212 H 0.8648 1.1309 1.3376 0.078 Uiso 1 1 calc . . . C3 C 0.9012(5) 1.3029(3) 1.8129(8) 0.0763(17) Uani 0.75 1 d P A 1 H3 H 0.9134 1.2609 1.7612 0.092 Uiso 0.75 1 calc P B 1 Cl2 Cl 0.79396(15) 1.32499(14) 1.7772(3) 0.1218(9) Uani 0.75 1 d P A 1 Cl3 Cl 0.9162(3) 1.2934(2) 2.0029(3) 0.209(2) Uani 0.75 1 d P A 1 Cl4 Cl 0.9681(3) 1.3627(3) 1.7348(9) 0.231(3) Uani 0.75 1 d P A 1 C4 C 0.8989(14) 1.3539(9) 1.792(3) 0.102(7) Uiso 0.25 1 d PD C 2 C5 C 0.8750(11) 1.4185(9) 1.794(2) 0.080(5) Uiso 0.25 1 d PD C 2 H5 H 0.8177 1.4294 1.8246 0.096 Uiso 0.25 1 calc P D 2 C6 C 0.9320(15) 1.4687(9) 1.752(3) 0.115(9) Uiso 0.25 1 d PD . 2 H6 H 0.9169 1.5123 1.7721 0.138 Uiso 0.25 1 calc P E 2 C7 C 1.0116(14) 1.4540(10) 1.681(3) 0.106(7) Uiso 0.25 1 d PD . 2 H7 H 1.0477 1.4865 1.6385 0.128 Uiso 0.25 1 calc P F 2 C8 C 1.0343(15) 1.3882(11) 1.676(4) 0.130(10) Uiso 0.25 1 d PD C 2 H8 H 1.0888 1.3771 1.6331 0.157 Uiso 0.25 1 calc P G 2 C9 C 0.983(2) 1.3384(10) 1.731(6) 0.16(2) Uiso 0.25 1 d PD C 2 H9 H 1.0024 1.2950 1.7273 0.187 Uiso 0.25 1 calc P H 2 C10 C 0.839(2) 1.3002(14) 1.857(4) 0.121(10) Uiso 0.25 1 d PD C 2 H10A H 0.8653 1.2828 1.9493 0.181 Uiso 0.25 1 calc PR C 2 H10B H 0.8333 1.2655 1.7821 0.181 Uiso 0.25 1 calc PR C 2 H10C H 0.7821 1.3183 1.8797 0.181 Uiso 0.25 1 calc PR C 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 Cl1 0.0593(6) 0.0669(6) 0.0589(6) 0.0095(5) -0.0008(5) -0.0037(5) P1 0.0338(5) 0.0444(5) 0.0451(5) 0.0002(4) 0.0008(4) 0.0033(4) P2 0.0379(5) 0.0519(6) 0.0643(6) 0.0032(5) 0.0075(5) 0.0063(5) C1 0.032(2) 0.048(3) 0.041(3) 0.000 0.000 0.004(2) C2 0.0349(19) 0.0443(19) 0.060(2) -0.0057(18) 0.0026(17) 0.0007(16) C101 0.0332(18) 0.050(2) 0.051(2) -0.0005(17) -0.0018(17) 0.0026(16) C102 0.044(2) 0.052(2) 0.078(3) 0.0011(19) -0.004(2) 0.001(2) C103 0.048(2) 0.075(3) 0.106(4) -0.007(3) -0.019(3) -0.009(2) C104 0.045(3) 0.088(3) 0.086(4) -0.029(3) -0.023(2) 0.003(2) C105 0.056(3) 0.097(3) 0.057(2) -0.005(3) -0.013(2) 0.009(3) C106 0.044(2) 0.072(3) 0.054(2) 0.000(2) -0.0001(18) -0.004(2) C107 0.0360(19) 0.050(2) 0.050(2) 0.0044(16) 0.0054(17) 0.0037(17) C108 0.052(2) 0.047(2) 0.056(2) 0.0032(18) 0.0054(19) -0.0031(18) C109 0.059(3) 0.049(2) 0.078(3) 0.004(2) 0.003(2) 0.0018(19) C110 0.062(3) 0.065(3) 0.072(3) 0.022(2) 0.005(2) 0.000(2) C111 0.075(3) 0.071(3) 0.053(2) 0.013(2) 0.000(2) 0.008(2) C112 0.062(3) 0.063(2) 0.053(3) -0.0035(19) 0.002(2) 0.013(2) C201 0.037(2) 0.054(2) 0.075(3) -0.002(2) -0.003(2) 0.0086(18) C202 0.050(3) 0.076(3) 0.123(4) 0.014(3) -0.017(3) -0.005(3) C203 0.068(4) 0.101(4) 0.189(7) 0.025(5) -0.056(4) -0.012(3) C204 0.096(5) 0.101(4) 0.133(5) -0.005(4) -0.060(4) 0.025(4) C205 0.094(4) 0.084(3) 0.081(3) 0.015(3) -0.004(3) 0.025(3) C206 0.049(2) 0.085(3) 0.079(3) 0.016(3) -0.001(2) 0.007(2) C207 0.050(2) 0.052(2) 0.051(2) 0.0030(18) 0.011(2) 0.0115(19) C208 0.059(3) 0.079(3) 0.070(3) -0.005(3) 0.001(2) 0.025(2) C209 0.090(4) 0.061(3) 0.075(3) 0.003(3) 0.013(3) 0.031(3) C210 0.100(4) 0.053(3) 0.070(3) -0.005(2) 0.013(3) 0.010(3) C211 0.081(3) 0.070(3) 0.074(3) -0.015(2) -0.002(3) 0.004(3) C212 0.064(3) 0.067(3) 0.064(3) -0.004(2) 0.001(2) 0.026(2) C3 0.070(4) 0.078(4) 0.081(4) -0.001(4) -0.010(4) 0.018(4) Cl2 0.0744(12) 0.155(2) 0.1354(19) -0.0569(17) -0.0248(13) 0.0285(13) Cl3 0.285(5) 0.251(4) 0.0901(16) -0.040(2) -0.050(2) 0.172(4) Cl4 0.097(2) 0.208(4) 0.387(8) 0.125(5) 0.009(3) -0.013(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 P1 C107 1.783(4) . ? P1 C101 1.783(4) . ? P1 C2 1.799(4) . ? P1 C1 1.804(2) . ? P2 C201 1.814(4) . ? P2 C207 1.825(4) . ? P2 C2 1.864(4) . ? C1 P1 1.804(2) 2_775 ? C101 C102 1.380(5) . ? C101 C106 1.392(6) . ? C102 C103 1.383(6) . ? C103 C104 1.361(8) . ? C104 C105 1.370(7) . ? C105 C106 1.391(6) . ? C107 C112 1.385(6) . ? C107 C108 1.407(5) . ? C108 C109 1.392(6) . ? C109 C110 1.371(7) . ? C110 C111 1.385(7) . ? C111 C112 1.371(6) . ? C201 C206 1.386(6) . ? C201 C202 1.386(6) . ? C202 C203 1.376(9) . ? C203 C204 1.338(10) . ? C204 C205 1.370(8) . ? C205 C206 1.386(7) . ? C207 C208 1.383(6) . ? C207 C212 1.399(6) . ? C208 C209 1.391(7) . ? C209 C210 1.348(8) . ? C210 C211 1.385(7) . ? C211 C212 1.368(6) . ? C3 Cl3 1.692(8) . ? C3 Cl2 1.724(7) . ? C3 Cl4 1.736(9) . ? C4 C5 1.375(15) . ? C4 C9 1.421(17) . ? C4 C10 1.536(18) . ? C5 C6 1.395(16) . ? C6 C7 1.398(16) . ? C6 C7 1.91(3) 2_785 ? C7 C8 1.394(16) . ? C7 C6 1.91(3) 2_785 ? C7 C7 1.92(4) 2_785 ? C8 C9 1.373(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C107 P1 C101 111.61(18) . . ? C107 P1 C2 111.81(18) . . ? C101 P1 C2 107.76(17) . . ? C107 P1 C1 109.38(15) . . ? C101 P1 C1 106.05(18) . . ? C2 P1 C1 110.06(13) . . ? C201 P2 C207 102.48(18) . . ? C201 P2 C2 103.33(19) . . ? C207 P2 C2 100.16(17) . . ? P1 C1 P1 120.9(2) . 2_775 ? P1 C2 P2 112.14(19) . . ? C102 C101 C106 120.3(4) . . ? C102 C101 P1 121.5(3) . . ? C106 C101 P1 118.1(3) . . ? C101 C102 C103 119.2(4) . . ? C104 C103 C102 120.4(4) . . ? C103 C104 C105 121.3(4) . . ? C104 C105 C106 119.2(4) . . ? C105 C106 C101 119.5(4) . . ? C112 C107 C108 118.9(3) . . ? C112 C107 P1 122.4(3) . . ? C108 C107 P1 118.6(3) . . ? C109 C108 C107 119.4(4) . . ? C110 C109 C108 120.4(4) . . ? C109 C110 C111 120.3(4) . . ? C112 C111 C110 119.9(4) . . ? C111 C112 C107 121.1(4) . . ? C206 C201 C202 118.4(4) . . ? C206 C201 P2 124.7(3) . . ? C202 C201 P2 116.9(4) . . ? C203 C202 C201 119.8(5) . . ? C204 C203 C202 122.1(5) . . ? C203 C204 C205 119.2(5) . . ? C204 C205 C206 120.6(5) . . ? C205 C206 C201 120.0(5) . . ? C208 C207 C212 117.5(4) . . ? C208 C207 P2 121.8(3) . . ? C212 C207 P2 120.3(3) . . ? C207 C208 C209 120.6(5) . . ? C210 C209 C208 120.7(4) . . ? C209 C210 C211 120.1(4) . . ? C212 C211 C210 119.5(5) . . ? C211 C212 C207 121.5(4) . . ? Cl3 C3 Cl2 109.7(5) . . ? Cl3 C3 Cl4 113.0(6) . . ? Cl2 C3 Cl4 107.4(4) . . ? C5 C4 C9 117.3(13) . . ? C5 C4 C10 122(2) . . ? C9 C4 C10 121(2) . . ? C4 C5 C6 122.8(13) . . ? C5 C6 C7 119.9(13) . . ? C5 C6 C7 168(2) . 2_785 ? C7 C6 C7 69.0(17) . 2_785 ? C8 C7 C6 115.9(13) . . ? C8 C7 C6 135(2) . 2_785 ? C6 C7 C6 94(2) . 2_785 ? C8 C7 C7 175.9(19) . 2_785 ? C6 C7 C7 68.2(15) . 2_785 ? C6 C7 C7 42.8(8) 2_785 2_785 ? C9 C8 C7 124.6(14) . . ? C8 C9 C4 118.6(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.594 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.047