# 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 ? loop_ _publ_author_name R.Bedford R.A.Baber M.Betham M.E.Blake S.Coles M.F.Haddow ; M.Hursthouse ; A.Orpen L.T.Pilarski P.Pringle R.L.Wingad _publ_contact_author_name 'Robin Bedford' _publ_contact_author_email R.BEDFORD@BRISTOL.AC.UK data_04src0835 _database_code_depnum_ccdc_archive 'CCDC 614135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H45 Cl7 O6 P2 Pd' _chemical_formula_weight 1230.41 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.7215(14) _cell_length_b 21.165(4) _cell_length_c 25.864(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5321.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6659 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7373 _exptl_absorpt_correction_T_max 0.8546 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 38750 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12089 _reflns_number_gt 10489 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+3.8023P] 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 0.019(18) _refine_ls_number_reflns 12089 _refine_ls_number_parameters 683 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_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_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 C1S C 0.2892(4) 0.44297(17) 0.95555(14) 0.0277(8) Uani 1 1 d . . . H1S H 0.3692 0.4726 0.9544 0.033 Uiso 1 1 calc R . . C1 C 0.5271(3) 0.43092(17) 0.07526(12) 0.0191(7) Uani 1 1 d . . . C2 C 0.4445(3) 0.44393(17) 0.11823(13) 0.0225(8) Uani 1 1 d . . . H2 H 0.3965 0.4829 0.1208 0.027 Uiso 1 1 calc R . . C2S C 0.8690(5) 0.5130(2) 0.80789(18) 0.0544(12) Uani 1 1 d . . . H2S H 0.7960 0.5087 0.8349 0.065 Uiso 1 1 calc R A 1 C3 C 0.4341(4) 0.39966(17) 0.15644(13) 0.0252(8) Uani 1 1 d . . . H3 H 0.3756 0.4070 0.1853 0.030 Uiso 1 1 calc R . . C4 C 0.5105(4) 0.34282(18) 0.15308(13) 0.0240(8) Uani 1 1 d . . . C5 C 0.5024(4) 0.29697(19) 0.19310(14) 0.0309(9) Uani 1 1 d . . . H5 H 0.4462 0.3050 0.2224 0.037 Uiso 1 1 calc R . . C6 C 0.5728(4) 0.24243(19) 0.19021(14) 0.0303(9) Uani 1 1 d . . . H6 H 0.5631 0.2117 0.2167 0.036 Uiso 1 1 calc R . . C7 C 0.6605(4) 0.23081(18) 0.14817(14) 0.0284(8) Uani 1 1 d . . . H7 H 0.7122 0.1928 0.1470 0.034 Uiso 1 1 calc R . . C8 C 0.6723(4) 0.27400(16) 0.10858(13) 0.0222(7) Uani 1 1 d . . . H8 H 0.7340 0.2659 0.0809 0.027 Uiso 1 1 calc R . . C9 C 0.5940(3) 0.33000(15) 0.10871(12) 0.0160(7) Uani 1 1 d . . . C10 C 0.5985(3) 0.37577(15) 0.06774(12) 0.0172(7) Uani 1 1 d . . . C11 C 0.7741(3) 0.41281(16) 0.00449(12) 0.0179(7) Uani 1 1 d . . . C12 C 0.6838(3) 0.36644(16) 0.01979(12) 0.0167(7) Uani 1 1 d . . . C13 C 0.6729(3) 0.31153(15) -0.01227(12) 0.0179(7) Uani 1 1 d . . . C14 C 0.5728(4) 0.26440(16) -0.00481(13) 0.0215(7) Uani 1 1 d . . . H14 H 0.5096 0.2684 0.0230 0.026 Uiso 1 1 calc R . . C15 C 0.5644(4) 0.21292(16) -0.03677(13) 0.0243(8) Uani 1 1 d . . . H15 H 0.4952 0.1820 -0.0311 0.029 Uiso 1 1 calc R . . C16 C 0.6587(4) 0.20557(18) -0.07834(14) 0.0309(9) Uani 1 1 d . . . H16 H 0.6543 0.1693 -0.0999 0.037 Uiso 1 1 calc R . . C17 C 0.7553(4) 0.25093(18) -0.08703(14) 0.0269(8) Uani 1 1 d . . . H17 H 0.8188 0.2460 -0.1146 0.032 Uiso 1 1 calc R . . C18 C 0.7621(3) 0.30562(15) -0.05521(13) 0.0185(7) Uani 1 1 d . . . C19 C 0.8582(4) 0.35380(16) -0.06704(13) 0.0230(7) Uani 1 1 d . . . H19 H 0.9204 0.3486 -0.0950 0.028 Uiso 1 1 calc R . . C20 C 0.8610(3) 0.40770(16) -0.03811(12) 0.0232(7) Uani 1 1 d . . . H20 H 0.9215 0.4413 -0.0469 0.028 Uiso 1 1 calc R . . C21 C 0.6436(4) 0.64417(15) 0.00296(12) 0.0190(7) Uani 1 1 d . . . C22 C 0.6728(3) 0.63025(15) 0.05436(13) 0.0202(7) Uani 1 1 d . . . C23 C 0.6866(4) 0.67607(17) 0.09231(12) 0.0215(7) Uani 1 1 d . . . C24 C 0.6762(4) 0.73826(17) 0.07433(13) 0.0231(8) Uani 1 1 d . . . H24 H 0.6893 0.7710 0.0989 0.028 Uiso 1 1 calc R . . C25 C 0.6483(4) 0.75660(16) 0.02333(13) 0.0241(8) Uani 1 1 d . . . C26 C 0.6295(4) 0.70671(16) -0.01127(12) 0.0208(7) Uani 1 1 d . . . C27 C 0.7216(4) 0.66091(18) 0.14851(13) 0.0261(8) Uani 1 1 d . . . C28 C 0.8699(4) 0.63637(18) 0.15274(13) 0.0307(8) Uani 1 1 d . . . H28A H 0.8809 0.5990 0.1308 0.046 Uiso 1 1 calc R . . H28B H 0.8896 0.6251 0.1887 0.046 Uiso 1 1 calc R . . H28C H 0.9339 0.6694 0.1414 0.046 Uiso 1 1 calc R . . C29 C 0.6196(5) 0.6103(2) 0.16937(14) 0.0425(11) Uani 1 1 d . . . H29A H 0.5256 0.6216 0.1593 0.064 Uiso 1 1 calc R . . H29B H 0.6259 0.6084 0.2072 0.064 Uiso 1 1 calc R . . H29C H 0.6431 0.5689 0.1548 0.064 Uiso 1 1 calc R . . C30 C 0.7051(4) 0.71922(18) 0.18363(14) 0.0323(9) Uani 1 1 d . . . H30A H 0.7745 0.7509 0.1745 0.048 Uiso 1 1 calc R . . H30B H 0.7172 0.7067 0.2198 0.048 Uiso 1 1 calc R . . H30C H 0.6130 0.7372 0.1789 0.048 Uiso 1 1 calc R . . C31 C 0.6391(4) 0.82639(16) 0.00747(13) 0.0268(8) Uani 1 1 d . . . C32 C 0.6748(5) 0.87015(18) 0.05178(17) 0.0476(12) Uani 1 1 d . . . H32A H 0.6763 0.9139 0.0394 0.071 Uiso 1 1 calc R . . H32B H 0.7655 0.8590 0.0655 0.071 Uiso 1 1 calc R . . H32C H 0.6056 0.8659 0.0791 0.071 Uiso 1 1 calc R . . C33 C 0.7408(5) 0.84071(19) -0.03625(17) 0.0421(11) Uani 1 1 d . . . H33A H 0.7420 0.8863 -0.0430 0.063 Uiso 1 1 calc R . . H33B H 0.7125 0.8182 -0.0676 0.063 Uiso 1 1 calc R . . H33C H 0.8331 0.8268 -0.0261 0.063 Uiso 1 1 calc R . . C34] C 0.4940(4) 0.84188(19) -0.00961(17) 0.0396(10) Uani 1 1 d . . . H34A H 0.4298 0.8330 0.0187 0.059 Uiso 1 1 calc R . . H34B H 0.4698 0.8160 -0.0397 0.059 Uiso 1 1 calc R . . H34C H 0.4883 0.8867 -0.0189 0.059 Uiso 1 1 calc R . . C35 C 0.6987(4) 0.72298(16) -0.17728(12) 0.0194(7) Uani 1 1 d . . . C36 C 0.7837(4) 0.77482(18) -0.16863(13) 0.0252(8) Uani 1 1 d . . . H36 H 0.8506 0.7743 -0.1418 0.030 Uiso 1 1 calc R . . C37 C 0.7682(4) 0.82605(18) -0.19953(14) 0.0287(8) Uani 1 1 d . . . H37 H 0.8251 0.8620 -0.1942 0.034 Uiso 1 1 calc R . . C38 C 0.6694(4) 0.82707(16) -0.23934(13) 0.0237(8) Uani 1 1 d . . . C39 C 0.6497(4) 0.88189(17) -0.27013(14) 0.0306(9) Uani 1 1 d . . . H39 H 0.7073 0.9176 -0.2649 0.037 Uiso 1 1 calc R . . C40 C 0.5526(4) 0.88423(18) -0.30596(15) 0.0310(9) Uani 1 1 d . . . H40 H 0.5412 0.9217 -0.3257 0.037 Uiso 1 1 calc R . . C41 C 0.4655(4) 0.83189(18) -0.31545(13) 0.0285(8) Uani 1 1 d . . . H41 H 0.3956 0.8344 -0.3411 0.034 Uiso 1 1 calc R . . C42 C 0.4829(4) 0.77721(17) -0.28723(13) 0.0249(8) Uani 1 1 d . . . H42 H 0.4259 0.7417 -0.2940 0.030 Uiso 1 1 calc R . . C43 C 0.5849(3) 0.77337(16) -0.24820(12) 0.0197(7) Uani 1 1 d . . . C44 C 0.6028(3) 0.71859(15) -0.21594(12) 0.0187(7) Uani 1 1 d . . . C45 C 0.4426(3) 0.64118(15) -0.17904(12) 0.0158(7) Uani 1 1 d . . . C46 C 0.5160(3) 0.66170(15) -0.22110(12) 0.0160(7) Uani 1 1 d . . . C47 C 0.5065(3) 0.62522(16) -0.26776(12) 0.0179(7) Uani 1 1 d . . . C48 C 0.5903(4) 0.63622(16) -0.31129(12) 0.0215(7) Uani 1 1 d . . . H48 H 0.6532 0.6706 -0.3107 0.026 Uiso 1 1 calc R . . C49 C 0.5837(4) 0.59913(17) -0.35400(13) 0.0250(8) Uani 1 1 d . . . H49 H 0.6417 0.6078 -0.3827 0.030 Uiso 1 1 calc R . . C50 C 0.4914(4) 0.54777(18) -0.35611(14) 0.0272(8) Uani 1 1 d . . . H50 H 0.4867 0.5220 -0.3861 0.033 Uiso 1 1 calc R . . C51 C 0.4087(4) 0.53551(16) -0.31451(13) 0.0237(8) Uani 1 1 d . . . H51 H 0.3460 0.5011 -0.3161 0.028 Uiso 1 1 calc R . . C52 C 0.4144(3) 0.57295(17) -0.26898(12) 0.0178(6) Uani 1 1 d . . . C53 C 0.3335(4) 0.55881(16) -0.22540(13) 0.0233(8) Uani 1 1 d . . . H53 H 0.2665 0.5262 -0.2275 0.028 Uiso 1 1 calc R . . C54 C 0.3496(3) 0.59097(15) -0.18038(12) 0.0195(7) Uani 1 1 d . . . H54 H 0.2987 0.5795 -0.1505 0.023 Uiso 1 1 calc R . . O1 O 0.5270(2) 0.47789(10) 0.03606(8) 0.0181(5) Uani 1 1 d . . . O2 O 0.7825(2) 0.46994(10) 0.03240(9) 0.0184(5) Uani 1 1 d . . . O3 O 0.6900(2) 0.56604(11) 0.06753(8) 0.0225(5) Uani 1 1 d . . . O4 O 0.5961(3) 0.71985(10) -0.06347(8) 0.0227(5) Uani 1 1 d . . . O5 O 0.7131(2) 0.67144(11) -0.14240(9) 0.0211(5) Uani 1 1 d . . . O6 O 0.4581(2) 0.67367(11) -0.13162(8) 0.0178(5) Uani 1 1 d . . . P1 P 0.65920(9) 0.51778(4) 0.02167(3) 0.01775(18) Uani 1 1 d . . . P2 P 0.59711(9) 0.65959(4) -0.10049(3) 0.01837(19) Uani 1 1 d . . . Cl1 Cl 0.59774(9) 0.49285(4) -0.10871(3) 0.0269(2) Uani 1 1 d . . . Cl2 Cl 0.35254(11) 0.36573(5) 0.95605(4) 0.0413(2) Uani 1 1 d . . . Cl3 Cl 0.19495(10) 0.45849(5) 1.01223(4) 0.0352(2) Uani 1 1 d . . . Cl4 Cl 0.18767(10) 0.45611(5) 0.90029(4) 0.0311(2) Uani 1 1 d . . . Cl5 Cl 0.9781(9) 0.5779(5) 0.8135(3) 0.109(3) Uani 0.394(16) 1 d P B 1 Cl6 Cl 0.8196(16) 0.5408(7) 0.7508(4) 0.153(6) Uani 0.394(16) 1 d P B 1 Cl7 Cl 0.9824(11) 0.4470(5) 0.7998(4) 0.056(2) Uani 0.394(16) 1 d P B 1 Cl5' Cl 0.9665(6) 0.5682(3) 0.8409(6) 0.150(4) Uani 0.606(16) 1 d P B 2 Cl6' Cl 0.7807(7) 0.5278(4) 0.7511(2) 0.113(2) Uani 0.606(16) 1 d P B 2 Cl7' Cl 0.9507(11) 0.4412(4) 0.8047(3) 0.085(3) Uani 0.606(16) 1 d P B 2 Pd1 Pd 0.62676(2) 0.575164(12) -0.049650(9) 0.01660(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1S 0.0255(17) 0.028(2) 0.0296(19) 0.0043(17) -0.0034(16) -0.0035(14) C1 0.0244(16) 0.0186(18) 0.0144(15) 0.0043(14) -0.0038(12) -0.0008(15) C2 0.0231(17) 0.0243(19) 0.0202(17) -0.0029(14) 0.0015(14) 0.0015(14) C2S 0.041(2) 0.076(3) 0.046(3) -0.009(2) 0.000(2) 0.011(3) C3 0.0312(19) 0.028(2) 0.0163(17) -0.0034(15) -0.0006(14) 0.0041(16) C4 0.0262(18) 0.027(2) 0.0185(17) 0.0045(15) -0.0023(14) -0.0060(16) C5 0.039(2) 0.037(2) 0.0165(17) 0.0069(16) 0.0011(16) -0.0079(19) C6 0.036(2) 0.036(2) 0.0194(18) 0.0125(16) -0.0053(16) -0.0059(18) C7 0.035(2) 0.0210(19) 0.0293(19) 0.0049(15) -0.0070(16) -0.0015(16) C8 0.0252(18) 0.0221(18) 0.0193(16) 0.0020(14) -0.0022(14) -0.0010(15) C9 0.0185(16) 0.0151(16) 0.0145(15) 0.0001(13) -0.0013(13) -0.0041(13) C10 0.0192(16) 0.0165(16) 0.0158(15) 0.0008(13) -0.0022(12) -0.0009(13) C11 0.0168(15) 0.0204(19) 0.0164(15) 0.0020(13) -0.0044(12) 0.0006(13) C12 0.0180(15) 0.0179(17) 0.0142(15) 0.0040(13) -0.0019(13) 0.0015(13) C13 0.0200(17) 0.0139(16) 0.0198(16) -0.0011(13) -0.0052(13) 0.0017(13) C14 0.0265(18) 0.0201(19) 0.0179(16) 0.0055(14) -0.0029(14) 0.0023(14) C15 0.0307(19) 0.0133(17) 0.029(2) 0.0008(14) -0.0047(15) -0.0031(14) C16 0.047(3) 0.0213(19) 0.0249(19) -0.0048(15) -0.0074(18) 0.0035(18) C17 0.0287(19) 0.029(2) 0.0231(18) 0.0001(16) -0.0004(15) 0.0085(17) C18 0.0234(16) 0.0156(16) 0.0165(16) 0.0033(14) -0.0059(14) 0.0009(13) C19 0.0208(17) 0.0257(18) 0.0227(16) 0.0047(14) 0.0023(14) 0.0068(15) C20 0.0171(15) 0.0256(19) 0.0270(18) 0.0075(13) -0.0023(14) 0.0003(14) C21 0.0257(18) 0.0167(16) 0.0146(14) -0.0033(13) -0.0040(14) -0.0008(15) C22 0.0249(16) 0.0158(16) 0.0199(16) 0.0012(14) -0.0045(15) -0.0011(13) C23 0.0303(18) 0.0210(18) 0.0133(15) -0.0027(14) -0.0060(14) 0.0012(15) C24 0.0272(19) 0.024(2) 0.0186(16) -0.0065(15) -0.0063(14) -0.0020(15) C25 0.030(2) 0.0184(18) 0.0238(17) -0.0036(14) -0.0058(16) 0.0002(16) C26 0.0271(17) 0.0212(17) 0.0141(15) 0.0003(13) -0.0032(15) 0.0000(16) C27 0.035(2) 0.026(2) 0.0168(17) -0.0031(15) -0.0031(15) -0.0038(16) C28 0.035(2) 0.036(2) 0.0212(16) -0.0017(15) -0.0128(17) 0.0047(19) C29 0.063(3) 0.043(2) 0.0220(18) 0.0007(17) 0.010(2) -0.016(2) C30 0.048(2) 0.031(2) 0.0181(18) -0.0035(16) -0.0097(17) -0.0092(19) C31 0.043(2) 0.0145(17) 0.0229(17) -0.0016(14) -0.0119(17) -0.0002(17) C32 0.086(3) 0.0189(19) 0.038(2) -0.0067(19) -0.026(3) 0.002(2) C33 0.057(3) 0.020(2) 0.049(3) 0.0043(19) -0.003(2) -0.0084(19) C34] 0.046(3) 0.026(2) 0.047(3) -0.001(2) -0.014(2) 0.0061(19) C35 0.0216(17) 0.0199(18) 0.0169(16) 0.0020(14) -0.0015(14) 0.0007(14) C36 0.0270(19) 0.030(2) 0.0184(17) 0.0006(16) -0.0030(14) -0.0080(16) C37 0.036(2) 0.023(2) 0.0270(19) -0.0010(16) 0.0055(16) -0.0103(16) C38 0.033(2) 0.0187(18) 0.0200(16) -0.0009(14) 0.0047(15) -0.0030(15) C39 0.049(2) 0.0152(17) 0.0279(19) 0.0021(15) 0.0095(18) -0.0032(17) C40 0.046(2) 0.0185(19) 0.028(2) 0.0109(16) 0.0021(18) 0.0069(18) C41 0.039(2) 0.029(2) 0.0170(17) 0.0044(16) -0.0033(16) 0.0061(18) C42 0.0312(19) 0.0214(19) 0.0222(18) 0.0055(15) -0.0023(15) 0.0000(16) C43 0.0254(18) 0.0169(17) 0.0169(16) 0.0004(14) 0.0048(13) 0.0016(14) C44 0.0256(18) 0.0150(16) 0.0156(15) 0.0010(13) 0.0034(13) 0.0004(14) C45 0.0191(16) 0.0158(16) 0.0126(15) -0.0036(13) -0.0023(12) 0.0027(13) C46 0.0191(16) 0.0128(16) 0.0160(15) 0.0020(13) -0.0035(13) 0.0001(13) C47 0.0197(16) 0.0190(18) 0.0151(16) -0.0001(13) -0.0034(13) 0.0028(14) C48 0.0268(18) 0.0209(18) 0.0168(15) -0.0012(14) -0.0027(13) -0.0023(14) C49 0.0273(19) 0.030(2) 0.0175(16) -0.0032(15) 0.0057(14) 0.0014(15) C50 0.036(2) 0.0251(19) 0.0205(18) -0.0081(16) -0.0037(15) 0.0044(17) C51 0.0294(19) 0.0198(18) 0.0218(17) -0.0023(14) -0.0054(14) -0.0025(15) C52 0.0186(15) 0.0176(16) 0.0172(15) -0.0006(14) -0.0016(12) 0.0036(15) C53 0.0258(18) 0.0204(19) 0.0236(17) -0.0001(14) -0.0049(14) -0.0031(14) C54 0.0210(17) 0.0216(18) 0.0159(15) 0.0011(13) 0.0016(13) -0.0016(13) O1 0.0223(11) 0.0137(12) 0.0184(12) 0.0037(9) -0.0019(9) 0.0013(9) O2 0.0187(11) 0.0140(12) 0.0226(12) 0.0024(9) -0.0061(9) -0.0036(9) O3 0.0359(13) 0.0158(13) 0.0158(11) 0.0022(9) -0.0065(10) -0.0037(11) O4 0.0377(14) 0.0147(12) 0.0159(11) 0.0005(9) -0.0075(10) 0.0012(10) O5 0.0224(12) 0.0226(13) 0.0182(12) 0.0053(10) -0.0019(10) 0.0007(10) O6 0.0242(12) 0.0184(12) 0.0107(10) -0.0007(9) 0.0003(9) -0.0011(10) P1 0.0225(5) 0.0149(4) 0.0158(4) 0.0007(3) -0.0040(3) -0.0017(3) P2 0.0255(5) 0.0166(4) 0.0130(4) -0.0004(3) -0.0028(3) -0.0013(4) Cl1 0.0358(5) 0.0222(4) 0.0226(4) -0.0079(4) -0.0035(4) -0.0031(4) Cl2 0.0442(6) 0.0320(5) 0.0475(6) 0.0002(5) -0.0073(5) 0.0092(4) Cl3 0.0343(5) 0.0431(6) 0.0281(5) -0.0027(4) 0.0006(4) -0.0026(5) Cl4 0.0291(5) 0.0377(5) 0.0265(5) 0.0040(4) -0.0023(4) 0.0004(4) Cl5 0.082(4) 0.138(6) 0.109(5) 0.007(5) 0.048(4) -0.002(4) Cl6 0.196(10) 0.166(8) 0.097(6) 0.095(6) 0.078(7) 0.103(7) Cl7 0.044(3) 0.063(4) 0.062(4) -0.033(3) -0.025(2) 0.018(2) Cl5' 0.062(3) 0.080(3) 0.308(11) -0.101(5) -0.079(4) 0.035(2) Cl6' 0.107(3) 0.172(5) 0.060(3) -0.021(3) -0.038(3) 0.103(3) Cl7' 0.110(6) 0.098(4) 0.047(2) 0.002(2) -0.040(3) 0.033(4) Pd1 0.02355(12) 0.01368(11) 0.01257(10) -0.00060(10) -0.00329(10) -0.00182(11) _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 C1S Cl2 1.747(4) . ? C1S Cl3 1.760(4) . ? C1S Cl4 1.759(4) . ? C1S H1S 1.0000 . ? C1 C10 1.372(5) . ? C1 C2 1.398(5) . ? C1 O1 1.420(4) . ? C2 C3 1.366(5) . ? C2 H2 0.9500 . ? C2S Cl6 1.660(10) . ? C2S Cl7' 1.718(9) . ? C2S Cl6' 1.729(6) . ? C2S Cl5' 1.730(7) . ? C2S Cl5 1.740(11) . ? C2S Cl7 1.792(11) . ? C2S H2S 1.0000 . ? C3 C4 1.416(5) . ? C3 H3 0.9500 . ? C4 C5 1.421(5) . ? C4 C9 1.432(5) . ? C5 C6 1.344(5) . ? C5 H5 0.9500 . ? C6 C7 1.403(5) . ? C6 H6 0.9500 . ? C7 C8 1.377(5) . ? C7 H7 0.9500 . ? C8 C9 1.408(5) . ? C8 H8 0.9500 . ? C9 C10 1.436(4) . ? C10 C12 1.505(4) . ? C11 C12 1.375(5) . ? C11 C20 1.393(5) . ? C11 O2 1.411(4) . ? C12 C13 1.432(5) . ? C13 C14 1.407(5) . ? C13 C18 1.415(5) . ? C14 C15 1.370(5) . ? C14 H14 0.9500 . ? C15 C16 1.422(5) . ? C15 H15 0.9500 . ? C16 C17 1.362(5) . ? C16 H16 0.9500 . ? C17 C18 1.422(5) . ? C17 H17 0.9500 . ? C18 C19 1.416(5) . ? C19 C20 1.365(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.381(4) . ? C21 C22 1.391(4) . ? C21 Pd1 2.003(3) . ? C22 C23 1.386(5) . ? C22 O3 1.411(4) . ? C23 C24 1.400(5) . ? C23 C27 1.527(5) . ? C24 C25 1.402(5) . ? C24 H24 0.9500 . ? C25 C26 1.396(5) . ? C25 C31 1.536(5) . ? C26 O4 1.416(4) . ? C27 C28 1.537(5) . ? C27 C30 1.541(5) . ? C27 C29 1.556(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.514(5) . ? C31 C34] 1.515(6) . ? C31 C33 1.532(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34] H34A 0.9800 . ? C34] H34B 0.9800 . ? C34] H34C 0.9800 . ? C35 C44 1.370(5) . ? C35 C36 1.392(5) . ? C35 O5 1.422(4) . ? C36 C37 1.355(5) . ? C36 H36 0.9500 . ? C37 C38 1.408(5) . ? C37 H37 0.9500 . ? C38 C43 1.421(5) . ? C38 C39 1.420(5) . ? C39 C40 1.324(5) . ? C39 H39 0.9500 . ? C40 C41 1.416(5) . ? C40 H40 0.9500 . ? C41 C42 1.379(5) . ? C41 H41 0.9500 . ? C42 C43 1.417(5) . ? C42 H42 0.9500 . ? C43 C44 1.439(4) . ? C44 C46 1.476(4) . ? C45 C46 1.372(4) . ? C45 C54 1.396(4) . ? C45 O6 1.414(4) . ? C46 C47 1.436(4) . ? C47 C48 1.409(4) . ? C47 C52 1.424(5) . ? C48 C49 1.357(5) . ? C48 H48 0.9500 . ? C49 C50 1.411(5) . ? C49 H49 0.9500 . ? C50 C51 1.368(5) . ? C50 H50 0.9500 . ? C51 C52 1.421(4) . ? C51 H51 0.9500 . ? C52 C53 1.407(4) . ? C53 C54 1.358(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? O1 P1 1.582(2) . ? O2 P1 1.594(2) . ? O3 P1 1.594(2) . ? O4 P2 1.595(2) . ? O5 P2 1.584(2) . ? O6 P2 1.601(2) . ? P1 Pd1 2.2309(9) . ? P2 Pd1 2.2372(10) . ? Cl1 Pd1 2.3342(9) . ? Cl5 Cl6 2.37(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 Cl2 C1S Cl3 110.6(2) . . ? Cl2 C1S Cl4 110.6(2) . . ? Cl3 C1S Cl4 110.83(19) . . ? Cl2 C1S H1S 108.2 . . ? Cl3 C1S H1S 108.2 . . ? Cl4 C1S H1S 108.2 . . ? C10 C1 C2 124.8(3) . . ? C10 C1 O1 119.7(3) . . ? C2 C1 O1 115.4(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? Cl6 C2S Cl7' 113.9(6) . . ? Cl6 C2S Cl6' 15.7(7) . . ? Cl7' C2S Cl6' 110.4(4) . . ? Cl6 C2S Cl5' 111.0(10) . . ? Cl7' C2S Cl5' 111.6(4) . . ? Cl6' C2S Cl5' 124.7(7) . . ? Cl6 C2S Cl5 88.3(8) . . ? Cl7' C2S Cl5 114.9(5) . . ? Cl6' C2S Cl5 103.3(6) . . ? Cl5' C2S Cl5 24.9(5) . . ? Cl6 C2S Cl7 110.5(6) . . ? Cl7' C2S Cl7 11.4(7) . . ? Cl6' C2S Cl7 110.3(5) . . ? Cl5' C2S Cl7 104.3(4) . . ? Cl5 C2S Cl7 104.5(5) . . ? Cl6 C2S H2S 116.6 . . ? Cl7' C2S H2S 106.3 . . ? Cl6' C2S H2S 104.8 . . ? Cl5' C2S H2S 96.1 . . ? Cl5 C2S H2S 116.6 . . ? Cl7 C2S H2S 116.6 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 C9 120.5(3) . . ? C5 C4 C9 119.1(3) . . ? C6 C5 C4 121.2(4) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C4 117.9(3) . . ? C8 C9 C10 123.3(3) . . ? C4 C9 C10 118.7(3) . . ? C1 C10 C9 117.0(3) . . ? C1 C10 C12 120.5(3) . . ? C9 C10 C12 122.4(3) . . ? C12 C11 C20 124.0(3) . . ? C12 C11 O2 120.1(3) . . ? C20 C11 O2 115.8(3) . . ? C11 C12 C13 117.4(3) . . ? C11 C12 C10 119.7(3) . . ? C13 C12 C10 122.9(3) . . ? C14 C13 C18 118.0(3) . . ? C14 C13 C12 123.2(3) . . ? C18 C13 C12 118.8(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C13 120.7(3) . . ? C19 C18 C17 119.5(3) . . ? C13 C18 C17 119.8(3) . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C11 119.1(3) . . ? C19 C20 H20 120.5 . . ? C11 C20 H20 120.5 . . ? C26 C21 C22 118.6(3) . . ? C26 C21 Pd1 120.7(2) . . ? C22 C21 Pd1 120.8(2) . . ? C23 C22 C21 123.3(3) . . ? C23 C22 O3 119.4(3) . . ? C21 C22 O3 117.3(3) . . ? C22 C23 C24 114.6(3) . . ? C22 C23 C27 123.3(3) . . ? C24 C23 C27 122.0(3) . . ? C23 C24 C25 125.9(3) . . ? C23 C24 H24 117.0 . . ? C25 C24 H24 117.0 . . ? C26 C25 C24 114.8(3) . . ? C26 C25 C31 123.3(3) . . ? C24 C25 C31 121.9(3) . . ? C21 C26 C25 122.8(3) . . ? C21 C26 O4 117.7(3) . . ? C25 C26 O4 119.5(3) . . ? C23 C27 C28 110.3(3) . . ? C23 C27 C30 111.7(3) . . ? C28 C27 C30 109.0(3) . . ? C23 C27 C29 109.5(3) . . ? C28 C27 C29 109.9(3) . . ? C30 C27 C29 106.3(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C34] 107.6(3) . . ? C32 C31 C33 106.9(3) . . ? C34] C31 C33 110.1(3) . . ? C32 C31 C25 111.9(3) . . ? C34] C31 C25 109.9(3) . . ? C33 C31 C25 110.5(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34] H34A 109.5 . . ? C31 C34] H34B 109.5 . . ? H34A C34] H34B 109.5 . . ? C31 C34] H34C 109.5 . . ? H34A C34] H34C 109.5 . . ? H34B C34] H34C 109.5 . . ? C44 C35 C36 125.1(3) . . ? C44 C35 O5 118.5(3) . . ? C36 C35 O5 116.4(3) . . ? C37 C36 C35 118.0(3) . . ? C37 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C36 C37 C38 121.3(3) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C43 120.0(3) . . ? C37 C38 C39 121.0(3) . . ? C43 C38 C39 119.0(3) . . ? C40 C39 C38 121.3(4) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 121.2(3) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 119.4(3) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 120.7(3) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C38 118.3(3) . . ? C42 C43 C44 122.9(3) . . ? C38 C43 C44 118.7(3) . . ? C35 C44 C43 116.8(3) . . ? C35 C44 C46 120.7(3) . . ? C43 C44 C46 122.4(3) . . ? C46 C45 C54 123.9(3) . . ? C46 C45 O6 118.6(3) . . ? C54 C45 O6 117.5(3) . . ? C45 C46 C47 117.6(3) . . ? C45 C46 C44 118.9(3) . . ? C47 C46 C44 123.5(3) . . ? C48 C47 C52 118.3(3) . . ? C48 C47 C46 123.1(3) . . ? C52 C47 C46 118.5(3) . . ? C49 C48 C47 121.8(3) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C48 C49 C50 120.5(3) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 119.3(3) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 121.6(3) . . ? C50 C51 H51 119.2 . . ? C52 C51 H51 119.2 . . ? C53 C52 C51 121.6(3) . . ? C53 C52 C47 119.9(3) . . ? C51 C52 C47 118.4(3) . . ? C54 C53 C52 121.1(3) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C45 118.5(3) . . ? C53 C54 H54 120.7 . . ? C45 C54 H54 120.7 . . ? C1 O1 P1 122.8(2) . . ? C11 O2 P1 114.30(19) . . ? C22 O3 P1 114.54(19) . . ? C26 O4 P2 114.5(2) . . ? C35 O5 P2 119.0(2) . . ? C45 O6 P2 115.8(2) . . ? O1 P1 O3 108.62(13) . . ? O1 P1 O2 103.35(12) . . ? O3 P1 O2 97.83(13) . . ? O1 P1 Pd1 111.74(9) . . ? O3 P1 Pd1 107.04(9) . . ? O2 P1 Pd1 126.61(9) . . ? O5 P2 O4 106.76(13) . . ? O5 P2 O6 103.13(12) . . ? O4 P2 O6 98.52(12) . . ? O5 P2 Pd1 115.92(10) . . ? O4 P2 Pd1 106.65(9) . . ? O6 P2 Pd1 123.57(9) . . ? C2S Cl5 Cl6 44.4(4) . . ? C2S Cl6 Cl5 47.2(5) . . ? C21 Pd1 P1 79.85(10) . . ? C21 Pd1 P2 80.06(10) . . ? P1 Pd1 P2 159.89(3) . . ? C21 Pd1 Cl1 177.16(10) . . ? P1 Pd1 Cl1 98.74(4) . . ? P2 Pd1 Cl1 101.29(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.533 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.077 #END # Attachment '5a_prongssad.cif' data_5a_prongssad _database_code_depnum_ccdc_archive 'CCDC 614136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H27 Cl O6 P2 Pd, 3(C H Cl3)' _chemical_formula_sum 'C49 H30 Cl10 O6 P2 Pd' _chemical_formula_weight 1237.57 _chemical_absolute_configuration ad 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.425(2) _cell_length_b 9.2502(19) _cell_length_c 25.909(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.57(3) _cell_angle_gamma 90.00 _cell_volume 2486.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1383 _cell_measurement_theta_min 2.339 _cell_measurement_theta_max 19.341 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.657985 _exptl_absorpt_correction_T_max 0.950000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17578 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10930 _reflns_number_gt 8341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT V6.28 (Bruker, 2001)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 10930 _refine_ls_number_parameters 608 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 0.16045(5) 0.25146(5) 0.240074(19) 0.01366(12) Uani 1 1 d . . . P1 P 0.12640(18) 0.28377(18) 0.15331(7) 0.0158(4) Uani 1 1 d . . . P2 P 0.11364(16) 0.2366(2) 0.32265(7) 0.0157(4) Uani 1 1 d . . . Cl1 Cl 0.38583(16) 0.2698(2) 0.25408(7) 0.0229(4) Uani 1 1 d . . . O1 O 0.1690(5) 0.4297(5) 0.12547(18) 0.0161(11) Uani 1 1 d . . . O2 O 0.1693(5) 0.1597(5) 0.11637(18) 0.0157(11) Uani 1 1 d . . . O3 O -0.0257(5) 0.2993(5) 0.13967(18) 0.0184(11) Uani 1 1 d . . . O4 O -0.0396(4) 0.2117(5) 0.32197(18) 0.0173(11) Uani 1 1 d . . . O5 O 0.1591(5) 0.1160(5) 0.36401(19) 0.0169(12) Uani 1 1 d . . . O6 O 0.1456(5) 0.3834(5) 0.35355(19) 0.0160(11) Uani 1 1 d . . . C1 C 0.2943(6) 0.4356(8) 0.1094(3) 0.0168(15) Uani 1 1 d U . . C2 C 0.3840(7) 0.5260(7) 0.1366(3) 0.0193(16) Uani 1 1 d . . . H2 H 0.3619 0.5768 0.1654 0.023 Uiso 1 1 calc R . . C3 C 0.5059(8) 0.5398(9) 0.1205(3) 0.0234(18) Uani 1 1 d . . . H3 H 0.5652 0.6032 0.1375 0.028 Uiso 1 1 calc R . . C4 C 0.5401(7) 0.4563(8) 0.0779(3) 0.0216(17) Uani 1 1 d . . . C5 C 0.6675(8) 0.4613(9) 0.0630(3) 0.0270(19) Uani 1 1 d . . . H5 H 0.7267 0.5254 0.0795 0.032 Uiso 1 1 calc R . . C6 C 0.7042(7) 0.3729(9) 0.0248(3) 0.0250(18) Uani 1 1 d . . . H6 H 0.7875 0.3780 0.0149 0.030 Uiso 1 1 calc R . . C7 C 0.6169(7) 0.2762(9) 0.0009(3) 0.0239(18) Uani 1 1 d . . . H7 H 0.6436 0.2148 -0.0244 0.029 Uiso 1 1 calc R . . C8 C 0.4914(6) 0.2673(9) 0.0132(3) 0.0191(15) Uani 1 1 d . . . H8 H 0.4344 0.2012 -0.0035 0.023 Uiso 1 1 calc R . . C9 C 0.4509(7) 0.3607(7) 0.0519(3) 0.0168(15) Uani 1 1 d . . . C10 C 0.3196(7) 0.3573(7) 0.0662(3) 0.0159(15) Uani 1 1 d . . . C11 C 0.1428(7) 0.1757(8) 0.0616(3) 0.0151(15) Uani 1 1 d . . . C12 C 0.2165(6) 0.2739(7) 0.0366(2) 0.0138(14) Uani 1 1 d . . . C13 C 0.1834(7) 0.2925(7) -0.0186(3) 0.0176(16) Uani 1 1 d U . . C14 C 0.2433(7) 0.3943(8) -0.0483(3) 0.0194(16) Uani 1 1 d . . . H14 H 0.3076 0.4530 -0.0322 0.023 Uiso 1 1 calc R . . C15 C 0.2096(7) 0.4096(9) -0.1004(3) 0.0243(18) Uani 1 1 d . . . H15 H 0.2523 0.4764 -0.1194 0.029 Uiso 1 1 calc R . . C16 C 0.1100(8) 0.3238(8) -0.1251(3) 0.0252(18) Uani 1 1 d . . . H16 H 0.0869 0.3344 -0.1605 0.030 Uiso 1 1 calc R . . C17 C 0.0477(7) 0.2260(8) -0.0976(3) 0.0198(17) Uani 1 1 d . . . H17 H -0.0183 0.1706 -0.1142 0.024 Uiso 1 1 calc R . . C18 C 0.0817(7) 0.2070(7) -0.0437(3) 0.0168(16) Uani 1 1 d . . . C19 C 0.0131(7) 0.1094(8) -0.0141(3) 0.0207(16) Uani 1 1 d . . . H19 H -0.0535 0.0548 -0.0307 0.025 Uiso 1 1 calc R . . C20 C 0.0421(7) 0.0937(8) 0.0377(3) 0.0197(16) Uani 1 1 d . . . H20 H -0.0039 0.0301 0.0567 0.024 Uiso 1 1 calc R . . C21 C -0.0292(6) 0.2503(9) 0.2307(3) 0.0188(10) Uani 1 1 d . . . C22 C -0.0962(7) 0.2732(8) 0.1825(3) 0.0185(16) Uani 1 1 d . . . C23 C -0.2289(7) 0.2791(8) 0.1748(3) 0.0229(18) Uani 1 1 d . . . H23 H -0.2712 0.2938 0.1420 0.027 Uiso 1 1 calc R . . C24 C -0.2981(6) 0.2618(8) 0.2187(3) 0.0188(10) Uani 1 1 d . . . H24 H -0.3875 0.2689 0.2146 0.023 Uiso 1 1 calc R . . C25 C -0.2378(7) 0.2350(9) 0.2667(3) 0.0228(17) Uani 1 1 d . . . H25 H -0.2846 0.2198 0.2951 0.027 Uiso 1 1 calc R . . C26 C -0.1046(7) 0.2312(8) 0.2719(3) 0.0199(16) Uani 1 1 d . . . C27 C 0.2866(7) 0.1295(8) 0.3872(3) 0.0187(16) Uani 1 1 d . . . C28 C 0.3765(7) 0.0376(8) 0.3677(3) 0.0193(16) Uani 1 1 d . . . H28 H 0.3528 -0.0272 0.3410 0.023 Uiso 1 1 calc R . . C29 C 0.5013(8) 0.0471(8) 0.3895(3) 0.0221(18) Uani 1 1 d . . . H29 H 0.5623 -0.0163 0.3786 0.027 Uiso 1 1 calc R . . C30 C 0.5405(7) 0.1502(7) 0.4283(3) 0.0152(15) Uani 1 1 d . . . C31 C 0.6697(7) 0.1645(8) 0.4486(3) 0.0237(18) Uani 1 1 d . . . H31 H 0.7309 0.1021 0.4371 0.028 Uiso 1 1 calc R . . C32 C 0.7079(7) 0.2650(10) 0.4841(3) 0.0262(17) Uani 1 1 d . . . H32 H 0.7937 0.2701 0.4977 0.031 Uiso 1 1 calc R . . C33 C 0.6156(7) 0.3641(8) 0.5006(3) 0.0218(17) Uani 1 1 d . . . H33 H 0.6419 0.4369 0.5240 0.026 Uiso 1 1 calc R . . C34 C 0.4898(7) 0.3530(8) 0.4825(3) 0.0160(15) Uani 1 1 d . . . H34 H 0.4307 0.4174 0.4942 0.019 Uiso 1 1 calc R . . C35 C 0.4464(6) 0.2457(9) 0.4461(2) 0.0166(13) Uani 1 1 d . . . C36 C 0.3126(6) 0.2296(7) 0.4261(2) 0.0116(14) Uani 1 1 d . . . C37 C 0.1263(7) 0.3936(7) 0.4067(3) 0.0181(16) Uani 1 1 d . . . C38 C 0.2084(7) 0.3216(7) 0.4431(3) 0.0171(16) Uani 1 1 d . . . C39 C 0.1807(7) 0.3335(8) 0.4962(3) 0.0181(16) Uani 1 1 d . . . C40 C 0.2509(6) 0.2591(9) 0.5374(2) 0.0197(15) Uani 1 1 d . . . H40 H 0.3181 0.1984 0.5303 0.024 Uiso 1 1 calc R . . C41 C 0.2219(7) 0.2745(8) 0.5880(3) 0.0229(17) Uani 1 1 d . . . H41 H 0.2697 0.2247 0.6145 0.027 Uiso 1 1 calc R . . C42 C 0.1199(7) 0.3655(8) 0.5998(3) 0.0228(17) Uani 1 1 d . . . H42 H 0.1025 0.3781 0.6340 0.027 Uiso 1 1 calc R . . C43 C 0.0465(7) 0.4353(9) 0.5607(3) 0.0235(17) Uani 1 1 d . . . H43 H -0.0227 0.4921 0.5684 0.028 Uiso 1 1 calc R . . C44 C 0.0753(7) 0.4216(8) 0.5087(3) 0.0170(15) Uani 1 1 d . . . C45 C -0.0003(7) 0.4961(8) 0.4687(3) 0.0209(17) Uani 1 1 d . . . H45 H -0.0660 0.5575 0.4768 0.025 Uiso 1 1 calc R . . C46 C 0.0230(7) 0.4780(8) 0.4187(3) 0.0224(17) Uani 1 1 d . . . H46 H -0.0301 0.5219 0.3923 0.027 Uiso 1 1 calc R . . C47 C 0.0314(9) 0.6972(8) 0.2820(3) 0.031(2) Uani 1 1 d . . . H47 H 0.0759 0.6834 0.3167 0.038 Uiso 1 1 calc R . . Cl2 Cl 0.1212(3) 0.6148(3) 0.23568(12) 0.0606(8) Uani 1 1 d . . . Cl3 Cl -0.1217(2) 0.6203(2) 0.27937(9) 0.0396(5) Uani 1 1 d . . . Cl4 Cl 0.0201(3) 0.8853(2) 0.26787(9) 0.0467(7) Uani 1 1 d . . . C48 C 0.4561(8) 0.5460(8) 0.3390(3) 0.0288(19) Uani 1 1 d . . . H48 H 0.3946 0.4742 0.3237 0.035 Uiso 1 1 calc R . . Cl5 Cl 0.6019(2) 0.4586(2) 0.36136(8) 0.0344(5) Uani 1 1 d . . . Cl6 Cl 0.3909(2) 0.6321(2) 0.39143(9) 0.0379(5) Uani 1 1 d . . . Cl7 Cl 0.4854(3) 0.6751(3) 0.29175(9) 0.0508(7) Uani 1 1 d . . . C49 C 0.4404(8) 0.9802(9) 0.1744(3) 0.031(2) Uani 1 1 d . . . H49 H 0.4383 1.0810 0.1860 0.037 Uiso 1 1 calc R . . Cl8 Cl 0.5789(2) 0.8995(2) 0.20482(8) 0.0393(6) Uani 1 1 d . . . Cl9 Cl 0.3002(2) 0.8931(2) 0.19186(10) 0.0432(6) Uani 1 1 d . . . Cl10 Cl 0.4420(3) 0.9796(3) 0.10711(10) 0.0596(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0127(2) 0.0140(2) 0.0148(2) -0.0002(3) 0.00376(18) 0.0003(3) P1 0.0163(9) 0.0158(11) 0.0157(9) 0.0015(7) 0.0040(7) 0.0005(7) P2 0.0157(9) 0.0142(9) 0.0174(9) -0.0009(8) 0.0035(7) -0.0011(9) Cl1 0.0147(8) 0.0271(11) 0.0275(9) -0.0058(9) 0.0048(7) 0.0000(8) O1 0.017(3) 0.014(2) 0.019(3) 0.002(2) 0.009(2) 0.002(2) O2 0.019(3) 0.015(3) 0.013(3) 0.000(2) 0.002(2) -0.003(2) O3 0.013(3) 0.023(3) 0.019(3) 0.001(2) 0.005(2) 0.001(2) O4 0.015(3) 0.020(3) 0.017(3) -0.0010(19) 0.003(2) 0.0021(19) O5 0.028(3) 0.007(2) 0.015(3) 0.000(2) 0.002(2) 0.000(2) O6 0.014(3) 0.017(3) 0.016(3) -0.001(2) 0.002(2) -0.002(2) C1 0.009(4) 0.022(4) 0.020(4) 0.012(3) 0.002(3) 0.003(3) C2 0.030(5) 0.013(4) 0.015(4) -0.005(3) -0.003(3) 0.000(3) C3 0.022(4) 0.025(4) 0.022(4) 0.007(3) -0.003(3) -0.007(3) C4 0.018(4) 0.017(4) 0.030(5) 0.015(3) -0.002(3) -0.001(3) C5 0.021(4) 0.030(5) 0.028(5) 0.012(4) -0.004(3) -0.008(4) C6 0.015(4) 0.033(5) 0.027(5) 0.007(4) 0.004(3) -0.001(3) C7 0.023(4) 0.026(5) 0.024(4) 0.000(3) 0.012(3) 0.008(4) C8 0.018(3) 0.019(4) 0.020(4) 0.006(3) 0.004(3) -0.004(4) C9 0.016(4) 0.016(4) 0.018(4) 0.009(3) -0.001(3) 0.005(3) C10 0.015(4) 0.019(4) 0.012(4) -0.001(3) -0.005(3) -0.004(3) C11 0.013(4) 0.023(4) 0.010(4) -0.001(3) 0.005(3) 0.003(3) C12 0.017(3) 0.007(4) 0.018(3) -0.002(3) 0.002(3) 0.000(3) C13 0.022(4) 0.016(4) 0.017(4) -0.005(3) 0.008(3) 0.007(3) C14 0.019(4) 0.021(4) 0.019(4) -0.004(3) 0.005(3) 0.001(3) C15 0.024(4) 0.029(5) 0.020(4) 0.003(3) 0.002(3) 0.003(3) C16 0.032(5) 0.029(4) 0.015(4) 0.003(3) 0.001(3) 0.011(4) C17 0.023(4) 0.016(4) 0.020(4) -0.003(3) -0.001(3) 0.000(3) C18 0.012(4) 0.023(4) 0.016(4) -0.004(3) 0.001(3) 0.003(3) C19 0.012(4) 0.024(4) 0.026(4) -0.006(3) 0.003(3) -0.006(3) C20 0.014(4) 0.027(4) 0.019(4) 0.003(3) 0.006(3) 0.001(3) C21 0.014(2) 0.013(2) 0.029(3) -0.003(3) 0.0006(19) 0.001(3) C22 0.023(4) 0.014(4) 0.018(4) 0.002(3) 0.006(3) 0.002(3) C23 0.017(4) 0.028(5) 0.021(4) 0.003(3) -0.007(3) 0.005(3) C24 0.014(2) 0.013(2) 0.029(3) -0.003(3) 0.0006(19) 0.001(3) C25 0.027(4) 0.015(4) 0.029(4) -0.003(4) 0.014(3) -0.006(4) C26 0.024(4) 0.018(4) 0.018(4) 0.005(3) 0.001(3) 0.002(3) C27 0.018(4) 0.014(4) 0.025(4) 0.003(3) 0.007(3) -0.001(3) C28 0.022(4) 0.018(4) 0.018(4) -0.001(3) 0.005(3) -0.006(3) C29 0.028(5) 0.013(4) 0.027(5) 0.005(3) 0.012(4) 0.008(3) C30 0.017(4) 0.016(4) 0.014(4) 0.006(3) 0.006(3) 0.003(3) C31 0.019(4) 0.022(4) 0.031(5) 0.008(3) 0.008(3) 0.014(3) C32 0.018(4) 0.030(5) 0.032(4) 0.002(4) 0.006(3) -0.012(4) C33 0.026(5) 0.020(4) 0.019(4) 0.006(3) 0.003(3) -0.002(3) C34 0.017(4) 0.018(4) 0.014(4) 0.002(3) 0.005(3) -0.002(3) C35 0.022(3) 0.013(3) 0.016(3) 0.000(4) 0.004(3) -0.001(4) C36 0.016(3) 0.006(3) 0.012(3) 0.004(3) 0.001(2) 0.002(3) C37 0.025(4) 0.015(4) 0.015(4) -0.002(3) 0.005(3) -0.003(3) C38 0.019(4) 0.017(4) 0.016(4) -0.004(3) 0.002(3) -0.008(3) C39 0.013(4) 0.018(4) 0.024(4) 0.001(3) 0.003(3) -0.008(3) C40 0.024(4) 0.016(3) 0.019(4) -0.007(4) 0.002(3) -0.011(4) C41 0.027(4) 0.018(4) 0.024(4) -0.004(3) 0.005(3) -0.002(3) C42 0.028(5) 0.025(4) 0.016(4) 0.000(3) 0.007(3) 0.000(3) C43 0.021(4) 0.025(4) 0.024(4) -0.008(3) 0.004(3) -0.001(3) C44 0.015(4) 0.025(4) 0.010(4) 0.002(3) -0.002(3) -0.005(3) C45 0.017(4) 0.018(4) 0.028(5) -0.002(3) 0.007(3) 0.005(3) C46 0.013(4) 0.022(4) 0.031(5) 0.005(3) 0.002(3) 0.005(3) C47 0.046(6) 0.013(4) 0.038(5) 0.004(3) 0.013(4) 0.000(4) Cl2 0.0720(19) 0.0197(11) 0.099(2) 0.0017(12) 0.0522(17) 0.0015(12) Cl3 0.0433(14) 0.0341(12) 0.0427(14) -0.0010(10) 0.0113(11) -0.0068(10) Cl4 0.0828(19) 0.0229(11) 0.0374(14) -0.0091(10) 0.0211(13) -0.0085(12) C48 0.038(5) 0.020(4) 0.029(5) -0.007(3) 0.005(4) 0.002(4) Cl5 0.0436(14) 0.0243(11) 0.0371(13) 0.0014(9) 0.0133(10) -0.0016(9) Cl6 0.0528(15) 0.0230(11) 0.0401(13) -0.0013(9) 0.0155(11) 0.0010(10) Cl7 0.080(2) 0.0407(14) 0.0327(14) 0.0143(10) 0.0110(13) 0.0006(13) C49 0.031(5) 0.023(4) 0.042(5) -0.002(4) 0.014(4) 0.001(4) Cl8 0.0444(14) 0.0430(14) 0.0311(12) 0.0105(10) 0.0066(10) -0.0080(11) Cl9 0.0431(14) 0.0300(12) 0.0576(16) 0.0153(11) 0.0106(12) -0.0033(10) Cl10 0.0588(18) 0.092(2) 0.0311(14) 0.0183(13) 0.0202(13) 0.0415(16) _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 C21 1.969(6) . yes Pd1 P2 2.2445(18) . yes Pd1 P1 2.2615(19) . yes Pd1 Cl1 2.3486(18) . yes P1 O2 1.586(5) . yes P1 O3 1.597(5) . yes P1 O1 1.613(5) . yes P2 O5 1.587(5) . yes P2 O6 1.595(5) . yes P2 O4 1.612(5) . yes O1 C1 1.410(8) . ? O2 C11 1.427(8) . ? O3 C22 1.411(8) . ? O4 C26 1.415(8) . ? O5 C27 1.411(9) . ? O6 C37 1.414(8) . ? C1 C10 1.381(10) . ? C1 C2 1.394(10) . ? C2 C3 1.382(11) . ? C2 H2 0.9300 . ? C3 C4 1.422(11) . ? C3 H3 0.9300 . ? C4 C9 1.406(10) . ? C4 C5 1.418(10) . ? C5 C6 1.368(11) . ? C5 H5 0.9300 . ? C6 C7 1.379(11) . ? C6 H6 0.9300 . ? C7 C8 1.379(9) . ? C7 H7 0.9300 . ? C8 C9 1.418(10) . ? C8 H8 0.9300 . ? C9 C10 1.452(10) . ? C10 C12 1.475(9) . ? C11 C12 1.389(9) . ? C11 C20 1.391(10) . ? C12 C13 1.449(9) . ? C13 C14 1.401(9) . ? C13 C18 1.427(10) . ? C14 C15 1.368(10) . ? C14 H14 0.9300 . ? C15 C16 1.411(11) . ? C15 H15 0.9300 . ? C16 C17 1.357(10) . ? C16 H16 0.9300 . ? C17 C18 1.417(9) . ? C17 H17 0.9300 . ? C18 C19 1.422(10) . ? C19 C20 1.353(10) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.387(9) . ? C21 C26 1.397(9) . ? C22 C23 1.379(10) . ? C23 C24 1.413(9) . ? C23 H23 0.9300 . ? C24 C25 1.361(9) . ? C24 H24 0.9300 . ? C25 C26 1.383(10) . ? C25 H25 0.9300 . ? C27 C36 1.374(9) . ? C27 C28 1.396(10) . ? C28 C29 1.370(11) . ? C28 H28 0.9300 . ? C29 C30 1.415(10) . ? C29 H29 0.9300 . ? C30 C31 1.405(10) . ? C30 C35 1.430(9) . ? C31 C32 1.340(11) . ? C31 H31 0.9300 . ? C32 C33 1.425(11) . ? C32 H32 0.9300 . ? C33 C34 1.352(10) . ? C33 H33 0.9300 . ? C34 C35 1.412(10) . ? C34 H34 0.9300 . ? C35 C36 1.448(9) . ? C36 C38 1.481(9) . ? C37 C38 1.382(10) . ? C37 C46 1.390(10) . ? C38 C39 1.438(10) . ? C39 C40 1.413(10) . ? C39 C44 1.430(10) . ? C40 C41 1.381(9) . ? C40 H40 0.9300 . ? C41 C42 1.412(10) . ? C41 H41 0.9300 . ? C42 C43 1.371(11) . ? C42 H42 0.9300 . ? C43 C44 1.413(9) . ? C43 H43 0.9300 . ? C44 C45 1.419(10) . ? C45 C46 1.350(10) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 Cl3 1.743(9) . ? C47 Cl2 1.765(8) . ? C47 Cl4 1.779(8) . ? C47 H47 0.9800 . ? C48 Cl7 1.758(8) . ? C48 Cl6 1.766(8) . ? C48 Cl5 1.769(9) . ? C48 H48 0.9800 . ? C49 Cl8 1.744(9) . ? C49 Cl10 1.746(9) . ? C49 Cl9 1.766(8) . ? C49 H49 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pd1 P2 78.9(2) . . yes C21 Pd1 P1 79.6(2) . . yes P2 Pd1 P1 158.13(7) . . yes C21 Pd1 Cl1 175.7(2) . . yes P2 Pd1 Cl1 99.44(7) . . yes P1 Pd1 Cl1 101.66(7) . . yes O2 P1 O3 105.3(3) . . yes O2 P1 O1 103.3(3) . . yes O3 P1 O1 97.8(3) . . yes O2 P1 Pd1 118.55(19) . . ? O3 P1 Pd1 106.76(19) . . ? O1 P1 Pd1 122.1(2) . . ? O5 P2 O6 103.0(2) . . yes O5 P2 O4 97.9(3) . . yes O6 P2 O4 106.6(3) . . yes O5 P2 Pd1 127.5(2) . . ? O6 P2 Pd1 111.8(2) . . ? O4 P2 Pd1 107.77(19) . . ? C1 O1 P1 117.9(4) . . ? C11 O2 P1 119.1(4) . . ? C22 O3 P1 113.1(4) . . ? C26 O4 P2 112.2(4) . . ? C27 O5 P2 115.7(4) . . ? C37 O6 P2 120.2(4) . . ? C10 C1 C2 123.6(7) . . ? C10 C1 O1 118.3(6) . . ? C2 C1 O1 117.9(6) . . ? C3 C2 C1 119.6(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.4(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C9 C4 C5 119.0(7) . . ? C9 C4 C3 120.6(7) . . ? C5 C4 C3 120.3(7) . . ? C6 C5 C4 120.8(8) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.6(7) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 122.3(7) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C4 C9 C8 119.5(7) . . ? C4 C9 C10 119.2(7) . . ? C8 C9 C10 121.3(7) . . ? C1 C10 C9 117.0(6) . . ? C1 C10 C12 120.6(6) . . ? C9 C10 C12 122.5(6) . . ? C12 C11 C20 125.2(6) . . ? C12 C11 O2 117.9(6) . . ? C20 C11 O2 116.9(6) . . ? C11 C12 C13 116.6(6) . . ? C11 C12 C10 120.5(6) . . ? C13 C12 C10 122.8(6) . . ? C14 C13 C18 118.3(7) . . ? C14 C13 C12 123.1(6) . . ? C18 C13 C12 118.6(6) . . ? C15 C14 C13 121.7(7) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.3(7) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.9(7) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 121.2(6) . . ? C17 C18 C13 118.9(6) . . ? C19 C18 C13 119.8(6) . . ? C20 C19 C18 121.8(7) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C11 118.0(7) . . ? C19 C20 H20 121.0 . . ? C11 C20 H20 121.0 . . ? C22 C21 C26 115.8(6) . . ? C22 C21 Pd1 121.5(5) . . ? C26 C21 Pd1 122.7(5) . . ? C23 C22 C21 123.2(6) . . ? C23 C22 O3 118.1(6) . . ? C21 C22 O3 118.6(6) . . ? C22 C23 C24 117.5(6) . . ? C22 C23 H23 121.2 . . ? C24 C23 H23 121.2 . . ? C25 C24 C23 122.0(6) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 117.6(6) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C25 C26 C21 123.8(6) . . ? C25 C26 O4 118.7(6) . . ? C21 C26 O4 117.5(6) . . ? C36 C27 C28 125.8(7) . . ? C36 C27 O5 118.8(6) . . ? C28 C27 O5 115.4(6) . . ? C29 C28 C27 117.0(7) . . ? C29 C28 H28 121.5 . . ? C27 C28 H28 121.5 . . ? C28 C29 C30 122.3(7) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 122.0(7) . . ? C31 C30 C35 118.9(7) . . ? C29 C30 C35 119.0(7) . . ? C32 C31 C30 122.2(7) . . ? C32 C31 H31 118.9 . . ? C30 C31 H31 118.9 . . ? C31 C32 C33 119.1(7) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 120.5(7) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 121.5(7) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C30 117.6(6) . . ? C34 C35 C36 123.2(6) . . ? C30 C35 C36 119.2(6) . . ? C27 C36 C35 116.5(6) . . ? C27 C36 C38 120.5(6) . . ? C35 C36 C38 122.9(6) . . ? C38 C37 C46 124.1(7) . . ? C38 C37 O6 119.7(6) . . ? C46 C37 O6 116.2(6) . . ? C37 C38 C39 116.6(7) . . ? C37 C38 C36 119.8(6) . . ? C39 C38 C36 123.4(7) . . ? C40 C39 C44 117.4(6) . . ? C40 C39 C38 123.2(7) . . ? C44 C39 C38 119.4(7) . . ? C41 C40 C39 121.4(7) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C40 C41 C42 120.4(7) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 119.9(7) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.5(7) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 119.9(7) . . ? C43 C44 C39 120.4(7) . . ? C45 C44 C39 119.7(6) . . ? C46 C45 C44 120.2(7) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C37 120.0(7) . . ? C45 C46 H46 120.0 . . ? C37 C46 H46 120.0 . . ? Cl3 C47 Cl2 110.0(5) . . ? Cl3 C47 Cl4 110.5(5) . . ? Cl2 C47 Cl4 108.1(4) . . ? Cl3 C47 H47 109.4 . . ? Cl2 C47 H47 109.4 . . ? Cl4 C47 H47 109.4 . . ? Cl7 C48 Cl6 109.6(4) . . ? Cl7 C48 Cl5 109.7(5) . . ? Cl6 C48 Cl5 109.7(5) . . ? Cl7 C48 H48 109.3 . . ? Cl6 C48 H48 109.3 . . ? Cl5 C48 H48 109.3 . . ? Cl8 C49 Cl10 111.2(4) . . ? Cl8 C49 Cl9 111.0(5) . . ? Cl10 C49 Cl9 110.0(5) . . ? Cl8 C49 H49 108.2 . . ? Cl10 C49 H49 108.2 . . ? Cl9 C49 H49 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pd1 P1 O2 -113.7(3) . . . . ? P2 Pd1 P1 O2 -124.9(3) . . . . ? Cl1 Pd1 P1 O2 70.5(2) . . . . ? C21 Pd1 P1 O3 4.9(3) . . . . ? P2 Pd1 P1 O3 -6.4(3) . . . . ? Cl1 Pd1 P1 O3 -171.01(19) . . . . ? C21 Pd1 P1 O1 115.8(3) . . . . ? P2 Pd1 P1 O1 104.5(3) . . . . ? Cl1 Pd1 P1 O1 -60.1(2) . . . . ? C21 Pd1 P2 O5 123.2(4) . . . . ? P1 Pd1 P2 O5 134.5(3) . . . . ? Cl1 Pd1 P2 O5 -60.8(3) . . . . ? C21 Pd1 P2 O6 -109.0(3) . . . . ? P1 Pd1 P2 O6 -97.7(3) . . . . ? Cl1 Pd1 P2 O6 67.0(2) . . . . ? C21 Pd1 P2 O4 7.9(3) . . . . ? P1 Pd1 P2 O4 19.2(3) . . . . ? Cl1 Pd1 P2 O4 -176.13(19) . . . . ? O2 P1 O1 C1 -47.5(5) . . . . ? O3 P1 O1 C1 -155.3(5) . . . . ? Pd1 P1 O1 C1 89.2(5) . . . . ? O3 P1 O2 C11 57.7(5) . . . . ? O1 P1 O2 C11 -44.4(5) . . . . ? Pd1 P1 O2 C11 177.0(4) . . . . ? O2 P1 O3 C22 120.2(4) . . . . ? O1 P1 O3 C22 -133.6(4) . . . . ? Pd1 P1 O3 C22 -6.6(5) . . . . ? O5 P2 O4 C26 -144.0(4) . . . . ? O6 P2 O4 C26 109.8(5) . . . . ? Pd1 P2 O4 C26 -10.4(5) . . . . ? O6 P2 O5 C27 -52.9(5) . . . . ? O4 P2 O5 C27 -162.1(5) . . . . ? Pd1 P2 O5 C27 78.2(5) . . . . ? O5 P2 O6 C37 -38.1(5) . . . . ? O4 P2 O6 C37 64.4(6) . . . . ? Pd1 P2 O6 C37 -178.1(5) . . . . ? P1 O1 C1 C10 73.9(7) . . . . ? P1 O1 C1 C2 -109.2(6) . . . . ? C10 C1 C2 C3 -0.3(11) . . . . ? O1 C1 C2 C3 -177.0(6) . . . . ? C1 C2 C3 C4 -2.9(11) . . . . ? C2 C3 C4 C9 0.3(11) . . . . ? C2 C3 C4 C5 -175.6(7) . . . . ? C9 C4 C5 C6 -1.2(11) . . . . ? C3 C4 C5 C6 174.7(7) . . . . ? C4 C5 C6 C7 -1.0(12) . . . . ? C5 C6 C7 C8 1.7(12) . . . . ? C6 C7 C8 C9 -0.1(11) . . . . ? C5 C4 C9 C8 2.8(10) . . . . ? C3 C4 C9 C8 -173.2(7) . . . . ? C5 C4 C9 C10 -178.7(6) . . . . ? C3 C4 C9 C10 5.4(10) . . . . ? C7 C8 C9 C4 -2.1(10) . . . . ? C7 C8 C9 C10 179.4(7) . . . . ? C2 C1 C10 C9 5.9(10) . . . . ? O1 C1 C10 C9 -177.4(6) . . . . ? C2 C1 C10 C12 -174.6(6) . . . . ? O1 C1 C10 C12 2.1(10) . . . . ? C4 C9 C10 C1 -8.2(10) . . . . ? C8 C9 C10 C1 170.3(7) . . . . ? C4 C9 C10 C12 172.2(6) . . . . ? C8 C9 C10 C12 -9.3(10) . . . . ? P1 O2 C11 C12 73.6(7) . . . . ? P1 O2 C11 C20 -104.8(6) . . . . ? C20 C11 C12 C13 0.9(10) . . . . ? O2 C11 C12 C13 -177.3(6) . . . . ? C20 C11 C12 C10 178.8(7) . . . . ? O2 C11 C12 C10 0.6(9) . . . . ? C1 C10 C12 C11 -52.5(9) . . . . ? C9 C10 C12 C11 127.0(7) . . . . ? C1 C10 C12 C13 125.2(7) . . . . ? C9 C10 C12 C13 -55.3(9) . . . . ? C11 C12 C13 C14 175.6(6) . . . . ? C10 C12 C13 C14 -2.2(10) . . . . ? C11 C12 C13 C18 -1.9(9) . . . . ? C10 C12 C13 C18 -179.7(6) . . . . ? C18 C13 C14 C15 -2.2(10) . . . . ? C12 C13 C14 C15 -179.8(7) . . . . ? C13 C14 C15 C16 1.6(11) . . . . ? C14 C15 C16 C17 -0.2(11) . . . . ? C15 C16 C17 C18 -0.5(11) . . . . ? C16 C17 C18 C19 177.2(7) . . . . ? C16 C17 C18 C13 -0.2(10) . . . . ? C14 C13 C18 C17 1.5(10) . . . . ? C12 C13 C18 C17 179.2(6) . . . . ? C14 C13 C18 C19 -175.9(6) . . . . ? C12 C13 C18 C19 1.8(10) . . . . ? C17 C18 C19 C20 -177.9(7) . . . . ? C13 C18 C19 C20 -0.6(11) . . . . ? C18 C19 C20 C11 -0.5(11) . . . . ? C12 C11 C20 C19 0.3(11) . . . . ? O2 C11 C20 C19 178.5(6) . . . . ? P2 Pd1 C21 C22 173.0(7) . . . . ? P1 Pd1 C21 C22 -2.7(6) . . . . ? P2 Pd1 C21 C26 -4.9(6) . . . . ? P1 Pd1 C21 C26 179.4(7) . . . . ? C26 C21 C22 C23 0.8(12) . . . . ? Pd1 C21 C22 C23 -177.3(6) . . . . ? C26 C21 C22 O3 177.4(6) . . . . ? Pd1 C21 C22 O3 -0.7(10) . . . . ? P1 O3 C22 C23 -178.0(6) . . . . ? P1 O3 C22 C21 5.3(8) . . . . ? C21 C22 C23 C24 0.5(12) . . . . ? O3 C22 C23 C24 -176.1(6) . . . . ? C22 C23 C24 C25 -2.3(12) . . . . ? C23 C24 C25 C26 2.7(12) . . . . ? C24 C25 C26 C21 -1.4(12) . . . . ? C24 C25 C26 O4 176.5(7) . . . . ? C22 C21 C26 C25 -0.4(12) . . . . ? Pd1 C21 C26 C25 177.6(6) . . . . ? C22 C21 C26 O4 -178.3(7) . . . . ? Pd1 C21 C26 O4 -0.3(10) . . . . ? P2 O4 C26 C25 -170.4(6) . . . . ? P2 O4 C26 C21 7.6(8) . . . . ? P2 O5 C27 C36 78.1(7) . . . . ? P2 O5 C27 C28 -101.6(6) . . . . ? C36 C27 C28 C29 0.7(11) . . . . ? O5 C27 C28 C29 -179.6(6) . . . . ? C27 C28 C29 C30 -3.3(11) . . . . ? C28 C29 C30 C31 -176.6(7) . . . . ? C28 C29 C30 C35 1.4(11) . . . . ? C29 C30 C31 C32 177.8(7) . . . . ? C35 C30 C31 C32 -0.2(11) . . . . ? C30 C31 C32 C33 -2.1(12) . . . . ? C31 C32 C33 C34 2.9(11) . . . . ? C32 C33 C34 C35 -1.3(11) . . . . ? C33 C34 C35 C30 -1.0(10) . . . . ? C33 C34 C35 C36 179.5(6) . . . . ? C31 C30 C35 C34 1.8(10) . . . . ? C29 C30 C35 C34 -176.3(6) . . . . ? C31 C30 C35 C36 -178.7(6) . . . . ? C29 C30 C35 C36 3.2(10) . . . . ? C28 C27 C36 C35 3.7(11) . . . . ? O5 C27 C36 C35 -176.0(6) . . . . ? C28 C27 C36 C38 179.6(7) . . . . ? O5 C27 C36 C38 0.0(10) . . . . ? C34 C35 C36 C27 173.9(6) . . . . ? C30 C35 C36 C27 -5.5(9) . . . . ? C34 C35 C36 C38 -1.9(10) . . . . ? C30 C35 C36 C38 178.7(6) . . . . ? P2 O6 C37 C38 72.0(8) . . . . ? P2 O6 C37 C46 -108.0(6) . . . . ? C46 C37 C38 C39 1.7(10) . . . . ? O6 C37 C38 C39 -178.3(6) . . . . ? C46 C37 C38 C36 177.6(7) . . . . ? O6 C37 C38 C36 -2.5(10) . . . . ? C27 C36 C38 C37 -48.9(9) . . . . ? C35 C36 C38 C37 126.8(7) . . . . ? C27 C36 C38 C39 126.6(8) . . . . ? C35 C36 C38 C39 -57.7(9) . . . . ? C37 C38 C39 C40 176.0(7) . . . . ? C36 C38 C39 C40 0.4(11) . . . . ? C37 C38 C39 C44 -2.4(10) . . . . ? C36 C38 C39 C44 -178.0(6) . . . . ? C44 C39 C40 C41 -2.1(11) . . . . ? C38 C39 C40 C41 179.4(7) . . . . ? C39 C40 C41 C42 0.3(11) . . . . ? C40 C41 C42 C43 2.1(11) . . . . ? C41 C42 C43 C44 -2.6(11) . . . . ? C42 C43 C44 C45 -179.1(7) . . . . ? C42 C43 C44 C39 0.6(11) . . . . ? C40 C39 C44 C43 1.7(10) . . . . ? C38 C39 C44 C43 -179.8(7) . . . . ? C40 C39 C44 C45 -178.6(7) . . . . ? C38 C39 C44 C45 -0.1(10) . . . . ? C43 C44 C45 C46 -176.9(7) . . . . ? C39 C44 C45 C46 3.4(11) . . . . ? C44 C45 C46 C37 -4.1(11) . . . . ? C38 C37 C46 C45 1.5(11) . . . . ? O6 C37 C46 C45 -178.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.812 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.123 # Attachment '8 _mb443csadsqueeze.cif' data_8_mb443csadsqueeze _database_code_depnum_ccdc_archive 'CCDC 614137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H88 Cl4 O12 P4 Pd2' _chemical_formula_sum 'C108 H88 Cl4 O12 P4 Pd2' _chemical_formula_weight 2056.26 _chemical_absolute_configuration ad 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' 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' 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 monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.6433(17) _cell_length_b 19.522(3) _cell_length_c 18.184(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.354(5) _cell_angle_gamma 90.00 _cell_volume 5543.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2544 _cell_measurement_theta_min 2.436 _cell_measurement_theta_max 68.341 _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 4.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.142495 _exptl_absorpt_correction_T_max 0.450000 _exptl_absorpt_process_details 'SADABS V2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21718 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 70.03 _reflns_number_total 14271 _reflns_number_gt 11754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.048 0.135 0.302 6.8 0.3 2 0.383 0.330 -0.025 633.0 185.2 3 0.195 0.762 0.102 14.8 -0.5 4 0.205 0.899 0.390 11.4 0.1 5 0.618 0.830 0.374 632.8 183.4 6 0.356 0.969 0.260 6.9 -0.2 7 0.644 0.469 0.740 7.2 -0.4 8 0.805 0.262 0.898 14.8 -0.7 9 0.799 0.404 0.612 10.8 -0.1 10 0.952 0.635 0.698 6.8 0.5 _platon_squeeze_details ; ? ; _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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(9) _refine_ls_number_reflns 14271 _refine_ls_number_parameters 1178 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd2 Pd 0.96561(3) 0.37960(3) 0.13688(3) 0.02022(13) Uani 1 1 d . . . Pd1 Pd 0.85482(3) 0.61986(3) 0.22308(3) 0.02094(13) Uani 1 1 d . . . P1 P 0.75740(12) 0.58272(11) 0.29635(9) 0.0216(4) Uani 1 1 d . . . P2 P 0.88250(13) 0.42710(11) 0.04623(9) 0.0235(4) Uani 1 1 d . . . P3 P 0.97181(12) 0.59355(10) 0.29256(9) 0.0197(4) Uani 1 1 d . . . P4 P 0.86938(12) 0.31766(11) 0.19085(9) 0.0190(4) Uani 1 1 d . . . Cl3 Cl 1.05731(11) 0.32271(11) 0.22209(9) 0.0262(4) Uani 1 1 d . . . Cl4 Cl 1.07757(13) 0.43627(12) 0.08680(11) 0.0331(5) Uani 1 1 d . . . Cl2 Cl 0.73291(12) 0.65736(11) 0.15411(9) 0.0304(4) Uani 1 1 d . . . Cl1 Cl 0.94398(12) 0.67117(11) 0.14292(10) 0.0306(4) Uani 1 1 d . . . O1 O 0.7942(3) 0.5544(3) 0.3740(2) 0.0202(11) Uani 1 1 d . . . O2 O 0.6918(3) 0.6404(3) 0.3195(3) 0.0249(13) Uani 1 1 d . . . O3 O 0.6934(3) 0.5247(3) 0.2696(3) 0.0266(12) Uani 1 1 d . . . O4 O 0.7811(4) 0.4270(3) 0.0431(3) 0.0296(13) Uani 1 1 d . . . O5 O 0.9100(4) 0.5022(3) 0.0310(3) 0.0317(14) Uani 1 1 d . . . O6 O 0.8871(3) 0.3870(3) -0.0297(2) 0.0281(12) Uani 1 1 d . . . O7 O 1.0480(3) 0.5681(3) 0.2450(3) 0.0244(12) Uani 1 1 d . . . O8 O 1.0068(3) 0.6583(3) 0.3380(3) 0.0222(11) Uani 1 1 d . . . O9 O 0.9727(3) 0.5455(3) 0.3618(2) 0.0218(11) Uani 1 1 d . . . O10 O 0.8531(3) 0.3287(3) 0.2748(2) 0.0190(11) Uani 1 1 d . . . O11 O 0.7764(3) 0.3227(3) 0.1512(3) 0.0232(11) Uani 1 1 d . . . O12 O 0.8865(3) 0.2371(3) 0.1920(3) 0.0219(11) Uani 1 1 d . . . C1 C 0.7400(5) 0.5441(4) 0.4304(4) 0.0232(17) Uani 1 1 d . . . C2 C 0.7225(5) 0.4756(5) 0.4511(4) 0.0274(19) Uani 1 1 d . . . H2 H 0.7463 0.4389 0.4268 0.033 Uiso 1 1 calc R . . C3 C 0.6706(5) 0.4649(5) 0.5065(5) 0.033(2) Uani 1 1 d . . . H3 H 0.6610 0.4203 0.5220 0.039 Uiso 1 1 calc R . . C4 C 0.6306(5) 0.5192(5) 0.5415(4) 0.029(2) Uani 1 1 d . . . C5 C 0.5710(5) 0.5095(6) 0.5957(4) 0.035(2) Uani 1 1 d . . . H5 H 0.5611 0.4653 0.6122 0.042 Uiso 1 1 calc R . . C6 C 0.5277(5) 0.5618(5) 0.6247(4) 0.036(2) Uani 1 1 d . . . H6 H 0.4883 0.5530 0.6598 0.043 Uiso 1 1 calc R . . C7 C 0.5415(4) 0.6281(5) 0.6024(4) 0.031(2) Uani 1 1 d . . . H7 H 0.5104 0.6638 0.6216 0.038 Uiso 1 1 calc R . . C8 C 0.6010(5) 0.6414(4) 0.5519(4) 0.0247(18) Uani 1 1 d . . . H8 H 0.6114 0.6865 0.5383 0.030 Uiso 1 1 calc R . . C9 C 0.6466(5) 0.5880(4) 0.5206(4) 0.0236(17) Uani 1 1 d . . . C10 C 0.7069(5) 0.5992(4) 0.4638(4) 0.0217(17) Uani 1 1 d . . . C11 C 0.7268(5) 0.6900(4) 0.3712(4) 0.0240(17) Uani 1 1 d . . . C12 C 0.7347(4) 0.6699(5) 0.4432(4) 0.0244(18) Uani 1 1 d . . . C13 C 0.7780(5) 0.7165(4) 0.4950(4) 0.0233(16) Uani 1 1 d . . . C14 C 0.7979(5) 0.7003(5) 0.5695(4) 0.0290(19) Uani 1 1 d . . . H14 H 0.7818 0.6578 0.5872 0.035 Uiso 1 1 calc R . . C15 C 0.8400(5) 0.7450(5) 0.6165(4) 0.032(2) Uani 1 1 d . . . H15 H 0.8528 0.7328 0.6654 0.038 Uiso 1 1 calc R . . C16 C 0.8634(5) 0.8083(5) 0.5914(5) 0.036(2) Uani 1 1 d . . . H16 H 0.8911 0.8390 0.6239 0.043 Uiso 1 1 calc R . . C17 C 0.8465(6) 0.8277(5) 0.5177(5) 0.035(2) Uani 1 1 d . . . H17 H 0.8632 0.8706 0.5016 0.042 Uiso 1 1 calc R . . C18 C 0.8043(5) 0.7819(5) 0.4685(4) 0.033(2) Uani 1 1 d . . . C19 C 0.7900(5) 0.7994(5) 0.3921(5) 0.035(2) Uani 1 1 d . . . H19 H 0.8053 0.8424 0.3753 0.041 Uiso 1 1 calc R . . C20 C 0.7539(6) 0.7528(5) 0.3447(4) 0.0305(19) Uani 1 1 d . . . H20 H 0.7474 0.7626 0.2946 0.037 Uiso 1 1 calc R . . C21 C 0.7355(5) 0.4793(4) 0.1568(4) 0.0252(18) Uani 1 1 d . . . H21 H 0.7920 0.4880 0.1729 0.030 Uiso 1 1 calc R . . C22 C 0.6718(5) 0.4967(4) 0.1996(4) 0.0246(17) Uani 1 1 d . . . C23 C 0.5872(5) 0.4853(5) 0.1793(5) 0.033(2) Uani 1 1 d . . . C24 C 0.5711(5) 0.4570(5) 0.1098(5) 0.035(2) Uani 1 1 d . . . H24 H 0.5142 0.4503 0.0937 0.043 Uiso 1 1 calc R . . C25 C 0.6339(5) 0.4378(5) 0.0621(4) 0.033(2) Uani 1 1 d . . . C26 C 0.7179(5) 0.4480(4) 0.0881(4) 0.0267(18) Uani 1 1 d . . . C27 C 0.5146(5) 0.4990(5) 0.2315(5) 0.036(2) Uani 1 1 d . . . C28 C 0.5287(6) 0.4586(6) 0.3023(6) 0.045(2) Uani 1 1 d . . . H28A H 0.5818 0.4724 0.3271 0.068 Uiso 1 1 calc R . . H28B H 0.5309 0.4106 0.2911 0.068 Uiso 1 1 calc R . . H28C H 0.4825 0.4672 0.3335 0.068 Uiso 1 1 calc R . . C29 C 0.4273(6) 0.4746(6) 0.1961(7) 0.054(3) Uani 1 1 d . . . H29A H 0.3829 0.4843 0.2289 0.081 Uiso 1 1 calc R . . H29B H 0.4295 0.4262 0.1872 0.081 Uiso 1 1 calc R . . H29C H 0.4154 0.4982 0.1504 0.081 Uiso 1 1 calc R . . C30 C 0.5056(6) 0.5749(6) 0.2471(7) 0.057(3) Uani 1 1 d . . . H30A H 0.4524 0.5830 0.2694 0.085 Uiso 1 1 calc R . . H30B H 0.5064 0.6001 0.2019 0.085 Uiso 1 1 calc R . . H30C H 0.5522 0.5896 0.2801 0.085 Uiso 1 1 calc R . . C31 C 0.6097(7) 0.4078(6) -0.0160(5) 0.045(3) Uani 1 1 d . . . C32 C 0.6428(7) 0.3340(5) -0.0192(5) 0.047(3) Uani 1 1 d . . . H32A H 0.6341 0.3169 -0.0686 0.071 Uiso 1 1 calc R . . H32B H 0.6123 0.3058 0.0137 0.071 Uiso 1 1 calc R . . H32C H 0.7028 0.3332 -0.0048 0.071 Uiso 1 1 calc R . . C33 C 0.6455(8) 0.4523(6) -0.0738(5) 0.057(3) Uani 1 1 d . . . H33A H 0.7068 0.4540 -0.0665 0.085 Uiso 1 1 calc R . . H33B H 0.6226 0.4977 -0.0703 0.085 Uiso 1 1 calc R . . H33C H 0.6302 0.4338 -0.1217 0.085 Uiso 1 1 calc R . . C34 C 0.5125(8) 0.4068(7) -0.0316(7) 0.073(4) Uani 1 1 d . . . H34A H 0.4900 0.4520 -0.0248 0.109 Uiso 1 1 calc R . . H34B H 0.4872 0.3756 0.0017 0.109 Uiso 1 1 calc R . . H34C H 0.4994 0.3923 -0.0814 0.109 Uiso 1 1 calc R . . C35 C 0.8679(5) 0.5364(4) -0.0317(4) 0.0249(18) Uani 1 1 d . . . C36 C 0.8076(6) 0.5851(5) -0.0163(4) 0.0305(19) Uani 1 1 d . . . H36 H 0.7983 0.5968 0.0322 0.037 Uiso 1 1 calc R . . C37 C 0.7613(6) 0.6162(5) -0.0740(4) 0.037(2) Uani 1 1 d . . . H37 H 0.7205 0.6493 -0.0650 0.044 Uiso 1 1 calc R . . C38 C 0.7768(5) 0.5970(5) -0.1464(4) 0.031(2) Uani 1 1 d . . . C39 C 0.7253(5) 0.6261(5) -0.2064(4) 0.0357(19) Uani 1 1 d . . . H39 H 0.6859 0.6602 -0.1969 0.043 Uiso 1 1 calc R . . C40 C 0.7329(5) 0.6043(5) -0.2778(5) 0.036(2) Uani 1 1 d . . . H40 H 0.6986 0.6231 -0.3161 0.043 Uiso 1 1 calc R . . C41 C 0.7937(5) 0.5531(5) -0.2920(4) 0.032(2) Uani 1 1 d . . . H41 H 0.7992 0.5379 -0.3400 0.038 Uiso 1 1 calc R . . C42 C 0.8442(5) 0.5258(4) -0.2356(4) 0.0255(17) Uani 1 1 d . . . H42 H 0.8842 0.4926 -0.2463 0.031 Uiso 1 1 calc R . . C43 C 0.8378(5) 0.5464(5) -0.1618(4) 0.0262(18) Uani 1 1 d . . . C44 C 0.8876(5) 0.5167(5) -0.1002(4) 0.0257(18) Uani 1 1 d . . . C45 C 0.9519(5) 0.4007(5) -0.0782(4) 0.028(2) Uani 1 1 d . . . C46 C 0.9564(5) 0.4636(4) -0.1125(4) 0.0208(16) Uani 1 1 d . . . C47 C 1.0241(5) 0.4758(5) -0.1591(4) 0.028(2) Uani 1 1 d . . . C48 C 1.0402(5) 0.5418(5) -0.1902(4) 0.031(2) Uani 1 1 d . . . H48 H 1.0042 0.5785 -0.1817 0.038 Uiso 1 1 calc R . . C49 C 1.1094(6) 0.5504(6) -0.2329(5) 0.046(3) Uani 1 1 d . . . H49 H 1.1193 0.5931 -0.2534 0.056 Uiso 1 1 calc R . . C50 C 1.1639(6) 0.4973(6) -0.2457(5) 0.041(2) Uani 1 1 d . . . H50 H 1.2108 0.5052 -0.2737 0.049 Uiso 1 1 calc R . . C51 C 1.1508(5) 0.4331(5) -0.2185(4) 0.036(2) Uani 1 1 d . . . H51 H 1.1870 0.3975 -0.2304 0.043 Uiso 1 1 calc R . . C52 C 1.0833(5) 0.4206(5) -0.1729(4) 0.034(2) Uani 1 1 d . . . C53 C 1.0662(6) 0.3564(5) -0.1412(4) 0.037(2) Uani 1 1 d . . . H53 H 1.0993 0.3192 -0.1538 0.044 Uiso 1 1 calc R . . C54 C 1.0047(5) 0.3462(5) -0.0939(4) 0.030(2) Uani 1 1 d . . . H54 H 0.9977 0.3037 -0.0721 0.036 Uiso 1 1 calc R . . C55 C 1.1259(4) 0.5524(4) 0.2864(4) 0.0219(16) Uani 1 1 d . . . C56 C 1.1488(5) 0.4847(5) 0.2925(4) 0.0273(18) Uani 1 1 d . . . H56 H 1.1149 0.4510 0.2695 0.033 Uiso 1 1 calc R . . C57 C 1.2222(5) 0.4673(5) 0.3328(5) 0.0316(19) Uani 1 1 d . . . H57 H 1.2409 0.4221 0.3340 0.038 Uiso 1 1 calc R . . C58 C 1.2695(5) 0.5184(5) 0.3729(4) 0.0274(18) Uani 1 1 d . . . C59 C 1.3419(6) 0.5004(6) 0.4187(5) 0.042(2) Uani 1 1 d . . . H59 H 1.3576 0.4545 0.4228 0.051 Uiso 1 1 calc R . . C60 C 1.3897(6) 0.5486(6) 0.4574(5) 0.049(3) Uani 1 1 d . . . H60 H 1.4391 0.5364 0.4853 0.059 Uiso 1 1 calc R . . C61 C 1.3620(5) 0.6165(6) 0.4539(4) 0.041(2) Uani 1 1 d . . . H61 H 1.3911 0.6490 0.4831 0.049 Uiso 1 1 calc R . . C62 C 1.2933(5) 0.6370(5) 0.4089(4) 0.032(2) Uani 1 1 d . . . H62 H 1.2770 0.6828 0.4074 0.038 Uiso 1 1 calc R . . C63 C 1.2476(5) 0.5884(4) 0.3652(4) 0.0231(16) Uani 1 1 d . . . C64 C 1.1729(5) 0.6076(5) 0.3180(4) 0.0268(19) Uani 1 1 d . . . C65 C 1.0693(5) 0.7032(4) 0.3111(4) 0.0266(18) Uani 1 1 d . . . C66 C 1.1509(4) 0.6790(4) 0.3020(4) 0.0206(16) Uani 1 1 d . . . C67 C 1.2103(5) 0.7272(5) 0.2744(4) 0.0277(19) Uani 1 1 d . . . C68 C 1.2942(5) 0.7077(5) 0.2552(4) 0.033(2) Uani 1 1 d . . . H68 H 1.3098 0.6618 0.2588 0.039 Uiso 1 1 calc R . . C69 C 1.3506(6) 0.7526(5) 0.2323(5) 0.039(2) Uani 1 1 d . . . H69 H 1.4035 0.7372 0.2186 0.047 Uiso 1 1 calc R . . C70 C 1.3324(7) 0.8220(7) 0.2283(6) 0.055(3) Uani 1 1 d . . . H70 H 1.3744 0.8531 0.2162 0.066 Uiso 1 1 calc R . . C71 C 1.2492(7) 0.8454(6) 0.2429(5) 0.045(2) Uani 1 1 d . . . H71 H 1.2348 0.8914 0.2379 0.054 Uiso 1 1 calc R . . C72 C 1.1873(6) 0.7962(5) 0.2659(4) 0.035(2) Uani 1 1 d . . . C73 C 1.1034(5) 0.8176(5) 0.2781(4) 0.0316(19) Uani 1 1 d . . . H73 H 1.0886 0.8635 0.2715 0.038 Uiso 1 1 calc R . . C74 C 1.0432(5) 0.7717(5) 0.2995(4) 0.0282(19) Uani 1 1 d . . . H74 H 0.9872 0.7853 0.3062 0.034 Uiso 1 1 calc R . . C75 C 0.9176(4) 0.4363(4) 0.3166(4) 0.0192(16) Uani 1 1 d . . . H75 H 0.9134 0.4531 0.2687 0.023 Uiso 1 1 calc R . . C76 C 0.9491(4) 0.4770(4) 0.3738(4) 0.0178(16) Uani 1 1 d . . . C77 C 0.9587(5) 0.4531(4) 0.4469(4) 0.0202(16) Uani 1 1 d . . . C78 C 0.9324(4) 0.3874(4) 0.4571(3) 0.0205(15) Uani 1 1 d . . . H78 H 0.9376 0.3711 0.5052 0.025 Uiso 1 1 calc R . . C79 C 0.8976(5) 0.3402(4) 0.4024(4) 0.0228(17) Uani 1 1 d . . . C80 C 0.8923(4) 0.3699(4) 0.3316(4) 0.0236(18) Uani 1 1 d . . . C81 C 0.9942(5) 0.4992(5) 0.5114(4) 0.0269(18) Uani 1 1 d . . . C82 C 1.0843(5) 0.5241(4) 0.4978(4) 0.0265(18) Uani 1 1 d . . . H82A H 1.0819 0.5555 0.4571 0.040 Uiso 1 1 calc R . . H82B H 1.1196 0.4857 0.4867 0.040 Uiso 1 1 calc R . . H82C H 1.1081 0.5469 0.5411 0.040 Uiso 1 1 calc R . . C83 C 0.9348(5) 0.5600(5) 0.5224(4) 0.033(2) Uani 1 1 d . . . H83A H 0.9563 0.5865 0.5639 0.049 Uiso 1 1 calc R . . H83B H 0.8785 0.5436 0.5311 0.049 Uiso 1 1 calc R . . H83C H 0.9324 0.5882 0.4790 0.049 Uiso 1 1 calc R . . C84 C 0.9983(5) 0.4584(5) 0.5842(4) 0.032(2) Uani 1 1 d . . . H84A H 1.0427 0.4246 0.5833 0.047 Uiso 1 1 calc R . . H84B H 0.9443 0.4362 0.5899 0.047 Uiso 1 1 calc R . . H84C H 1.0103 0.4891 0.6248 0.047 Uiso 1 1 calc R . . C85 C 0.8676(5) 0.2691(5) 0.4203(4) 0.0250(18) Uani 1 1 d . . . C86 C 0.7709(6) 0.2635(5) 0.4030(5) 0.038(2) Uani 1 1 d . . . H86A H 0.7420 0.2974 0.4306 0.057 Uiso 1 1 calc R . . H86B H 0.7517 0.2187 0.4162 0.057 Uiso 1 1 calc R . . H86C H 0.7584 0.2709 0.3513 0.057 Uiso 1 1 calc R . . C87 C 0.9177(6) 0.2150(5) 0.3787(4) 0.035(2) Uani 1 1 d . . . H87A H 0.9040 0.2193 0.3267 0.052 Uiso 1 1 calc R . . H87B H 0.9022 0.1700 0.3947 0.052 Uiso 1 1 calc R . . H87C H 0.9780 0.2219 0.3886 0.052 Uiso 1 1 calc R . . C88 C 0.8848(6) 0.2526(5) 0.5043(4) 0.036(2) Uani 1 1 d . . . H88A H 0.9451 0.2554 0.5170 0.054 Uiso 1 1 calc R . . H88B H 0.8649 0.2072 0.5142 0.054 Uiso 1 1 calc R . . H88C H 0.8549 0.2851 0.5330 0.054 Uiso 1 1 calc R . . C89 C 0.7118(5) 0.2740(4) 0.1662(4) 0.0229(17) Uani 1 1 d . . . C90 C 0.6425(5) 0.2994(5) 0.2027(4) 0.033(2) Uani 1 1 d . . . H90 H 0.6411 0.3448 0.2181 0.040 Uiso 1 1 calc R . . C91 C 0.5759(5) 0.2551(5) 0.2154(4) 0.032(2) Uani 1 1 d . . . H91 H 0.5280 0.2708 0.2383 0.039 Uiso 1 1 calc R . . C92 C 0.5811(5) 0.1851(5) 0.1933(5) 0.037(2) Uani 1 1 d . . . C93 C 0.5149(5) 0.1390(6) 0.2068(5) 0.044(3) Uani 1 1 d . . . H93 H 0.4659 0.1550 0.2278 0.053 Uiso 1 1 calc R . . C94 C 0.5215(6) 0.0699(6) 0.1893(5) 0.048(3) Uani 1 1 d . . . H94 H 0.4767 0.0399 0.1970 0.058 Uiso 1 1 calc R . . C95 C 0.5960(6) 0.0467(5) 0.1601(4) 0.035(2) Uani 1 1 d . . . H95 H 0.6022 0.0001 0.1517 0.042 Uiso 1 1 calc R . . C96 C 0.6605(5) 0.0896(5) 0.1434(4) 0.031(2) Uani 1 1 d . . . H96 H 0.7089 0.0727 0.1223 0.038 Uiso 1 1 calc R . . C97 C 0.6527(5) 0.1603(5) 0.1586(4) 0.0275(18) Uani 1 1 d . . . C98 C 0.7195(5) 0.2092(4) 0.1403(3) 0.0215(16) Uani 1 1 d . . . C99 C 0.8756(5) 0.2045(4) 0.1226(4) 0.0191(15) Uani 1 1 d . . . C100 C 0.7928(4) 0.1901(4) 0.0972(4) 0.0188(15) Uani 1 1 d . . . C101 C 0.7826(5) 0.1580(4) 0.0248(4) 0.0212(16) Uani 1 1 d . . . C102 C 0.7016(5) 0.1468(4) -0.0118(4) 0.0287(13) Uani 1 1 d . . . H102 H 0.6523 0.1606 0.0104 0.034 Uiso 1 1 calc R . . C103 C 0.6947(5) 0.1158(5) -0.0792(4) 0.034(2) Uani 1 1 d . . . H103 H 0.6410 0.1099 -0.1031 0.041 Uiso 1 1 calc R . . C104 C 0.7670(6) 0.0931(5) -0.1123(4) 0.035(2) Uani 1 1 d . . . H104 H 0.7610 0.0706 -0.1573 0.042 Uiso 1 1 calc R . . C105 C 0.8461(5) 0.1032(4) -0.0804(4) 0.0287(13) Uani 1 1 d . . . H105 H 0.8941 0.0873 -0.1031 0.034 Uiso 1 1 calc R . . C106 C 0.8553(5) 0.1386(4) -0.0112(4) 0.0272(19) Uani 1 1 d . . . C107 C 0.9391(5) 0.1527(5) 0.0204(4) 0.0270(17) Uani 1 1 d . . . H107 H 0.9870 0.1384 -0.0036 0.032 Uiso 1 1 calc R . . C108 C 0.9491(5) 0.1870(4) 0.0856(4) 0.0240(17) Uani 1 1 d . . . H108 H 1.0034 0.1986 0.1052 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2 0.0251(3) 0.0190(3) 0.0160(2) 0.0017(2) -0.00450(18) -0.0008(2) Pd1 0.0254(3) 0.0192(3) 0.0177(2) 0.0022(2) -0.00358(18) 0.0011(2) P1 0.0220(10) 0.0237(13) 0.0188(8) 0.0043(7) -0.0026(7) 0.0019(7) P2 0.0366(11) 0.0184(13) 0.0145(8) 0.0028(7) -0.0074(7) 0.0018(8) P3 0.0247(10) 0.0152(12) 0.0185(8) -0.0007(7) -0.0059(7) -0.0011(7) P4 0.0244(10) 0.0169(12) 0.0150(8) 0.0025(7) -0.0055(6) -0.0004(7) Cl3 0.0240(9) 0.0275(12) 0.0257(8) 0.0022(7) -0.0106(7) 0.0025(7) Cl4 0.0365(11) 0.0308(14) 0.0323(9) 0.0048(8) 0.0041(7) -0.0057(8) Cl2 0.0318(10) 0.0349(13) 0.0234(8) 0.0057(8) -0.0081(7) 0.0088(8) Cl1 0.0351(11) 0.0282(13) 0.0285(9) 0.0068(8) 0.0026(7) -0.0005(8) O1 0.022(3) 0.019(3) 0.019(2) 0.003(2) -0.0038(19) -0.002(2) O2 0.031(3) 0.021(4) 0.021(2) -0.001(2) -0.007(2) -0.004(2) O3 0.028(3) 0.035(4) 0.016(2) -0.002(2) -0.0027(19) 0.007(2) O4 0.043(3) 0.026(4) 0.018(2) 0.000(2) -0.012(2) 0.002(2) O5 0.045(3) 0.037(4) 0.012(2) 0.004(2) -0.009(2) 0.008(3) O6 0.038(3) 0.026(4) 0.019(2) -0.004(2) -0.0027(19) -0.005(3) O7 0.019(3) 0.032(4) 0.022(2) -0.001(2) -0.0015(19) -0.005(2) O8 0.029(3) 0.015(3) 0.023(2) -0.002(2) -0.002(2) -0.001(2) O9 0.028(3) 0.021(4) 0.015(2) 0.005(2) -0.0031(18) 0.001(2) O10 0.022(3) 0.018(3) 0.016(2) 0.0010(19) -0.0041(18) -0.006(2) O11 0.031(3) 0.019(3) 0.020(2) 0.002(2) -0.0044(19) -0.003(2) O12 0.024(3) 0.025(4) 0.016(2) -0.006(2) -0.0058(18) -0.002(2) C1 0.025(4) 0.019(6) 0.025(3) 0.008(3) -0.005(3) -0.006(3) C2 0.030(5) 0.027(6) 0.025(4) 0.006(3) -0.004(3) 0.003(3) C3 0.036(5) 0.028(6) 0.031(4) 0.016(4) -0.015(4) -0.008(4) C4 0.023(4) 0.043(7) 0.019(3) 0.004(3) -0.007(3) -0.004(3) C5 0.023(4) 0.055(7) 0.027(4) 0.012(4) -0.006(3) -0.006(4) C6 0.030(5) 0.052(7) 0.026(4) -0.010(4) -0.002(3) -0.006(4) C7 0.019(4) 0.049(7) 0.025(3) -0.005(4) -0.006(3) 0.006(4) C8 0.022(4) 0.025(6) 0.026(3) 0.000(3) -0.006(3) 0.004(3) C9 0.029(4) 0.021(5) 0.019(3) 0.007(3) -0.011(3) 0.000(3) C10 0.024(4) 0.020(5) 0.019(3) 0.010(3) -0.006(3) -0.003(3) C11 0.030(4) 0.025(6) 0.016(3) 0.001(3) -0.006(3) 0.001(3) C12 0.021(4) 0.029(6) 0.022(3) -0.009(3) -0.005(3) 0.012(3) C13 0.028(4) 0.010(5) 0.031(4) -0.005(3) -0.004(3) 0.002(3) C14 0.029(4) 0.031(6) 0.026(4) 0.004(3) -0.010(3) -0.005(3) C15 0.031(5) 0.039(6) 0.025(4) 0.002(4) -0.002(3) 0.004(4) C16 0.037(5) 0.037(7) 0.032(4) -0.013(4) -0.011(3) -0.001(4) C17 0.043(5) 0.027(6) 0.034(4) -0.001(4) -0.008(3) 0.002(4) C18 0.039(5) 0.036(6) 0.022(4) 0.005(4) -0.003(3) -0.002(4) C19 0.038(5) 0.027(6) 0.038(4) 0.009(4) 0.000(3) -0.002(4) C20 0.047(5) 0.020(5) 0.024(4) 0.000(3) -0.004(3) 0.010(4) C21 0.033(4) 0.020(5) 0.022(4) 0.001(3) -0.008(3) -0.005(3) C22 0.030(4) 0.022(5) 0.021(3) -0.005(3) -0.013(3) 0.003(3) C23 0.036(5) 0.024(6) 0.038(4) 0.006(4) -0.009(4) 0.006(3) C24 0.022(4) 0.039(7) 0.043(5) -0.007(4) -0.016(4) 0.001(3) C25 0.037(5) 0.036(6) 0.023(4) -0.002(3) -0.022(3) -0.004(4) C26 0.041(5) 0.012(5) 0.026(4) -0.003(3) -0.011(3) 0.009(3) C27 0.012(4) 0.033(6) 0.062(6) -0.010(4) -0.002(4) 0.007(3) C28 0.025(5) 0.048(7) 0.062(6) 0.007(5) 0.003(4) 0.005(4) C29 0.030(5) 0.045(8) 0.086(8) -0.015(6) 0.005(5) -0.005(4) C30 0.031(5) 0.061(9) 0.078(7) -0.005(6) -0.002(5) -0.003(5) C31 0.060(6) 0.039(7) 0.034(5) -0.011(4) -0.028(4) -0.002(4) C32 0.071(7) 0.030(7) 0.037(5) 0.003(4) -0.033(4) -0.003(5) C33 0.097(9) 0.040(8) 0.031(5) -0.010(4) -0.021(5) 0.007(6) C34 0.089(9) 0.058(10) 0.065(7) -0.011(6) -0.055(7) 0.011(6) C35 0.043(5) 0.008(5) 0.022(3) 0.008(3) -0.013(3) -0.005(3) C36 0.057(5) 0.024(5) 0.012(3) 0.004(3) 0.010(3) 0.010(4) C37 0.051(5) 0.029(6) 0.031(4) 0.020(4) 0.010(3) 0.019(4) C38 0.040(5) 0.028(6) 0.024(4) 0.013(3) 0.002(3) 0.005(3) C39 0.038(5) 0.033(6) 0.037(4) 0.011(4) 0.002(3) 0.001(4) C40 0.030(5) 0.041(7) 0.036(4) 0.016(4) -0.009(3) 0.001(4) C41 0.032(5) 0.045(6) 0.019(3) 0.003(3) -0.002(3) -0.006(4) C42 0.030(4) 0.024(5) 0.023(3) 0.002(3) -0.003(3) 0.000(3) C43 0.036(5) 0.023(6) 0.019(3) 0.008(3) -0.004(3) -0.008(3) C44 0.029(4) 0.026(6) 0.022(3) 0.005(3) 0.000(3) -0.008(3) C45 0.038(5) 0.032(6) 0.011(3) 0.005(3) -0.009(3) -0.006(3) C46 0.028(4) 0.018(5) 0.015(3) 0.002(3) -0.010(3) 0.000(3) C47 0.027(4) 0.040(6) 0.016(3) -0.011(3) -0.008(3) -0.003(3) C48 0.034(5) 0.036(6) 0.024(4) 0.000(3) -0.004(3) -0.001(4) C49 0.053(6) 0.044(8) 0.040(5) 0.005(4) -0.011(4) -0.021(5) C50 0.037(5) 0.051(8) 0.034(4) 0.009(4) -0.002(4) -0.011(4) C51 0.036(5) 0.045(7) 0.027(4) -0.004(4) -0.003(3) 0.004(4) C52 0.039(5) 0.043(7) 0.019(4) -0.005(4) -0.010(3) -0.002(4) C53 0.057(6) 0.032(6) 0.018(4) -0.001(3) -0.019(4) 0.010(4) C54 0.046(5) 0.022(6) 0.021(4) -0.011(3) -0.010(3) 0.009(4) C55 0.018(4) 0.026(5) 0.022(3) -0.001(3) -0.001(3) 0.004(3) C56 0.023(4) 0.025(6) 0.034(4) 0.000(3) 0.008(3) 0.004(3) C57 0.041(5) 0.015(5) 0.039(4) -0.002(3) 0.007(4) 0.004(3) C58 0.032(5) 0.028(6) 0.022(3) -0.002(3) 0.002(3) 0.003(3) C59 0.046(6) 0.048(7) 0.032(4) 0.005(4) -0.007(4) 0.010(4) C60 0.046(6) 0.062(9) 0.038(5) 0.008(5) -0.018(4) 0.010(5) C61 0.038(5) 0.053(7) 0.031(4) -0.011(4) -0.008(3) 0.003(5) C62 0.031(4) 0.030(6) 0.032(4) 0.000(3) -0.005(3) 0.001(3) C63 0.020(4) 0.022(5) 0.026(3) -0.002(3) -0.005(3) -0.005(3) C64 0.027(4) 0.029(6) 0.024(3) -0.006(3) -0.001(3) 0.001(3) C65 0.044(5) 0.019(5) 0.016(3) -0.001(3) -0.005(3) 0.001(3) C66 0.024(4) 0.020(5) 0.017(3) -0.001(3) -0.007(3) -0.002(3) C67 0.032(5) 0.033(6) 0.017(3) 0.006(3) -0.005(3) -0.006(3) C68 0.040(5) 0.032(6) 0.026(4) 0.006(3) 0.001(3) -0.001(4) C69 0.042(6) 0.032(7) 0.045(5) 0.008(4) 0.016(4) 0.002(4) C70 0.047(6) 0.061(9) 0.061(6) 0.009(6) 0.020(5) -0.023(5) C71 0.061(7) 0.032(7) 0.040(5) 0.007(4) -0.003(4) -0.009(5) C72 0.037(5) 0.040(7) 0.027(4) 0.002(4) -0.002(3) -0.019(4) C73 0.045(5) 0.022(6) 0.027(4) 0.001(3) -0.007(3) -0.002(4) C74 0.033(5) 0.027(6) 0.024(4) 0.001(3) -0.010(3) -0.001(3) C75 0.020(4) 0.021(5) 0.016(3) 0.001(3) -0.002(3) 0.005(3) C76 0.014(4) 0.020(5) 0.020(3) 0.001(3) 0.000(3) 0.001(3) C77 0.029(4) 0.016(5) 0.014(3) 0.000(3) -0.010(3) 0.002(3) C78 0.029(4) 0.019(5) 0.013(3) 0.000(3) -0.006(2) -0.001(3) C79 0.028(4) 0.016(5) 0.023(3) 0.003(3) -0.004(3) 0.004(3) C80 0.028(4) 0.025(6) 0.016(3) 0.001(3) -0.013(3) -0.003(3) C81 0.034(5) 0.028(6) 0.019(3) -0.009(3) -0.003(3) 0.004(3) C82 0.026(4) 0.019(5) 0.033(4) -0.009(3) -0.016(3) 0.004(3) C83 0.046(5) 0.034(6) 0.016(3) 0.000(3) -0.017(3) -0.008(4) C84 0.034(5) 0.046(6) 0.014(3) -0.005(3) -0.013(3) 0.003(4) C85 0.033(4) 0.024(6) 0.017(3) 0.009(3) -0.006(3) -0.005(3) C86 0.042(5) 0.041(7) 0.031(4) 0.007(4) -0.001(4) -0.009(4) C87 0.064(6) 0.013(6) 0.027(4) 0.003(3) -0.005(4) -0.004(4) C88 0.049(5) 0.035(6) 0.023(4) 0.012(4) 0.001(3) -0.017(4) C89 0.033(4) 0.018(5) 0.016(3) -0.001(3) -0.014(3) 0.000(3) C90 0.023(4) 0.049(7) 0.027(4) -0.007(4) -0.002(3) 0.008(4) C91 0.031(5) 0.039(6) 0.026(4) -0.011(4) -0.007(3) 0.009(4) C92 0.028(5) 0.053(7) 0.029(4) -0.010(4) -0.007(3) -0.004(4) C93 0.024(5) 0.073(9) 0.034(4) -0.013(4) 0.001(3) -0.014(4) C94 0.049(6) 0.052(8) 0.042(5) -0.006(5) -0.001(4) -0.036(5) C95 0.058(6) 0.021(6) 0.027(4) 0.005(3) 0.001(4) -0.004(4) C96 0.032(5) 0.036(6) 0.026(4) -0.009(3) -0.001(3) -0.002(4) C97 0.039(5) 0.022(6) 0.021(3) 0.003(3) -0.006(3) -0.008(3) C98 0.042(5) 0.015(5) 0.006(3) -0.002(2) -0.010(3) 0.001(3) C99 0.032(4) 0.007(4) 0.018(3) -0.003(3) -0.004(3) 0.001(3) C100 0.025(4) 0.011(5) 0.021(3) -0.002(3) -0.001(3) 0.002(3) C101 0.029(4) 0.010(5) 0.024(3) -0.003(3) -0.002(3) -0.007(3) C102 0.038(3) 0.022(4) 0.026(3) -0.011(2) -0.001(2) -0.002(2) C103 0.035(4) 0.036(6) 0.029(4) -0.014(4) -0.011(3) 0.003(4) C104 0.055(6) 0.028(6) 0.022(4) -0.009(3) 0.003(3) -0.004(4) C105 0.038(3) 0.022(4) 0.026(3) -0.011(2) -0.001(2) -0.002(2) C106 0.046(5) 0.019(6) 0.017(3) -0.001(3) 0.001(3) -0.001(3) C107 0.032(4) 0.027(5) 0.021(3) 0.000(3) 0.003(3) 0.008(3) C108 0.030(4) 0.019(5) 0.022(3) 0.000(3) -0.007(3) 0.004(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 Pd2 P4 2.206(2) . yes Pd2 P2 2.2398(17) . yes Pd2 Cl4 2.304(2) . yes Pd2 Cl3 2.3306(17) . yes Pd1 P1 2.205(2) . yes Pd1 P3 2.2224(17) . yes Pd1 Cl1 2.305(2) . yes Pd1 Cl2 2.3379(17) . yes P1 O3 1.570(6) . yes P1 O1 1.592(5) . yes P1 O2 1.597(6) . yes P2 O5 1.557(7) . yes P2 O4 1.583(6) . yes P2 O6 1.593(5) . yes P3 O9 1.570(5) . yes P3 O8 1.590(6) . yes P3 O7 1.593(6) . yes P4 O10 1.577(5) . yes P4 O11 1.589(5) . yes P4 O12 1.595(6) . yes O1 C1 1.383(9) . ? O2 C11 1.436(9) . ? O3 C22 1.407(8) . ? O4 C26 1.384(10) . ? O5 C35 1.447(8) . ? O6 C45 1.407(10) . ? O7 C55 1.427(8) . ? O8 C65 1.420(10) . ? O9 C76 1.408(10) . ? O10 C80 1.420(8) . ? O11 C89 1.425(10) . ? O12 C99 1.414(8) . ? C1 C10 1.354(12) . ? C1 C2 1.419(12) . ? C2 C3 1.347(12) . ? C2 H2 0.9300 . ? C3 C4 1.403(13) . ? C3 H3 0.9300 . ? C4 C5 1.410(12) . ? C4 C9 1.421(12) . ? C5 C6 1.349(14) . ? C5 H5 0.9300 . ? C6 C7 1.377(14) . ? C6 H6 0.9300 . ? C7 C8 1.371(11) . ? C7 H7 0.9300 . ? C8 C9 1.402(11) . ? C8 H8 0.9300 . ? C9 C10 1.457(11) . ? C10 C12 1.500(12) . ? C11 C12 1.367(10) . ? C11 C20 1.391(12) . ? C12 C13 1.448(11) . ? C13 C14 1.409(11) . ? C13 C18 1.434(12) . ? C14 C15 1.365(12) . ? C14 H14 0.9300 . ? C15 C16 1.375(14) . ? C15 H15 0.9300 . ? C16 C17 1.402(12) . ? C16 H16 0.9300 . ? C17 C18 1.402(13) . ? C17 H17 0.9300 . ? C18 C19 1.435(11) . ? C19 C20 1.354(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.344(12) . ? C21 C26 1.402(11) . ? C21 H21 0.9300 . ? C22 C23 1.372(11) . ? C23 C24 1.389(13) . ? C23 C27 1.545(13) . ? C24 C25 1.398(13) . ? C24 H24 0.9300 . ? C25 C26 1.385(11) . ? C25 C31 1.563(10) . ? C27 C28 1.515(14) . ? C27 C30 1.516(15) . ? C27 C29 1.550(12) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.498(16) . ? C31 C34 1.530(15) . ? C31 C32 1.533(15) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C44 1.356(11) . ? C35 C36 1.380(12) . ? C36 C37 1.380(11) . ? C36 H36 0.9300 . ? C37 C38 1.404(12) . ? C37 H37 0.9300 . ? C38 C43 1.413(12) . ? C38 C39 1.434(11) . ? C39 C40 1.377(13) . ? C39 H39 0.9300 . ? C40 C41 1.415(13) . ? C40 H40 0.9300 . ? C41 C42 1.366(11) . ? C41 H41 0.9300 . ? C42 C43 1.411(11) . ? C42 H42 0.9300 . ? C43 C44 1.447(10) . ? C44 C46 1.519(12) . ? C45 C46 1.381(11) . ? C45 C54 1.386(12) . ? C46 C47 1.415(11) . ? C47 C48 1.436(13) . ? C47 C52 1.452(13) . ? C48 C49 1.378(13) . ? C48 H48 0.9300 . ? C49 C50 1.370(16) . ? C49 H49 0.9300 . ? C50 C51 1.368(14) . ? C50 H50 0.9300 . ? C51 C52 1.402(13) . ? C51 H51 0.9300 . ? C52 C53 1.410(13) . ? C53 C54 1.344(13) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.373(12) . ? C55 C64 1.407(11) . ? C56 C57 1.368(11) . ? C56 H56 0.9300 . ? C57 C58 1.418(12) . ? C57 H57 0.9300 . ? C58 C59 1.411(11) . ? C58 C63 1.414(12) . ? C59 C60 1.371(15) . ? C59 H59 0.9300 . ? C60 C61 1.394(16) . ? C60 H60 0.9300 . ? C61 C62 1.371(11) . ? C61 H61 0.9300 . ? C62 C63 1.406(11) . ? C62 H62 0.9300 . ? C63 C64 1.458(10) . ? C64 C66 1.462(12) . ? C65 C66 1.381(11) . ? C65 C74 1.409(13) . ? C66 C67 1.433(11) . ? C67 C72 1.400(14) . ? C67 C68 1.429(12) . ? C68 C69 1.329(13) . ? C68 H68 0.9300 . ? C69 C70 1.385(16) . ? C69 H69 0.9300 . ? C70 C71 1.419(15) . ? C70 H70 0.9300 . ? C71 C72 1.443(13) . ? C71 H71 0.9300 . ? C72 C73 1.407(13) . ? C73 C74 1.373(12) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C76 1.376(10) . ? C75 C80 1.387(12) . ? C75 H75 0.9300 . ? C76 C77 1.408(10) . ? C77 C78 1.363(11) . ? C77 C81 1.555(10) . ? C78 C79 1.440(11) . ? C78 H78 0.9300 . ? C79 C80 1.410(10) . ? C79 C85 1.507(12) . ? C81 C82 1.524(12) . ? C81 C83 1.528(12) . ? C81 C84 1.543(11) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 C86 1.531(11) . ? C85 C87 1.541(13) . ? C85 C88 1.568(10) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 C98 1.357(12) . ? C89 C90 1.395(11) . ? C90 C91 1.384(13) . ? C90 H90 0.9300 . ? C91 C92 1.429(14) . ? C91 H91 0.9300 . ? C92 C97 1.403(12) . ? C92 C93 1.404(13) . ? C93 C94 1.391(16) . ? C93 H93 0.9300 . ? C94 C95 1.386(15) . ? C94 H94 0.9300 . ? C95 C96 1.358(13) . ? C95 H95 0.9300 . ? C96 C97 1.415(12) . ? C96 H96 0.9300 . ? C97 C98 1.466(11) . ? C98 C100 1.474(11) . ? C99 C100 1.380(10) . ? C99 C108 1.408(11) . ? C100 C101 1.458(10) . ? C101 C106 1.396(11) . ? C101 C102 1.415(10) . ? C102 C103 1.365(11) . ? C102 H102 0.9300 . ? C103 C104 1.385(12) . ? C103 H103 0.9300 . ? C104 C105 1.349(12) . ? C104 H104 0.9300 . ? C105 C106 1.437(10) . ? C105 H105 0.9300 . ? C106 C107 1.427(11) . ? C107 C108 1.363(11) . ? C107 H107 0.9300 . ? C108 H108 0.9300 . ? 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 P4 Pd2 P2 99.94(7) . . yes P4 Pd2 Cl4 173.55(8) . . yes P2 Pd2 Cl4 86.11(8) . . yes P4 Pd2 Cl3 81.52(7) . . yes P2 Pd2 Cl3 174.13(8) . . yes Cl4 Pd2 Cl3 92.24(7) . . yes P1 Pd1 P3 98.96(7) . . yes P1 Pd1 Cl1 172.08(8) . . yes P3 Pd1 Cl1 87.21(7) . . yes P1 Pd1 Cl2 81.73(7) . . yes P3 Pd1 Cl2 174.94(8) . . yes Cl1 Pd1 Cl2 91.69(7) . . yes O3 P1 O1 102.5(3) . . yes O3 P1 O2 100.5(3) . . yes O1 P1 O2 102.5(3) . . yes O3 P1 Pd1 120.0(2) . . ? O1 P1 Pd1 115.0(2) . . ? O2 P1 Pd1 113.9(2) . . ? O5 P2 O4 106.4(3) . . yes O5 P2 O6 106.4(3) . . yes O4 P2 O6 93.6(3) . . yes O5 P2 Pd2 111.5(2) . . ? O4 P2 Pd2 124.3(2) . . ? O6 P2 Pd2 112.4(2) . . ? O9 P3 O8 94.1(3) . . yes O9 P3 O7 106.1(3) . . yes O8 P3 O7 106.5(3) . . yes O9 P3 Pd1 124.2(2) . . ? O8 P3 Pd1 111.0(2) . . ? O7 P3 Pd1 112.37(19) . . ? O10 P4 O11 103.6(3) . . yes O10 P4 O12 99.2(3) . . yes O11 P4 O12 102.4(3) . . yes O10 P4 Pd2 120.6(2) . . ? O11 P4 Pd2 113.3(2) . . ? O12 P4 Pd2 115.4(2) . . ? C1 O1 P1 120.1(4) . . ? C11 O2 P1 115.0(4) . . ? C22 O3 P1 132.5(5) . . ? C26 O4 P2 136.7(5) . . ? C35 O5 P2 117.2(5) . . ? C45 O6 P2 121.4(5) . . ? C55 O7 P3 115.0(4) . . ? C65 O8 P3 122.3(5) . . ? C76 O9 P3 134.6(4) . . ? C80 O10 P4 134.0(5) . . ? C89 O11 P4 120.8(5) . . ? C99 O12 P4 114.9(4) . . ? C10 C1 O1 118.9(7) . . ? C10 C1 C2 123.0(7) . . ? O1 C1 C2 118.1(7) . . ? C3 C2 C1 118.6(8) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 121.8(9) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 123.1(9) . . ? C3 C4 C9 120.2(8) . . ? C5 C4 C9 116.6(8) . . ? C6 C5 C4 122.6(9) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 120.4(9) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.0(8) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.8(8) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C4 119.5(7) . . ? C8 C9 C10 122.8(7) . . ? C4 C9 C10 117.5(7) . . ? C1 C10 C9 118.7(7) . . ? C1 C10 C12 119.7(7) . . ? C9 C10 C12 121.6(7) . . ? C12 C11 C20 125.0(7) . . ? C12 C11 O2 116.3(7) . . ? C20 C11 O2 118.6(6) . . ? C11 C12 C13 117.1(8) . . ? C11 C12 C10 119.5(7) . . ? C13 C12 C10 123.2(7) . . ? C14 C13 C18 118.1(7) . . ? C14 C13 C12 123.6(8) . . ? C18 C13 C12 118.3(7) . . ? C15 C14 C13 122.0(8) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 119.7(8) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 121.4(8) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 119.6(9) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 120.5(9) . . ? C17 C18 C13 119.2(7) . . ? C19 C18 C13 120.4(8) . . ? C20 C19 C18 119.5(9) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C11 119.7(7) . . ? C19 C20 H20 120.2 . . ? C11 C20 H20 120.2 . . ? C22 C21 C26 120.8(7) . . ? C22 C21 H21 119.6 . . ? C26 C21 H21 119.6 . . ? C21 C22 C23 122.7(7) . . ? C21 C22 O3 118.4(6) . . ? C23 C22 O3 118.9(7) . . ? C22 C23 C24 115.5(8) . . ? C22 C23 C27 122.6(8) . . ? C24 C23 C27 121.8(7) . . ? C23 C24 C25 125.1(7) . . ? C23 C24 H24 117.5 . . ? C25 C24 H24 117.5 . . ? C26 C25 C24 115.9(7) . . ? C26 C25 C31 122.6(8) . . ? C24 C25 C31 121.5(7) . . ? O4 C26 C25 116.9(7) . . ? O4 C26 C21 123.1(7) . . ? C25 C26 C21 120.0(8) . . ? C28 C27 C30 111.1(9) . . ? C28 C27 C23 110.8(7) . . ? C30 C27 C23 111.4(8) . . ? C28 C27 C29 105.9(8) . . ? C30 C27 C29 106.8(7) . . ? C23 C27 C29 110.7(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 106.6(9) . . ? C33 C31 C32 112.2(10) . . ? C34 C31 C32 108.4(9) . . ? C33 C31 C25 109.9(8) . . ? C34 C31 C25 111.0(9) . . ? C32 C31 C25 108.8(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C44 C35 C36 125.2(7) . . ? C44 C35 O5 118.5(7) . . ? C36 C35 O5 116.2(7) . . ? C37 C36 C35 118.8(7) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 119.0(8) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C37 C38 C43 121.8(7) . . ? C37 C38 C39 119.2(8) . . ? C43 C38 C39 118.9(8) . . ? C40 C39 C38 121.2(9) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.2(7) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 120.2(8) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 122.2(8) . . ? C41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C42 C43 C38 118.3(7) . . ? C42 C43 C44 123.8(8) . . ? C38 C43 C44 117.9(7) . . ? C35 C44 C43 117.1(8) . . ? C35 C44 C46 121.9(7) . . ? C43 C44 C46 120.9(7) . . ? C46 C45 C54 122.9(8) . . ? C46 C45 O6 120.6(8) . . ? C54 C45 O6 116.3(7) . . ? C45 C46 C47 118.6(8) . . ? C45 C46 C44 119.1(7) . . ? C47 C46 C44 122.3(7) . . ? C46 C47 C48 122.8(8) . . ? C46 C47 C52 119.1(8) . . ? C48 C47 C52 118.0(8) . . ? C49 C48 C47 119.6(9) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C50 C49 C48 121.3(10) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C51 C50 C49 121.6(10) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C50 C51 C52 120.5(9) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C51 C52 C53 124.3(9) . . ? C51 C52 C47 118.9(9) . . ? C53 C52 C47 116.8(8) . . ? C54 C53 C52 123.6(9) . . ? C54 C53 H53 118.2 . . ? C52 C53 H53 118.2 . . ? C53 C54 C45 118.4(9) . . ? C53 C54 H54 120.8 . . ? C45 C54 H54 120.8 . . ? C56 C55 C64 125.1(7) . . ? C56 C55 O7 117.4(7) . . ? C64 C55 O7 117.5(7) . . ? C57 C56 C55 119.4(8) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 119.8(8) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C59 C58 C63 118.8(8) . . ? C59 C58 C57 120.3(9) . . ? C63 C58 C57 120.9(7) . . ? C60 C59 C58 121.8(10) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C59 C60 C61 118.0(8) . . ? C59 C60 H60 121.0 . . ? C61 C60 H60 121.0 . . ? C62 C61 C60 122.4(9) . . ? C62 C61 H61 118.8 . . ? C60 C61 H61 118.8 . . ? C61 C62 C63 119.7(9) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C62 C63 C58 118.9(7) . . ? C62 C63 C64 121.6(8) . . ? C58 C63 C64 119.2(7) . . ? C55 C64 C63 115.2(7) . . ? C55 C64 C66 122.5(6) . . ? C63 C64 C66 122.2(7) . . ? C66 C65 C74 124.6(8) . . ? C66 C65 O8 119.3(7) . . ? C74 C65 O8 116.0(7) . . ? C65 C66 C67 116.1(8) . . ? C65 C66 C64 120.7(7) . . ? C67 C66 C64 123.1(7) . . ? C72 C67 C68 117.6(8) . . ? C72 C67 C66 120.1(8) . . ? C68 C67 C66 122.3(8) . . ? C69 C68 C67 122.4(10) . . ? C69 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? C68 C69 C70 121.6(9) . . ? C68 C69 H69 119.2 . . ? C70 C69 H69 119.2 . . ? C69 C70 C71 119.5(9) . . ? C69 C70 H70 120.2 . . ? C71 C70 H70 120.2 . . ? C70 C71 C72 118.6(10) . . ? C70 C71 H71 120.7 . . ? C72 C71 H71 120.7 . . ? C67 C72 C73 120.3(8) . . ? C67 C72 C71 120.0(9) . . ? C73 C72 C71 119.6(9) . . ? C74 C73 C72 120.7(9) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C65 117.7(8) . . ? C73 C74 H74 121.1 . . ? C65 C74 H74 121.1 . . ? C76 C75 C80 119.0(6) . . ? C76 C75 H75 120.5 . . ? C80 C75 H75 120.5 . . ? C75 C76 O9 121.1(6) . . ? C75 C76 C77 122.4(7) . . ? O9 C76 C77 116.5(6) . . ? C78 C77 C76 115.1(6) . . ? C78 C77 C81 122.6(6) . . ? C76 C77 C81 122.3(7) . . ? C77 C78 C79 127.8(6) . . ? C77 C78 H78 116.1 . . ? C79 C78 H78 116.1 . . ? C80 C79 C78 111.6(7) . . ? C80 C79 C85 125.0(7) . . ? C78 C79 C85 123.3(6) . . ? C75 C80 C79 124.2(7) . . ? C75 C80 O10 120.2(6) . . ? C79 C80 O10 115.5(7) . . ? C82 C81 C83 110.4(7) . . ? C82 C81 C84 108.2(6) . . ? C83 C81 C84 106.5(6) . . ? C82 C81 C77 110.8(6) . . ? C83 C81 C77 110.8(6) . . ? C84 C81 C77 110.1(7) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C79 C85 C86 109.7(7) . . ? C79 C85 C87 110.6(7) . . ? C86 C85 C87 112.0(7) . . ? C79 C85 C88 111.2(6) . . ? C86 C85 C88 107.3(6) . . ? C87 C85 C88 105.9(7) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C98 C89 C90 125.7(8) . . ? C98 C89 O11 118.5(7) . . ? C90 C89 O11 115.6(8) . . ? C91 C90 C89 118.0(9) . . ? C91 C90 H90 121.0 . . ? C89 C90 H90 121.0 . . ? C90 C91 C92 119.7(8) . . ? C90 C91 H91 120.2 . . ? C92 C91 H91 120.2 . . ? C97 C92 C93 118.3(9) . . ? C97 C92 C91 121.1(8) . . ? C93 C92 C91 120.6(9) . . ? C94 C93 C92 121.1(9) . . ? C94 C93 H93 119.5 . . ? C92 C93 H93 119.5 . . ? C95 C94 C93 118.6(8) . . ? C95 C94 H94 120.7 . . ? C93 C94 H94 120.7 . . ? C96 C95 C94 122.5(9) . . ? C96 C95 H95 118.8 . . ? C94 C95 H95 118.8 . . ? C95 C96 C97 119.0(8) . . ? C95 C96 H96 120.5 . . ? C97 C96 H96 120.5 . . ? C92 C97 C96 120.2(8) . . ? C92 C97 C98 118.4(8) . . ? C96 C97 C98 121.4(8) . . ? C89 C98 C97 116.7(7) . . ? C89 C98 C100 120.4(7) . . ? C97 C98 C100 122.9(7) . . ? C100 C99 C108 124.6(6) . . ? C100 C99 O12 116.9(6) . . ? C108 C99 O12 118.6(6) . . ? C99 C100 C101 116.1(6) . . ? C99 C100 C98 121.0(6) . . ? C101 C100 C98 122.8(6) . . ? C106 C101 C102 118.0(7) . . ? C106 C101 C100 119.4(6) . . ? C102 C101 C100 122.6(7) . . ? C103 C102 C101 120.9(8) . . ? C103 C102 H102 119.6 . . ? C101 C102 H102 119.6 . . ? C102 C103 C104 120.5(7) . . ? C102 C103 H103 119.7 . . ? C104 C103 H103 119.7 . . ? C105 C104 C103 121.3(7) . . ? C105 C104 H104 119.4 . . ? C103 C104 H104 119.4 . . ? C104 C105 C106 119.2(8) . . ? C104 C105 H105 120.4 . . ? C106 C105 H105 120.4 . . ? C101 C106 C107 120.9(7) . . ? C101 C106 C105 119.9(7) . . ? C107 C106 C105 119.2(7) . . ? C108 C107 C106 120.0(7) . . ? C108 C107 H107 120.0 . . ? C106 C107 H107 120.0 . . ? C107 C108 C99 118.7(7) . . ? C107 C108 H108 120.6 . . ? C99 C108 H108 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Pd1 P1 O3 -119.5(3) . . . . ? Cl2 Pd1 P1 O3 65.6(3) . . . . ? P3 Pd1 P1 O1 3.6(3) . . . . ? Cl2 Pd1 P1 O1 -171.4(3) . . . . ? P3 Pd1 P1 O2 121.4(2) . . . . ? Cl2 Pd1 P1 O2 -53.5(2) . . . . ? P4 Pd2 P2 O5 143.3(3) . . . . ? Cl4 Pd2 P2 O5 -39.0(3) . . . . ? P4 Pd2 P2 O4 13.9(3) . . . . ? Cl4 Pd2 P2 O4 -168.3(3) . . . . ? P4 Pd2 P2 O6 -97.4(2) . . . . ? Cl4 Pd2 P2 O6 80.3(2) . . . . ? P1 Pd1 P3 O9 13.3(3) . . . . ? Cl1 Pd1 P3 O9 -171.7(3) . . . . ? P1 Pd1 P3 O8 -97.5(2) . . . . ? Cl1 Pd1 P3 O8 77.5(2) . . . . ? P1 Pd1 P3 O7 143.3(3) . . . . ? Cl1 Pd1 P3 O7 -41.7(3) . . . . ? P2 Pd2 P4 O10 -121.9(2) . . . . ? Cl3 Pd2 P4 O10 63.9(2) . . . . ? P2 Pd2 P4 O11 1.6(2) . . . . ? Cl3 Pd2 P4 O11 -172.7(2) . . . . ? P2 Pd2 P4 O12 119.1(2) . . . . ? Cl3 Pd2 P4 O12 -55.1(2) . . . . ? O3 P1 O1 C1 -62.4(6) . . . . ? O2 P1 O1 C1 41.5(6) . . . . ? Pd1 P1 O1 C1 165.7(5) . . . . ? O3 P1 O2 C11 157.7(5) . . . . ? O1 P1 O2 C11 52.2(5) . . . . ? Pd1 P1 O2 C11 -72.6(5) . . . . ? O1 P1 O3 C22 -143.1(6) . . . . ? O2 P1 O3 C22 111.5(7) . . . . ? Pd1 P1 O3 C22 -14.2(7) . . . . ? O5 P2 O4 C26 -75.5(8) . . . . ? O6 P2 O4 C26 176.3(8) . . . . ? Pd2 P2 O4 C26 55.9(9) . . . . ? O4 P2 O5 C35 -48.6(6) . . . . ? O6 P2 O5 C35 50.3(6) . . . . ? Pd2 P2 O5 C35 173.2(5) . . . . ? O5 P2 O6 C45 37.2(6) . . . . ? O4 P2 O6 C45 145.4(6) . . . . ? Pd2 P2 O6 C45 -85.1(6) . . . . ? O9 P3 O7 C55 -43.1(6) . . . . ? O8 P3 O7 C55 56.4(6) . . . . ? Pd1 P3 O7 C55 178.2(5) . . . . ? O9 P3 O8 C65 138.6(6) . . . . ? O7 P3 O8 C65 30.4(6) . . . . ? Pd1 P3 O8 C65 -92.2(5) . . . . ? O8 P3 O9 C76 178.2(6) . . . . ? O7 P3 O9 C76 -73.3(7) . . . . ? Pd1 P3 O9 C76 59.2(7) . . . . ? O11 P4 O10 C80 -133.0(7) . . . . ? O12 P4 O10 C80 121.8(7) . . . . ? Pd2 P4 O10 C80 -5.0(8) . . . . ? O10 P4 O11 C89 -63.6(6) . . . . ? O12 P4 O11 C89 39.2(6) . . . . ? Pd2 P4 O11 C89 164.0(5) . . . . ? O10 P4 O12 C99 159.8(5) . . . . ? O11 P4 O12 C99 53.6(5) . . . . ? Pd2 P4 O12 C99 -69.9(5) . . . . ? P1 O1 C1 C10 -70.8(8) . . . . ? P1 O1 C1 C2 109.9(7) . . . . ? C10 C1 C2 C3 -0.1(11) . . . . ? O1 C1 C2 C3 179.2(6) . . . . ? C1 C2 C3 C4 3.1(11) . . . . ? C2 C3 C4 C5 175.0(7) . . . . ? C2 C3 C4 C9 -2.2(11) . . . . ? C3 C4 C5 C6 -174.4(7) . . . . ? C9 C4 C5 C6 3.0(10) . . . . ? C4 C5 C6 C7 -1.0(11) . . . . ? C5 C6 C7 C8 -1.6(11) . . . . ? C6 C7 C8 C9 2.0(10) . . . . ? C7 C8 C9 C4 0.0(10) . . . . ? C7 C8 C9 C10 176.5(6) . . . . ? C3 C4 C9 C8 175.0(6) . . . . ? C5 C4 C9 C8 -2.4(9) . . . . ? C3 C4 C9 C10 -1.6(9) . . . . ? C5 C4 C9 C10 -179.0(6) . . . . ? O1 C1 C10 C9 177.0(5) . . . . ? C2 C1 C10 C9 -3.7(10) . . . . ? O1 C1 C10 C12 -4.7(9) . . . . ? C2 C1 C10 C12 174.6(6) . . . . ? C8 C9 C10 C1 -172.0(6) . . . . ? C4 C9 C10 C1 4.4(9) . . . . ? C8 C9 C10 C12 9.7(10) . . . . ? C4 C9 C10 C12 -173.8(6) . . . . ? P1 O2 C11 C12 -78.5(7) . . . . ? P1 O2 C11 C20 98.2(7) . . . . ? C20 C11 C12 C13 -2.7(12) . . . . ? O2 C11 C12 C13 173.8(6) . . . . ? C20 C11 C12 C10 -176.7(8) . . . . ? O2 C11 C12 C10 -0.3(10) . . . . ? C1 C10 C12 C11 55.5(9) . . . . ? C9 C10 C12 C11 -126.3(7) . . . . ? C1 C10 C12 C13 -118.2(8) . . . . ? C9 C10 C12 C13 60.0(9) . . . . ? C11 C12 C13 C14 -174.1(8) . . . . ? C10 C12 C13 C14 -0.2(12) . . . . ? C11 C12 C13 C18 4.0(11) . . . . ? C10 C12 C13 C18 177.8(7) . . . . ? C18 C13 C14 C15 0.8(13) . . . . ? C12 C13 C14 C15 178.9(8) . . . . ? C13 C14 C15 C16 0.6(13) . . . . ? C14 C15 C16 C17 -1.3(14) . . . . ? C15 C16 C17 C18 0.5(14) . . . . ? C16 C17 C18 C19 -177.1(8) . . . . ? C16 C17 C18 C13 1.0(13) . . . . ? C14 C13 C18 C17 -1.7(12) . . . . ? C12 C13 C18 C17 -179.8(8) . . . . ? C14 C13 C18 C19 176.4(8) . . . . ? C12 C13 C18 C19 -1.7(12) . . . . ? C17 C18 C19 C20 175.9(9) . . . . ? C13 C18 C19 C20 -2.2(13) . . . . ? C18 C19 C20 C11 3.7(13) . . . . ? C12 C11 C20 C19 -1.3(13) . . . . ? O2 C11 C20 C19 -177.6(7) . . . . ? C26 C21 C22 C23 0.0(13) . . . . ? C26 C21 C22 O3 176.9(8) . . . . ? P1 O3 C22 C21 47.3(11) . . . . ? P1 O3 C22 C23 -135.7(7) . . . . ? C21 C22 C23 C24 -2.6(13) . . . . ? O3 C22 C23 C24 -179.5(8) . . . . ? C21 C22 C23 C27 174.1(8) . . . . ? O3 C22 C23 C27 -2.8(13) . . . . ? C22 C23 C24 C25 2.4(15) . . . . ? C27 C23 C24 C25 -174.3(9) . . . . ? C23 C24 C25 C26 0.4(15) . . . . ? C23 C24 C25 C31 -178.6(9) . . . . ? P2 O4 C26 C25 179.7(7) . . . . ? P2 O4 C26 C21 0.4(13) . . . . ? C24 C25 C26 O4 177.6(8) . . . . ? C31 C25 C26 O4 -3.4(13) . . . . ? C24 C25 C26 C21 -3.2(13) . . . . ? C31 C25 C26 C21 175.9(9) . . . . ? C22 C21 C26 O4 -177.7(8) . . . . ? C22 C21 C26 C25 3.1(13) . . . . ? C22 C23 C27 C28 -57.2(12) . . . . ? C24 C23 C27 C28 119.3(10) . . . . ? C22 C23 C27 C30 67.0(11) . . . . ? C24 C23 C27 C30 -116.5(10) . . . . ? C22 C23 C27 C29 -174.4(9) . . . . ? C24 C23 C27 C29 2.2(13) . . . . ? C26 C25 C31 C33 -58.5(12) . . . . ? C24 C25 C31 C33 120.5(11) . . . . ? C26 C25 C31 C34 -176.2(9) . . . . ? C24 C25 C31 C34 2.8(14) . . . . ? C26 C25 C31 C32 64.7(12) . . . . ? C24 C25 C31 C32 -116.4(10) . . . . ? P2 O5 C35 C44 -72.0(9) . . . . ? P2 O5 C35 C36 105.3(8) . . . . ? C44 C35 C36 C37 1.4(14) . . . . ? O5 C35 C36 C37 -175.7(8) . . . . ? C35 C36 C37 C38 0.3(14) . . . . ? C36 C37 C38 C43 0.6(14) . . . . ? C36 C37 C38 C39 176.2(9) . . . . ? C37 C38 C39 C40 -174.1(9) . . . . ? C43 C38 C39 C40 1.6(14) . . . . ? C38 C39 C40 C41 -0.9(14) . . . . ? C39 C40 C41 C42 -0.3(13) . . . . ? C40 C41 C42 C43 0.7(13) . . . . ? C41 C42 C43 C38 0.0(13) . . . . ? C41 C42 C43 C44 177.3(8) . . . . ? C37 C38 C43 C42 174.5(9) . . . . ? C39 C38 C43 C42 -1.1(12) . . . . ? C37 C38 C43 C44 -3.0(13) . . . . ? C39 C38 C43 C44 -178.6(8) . . . . ? C36 C35 C44 C43 -3.8(13) . . . . ? O5 C35 C44 C43 173.3(7) . . . . ? C36 C35 C44 C46 178.8(8) . . . . ? O5 C35 C44 C46 -4.1(12) . . . . ? C42 C43 C44 C35 -173.0(8) . . . . ? C38 C43 C44 C35 4.4(11) . . . . ? C42 C43 C44 C46 4.5(12) . . . . ? C38 C43 C44 C46 -178.1(7) . . . . ? P2 O6 C45 C46 -65.5(7) . . . . ? P2 O6 C45 C54 119.9(7) . . . . ? C54 C45 C46 C47 -7.7(10) . . . . ? O6 C45 C46 C47 178.1(6) . . . . ? C54 C45 C46 C44 171.1(6) . . . . ? O6 C45 C46 C44 -3.1(9) . . . . ? C35 C44 C46 C45 53.6(11) . . . . ? C43 C44 C46 C45 -123.7(8) . . . . ? C35 C44 C46 C47 -127.6(8) . . . . ? C43 C44 C46 C47 55.0(10) . . . . ? C45 C46 C47 C48 -172.5(7) . . . . ? C44 C46 C47 C48 8.8(10) . . . . ? C45 C46 C47 C52 3.8(9) . . . . ? C44 C46 C47 C52 -174.9(6) . . . . ? C46 C47 C48 C49 177.6(7) . . . . ? C52 C47 C48 C49 1.2(10) . . . . ? C47 C48 C49 C50 -0.6(12) . . . . ? C48 C49 C50 C51 1.8(14) . . . . ? C49 C50 C51 C52 -3.5(13) . . . . ? C50 C51 C52 C53 -178.6(7) . . . . ? C50 C51 C52 C47 4.1(11) . . . . ? C46 C47 C52 C51 -179.4(6) . . . . ? C48 C47 C52 C51 -2.9(10) . . . . ? C46 C47 C52 C53 3.1(9) . . . . ? C48 C47 C52 C53 179.6(6) . . . . ? C51 C52 C53 C54 175.6(7) . . . . ? C47 C52 C53 C54 -7.1(11) . . . . ? C52 C53 C54 C45 3.7(11) . . . . ? C46 C45 C54 C53 4.0(11) . . . . ? O6 C45 C54 C53 178.5(6) . . . . ? P3 O7 C55 C56 109.0(7) . . . . ? P3 O7 C55 C64 -70.7(8) . . . . ? C64 C55 C56 C57 0.8(13) . . . . ? O7 C55 C56 C57 -178.8(7) . . . . ? C55 C56 C57 C58 5.4(12) . . . . ? C56 C57 C58 C59 175.6(8) . . . . ? C56 C57 C58 C63 -7.2(13) . . . . ? C63 C58 C59 C60 1.9(14) . . . . ? C57 C58 C59 C60 179.2(9) . . . . ? C58 C59 C60 C61 3.7(15) . . . . ? C59 C60 C61 C62 -5.2(15) . . . . ? C60 C61 C62 C63 0.9(14) . . . . ? C61 C62 C63 C58 4.9(12) . . . . ? C61 C62 C63 C64 178.4(8) . . . . ? C59 C58 C63 C62 -6.2(12) . . . . ? C57 C58 C63 C62 176.5(8) . . . . ? C59 C58 C63 C64 -179.9(8) . . . . ? C57 C58 C63 C64 2.9(12) . . . . ? C56 C55 C64 C63 -5.0(12) . . . . ? O7 C55 C64 C63 174.7(6) . . . . ? C56 C55 C64 C66 172.1(8) . . . . ? O7 C55 C64 C66 -8.3(11) . . . . ? C62 C63 C64 C55 -170.6(7) . . . . ? C58 C63 C64 C55 2.9(11) . . . . ? C62 C63 C64 C66 12.4(12) . . . . ? C58 C63 C64 C66 -174.2(7) . . . . ? P3 O8 C65 C66 -65.6(7) . . . . ? P3 O8 C65 C74 117.8(6) . . . . ? C74 C65 C66 C67 -4.0(10) . . . . ? O8 C65 C66 C67 179.8(6) . . . . ? C74 C65 C66 C64 177.7(7) . . . . ? O8 C65 C66 C64 1.4(10) . . . . ? C55 C64 C66 C65 53.8(10) . . . . ? C63 C64 C66 C65 -129.3(8) . . . . ? C55 C64 C66 C67 -124.4(8) . . . . ? C63 C64 C66 C67 52.5(10) . . . . ? C65 C66 C67 C72 6.8(10) . . . . ? C64 C66 C67 C72 -174.8(7) . . . . ? C65 C66 C67 C68 -173.5(7) . . . . ? C64 C66 C67 C68 4.8(10) . . . . ? C72 C67 C68 C69 2.3(12) . . . . ? C66 C67 C68 C69 -177.4(8) . . . . ? C67 C68 C69 C70 2.5(14) . . . . ? C68 C69 C70 C71 -5.5(16) . . . . ? C69 C70 C71 C72 3.6(15) . . . . ? C68 C67 C72 C73 174.8(7) . . . . ? C66 C67 C72 C73 -5.5(11) . . . . ? C68 C67 C72 C71 -4.0(11) . . . . ? C66 C67 C72 C71 175.7(7) . . . . ? C70 C71 C72 C67 1.1(13) . . . . ? C70 C71 C72 C73 -177.7(8) . . . . ? C67 C72 C73 C74 0.9(11) . . . . ? C71 C72 C73 C74 179.7(7) . . . . ? C72 C73 C74 C65 2.0(11) . . . . ? C66 C65 C74 C73 -0.4(11) . . . . ? O8 C65 C74 C73 176.0(6) . . . . ? C80 C75 C76 O9 -177.6(6) . . . . ? C80 C75 C76 C77 1.7(11) . . . . ? P3 O9 C76 C75 0.6(10) . . . . ? P3 O9 C76 C77 -178.7(5) . . . . ? C75 C76 C77 C78 -1.6(11) . . . . ? O9 C76 C77 C78 177.7(6) . . . . ? C75 C76 C77 C81 -179.9(7) . . . . ? O9 C76 C77 C81 -0.6(10) . . . . ? C76 C77 C78 C79 0.9(12) . . . . ? C81 C77 C78 C79 179.1(7) . . . . ? C77 C78 C79 C80 -0.1(11) . . . . ? C77 C78 C79 C85 -177.8(8) . . . . ? C76 C75 C80 C79 -0.9(12) . . . . ? C76 C75 C80 O10 174.9(6) . . . . ? C78 C79 C80 C75 0.1(11) . . . . ? C85 C79 C80 C75 177.8(7) . . . . ? C78 C79 C80 O10 -175.8(6) . . . . ? C85 C79 C80 O10 1.8(11) . . . . ? P4 O10 C80 C75 40.1(11) . . . . ? P4 O10 C80 C79 -143.8(6) . . . . ? C78 C77 C81 C82 122.3(8) . . . . ? C76 C77 C81 C82 -59.6(9) . . . . ? C78 C77 C81 C83 -114.9(8) . . . . ? C76 C77 C81 C83 63.3(10) . . . . ? C78 C77 C81 C84 2.6(10) . . . . ? C76 C77 C81 C84 -179.2(7) . . . . ? C80 C79 C85 C86 -62.4(10) . . . . ? C78 C79 C85 C86 115.0(8) . . . . ? C80 C79 C85 C87 61.6(10) . . . . ? C78 C79 C85 C87 -121.0(8) . . . . ? C80 C79 C85 C88 179.1(8) . . . . ? C78 C79 C85 C88 -3.6(11) . . . . ? P4 O11 C89 C98 -71.3(7) . . . . ? P4 O11 C89 C90 112.9(6) . . . . ? C98 C89 C90 C91 1.4(11) . . . . ? O11 C89 C90 C91 176.8(6) . . . . ? C89 C90 C91 C92 2.0(11) . . . . ? C90 C91 C92 C97 -0.1(11) . . . . ? C90 C91 C92 C93 178.9(8) . . . . ? C97 C92 C93 C94 2.8(12) . . . . ? C91 C92 C93 C94 -176.3(8) . . . . ? C92 C93 C94 C95 1.9(13) . . . . ? C93 C94 C95 C96 -4.5(13) . . . . ? C94 C95 C96 C97 2.2(12) . . . . ? C93 C92 C97 C96 -5.1(11) . . . . ? C91 C92 C97 C96 174.0(7) . . . . ? C93 C92 C97 C98 176.3(7) . . . . ? C91 C92 C97 C98 -4.7(11) . . . . ? C95 C96 C97 C92 2.7(11) . . . . ? C95 C96 C97 C98 -178.7(7) . . . . ? C90 C89 C98 C97 -6.1(10) . . . . ? O11 C89 C98 C97 178.6(5) . . . . ? C90 C89 C98 C100 174.9(6) . . . . ? O11 C89 C98 C100 -0.4(9) . . . . ? C92 C97 C98 C89 7.5(9) . . . . ? C96 C97 C98 C89 -171.1(7) . . . . ? C92 C97 C98 C100 -173.5(6) . . . . ? C96 C97 C98 C100 7.9(10) . . . . ? P4 O12 C99 C100 -79.6(7) . . . . ? P4 O12 C99 C108 102.6(7) . . . . ? C108 C99 C100 C101 -3.7(12) . . . . ? O12 C99 C100 C101 178.5(6) . . . . ? C108 C99 C100 C98 178.8(7) . . . . ? O12 C99 C100 C98 1.1(11) . . . . ? C89 C98 C100 C99 50.8(10) . . . . ? C97 C98 C100 C99 -128.2(8) . . . . ? C89 C98 C100 C101 -126.5(8) . . . . ? C97 C98 C100 C101 54.5(10) . . . . ? C99 C100 C101 C106 5.5(11) . . . . ? C98 C100 C101 C106 -177.1(7) . . . . ? C99 C100 C101 C102 -173.2(7) . . . . ? C98 C100 C101 C102 4.2(12) . . . . ? C106 C101 C102 C103 2.1(13) . . . . ? C100 C101 C102 C103 -179.2(8) . . . . ? C101 C102 C103 C104 1.7(15) . . . . ? C102 C103 C104 C105 -2.5(15) . . . . ? C103 C104 C105 C106 -0.6(14) . . . . ? C102 C101 C106 C107 175.8(8) . . . . ? C100 C101 C106 C107 -3.0(12) . . . . ? C102 C101 C106 C105 -5.1(12) . . . . ? C100 C101 C106 C105 176.1(7) . . . . ? C104 C105 C106 C101 4.4(12) . . . . ? C104 C105 C106 C107 -176.4(8) . . . . ? C101 C106 C107 C108 -1.7(13) . . . . ? C105 C106 C107 C108 179.2(8) . . . . ? C106 C107 C108 C99 3.6(12) . . . . ? C100 C99 C108 C107 -0.8(12) . . . . ? O12 C99 C108 C107 176.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 70.03 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 1.296 _refine_diff_density_min -1.222 _refine_diff_density_rms 0.109