# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers # This journal is © The Partner Organisations 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1A _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H39 Cl O2 P2 Pd' _chemical_formula_sum 'C22 H39 Cl O2 P2 Pd' _chemical_formula_weight 539.32 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3191(2) _cell_length_b 12.0094(2) _cell_length_c 13.3760(2) _cell_angle_alpha 100.2960(10) _cell_angle_beta 96.1270(10) _cell_angle_gamma 103.9030(10) _cell_volume 1260.55(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8283 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 67.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 8.220 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2068 _exptl_absorpt_correction_T_max 0.5592 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(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 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 10578 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 67.78 _reflns_number_total 4321 _reflns_number_gt 4098 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.634' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0476P)^2^+1.2594P] 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_number_reflns 4321 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.03528(2) 0.733138(16) 0.773479(14) 0.01900(8) Uani 1 1 d . . . Cl1 Cl 0.19717(12) 0.72635(8) 0.92914(7) 0.0473(2) Uani 1 1 d . . . P1 P 0.18536(8) 0.90891(6) 0.74610(5) 0.01851(15) Uani 1 1 d . . . P2 P -0.16525(8) 0.55766(6) 0.74727(5) 0.01791(15) Uani 1 1 d . . . O1 O 0.0819(2) 0.92602(17) 0.63928(15) 0.0241(4) Uani 1 1 d . . . O2 O -0.2893(2) 0.55310(16) 0.64011(14) 0.0228(4) Uani 1 1 d . . . C1 C -0.1019(3) 0.7400(2) 0.6426(2) 0.0183(5) Uani 1 1 d . . . C2 C -0.0597(3) 0.8349(2) 0.5956(2) 0.0205(6) Uani 1 1 d . . . C3 C -0.1532(4) 0.8422(2) 0.5059(2) 0.0236(6) Uani 1 1 d . . . H3 H -0.1225 0.9084 0.4756 0.028 Uiso 1 1 calc R . . C4 C -0.2928(4) 0.7501(3) 0.4617(2) 0.0244(6) Uani 1 1 d . . . H4 H -0.3582 0.7536 0.4002 0.029 Uiso 1 1 calc R . . C5 C -0.3392(3) 0.6530(2) 0.5054(2) 0.0215(6) Uani 1 1 d . . . H5 H -0.4348 0.5902 0.4745 0.026 Uiso 1 1 calc R . . C6 C -0.2421(3) 0.6501(2) 0.5955(2) 0.0191(5) Uani 1 1 d . . . C7 C 0.1833(4) 1.0434(3) 0.8382(2) 0.0257(6) Uani 1 1 d . . . C8 C 0.2681(5) 1.1572(3) 0.8080(3) 0.0371(8) Uani 1 1 d . . . H8A H 0.2478 1.2238 0.8541 0.056 Uiso 1 1 calc R . . H8B H 0.2220 1.1553 0.7369 0.056 Uiso 1 1 calc R . . H8C H 0.3890 1.1656 0.8134 0.056 Uiso 1 1 calc R . . C9 C 0.2661(6) 1.0402(3) 0.9453(3) 0.0454(9) Uani 1 1 d . . . H9A H 0.2440 1.1015 0.9967 0.068 Uiso 1 1 calc R . . H9B H 0.3874 1.0538 0.9467 0.068 Uiso 1 1 calc R . . H9C H 0.2199 0.9633 0.9609 0.068 Uiso 1 1 calc R . . C10 C -0.0016(5) 1.0372(3) 0.8396(3) 0.0468(9) Uani 1 1 d . . . H10A H -0.0119 1.1052 0.8888 0.070 Uiso 1 1 calc R . . H10B H -0.0566 0.9649 0.8602 0.070 Uiso 1 1 calc R . . H10C H -0.0551 1.0374 0.7708 0.070 Uiso 1 1 calc R . . C11 C 0.3926(4) 0.9086(3) 0.7059(2) 0.0277(6) Uani 1 1 d . . . C12 C 0.5234(4) 0.9262(3) 0.8009(3) 0.0416(8) Uani 1 1 d . . . H12A H 0.6260 0.9102 0.7793 0.062 Uiso 1 1 calc R . . H12B H 0.4792 0.8724 0.8446 0.062 Uiso 1 1 calc R . . H12C H 0.5488 1.0073 0.8397 0.062 Uiso 1 1 calc R . . C13 C 0.4514(5) 0.9991(4) 0.6412(3) 0.0448(9) Uani 1 1 d . . . H13A H 0.5545 0.9883 0.6164 0.067 Uiso 1 1 calc R . . H13B H 0.4733 1.0783 0.6834 0.067 Uiso 1 1 calc R . . H13C H 0.3642 0.9885 0.5824 0.067 Uiso 1 1 calc R . . C14 C 0.3660(5) 0.7850(3) 0.6413(3) 0.0468(9) Uani 1 1 d . . . H14A H 0.4721 0.7763 0.6198 0.070 Uiso 1 1 calc R . . H14B H 0.2820 0.7726 0.5804 0.070 Uiso 1 1 calc R . . H14C H 0.3269 0.7270 0.6825 0.070 Uiso 1 1 calc R . . C15 C -0.3174(4) 0.5474(3) 0.8394(2) 0.0247(6) Uani 1 1 d . . . C16 C -0.3618(6) 0.6647(4) 0.8525(4) 0.0670(14) Uani 1 1 d . . . H16A H -0.4436 0.6662 0.9000 0.101 Uiso 1 1 calc R . . H16B H -0.4100 0.6746 0.7856 0.101 Uiso 1 1 calc R . . H16C H -0.2603 0.7286 0.8804 0.101 Uiso 1 1 calc R . . C17 C -0.4792(5) 0.4517(4) 0.7998(3) 0.0550(12) Uani 1 1 d . . . H17A H -0.5633 0.4640 0.8436 0.083 Uiso 1 1 calc R . . H17B H -0.4585 0.3750 0.8012 0.083 Uiso 1 1 calc R . . H17C H -0.5203 0.4543 0.7290 0.083 Uiso 1 1 calc R . . C18 C -0.2324(6) 0.5357(6) 0.9415(3) 0.087(2) Uani 1 1 d . . . H18A H -0.3001 0.5524 0.9950 0.131 Uiso 1 1 calc R . . H18B H -0.1211 0.5916 0.9594 0.131 Uiso 1 1 calc R . . H18C H -0.2207 0.4557 0.9360 0.131 Uiso 1 1 calc R . . C19 C -0.0937(4) 0.4228(2) 0.7108(2) 0.0269(6) Uani 1 1 d . . . C20 C 0.0039(7) 0.4450(4) 0.6223(4) 0.0686(15) Uani 1 1 d . . . H20A H 0.0378 0.3745 0.5942 0.103 Uiso 1 1 calc R . . H20B H 0.1039 0.5109 0.6478 0.103 Uiso 1 1 calc R . . H20C H -0.0675 0.4639 0.5681 0.103 Uiso 1 1 calc R . . C21 C -0.2346(5) 0.3111(3) 0.6714(3) 0.0403(8) Uani 1 1 d . . . H21A H -0.1878 0.2470 0.6427 0.060 Uiso 1 1 calc R . . H21B H -0.3143 0.3236 0.6179 0.060 Uiso 1 1 calc R . . H21C H -0.2924 0.2906 0.7284 0.060 Uiso 1 1 calc R . . C22 C 0.0230(6) 0.4102(4) 0.8013(4) 0.0664(14) Uani 1 1 d . . . H22A H 0.0811 0.3508 0.7778 0.100 Uiso 1 1 calc R . . H22B H -0.0425 0.3862 0.8542 0.100 Uiso 1 1 calc R . . H22C H 0.1055 0.4857 0.8301 0.100 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 Pd 0.01988(13) 0.01790(12) 0.01751(12) 0.00675(8) -0.00166(7) 0.00156(8) Cl1 0.0518(5) 0.0426(5) 0.0397(5) 0.0178(4) -0.0140(4) 0.0005(4) P1 0.0185(3) 0.0175(3) 0.0179(3) 0.0057(3) 0.0000(2) 0.0013(2) P2 0.0196(3) 0.0160(3) 0.0175(3) 0.0057(3) 0.0011(2) 0.0028(2) O1 0.0234(10) 0.0200(10) 0.0252(10) 0.0093(8) -0.0028(8) -0.0016(8) O2 0.0253(10) 0.0185(9) 0.0210(10) 0.0079(8) -0.0010(7) -0.0018(8) C1 0.0169(14) 0.0174(13) 0.0205(13) 0.0056(10) 0.0031(10) 0.0029(10) C2 0.0182(14) 0.0214(14) 0.0204(13) 0.0042(11) 0.0016(10) 0.0031(10) C3 0.0274(16) 0.0209(14) 0.0223(14) 0.0098(11) -0.0005(11) 0.0038(11) C4 0.0255(15) 0.0284(15) 0.0197(14) 0.0108(12) -0.0012(11) 0.0055(12) C5 0.0210(14) 0.0202(14) 0.0201(13) 0.0034(11) -0.0010(10) 0.0016(10) C6 0.0238(15) 0.0174(13) 0.0184(13) 0.0062(10) 0.0056(10) 0.0073(11) C7 0.0314(17) 0.0209(14) 0.0234(15) 0.0038(11) 0.0051(12) 0.0048(12) C8 0.050(2) 0.0209(15) 0.0393(19) 0.0091(13) 0.0094(15) 0.0050(14) C9 0.075(3) 0.0339(19) 0.0233(17) 0.0012(14) -0.0001(16) 0.0141(18) C10 0.038(2) 0.041(2) 0.060(2) -0.0008(18) 0.0188(17) 0.0109(16) C11 0.0200(15) 0.0334(17) 0.0309(16) 0.0099(13) 0.0054(12) 0.0066(12) C12 0.0221(17) 0.053(2) 0.049(2) 0.0184(17) -0.0005(14) 0.0068(14) C13 0.035(2) 0.059(2) 0.052(2) 0.0307(19) 0.0214(16) 0.0145(16) C14 0.040(2) 0.051(2) 0.051(2) -0.0010(18) 0.0156(17) 0.0180(17) C15 0.0260(16) 0.0277(15) 0.0196(14) 0.0054(12) 0.0066(11) 0.0038(12) C16 0.072(3) 0.041(2) 0.102(4) 0.015(2) 0.060(3) 0.024(2) C17 0.044(2) 0.053(2) 0.052(2) -0.0071(19) 0.0279(18) -0.0149(18) C18 0.054(3) 0.187(7) 0.034(2) 0.056(3) 0.0163(19) 0.030(3) C19 0.0283(16) 0.0188(14) 0.0343(16) 0.0048(12) 0.0037(12) 0.0085(11) C20 0.086(4) 0.040(2) 0.098(4) 0.017(2) 0.068(3) 0.027(2) C21 0.043(2) 0.0217(16) 0.052(2) -0.0018(15) 0.0010(16) 0.0094(14) C22 0.073(3) 0.043(2) 0.075(3) -0.010(2) -0.036(2) 0.037(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.011(3) . ? Pd P1 2.2926(7) . ? Pd P2 2.2954(7) . ? Pd Cl1 2.3813(8) . ? P1 O1 1.659(2) . ? P1 C7 1.853(3) . ? P1 C11 1.861(3) . ? P2 O2 1.6588(19) . ? P2 C15 1.857(3) . ? P2 C19 1.860(3) . ? O1 C2 1.390(3) . ? O2 C6 1.394(3) . ? C1 C6 1.385(4) . ? C1 C2 1.389(4) . ? C2 C3 1.387(4) . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C7 C10 1.524(5) . ? C7 C8 1.524(4) . ? C7 C9 1.533(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.529(4) . ? C11 C14 1.530(5) . ? C11 C12 1.531(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C18 1.515(5) . ? C15 C17 1.516(4) . ? C15 C16 1.525(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.520(4) . ? C19 C22 1.521(5) . ? C19 C20 1.532(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C1 Pd P1 80.03(8) . . ? C1 Pd P2 80.13(8) . . ? P1 Pd P2 160.12(3) . . ? C1 Pd Cl1 179.55(8) . . ? P1 Pd Cl1 99.78(3) . . ? P2 Pd Cl1 100.06(3) . . ? O1 P1 C7 101.26(12) . . ? O1 P1 C11 100.64(12) . . ? C7 P1 C11 114.67(14) . . ? O1 P1 Pd 104.72(7) . . ? C7 P1 Pd 117.13(10) . . ? C11 P1 Pd 115.12(10) . . ? O2 P2 C15 100.82(12) . . ? O2 P2 C19 101.25(12) . . ? C15 P2 C19 114.43(14) . . ? O2 P2 Pd 104.57(7) . . ? C15 P2 Pd 116.13(10) . . ? C19 P2 Pd 116.34(10) . . ? C2 O1 P1 114.73(16) . . ? C6 O2 P2 114.71(17) . . ? C6 C1 C2 117.3(2) . . ? C6 C1 Pd 121.36(19) . . ? C2 C1 Pd 121.4(2) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 O1 118.4(2) . . ? C1 C2 O1 119.1(2) . . ? C2 C3 C4 118.2(3) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.2(3) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 122.4(2) . . ? C1 C6 O2 119.2(2) . . ? C5 C6 O2 118.3(2) . . ? C10 C7 C8 109.0(3) . . ? C10 C7 C9 109.5(3) . . ? C8 C7 C9 109.9(3) . . ? C10 C7 P1 105.2(2) . . ? C8 C7 P1 114.1(2) . . ? C9 C7 P1 109.1(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 109.4(3) . . ? C13 C11 C12 110.7(3) . . ? C14 C11 C12 108.7(3) . . ? C13 C11 P1 113.8(2) . . ? C14 C11 P1 104.3(2) . . ? C12 C11 P1 109.6(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C17 112.0(4) . . ? C18 C15 C16 109.5(4) . . ? C17 C15 C16 107.3(3) . . ? C18 C15 P2 109.4(2) . . ? C17 C15 P2 114.1(2) . . ? C16 C15 P2 104.2(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C22 110.8(3) . . ? C21 C19 C20 107.8(3) . . ? C22 C19 C20 109.8(4) . . ? C21 C19 P2 114.5(2) . . ? C22 C19 P2 109.4(2) . . ? C20 C19 P2 104.3(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 C1 Pd P1 O1 0.75(11) . . . . ? P2 Pd P1 O1 4.61(12) . . . . ? Cl1 Pd P1 O1 -178.84(8) . . . . ? C1 Pd P1 C7 111.94(14) . . . . ? P2 Pd P1 C7 115.80(13) . . . . ? Cl1 Pd P1 C7 -67.64(12) . . . . ? C1 Pd P1 C11 -108.76(13) . . . . ? P2 Pd P1 C11 -104.90(13) . . . . ? Cl1 Pd P1 C11 71.65(11) . . . . ? C1 Pd P2 O2 -0.40(10) . . . . ? P1 Pd P2 O2 -4.26(12) . . . . ? Cl1 Pd P2 O2 179.19(8) . . . . ? C1 Pd P2 C15 -110.49(13) . . . . ? P1 Pd P2 C15 -114.35(12) . . . . ? Cl1 Pd P2 C15 69.10(11) . . . . ? C1 Pd P2 C19 110.31(13) . . . . ? P1 Pd P2 C19 106.45(13) . . . . ? Cl1 Pd P2 C19 -70.10(11) . . . . ? C7 P1 O1 C2 -122.71(19) . . . . ? C11 P1 O1 C2 119.2(2) . . . . ? Pd P1 O1 C2 -0.49(19) . . . . ? C15 P2 O2 C6 121.50(19) . . . . ? C19 P2 O2 C6 -120.63(19) . . . . ? Pd P2 O2 C6 0.64(19) . . . . ? P1 Pd C1 C6 178.8(2) . . . . ? P2 Pd C1 C6 0.1(2) . . . . ? Cl1 Pd C1 C6 -116(11) . . . . ? P1 Pd C1 C2 -1.0(2) . . . . ? P2 Pd C1 C2 -179.7(2) . . . . ? Cl1 Pd C1 C2 65(11) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? Pd C1 C2 C3 -179.4(2) . . . . ? C6 C1 C2 O1 -178.8(2) . . . . ? Pd C1 C2 O1 1.1(4) . . . . ? P1 O1 C2 C3 -179.8(2) . . . . ? P1 O1 C2 C1 -0.3(3) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? O1 C2 C3 C4 178.9(3) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? Pd C1 C6 C5 179.7(2) . . . . ? C2 C1 C6 O2 -179.9(2) . . . . ? Pd C1 C6 O2 0.2(3) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C4 C5 C6 O2 179.4(2) . . . . ? P2 O2 C6 C1 -0.6(3) . . . . ? P2 O2 C6 C5 179.9(2) . . . . ? O1 P1 C7 C10 59.4(2) . . . . ? C11 P1 C7 C10 166.8(2) . . . . ? Pd P1 C7 C10 -53.8(2) . . . . ? O1 P1 C7 C8 -59.9(3) . . . . ? C11 P1 C7 C8 47.4(3) . . . . ? Pd P1 C7 C8 -173.1(2) . . . . ? O1 P1 C7 C9 176.7(2) . . . . ? C11 P1 C7 C9 -75.9(3) . . . . ? Pd P1 C7 C9 63.6(3) . . . . ? O1 P1 C11 C13 40.6(3) . . . . ? C7 P1 C11 C13 -67.1(3) . . . . ? Pd P1 C11 C13 152.6(2) . . . . ? O1 P1 C11 C14 -78.6(2) . . . . ? C7 P1 C11 C14 173.7(2) . . . . ? Pd P1 C11 C14 33.4(2) . . . . ? O1 P1 C11 C12 165.1(2) . . . . ? C7 P1 C11 C12 57.4(3) . . . . ? Pd P1 C11 C12 -82.9(2) . . . . ? O2 P2 C15 C18 173.4(3) . . . . ? C19 P2 C15 C18 65.6(4) . . . . ? Pd P2 C15 C18 -74.3(3) . . . . ? O2 P2 C15 C17 47.0(3) . . . . ? C19 P2 C15 C17 -60.7(3) . . . . ? Pd P2 C15 C17 159.3(3) . . . . ? O2 P2 C15 C16 -69.6(3) . . . . ? C19 P2 C15 C16 -177.4(3) . . . . ? Pd P2 C15 C16 42.6(3) . . . . ? O2 P2 C19 C21 -54.5(3) . . . . ? C15 P2 C19 C21 53.0(3) . . . . ? Pd P2 C19 C21 -167.1(2) . . . . ? O2 P2 C19 C22 -179.5(3) . . . . ? C15 P2 C19 C22 -72.0(3) . . . . ? Pd P2 C19 C22 67.9(3) . . . . ? O2 P2 C19 C20 63.0(3) . . . . ? C15 P2 C19 C20 170.5(3) . . . . ? Pd P2 C19 C20 -49.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 67.78 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.578 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.081 _iucr_refine_instructions_details ; TITL 1A in P-1 CELL 1.54178 8.3191 12.0094 13.3760 100.296 96.127 103.903 ZERR 2.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H O P CL PD UNIT 44 78 4 4 2 2 TEMP -123.0 L.S. 5 size 0.28 0.26 0.08 rem colorles plate bond $h conf mpla 6 c1 c2 c3 c4 c5 c6 acta FMAP 2 PLAN 5 WGHT 0.047600 1.259400 FVAR 0.14896 PD 6 0.035283 0.733138 0.773479 11.00000 0.01988 0.01790 = 0.01751 0.00675 -0.00166 0.00156 CL1 5 0.197174 0.726349 0.929142 11.00000 0.05183 0.04256 = 0.03972 0.01783 -0.01403 0.00048 P1 4 0.185364 0.908906 0.746100 11.00000 0.01846 0.01747 = 0.01791 0.00572 0.00005 0.00132 P2 4 -0.165250 0.557658 0.747274 11.00000 0.01964 0.01598 = 0.01753 0.00573 0.00111 0.00278 O1 3 0.081892 0.926017 0.639285 11.00000 0.02342 0.02001 = 0.02519 0.00930 -0.00281 -0.00159 O2 3 -0.289290 0.553096 0.640107 11.00000 0.02530 0.01854 = 0.02101 0.00786 -0.00099 -0.00181 C1 1 -0.101912 0.739971 0.642627 11.00000 0.01686 0.01738 = 0.02046 0.00565 0.00307 0.00287 C2 1 -0.059740 0.834923 0.595631 11.00000 0.01818 0.02139 = 0.02043 0.00420 0.00160 0.00310 C3 1 -0.153226 0.842175 0.505937 11.00000 0.02735 0.02092 = 0.02230 0.00979 -0.00053 0.00378 AFIX 43 H3 2 -0.122488 0.908393 0.475584 11.00000 -1.20000 AFIX 0 C4 1 -0.292839 0.750109 0.461744 11.00000 0.02548 0.02839 = 0.01966 0.01077 -0.00120 0.00551 AFIX 43 H4 2 -0.358182 0.753598 0.400209 11.00000 -1.20000 AFIX 0 C5 1 -0.339189 0.652992 0.505443 11.00000 0.02096 0.02015 = 0.02006 0.00341 -0.00099 0.00155 AFIX 43 H5 2 -0.434792 0.590189 0.474516 11.00000 -1.20000 AFIX 0 C6 1 -0.242126 0.650085 0.595537 11.00000 0.02384 0.01743 = 0.01839 0.00617 0.00559 0.00728 C7 1 0.183274 1.043407 0.838187 11.00000 0.03138 0.02095 = 0.02345 0.00379 0.00513 0.00483 C8 1 0.268082 1.157200 0.807958 11.00000 0.05022 0.02092 = 0.03935 0.00910 0.00941 0.00498 AFIX 137 H8A 2 0.247751 1.223830 0.854084 11.00000 -1.50000 H8B 2 0.222009 1.155321 0.736934 11.00000 -1.50000 H8C 2 0.389005 1.165601 0.813423 11.00000 -1.50000 AFIX 0 C9 1 0.266105 1.040204 0.945270 11.00000 0.07519 0.03389 = 0.02329 0.00123 -0.00010 0.01406 AFIX 137 H9A 2 0.243967 1.101493 0.996718 11.00000 -1.50000 H9B 2 0.387369 1.053804 0.946673 11.00000 -1.50000 H9C 2 0.219935 0.963265 0.960880 11.00000 -1.50000 AFIX 0 C10 1 -0.001577 1.037171 0.839617 11.00000 0.03762 0.04138 = 0.05979 -0.00077 0.01883 0.01091 AFIX 137 H10A 2 -0.011902 1.105175 0.888767 11.00000 -1.50000 H10B 2 -0.056581 0.964891 0.860222 11.00000 -1.50000 H10C 2 -0.055125 1.037436 0.770782 11.00000 -1.50000 AFIX 0 C11 1 0.392610 0.908618 0.705892 11.00000 0.02002 0.03335 = 0.03087 0.00991 0.00541 0.00661 C12 1 0.523429 0.926200 0.800915 11.00000 0.02209 0.05302 = 0.04948 0.01836 -0.00047 0.00682 AFIX 137 H12A 2 0.625986 0.910152 0.779301 11.00000 -1.50000 H12B 2 0.479238 0.872370 0.844560 11.00000 -1.50000 H12C 2 0.548821 1.007337 0.839723 11.00000 -1.50000 AFIX 0 C13 1 0.451419 0.999050 0.641203 11.00000 0.03531 0.05851 = 0.05232 0.03070 0.02140 0.01453 AFIX 137 H13A 2 0.554481 0.988339 0.616379 11.00000 -1.50000 H13B 2 0.473286 1.078295 0.683416 11.00000 -1.50000 H13C 2 0.364179 0.988470 0.582358 11.00000 -1.50000 AFIX 0 C14 1 0.365982 0.785039 0.641336 11.00000 0.03951 0.05056 = 0.05103 -0.00104 0.01560 0.01803 AFIX 137 H14A 2 0.472058 0.776306 0.619826 11.00000 -1.50000 H14B 2 0.281977 0.772645 0.580376 11.00000 -1.50000 H14C 2 0.326852 0.727003 0.682451 11.00000 -1.50000 AFIX 0 C15 1 -0.317447 0.547411 0.839426 11.00000 0.02601 0.02767 = 0.01955 0.00539 0.00662 0.00383 C16 1 -0.361791 0.664668 0.852549 11.00000 0.07243 0.04114 = 0.10240 0.01484 0.05965 0.02367 AFIX 137 H16A 2 -0.443585 0.666227 0.900006 11.00000 -1.50000 H16B 2 -0.410005 0.674554 0.785631 11.00000 -1.50000 H16C 2 -0.260283 0.728586 0.880444 11.00000 -1.50000 AFIX 0 C17 1 -0.479197 0.451722 0.799814 11.00000 0.04350 0.05269 = 0.05188 -0.00713 0.02790 -0.01492 AFIX 137 H17A 2 -0.563336 0.464007 0.843565 11.00000 -1.50000 H17B 2 -0.458462 0.375024 0.801226 11.00000 -1.50000 H17C 2 -0.520335 0.454287 0.729048 11.00000 -1.50000 AFIX 0 C18 1 -0.232354 0.535724 0.941490 11.00000 0.05379 0.18724 = 0.03420 0.05625 0.01632 0.03008 AFIX 137 H18A 2 -0.300144 0.552379 0.995044 11.00000 -1.50000 H18B 2 -0.121134 0.591577 0.959424 11.00000 -1.50000 H18C 2 -0.220732 0.455656 0.936035 11.00000 -1.50000 AFIX 0 C19 1 -0.093734 0.422765 0.710778 11.00000 0.02830 0.01879 = 0.03433 0.00484 0.00368 0.00851 C20 1 0.003905 0.445007 0.622254 11.00000 0.08595 0.04033 = 0.09836 0.01705 0.06793 0.02720 AFIX 137 H20A 2 0.037758 0.374504 0.594227 11.00000 -1.50000 H20B 2 0.103866 0.510851 0.647823 11.00000 -1.50000 H20C 2 -0.067454 0.463891 0.568089 11.00000 -1.50000 AFIX 0 C21 1 -0.234568 0.311068 0.671442 11.00000 0.04288 0.02166 = 0.05166 -0.00180 0.00101 0.00944 AFIX 137 H21A 2 -0.187834 0.247035 0.642677 11.00000 -1.50000 H21B 2 -0.314300 0.323584 0.617903 11.00000 -1.50000 H21C 2 -0.292383 0.290561 0.728383 11.00000 -1.50000 AFIX 0 C22 1 0.022956 0.410245 0.801273 11.00000 0.07310 0.04314 = 0.07463 -0.01005 -0.03579 0.03678 AFIX 137 H22A 2 0.081105 0.350803 0.777805 11.00000 -1.50000 H22B 2 -0.042544 0.386199 0.854158 11.00000 -1.50000 H22C 2 0.105475 0.485667 0.830149 11.00000 -1.50000 HKLF 4 REM 1A in P-1 REM R1 = 0.0284 for 4098 Fo > 4sig(Fo) and 0.0301 for all 4321 data REM 265 parameters refined using 0 restraints END WGHT 0.0476 1.2600 REM Highest difference peak 0.578, deepest hole -0.749, 1-sigma level 0.081 Q1 1 0.0095 0.6856 0.8209 11.00000 0.05 0.58 Q2 1 0.0499 0.7772 0.7241 11.00000 0.05 0.57 Q3 1 -0.1114 0.8028 0.6719 11.00000 0.05 0.57 Q4 1 0.0857 0.6768 0.7833 11.00000 0.05 0.51 Q5 1 -0.2509 0.5516 0.7995 11.00000 0.05 0.42 ; _database_code_depnum_ccdc_archive 'CCDC 965919' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1C _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H39 Cl O2 P2 Pd' _chemical_formula_sum 'C26 H39 Cl O2 P2 Pd' _chemical_formula_weight 587.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0026 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0042 0.0097 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' P P 0.1234 0.1465 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' Cl Cl 0.1675 0.2435 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' Pd Pd -0.8564 1.4848 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 21.578(2) _cell_length_b 21.578(2) _cell_length_c 11.5095(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5358.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 4.16 _cell_measurement_theta_max 33.31 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 1.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9220 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop mount with paratone ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.88560 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'Si-<111> channel cut crystal' _diffrn_measurement_device_type 'Bruker AXS APEXII CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24904 _diffrn_reflns_av_R_equivalents 0.0987 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 33.57 _reflns_number_total 2737 _reflns_number_gt 2608 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 v2010.3.0' _computing_cell_refinement 'Bruker SAINT v7.60A' _computing_data_reduction 'Bruker SAINT v7.60A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0442P)^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 0.37(2) _refine_ls_number_reflns 2737 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.914415(12) 0.2500 0.1250 0.02804(10) Uani 1 2 d S . . Cl1 Cl 0.80429(4) 0.2500 0.1250 0.0371(2) Uani 1 2 d S . . P1 P 0.93238(3) 0.26087(4) 0.31869(7) 0.03126(19) Uani 1 1 d . . . O1 O 1.00842(9) 0.26067(11) 0.33241(17) 0.0347(5) Uani 1 1 d . . . C1 C 1.00655(16) 0.2500 0.1250 0.0299(8) Uani 1 2 d S . . C2 C 1.04037(12) 0.25563(15) 0.2276(2) 0.0297(6) Uani 1 1 d . . . C3 C 1.10489(14) 0.25641(14) 0.2296(3) 0.0314(6) Uani 1 1 d . . . H3 H 1.1268 0.2612 0.3006 0.038 Uiso 1 1 calc R . . C4 C 1.13618(17) 0.2500 0.1250 0.0312(8) Uani 1 2 d S . . H4 H 1.1802 0.2500 0.1250 0.037 Uiso 1 2 calc SR . . C5 C 0.90903(17) 0.20197(16) 0.4215(3) 0.0404(7) Uani 1 1 d . . . H5 H 0.9308 0.2098 0.4968 0.048 Uiso 1 1 calc R . . C6 C 0.83830(17) 0.20239(18) 0.4437(3) 0.0457(8) Uani 1 1 d . . . H6A H 0.8278 0.2296 0.5101 0.055 Uiso 1 1 calc R . . H6B H 0.8156 0.2169 0.3741 0.055 Uiso 1 1 calc R . . C7 C 0.82287(18) 0.1361(2) 0.4705(4) 0.0530(9) Uani 1 1 d . . . H7A H 0.7783 0.1276 0.4578 0.064 Uiso 1 1 calc R . . H7B H 0.8338 0.1254 0.5516 0.064 Uiso 1 1 calc R . . C8 C 0.8624(2) 0.1009(2) 0.3853(5) 0.0687(12) Uani 1 1 d . . . H8A H 0.8426 0.1003 0.3077 0.082 Uiso 1 1 calc R . . H8B H 0.8684 0.0576 0.4116 0.082 Uiso 1 1 calc R . . C9 C 0.92449(18) 0.13523(16) 0.3808(4) 0.0560(9) Uani 1 1 d . . . H9A H 0.9414 0.1354 0.3009 0.067 Uiso 1 1 calc R . . H9B H 0.9551 0.1156 0.4334 0.067 Uiso 1 1 calc R . . C20 C 0.91032(15) 0.33373(14) 0.3835(3) 0.0352(6) Uani 1 1 d . . . H20 H 0.8640 0.3343 0.3882 0.042 Uiso 1 1 calc R . . C24 C 0.9354(2) 0.34633(18) 0.5073(3) 0.0492(9) Uani 1 1 d . . . H24A H 0.9057 0.3314 0.5667 0.059 Uiso 1 1 calc R . . H24B H 0.9756 0.3253 0.5192 0.059 Uiso 1 1 calc R . . C21 C 0.92995(17) 0.39029(17) 0.3123(3) 0.0438(8) Uani 1 1 d . . . H21A H 0.9726 0.3855 0.2820 0.053 Uiso 1 1 calc R . . H21B H 0.9013 0.3976 0.2465 0.053 Uiso 1 1 calc R . . C23 C 0.9429(3) 0.4153(2) 0.5147(5) 0.0877(18) Uani 1 1 d . . . H23A H 0.9156 0.4322 0.5762 0.105 Uiso 1 1 calc R . . H23B H 0.9863 0.4258 0.5344 0.105 Uiso 1 1 calc R . . C22 C 0.9263(3) 0.4426(2) 0.4011(4) 0.0710(13) Uani 1 1 d . . . H22A H 0.9555 0.4762 0.3805 0.085 Uiso 1 1 calc R . . H22B H 0.8838 0.4599 0.4036 0.085 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 Pd 0.02280(15) 0.03929(18) 0.02203(15) -0.00104(13) 0.000 0.000 Cl1 0.0245(4) 0.0487(6) 0.0380(5) -0.0114(6) 0.000 0.000 P1 0.0280(3) 0.0427(5) 0.0232(3) 0.0014(3) 0.0011(3) 0.0012(3) O1 0.0293(10) 0.0535(14) 0.0214(9) -0.0007(9) -0.0014(7) 0.0013(10) C1 0.0227(16) 0.0361(19) 0.031(2) 0.002(2) 0.000 0.000 C2 0.0273(13) 0.0317(15) 0.0301(15) 0.0011(13) 0.0001(10) 0.0014(12) C3 0.0315(14) 0.0290(15) 0.0336(16) 0.0029(13) -0.0054(12) 0.0038(13) C4 0.0255(17) 0.0262(18) 0.042(2) 0.006(2) 0.000 0.000 C5 0.0427(18) 0.0477(19) 0.0306(15) 0.0048(14) 0.0063(15) 0.0024(15) C6 0.0410(19) 0.058(2) 0.0378(19) 0.0058(16) 0.0097(16) -0.0026(15) C7 0.052(2) 0.061(2) 0.045(2) 0.0113(18) -0.0044(18) -0.0138(18) C8 0.079(3) 0.057(2) 0.070(3) -0.002(2) -0.012(3) -0.006(2) C9 0.062(2) 0.0500(19) 0.056(2) 0.007(2) 0.015(2) 0.0090(17) C20 0.0329(14) 0.0445(15) 0.0283(14) -0.0001(15) 0.0040(14) 0.0029(13) C24 0.068(2) 0.054(2) 0.0256(16) -0.0039(15) -0.0060(16) 0.0117(18) C21 0.0441(19) 0.051(2) 0.0363(19) 0.0097(16) 0.0076(15) 0.0016(15) C23 0.149(5) 0.050(3) 0.064(3) -0.006(2) -0.035(3) 0.014(3) C22 0.097(4) 0.059(2) 0.057(3) 0.003(2) -0.007(2) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 1.988(4) . ? Pd P1 2.2748(8) . ? Pd P1 2.2748(8) 14_454 ? Pd Cl1 2.3763(9) . ? P1 O1 1.648(2) . ? P1 C20 1.804(3) . ? P1 C5 1.808(3) . ? O1 C2 1.394(3) . ? C1 C2 1.393(3) . ? C1 C2 1.393(3) 14_454 ? C2 C3 1.392(4) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C3 1.387(3) 14_454 ? C4 H4 0.9500 . ? C5 C6 1.548(5) . ? C5 C9 1.551(5) . ? C5 H5 1.0000 . ? C6 C7 1.501(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.504(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.533(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C20 C21 1.530(4) . ? C20 C24 1.549(5) . ? C20 H20 1.0000 . ? C24 C23 1.499(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C21 C22 1.524(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C23 C22 1.478(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd P1 80.189(19) . . ? C1 Pd P1 80.189(19) . 14_454 ? P1 Pd P1 160.38(4) . 14_454 ? C1 Pd Cl1 180.0 . . ? P1 Pd Cl1 99.811(19) . . ? P1 Pd Cl1 99.811(19) 14_454 . ? O1 P1 C20 103.03(14) . . ? O1 P1 C5 102.29(15) . . ? C20 P1 C5 105.58(16) . . ? O1 P1 Pd 105.26(8) . . ? C20 P1 Pd 116.74(11) . . ? C5 P1 Pd 121.42(13) . . ? C2 O1 P1 114.17(17) . . ? C2 C1 C2 116.8(3) . 14_454 ? C2 C1 Pd 121.59(16) . . ? C2 C1 Pd 121.59(16) 14_454 . ? C3 C2 C1 122.6(3) . . ? C3 C2 O1 118.6(2) . . ? C1 C2 O1 118.8(2) . . ? C4 C3 C2 118.1(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C3 121.7(4) 14_454 . ? C3 C4 H4 119.1 14_454 . ? C3 C4 H4 119.1 . . ? C6 C5 C9 105.5(3) . . ? C6 C5 P1 112.3(2) . . ? C9 C5 P1 113.3(2) . . ? C6 C5 H5 108.5 . . ? C9 C5 H5 108.5 . . ? P1 C5 H5 108.5 . . ? C7 C6 C5 104.3(3) . . ? C7 C6 H6A 110.9 . . ? C5 C6 H6A 110.9 . . ? C7 C6 H6B 110.9 . . ? C5 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C6 C7 C8 102.8(3) . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7B 111.2 . . ? C8 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C7 C8 C9 105.9(4) . . ? C7 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? C7 C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? C8 C9 C5 104.5(3) . . ? C8 C9 H9A 110.9 . . ? C5 C9 H9A 110.9 . . ? C8 C9 H9B 110.9 . . ? C5 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? C21 C20 C24 104.8(3) . . ? C21 C20 P1 113.6(2) . . ? C24 C20 P1 116.2(2) . . ? C21 C20 H20 107.2 . . ? C24 C20 H20 107.2 . . ? P1 C20 H20 107.2 . . ? C23 C24 C20 105.3(3) . . ? C23 C24 H24A 110.7 . . ? C20 C24 H24A 110.7 . . ? C23 C24 H24B 110.7 . . ? C20 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C22 C21 C20 102.5(3) . . ? C22 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? C22 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C22 C23 C24 108.6(4) . . ? C22 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? C23 C22 C21 106.6(4) . . ? C23 C22 H22A 110.4 . . ? C21 C22 H22A 110.4 . . ? C23 C22 H22B 110.4 . . ? C21 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? 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 C1 Pd P1 O1 -0.75(9) . . . . ? P1 Pd P1 O1 -0.75(9) 14_454 . . . ? Cl1 Pd P1 O1 179.25(9) . . . . ? C1 Pd P1 C20 112.77(12) . . . . ? P1 Pd P1 C20 112.77(12) 14_454 . . . ? Cl1 Pd P1 C20 -67.23(12) . . . . ? C1 Pd P1 C5 -115.92(14) . . . . ? P1 Pd P1 C5 -115.92(14) 14_454 . . . ? Cl1 Pd P1 C5 64.08(14) . . . . ? C20 P1 O1 C2 -121.5(2) . . . . ? C5 P1 O1 C2 129.1(2) . . . . ? Pd P1 O1 C2 1.3(2) . . . . ? P1 Pd C1 C2 0.13(16) . . . . ? P1 Pd C1 C2 -179.87(16) 14_454 . . . ? Cl1 Pd C1 C2 0(56) . . . . ? P1 Pd C1 C2 -179.87(16) . . . 14_454 ? P1 Pd C1 C2 0.13(16) 14_454 . . 14_454 ? Cl1 Pd C1 C2 0(64) . . . 14_454 ? C2 C1 C2 C3 0.7(2) 14_454 . . . ? Pd C1 C2 C3 -179.3(2) . . . . ? C2 C1 C2 O1 -179.3(3) 14_454 . . . ? Pd C1 C2 O1 0.7(3) . . . . ? P1 O1 C2 C3 178.6(2) . . . . ? P1 O1 C2 C1 -1.4(3) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? O1 C2 C3 C4 178.6(2) . . . . ? C2 C3 C4 C3 0.7(2) . . . 14_454 ? O1 P1 C5 C6 168.2(3) . . . . ? C20 P1 C5 C6 60.7(3) . . . . ? Pd P1 C5 C6 -75.1(3) . . . . ? O1 P1 C5 C9 -72.4(3) . . . . ? C20 P1 C5 C9 -179.8(3) . . . . ? Pd P1 C5 C9 44.3(3) . . . . ? C9 C5 C6 C7 25.6(4) . . . . ? P1 C5 C6 C7 149.5(3) . . . . ? C5 C6 C7 C8 -40.0(4) . . . . ? C6 C7 C8 C9 39.6(4) . . . . ? C7 C8 C9 C5 -23.2(4) . . . . ? C6 C5 C9 C8 -1.5(4) . . . . ? P1 C5 C9 C8 -124.7(3) . . . . ? O1 P1 C20 C21 69.5(3) . . . . ? C5 P1 C20 C21 176.4(3) . . . . ? Pd P1 C20 C21 -45.3(3) . . . . ? O1 P1 C20 C24 -52.3(3) . . . . ? C5 P1 C20 C24 54.6(3) . . . . ? Pd P1 C20 C24 -167.1(2) . . . . ? C21 C20 C24 C23 22.9(4) . . . . ? P1 C20 C24 C23 149.2(3) . . . . ? C24 C20 C21 C22 -33.8(4) . . . . ? P1 C20 C21 C22 -161.7(3) . . . . ? C20 C24 C23 C22 -2.4(6) . . . . ? C24 C23 C22 C21 -19.1(6) . . . . ? C20 C21 C22 C23 32.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.349 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.067 _iucr_refine_instructions_details ; TITL 1C in I-42d CELL 0.88560 21.5777 21.5777 11.5095 90.000 90.000 90.000 ZERR 8.00 0.0020 0.0020 0.0013 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SYMM 0.5-X, Y, 0.75-Z SYMM 0.5+X, -Y, 0.75-Z SYMM 0.5-Y, -X, 0.75+Z SYMM 0.5+Y, X, 0.75+Z SFAC C H O P CL PD DISP Pd -0.85637 1.48480 7687.51 DISP C -0.00203 0.00263 18.31 DISP O -0.00422 0.00974 56.95 DISP P 0.12339 0.14646 754.71 DISP Cl 0.16750 0.24349 1243.89 UNIT 208 312 16 16 8 8 TEMP -123.000 OMIT 0 0 4 L.S. 5 acta size 0.05 0.04 0.02 rem colorless block, als, apex2 rem H-atoms calculated, riding model bond $h conf mpla 6 c1 c2 c3 c4 c5 c6 FMAP 2 PLAN 5 TWIN WGHT 0.044200 BASF 0.36932 FVAR 0.06959 PD 6 0.914415 0.250000 0.125000 10.50000 0.02280 0.03929 = 0.02203 -0.00104 0.00000 0.00000 CL1 5 0.804286 0.250000 0.125000 10.50000 0.02451 0.04872 = 0.03805 -0.01145 0.00000 0.00000 P1 4 0.932379 0.260873 0.318689 11.00000 0.02797 0.04265 = 0.02316 0.00141 0.00107 0.00121 O1 3 1.008423 0.260674 0.332408 11.00000 0.02931 0.05352 = 0.02142 -0.00072 -0.00145 0.00132 C1 1 1.006550 0.250000 0.125000 10.50000 0.02269 0.03607 = 0.03102 0.00163 0.00000 0.00000 C2 1 1.040366 0.255633 0.227567 11.00000 0.02731 0.03171 = 0.03005 0.00114 0.00006 0.00138 C3 1 1.104885 0.256414 0.229588 11.00000 0.03151 0.02903 = 0.03359 0.00293 -0.00535 0.00379 AFIX 43 H3 2 1.126844 0.261203 0.300564 11.00000 -1.20000 AFIX 0 C4 1 1.136176 0.250000 0.125000 10.50000 0.02546 0.02623 = 0.04200 0.00629 0.00000 0.00000 AFIX 43 H4 2 1.180203 0.250000 0.125000 10.50000 -1.20000 AFIX 0 C5 1 0.909027 0.201974 0.421487 11.00000 0.04270 0.04774 = 0.03064 0.00476 0.00633 0.00235 AFIX 13 H5 2 0.930753 0.209811 0.496813 11.00000 -1.20000 AFIX 0 C6 1 0.838299 0.202392 0.443743 11.00000 0.04098 0.05830 = 0.03780 0.00581 0.00965 -0.00260 AFIX 23 H6A 2 0.827814 0.229609 0.510141 11.00000 -1.20000 H6B 2 0.815562 0.216864 0.374133 11.00000 -1.20000 AFIX 0 C7 1 0.822867 0.136087 0.470468 11.00000 0.05211 0.06137 = 0.04538 0.01128 -0.00437 -0.01383 AFIX 23 H7A 2 0.778282 0.127611 0.457846 11.00000 -1.20000 H7B 2 0.833831 0.125430 0.551567 11.00000 -1.20000 AFIX 0 C8 1 0.862350 0.100911 0.385338 11.00000 0.07944 0.05692 = 0.06972 -0.00187 -0.01172 -0.00620 AFIX 23 H8A 2 0.842643 0.100348 0.307668 11.00000 -1.20000 H8B 2 0.868372 0.057643 0.411629 11.00000 -1.20000 AFIX 0 C9 1 0.924489 0.135225 0.380828 11.00000 0.06222 0.04997 = 0.05576 0.00660 0.01461 0.00904 AFIX 23 H9A 2 0.941401 0.135415 0.300869 11.00000 -1.20000 H9B 2 0.955069 0.115618 0.433370 11.00000 -1.20000 AFIX 0 C20 1 0.910317 0.333727 0.383458 11.00000 0.03290 0.04448 = 0.02830 -0.00008 0.00398 0.00292 AFIX 13 H20 2 0.864045 0.334273 0.388201 11.00000 -1.20000 AFIX 0 C24 1 0.935382 0.346332 0.507320 11.00000 0.06818 0.05382 = 0.02563 -0.00395 -0.00604 0.01171 AFIX 23 H24A 2 0.905743 0.331427 0.566737 11.00000 -1.20000 H24B 2 0.975643 0.325265 0.519225 11.00000 -1.20000 AFIX 0 C21 1 0.929950 0.390293 0.312291 11.00000 0.04415 0.05107 = 0.03628 0.00971 0.00761 0.00163 AFIX 23 H21A 2 0.972614 0.385479 0.281966 11.00000 -1.20000 H21B 2 0.901276 0.397557 0.246538 11.00000 -1.20000 AFIX 0 C23 1 0.942883 0.415289 0.514670 11.00000 0.14888 0.04982 = 0.06433 -0.00641 -0.03457 0.01446 AFIX 23 H23A 2 0.915604 0.432177 0.576159 11.00000 -1.20000 H23B 2 0.986298 0.425754 0.534387 11.00000 -1.20000 AFIX 0 C22 1 0.926261 0.442576 0.401053 11.00000 0.09700 0.05865 = 0.05737 0.00321 -0.00719 -0.01702 AFIX 23 H22A 2 0.955499 0.476189 0.380484 11.00000 -1.20000 H22B 2 0.883819 0.459949 0.403634 11.00000 -1.20000 HKLF 4 REM 1C in I-42d REM R1 = 0.0298 for 2608 Fo > 4sig(Fo) and 0.0313 for all 2737 data REM 148 parameters refined using 0 restraints END WGHT 0.0442 0.0000 REM Highest difference peak 0.349, deepest hole -0.308, 1-sigma level 0.067 Q1 1 0.9650 0.4227 0.4144 11.00000 0.05 0.35 Q2 1 0.9639 0.1383 0.3616 11.00000 0.05 0.22 Q3 1 0.9772 0.1390 0.3973 11.00000 0.05 0.22 Q4 1 1.0320 0.2505 0.4140 11.00000 0.05 0.21 Q5 1 0.9641 0.1406 0.2136 11.00000 0.05 0.21 ; _database_code_depnum_ccdc_archive 'CCDC 965920' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2A _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H40 O2 P2 Pd' _chemical_formula_sum 'C22 H40 O2 P2 Pd' _chemical_formula_weight 504.88 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' 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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4881(2) _cell_length_b 10.60350(10) _cell_length_c 15.7094(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.9270(10) _cell_angle_gamma 90.00 _cell_volume 2490.65(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9913 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 67.62 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 7.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3086 _exptl_absorpt_correction_T_max 0.8674 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(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 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 20794 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 67.99 _reflns_number_total 4482 _reflns_number_gt 4030 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.634' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. Hydride located directly from the difference map and the coordinates refined. All other H-atoms were calculated and treated with a riding model. U~eq~(H)= a*U~eq~(C,Pd) where a=1.5 for methyl and 1.2 for others. ; _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^)+(0.0421P)^2^+1.1632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4482 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.223977(11) 0.967390(15) 0.424553(11) 0.02467(8) Uani 1 1 d . . . H1 H 0.1526(18) 0.878(3) 0.3285(18) 0.030 Uiso 1 1 d . . . P1 P 0.30972(4) 0.81249(6) 0.51876(4) 0.02368(14) Uani 1 1 d . . . P2 P 0.17037(4) 1.16279(6) 0.37351(4) 0.02485(14) Uani 1 1 d . . . O1 O 0.38450(11) 0.88541(15) 0.61299(11) 0.0256(4) Uani 1 1 d . . . O2 O 0.23348(11) 1.26053(15) 0.45885(12) 0.0282(4) Uani 1 1 d . . . C1 C 0.30891(15) 1.0726(2) 0.53435(16) 0.0234(5) Uani 1 1 d . . . C2 C 0.37690(16) 1.0164(2) 0.61098(17) 0.0235(5) Uani 1 1 d . . . C3 C 0.43784(16) 1.0859(2) 0.68592(16) 0.0266(5) Uani 1 1 d . . . H3 H 0.4833 1.0454 0.7382 0.032 Uiso 1 1 calc R . . C4 C 0.42982(16) 1.2163(2) 0.68156(17) 0.0286(5) Uani 1 1 d . . . H4 H 0.4716 1.2657 0.7311 0.034 Uiso 1 1 calc R . . C5 C 0.36213(16) 1.2766(2) 0.60630(17) 0.0280(5) Uani 1 1 d . . . H5 H 0.3568 1.3659 0.6044 0.034 Uiso 1 1 calc R . . C6 C 0.30276(15) 1.2027(2) 0.53430(16) 0.0252(5) Uani 1 1 d . . . C7 C 0.25464(17) 0.7108(3) 0.57547(18) 0.0323(6) Uani 1 1 d . . . C8 C 0.31985(18) 0.6409(3) 0.66229(19) 0.0359(6) Uani 1 1 d . . . H8A H 0.2865 0.5982 0.6929 0.054 Uiso 1 1 calc R . . H8B H 0.3619 0.7012 0.7061 0.054 Uiso 1 1 calc R . . H8C H 0.3530 0.5783 0.6436 0.054 Uiso 1 1 calc R . . C9 C 0.1922(3) 0.6172(4) 0.5037(2) 0.0695(12) Uani 1 1 d . . . H9A H 0.1554 0.5743 0.5302 0.104 Uiso 1 1 calc R . . H9B H 0.2278 0.5547 0.4884 0.104 Uiso 1 1 calc R . . H9C H 0.1534 0.6624 0.4466 0.104 Uiso 1 1 calc R . . C10 C 0.2018(2) 0.8030(3) 0.6074(3) 0.0576(10) Uani 1 1 d . . . H10A H 0.1709 0.7564 0.6388 0.086 Uiso 1 1 calc R . . H10B H 0.1578 0.8473 0.5527 0.086 Uiso 1 1 calc R . . H10C H 0.2428 0.8643 0.6510 0.086 Uiso 1 1 calc R . . C11 C 0.38510(19) 0.7287(2) 0.47681(18) 0.0342(6) Uani 1 1 d . . . C12 C 0.3302(3) 0.6508(4) 0.3902(2) 0.0715(12) Uani 1 1 d . . . H12A H 0.3689 0.6209 0.3612 0.107 Uiso 1 1 calc R . . H12B H 0.2822 0.7030 0.3452 0.107 Uiso 1 1 calc R . . H12C H 0.3042 0.5783 0.4084 0.107 Uiso 1 1 calc R . . C13 C 0.45654(19) 0.6471(3) 0.5509(2) 0.0413(7) Uani 1 1 d . . . H13A H 0.5011 0.6218 0.5282 0.062 Uiso 1 1 calc R . . H13B H 0.4285 0.5718 0.5629 0.062 Uiso 1 1 calc R . . H13C H 0.4858 0.6954 0.6092 0.062 Uiso 1 1 calc R . . C14 C 0.4325(3) 0.8360(3) 0.4500(3) 0.0630(10) Uani 1 1 d . . . H14A H 0.4733 0.8003 0.4256 0.095 Uiso 1 1 calc R . . H14B H 0.4665 0.8874 0.5055 0.095 Uiso 1 1 calc R . . H14C H 0.3879 0.8889 0.4016 0.095 Uiso 1 1 calc R . . C15 C 0.05831(16) 1.1995(2) 0.36849(18) 0.0311(6) Uani 1 1 d . . . C16 C 0.0525(2) 1.1217(3) 0.4481(2) 0.0479(8) Uani 1 1 d . . . H16A H -0.0037 1.1407 0.4525 0.072 Uiso 1 1 calc R . . H16B H 0.1030 1.1431 0.5076 0.072 Uiso 1 1 calc R . . H16C H 0.0547 1.0317 0.4351 0.072 Uiso 1 1 calc R . . C17 C 0.04472(19) 1.3383(3) 0.3847(2) 0.0422(7) Uani 1 1 d . . . H17A H -0.0143 1.3496 0.3846 0.063 Uiso 1 1 calc R . . H17B H 0.0487 1.3893 0.3346 0.063 Uiso 1 1 calc R . . H17C H 0.0911 1.3651 0.4455 0.063 Uiso 1 1 calc R . . C18 C -0.0139(2) 1.1543(3) 0.2738(2) 0.0511(8) Uani 1 1 d . . . H18A H -0.0721 1.1534 0.2766 0.077 Uiso 1 1 calc R . . H18B H 0.0007 1.0690 0.2607 0.077 Uiso 1 1 calc R . . H18C H -0.0162 1.2115 0.2239 0.077 Uiso 1 1 calc R . . C19 C 0.1904(2) 1.2260(3) 0.27362(19) 0.0375(6) Uani 1 1 d . . . C20 C 0.2922(2) 1.2182(4) 0.3076(3) 0.0622(10) Uani 1 1 d . . . H20A H 0.3086 1.2489 0.2580 0.093 Uiso 1 1 calc R . . H20B H 0.3116 1.1304 0.3225 0.093 Uiso 1 1 calc R . . H20C H 0.3214 1.2704 0.3638 0.093 Uiso 1 1 calc R . . C21 C 0.1596(3) 1.3625(3) 0.2476(2) 0.0525(8) Uani 1 1 d . . . H21A H 0.1841 1.3954 0.2051 0.079 Uiso 1 1 calc R . . H21B H 0.1808 1.4141 0.3046 0.079 Uiso 1 1 calc R . . H21C H 0.0941 1.3652 0.2164 0.079 Uiso 1 1 calc R . . C22 C 0.1458(2) 1.1394(3) 0.1880(2) 0.0518(8) Uani 1 1 d . . . H22A H 0.1662 1.1626 0.1398 0.078 Uiso 1 1 calc R . . H22B H 0.0807 1.1488 0.1626 0.078 Uiso 1 1 calc R . . H22C H 0.1621 1.0516 0.2069 0.078 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 Pd 0.02535(11) 0.02010(11) 0.02171(11) -0.00139(6) 0.00322(8) -0.00033(6) P1 0.0244(3) 0.0208(3) 0.0221(3) -0.0010(2) 0.0060(2) 0.0000(2) P2 0.0252(3) 0.0222(3) 0.0229(3) 0.0013(2) 0.0060(2) 0.0005(2) O1 0.0242(8) 0.0237(8) 0.0236(8) -0.0003(7) 0.0049(7) 0.0004(6) O2 0.0268(9) 0.0216(8) 0.0298(9) 0.0004(7) 0.0056(7) 0.0005(7) C1 0.0205(11) 0.0268(12) 0.0209(11) -0.0047(10) 0.0068(9) -0.0024(9) C2 0.0232(12) 0.0236(12) 0.0247(12) -0.0019(9) 0.0112(10) -0.0011(9) C3 0.0234(12) 0.0316(13) 0.0219(12) -0.0021(10) 0.0067(9) -0.0018(10) C4 0.0257(12) 0.0320(13) 0.0256(12) -0.0094(10) 0.0083(10) -0.0069(10) C5 0.0298(13) 0.0230(12) 0.0332(13) -0.0060(10) 0.0151(11) -0.0028(10) C6 0.0205(12) 0.0292(13) 0.0253(12) 0.0002(10) 0.0092(9) 0.0003(9) C7 0.0293(13) 0.0314(14) 0.0317(14) 0.0047(11) 0.0083(11) -0.0053(11) C8 0.0379(15) 0.0327(14) 0.0370(15) 0.0083(11) 0.0157(12) 0.0031(11) C9 0.069(2) 0.070(2) 0.0455(19) 0.0056(17) 0.0007(17) -0.045(2) C10 0.053(2) 0.062(2) 0.079(2) 0.0344(19) 0.0478(19) 0.0229(16) C11 0.0428(15) 0.0312(14) 0.0294(14) -0.0020(11) 0.0159(12) 0.0092(11) C12 0.064(2) 0.083(3) 0.050(2) -0.0332(19) 0.0071(18) 0.024(2) C13 0.0391(16) 0.0423(16) 0.0453(17) 0.0022(13) 0.0206(13) 0.0130(13) C14 0.081(3) 0.055(2) 0.086(3) 0.0220(19) 0.067(2) 0.0219(19) C15 0.0225(12) 0.0291(13) 0.0349(14) 0.0007(11) 0.0056(10) 0.0031(10) C16 0.0397(17) 0.0493(18) 0.064(2) 0.0147(15) 0.0305(15) 0.0081(13) C17 0.0363(16) 0.0345(15) 0.0526(18) -0.0024(13) 0.0156(13) 0.0052(12) C18 0.0307(16) 0.0481(18) 0.056(2) -0.0131(15) 0.0005(14) -0.0011(13) C19 0.0511(17) 0.0357(15) 0.0296(14) 0.0040(11) 0.0209(12) -0.0010(12) C20 0.057(2) 0.087(3) 0.058(2) 0.0087(19) 0.0392(18) -0.0052(19) C21 0.080(2) 0.0387(17) 0.0405(17) 0.0089(13) 0.0271(17) -0.0037(16) C22 0.078(2) 0.0456(18) 0.0331(16) 0.0018(13) 0.0251(16) 0.0080(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 Pd C1 2.036(2) . ? Pd P2 2.2627(6) . ? Pd P1 2.2634(6) . ? Pd H1 1.75(3) . ? P1 O1 1.6645(16) . ? P1 C11 1.860(3) . ? P1 C7 1.861(3) . ? P2 O2 1.6669(17) . ? P2 C15 1.857(3) . ? P2 C19 1.859(3) . ? O1 C2 1.394(3) . ? O2 C6 1.395(3) . ? C1 C6 1.383(3) . ? C1 C2 1.387(3) . ? C2 C3 1.393(3) . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C7 C8 1.526(4) . ? C7 C10 1.527(4) . ? C7 C9 1.529(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.522(4) . ? C11 C13 1.528(4) . ? C11 C14 1.537(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.526(4) . ? C15 C16 1.534(4) . ? C15 C18 1.538(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.531(4) . ? C19 C20 1.535(4) . ? C19 C22 1.536(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C1 Pd P2 79.92(7) . . ? C1 Pd P1 80.02(7) . . ? P2 Pd P1 159.93(2) . . ? C1 Pd H1 178.5(9) . . ? P2 Pd H1 99.7(9) . . ? P1 Pd H1 100.4(9) . . ? O1 P1 C11 100.48(11) . . ? O1 P1 C7 99.87(10) . . ? C11 P1 C7 115.26(12) . . ? O1 P1 Pd 105.59(6) . . ? C11 P1 Pd 116.20(8) . . ? C7 P1 Pd 115.92(9) . . ? O2 P2 C15 100.16(10) . . ? O2 P2 C19 100.49(11) . . ? C15 P2 C19 114.56(13) . . ? O2 P2 Pd 105.43(6) . . ? C15 P2 Pd 116.11(9) . . ? C19 P2 Pd 116.59(9) . . ? C2 O1 P1 114.64(14) . . ? C6 O2 P2 114.84(15) . . ? C6 C1 C2 117.5(2) . . ? C6 C1 Pd 121.46(17) . . ? C2 C1 Pd 121.05(18) . . ? C1 C2 C3 122.5(2) . . ? C1 C2 O1 118.7(2) . . ? C3 C2 O1 118.8(2) . . ? C4 C3 C2 117.7(2) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 121.7(2) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 118.1(2) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C1 C6 C5 122.5(2) . . ? C1 C6 O2 118.2(2) . . ? C5 C6 O2 119.3(2) . . ? C8 C7 C10 107.6(2) . . ? C8 C7 C9 110.2(2) . . ? C10 C7 C9 110.9(3) . . ? C8 C7 P1 114.02(18) . . ? C10 C7 P1 104.31(19) . . ? C9 C7 P1 109.7(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 110.5(3) . . ? C12 C11 C14 109.6(3) . . ? C13 C11 C14 108.1(3) . . ? C12 C11 P1 110.0(2) . . ? C13 C11 P1 114.59(18) . . ? C14 C11 P1 103.69(19) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 108.6(2) . . ? C17 C15 C18 110.8(2) . . ? C16 C15 C18 109.4(3) . . ? C17 C15 P2 114.13(19) . . ? C16 C15 P2 104.78(17) . . ? C18 C15 P2 109.0(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 109.6(3) . . ? C21 C19 C22 110.4(2) . . ? C20 C19 C22 108.7(3) . . ? C21 C19 P2 114.2(2) . . ? C20 C19 P2 104.2(2) . . ? C22 C19 P2 109.5(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 C1 Pd P1 O1 -0.52(9) . . . . ? P2 Pd P1 O1 -1.93(10) . . . . ? C1 Pd P1 C11 -110.87(12) . . . . ? P2 Pd P1 C11 -112.28(12) . . . . ? C1 Pd P1 C7 108.97(12) . . . . ? P2 Pd P1 C7 107.55(11) . . . . ? C1 Pd P2 O2 -1.04(9) . . . . ? P1 Pd P2 O2 0.37(11) . . . . ? C1 Pd P2 C15 -110.86(11) . . . . ? P1 Pd P2 C15 -109.45(11) . . . . ? C1 Pd P2 C19 109.41(13) . . . . ? P1 Pd P2 C19 110.82(12) . . . . ? C11 P1 O1 C2 120.93(16) . . . . ? C7 P1 O1 C2 -120.87(16) . . . . ? Pd P1 O1 C2 -0.25(16) . . . . ? C15 P2 O2 C6 123.90(17) . . . . ? C19 P2 O2 C6 -118.55(18) . . . . ? Pd P2 O2 C6 3.01(17) . . . . ? P2 Pd C1 C6 -1.01(18) . . . . ? P1 Pd C1 C6 179.5(2) . . . . ? P2 Pd C1 C2 -179.1(2) . . . . ? P1 Pd C1 C2 1.36(18) . . . . ? C6 C1 C2 C3 -0.2(4) . . . . ? Pd C1 C2 C3 177.99(18) . . . . ? C6 C1 C2 O1 179.8(2) . . . . ? Pd C1 C2 O1 -2.0(3) . . . . ? P1 O1 C2 C1 1.3(3) . . . . ? P1 O1 C2 C3 -178.62(17) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? O1 C2 C3 C4 178.9(2) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? Pd C1 C6 C5 -177.16(18) . . . . ? C2 C1 C6 O2 -178.5(2) . . . . ? Pd C1 C6 O2 3.3(3) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C4 C5 C6 O2 179.0(2) . . . . ? P2 O2 C6 C1 -4.1(3) . . . . ? P2 O2 C6 C5 176.32(17) . . . . ? O1 P1 C7 C8 -46.7(2) . . . . ? C11 P1 C7 C8 60.0(2) . . . . ? Pd P1 C7 C8 -159.50(17) . . . . ? O1 P1 C7 C10 70.4(2) . . . . ? C11 P1 C7 C10 177.0(2) . . . . ? Pd P1 C7 C10 -42.4(2) . . . . ? O1 P1 C7 C9 -170.7(2) . . . . ? C11 P1 C7 C9 -64.1(3) . . . . ? Pd P1 C7 C9 76.4(2) . . . . ? O1 P1 C11 C12 178.5(2) . . . . ? C7 P1 C11 C12 72.3(3) . . . . ? Pd P1 C11 C12 -68.1(3) . . . . ? O1 P1 C11 C13 53.3(2) . . . . ? C7 P1 C11 C13 -53.0(2) . . . . ? Pd P1 C11 C13 166.60(18) . . . . ? O1 P1 C11 C14 -64.3(2) . . . . ? C7 P1 C11 C14 -170.5(2) . . . . ? Pd P1 C11 C14 49.0(2) . . . . ? O2 P2 C15 C17 36.7(2) . . . . ? C19 P2 C15 C17 -69.9(2) . . . . ? Pd P2 C15 C17 149.59(17) . . . . ? O2 P2 C15 C16 -81.9(2) . . . . ? C19 P2 C15 C16 171.53(19) . . . . ? Pd P2 C15 C16 31.0(2) . . . . ? O2 P2 C15 C18 161.12(19) . . . . ? C19 P2 C15 C18 54.5(2) . . . . ? Pd P2 C15 C18 -86.0(2) . . . . ? O2 P2 C19 C21 -61.9(2) . . . . ? C15 P2 C19 C21 44.5(3) . . . . ? Pd P2 C19 C21 -175.15(19) . . . . ? O2 P2 C19 C20 57.6(2) . . . . ? C15 P2 C19 C20 164.0(2) . . . . ? Pd P2 C19 C20 -55.7(2) . . . . ? O2 P2 C19 C22 173.8(2) . . . . ? C15 P2 C19 C22 -79.9(2) . . . . ? Pd P2 C19 C22 60.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.602 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.071 _iucr_refine_instructions_details ; TITL 2A in P2(1)/c CELL 1.54178 16.4881 10.6035 15.7094 90.000 114.927 90.000 ZERR 4.00 0.0002 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P PD UNIT 88 160 8 8 4 TEMP -123.0 L.S. 5 acta size 0.21 0.02 0.05 rem colorless plate bond $h conf mpla 6 c1 c2 c3 c4 c5 c6 rem hydride located directly, refxyz rem all other H-atoms calculated, riding FMAP 2 PLAN 5 WGHT 0.042100 1.163200 FVAR 0.08623 PD 5 0.223977 0.967390 0.424553 11.00000 0.02535 0.02010 = 0.02171 -0.00139 0.00322 -0.00033 H1 2 0.152584 0.878468 0.328546 11.00000 -1.20000 P1 4 0.309720 0.812487 0.518763 11.00000 0.02437 0.02076 = 0.02208 -0.00099 0.00604 -0.00002 P2 4 0.170372 1.162791 0.373508 11.00000 0.02521 0.02221 = 0.02292 0.00135 0.00605 0.00054 O1 3 0.384498 0.885407 0.612988 11.00000 0.02421 0.02373 = 0.02364 -0.00026 0.00490 0.00041 O2 3 0.233482 1.260534 0.458854 11.00000 0.02681 0.02163 = 0.02977 0.00036 0.00564 0.00047 C1 1 0.308911 1.072613 0.534351 11.00000 0.02047 0.02676 = 0.02090 -0.00467 0.00680 -0.00240 C2 1 0.376895 1.016444 0.610977 11.00000 0.02323 0.02360 = 0.02474 -0.00189 0.01117 -0.00109 C3 1 0.437841 1.085926 0.685919 11.00000 0.02337 0.03162 = 0.02192 -0.00209 0.00671 -0.00176 AFIX 43 H3 2 0.483330 1.045427 0.738216 11.00000 -1.20000 AFIX 0 C4 1 0.429821 1.216332 0.681557 11.00000 0.02571 0.03203 = 0.02560 -0.00944 0.00829 -0.00694 AFIX 43 H4 2 0.471551 1.265700 0.731148 11.00000 -1.20000 AFIX 0 C5 1 0.362130 1.276625 0.606299 11.00000 0.02976 0.02301 = 0.03321 -0.00600 0.01508 -0.00284 AFIX 43 H5 2 0.356824 1.365903 0.604396 11.00000 -1.20000 AFIX 0 C6 1 0.302759 1.202673 0.534301 11.00000 0.02047 0.02918 = 0.02535 0.00021 0.00915 0.00035 C7 1 0.254639 0.710803 0.575472 11.00000 0.02927 0.03138 = 0.03166 0.00472 0.00832 -0.00528 C8 1 0.319851 0.640858 0.662286 11.00000 0.03786 0.03267 = 0.03702 0.00830 0.01568 0.00314 AFIX 137 H8A 2 0.286538 0.598213 0.692913 11.00000 -1.50000 H8B 2 0.361871 0.701175 0.706064 11.00000 -1.50000 H8C 2 0.353010 0.578280 0.643615 11.00000 -1.50000 AFIX 0 C9 1 0.192202 0.617152 0.503741 11.00000 0.06876 0.07028 = 0.04553 0.00562 0.00071 -0.04502 AFIX 137 H9A 2 0.155367 0.574348 0.530200 11.00000 -1.50000 H9B 2 0.227788 0.554664 0.488412 11.00000 -1.50000 H9C 2 0.153432 0.662420 0.446637 11.00000 -1.50000 AFIX 0 C10 1 0.201803 0.802974 0.607359 11.00000 0.05290 0.06150 = 0.07883 0.03435 0.04779 0.02286 AFIX 137 H10A 2 0.170875 0.756447 0.638832 11.00000 -1.50000 H10B 2 0.157787 0.847307 0.552659 11.00000 -1.50000 H10C 2 0.242846 0.864306 0.651045 11.00000 -1.50000 AFIX 0 C11 1 0.385095 0.728701 0.476813 11.00000 0.04280 0.03115 = 0.02935 -0.00200 0.01588 0.00917 C12 1 0.330234 0.650781 0.390186 11.00000 0.06408 0.08345 = 0.04975 -0.03322 0.00713 0.02375 AFIX 137 H12A 2 0.368936 0.620891 0.361179 11.00000 -1.50000 H12B 2 0.282245 0.702968 0.345197 11.00000 -1.50000 H12C 2 0.304187 0.578299 0.408387 11.00000 -1.50000 AFIX 0 C13 1 0.456540 0.647110 0.550927 11.00000 0.03913 0.04229 = 0.04529 0.00224 0.02060 0.01295 AFIX 137 H13A 2 0.501128 0.621818 0.528235 11.00000 -1.50000 H13B 2 0.428517 0.571762 0.562897 11.00000 -1.50000 H13C 2 0.485788 0.695429 0.609175 11.00000 -1.50000 AFIX 0 C14 1 0.432504 0.836035 0.449970 11.00000 0.08124 0.05535 = 0.08563 0.02202 0.06744 0.02187 AFIX 137 H14A 2 0.473333 0.800298 0.425610 11.00000 -1.50000 H14B 2 0.466515 0.887389 0.505539 11.00000 -1.50000 H14C 2 0.387893 0.888860 0.401645 11.00000 -1.50000 AFIX 0 C15 1 0.058310 1.199528 0.368489 11.00000 0.02249 0.02905 = 0.03494 0.00075 0.00558 0.00314 C16 1 0.052532 1.121723 0.448097 11.00000 0.03972 0.04932 = 0.06352 0.01474 0.03050 0.00809 AFIX 137 H16A 2 -0.003738 1.140686 0.452521 11.00000 -1.50000 H16B 2 0.102962 1.143084 0.507551 11.00000 -1.50000 H16C 2 0.054682 1.031703 0.435066 11.00000 -1.50000 AFIX 0 C17 1 0.044720 1.338294 0.384739 11.00000 0.03625 0.03449 = 0.05262 -0.00245 0.01558 0.00517 AFIX 137 H17A 2 -0.014343 1.349609 0.384554 11.00000 -1.50000 H17B 2 0.048721 1.389294 0.334623 11.00000 -1.50000 H17C 2 0.091057 1.365097 0.445477 11.00000 -1.50000 AFIX 0 C18 1 -0.013864 1.154252 0.273849 11.00000 0.03069 0.04806 = 0.05637 -0.01311 0.00052 -0.00112 AFIX 137 H18A 2 -0.072130 1.153403 0.276637 11.00000 -1.50000 H18B 2 0.000722 1.068963 0.260684 11.00000 -1.50000 H18C 2 -0.016169 1.211541 0.223926 11.00000 -1.50000 AFIX 0 C19 1 0.190358 1.226019 0.273624 11.00000 0.05112 0.03574 = 0.02960 0.00398 0.02087 -0.00101 C20 1 0.292186 1.218218 0.307553 11.00000 0.05687 0.08688 = 0.05809 0.00875 0.03920 -0.00521 AFIX 137 H20A 2 0.308552 1.248875 0.258040 11.00000 -1.50000 H20B 2 0.311589 1.130436 0.322458 11.00000 -1.50000 H20C 2 0.321439 1.270361 0.363826 11.00000 -1.50000 AFIX 0 C21 1 0.159563 1.362458 0.247599 11.00000 0.08011 0.03870 = 0.04046 0.00892 0.02709 -0.00370 AFIX 137 H21A 2 0.184123 1.395424 0.205077 11.00000 -1.50000 H21B 2 0.180759 1.414074 0.304629 11.00000 -1.50000 H21C 2 0.094091 1.365229 0.216429 11.00000 -1.50000 AFIX 0 C22 1 0.145816 1.139444 0.187986 11.00000 0.07848 0.04564 = 0.03308 0.00179 0.02514 0.00797 AFIX 137 H22A 2 0.166207 1.162631 0.139822 11.00000 -1.50000 H22B 2 0.080711 1.148838 0.162576 11.00000 -1.50000 H22C 2 0.162112 1.051626 0.206921 11.00000 -1.50000 HKLF 4 REM 2A in P2(1)/c REM R1 = 0.0270 for 4030 Fo > 4sig(Fo) and 0.0308 for all 4482 data REM 259 parameters refined using 0 restraints END WGHT 0.0421 1.1632 REM Highest difference peak 0.602, deepest hole -0.406, 1-sigma level 0.071 Q1 1 0.2208 1.0882 0.4203 11.00000 0.05 0.59 Q2 1 0.1767 0.9234 0.3713 11.00000 0.05 0.53 Q3 1 0.2727 1.0193 0.4848 11.00000 0.05 0.50 Q4 1 0.1772 0.9875 0.4339 11.00000 0.05 0.48 Q5 1 0.3292 0.9665 0.7276 11.00000 0.05 0.42 ; _database_code_depnum_ccdc_archive 'CCDC 965921' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2C _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 O2 P2 Pd' _chemical_formula_sum 'C26 H40 O2 P2 Pd' _chemical_formula_weight 552.92 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' 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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2605(2) _cell_length_b 17.3087(4) _cell_length_c 12.3482(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.8110(10) _cell_angle_gamma 90.00 _cell_volume 2582.13(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9121 _cell_measurement_theta_min 4.44 _cell_measurement_theta_max 67.64 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 7.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4358 _exptl_absorpt_correction_T_max 0.5364 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(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 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 21918 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.44 _diffrn_reflns_theta_max 67.98 _reflns_number_total 4651 _reflns_number_gt 3758 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.634' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The hydride was located directly from the difference map and the coordinates refined. Pd-H1 1.53(4)\%A All remaining H-atoms were calculated and treated with a riding model. Typical disorder is observed for 2 of the cyclopentyl rings; a suitable multi-component model is given. ; _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^)+(0.0477P)^2^+1.2433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4651 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.53289(2) 0.653091(13) 0.166420(19) 0.02296(9) Uani 1 1 d . . . H1 H 0.533(3) 0.565(2) 0.183(3) 0.028 Uiso 1 1 d . . . P1 P 0.47577(7) 0.69344(5) 0.32087(7) 0.02380(19) Uani 1 1 d . . . P2 P 0.59059(7) 0.65689(5) 0.00280(7) 0.02435(19) Uani 1 1 d . . . O1 O 0.47122(19) 0.78964(13) 0.31324(18) 0.0284(5) Uani 1 1 d . . . O2 O 0.6014(2) 0.75042(13) -0.02617(18) 0.0299(5) Uani 1 1 d . . . C1 C 0.5363(3) 0.76925(18) 0.1439(3) 0.0235(7) Uani 1 1 d . . . C2 C 0.5053(3) 0.82055(19) 0.2198(3) 0.0249(7) Uani 1 1 d . . . C3 C 0.5071(3) 0.8996(2) 0.2076(3) 0.0296(8) Uani 1 1 d . . . H3 H 0.4847 0.9330 0.2607 0.036 Uiso 1 1 calc R . . C4 C 0.5430(3) 0.9290(2) 0.1145(3) 0.0329(8) Uani 1 1 d . . . H4 H 0.5458 0.9833 0.1047 0.039 Uiso 1 1 calc R . . C5 C 0.5751(3) 0.8803(2) 0.0353(3) 0.0304(8) Uani 1 1 d . . . H5 H 0.5990 0.9008 -0.0281 0.036 Uiso 1 1 calc R . . C6 C 0.5710(3) 0.80084(19) 0.0517(3) 0.0245(7) Uani 1 1 d . . . C7 C 0.5692(3) 0.6796(2) 0.4513(3) 0.0301(8) Uani 1 1 d . B . H7 H 0.5365 0.7027 0.5127 0.036 Uiso 1 1 calc R . . C8 C 0.5965(3) 0.5927(2) 0.4751(3) 0.0360(9) Uani 1 1 d . . . H8A H 0.5519 0.5709 0.5274 0.043 Uiso 0.50 1 calc PR A 1 H8B H 0.5844 0.5617 0.4067 0.043 Uiso 0.50 1 calc PR A 1 H8C H 0.5893 0.5796 0.5516 0.043 Uiso 0.50 1 calc PR A 2 H8D H 0.5455 0.5595 0.4244 0.043 Uiso 0.50 1 calc PR A 2 C9A C 0.7203(10) 0.5966(7) 0.5260(10) 0.059(3) Uani 0.50 1 d P B 1 H9A H 0.7286 0.6037 0.6065 0.071 Uiso 0.50 1 calc PR B 1 H9B H 0.7574 0.5478 0.5116 0.071 Uiso 0.50 1 calc PR B 1 C10A C 0.7699(13) 0.6595(11) 0.4789(12) 0.062(5) Uani 0.50 1 d P B 1 H10A H 0.8014 0.6418 0.4145 0.075 Uiso 0.50 1 calc PR B 1 H10B H 0.8303 0.6818 0.5333 0.075 Uiso 0.50 1 calc PR B 1 C9B C 0.7149(9) 0.5809(7) 0.4576(12) 0.060(3) Uani 0.50 1 d P B 2 H9C H 0.7606 0.5625 0.5266 0.072 Uiso 0.50 1 calc PR B 2 H9D H 0.7169 0.5411 0.4004 0.072 Uiso 0.50 1 calc PR B 2 C10B C 0.7573(10) 0.6490(10) 0.4258(13) 0.055(4) Uani 0.50 1 d P B 2 H10C H 0.7633 0.6461 0.3469 0.066 Uiso 0.50 1 calc PR B 2 H10D H 0.8326 0.6570 0.4683 0.066 Uiso 0.50 1 calc PR B 2 C11 C 0.6826(3) 0.7182(2) 0.4448(3) 0.0393(9) Uani 1 1 d . . . H11A H 0.6845 0.7357 0.3689 0.047 Uiso 0.50 1 calc PR B 1 H11B H 0.6943 0.7635 0.4943 0.047 Uiso 0.50 1 calc PR B 1 H11C H 0.6758 0.7553 0.3831 0.047 Uiso 0.50 1 calc PR B 2 H11D H 0.7122 0.7454 0.5141 0.047 Uiso 0.50 1 calc PR B 2 C12 C 0.3353(3) 0.6737(2) 0.3429(3) 0.0334(8) Uani 1 1 d . D . H12 H 0.3215 0.7009 0.4108 0.040 Uiso 1 1 calc R . . C13 C 0.3123(3) 0.5860(2) 0.3526(4) 0.0439(10) Uani 1 1 d . D . H13A H 0.3746 0.5553 0.3338 0.053 Uiso 1 1 calc R . . H13B H 0.3026 0.5729 0.4284 0.053 Uiso 1 1 calc R . . C14 C 0.2066(4) 0.5696(3) 0.2717(4) 0.0524(12) Uani 1 1 d . . . H14A H 0.1400 0.5767 0.3061 0.063 Uiso 0.55 1 calc PR C 1 H14B H 0.2065 0.5166 0.2413 0.063 Uiso 0.55 1 calc PR C 1 H14C H 0.1550 0.5383 0.3072 0.063 Uiso 0.45 1 calc PR C 2 H14D H 0.2236 0.5409 0.2073 0.063 Uiso 0.45 1 calc PR C 2 C15A C 0.2135(7) 0.6316(5) 0.1825(6) 0.0485(19) Uani 0.55 1 d P D 1 H15A H 0.2666 0.6157 0.1345 0.058 Uiso 0.55 1 calc PR D 1 H15B H 0.1401 0.6399 0.1365 0.058 Uiso 0.55 1 calc PR D 1 C15B C 0.1543(8) 0.6493(6) 0.2358(8) 0.049(3) Uani 0.45 1 d P D 2 H15C H 0.1128 0.6472 0.1597 0.059 Uiso 0.45 1 calc PR D 2 H15D H 0.1038 0.6664 0.2857 0.059 Uiso 0.45 1 calc PR D 2 C16 C 0.2516(3) 0.7017(3) 0.2434(4) 0.0496(11) Uani 1 1 d . . . H16A H 0.1889 0.7289 0.2677 0.060 Uiso 0.55 1 calc PR D 1 H16B H 0.2874 0.7373 0.1973 0.060 Uiso 0.55 1 calc PR D 1 H16C H 0.2295 0.7558 0.2542 0.060 Uiso 0.45 1 calc PR D 2 H16D H 0.2842 0.6989 0.1754 0.060 Uiso 0.45 1 calc PR D 2 C17 C 0.7253(3) 0.6202(2) -0.0131(3) 0.0351(8) Uani 1 1 d . . . H17 H 0.7427 0.6375 -0.0856 0.042 Uiso 1 1 calc R . . C18 C 0.8195(3) 0.6466(2) 0.0798(4) 0.0469(11) Uani 1 1 d . . . H18A H 0.8767 0.6759 0.0494 0.056 Uiso 1 1 calc R . . H18B H 0.7900 0.6795 0.1337 0.056 Uiso 1 1 calc R . . C19 C 0.8671(4) 0.5716(3) 0.1332(5) 0.0787(17) Uani 1 1 d . . . H19A H 0.9478 0.5766 0.1590 0.094 Uiso 1 1 calc R . . H19B H 0.8312 0.5582 0.1967 0.094 Uiso 1 1 calc R . . C20 C 0.8433(4) 0.5104(3) 0.0443(4) 0.0600(13) Uani 1 1 d . . . H20A H 0.8952 0.5142 -0.0088 0.072 Uiso 1 1 calc R . . H20B H 0.8471 0.4577 0.0760 0.072 Uiso 1 1 calc R . . C21 C 0.7266(3) 0.5311(2) -0.0086(3) 0.0429(10) Uani 1 1 d . . . H21A H 0.6725 0.5118 0.0359 0.051 Uiso 1 1 calc R . . H21B H 0.7086 0.5089 -0.0834 0.051 Uiso 1 1 calc R . . C22 C 0.4959(3) 0.6195(2) -0.1152(3) 0.0273(7) Uani 1 1 d . . . H22 H 0.4917 0.5623 -0.1052 0.033 Uiso 1 1 calc R . . C23 C 0.5221(3) 0.6332(3) -0.2300(3) 0.0404(9) Uani 1 1 d . . . H23A H 0.5740 0.5936 -0.2487 0.049 Uiso 1 1 calc R . . H23B H 0.5553 0.6849 -0.2352 0.049 Uiso 1 1 calc R . . C24 C 0.4106(4) 0.6274(3) -0.3061(3) 0.0526(11) Uani 1 1 d . . . H24A H 0.4004 0.6719 -0.3573 0.063 Uiso 1 1 calc R . . H24B H 0.4069 0.5792 -0.3499 0.063 Uiso 1 1 calc R . . C25 C 0.3218(4) 0.6273(3) -0.2353(3) 0.0521(11) Uani 1 1 d . . . H25A H 0.2890 0.5752 -0.2337 0.063 Uiso 1 1 calc R . . H25B H 0.2624 0.6643 -0.2644 0.063 Uiso 1 1 calc R . . C26 C 0.3780(3) 0.6513(2) -0.1206(3) 0.0315(8) Uani 1 1 d . . . H26A H 0.3411 0.6277 -0.0634 0.038 Uiso 1 1 calc R . . H26B H 0.3785 0.7081 -0.1120 0.038 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 Pd 0.02881(14) 0.01953(14) 0.02102(14) -0.00048(9) 0.00561(9) -0.00014(10) P1 0.0278(4) 0.0209(4) 0.0235(4) -0.0002(3) 0.0066(3) -0.0009(3) P2 0.0257(4) 0.0282(5) 0.0196(4) -0.0005(3) 0.0051(3) 0.0020(4) O1 0.0404(14) 0.0212(12) 0.0251(12) 0.0001(9) 0.0101(10) 0.0016(10) O2 0.0371(13) 0.0302(13) 0.0237(12) 0.0020(10) 0.0090(10) -0.0014(11) C1 0.0219(16) 0.0198(16) 0.0274(17) 0.0024(13) -0.0002(13) -0.0010(13) C2 0.0257(17) 0.0255(17) 0.0225(17) 0.0013(13) 0.0010(13) -0.0004(14) C3 0.0330(19) 0.0266(18) 0.0278(19) 0.0000(14) 0.0010(15) 0.0006(15) C4 0.039(2) 0.0212(18) 0.035(2) 0.0023(15) -0.0027(16) -0.0039(15) C5 0.0328(19) 0.0302(19) 0.0276(19) 0.0078(15) 0.0034(15) -0.0043(15) C6 0.0224(16) 0.0264(18) 0.0229(17) -0.0004(13) -0.0010(13) -0.0031(14) C7 0.038(2) 0.0311(19) 0.0213(17) -0.0004(14) 0.0049(15) -0.0001(16) C8 0.033(2) 0.038(2) 0.037(2) 0.0134(16) 0.0075(16) -0.0014(17) C9A 0.043(6) 0.057(8) 0.072(8) 0.038(7) -0.004(7) 0.004(5) C10A 0.040(6) 0.054(8) 0.080(11) 0.005(8) -0.025(7) 0.005(5) C9B 0.036(5) 0.047(6) 0.101(10) 0.010(7) 0.019(7) 0.006(4) C10B 0.016(5) 0.055(8) 0.092(11) 0.022(9) 0.005(7) -0.010(5) C11 0.038(2) 0.040(2) 0.035(2) 0.0029(17) -0.0053(17) -0.0098(18) C12 0.0294(19) 0.037(2) 0.036(2) 0.0031(16) 0.0096(16) 0.0014(16) C13 0.037(2) 0.040(2) 0.057(3) 0.0076(19) 0.017(2) -0.0072(18) C14 0.059(3) 0.057(3) 0.044(3) -0.014(2) 0.017(2) -0.020(2) C15A 0.051(5) 0.058(5) 0.036(4) -0.003(4) 0.007(4) -0.010(4) C15B 0.031(5) 0.083(8) 0.035(5) 0.002(5) 0.008(4) -0.005(5) C16 0.030(2) 0.058(3) 0.059(3) 0.007(2) 0.0002(19) 0.008(2) C17 0.0266(18) 0.048(2) 0.032(2) 0.0008(17) 0.0062(15) 0.0057(17) C18 0.029(2) 0.053(3) 0.055(3) 0.006(2) -0.0006(18) -0.0017(19) C19 0.061(3) 0.078(4) 0.084(4) 0.020(3) -0.025(3) 0.002(3) C20 0.044(3) 0.058(3) 0.074(3) 0.007(3) 0.000(2) 0.016(2) C21 0.037(2) 0.048(2) 0.044(2) -0.0063(18) 0.0079(18) 0.0154(19) C22 0.0301(18) 0.0263(18) 0.0257(18) -0.0039(14) 0.0051(14) 0.0029(15) C23 0.041(2) 0.057(3) 0.0248(19) -0.0062(17) 0.0083(16) -0.0019(19) C24 0.048(3) 0.078(3) 0.031(2) 0.000(2) 0.0039(19) 0.011(2) C25 0.039(2) 0.081(3) 0.035(2) 0.002(2) 0.0006(18) 0.003(2) C26 0.0282(18) 0.035(2) 0.0317(19) -0.0023(15) 0.0069(15) 0.0032(15) _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 Pd C1 2.031(3) . ? Pd P1 2.2518(8) . ? Pd P2 2.2525(9) . ? Pd H1 1.53(4) . ? P1 O1 1.668(2) . ? P1 C12 1.821(4) . ? P1 C7 1.826(3) . ? P2 O2 1.668(2) . ? P2 C17 1.812(4) . ? P2 C22 1.820(3) . ? O1 C2 1.399(4) . ? O2 C6 1.396(4) . ? C1 C2 1.390(5) . ? C1 C6 1.393(5) . ? C2 C3 1.377(5) . ? C3 C4 1.395(5) . ? C3 H3 0.9500 . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C7 C11 1.556(5) . ? C7 C8 1.558(5) . ? C7 H7 1.0000 . ? C8 C9B 1.516(11) . ? C8 C9A 1.542(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C8 H8D 0.9900 . ? C9A C10A 1.42(2) . ? C9A H9A 0.9900 . ? C9A H9B 0.9900 . ? C10A C11 1.484(18) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C9B C10B 1.37(2) . ? C9B H9C 0.9900 . ? C9B H9D 0.9900 . ? C10B C11 1.550(17) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 H11C 0.9900 . ? C11 H11D 0.9900 . ? C12 C16 1.539(5) . ? C12 C13 1.552(5) . ? C12 H12 1.0000 . ? C13 C14 1.523(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15A 1.551(9) . ? C14 C15B 1.554(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15A C16 1.462(9) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C15B C16 1.489(10) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 H16C 0.9900 . ? C16 H16D 0.9900 . ? C17 C21 1.542(5) . ? C17 C18 1.552(5) . ? C17 H17 1.0000 . ? C18 C19 1.526(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.518(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.511(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.524(5) . ? C22 C26 1.537(5) . ? C22 H22 1.0000 . ? C23 C24 1.525(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.508(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.523(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd P1 79.95(10) . . ? C1 Pd P2 80.29(10) . . ? P1 Pd P2 160.25(3) . . ? C1 Pd H1 178.8(12) . . ? P1 Pd H1 100.9(12) . . ? P2 Pd H1 98.9(12) . . ? O1 P1 C12 99.91(15) . . ? O1 P1 C7 101.00(14) . . ? C12 P1 C7 108.11(17) . . ? O1 P1 Pd 105.90(8) . . ? C12 P1 Pd 120.46(13) . . ? C7 P1 Pd 117.86(12) . . ? O2 P2 C17 102.10(16) . . ? O2 P2 C22 103.67(14) . . ? C17 P2 C22 104.93(16) . . ? O2 P2 Pd 105.62(9) . . ? C17 P2 Pd 121.25(13) . . ? C22 P2 Pd 116.92(11) . . ? C2 O1 P1 114.6(2) . . ? C6 O2 P2 114.7(2) . . ? C2 C1 C6 117.2(3) . . ? C2 C1 Pd 121.7(2) . . ? C6 C1 Pd 121.1(2) . . ? C3 C2 C1 123.4(3) . . ? C3 C2 O1 118.9(3) . . ? C1 C2 O1 117.8(3) . . ? C2 C3 C4 117.7(3) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 118.2(3) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C1 122.1(3) . . ? C5 C6 O2 119.7(3) . . ? C1 C6 O2 118.2(3) . . ? C11 C7 C8 105.0(3) . . ? C11 C7 P1 109.3(2) . . ? C8 C7 P1 112.1(2) . . ? C11 C7 H7 110.1 . . ? C8 C7 H7 110.1 . . ? P1 C7 H7 110.1 . . ? C9B C8 C7 106.5(5) . . ? C9A C8 C7 101.5(5) . . ? C9B C8 H8A 133.7 . . ? C9A C8 H8A 111.5 . . ? C7 C8 H8A 111.5 . . ? C9A C8 H8B 111.5 . . ? C7 C8 H8B 111.5 . . ? H8A C8 H8B 109.3 . . ? C9B C8 H8C 110.4 . . ? C7 C8 H8C 110.4 . . ? H8B C8 H8C 131.7 . . ? C9B C8 H8D 110.4 . . ? C9A C8 H8D 139.1 . . ? C7 C8 H8D 110.4 . . ? C10A C9A C8 109.1(9) . . ? C10A C9A H9A 109.9 . . ? C8 C9A H9A 109.9 . . ? C10A C9A H9B 109.9 . . ? C8 C9A H9B 109.9 . . ? H9A C9A H9B 108.3 . . ? C9A C10A C11 107.6(12) . . ? C9A C10A H10A 110.2 . . ? C11 C10A H10A 110.2 . . ? C9A C10A H10B 110.2 . . ? C11 C10A H10B 110.2 . . ? H10A C10A H10B 108.5 . . ? C10B C9B C8 110.1(10) . . ? C10B C9B H9C 109.6 . . ? C8 C9B H9C 109.6 . . ? C10B C9B H9D 109.6 . . ? C8 C9B H9D 109.6 . . ? H9C C9B H9D 108.1 . . ? C9B C10B C11 110.9(10) . . ? C9B C10B H10C 109.5 . . ? C11 C10B H10C 109.5 . . ? C9B C10B H10D 109.5 . . ? C11 C10B H10D 109.5 . . ? H10C C10B H10D 108.0 . . ? C10A C11 C7 107.4(7) . . ? C10B C11 C7 103.4(5) . . ? C10A C11 H11A 110.2 . . ? C7 C11 H11A 110.2 . . ? C10A C11 H11B 110.2 . . ? C10B C11 H11B 132.7 . . ? C7 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C10A C11 H11C 128.7 . . ? C10B C11 H11C 111.1 . . ? C7 C11 H11C 111.1 . . ? C10B C11 H11D 111.1 . . ? C7 C11 H11D 111.1 . . ? H11A C11 H11D 127.5 . . ? H11C C11 H11D 109.0 . . ? C16 C12 C13 105.4(3) . . ? C16 C12 P1 109.9(3) . . ? C13 C12 P1 112.5(3) . . ? C16 C12 H12 109.7 . . ? C13 C12 H12 109.7 . . ? P1 C12 H12 109.7 . . ? C14 C13 C12 106.1(3) . . ? C14 C13 H13A 110.5 . . ? C12 C13 H13A 110.5 . . ? C14 C13 H13B 110.5 . . ? C12 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C15A 101.1(4) . . ? C13 C14 C15B 106.5(5) . . ? C13 C14 H14A 111.6 . . ? C15A C14 H14A 111.6 . . ? C13 C14 H14B 111.6 . . ? C15A C14 H14B 111.6 . . ? C15B C14 H14B 137.7 . . ? H14A C14 H14B 109.4 . . ? C13 C14 H14C 110.4 . . ? C15A C14 H14C 144.1 . . ? C15B C14 H14C 110.4 . . ? C13 C14 H14D 110.4 . . ? C15B C14 H14D 110.4 . . ? H14A C14 H14D 135.2 . . ? H14C C14 H14D 108.6 . . ? C16 C15A C14 105.1(5) . . ? C16 C15A H15A 110.7 . . ? C14 C15A H15A 110.7 . . ? C16 C15A H15B 110.7 . . ? C14 C15A H15B 110.7 . . ? H15A C15A H15B 108.8 . . ? C16 C15B C14 103.7(6) . . ? C16 C15B H15C 111.0 . . ? C14 C15B H15C 111.0 . . ? C16 C15B H15D 111.0 . . ? C14 C15B H15D 111.0 . . ? H15C C15B H15D 109.0 . . ? C15A C16 C12 105.1(5) . . ? C15B C16 C12 106.0(5) . . ? C15A C16 H16A 110.7 . . ? C12 C16 H16A 110.7 . . ? C15A C16 H16B 110.7 . . ? C15B C16 H16B 140.5 . . ? C12 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? C15A C16 H16C 141.7 . . ? C15B C16 H16C 110.5 . . ? C12 C16 H16C 110.5 . . ? C15B C16 H16D 110.5 . . ? C12 C16 H16D 110.5 . . ? H16A C16 H16D 136.6 . . ? H16C C16 H16D 108.7 . . ? C21 C17 C18 105.4(3) . . ? C21 C17 P2 110.5(3) . . ? C18 C17 P2 113.2(3) . . ? C21 C17 H17 109.2 . . ? C18 C17 H17 109.2 . . ? P2 C17 H17 109.2 . . ? C19 C18 C17 104.5(4) . . ? C19 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? C19 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? C20 C19 C18 105.6(4) . . ? C20 C19 H19A 110.6 . . ? C18 C19 H19A 110.6 . . ? C20 C19 H19B 110.6 . . ? C18 C19 H19B 110.6 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 101.4(4) . . ? C21 C20 H20A 111.5 . . ? C19 C20 H20A 111.5 . . ? C21 C20 H20B 111.5 . . ? C19 C20 H20B 111.5 . . ? H20A C20 H20B 109.3 . . ? C20 C21 C17 104.8(3) . . ? C20 C21 H21A 110.8 . . ? C17 C21 H21A 110.8 . . ? C20 C21 H21B 110.8 . . ? C17 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? C23 C22 C26 104.5(3) . . ? C23 C22 P2 118.8(3) . . ? C26 C22 P2 112.0(2) . . ? C23 C22 H22 107.0 . . ? C26 C22 H22 107.0 . . ? P2 C22 H22 107.0 . . ? C22 C23 C24 104.7(3) . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C25 C24 C23 107.6(3) . . ? C25 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? C25 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? C24 C25 C26 106.4(3) . . ? C24 C25 H25A 110.4 . . ? C26 C25 H25A 110.4 . . ? C24 C25 H25B 110.4 . . ? C26 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C25 C26 C22 102.5(3) . . ? C25 C26 H26A 111.3 . . ? C22 C26 H26A 111.3 . . ? C25 C26 H26B 111.3 . . ? C22 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? 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 C1 Pd P1 O1 1.31(13) . . . . ? P2 Pd P1 O1 0.55(15) . . . . ? C1 Pd P1 C12 113.34(17) . . . . ? P2 Pd P1 C12 112.58(16) . . . . ? C1 Pd P1 C7 -110.71(16) . . . . ? P2 Pd P1 C7 -111.47(16) . . . . ? C1 Pd P2 O2 1.66(13) . . . . ? P1 Pd P2 O2 2.42(15) . . . . ? C1 Pd P2 C17 116.76(18) . . . . ? P1 Pd P2 C17 117.51(18) . . . . ? C1 Pd P2 C22 -113.00(16) . . . . ? P1 Pd P2 C22 -112.24(15) . . . . ? C12 P1 O1 C2 -127.6(2) . . . . ? C7 P1 O1 C2 121.6(2) . . . . ? Pd P1 O1 C2 -1.8(2) . . . . ? C17 P2 O2 C6 -129.3(2) . . . . ? C22 P2 O2 C6 121.9(2) . . . . ? Pd P2 O2 C6 -1.6(2) . . . . ? P1 Pd C1 C2 -0.8(2) . . . . ? P2 Pd C1 C2 178.9(3) . . . . ? P1 Pd C1 C6 178.5(3) . . . . ? P2 Pd C1 C6 -1.8(2) . . . . ? C6 C1 C2 C3 0.3(5) . . . . ? Pd C1 C2 C3 179.7(3) . . . . ? C6 C1 C2 O1 -179.4(3) . . . . ? Pd C1 C2 O1 -0.1(4) . . . . ? P1 O1 C2 C3 -178.4(2) . . . . ? P1 O1 C2 C1 1.4(4) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? O1 C2 C3 C4 179.1(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C4 C5 C6 C1 0.0(5) . . . . ? C4 C5 C6 O2 179.4(3) . . . . ? C2 C1 C6 C5 0.1(5) . . . . ? Pd C1 C6 C5 -179.3(2) . . . . ? C2 C1 C6 O2 -179.4(3) . . . . ? Pd C1 C6 O2 1.3(4) . . . . ? P2 O2 C6 C5 -179.0(2) . . . . ? P2 O2 C6 C1 0.4(4) . . . . ? O1 P1 C7 C11 -59.3(3) . . . . ? C12 P1 C7 C11 -163.7(2) . . . . ? Pd P1 C7 C11 55.4(3) . . . . ? O1 P1 C7 C8 -175.3(2) . . . . ? C12 P1 C7 C8 80.4(3) . . . . ? Pd P1 C7 C8 -60.5(3) . . . . ? C11 C7 C8 C9B -11.7(7) . . . . ? P1 C7 C8 C9B 106.8(6) . . . . ? C11 C7 C8 C9A 22.4(6) . . . . ? P1 C7 C8 C9A 140.9(5) . . . . ? C9B C8 C9A C10A 71.0(14) . . . . ? C7 C8 C9A C10A -31.5(12) . . . . ? C8 C9A C10A C11 27.8(14) . . . . ? C9A C8 C9B C10B -86.8(16) . . . . ? C7 C8 C9B C10B -0.8(13) . . . . ? C8 C9B C10B C11 13.5(15) . . . . ? C9A C10A C11 C10B -97(3) . . . . ? C9A C10A C11 C7 -12.0(12) . . . . ? C9B C10B C11 C10A 82(3) . . . . ? C9B C10B C11 C7 -20.4(13) . . . . ? C8 C7 C11 C10A -7.7(7) . . . . ? P1 C7 C11 C10A -128.0(7) . . . . ? C8 C7 C11 C10B 18.5(7) . . . . ? P1 C7 C11 C10B -101.9(6) . . . . ? O1 P1 C12 C16 62.4(3) . . . . ? C7 P1 C12 C16 167.5(3) . . . . ? Pd P1 C12 C16 -52.8(3) . . . . ? O1 P1 C12 C13 179.4(3) . . . . ? C7 P1 C12 C13 -75.4(3) . . . . ? Pd P1 C12 C13 64.3(3) . . . . ? C16 C12 C13 C14 -8.7(4) . . . . ? P1 C12 C13 C14 -128.5(3) . . . . ? C12 C13 C14 C15A 29.8(5) . . . . ? C12 C13 C14 C15B -12.7(5) . . . . ? C13 C14 C15A C16 -42.0(6) . . . . ? C15B C14 C15A C16 60.5(7) . . . . ? C13 C14 C15B C16 30.1(7) . . . . ? C15A C14 C15B C16 -58.1(6) . . . . ? C14 C15A C16 C15B -60.5(7) . . . . ? C14 C15A C16 C12 37.1(6) . . . . ? C14 C15B C16 C15A 59.6(7) . . . . ? C14 C15B C16 C12 -35.6(7) . . . . ? C13 C12 C16 C15A -17.6(5) . . . . ? P1 C12 C16 C15A 103.8(4) . . . . ? C13 C12 C16 C15B 28.0(6) . . . . ? P1 C12 C16 C15B 149.5(5) . . . . ? O2 P2 C17 C21 -170.6(2) . . . . ? C22 P2 C17 C21 -62.7(3) . . . . ? Pd P2 C17 C21 72.5(3) . . . . ? O2 P2 C17 C18 71.4(3) . . . . ? C22 P2 C17 C18 179.3(3) . . . . ? Pd P2 C17 C18 -45.4(3) . . . . ? C21 C17 C18 C19 -1.1(5) . . . . ? P2 C17 C18 C19 119.7(4) . . . . ? C17 C18 C19 C20 26.4(5) . . . . ? C18 C19 C20 C21 -41.6(5) . . . . ? C19 C20 C21 C17 40.3(5) . . . . ? C18 C17 C21 C20 -24.5(4) . . . . ? P2 C17 C21 C20 -147.1(3) . . . . ? O2 P2 C22 C23 53.9(3) . . . . ? C17 P2 C22 C23 -52.8(3) . . . . ? Pd P2 C22 C23 169.7(2) . . . . ? O2 P2 C22 C26 -68.1(3) . . . . ? C17 P2 C22 C26 -174.8(3) . . . . ? Pd P2 C22 C26 47.6(3) . . . . ? C26 C22 C23 C24 -30.8(4) . . . . ? P2 C22 C23 C24 -156.5(3) . . . . ? C22 C23 C24 C25 11.4(5) . . . . ? C23 C24 C25 C26 12.5(5) . . . . ? C24 C25 C26 C22 -31.1(4) . . . . ? C23 C22 C26 C25 38.2(4) . . . . ? P2 C22 C26 C25 168.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 67.98 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.638 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.084 _iucr_refine_instructions_details ; TITL 2C in P2(1)/n CELL 1.54178 12.2605 17.3087 12.3482 90.000 99.811 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O P PD UNIT 104 160 8 8 4 TEMP -123 L.S. 5 size 0.14 0.13 0.10 rem colorless irregular block rem hydride located directly, refxyz conf mpla 6 c1 c2 c3 c4 c5 c6 acta FMAP 2 PLAN 5 bond $h WGHT 0.047700 1.243300 FVAR 0.09019 PD 5 0.532890 0.653091 0.166420 11.00000 0.02881 0.01953 = 0.02102 -0.00048 0.00561 -0.00014 H1 2 0.532784 0.565424 0.182747 11.00000 -1.20000 P1 4 0.475769 0.693441 0.320871 11.00000 0.02780 0.02090 = 0.02351 -0.00023 0.00664 -0.00088 P2 4 0.590586 0.656886 0.002798 11.00000 0.02570 0.02817 = 0.01964 -0.00050 0.00513 0.00197 O1 3 0.471218 0.789643 0.313237 11.00000 0.04044 0.02122 = 0.02509 0.00010 0.01010 0.00159 O2 3 0.601436 0.750420 -0.026169 11.00000 0.03710 0.03022 = 0.02365 0.00200 0.00899 -0.00143 C1 1 0.536283 0.769254 0.143892 11.00000 0.02193 0.01977 = 0.02740 0.00245 -0.00018 -0.00103 C2 1 0.505341 0.820547 0.219759 11.00000 0.02572 0.02554 = 0.02251 0.00130 0.00105 -0.00040 C3 1 0.507118 0.899601 0.207558 11.00000 0.03296 0.02662 = 0.02775 0.00000 0.00096 0.00060 AFIX 43 H3 2 0.484653 0.932994 0.260720 11.00000 -1.20000 AFIX 0 C4 1 0.543040 0.928977 0.114451 11.00000 0.03942 0.02119 = 0.03488 0.00234 -0.00269 -0.00388 AFIX 43 H4 2 0.545775 0.983342 0.104685 11.00000 -1.20000 AFIX 0 C5 1 0.575079 0.880283 0.035254 11.00000 0.03278 0.03021 = 0.02764 0.00784 0.00339 -0.00433 AFIX 43 H5 2 0.598989 0.900815 -0.028105 11.00000 -1.20000 AFIX 0 C6 1 0.570999 0.800844 0.051748 11.00000 0.02241 0.02645 = 0.02292 -0.00042 -0.00095 -0.00307 C7 1 0.569198 0.679594 0.451279 11.00000 0.03781 0.03108 = 0.02127 -0.00041 0.00493 -0.00013 AFIX 13 H7 2 0.536495 0.702697 0.512723 11.00000 -1.20000 AFIX 0 C8 1 0.596549 0.592718 0.475063 11.00000 0.03303 0.03843 = 0.03711 0.01342 0.00752 -0.00144 part 1 10.5 AFIX 23 H8A 2 0.551900 0.570907 0.527382 10.50000 -1.20000 H8B 2 0.584413 0.561730 0.406677 10.50000 -1.20000 AFIX 23 part 2 10.5 H8C 2 0.589256 0.579637 0.551551 10.50000 -1.20000 H8D 2 0.545501 0.559490 0.424427 10.50000 -1.20000 AFIX 0 part 0 PART 1 C9A 1 0.720347 0.596631 0.525979 10.50000 0.04313 0.05698 = 0.07225 0.03835 -0.00381 0.00403 AFIX 23 H9A 2 0.728576 0.603691 0.606523 10.50000 -1.20000 H9B 2 0.757432 0.547791 0.511646 10.50000 -1.20000 AFIX 0 C10A 1 0.769905 0.659455 0.478917 10.50000 0.03959 0.05448 = 0.08027 0.00534 -0.02480 0.00469 AFIX 23 H10A 2 0.801372 0.641763 0.414491 10.50000 -1.20000 H10B 2 0.830334 0.681804 0.533310 10.50000 -1.20000 AFIX 0 PART 2 C9B 1 0.714855 0.580932 0.457589 10.50000 0.03569 0.04670 = 0.10060 0.00980 0.01928 0.00604 AFIX 23 H9C 2 0.760595 0.562521 0.526639 10.50000 -1.20000 H9D 2 0.716868 0.541148 0.400362 10.50000 -1.20000 AFIX 0 C10B 1 0.757317 0.648975 0.425786 10.50000 0.01628 0.05489 = 0.09164 0.02180 0.00517 -0.00963 AFIX 23 H10C 2 0.763276 0.646070 0.346937 10.50000 -1.20000 H10D 2 0.832550 0.656968 0.468253 10.50000 -1.20000 AFIX 0 PART 0 C11 1 0.682577 0.718174 0.444842 11.00000 0.03839 0.04016 = 0.03524 0.00286 -0.00527 -0.00983 part 1 10.5 AFIX 23 H11A 2 0.684522 0.735705 0.368880 10.50000 -1.20000 H11B 2 0.694322 0.763515 0.494333 10.50000 -1.20000 AFIX 23 part 2 10.5 H11C 2 0.675794 0.755345 0.383121 10.50000 -1.20000 H11D 2 0.712212 0.745400 0.514127 10.50000 -1.20000 AFIX 0 part 0 C12 1 0.335262 0.673730 0.342905 11.00000 0.02943 0.03664 = 0.03558 0.00311 0.00961 0.00140 AFIX 13 H12 2 0.321478 0.700877 0.410776 11.00000 -1.20000 AFIX 0 C13 1 0.312334 0.586033 0.352578 11.00000 0.03708 0.04040 = 0.05716 0.00755 0.01651 -0.00721 AFIX 23 H13A 2 0.374610 0.555308 0.333780 11.00000 -1.20000 H13B 2 0.302586 0.572880 0.428368 11.00000 -1.20000 AFIX 0 C14 1 0.206572 0.569555 0.271722 11.00000 0.05931 0.05651 = 0.04438 -0.01355 0.01700 -0.02045 part 1 10.55 AFIX 23 H14A 2 0.140005 0.576716 0.306127 10.55000 -1.20000 H14B 2 0.206536 0.516633 0.241304 10.55000 -1.20000 AFIX 23 part 2 10.45 H14C 2 0.154999 0.538252 0.307230 10.45000 -1.20000 H14D 2 0.223554 0.540871 0.207251 10.45000 -1.20000 AFIX 0 part 0 PART 1 10.55 C15A 1 0.213533 0.631573 0.182493 10.55000 0.05115 0.05784 = 0.03648 -0.00302 0.00725 -0.00982 AFIX 23 H15A 2 0.266555 0.615679 0.134539 10.55000 -1.20000 H15B 2 0.140099 0.639886 0.136451 10.55000 -1.20000 AFIX 0 PART 2 10.45 C15B 1 0.154295 0.649301 0.235810 10.45000 0.03064 0.08286 = 0.03521 0.00186 0.00813 -0.00548 AFIX 23 H15C 2 0.112766 0.647216 0.159730 10.45000 -1.20000 H15D 2 0.103754 0.666356 0.285664 10.45000 -1.20000 AFIX 0 PART 0 C16 1 0.251590 0.701745 0.243382 11.00000 0.02980 0.05750 = 0.05887 0.00671 0.00023 0.00840 part 1 10.55 AFIX 23 H16A 2 0.188910 0.728911 0.267664 10.55000 -1.20000 H16B 2 0.287424 0.737258 0.197286 10.55000 -1.20000 AFIX 23 part 2 10.45 H16C 2 0.229530 0.755845 0.254183 10.45000 -1.20000 H16D 2 0.284163 0.698876 0.175436 10.45000 -1.20000 AFIX 0 part 0 C17 1 0.725335 0.620177 -0.013139 11.00000 0.02657 0.04756 = 0.03153 0.00076 0.00622 0.00570 AFIX 13 H17 2 0.742676 0.637463 -0.085593 11.00000 -1.20000 AFIX 0 C18 1 0.819502 0.646563 0.079834 11.00000 0.02944 0.05320 = 0.05536 0.00598 -0.00058 -0.00172 AFIX 23 H18A 2 0.876711 0.675854 0.049399 11.00000 -1.20000 H18B 2 0.790018 0.679486 0.133718 11.00000 -1.20000 AFIX 0 C19 1 0.867121 0.571595 0.133217 11.00000 0.06109 0.07837 = 0.08365 0.02001 -0.02459 0.00211 AFIX 23 H19A 2 0.947805 0.576609 0.158996 11.00000 -1.20000 H19B 2 0.831157 0.558179 0.196674 11.00000 -1.20000 AFIX 0 C20 1 0.843310 0.510373 0.044267 11.00000 0.04433 0.05783 = 0.07413 0.00657 -0.00038 0.01635 AFIX 23 H20A 2 0.895205 0.514162 -0.008773 11.00000 -1.20000 H20B 2 0.847056 0.457710 0.075967 11.00000 -1.20000 AFIX 0 C21 1 0.726617 0.531120 -0.008604 11.00000 0.03681 0.04818 = 0.04392 -0.00631 0.00789 0.01539 AFIX 23 H21A 2 0.672461 0.511761 0.035936 11.00000 -1.20000 H21B 2 0.708633 0.508919 -0.083409 11.00000 -1.20000 AFIX 0 C22 1 0.495890 0.619544 -0.115194 11.00000 0.03006 0.02631 = 0.02572 -0.00392 0.00514 0.00285 AFIX 13 H22 2 0.491734 0.562350 -0.105199 11.00000 -1.20000 AFIX 0 C23 1 0.522094 0.633222 -0.229986 11.00000 0.04052 0.05687 = 0.02484 -0.00616 0.00834 -0.00194 AFIX 23 H23A 2 0.574041 0.593571 -0.248689 11.00000 -1.20000 H23B 2 0.555316 0.684932 -0.235204 11.00000 -1.20000 AFIX 0 C24 1 0.410590 0.627402 -0.306137 11.00000 0.04766 0.07812 = 0.03109 -0.00023 0.00392 0.01147 AFIX 23 H24A 2 0.400351 0.671855 -0.357315 11.00000 -1.20000 H24B 2 0.406870 0.579248 -0.349876 11.00000 -1.20000 AFIX 0 C25 1 0.321838 0.627347 -0.235335 11.00000 0.03910 0.08057 = 0.03474 0.00152 0.00059 0.00289 AFIX 23 H25A 2 0.288973 0.575208 -0.233650 11.00000 -1.20000 H25B 2 0.262391 0.664319 -0.264350 11.00000 -1.20000 AFIX 0 C26 1 0.378036 0.651263 -0.120599 11.00000 0.02819 0.03521 = 0.03174 -0.00233 0.00695 0.00324 AFIX 23 H26A 2 0.341117 0.627692 -0.063350 11.00000 -1.20000 H26B 2 0.378469 0.708138 -0.112047 11.00000 -1.20000 HKLF 4 REM 2C in P2(1)/n REM R1 = 0.0339 for 3758 Fo > 4sig(Fo) and 0.0458 for all 4651 data REM 310 parameters refined using 0 restraints END WGHT 0.0477 1.2437 REM Highest difference peak 0.638, deepest hole -0.354, 1-sigma level 0.084 Q1 1 0.5374 1.0400 0.1653 11.00000 0.05 0.64 Q2 1 0.4003 0.6516 0.5029 11.00000 0.05 0.56 Q3 1 0.5203 0.6936 0.1226 11.00000 0.05 0.50 Q4 1 0.4967 0.6241 0.1109 11.00000 0.05 0.48 Q5 1 0.5427 0.6809 0.2328 11.00000 0.05 0.46 ; _database_code_depnum_ccdc_archive 'CCDC 965922' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3A _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 O2 P2 Pd' _chemical_formula_sum 'C30 H44 O2 P2 Pd' _chemical_formula_weight 604.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0041 0.0074 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' P P 0.1013 0.1134 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' Pd Pd -1.0437 1.1817 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 26.224(3) _cell_length_b 15.8839(18) _cell_length_c 11.0864(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.9650(16) _cell_angle_gamma 90.00 _cell_volume 4583.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 31.73 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9954 _exptl_absorpt_process_details 'SADABS v2012/1 (Sheldrick)' _exptl_special_details ; loop mount with paratone ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'Si-<111> channel cut crystal' _diffrn_measurement_device_type 'Bruker AXS APEXII CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 57801 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 31.11 _reflns_number_total 22449 _reflns_number_gt 18123 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 v2013.6.2' _computing_cell_refinement 'Bruker SAINT v8.32B' _computing_data_reduction 'Bruker SAINT v8.32B' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. For the worse of the disordered t-butyl carbons, C16A and C20C, a two-component disorder model was isotropically refined (major occupancies 65 and 60%, respectively). Other t-butyl carbons show minimal enlargement in the anisotropic displacement parameters, further multi-component models were not refined. A bond restraint was applied to C19C-C20. Flack parameter value is indicative of a racemic twin. ; _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^)+(0.0307P)^2^+0.1236P] 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, 6579 Friedel pairs' _refine_ls_abs_structure_Flack 0.358(15) _refine_ls_number_reflns 22449 _refine_ls_number_parameters 983 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.315199(10) 0.752943(17) 0.39677(2) 0.01918(6) Uani 1 1 d . . . P1A P 0.33362(4) 0.80356(7) 0.58902(9) 0.0268(2) Uani 1 1 d . A . P2A P 0.27469(4) 0.68087(6) 0.23585(9) 0.0218(2) Uani 1 1 d . . . O1A O 0.28889(12) 0.76373(19) 0.6656(3) 0.0365(7) Uani 1 1 d . . . O2A O 0.22368(10) 0.63781(17) 0.2866(2) 0.0281(6) Uani 1 1 d . . . C1A C 0.25695(15) 0.7019(3) 0.4741(4) 0.0242(9) Uani 1 1 d . . . C2A C 0.25210(16) 0.7148(3) 0.5964(4) 0.0296(9) Uani 1 1 d . . . C3A C 0.21256(17) 0.6808(3) 0.6528(4) 0.0409(12) Uani 1 1 d . . . H3A H 0.2097 0.6918 0.7359 0.049 Uiso 1 1 calc R . . C4A C 0.17716(18) 0.6299(3) 0.5833(4) 0.0452(13) Uani 1 1 d . . . H4A H 0.1501 0.6050 0.6205 0.054 Uiso 1 1 calc R . . C5A C 0.18020(17) 0.6145(3) 0.4624(4) 0.0372(10) Uani 1 1 d . . . H5A H 0.1556 0.5798 0.4161 0.045 Uiso 1 1 calc R . . C6A C 0.22051(14) 0.6514(3) 0.4096(4) 0.0260(8) Uani 1 1 d . . . C7A C 0.3231(2) 0.9179(3) 0.6090(4) 0.0447(12) Uani 1 1 d . . . C8A C 0.3618(2) 0.9678(3) 0.5440(4) 0.0549(15) Uani 1 1 d . . . H8A H 0.3524 1.0275 0.5420 0.082 Uiso 1 1 calc R . . H8B H 0.3613 0.9468 0.4608 0.082 Uiso 1 1 calc R . . H8C H 0.3963 0.9609 0.5878 0.082 Uiso 1 1 calc R . . C9A C 0.2696(2) 0.9338(4) 0.5463(6) 0.076(2) Uani 1 1 d . . . H9A H 0.2621 0.9942 0.5479 0.114 Uiso 1 1 calc R . . H9B H 0.2447 0.9029 0.5884 0.114 Uiso 1 1 calc R . . H9C H 0.2674 0.9145 0.4618 0.114 Uiso 1 1 calc R . . C10A C 0.3271(3) 0.9453(4) 0.7432(5) 0.075(2) Uani 1 1 d . . . H10A H 0.3169 1.0045 0.7477 0.113 Uiso 1 1 calc R . . H10B H 0.3626 0.9384 0.7812 0.113 Uiso 1 1 calc R . . H10C H 0.3042 0.9103 0.7860 0.113 Uiso 1 1 calc R . . C13A C 0.3924(2) 0.7604(3) 0.6761(5) 0.0364(12) Uani 1 1 d . . . C14A C 0.3943(2) 0.6679(3) 0.6366(6) 0.082(2) Uani 1 1 d . A . H14A H 0.4235 0.6398 0.6836 0.123 Uiso 1 1 calc R . . H14B H 0.3982 0.6651 0.5499 0.123 Uiso 1 1 calc R . . H14C H 0.3624 0.6397 0.6511 0.123 Uiso 1 1 calc R . . C15A C 0.4399(2) 0.8047(4) 0.6412(6) 0.0574(15) Uani 1 1 d . A . H15A H 0.4704 0.7705 0.6670 0.086 Uiso 1 1 calc R . . H15B H 0.4434 0.8598 0.6812 0.086 Uiso 1 1 calc R . . H15C H 0.4365 0.8124 0.5528 0.086 Uiso 1 1 calc R . . C16A C 0.3896(3) 0.7477(5) 0.8121(7) 0.0430(18) Uiso 0.65 1 d P A 1 H16A H 0.4207 0.7190 0.8489 0.065 Uiso 0.65 1 calc PR A 1 H16B H 0.3594 0.7133 0.8231 0.065 Uiso 0.65 1 calc PR A 1 H16C H 0.3867 0.8025 0.8512 0.065 Uiso 0.65 1 calc PR A 1 C16 C 0.3980(6) 0.7898(10) 0.8118(13) 0.045(3) Uiso 0.35 1 d P A 2 H16J H 0.4235 0.7547 0.8601 0.068 Uiso 0.35 1 calc PR A 2 H16K H 0.3648 0.7844 0.8432 0.068 Uiso 0.35 1 calc PR A 2 H16L H 0.4091 0.8488 0.8170 0.068 Uiso 0.35 1 calc PR A 2 C19A C 0.24403(18) 0.7450(3) 0.1089(4) 0.0339(11) Uani 1 1 d . . . C20A C 0.2245(2) 0.8234(3) 0.1703(5) 0.0461(12) Uani 1 1 d . . . H20A H 0.2057 0.8596 0.1086 0.069 Uiso 1 1 calc R . . H20B H 0.2538 0.8545 0.2118 0.069 Uiso 1 1 calc R . . H20C H 0.2017 0.8062 0.2296 0.069 Uiso 1 1 calc R . . C21A C 0.2830(2) 0.7716(4) 0.0255(5) 0.0519(15) Uani 1 1 d . . . H21A H 0.2685 0.8168 -0.0281 0.078 Uiso 1 1 calc R . . H21B H 0.2914 0.7233 -0.0236 0.078 Uiso 1 1 calc R . . H21C H 0.3143 0.7916 0.0744 0.078 Uiso 1 1 calc R . . C22A C 0.19904(17) 0.7006(3) 0.0330(4) 0.0403(11) Uani 1 1 d . . . H22A H 0.1781 0.7423 -0.0155 0.060 Uiso 1 1 calc R . . H22B H 0.1779 0.6716 0.0873 0.060 Uiso 1 1 calc R . . H22C H 0.2124 0.6595 -0.0211 0.060 Uiso 1 1 calc R . . C25A C 0.30825(16) 0.5861(3) 0.1895(4) 0.0292(9) Uani 1 1 d . . . C26A C 0.3206(2) 0.5338(3) 0.3057(5) 0.0519(14) Uani 1 1 d . . . H26A H 0.3398 0.4834 0.2877 0.078 Uiso 1 1 calc R . . H26B H 0.2886 0.5172 0.3362 0.078 Uiso 1 1 calc R . . H26C H 0.3414 0.5676 0.3673 0.078 Uiso 1 1 calc R . . C27A C 0.2751(2) 0.5334(3) 0.0937(5) 0.0587(16) Uani 1 1 d . . . H27A H 0.2915 0.4786 0.0852 0.088 Uiso 1 1 calc R . . H27B H 0.2718 0.5629 0.0155 0.088 Uiso 1 1 calc R . . H27C H 0.2410 0.5251 0.1192 0.088 Uiso 1 1 calc R . . C28A C 0.3594(2) 0.6108(4) 0.1448(6) 0.0614(16) Uani 1 1 d . . . H28A H 0.3780 0.5598 0.1261 0.092 Uiso 1 1 calc R . . H28B H 0.3802 0.6429 0.2083 0.092 Uiso 1 1 calc R . . H28C H 0.3526 0.6454 0.0715 0.092 Uiso 1 1 calc R . . C31A C 0.37294(16) 0.8048(3) 0.3177(4) 0.0270(9) Uani 1 1 d . . . C32A C 0.40727(15) 0.8387(3) 0.2717(4) 0.0268(9) Uani 1 1 d . . . C33A C 0.44701(15) 0.8809(3) 0.2152(4) 0.0238(8) Uani 1 1 d . . . C34A C 0.47286(16) 0.9514(3) 0.2705(4) 0.0316(9) Uani 1 1 d . . . H34A H 0.4648 0.9706 0.3471 0.038 Uiso 1 1 calc R . . C35A C 0.50962(17) 0.9926(3) 0.2145(5) 0.0387(11) Uani 1 1 d . . . H35A H 0.5265 1.0403 0.2527 0.046 Uiso 1 1 calc R . . C36A C 0.52237(18) 0.9658(3) 0.1039(5) 0.0430(12) Uani 1 1 d . . . H36A H 0.5477 0.9948 0.0657 0.052 Uiso 1 1 calc R . . C37A C 0.49804(19) 0.8966(3) 0.0492(4) 0.0415(12) Uani 1 1 d . . . H37A H 0.5070 0.8778 -0.0269 0.050 Uiso 1 1 calc R . . C38A C 0.46083(17) 0.8538(3) 0.1029(4) 0.0312(10) Uani 1 1 d . . . H38A H 0.4445 0.8060 0.0638 0.037 Uiso 1 1 calc R . . Pd2 Pd 0.667340(9) 0.251218(17) 0.178071(18) 0.01770(6) Uani 1 1 d . . . P1B P 0.64377(4) 0.30115(6) -0.01341(9) 0.0212(2) Uani 1 1 d . . . P2B P 0.71306(4) 0.18152(6) 0.33479(9) 0.0200(2) Uani 1 1 d . . . O1B O 0.69002(11) 0.27030(17) -0.0935(2) 0.0261(6) Uani 1 1 d . . . O2B O 0.76416(10) 0.14424(16) 0.2786(2) 0.0255(6) Uani 1 1 d . . . C1B C 0.72616(14) 0.2078(2) 0.0936(3) 0.0191(8) Uani 1 1 d . . . C2B C 0.72916(15) 0.2231(2) -0.0279(3) 0.0238(8) Uani 1 1 d . . . C3B C 0.76922(16) 0.1939(3) -0.0879(4) 0.0307(9) Uani 1 1 d . . . H3B H 0.7703 0.2054 -0.1716 0.037 Uiso 1 1 calc R . . C4B C 0.80755(16) 0.1475(3) -0.0217(4) 0.0316(9) Uani 1 1 d . . . H4B H 0.8355 0.1276 -0.0608 0.038 Uiso 1 1 calc R . . C5B C 0.80633(15) 0.1294(3) 0.0994(4) 0.0298(9) Uani 1 1 d . . . H5B H 0.8324 0.0962 0.1432 0.036 Uiso 1 1 calc R . . C6B C 0.76598(14) 0.1610(2) 0.1557(3) 0.0223(8) Uani 1 1 d . . . C7B C 0.64638(15) 0.4168(2) -0.0323(3) 0.0244(8) Uani 1 1 d . . . C8B C 0.60550(16) 0.4594(3) 0.0324(4) 0.0325(9) Uani 1 1 d . . . H8D H 0.6120 0.5201 0.0369 0.049 Uiso 1 1 calc R . . H8E H 0.6065 0.4364 0.1147 0.049 Uiso 1 1 calc R . . H8F H 0.5716 0.4490 -0.0127 0.049 Uiso 1 1 calc R . . C9B C 0.69965(16) 0.4413(3) 0.0319(4) 0.0356(10) Uani 1 1 d . . . H9D H 0.7041 0.5024 0.0270 0.053 Uiso 1 1 calc R . . H9E H 0.7263 0.4129 -0.0078 0.053 Uiso 1 1 calc R . . H9F H 0.7024 0.4242 0.1174 0.053 Uiso 1 1 calc R . . C10B C 0.64219(19) 0.4451(3) -0.1663(4) 0.0409(11) Uani 1 1 d . . . H10D H 0.6459 0.5064 -0.1700 0.061 Uiso 1 1 calc R . . H10E H 0.6086 0.4287 -0.2081 0.061 Uiso 1 1 calc R . . H10F H 0.6694 0.4181 -0.2059 0.061 Uiso 1 1 calc R . . C13B C 0.58689(19) 0.2496(3) -0.0995(4) 0.0321(11) Uani 1 1 d . . . C14B C 0.5892(2) 0.1577(3) -0.0553(5) 0.0584(15) Uani 1 1 d . . . H14D H 0.5605 0.1261 -0.0983 0.088 Uiso 1 1 calc R . . H14E H 0.5869 0.1563 0.0322 0.088 Uiso 1 1 calc R . . H14F H 0.6217 0.1323 -0.0718 0.088 Uiso 1 1 calc R . . C15B C 0.53757(18) 0.2879(4) -0.0660(6) 0.0536(14) Uani 1 1 d . . . H15D H 0.5082 0.2545 -0.1023 0.080 Uiso 1 1 calc R . . H15E H 0.5343 0.3458 -0.0968 0.080 Uiso 1 1 calc R . . H15F H 0.5383 0.2883 0.0226 0.080 Uiso 1 1 calc R . . C16B C 0.5873(2) 0.2518(4) -0.2364(4) 0.069(2) Uani 1 1 d . . . H16D H 0.5589 0.2176 -0.2757 0.104 Uiso 1 1 calc R . . H16E H 0.6200 0.2291 -0.2567 0.104 Uiso 1 1 calc R . . H16F H 0.5834 0.3100 -0.2652 0.104 Uiso 1 1 calc R . . C19B C 0.74424(18) 0.2457(2) 0.4623(4) 0.0283(9) Uani 1 1 d . . . C20B C 0.7630(2) 0.3251(3) 0.4021(4) 0.0446(12) Uani 1 1 d . . . H20D H 0.7827 0.3602 0.4638 0.067 Uiso 1 1 calc R . . H20E H 0.7334 0.3568 0.3635 0.067 Uiso 1 1 calc R . . H20F H 0.7850 0.3088 0.3404 0.067 Uiso 1 1 calc R . . C21B C 0.7056(3) 0.2718(4) 0.5489(5) 0.0582(16) Uani 1 1 d . . . H21D H 0.7199 0.3184 0.6002 0.087 Uiso 1 1 calc R . . H21E H 0.6989 0.2238 0.6003 0.087 Uiso 1 1 calc R . . H21F H 0.6735 0.2897 0.5015 0.087 Uiso 1 1 calc R . . C22B C 0.79145(19) 0.2027(3) 0.5331(4) 0.0454(12) Uani 1 1 d . . . H22D H 0.8058 0.2393 0.5999 0.068 Uiso 1 1 calc R . . H22E H 0.8175 0.1925 0.4784 0.068 Uiso 1 1 calc R . . H22F H 0.7811 0.1490 0.5661 0.068 Uiso 1 1 calc R . . C25B C 0.68331(16) 0.0827(2) 0.3820(4) 0.0285(9) Uani 1 1 d . . . C26B C 0.6695(2) 0.0341(3) 0.2625(4) 0.0527(14) Uani 1 1 d . . . H26D H 0.6523 -0.0187 0.2792 0.079 Uiso 1 1 calc R . . H26E H 0.7010 0.0215 0.2263 0.079 Uiso 1 1 calc R . . H26F H 0.6466 0.0684 0.2060 0.079 Uiso 1 1 calc R . . C27B C 0.7190(2) 0.0293(3) 0.4682(5) 0.0473(12) Uani 1 1 d . . . H27D H 0.7036 -0.0263 0.4765 0.071 Uiso 1 1 calc R . . H27E H 0.7245 0.0567 0.5479 0.071 Uiso 1 1 calc R . . H27F H 0.7520 0.0230 0.4360 0.071 Uiso 1 1 calc R . . C28B C 0.6341(2) 0.1028(3) 0.4362(5) 0.0523(14) Uani 1 1 d . . . H28D H 0.6130 0.0519 0.4367 0.078 Uiso 1 1 calc R . . H28E H 0.6148 0.1463 0.3872 0.078 Uiso 1 1 calc R . . H28F H 0.6426 0.1233 0.5196 0.078 Uiso 1 1 calc R . . C31B C 0.60817(16) 0.2968(3) 0.2605(4) 0.0245(9) Uani 1 1 d . . . C32B C 0.57391(15) 0.3301(3) 0.3071(4) 0.0257(8) Uani 1 1 d . . . C33B C 0.53442(15) 0.3740(2) 0.3602(4) 0.0248(8) Uani 1 1 d . . . C34B C 0.51008(15) 0.4441(3) 0.3007(4) 0.0274(9) Uani 1 1 d . . . H34B H 0.5188 0.4606 0.2234 0.033 Uiso 1 1 calc R . . C35B C 0.47347(16) 0.4891(3) 0.3542(4) 0.0340(10) Uani 1 1 d . . . H35B H 0.4569 0.5361 0.3133 0.041 Uiso 1 1 calc R . . C36B C 0.46100(17) 0.4656(3) 0.4677(5) 0.0380(11) Uani 1 1 d . . . H36B H 0.4367 0.4975 0.5053 0.046 Uiso 1 1 calc R . . C37B C 0.48386(18) 0.3961(3) 0.5259(4) 0.0414(12) Uani 1 1 d . . . H37B H 0.4746 0.3794 0.6025 0.050 Uiso 1 1 calc R . . C38B C 0.52084(16) 0.3500(3) 0.4722(4) 0.0279(9) Uani 1 1 d . . . H38B H 0.5366 0.3022 0.5127 0.034 Uiso 1 1 calc R . . Pd3 Pd 1.000865(12) 0.750012(16) -0.00015(2) 0.02207(6) Uani 1 1 d . . . P1C P 1.00108(4) 0.67961(6) -0.17879(9) 0.0246(2) Uani 1 1 d . . . P2C P 1.02383(4) 0.84326(6) 0.15148(9) 0.0290(2) Uani 1 1 d . B . O1C O 1.04854(10) 0.72128(18) -0.2452(2) 0.0307(6) Uani 1 1 d . . . O2C O 1.06837(11) 0.90308(16) 0.1009(3) 0.0366(7) Uani 1 1 d . . . C1C C 1.05667(14) 0.8124(2) -0.0720(3) 0.0224(8) Uani 1 1 d . . . C2C C 1.07284(15) 0.7890(3) -0.1821(4) 0.0282(8) Uani 1 1 d . . . C3C C 1.11231(16) 0.8313(3) -0.2328(4) 0.0338(10) Uani 1 1 d . . . H3C H 1.1224 0.8145 -0.3087 0.041 Uiso 1 1 calc R . . C4C C 1.13589(17) 0.8980(3) -0.1688(4) 0.0379(10) Uani 1 1 d . . . H4C H 1.1623 0.9277 -0.2021 0.045 Uiso 1 1 calc R . . C5C C 1.12208(16) 0.9233(3) -0.0562(4) 0.0348(10) Uani 1 1 d . . . H5C H 1.1388 0.9691 -0.0128 0.042 Uiso 1 1 calc R . . C6C C 1.08297(15) 0.8788(2) -0.0101(4) 0.0292(8) Uani 1 1 d . . . C7C C 0.94445(16) 0.6991(3) -0.2922(4) 0.0331(9) Uani 1 1 d . . . C8C C 0.89537(17) 0.6806(3) -0.2366(4) 0.0453(11) Uani 1 1 d . . . H8G H 0.8656 0.6979 -0.2932 0.068 Uiso 1 1 calc R . . H8H H 0.8957 0.7119 -0.1603 0.068 Uiso 1 1 calc R . . H8I H 0.8933 0.6201 -0.2203 0.068 Uiso 1 1 calc R . . C9C C 0.94668(19) 0.7936(3) -0.3227(5) 0.0481(12) Uani 1 1 d . . . H9G H 0.9171 0.8085 -0.3817 0.072 Uiso 1 1 calc R . . H9H H 0.9785 0.8057 -0.3574 0.072 Uiso 1 1 calc R . . H9I H 0.9458 0.8268 -0.2484 0.072 Uiso 1 1 calc R . . C10C C 0.94580(19) 0.6485(3) -0.4100(4) 0.0496(12) Uani 1 1 d . . . H10G H 0.9174 0.6663 -0.4702 0.074 Uiso 1 1 calc R . . H10H H 0.9424 0.5884 -0.3929 0.074 Uiso 1 1 calc R . . H10I H 0.9785 0.6586 -0.4420 0.074 Uiso 1 1 calc R . . C13C C 1.02197(16) 0.5688(2) -0.1658(4) 0.0312(9) Uani 1 1 d . . . C14C C 1.06628(18) 0.5679(3) -0.0620(4) 0.0441(11) Uani 1 1 d . . . H14G H 1.0790 0.5102 -0.0489 0.066 Uiso 1 1 calc R . . H14H H 1.0540 0.5889 0.0125 0.066 Uiso 1 1 calc R . . H14I H 1.0941 0.6041 -0.0833 0.066 Uiso 1 1 calc R . . C15C C 0.97831(18) 0.5146(3) -0.1296(4) 0.0418(11) Uani 1 1 d . . . H15G H 0.9915 0.4586 -0.1056 0.063 Uiso 1 1 calc R . . H15H H 0.9514 0.5095 -0.1987 0.063 Uiso 1 1 calc R . . H15I H 0.9640 0.5410 -0.0612 0.063 Uiso 1 1 calc R . . C16C C 1.0423(2) 0.5331(3) -0.2818(4) 0.0497(12) Uani 1 1 d . . . H16G H 1.0586 0.4784 -0.2632 0.075 Uiso 1 1 calc R . . H16H H 1.0675 0.5722 -0.3090 0.075 Uiso 1 1 calc R . . H16I H 1.0135 0.5263 -0.3463 0.075 Uiso 1 1 calc R . . C19C C 0.9756(2) 0.9235(3) 0.1835(4) 0.0464(12) Uani 1 1 d D . . C20C C 0.9623(4) 0.9677(6) 0.0607(8) 0.062(3) Uiso 0.60 1 d P B 1 H20G H 0.9355 1.0099 0.0675 0.093 Uiso 0.60 1 calc PR B 1 H20H H 0.9498 0.9261 -0.0012 0.093 Uiso 0.60 1 calc PR B 1 H20I H 0.9930 0.9953 0.0374 0.093 Uiso 0.60 1 calc PR B 1 C20 C 0.9385(5) 0.9377(10) 0.0610(12) 0.061(4) Uiso 0.40 1 d PD B 2 H20J H 0.9133 0.9815 0.0735 0.092 Uiso 0.40 1 calc PR B 2 H20K H 0.9205 0.8851 0.0373 0.092 Uiso 0.40 1 calc PR B 2 H20L H 0.9587 0.9553 -0.0034 0.092 Uiso 0.40 1 calc PR B 2 C21C C 0.9330(2) 0.8828(4) 0.2462(6) 0.080(2) Uani 1 1 d . B . H21G H 0.9038 0.9216 0.2438 0.120 Uiso 1 1 calc R . . H21H H 0.9460 0.8703 0.3309 0.120 Uiso 1 1 calc R . . H21I H 0.9218 0.8305 0.2040 0.120 Uiso 1 1 calc R . . C22C C 1.0009(3) 0.9958(4) 0.2627(7) 0.089(2) Uani 1 1 d . B . H22G H 0.9781 1.0448 0.2567 0.134 Uiso 1 1 calc R . . H22H H 1.0336 1.0111 0.2341 0.134 Uiso 1 1 calc R . . H22I H 1.0072 0.9773 0.3476 0.134 Uiso 1 1 calc R . . C25C C 1.0600(2) 0.7963(3) 0.2903(4) 0.0404(11) Uani 1 1 d . . . C26C C 1.0942(2) 0.7304(4) 0.2379(5) 0.0680(18) Uani 1 1 d . B . H26G H 1.1153 0.7018 0.3046 0.102 Uiso 1 1 calc R . . H26H H 1.1166 0.7584 0.1856 0.102 Uiso 1 1 calc R . . H26I H 1.0726 0.6891 0.1902 0.102 Uiso 1 1 calc R . . C27C C 1.0948(3) 0.8580(4) 0.3661(5) 0.082(2) Uani 1 1 d . B . H27G H 1.1198 0.8268 0.4219 0.123 Uiso 1 1 calc R . . H27H H 1.0741 0.8940 0.4129 0.123 Uiso 1 1 calc R . . H27I H 1.1130 0.8930 0.3124 0.123 Uiso 1 1 calc R . . C28C C 1.0240(3) 0.7504(4) 0.3656(6) 0.075(2) Uani 1 1 d . B . H28G H 1.0439 0.7133 0.4240 0.112 Uiso 1 1 calc R . . H28H H 0.9994 0.7168 0.3119 0.112 Uiso 1 1 calc R . . H28I H 1.0053 0.7916 0.4094 0.112 Uiso 1 1 calc R . . C31C C 0.94578(16) 0.6875(3) 0.0756(4) 0.0296(9) Uani 1 1 d . . . C32C C 0.91256(15) 0.6520(3) 0.1229(4) 0.0289(9) Uani 1 1 d . . . C33C C 0.87283(14) 0.6109(2) 0.1808(3) 0.0246(8) Uani 1 1 d . . . C34C C 0.85075(15) 0.5368(2) 0.1346(4) 0.0306(9) Uani 1 1 d . . . H34C H 0.8612 0.5129 0.0630 0.037 Uiso 1 1 calc R . . C35C C 0.81340(15) 0.4974(3) 0.1928(4) 0.0370(10) Uani 1 1 d . . . H35C H 0.7985 0.4463 0.1609 0.044 Uiso 1 1 calc R . . C36C C 0.79759(16) 0.5316(3) 0.2968(4) 0.0406(11) Uani 1 1 d . . . H36C H 0.7723 0.5037 0.3367 0.049 Uiso 1 1 calc R . . C37C C 0.81847(17) 0.6057(3) 0.3418(4) 0.0378(10) Uani 1 1 d . . . H37C H 0.8071 0.6301 0.4121 0.045 Uiso 1 1 calc R . . C38C C 0.85681(17) 0.6460(3) 0.2840(4) 0.0322(9) Uani 1 1 d . . . H38C H 0.8716 0.6972 0.3158 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02197(12) 0.01838(13) 0.01754(12) -0.00101(12) 0.00377(10) -0.00234(12) P1A 0.0353(6) 0.0260(5) 0.0187(5) -0.0031(4) 0.0019(4) -0.0015(4) P2A 0.0242(5) 0.0217(5) 0.0196(5) -0.0001(4) 0.0029(4) -0.0038(4) O1A 0.0389(17) 0.051(2) 0.0200(15) -0.0022(13) 0.0064(13) -0.0033(14) O2A 0.0292(15) 0.0319(15) 0.0230(14) 0.0014(11) 0.0027(11) -0.0132(12) C1A 0.024(2) 0.028(2) 0.022(2) 0.0045(16) 0.0086(16) 0.0017(17) C2A 0.028(2) 0.035(2) 0.026(2) 0.0069(18) 0.0036(17) 0.0067(18) C3A 0.035(2) 0.066(3) 0.025(2) 0.014(2) 0.0144(19) 0.009(2) C4A 0.027(2) 0.069(3) 0.042(3) 0.026(2) 0.010(2) -0.006(2) C5A 0.028(2) 0.047(3) 0.037(2) 0.013(2) 0.0020(19) -0.0090(19) C6A 0.022(2) 0.030(2) 0.025(2) 0.0061(16) 0.0024(16) 0.0007(16) C7A 0.063(3) 0.034(3) 0.037(3) -0.014(2) 0.002(2) 0.004(2) C8A 0.100(5) 0.027(2) 0.033(3) 0.0015(19) -0.010(3) -0.005(3) C9A 0.073(4) 0.044(3) 0.105(5) -0.028(3) -0.012(4) 0.026(3) C10A 0.144(6) 0.052(3) 0.032(3) -0.020(2) 0.016(3) 0.001(4) C13A 0.037(3) 0.036(3) 0.033(3) -0.0030(19) -0.008(2) -0.008(2) C14A 0.083(5) 0.029(3) 0.116(6) 0.016(3) -0.060(4) 0.003(3) C15A 0.039(3) 0.063(4) 0.070(4) 0.019(3) 0.005(3) -0.002(3) C19A 0.032(2) 0.045(3) 0.025(2) 0.003(2) 0.0029(18) -0.007(2) C20A 0.050(3) 0.035(3) 0.049(3) 0.005(2) -0.011(2) 0.008(2) C21A 0.049(3) 0.072(4) 0.035(3) 0.024(3) 0.005(2) -0.016(3) C22A 0.038(3) 0.058(3) 0.022(2) 0.004(2) -0.0070(18) 0.001(2) C25A 0.037(2) 0.028(2) 0.023(2) -0.0111(16) 0.0056(17) -0.0012(17) C26A 0.077(4) 0.034(3) 0.044(3) -0.004(2) 0.004(3) 0.019(3) C27A 0.080(4) 0.040(3) 0.051(3) -0.027(2) -0.013(3) 0.008(3) C28A 0.056(3) 0.054(3) 0.080(4) -0.010(3) 0.034(3) 0.017(3) C31A 0.029(2) 0.032(2) 0.020(2) -0.0024(16) 0.0022(17) 0.0020(18) C32A 0.029(2) 0.027(2) 0.024(2) 0.0015(16) 0.0007(17) -0.0018(17) C33A 0.020(2) 0.029(2) 0.022(2) 0.0041(16) 0.0033(16) 0.0002(16) C34A 0.025(2) 0.035(2) 0.033(2) 0.0017(18) 0.0003(18) -0.0004(18) C35A 0.028(2) 0.030(2) 0.058(3) 0.006(2) 0.001(2) -0.0043(19) C36A 0.035(3) 0.041(3) 0.055(3) 0.022(2) 0.016(2) 0.001(2) C37A 0.045(3) 0.047(3) 0.035(3) 0.011(2) 0.018(2) 0.007(2) C38A 0.032(2) 0.032(2) 0.030(2) 0.0042(19) 0.0049(19) 0.0024(19) Pd2 0.02234(14) 0.01765(12) 0.01364(12) 0.00086(12) 0.00440(9) 0.00192(12) P1B 0.0262(5) 0.0230(5) 0.0146(4) 0.0003(4) 0.0030(4) 0.0008(4) P2B 0.0250(5) 0.0191(5) 0.0160(5) 0.0023(4) 0.0022(4) 0.0005(4) O1B 0.0309(15) 0.0329(15) 0.0150(13) 0.0032(11) 0.0055(11) 0.0050(12) O2B 0.0265(14) 0.0255(14) 0.0251(14) 0.0065(11) 0.0056(11) 0.0047(11) C1B 0.0206(19) 0.0168(18) 0.0206(19) -0.0023(14) 0.0058(15) 0.0012(14) C2B 0.029(2) 0.0242(18) 0.0199(19) 0.0001(15) 0.0083(16) -0.0027(16) C3B 0.034(2) 0.032(2) 0.027(2) -0.0016(17) 0.0108(17) -0.0011(18) C4B 0.030(2) 0.033(2) 0.034(2) -0.0045(18) 0.0132(18) 0.0014(18) C5B 0.025(2) 0.028(2) 0.037(2) -0.0004(17) 0.0079(17) 0.0023(16) C6B 0.027(2) 0.0190(18) 0.0219(18) -0.0015(14) 0.0061(15) -0.0013(15) C7B 0.034(2) 0.0165(17) 0.0225(19) 0.0066(14) 0.0015(16) 0.0011(15) C8B 0.042(2) 0.029(2) 0.028(2) 0.0010(17) 0.0059(17) 0.0072(18) C9B 0.039(2) 0.027(2) 0.042(3) 0.0057(18) 0.0069(19) -0.0047(18) C10B 0.062(3) 0.036(2) 0.026(2) 0.0124(18) 0.011(2) 0.008(2) C13B 0.038(3) 0.040(3) 0.016(2) 0.0003(18) -0.0018(18) -0.009(2) C14B 0.068(4) 0.036(3) 0.064(4) -0.004(2) -0.022(3) -0.009(3) C15B 0.028(2) 0.050(3) 0.079(4) -0.015(3) -0.006(3) -0.006(2) C16B 0.073(4) 0.111(5) 0.020(2) -0.010(3) -0.009(2) -0.035(4) C19B 0.037(2) 0.022(2) 0.023(2) -0.0034(17) -0.0072(18) -0.0010(18) C20B 0.059(3) 0.028(2) 0.042(3) 0.004(2) -0.014(2) -0.019(2) C21B 0.071(4) 0.061(3) 0.043(3) -0.022(3) 0.009(3) -0.009(3) C22B 0.048(3) 0.043(3) 0.040(3) -0.005(2) -0.018(2) -0.001(2) C25B 0.036(2) 0.021(2) 0.030(2) 0.0038(16) 0.0083(18) -0.0048(16) C26B 0.086(4) 0.031(3) 0.040(3) -0.002(2) 0.005(3) -0.027(3) C27B 0.057(3) 0.030(2) 0.056(3) 0.022(2) 0.008(2) -0.002(2) C28B 0.056(3) 0.038(3) 0.069(4) 0.011(2) 0.032(3) -0.008(2) C31B 0.027(2) 0.025(2) 0.021(2) 0.0051(16) 0.0048(16) 0.0064(17) C32B 0.027(2) 0.030(2) 0.0204(19) 0.0010(16) 0.0051(16) 0.0000(17) C33B 0.025(2) 0.025(2) 0.024(2) -0.0061(16) 0.0036(16) 0.0000(16) C34B 0.028(2) 0.030(2) 0.023(2) 0.0038(16) 0.0020(17) -0.0014(17) C35B 0.023(2) 0.034(2) 0.045(3) -0.006(2) 0.0025(19) 0.0043(18) C36B 0.030(2) 0.033(2) 0.054(3) -0.014(2) 0.016(2) 0.0025(19) C37B 0.046(3) 0.048(3) 0.034(3) -0.013(2) 0.021(2) -0.007(2) C38B 0.033(2) 0.026(2) 0.025(2) 0.0006(17) 0.0037(18) -0.0002(18) Pd3 0.02480(13) 0.01982(13) 0.02227(12) -0.00174(11) 0.00559(10) -0.00255(11) P1C 0.0278(5) 0.0252(5) 0.0220(4) -0.0016(4) 0.0074(4) -0.0038(4) P2C 0.0419(6) 0.0199(5) 0.0260(5) -0.0022(4) 0.0070(4) -0.0036(4) O1C 0.0345(16) 0.0317(14) 0.0278(14) -0.0018(12) 0.0121(12) -0.0058(12) O2C 0.0525(18) 0.0257(14) 0.0324(15) -0.0021(12) 0.0080(13) -0.0138(13) C1C 0.0204(18) 0.0219(18) 0.0247(19) 0.0047(15) 0.0016(15) -0.0010(14) C2C 0.027(2) 0.028(2) 0.029(2) 0.0083(16) 0.0018(16) 0.0033(16) C3C 0.036(2) 0.040(2) 0.027(2) 0.0076(18) 0.0098(17) 0.0055(19) C4C 0.032(2) 0.039(2) 0.044(3) 0.016(2) 0.009(2) -0.0031(19) C5C 0.031(2) 0.029(2) 0.042(3) 0.0078(19) -0.0039(19) -0.0048(18) C6C 0.032(2) 0.027(2) 0.027(2) 0.0064(16) 0.0015(16) -0.0012(16) C7C 0.031(2) 0.035(2) 0.033(2) -0.0026(18) 0.0015(17) -0.0054(18) C8C 0.038(3) 0.054(3) 0.043(3) -0.004(2) -0.001(2) -0.002(2) C9C 0.049(3) 0.039(3) 0.054(3) 0.008(2) -0.007(2) -0.003(2) C10C 0.054(3) 0.064(3) 0.028(2) -0.004(2) -0.002(2) -0.012(2) C13C 0.044(2) 0.0229(19) 0.029(2) -0.0023(16) 0.0149(18) -0.0003(17) C14C 0.050(3) 0.033(2) 0.048(3) 0.005(2) 0.003(2) 0.014(2) C15C 0.057(3) 0.029(2) 0.041(3) 0.0007(19) 0.011(2) -0.005(2) C16C 0.068(3) 0.043(3) 0.041(3) -0.006(2) 0.022(2) 0.005(2) C19C 0.063(3) 0.029(2) 0.049(3) -0.007(2) 0.018(2) 0.010(2) C21C 0.066(4) 0.051(3) 0.130(6) -0.017(4) 0.045(4) 0.006(3) C22C 0.101(5) 0.043(3) 0.132(6) -0.043(4) 0.044(5) -0.009(3) C25C 0.059(3) 0.032(2) 0.028(2) 0.0032(18) -0.003(2) -0.007(2) C26C 0.067(4) 0.082(4) 0.051(4) 0.007(3) -0.010(3) 0.028(3) C27C 0.123(6) 0.061(4) 0.053(4) 0.000(3) -0.019(4) -0.031(4) C28C 0.075(5) 0.099(6) 0.048(3) 0.039(3) 0.000(3) -0.024(4) C31C 0.038(2) 0.026(2) 0.026(2) -0.0023(16) 0.0088(17) -0.0019(17) C32C 0.027(2) 0.034(2) 0.025(2) 0.0010(17) 0.0009(16) -0.0002(17) C33C 0.0236(19) 0.0245(19) 0.0258(19) 0.0057(15) 0.0033(16) 0.0044(15) C34C 0.027(2) 0.028(2) 0.035(2) -0.0004(17) -0.0008(17) 0.0027(16) C35C 0.023(2) 0.027(2) 0.060(3) 0.0015(19) 0.0018(19) -0.0021(16) C36C 0.031(2) 0.033(2) 0.062(3) 0.012(2) 0.019(2) -0.0006(18) C37C 0.046(3) 0.028(2) 0.043(2) 0.0059(19) 0.021(2) 0.0034(18) C38C 0.041(3) 0.024(2) 0.032(2) 0.0008(18) 0.0089(18) 0.0034(18) _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 C1A 2.011(4) . ? Pd1 C31A 2.016(4) . ? Pd1 P2A 2.2720(10) . ? Pd1 P1A 2.2745(11) . ? P1A O1A 1.655(3) . ? P1A C13A 1.849(5) . ? P1A C7A 1.854(5) . ? P2A O2A 1.660(3) . ? P2A C19A 1.841(5) . ? P2A C25A 1.848(4) . ? O1A C2A 1.394(5) . ? O2A C6A 1.393(5) . ? C1A C6A 1.379(6) . ? C1A C2A 1.392(6) . ? C2A C3A 1.384(6) . ? C3A C4A 1.391(7) . ? C3A H3A 0.9500 . ? C4A C5A 1.374(7) . ? C4A H4A 0.9500 . ? C5A C6A 1.398(6) . ? C5A H5A 0.9500 . ? C7A C9A 1.509(7) . ? C7A C8A 1.534(7) . ? C7A C10A 1.541(6) . ? C8A H8A 0.9800 . ? C8A H8B 0.9800 . ? C8A H8C 0.9800 . ? C9A H9A 0.9800 . ? C9A H9B 0.9800 . ? C9A H9C 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C13A C15A 1.519(7) . ? C13A C16A 1.532(9) . ? C13A C14A 1.536(7) . ? C13A C16 1.565(15) . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16 H16J 0.9800 . ? C16 H16K 0.9800 . ? C16 H16L 0.9800 . ? C19A C21A 1.520(7) . ? C19A C22A 1.535(6) . ? C19A C20A 1.537(7) . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C25A C26A 1.533(6) . ? C25A C28A 1.536(7) . ? C25A C27A 1.536(6) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C31A C32A 1.213(6) . ? C32A C33A 1.444(6) . ? C33A C38A 1.406(6) . ? C33A C34A 1.411(6) . ? C34A C35A 1.374(6) . ? C34A H34A 0.9500 . ? C35A C36A 1.378(7) . ? C35A H35A 0.9500 . ? C36A C37A 1.374(7) . ? C36A H36A 0.9500 . ? C37A C38A 1.382(6) . ? C37A H37A 0.9500 . ? C38A H38A 0.9500 . ? Pd2 C1B 2.020(4) . ? Pd2 C31B 2.027(4) . ? Pd2 P2B 2.2753(10) . ? Pd2 P1B 2.2802(10) . ? P1B O1B 1.662(3) . ? P1B C7B 1.851(4) . ? P1B C13B 1.860(5) . ? P2B O2B 1.654(3) . ? P2B C19B 1.851(4) . ? P2B C25B 1.856(4) . ? O1B C2B 1.401(5) . ? O2B C6B 1.395(4) . ? C1B C2B 1.381(5) . ? C1B C6B 1.393(5) . ? C2B C3B 1.389(6) . ? C3B C4B 1.383(6) . ? C3B H3B 0.9500 . ? C4B C5B 1.377(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.385(5) . ? C5B H5B 0.9500 . ? C7B C8B 1.519(6) . ? C7B C9B 1.539(5) . ? C7B C10B 1.543(5) . ? C8B H8D 0.9800 . ? C8B H8E 0.9800 . ? C8B H8F 0.9800 . ? C9B H9D 0.9800 . ? C9B H9E 0.9800 . ? C9B H9F 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C13B C15B 1.516(7) . ? C13B C16B 1.520(6) . ? C13B C14B 1.539(6) . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C19B C21B 1.534(8) . ? C19B C20B 1.536(6) . ? C19B C22B 1.543(6) . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C25B C27B 1.514(6) . ? C25B C28B 1.523(6) . ? C25B C26B 1.537(6) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C31B C32B 1.211(5) . ? C32B C33B 1.433(5) . ? C33B C38B 1.386(6) . ? C33B C34B 1.407(6) . ? C34B C35B 1.387(6) . ? C34B H34B 0.9500 . ? C35B C36B 1.389(6) . ? C35B H35B 0.9500 . ? C36B C37B 1.379(7) . ? C36B H36B 0.9500 . ? C37B C38B 1.404(6) . ? C37B H37B 0.9500 . ? C38B H38B 0.9500 . ? Pd3 C1C 2.011(4) . ? Pd3 C31C 2.018(4) . ? Pd3 P2C 2.2664(10) . ? Pd3 P1C 2.2750(10) . ? P1C O1C 1.659(3) . ? P1C C13C 1.844(4) . ? P1C C7C 1.852(4) . ? P2C O2C 1.656(3) . ? P2C C19C 1.860(5) . ? P2C C25C 1.863(4) . ? O1C C2C 1.394(5) . ? O2C C6C 1.387(5) . ? C1C C2C 1.391(5) . ? C1C C6C 1.394(5) . ? C2C C3C 1.407(6) . ? C3C C4C 1.379(6) . ? C3C H3C 0.9500 . ? C4C C5C 1.400(6) . ? C4C H4C 0.9500 . ? C5C C6C 1.392(6) . ? C5C H5C 0.9500 . ? C7C C8C 1.522(6) . ? C7C C10C 1.538(6) . ? C7C C9C 1.541(6) . ? C8C H8G 0.9800 . ? C8C H8H 0.9800 . ? C8C H8I 0.9800 . ? C9C H9G 0.9800 . ? C9C H9H 0.9800 . ? C9C H9I 0.9800 . ? C10C H10G 0.9800 . ? C10C H10H 0.9800 . ? C10C H10I 0.9800 . ? C13C C15C 1.524(6) . ? C13C C14C 1.533(6) . ? C13C C16C 1.558(6) . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C14C H14I 0.9800 . ? C15C H15G 0.9800 . ? C15C H15H 0.9800 . ? C15C H15I 0.9800 . ? C16C H16G 0.9800 . ? C16C H16H 0.9800 . ? C16C H16I 0.9800 . ? C19C C21C 1.529(7) . ? C19C C20C 1.534(10) . ? C19C C22C 1.546(7) . ? C19C C20 1.588(12) . ? C20C H20G 0.9800 . ? C20C H20H 0.9800 . ? C20C H20I 0.9800 . ? C20 H20J 0.9800 . ? C20 H20K 0.9800 . ? C20 H20L 0.9800 . ? C21C H21G 0.9800 . ? C21C H21H 0.9800 . ? C21C H21I 0.9800 . ? C22C H22G 0.9800 . ? C22C H22H 0.9800 . ? C22C H22I 0.9800 . ? C25C C28C 1.521(7) . ? C25C C27C 1.523(7) . ? C25C C26C 1.537(8) . ? C26C H26G 0.9800 . ? C26C H26H 0.9800 . ? C26C H26I 0.9800 . ? C27C H27G 0.9800 . ? C27C H27H 0.9800 . ? C27C H27I 0.9800 . ? C28C H28G 0.9800 . ? C28C H28H 0.9800 . ? C28C H28I 0.9800 . ? C31C C32C 1.210(6) . ? C32C C33C 1.444(5) . ? C33C C34C 1.383(5) . ? C33C C38C 1.383(5) . ? C34C C35C 1.386(6) . ? C34C H34C 0.9500 . ? C35C C36C 1.382(6) . ? C35C H35C 0.9500 . ? C36C C37C 1.367(6) . ? C36C H36C 0.9500 . ? C37C C38C 1.410(6) . ? C37C H37C 0.9500 . ? C38C H38C 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Pd1 C31A 179.27(18) . . ? C1A Pd1 P2A 79.90(12) . . ? C31A Pd1 P2A 99.72(12) . . ? C1A Pd1 P1A 80.15(12) . . ? C31A Pd1 P1A 100.24(12) . . ? P2A Pd1 P1A 160.03(4) . . ? O1A P1A C13A 100.9(2) . . ? O1A P1A C7A 100.8(2) . . ? C13A P1A C7A 115.3(2) . . ? O1A P1A Pd1 105.20(11) . . ? C13A P1A Pd1 115.28(18) . . ? C7A P1A Pd1 116.14(16) . . ? O2A P2A C19A 101.04(18) . . ? O2A P2A C25A 100.89(17) . . ? C19A P2A C25A 114.6(2) . . ? O2A P2A Pd1 105.12(11) . . ? C19A P2A Pd1 116.16(15) . . ? C25A P2A Pd1 115.83(13) . . ? C2A O1A P1A 114.7(3) . . ? C6A O2A P2A 114.4(2) . . ? C6A C1A C2A 116.8(4) . . ? C6A C1A Pd1 121.8(3) . . ? C2A C1A Pd1 121.3(3) . . ? C3A C2A C1A 123.0(4) . . ? C3A C2A O1A 118.4(4) . . ? C1A C2A O1A 118.6(4) . . ? C2A C3A C4A 117.5(4) . . ? C2A C3A H3A 121.2 . . ? C4A C3A H3A 121.2 . . ? C5A C4A C3A 122.0(4) . . ? C5A C4A H4A 119.0 . . ? C3A C4A H4A 119.0 . . ? C4A C5A C6A 118.1(4) . . ? C4A C5A H5A 121.0 . . ? C6A C5A H5A 121.0 . . ? C1A C6A O2A 118.6(3) . . ? C1A C6A C5A 122.5(4) . . ? O2A C6A C5A 118.9(4) . . ? C9A C7A C8A 109.1(5) . . ? C9A C7A C10A 110.4(5) . . ? C8A C7A C10A 109.6(4) . . ? C9A C7A P1A 104.6(3) . . ? C8A C7A P1A 109.5(3) . . ? C10A C7A P1A 113.5(4) . . ? C7A C8A H8A 109.5 . . ? C7A C8A H8B 109.5 . . ? H8A C8A H8B 109.5 . . ? C7A C8A H8C 109.5 . . ? H8A C8A H8C 109.5 . . ? H8B C8A H8C 109.5 . . ? C7A C9A H9A 109.5 . . ? C7A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? C7A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? C7A C10A H10A 109.5 . . ? C7A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C7A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C15A C13A C16A 116.9(5) . . ? C15A C13A C14A 108.3(5) . . ? C16A C13A C14A 99.2(5) . . ? C15A C13A C16 97.1(7) . . ? C14A C13A C16 123.8(7) . . ? C15A C13A P1A 110.7(4) . . ? C16A C13A P1A 115.1(5) . . ? C14A C13A P1A 105.0(3) . . ? C16 C13A P1A 111.4(6) . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13A C15A H15A 109.5 . . ? C13A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C13A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13A C16A H16A 109.5 . . ? C13A C16A H16B 109.5 . . ? C13A C16A H16C 109.5 . . ? C13A C16 H16J 109.5 . . ? C13A C16 H16K 109.5 . . ? H16J C16 H16K 109.5 . . ? C13A C16 H16L 109.5 . . ? H16J C16 H16L 109.5 . . ? H16K C16 H16L 109.5 . . ? C21A C19A C22A 108.9(4) . . ? C21A C19A C20A 109.2(4) . . ? C22A C19A C20A 109.9(4) . . ? C21A C19A P2A 110.8(4) . . ? C22A C19A P2A 113.6(3) . . ? C20A C19A P2A 104.4(3) . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C19A C22A H22A 109.5 . . ? C19A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C19A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C26A C25A C28A 107.8(4) . . ? C26A C25A C27A 109.3(4) . . ? C28A C25A C27A 111.0(4) . . ? C26A C25A P2A 105.5(3) . . ? C28A C25A P2A 110.2(3) . . ? C27A C25A P2A 112.8(3) . . ? C25A C26A H26A 109.5 . . ? C25A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25A C27A H27A 109.5 . . ? C25A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C25A C28A H28A 109.5 . . ? C25A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C25A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C32A C31A Pd1 177.7(4) . . ? C31A C32A C33A 178.3(5) . . ? C38A C33A C34A 117.8(4) . . ? C38A C33A C32A 121.3(4) . . ? C34A C33A C32A 120.9(4) . . ? C35A C34A C33A 120.6(4) . . ? C35A C34A H34A 119.7 . . ? C33A C34A H34A 119.7 . . ? C34A C35A C36A 120.9(5) . . ? C34A C35A H35A 119.5 . . ? C36A C35A H35A 119.5 . . ? C37A C36A C35A 119.4(4) . . ? C37A C36A H36A 120.3 . . ? C35A C36A H36A 120.3 . . ? C36A C37A C38A 121.2(5) . . ? C36A C37A H37A 119.4 . . ? C38A C37A H37A 119.4 . . ? C37A C38A C33A 120.2(4) . . ? C37A C38A H38A 119.9 . . ? C33A C38A H38A 119.9 . . ? C1B Pd2 C31B 178.85(17) . . ? C1B Pd2 P2B 80.00(11) . . ? C31B Pd2 P2B 101.00(12) . . ? C1B Pd2 P1B 79.83(11) . . ? C31B Pd2 P1B 99.18(12) . . ? P2B Pd2 P1B 159.79(4) . . ? O1B P1B C7B 101.10(16) . . ? O1B P1B C13B 100.83(19) . . ? C7B P1B C13B 114.63(19) . . ? O1B P1B Pd2 105.19(10) . . ? C7B P1B Pd2 116.17(13) . . ? C13B P1B Pd2 115.77(15) . . ? O2B P2B C19B 100.47(18) . . ? O2B P2B C25B 100.99(17) . . ? C19B P2B C25B 114.36(19) . . ? O2B P2B Pd2 105.21(10) . . ? C19B P2B Pd2 117.29(13) . . ? C25B P2B Pd2 115.21(14) . . ? C2B O1B P1B 114.6(2) . . ? C6B O2B P2B 115.1(2) . . ? C2B C1B C6B 116.6(3) . . ? C2B C1B Pd2 121.9(3) . . ? C6B C1B Pd2 121.5(3) . . ? C1B C2B C3B 123.0(4) . . ? C1B C2B O1B 118.4(3) . . ? C3B C2B O1B 118.6(3) . . ? C4B C3B C2B 117.8(4) . . ? C4B C3B H3B 121.1 . . ? C2B C3B H3B 121.1 . . ? C5B C4B C3B 121.8(4) . . ? C5B C4B H4B 119.1 . . ? C3B C4B H4B 119.1 . . ? C4B C5B C6B 118.2(4) . . ? C4B C5B H5B 120.9 . . ? C6B C5B H5B 120.9 . . ? C5B C6B C1B 122.6(4) . . ? C5B C6B O2B 119.3(3) . . ? C1B C6B O2B 118.1(3) . . ? C8B C7B C9B 108.8(3) . . ? C8B C7B C10B 110.7(3) . . ? C9B C7B C10B 109.1(3) . . ? C8B C7B P1B 110.5(3) . . ? C9B C7B P1B 104.0(3) . . ? C10B C7B P1B 113.5(3) . . ? C7B C8B H8D 109.5 . . ? C7B C8B H8E 109.5 . . ? H8D C8B H8E 109.5 . . ? C7B C8B H8F 109.5 . . ? H8D C8B H8F 109.5 . . ? H8E C8B H8F 109.5 . . ? C7B C9B H9D 109.5 . . ? C7B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C7B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C15B C13B C16B 110.2(4) . . ? C15B C13B C14B 107.7(4) . . ? C16B C13B C14B 109.6(4) . . ? C15B C13B P1B 110.7(3) . . ? C16B C13B P1B 113.6(4) . . ? C14B C13B P1B 104.8(3) . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C13B C16B H16D 109.5 . . ? C13B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C13B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C21B C19B C20B 108.7(4) . . ? C21B C19B C22B 110.5(4) . . ? C20B C19B C22B 107.8(4) . . ? C21B C19B P2B 111.3(3) . . ? C20B C19B P2B 104.8(3) . . ? C22B C19B P2B 113.5(3) . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5 . . ? C19B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C19B C22B H22D 109.5 . . ? C19B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C19B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C27B C25B C28B 110.9(4) . . ? C27B C25B C26B 109.0(4) . . ? C28B C25B C26B 108.9(4) . . ? C27B C25B P2B 113.7(3) . . ? C28B C25B P2B 109.8(3) . . ? C26B C25B P2B 104.2(3) . . ? C25B C26B H26D 109.5 . . ? C25B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C25B C27B H27D 109.5 . . ? C25B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C25B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C25B C28B H28D 109.5 . . ? C25B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C25B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C32B C31B Pd2 175.0(4) . . ? C31B C32B C33B 176.8(4) . . ? C38B C33B C34B 119.1(4) . . ? C38B C33B C32B 120.8(4) . . ? C34B C33B C32B 120.1(4) . . ? C35B C34B C33B 120.4(4) . . ? C35B C34B H34B 119.8 . . ? C33B C34B H34B 119.8 . . ? C34B C35B C36B 120.0(4) . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C37B C36B C35B 120.2(4) . . ? C37B C36B H36B 119.9 . . ? C35B C36B H36B 119.9 . . ? C36B C37B C38B 120.2(4) . . ? C36B C37B H37B 119.9 . . ? C38B C37B H37B 119.9 . . ? C33B C38B C37B 120.1(4) . . ? C33B C38B H38B 119.9 . . ? C37B C38B H38B 119.9 . . ? C1C Pd3 C31C 178.75(18) . . ? C1C Pd3 P2C 80.25(12) . . ? C31C Pd3 P2C 98.77(11) . . ? C1C Pd3 P1C 79.56(11) . . ? C31C Pd3 P1C 101.39(11) . . ? P2C Pd3 P1C 159.79(4) . . ? O1C P1C C13C 100.59(17) . . ? O1C P1C C7C 102.41(17) . . ? C13C P1C C7C 114.78(19) . . ? O1C P1C Pd3 105.75(10) . . ? C13C P1C Pd3 115.67(13) . . ? C7C P1C Pd3 114.98(14) . . ? O2C P2C C19C 101.27(19) . . ? O2C P2C C25C 101.57(19) . . ? C19C P2C C25C 114.0(2) . . ? O2C P2C Pd3 104.99(11) . . ? C19C P2C Pd3 117.62(16) . . ? C25C P2C Pd3 114.43(14) . . ? C2C O1C P1C 114.0(2) . . ? C6C O2C P2C 115.0(2) . . ? C2C C1C C6C 116.7(4) . . ? C2C C1C Pd3 122.0(3) . . ? C6C C1C Pd3 121.2(3) . . ? C1C C2C O1C 118.5(3) . . ? C1C C2C C3C 122.7(4) . . ? O1C C2C C3C 118.8(4) . . ? C4C C3C C2C 117.8(4) . . ? C4C C3C H3C 121.1 . . ? C2C C3C H3C 121.1 . . ? C3C C4C C5C 122.1(4) . . ? C3C C4C H4C 119.0 . . ? C5C C4C H4C 119.0 . . ? C6C C5C C4C 117.6(4) . . ? C6C C5C H5C 121.2 . . ? C4C C5C H5C 121.2 . . ? O2C C6C C5C 118.6(4) . . ? O2C C6C C1C 118.3(3) . . ? C5C C6C C1C 123.1(4) . . ? C8C C7C C10C 110.5(4) . . ? C8C C7C C9C 109.5(4) . . ? C10C C7C C9C 108.5(4) . . ? C8C C7C P1C 109.9(3) . . ? C10C C7C P1C 112.9(3) . . ? C9C C7C P1C 105.3(3) . . ? C7C C8C H8G 109.5 . . ? C7C C8C H8H 109.5 . . ? H8G C8C H8H 109.5 . . ? C7C C8C H8I 109.5 . . ? H8G C8C H8I 109.5 . . ? H8H C8C H8I 109.5 . . ? C7C C9C H9G 109.5 . . ? C7C C9C H9H 109.5 . . ? H9G C9C H9H 109.5 . . ? C7C C9C H9I 109.5 . . ? H9G C9C H9I 109.5 . . ? H9H C9C H9I 109.5 . . ? C7C C10C H10G 109.5 . . ? C7C C10C H10H 109.5 . . ? H10G C10C H10H 109.5 . . ? C7C C10C H10I 109.5 . . ? H10G C10C H10I 109.5 . . ? H10H C10C H10I 109.5 . . ? C15C C13C C14C 108.8(4) . . ? C15C C13C C16C 110.8(3) . . ? C14C C13C C16C 108.2(4) . . ? C15C C13C P1C 109.5(3) . . ? C14C C13C P1C 105.0(3) . . ? C16C C13C P1C 114.3(3) . . ? C13C C14C H14G 109.5 . . ? C13C C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? C13C C14C H14I 109.5 . . ? H14G C14C H14I 109.5 . . ? H14H C14C H14I 109.5 . . ? C13C C15C H15G 109.5 . . ? C13C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C13C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C13C C16C H16G 109.5 . . ? C13C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C13C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C21C C19C C20C 119.8(6) . . ? C21C C19C C22C 110.0(5) . . ? C20C C19C C22C 101.6(6) . . ? C21C C19C C20 92.5(7) . . ? C22C C19C C20 123.9(7) . . ? C21C C19C P2C 110.4(3) . . ? C20C C19C P2C 103.4(5) . . ? C22C C19C P2C 111.2(4) . . ? C20 C19C P2C 107.2(6) . . ? C19C C20C H20G 109.5 . . ? C19C C20C H20H 109.5 . . ? C19C C20C H20I 109.5 . . ? C19C C20 H20J 109.5 . . ? C19C C20 H20K 109.5 . . ? H20J C20 H20K 109.5 . . ? C19C C20 H20L 109.5 . . ? H20J C20 H20L 109.5 . . ? H20K C20 H20L 109.5 . . ? C19C C21C H21G 109.5 . . ? C19C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C19C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C19C C22C H22G 109.5 . . ? C19C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C19C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? C28C C25C C27C 112.1(5) . . ? C28C C25C C26C 108.2(5) . . ? C27C C25C C26C 107.9(5) . . ? C28C C25C P2C 110.9(4) . . ? C27C C25C P2C 114.2(3) . . ? C26C C25C P2C 102.9(3) . . ? C25C C26C H26G 109.5 . . ? C25C C26C H26H 109.5 . . ? H26G C26C H26H 109.5 . . ? C25C C26C H26I 109.5 . . ? H26G C26C H26I 109.5 . . ? H26H C26C H26I 109.5 . . ? C25C C27C H27G 109.5 . . ? C25C C27C H27H 109.5 . . ? H27G C27C H27H 109.5 . . ? C25C C27C H27I 109.5 . . ? H27G C27C H27I 109.5 . . ? H27H C27C H27I 109.5 . . ? C25C C28C H28G 109.5 . . ? C25C C28C H28H 109.5 . . ? H28G C28C H28H 109.5 . . ? C25C C28C H28I 109.5 . . ? H28G C28C H28I 109.5 . . ? H28H C28C H28I 109.5 . . ? C32C C31C Pd3 178.1(4) . . ? C31C C32C C33C 179.0(5) . . ? C34C C33C C38C 119.6(4) . . ? C34C C33C C32C 120.8(4) . . ? C38C C33C C32C 119.6(4) . . ? C33C C34C C35C 120.0(4) . . ? C33C C34C H34C 120.0 . . ? C35C C34C H34C 120.0 . . ? C36C C35C C34C 120.7(4) . . ? C36C C35C H35C 119.6 . . ? C34C C35C H35C 119.6 . . ? C37C C36C C35C 119.7(4) . . ? C37C C36C H36C 120.1 . . ? C35C C36C H36C 120.1 . . ? C36C C37C C38C 120.1(4) . . ? C36C C37C H37C 120.0 . . ? C38C C37C H37C 120.0 . . ? C33C C38C C37C 119.9(4) . . ? C33C C38C H38C 120.1 . . ? C37C C38C H38C 120.1 . . ? 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 C1A Pd1 P1A O1A 1.55(16) . . . . ? C31A Pd1 P1A O1A -179.07(17) . . . . ? P2A Pd1 P1A O1A -0.75(19) . . . . ? C1A Pd1 P1A C13A 111.7(2) . . . . ? C31A Pd1 P1A C13A -68.9(2) . . . . ? P2A Pd1 P1A C13A 109.4(2) . . . . ? C1A Pd1 P1A C7A -109.0(2) . . . . ? C31A Pd1 P1A C7A 70.4(2) . . . . ? P2A Pd1 P1A C7A -111.3(2) . . . . ? C1A Pd1 P2A O2A 2.06(16) . . . . ? C31A Pd1 P2A O2A -177.31(16) . . . . ? P1A Pd1 P2A O2A 4.36(18) . . . . ? C1A Pd1 P2A C19A 112.8(2) . . . . ? C31A Pd1 P2A C19A -66.6(2) . . . . ? P1A Pd1 P2A C19A 115.1(2) . . . . ? C1A Pd1 P2A C25A -108.32(19) . . . . ? C31A Pd1 P2A C25A 72.3(2) . . . . ? P1A Pd1 P2A C25A -106.02(18) . . . . ? C13A P1A O1A C2A -122.5(3) . . . . ? C7A P1A O1A C2A 118.8(3) . . . . ? Pd1 P1A O1A C2A -2.3(3) . . . . ? C19A P2A O2A C6A -124.9(3) . . . . ? C25A P2A O2A C6A 117.1(3) . . . . ? Pd1 P2A O2A C6A -3.7(3) . . . . ? C31A Pd1 C1A C6A 58(15) . . . . ? P2A Pd1 C1A C6A -0.4(3) . . . . ? P1A Pd1 C1A C6A -179.6(3) . . . . ? C31A Pd1 C1A C2A -123(15) . . . . ? P2A Pd1 C1A C2A 178.4(4) . . . . ? P1A Pd1 C1A C2A -0.8(3) . . . . ? C6A C1A C2A C3A -1.2(6) . . . . ? Pd1 C1A C2A C3A 180.0(3) . . . . ? C6A C1A C2A O1A 178.4(3) . . . . ? Pd1 C1A C2A O1A -0.5(5) . . . . ? P1A O1A C2A C3A -178.4(3) . . . . ? P1A O1A C2A C1A 2.0(5) . . . . ? C1A C2A C3A C4A 1.6(7) . . . . ? O1A C2A C3A C4A -177.9(4) . . . . ? C2A C3A C4A C5A -1.2(7) . . . . ? C3A C4A C5A C6A 0.3(7) . . . . ? C2A C1A C6A O2A 179.2(3) . . . . ? Pd1 C1A C6A O2A -1.9(5) . . . . ? C2A C1A C6A C5A 0.2(6) . . . . ? Pd1 C1A C6A C5A 179.1(3) . . . . ? P2A O2A C6A C1A 3.8(5) . . . . ? P2A O2A C6A C5A -177.1(3) . . . . ? C4A C5A C6A C1A 0.2(7) . . . . ? C4A C5A C6A O2A -178.8(4) . . . . ? O1A P1A C7A C9A -63.5(4) . . . . ? C13A P1A C7A C9A -171.2(4) . . . . ? Pd1 P1A C7A C9A 49.5(4) . . . . ? O1A P1A C7A C8A 179.7(3) . . . . ? C13A P1A C7A C8A 72.0(4) . . . . ? Pd1 P1A C7A C8A -67.3(4) . . . . ? O1A P1A C7A C10A 56.8(4) . . . . ? C13A P1A C7A C10A -50.8(5) . . . . ? Pd1 P1A C7A C10A 169.9(4) . . . . ? O1A P1A C13A C15A -166.7(4) . . . . ? C7A P1A C13A C15A -59.1(5) . . . . ? Pd1 P1A C13A C15A 80.6(4) . . . . ? O1A P1A C13A C16A -31.4(4) . . . . ? C7A P1A C13A C16A 76.2(5) . . . . ? Pd1 P1A C13A C16A -144.2(4) . . . . ? O1A P1A C13A C14A 76.6(4) . . . . ? C7A P1A C13A C14A -175.8(4) . . . . ? Pd1 P1A C13A C14A -36.1(5) . . . . ? O1A P1A C13A C16 -59.8(7) . . . . ? C7A P1A C13A C16 47.8(7) . . . . ? Pd1 P1A C13A C16 -172.6(6) . . . . ? O2A P2A C19A C21A -164.0(4) . . . . ? C25A P2A C19A C21A -56.5(4) . . . . ? Pd1 P2A C19A C21A 82.9(4) . . . . ? O2A P2A C19A C22A -41.1(4) . . . . ? C25A P2A C19A C22A 66.4(4) . . . . ? Pd1 P2A C19A C22A -154.2(3) . . . . ? O2A P2A C19A C20A 78.6(3) . . . . ? C25A P2A C19A C20A -173.9(3) . . . . ? Pd1 P2A C19A C20A -34.5(4) . . . . ? O2A P2A C25A C26A -60.9(3) . . . . ? C19A P2A C25A C26A -168.5(3) . . . . ? Pd1 P2A C25A C26A 52.0(3) . . . . ? O2A P2A C25A C28A -176.9(3) . . . . ? C19A P2A C25A C28A 75.5(4) . . . . ? Pd1 P2A C25A C28A -64.1(4) . . . . ? O2A P2A C25A C27A 58.4(4) . . . . ? C19A P2A C25A C27A -49.3(4) . . . . ? Pd1 P2A C25A C27A 171.2(3) . . . . ? C1A Pd1 C31A C32A 72(20) . . . . ? P2A Pd1 C31A C32A 130(10) . . . . ? P1A Pd1 C31A C32A -50(10) . . . . ? Pd1 C31A C32A C33A -54(22) . . . . ? C31A C32A C33A C38A -93(16) . . . . ? C31A C32A C33A C34A 86(16) . . . . ? C38A C33A C34A C35A 1.1(6) . . . . ? C32A C33A C34A C35A -178.2(4) . . . . ? C33A C34A C35A C36A -0.5(7) . . . . ? C34A C35A C36A C37A -0.2(7) . . . . ? C35A C36A C37A C38A 0.4(7) . . . . ? C36A C37A C38A C33A 0.3(7) . . . . ? C34A C33A C38A C37A -1.0(6) . . . . ? C32A C33A C38A C37A 178.3(4) . . . . ? C1B Pd2 P1B O1B -0.63(15) . . . . ? C31B Pd2 P1B O1B 178.78(16) . . . . ? P2B Pd2 P1B O1B -4.39(17) . . . . ? C1B Pd2 P1B C7B -111.47(18) . . . . ? C31B Pd2 P1B C7B 67.94(19) . . . . ? P2B Pd2 P1B C7B -115.23(17) . . . . ? C1B Pd2 P1B C13B 109.7(2) . . . . ? C31B Pd2 P1B C13B -70.9(2) . . . . ? P2B Pd2 P1B C13B 105.9(2) . . . . ? C1B Pd2 P2B O2B 1.53(15) . . . . ? C31B Pd2 P2B O2B -177.91(16) . . . . ? P1B Pd2 P2B O2B 5.28(16) . . . . ? C1B Pd2 P2B C19B 112.1(2) . . . . ? C31B Pd2 P2B C19B -67.3(2) . . . . ? P1B Pd2 P2B C19B 115.9(2) . . . . ? C1B Pd2 P2B C25B -108.75(19) . . . . ? C31B Pd2 P2B C25B 71.82(19) . . . . ? P1B Pd2 P2B C25B -104.99(18) . . . . ? C7B P1B O1B C2B 122.2(3) . . . . ? C13B P1B O1B C2B -119.8(3) . . . . ? Pd2 P1B O1B C2B 0.9(3) . . . . ? C19B P2B O2B C6B -124.1(3) . . . . ? C25B P2B O2B C6B 118.3(3) . . . . ? Pd2 P2B O2B C6B -1.9(3) . . . . ? C31B Pd2 C1B C2B -30(9) . . . . ? P2B Pd2 C1B C2B 179.1(3) . . . . ? P1B Pd2 C1B C2B 0.4(3) . . . . ? C31B Pd2 C1B C6B 150(9) . . . . ? P2B Pd2 C1B C6B -1.2(3) . . . . ? P1B Pd2 C1B C6B -179.9(3) . . . . ? C6B C1B C2B C3B 0.2(6) . . . . ? Pd2 C1B C2B C3B 180.0(3) . . . . ? C6B C1B C2B O1B -179.7(3) . . . . ? Pd2 C1B C2B O1B 0.1(5) . . . . ? P1B O1B C2B C1B -0.7(5) . . . . ? P1B O1B C2B C3B 179.4(3) . . . . ? C1B C2B C3B C4B 0.0(6) . . . . ? O1B C2B C3B C4B 179.9(4) . . . . ? C2B C3B C4B C5B 0.8(6) . . . . ? C3B C4B C5B C6B -1.7(6) . . . . ? C4B C5B C6B C1B 2.0(6) . . . . ? C4B C5B C6B O2B -179.4(3) . . . . ? C2B C1B C6B C5B -1.2(6) . . . . ? Pd2 C1B C6B C5B 179.0(3) . . . . ? C2B C1B C6B O2B -179.9(3) . . . . ? Pd2 C1B C6B O2B 0.3(5) . . . . ? P2B O2B C6B C5B -177.5(3) . . . . ? P2B O2B C6B C1B 1.2(4) . . . . ? O1B P1B C7B C8B 178.6(3) . . . . ? C13B P1B C7B C8B 71.1(3) . . . . ? Pd2 P1B C7B C8B -68.2(3) . . . . ? O1B P1B C7B C9B -64.8(3) . . . . ? C13B P1B C7B C9B -172.3(3) . . . . ? Pd2 P1B C7B C9B 48.4(3) . . . . ? O1B P1B C7B C10B 53.6(3) . . . . ? C13B P1B C7B C10B -53.9(4) . . . . ? Pd2 P1B C7B C10B 166.8(3) . . . . ? O1B P1B C13B C15B -163.9(3) . . . . ? C7B P1B C13B C15B -56.2(4) . . . . ? Pd2 P1B C13B C15B 83.3(4) . . . . ? O1B P1B C13B C16B -39.3(4) . . . . ? C7B P1B C13B C16B 68.4(4) . . . . ? Pd2 P1B C13B C16B -152.1(3) . . . . ? O1B P1B C13B C14B 80.3(4) . . . . ? C7B P1B C13B C14B -172.1(3) . . . . ? Pd2 P1B C13B C14B -32.6(4) . . . . ? O2B P2B C19B C21B -166.9(3) . . . . ? C25B P2B C19B C21B -59.6(4) . . . . ? Pd2 P2B C19B C21B 79.8(4) . . . . ? O2B P2B C19B C20B 75.8(3) . . . . ? C25B P2B C19B C20B -176.9(3) . . . . ? Pd2 P2B C19B C20B -37.5(4) . . . . ? O2B P2B C19B C22B -41.5(4) . . . . ? C25B P2B C19B C22B 65.8(4) . . . . ? Pd2 P2B C19B C22B -154.8(3) . . . . ? O2B P2B C25B C27B 55.7(4) . . . . ? C19B P2B C25B C27B -51.2(4) . . . . ? Pd2 P2B C25B C27B 168.5(3) . . . . ? O2B P2B C25B C28B -179.3(3) . . . . ? C19B P2B C25B C28B 73.8(4) . . . . ? Pd2 P2B C25B C28B -66.5(3) . . . . ? O2B P2B C25B C26B -62.8(3) . . . . ? C19B P2B C25B C26B -169.8(3) . . . . ? Pd2 P2B C25B C26B 49.9(3) . . . . ? C1B Pd2 C31B C32B -29(12) . . . . ? P2B Pd2 C31B C32B 122(4) . . . . ? P1B Pd2 C31B C32B -59(4) . . . . ? Pd2 C31B C32B C33B -1(12) . . . . ? C31B C32B C33B C38B -139(8) . . . . ? C31B C32B C33B C34B 39(8) . . . . ? C38B C33B C34B C35B 0.8(6) . . . . ? C32B C33B C34B C35B -177.1(4) . . . . ? C33B C34B C35B C36B 0.6(6) . . . . ? C34B C35B C36B C37B -1.8(7) . . . . ? C35B C36B C37B C38B 1.6(7) . . . . ? C34B C33B C38B C37B -1.0(6) . . . . ? C32B C33B C38B C37B 176.9(4) . . . . ? C36B C37B C38B C33B -0.2(7) . . . . ? C1C Pd3 P1C O1C 3.40(15) . . . . ? C31C Pd3 P1C O1C -175.77(16) . . . . ? P2C Pd3 P1C O1C 0.27(17) . . . . ? C1C Pd3 P1C C13C 113.73(18) . . . . ? C31C Pd3 P1C C13C -65.4(2) . . . . ? P2C Pd3 P1C C13C 110.60(18) . . . . ? C1C Pd3 P1C C7C -108.80(18) . . . . ? C31C Pd3 P1C C7C 72.03(19) . . . . ? P2C Pd3 P1C C7C -111.93(18) . . . . ? C1C Pd3 P2C O2C 2.77(16) . . . . ? C31C Pd3 P2C O2C -178.04(17) . . . . ? P1C Pd3 P2C O2C 5.90(18) . . . . ? C1C Pd3 P2C C19C 114.4(2) . . . . ? C31C Pd3 P2C C19C -66.4(2) . . . . ? P1C Pd3 P2C C19C 117.5(2) . . . . ? C1C Pd3 P2C C25C -107.7(2) . . . . ? C31C Pd3 P2C C25C 71.5(2) . . . . ? P1C Pd3 P2C C25C -104.6(2) . . . . ? C13C P1C O1C C2C -124.5(3) . . . . ? C7C P1C O1C C2C 116.9(3) . . . . ? Pd3 P1C O1C C2C -3.8(3) . . . . ? C19C P2C O2C C6C -127.8(3) . . . . ? C25C P2C O2C C6C 114.6(3) . . . . ? Pd3 P2C O2C C6C -4.9(3) . . . . ? C31C Pd3 C1C C2C 137(8) . . . . ? P2C Pd3 C1C C2C 175.9(3) . . . . ? P1C Pd3 C1C C2C -3.0(3) . . . . ? C31C Pd3 C1C C6C -40(8) . . . . ? P2C Pd3 C1C C6C -0.6(3) . . . . ? P1C Pd3 C1C C6C -179.5(3) . . . . ? C6C C1C C2C O1C 178.2(3) . . . . ? Pd3 C1C C2C O1C 1.5(5) . . . . ? C6C C1C C2C C3C -2.5(6) . . . . ? Pd3 C1C C2C C3C -179.1(3) . . . . ? P1C O1C C2C C1C 2.0(4) . . . . ? P1C O1C C2C C3C -177.5(3) . . . . ? C1C C2C C3C C4C 0.7(6) . . . . ? O1C C2C C3C C4C -179.9(4) . . . . ? C2C C3C C4C C5C 0.8(6) . . . . ? C3C C4C C5C C6C -0.4(6) . . . . ? P2C O2C C6C C5C -176.8(3) . . . . ? P2C O2C C6C C1C 5.0(5) . . . . ? C4C C5C C6C O2C -179.6(4) . . . . ? C4C C5C C6C C1C -1.5(6) . . . . ? C2C C1C C6C O2C -179.1(3) . . . . ? Pd3 C1C C6C O2C -2.4(5) . . . . ? C2C C1C C6C C5C 2.9(6) . . . . ? Pd3 C1C C6C C5C 179.5(3) . . . . ? O1C P1C C7C C8C -168.8(3) . . . . ? C13C P1C C7C C8C 83.2(3) . . . . ? Pd3 P1C C7C C8C -54.6(3) . . . . ? O1C P1C C7C C10C 67.2(3) . . . . ? C13C P1C C7C C10C -40.7(4) . . . . ? Pd3 P1C C7C C10C -178.6(3) . . . . ? O1C P1C C7C C9C -51.0(3) . . . . ? C13C P1C C7C C9C -159.0(3) . . . . ? Pd3 P1C C7C C9C 63.2(3) . . . . ? O1C P1C C13C C15C -168.7(3) . . . . ? C7C P1C C13C C15C -59.6(3) . . . . ? Pd3 P1C C13C C15C 77.9(3) . . . . ? O1C P1C C13C C14C 74.6(3) . . . . ? C7C P1C C13C C14C -176.3(3) . . . . ? Pd3 P1C C13C C14C -38.7(3) . . . . ? O1C P1C C13C C16C -43.8(3) . . . . ? C7C P1C C13C C16C 65.3(4) . . . . ? Pd3 P1C C13C C16C -157.1(3) . . . . ? O2C P2C C19C C21C -173.4(4) . . . . ? C25C P2C C19C C21C -65.1(4) . . . . ? Pd3 P2C C19C C21C 72.9(4) . . . . ? O2C P2C C19C C20C 57.4(5) . . . . ? C25C P2C C19C C20C 165.6(5) . . . . ? Pd3 P2C C19C C20C -56.3(5) . . . . ? O2C P2C C19C C22C -50.9(4) . . . . ? C25C P2C C19C C22C 57.3(5) . . . . ? Pd3 P2C C19C C22C -164.6(4) . . . . ? O2C P2C C19C C20 87.3(7) . . . . ? C25C P2C C19C C20 -164.5(6) . . . . ? Pd3 P2C C19C C20 -26.4(7) . . . . ? O2C P2C C25C C28C 169.7(4) . . . . ? C19C P2C C25C C28C 61.7(5) . . . . ? Pd3 P2C C25C C28C -77.7(4) . . . . ? O2C P2C C25C C27C 41.9(5) . . . . ? C19C P2C C25C C27C -66.2(5) . . . . ? Pd3 P2C C25C C27C 154.4(4) . . . . ? O2C P2C C25C C26C -74.8(4) . . . . ? C19C P2C C25C C26C 177.2(4) . . . . ? Pd3 P2C C25C C26C 37.7(4) . . . . ? C1C Pd3 C31C C32C 64(16) . . . . ? P2C Pd3 C31C C32C 25(12) . . . . ? P1C Pd3 C31C C32C -156(12) . . . . ? Pd3 C31C C32C C33C -4(36) . . . . ? C31C C32C C33C C34C 170(100) . . . . ? C31C C32C C33C C38C -10(27) . . . . ? C38C C33C C34C C35C -1.1(6) . . . . ? C32C C33C C34C C35C 178.7(4) . . . . ? C33C C34C C35C C36C 0.4(6) . . . . ? C34C C35C C36C C37C 0.9(7) . . . . ? C35C C36C C37C C38C -1.5(7) . . . . ? C34C C33C C38C C37C 0.5(6) . . . . ? C32C C33C C38C C37C -179.2(4) . . . . ? C36C C37C C38C C33C 0.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 31.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.965 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.072 _iucr_refine_instructions_details ; TITL 3A in Pc CELL 0.77490 26.2244 15.8839 11.0864 90.000 96.965 90.000 ZERR 6.00 0.00300 0.00180 0.00120 0.0000 0.0016 0.0000 LATT -1 SYMM X, -Y, 1/2+Z SFAC C H O P PD DISP C -0.00202 0.00197 13.60 DISP O -0.00415 0.00737 40.17 DISP P 0.10128 0.11338 519.87 DISP Pd -1.04371 1.18168 5435.86 UNIT 180 264 12 12 6 TEMP -123.000 L.S. 5 ACTA size 0.05 0.05 0.005 rem colorless plate, als, apex2 bond $h conf mpla 6 c1a c2a c3a c4a c5a c6a mpla 6 c33a c34a c35a c36a c37a c38a mpla 6 c1b c2b c3b c4b c5b c6b mpla 6 c33b c34b c35b c36b c37b c38b mpla 6 c1c c2c c3c c4c c5c c6c mpla 6 c33c c34c c35c c36c c37c c38c dfix 1.5 c19c c20 rem two-component disorder (C16A/C16, C20C/C20) refined isotropic FMAP 2 PLAN 5 TWIN WGHT 0.030700 0.123600 BASF 0.35837 FVAR 0.08624 PD1 5 0.315199 0.752943 0.396768 11.00000 0.02197 0.01838 = 0.01754 -0.00101 0.00377 -0.00234 P1A 4 0.333621 0.803561 0.589025 11.00000 0.03532 0.02600 = 0.01874 -0.00310 0.00186 -0.00151 P2A 4 0.274691 0.680871 0.235855 11.00000 0.02418 0.02173 = 0.01959 -0.00008 0.00293 -0.00379 O1A 3 0.288891 0.763735 0.665572 11.00000 0.03889 0.05121 = 0.01997 -0.00223 0.00639 -0.00335 O2A 3 0.223684 0.637811 0.286567 11.00000 0.02923 0.03190 = 0.02300 0.00141 0.00268 -0.01317 C1A 1 0.256954 0.701912 0.474094 11.00000 0.02356 0.02849 = 0.02205 0.00450 0.00861 0.00172 C2A 1 0.252101 0.714801 0.596375 11.00000 0.02818 0.03476 = 0.02603 0.00691 0.00363 0.00672 C3A 1 0.212560 0.680817 0.652807 11.00000 0.03463 0.06561 = 0.02496 0.01439 0.01439 0.00871 AFIX 43 H3A 2 0.209693 0.691836 0.735939 11.00000 -1.20000 AFIX 0 C4A 1 0.177161 0.629912 0.583282 11.00000 0.02662 0.06872 = 0.04182 0.02575 0.01027 -0.00551 AFIX 43 H4A 2 0.150068 0.605036 0.620519 11.00000 -1.20000 AFIX 0 C5A 1 0.180204 0.614540 0.462436 11.00000 0.02776 0.04659 = 0.03668 0.01316 0.00196 -0.00901 AFIX 43 H5A 2 0.155628 0.579842 0.416120 11.00000 -1.20000 AFIX 0 C6A 1 0.220513 0.651430 0.409569 11.00000 0.02240 0.03008 = 0.02526 0.00610 0.00243 0.00065 C7A 1 0.323099 0.917859 0.609035 11.00000 0.06276 0.03377 = 0.03666 -0.01378 0.00176 0.00401 C8A 1 0.361788 0.967764 0.544032 11.00000 0.09985 0.02716 = 0.03314 0.00149 -0.01024 -0.00450 AFIX 137 H8A 2 0.352425 1.027521 0.541952 11.00000 -1.50000 H8B 2 0.361346 0.946755 0.460798 11.00000 -1.50000 H8C 2 0.396304 0.960888 0.587830 11.00000 -1.50000 AFIX 0 C9A 1 0.269647 0.933762 0.546273 11.00000 0.07345 0.04365 = 0.10522 -0.02830 -0.01169 0.02584 AFIX 137 H9A 2 0.262125 0.994158 0.547875 11.00000 -1.50000 H9B 2 0.244693 0.902911 0.588380 11.00000 -1.50000 H9C 2 0.267405 0.914545 0.461795 11.00000 -1.50000 AFIX 0 C10A 1 0.327071 0.945266 0.743204 11.00000 0.14378 0.05193 = 0.03155 -0.01985 0.01615 0.00093 AFIX 137 H10A 2 0.316949 1.004466 0.747723 11.00000 -1.50000 H10B 2 0.362558 0.938429 0.781225 11.00000 -1.50000 H10C 2 0.304232 0.910332 0.785979 11.00000 -1.50000 AFIX 0 C13A 1 0.392447 0.760437 0.676077 11.00000 0.03703 0.03582 = 0.03340 -0.00300 -0.00801 -0.00827 C14A 1 0.394309 0.667879 0.636586 11.00000 0.08290 0.02943 = 0.11608 0.01619 -0.06046 0.00305 AFIX 137 H14A 2 0.423537 0.639834 0.683566 11.00000 -1.50000 H14B 2 0.398190 0.665099 0.549864 11.00000 -1.50000 H14C 2 0.362387 0.639667 0.651140 11.00000 -1.50000 AFIX 0 C15A 1 0.439885 0.804689 0.641164 11.00000 0.03863 0.06266 = 0.07033 0.01898 0.00456 -0.00234 AFIX 137 H15A 2 0.470367 0.770493 0.666967 11.00000 -1.50000 H15B 2 0.443430 0.859757 0.681163 11.00000 -1.50000 H15C 2 0.436456 0.812360 0.552840 11.00000 -1.50000 AFIX 0 PART 1 10.65 C16A 1 0.389557 0.747656 0.812059 10.65000 0.04304 AFIX 137 H16A 2 0.420710 0.719004 0.848893 10.65000 -1.50000 H16B 2 0.359431 0.713295 0.823084 10.65000 -1.50000 H16C 2 0.386682 0.802493 0.851179 10.65000 -1.50000 AFIX 0 PART 2 10.35 C16 1 0.397961 0.789821 0.811775 10.35000 0.04534 AFIX 137 H16J 2 0.423496 0.754676 0.860133 10.35000 -1.50000 H16K 2 0.364761 0.784438 0.843212 10.35000 -1.50000 H16L 2 0.409079 0.848751 0.816955 10.35000 -1.50000 AFIX 0 PART 0 C19A 1 0.244028 0.744963 0.108934 11.00000 0.03150 0.04505 = 0.02507 0.00314 0.00286 -0.00662 C20A 1 0.224541 0.823424 0.170291 11.00000 0.04973 0.03540 = 0.04909 0.00472 -0.01069 0.00797 AFIX 137 H20A 2 0.205652 0.859567 0.108612 11.00000 -1.50000 H20B 2 0.253826 0.854546 0.211821 11.00000 -1.50000 H20C 2 0.201718 0.806197 0.229569 11.00000 -1.50000 AFIX 0 C21A 1 0.283028 0.771550 0.025481 11.00000 0.04874 0.07228 = 0.03490 0.02357 0.00547 -0.01557 AFIX 137 H21A 2 0.268546 0.816845 -0.028133 11.00000 -1.50000 H21B 2 0.291387 0.723316 -0.023627 11.00000 -1.50000 H21C 2 0.314298 0.791634 0.074392 11.00000 -1.50000 AFIX 0 C22A 1 0.199042 0.700593 0.033048 11.00000 0.03823 0.05778 = 0.02221 0.00378 -0.00702 0.00051 AFIX 137 H22A 2 0.178070 0.742343 -0.015527 11.00000 -1.50000 H22B 2 0.177919 0.671640 0.087268 11.00000 -1.50000 H22C 2 0.212410 0.659465 -0.021052 11.00000 -1.50000 AFIX 0 C25A 1 0.308249 0.586074 0.189506 11.00000 0.03697 0.02831 = 0.02268 -0.01109 0.00557 -0.00124 C26A 1 0.320610 0.533843 0.305680 11.00000 0.07680 0.03423 = 0.04386 -0.00435 0.00373 0.01908 AFIX 137 H26A 2 0.339805 0.483362 0.287698 11.00000 -1.50000 H26B 2 0.288552 0.517227 0.336247 11.00000 -1.50000 H26C 2 0.341375 0.567556 0.367348 11.00000 -1.50000 AFIX 0 C27A 1 0.275125 0.533391 0.093677 11.00000 0.07983 0.03992 = 0.05123 -0.02693 -0.01270 0.00788 AFIX 137 H27A 2 0.291464 0.478574 0.085176 11.00000 -1.50000 H27B 2 0.271787 0.562917 0.015499 11.00000 -1.50000 H27C 2 0.240991 0.525072 0.119220 11.00000 -1.50000 AFIX 0 C28A 1 0.359380 0.610799 0.144812 11.00000 0.05642 0.05383 = 0.08036 -0.00962 0.03398 0.01655 AFIX 137 H28A 2 0.377978 0.559842 0.126128 11.00000 -1.50000 H28B 2 0.380198 0.642895 0.208317 11.00000 -1.50000 H28C 2 0.352591 0.645437 0.071471 11.00000 -1.50000 AFIX 0 C31A 1 0.372943 0.804832 0.317655 11.00000 0.02915 0.03181 = 0.01995 -0.00243 0.00225 0.00205 C32A 1 0.407265 0.838711 0.271674 11.00000 0.02869 0.02682 = 0.02424 0.00150 0.00074 -0.00177 C33A 1 0.447012 0.880853 0.215201 11.00000 0.02048 0.02887 = 0.02233 0.00414 0.00327 0.00021 C34A 1 0.472857 0.951412 0.270515 11.00000 0.02543 0.03505 = 0.03344 0.00167 0.00025 -0.00036 AFIX 43 H34A 2 0.464772 0.970597 0.347107 11.00000 -1.20000 AFIX 0 C35A 1 0.509617 0.992609 0.214548 11.00000 0.02795 0.02975 = 0.05753 0.00586 0.00122 -0.00431 AFIX 43 H35A 2 0.526483 1.040283 0.252691 11.00000 -1.20000 AFIX 0 C36A 1 0.522368 0.965753 0.103861 11.00000 0.03544 0.04062 = 0.05539 0.02182 0.01565 0.00056 AFIX 43 H36A 2 0.547743 0.994792 0.065727 11.00000 -1.20000 AFIX 0 C37A 1 0.498039 0.896583 0.049170 11.00000 0.04503 0.04742 = 0.03527 0.01108 0.01832 0.00658 AFIX 43 H37A 2 0.506957 0.877844 -0.026908 11.00000 -1.20000 AFIX 0 C38A 1 0.460829 0.853798 0.102872 11.00000 0.03214 0.03159 = 0.03000 0.00417 0.00491 0.00240 AFIX 43 H38A 2 0.444541 0.805972 0.063778 11.00000 -1.20000 AFIX 0 PD2 5 0.667340 0.251218 0.178071 11.00000 0.02234 0.01765 = 0.01364 0.00086 0.00440 0.00192 P1B 4 0.643770 0.301147 -0.013413 11.00000 0.02617 0.02300 = 0.01464 0.00030 0.00296 0.00082 P2B 4 0.713061 0.181521 0.334794 11.00000 0.02495 0.01906 = 0.01605 0.00229 0.00224 0.00046 O1B 3 0.690021 0.270305 -0.093517 11.00000 0.03088 0.03293 = 0.01503 0.00325 0.00548 0.00497 O2B 3 0.764157 0.144237 0.278588 11.00000 0.02654 0.02554 = 0.02505 0.00647 0.00558 0.00465 C1B 1 0.726160 0.207791 0.093638 11.00000 0.02064 0.01678 = 0.02056 -0.00228 0.00576 0.00121 C2B 1 0.729163 0.223094 -0.027943 11.00000 0.02850 0.02423 = 0.01991 0.00007 0.00828 -0.00268 C3B 1 0.769220 0.193916 -0.087878 11.00000 0.03448 0.03216 = 0.02705 -0.00163 0.01080 -0.00108 AFIX 43 H3B 2 0.770257 0.205447 -0.171628 11.00000 -1.20000 AFIX 0 C4B 1 0.807546 0.147535 -0.021695 11.00000 0.03016 0.03267 = 0.03415 -0.00449 0.01318 0.00136 AFIX 43 H4B 2 0.835484 0.127610 -0.060846 11.00000 -1.20000 AFIX 0 C5B 1 0.806327 0.129434 0.099415 11.00000 0.02519 0.02835 = 0.03673 -0.00038 0.00790 0.00226 AFIX 43 H5B 2 0.832442 0.096212 0.143201 11.00000 -1.20000 AFIX 0 C6B 1 0.765981 0.160991 0.155652 11.00000 0.02665 0.01902 = 0.02193 -0.00148 0.00606 -0.00132 C7B 1 0.646383 0.416799 -0.032330 11.00000 0.03369 0.01652 = 0.02254 0.00660 0.00154 0.00112 C8B 1 0.605502 0.459359 0.032410 11.00000 0.04170 0.02877 = 0.02755 0.00097 0.00588 0.00718 AFIX 137 H8D 2 0.612033 0.520092 0.036950 11.00000 -1.50000 H8E 2 0.606522 0.436417 0.114726 11.00000 -1.50000 H8F 2 0.571580 0.449020 -0.012685 11.00000 -1.50000 AFIX 0 C9B 1 0.699654 0.441316 0.031902 11.00000 0.03870 0.02673 = 0.04198 0.00567 0.00692 -0.00473 AFIX 137 H9D 2 0.704144 0.502421 0.026998 11.00000 -1.50000 H9E 2 0.726331 0.412950 -0.007762 11.00000 -1.50000 H9F 2 0.702405 0.424188 0.117367 11.00000 -1.50000 AFIX 0 C10B 1 0.642191 0.445083 -0.166303 11.00000 0.06236 0.03611 = 0.02566 0.01236 0.01133 0.00793 AFIX 137 H10D 2 0.645935 0.506386 -0.169958 11.00000 -1.50000 H10E 2 0.608589 0.428687 -0.208148 11.00000 -1.50000 H10F 2 0.669386 0.418143 -0.205902 11.00000 -1.50000 AFIX 0 C13B 1 0.586893 0.249627 -0.099529 11.00000 0.03842 0.04024 = 0.01643 0.00029 -0.00182 -0.00929 C14B 1 0.589201 0.157731 -0.055341 11.00000 0.06830 0.03551 = 0.06390 -0.00449 -0.02248 -0.00875 AFIX 137 H14D 2 0.560463 0.126099 -0.098327 11.00000 -1.50000 H14E 2 0.586904 0.156252 0.032207 11.00000 -1.50000 H14F 2 0.621705 0.132308 -0.071756 11.00000 -1.50000 AFIX 0 C15B 1 0.537565 0.287920 -0.066046 11.00000 0.02799 0.05048 = 0.07920 -0.01543 -0.00564 -0.00625 AFIX 137 H15D 2 0.508220 0.254498 -0.102273 11.00000 -1.50000 H15E 2 0.534255 0.345759 -0.096766 11.00000 -1.50000 H15F 2 0.538329 0.288260 0.022551 11.00000 -1.50000 AFIX 0 C16B 1 0.587341 0.251786 -0.236441 11.00000 0.07349 0.11053 = 0.01993 -0.00963 -0.00880 -0.03467 AFIX 137 H16D 2 0.558930 0.217612 -0.275682 11.00000 -1.50000 H16E 2 0.620004 0.229113 -0.256690 11.00000 -1.50000 H16F 2 0.583379 0.310024 -0.265240 11.00000 -1.50000 AFIX 0 C19B 1 0.744243 0.245672 0.462285 11.00000 0.03719 0.02174 = 0.02335 -0.00339 -0.00721 -0.00102 C20B 1 0.763009 0.325063 0.402066 11.00000 0.05923 0.02797 = 0.04157 0.00414 -0.01388 -0.01858 AFIX 137 H20D 2 0.782656 0.360220 0.463814 11.00000 -1.50000 H20E 2 0.733378 0.356816 0.363506 11.00000 -1.50000 H20F 2 0.784971 0.308821 0.340444 11.00000 -1.50000 AFIX 0 C21B 1 0.705626 0.271760 0.548876 11.00000 0.07129 0.06108 = 0.04289 -0.02223 0.00904 -0.00872 AFIX 137 H21D 2 0.719862 0.318415 0.600166 11.00000 -1.50000 H21E 2 0.698873 0.223813 0.600263 11.00000 -1.50000 H21F 2 0.673482 0.289712 0.501500 11.00000 -1.50000 AFIX 0 C22B 1 0.791453 0.202715 0.533136 11.00000 0.04773 0.04273 = 0.04008 -0.00490 -0.01783 -0.00089 AFIX 137 H22D 2 0.805814 0.239327 0.599907 11.00000 -1.50000 H22E 2 0.817460 0.192539 0.478365 11.00000 -1.50000 H22F 2 0.781078 0.148987 0.566146 11.00000 -1.50000 AFIX 0 C25B 1 0.683307 0.082689 0.381955 11.00000 0.03588 0.02088 = 0.02972 0.00383 0.00829 -0.00483 C26B 1 0.669529 0.034071 0.262548 11.00000 0.08641 0.03093 = 0.04006 -0.00220 0.00511 -0.02686 AFIX 137 H26D 2 0.652296 -0.018681 0.279152 11.00000 -1.50000 H26E 2 0.700957 0.021547 0.226322 11.00000 -1.50000 H26F 2 0.646552 0.068353 0.206050 11.00000 -1.50000 AFIX 0 C27B 1 0.718998 0.029323 0.468194 11.00000 0.05668 0.02984 = 0.05557 0.02221 0.00754 -0.00202 AFIX 137 H27D 2 0.703595 -0.026275 0.476453 11.00000 -1.50000 H27E 2 0.724517 0.056718 0.547914 11.00000 -1.50000 H27F 2 0.751986 0.022977 0.436042 11.00000 -1.50000 AFIX 0 C28B 1 0.634055 0.102849 0.436186 11.00000 0.05575 0.03807 = 0.06915 0.01128 0.03232 -0.00843 AFIX 137 H28D 2 0.613031 0.051874 0.436730 11.00000 -1.50000 H28E 2 0.614814 0.146320 0.387151 11.00000 -1.50000 H28F 2 0.642636 0.123320 0.519566 11.00000 -1.50000 AFIX 0 C31B 1 0.608171 0.296788 0.260491 11.00000 0.02745 0.02499 = 0.02137 0.00511 0.00479 0.00637 C32B 1 0.573913 0.330112 0.307115 11.00000 0.02744 0.02965 = 0.02043 0.00101 0.00507 0.00001 C33B 1 0.534417 0.373982 0.360234 11.00000 0.02548 0.02486 = 0.02407 -0.00611 0.00355 0.00002 C34B 1 0.510080 0.444073 0.300682 11.00000 0.02825 0.03030 = 0.02347 0.00382 0.00199 -0.00144 AFIX 43 H34B 2 0.518773 0.460619 0.223399 11.00000 -1.20000 AFIX 0 C35B 1 0.473467 0.489140 0.354197 11.00000 0.02337 0.03366 = 0.04469 -0.00646 0.00255 0.00431 AFIX 43 H35B 2 0.456929 0.536088 0.313251 11.00000 -1.20000 AFIX 0 C36B 1 0.461000 0.465591 0.467667 11.00000 0.02954 0.03295 = 0.05415 -0.01375 0.01645 0.00246 AFIX 43 H36B 2 0.436654 0.497465 0.505286 11.00000 -1.20000 AFIX 0 C37B 1 0.483860 0.396089 0.525850 11.00000 0.04629 0.04802 = 0.03391 -0.01262 0.02096 -0.00708 AFIX 43 H37B 2 0.474561 0.379351 0.602499 11.00000 -1.20000 AFIX 0 C38B 1 0.520836 0.349972 0.472195 11.00000 0.03334 0.02550 = 0.02497 0.00055 0.00373 -0.00020 AFIX 43 H38B 2 0.536576 0.302219 0.512711 11.00000 -1.20000 AFIX 0 PD3 5 1.000865 0.750012 -0.000148 11.00000 0.02480 0.01982 = 0.02227 -0.00174 0.00559 -0.00255 P1C 4 1.001083 0.679609 -0.178786 11.00000 0.02777 0.02521 = 0.02199 -0.00155 0.00737 -0.00376 P2C 4 1.023833 0.843258 0.151477 11.00000 0.04194 0.01985 = 0.02597 -0.00223 0.00703 -0.00358 O1C 3 1.048541 0.721278 -0.245174 11.00000 0.03450 0.03166 = 0.02784 -0.00181 0.01209 -0.00583 O2C 3 1.068370 0.903075 0.100856 11.00000 0.05251 0.02571 = 0.03238 -0.00210 0.00801 -0.01385 C1C 1 1.056668 0.812449 -0.071992 11.00000 0.02036 0.02194 = 0.02472 0.00466 0.00164 -0.00099 C2C 1 1.072837 0.788987 -0.182117 11.00000 0.02713 0.02786 = 0.02932 0.00832 0.00185 0.00328 C3C 1 1.112312 0.831300 -0.232800 11.00000 0.03624 0.03991 = 0.02675 0.00764 0.00976 0.00548 AFIX 43 H3C 2 1.122391 0.814468 -0.308657 11.00000 -1.20000 AFIX 0 C4C 1 1.135892 0.897988 -0.168791 11.00000 0.03225 0.03899 = 0.04367 0.01574 0.00935 -0.00312 AFIX 43 H4C 2 1.162336 0.927701 -0.202137 11.00000 -1.20000 AFIX 0 C5C 1 1.122079 0.923288 -0.056171 11.00000 0.03134 0.02890 = 0.04212 0.00784 -0.00391 -0.00483 AFIX 43 H5C 2 1.138789 0.969125 -0.012769 11.00000 -1.20000 AFIX 0 C6C 1 1.082965 0.878815 -0.010129 11.00000 0.03242 0.02738 = 0.02715 0.00639 0.00152 -0.00124 C7C 1 0.944449 0.699127 -0.292225 11.00000 0.03095 0.03484 = 0.03281 -0.00262 0.00153 -0.00539 C8C 1 0.895372 0.680607 -0.236577 11.00000 0.03772 0.05397 = 0.04279 -0.00399 -0.00135 -0.00219 AFIX 137 H8G 2 0.865598 0.697850 -0.293244 11.00000 -1.50000 H8H 2 0.895656 0.711905 -0.160321 11.00000 -1.50000 H8I 2 0.893261 0.620139 -0.220334 11.00000 -1.50000 AFIX 0 C9C 1 0.946677 0.793638 -0.322716 11.00000 0.04858 0.03896 = 0.05351 0.00767 -0.00665 -0.00321 AFIX 137 H9G 2 0.917140 0.808524 -0.381678 11.00000 -1.50000 H9H 2 0.978529 0.805704 -0.357419 11.00000 -1.50000 H9I 2 0.945779 0.826772 -0.248436 11.00000 -1.50000 AFIX 0 C10C 1 0.945803 0.648502 -0.410011 11.00000 0.05448 0.06412 = 0.02830 -0.00357 -0.00226 -0.01171 AFIX 137 H10G 2 0.917382 0.666321 -0.470211 11.00000 -1.50000 H10H 2 0.942383 0.588369 -0.392912 11.00000 -1.50000 H10I 2 0.978508 0.658551 -0.441982 11.00000 -1.50000 AFIX 0 C13C 1 1.021971 0.568818 -0.165777 11.00000 0.04388 0.02293 = 0.02941 -0.00228 0.01488 -0.00025 C14C 1 1.066277 0.567937 -0.062006 11.00000 0.05029 0.03331 = 0.04802 0.00544 0.00300 0.01437 AFIX 137 H14G 2 1.078999 0.510246 -0.048891 11.00000 -1.50000 H14H 2 1.054032 0.588913 0.012482 11.00000 -1.50000 H14I 2 1.094126 0.604088 -0.083264 11.00000 -1.50000 AFIX 0 C15C 1 0.978313 0.514643 -0.129582 11.00000 0.05650 0.02936 = 0.04077 0.00068 0.01133 -0.00524 AFIX 137 H15G 2 0.991475 0.458593 -0.105560 11.00000 -1.50000 H15H 2 0.951419 0.509511 -0.198716 11.00000 -1.50000 H15I 2 0.963978 0.540997 -0.061200 11.00000 -1.50000 AFIX 0 C16C 1 1.042273 0.533114 -0.281828 11.00000 0.06811 0.04330 = 0.04147 -0.00611 0.02204 0.00520 AFIX 137 H16G 2 1.058598 0.478377 -0.263206 11.00000 -1.50000 H16H 2 1.067458 0.572207 -0.308953 11.00000 -1.50000 H16I 2 1.013535 0.526297 -0.346334 11.00000 -1.50000 AFIX 0 C19C 1 0.975596 0.923492 0.183473 11.00000 0.06343 0.02935 = 0.04907 -0.00687 0.01808 0.01014 PART 1 10.60 C20C 1 0.962270 0.967682 0.060714 10.60000 0.06197 AFIX 137 H20G 2 0.935515 1.009899 0.067495 10.60000 -1.50000 H20H 2 0.949767 0.926067 -0.001157 10.60000 -1.50000 H20I 2 0.993013 0.995321 0.037354 10.60000 -1.50000 AFIX 0 PART 2 10.40 C20 1 0.938456 0.937689 0.060967 10.40000 0.06135 AFIX 137 H20J 2 0.913315 0.981507 0.073450 10.40000 -1.50000 H20K 2 0.920463 0.885058 0.037288 10.40000 -1.50000 H20L 2 0.958678 0.955260 -0.003416 10.40000 -1.50000 AFIX 0 PART 0 C21C 1 0.932995 0.882830 0.246195 11.00000 0.06571 0.05130 = 0.13036 -0.01684 0.04467 0.00634 AFIX 137 H21G 2 0.903830 0.921617 0.243845 11.00000 -1.50000 H21H 2 0.946001 0.870262 0.330902 11.00000 -1.50000 H21I 2 0.921847 0.830545 0.204045 11.00000 -1.50000 AFIX 0 C22C 1 1.000949 0.995794 0.262741 11.00000 0.10081 0.04269 = 0.13223 -0.04331 0.04384 -0.00937 AFIX 137 H22G 2 0.978056 1.044772 0.256743 11.00000 -1.50000 H22H 2 1.033632 1.011131 0.234138 11.00000 -1.50000 H22I 2 1.007226 0.977298 0.347574 11.00000 -1.50000 AFIX 0 C25C 1 1.059999 0.796251 0.290266 11.00000 0.05878 0.03232 = 0.02810 0.00320 -0.00319 -0.00748 C26C 1 1.094227 0.730424 0.237944 11.00000 0.06682 0.08204 = 0.05104 0.00708 -0.00999 0.02847 AFIX 137 H26G 2 1.115344 0.701810 0.304620 11.00000 -1.50000 H26H 2 1.116572 0.758422 0.185599 11.00000 -1.50000 H26I 2 1.072591 0.689063 0.190246 11.00000 -1.50000 AFIX 0 C27C 1 1.094839 0.858019 0.366117 11.00000 0.12338 0.06125 = 0.05308 0.00037 -0.01906 -0.03129 AFIX 137 H27G 2 1.119834 0.826793 0.421949 11.00000 -1.50000 H27H 2 1.074075 0.894018 0.412856 11.00000 -1.50000 H27I 2 1.113032 0.893001 0.312369 11.00000 -1.50000 AFIX 0 C28C 1 1.023958 0.750399 0.365590 11.00000 0.07527 0.09923 = 0.04788 0.03872 0.00015 -0.02423 AFIX 137 H28G 2 1.043943 0.713255 0.424046 11.00000 -1.50000 H28H 2 0.999408 0.716823 0.311892 11.00000 -1.50000 H28I 2 1.005298 0.791572 0.409375 11.00000 -1.50000 AFIX 0 C31C 1 0.945780 0.687457 0.075563 11.00000 0.03791 0.02643 = 0.02574 -0.00230 0.00880 -0.00190 C32C 1 0.912557 0.651970 0.122898 11.00000 0.02730 0.03426 = 0.02451 0.00103 0.00092 -0.00016 C33C 1 0.872831 0.610922 0.180771 11.00000 0.02364 0.02446 = 0.02582 0.00573 0.00334 0.00440 C34C 1 0.850747 0.536782 0.134606 11.00000 0.02721 0.02826 = 0.03510 -0.00041 -0.00084 0.00273 AFIX 43 H34C 2 0.861176 0.512856 0.062978 11.00000 -1.20000 AFIX 0 C35C 1 0.813405 0.497386 0.192818 11.00000 0.02321 0.02659 = 0.06037 0.00146 0.00182 -0.00212 AFIX 43 H35C 2 0.798506 0.446300 0.160942 11.00000 -1.20000 AFIX 0 C36C 1 0.797594 0.531596 0.296754 11.00000 0.03058 0.03272 = 0.06177 0.01159 0.01892 -0.00057 AFIX 43 H36C 2 0.772334 0.503713 0.336720 11.00000 -1.20000 AFIX 0 C37C 1 0.818468 0.605743 0.341800 11.00000 0.04648 0.02788 = 0.04285 0.00592 0.02103 0.00337 AFIX 43 H37C 2 0.807124 0.630126 0.412118 11.00000 -1.20000 AFIX 0 C38C 1 0.856812 0.646045 0.283985 11.00000 0.04132 0.02437 = 0.03206 0.00082 0.00887 0.00343 AFIX 43 H38C 2 0.871613 0.697205 0.315841 11.00000 -1.20000 HKLF 4 REM 3A in Pc REM R1 = 0.0389 for 18123 Fo > 4sig(Fo) and 0.0540 for all 22449 data REM 983 parameters refined using 3 restraints END WGHT 0.0307 0.1237 REM Highest difference peak 0.965, deepest hole -0.506, 1-sigma level 0.072 Q1 1 0.9776 0.7512 0.0371 11.00000 0.05 0.96 Q2 1 0.6342 0.2458 0.1653 11.00000 0.05 0.85 Q3 1 0.6410 0.2477 0.2488 11.00000 0.05 0.78 Q4 1 0.3384 0.7459 0.3682 11.00000 0.05 0.75 Q5 1 0.3575 0.7509 0.3302 11.00000 0.05 0.72 ; _database_code_depnum_ccdc_archive 'CCDC 965923' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4B _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 O2 P2 Pd' _chemical_formula_sum 'C26 H38 O2 P2 Pd' _chemical_formula_weight 550.90 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' 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 P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.8023(2) _cell_length_b 14.4839(4) _cell_length_c 12.0669(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.659(2) _cell_angle_gamma 90.00 _cell_volume 1335.52(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7155 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 66.87 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 6.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3261 _exptl_absorpt_correction_T_max 0.3707 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(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 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 10793 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 67.28 _reflns_number_total 2453 _reflns_number_gt 2219 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.634' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0480P)^2^+0.3075P] 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_number_reflns 2453 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Pd Pd 0.24755(3) 0.2500 0.758012(18) 0.02528(11) Uani 1 2 d S . . P1 P 0.28122(8) 0.09681(5) 0.73679(5) 0.02888(16) Uani 1 1 d . . . O1 O 0.3707(3) 0.08481(13) 0.62374(15) 0.0416(5) Uani 1 1 d . . . C1 C 0.3700(4) 0.2500 0.6246(3) 0.0330(8) Uani 1 2 d S . . C2 C 0.4178(3) 0.1680(2) 0.5794(2) 0.0386(7) Uani 1 1 d . . . C3 C 0.5090(4) 0.1661(2) 0.4911(2) 0.0498(8) Uani 1 1 d . . . H3 H 0.5404 0.1094 0.4609 0.060 Uiso 1 1 calc R . . C4 C 0.5518(5) 0.2500 0.4493(3) 0.0547(13) Uani 1 2 d S . . H4 H 0.6135 0.2500 0.3890 0.066 Uiso 1 2 calc SR . . C7 C 0.4434(3) 0.04006(17) 0.8462(2) 0.0321(5) Uani 1 1 d . . . H7 H 0.3898 0.0323 0.9143 0.039 Uiso 1 1 calc R . . C8 C 0.6025(3) 0.1035(2) 0.8799(2) 0.0411(6) Uani 1 1 d . . . H8A H 0.6903 0.0732 0.9381 0.062 Uiso 1 1 calc R . . H8B H 0.5661 0.1616 0.9099 0.062 Uiso 1 1 calc R . . H8C H 0.6528 0.1163 0.8134 0.062 Uiso 1 1 calc R . . C9 C 0.4966(4) -0.05535(19) 0.8124(2) 0.0433(7) Uani 1 1 d . . . H9A H 0.5801 -0.0827 0.8754 0.065 Uiso 1 1 calc R . . H9B H 0.5513 -0.0500 0.7463 0.065 Uiso 1 1 calc R . . H9C H 0.3927 -0.0948 0.7935 0.065 Uiso 1 1 calc R . . C10 C 0.0918(3) 0.02041(19) 0.7029(2) 0.0419(7) Uani 1 1 d . . . H10 H 0.1282 -0.0380 0.6699 0.050 Uiso 1 1 calc R . . C11 C -0.0498(4) 0.0679(2) 0.6137(3) 0.0625(10) Uani 1 1 d . . . H11A H -0.1466 0.0248 0.5882 0.094 Uiso 1 1 calc R . . H11B H 0.0005 0.0865 0.5490 0.094 Uiso 1 1 calc R . . H11C H -0.0935 0.1225 0.6470 0.094 Uiso 1 1 calc R . . C12 C 0.0248(4) -0.0033(2) 0.8099(3) 0.0495(7) Uani 1 1 d . . . H12A H -0.0868 -0.0363 0.7892 0.074 Uiso 1 1 calc R . . H12B H 0.0077 0.0537 0.8501 0.074 Uiso 1 1 calc R . . H12C H 0.1105 -0.0425 0.8590 0.074 Uiso 1 1 calc R . . C27 C 0.1237(4) 0.2500 0.8940(3) 0.0267(7) Uani 1 2 d S . . H27 H -0.0006 0.2500 0.8752 0.032 Uiso 1 2 calc SR . . C28 C 0.1931(4) 0.2500 1.0041(3) 0.0262(7) Uani 1 2 d S . . H28 H 0.3173 0.2500 1.0236 0.031 Uiso 1 2 calc SR . . C29 C 0.1012(4) 0.2500 1.1001(3) 0.0262(7) Uani 1 2 d S . . C30 C 0.1971(4) 0.2500 1.2116(3) 0.0283(7) Uani 1 2 d S . . H30 H 0.3213 0.2500 1.2246 0.034 Uiso 1 2 calc SR . . C31 C 0.1150(5) 0.2500 1.3033(3) 0.0349(8) Uani 1 2 d S . . H31 H 0.1829 0.2500 1.3781 0.042 Uiso 1 2 calc SR . . C32 C -0.0654(5) 0.2500 1.2857(3) 0.0398(9) Uani 1 2 d S . . H32 H -0.1221 0.2500 1.3484 0.048 Uiso 1 2 calc SR . . C33 C -0.1631(5) 0.2500 1.1766(3) 0.0381(9) Uani 1 2 d S . . H33 H -0.2872 0.2500 1.1644 0.046 Uiso 1 2 calc SR . . C34 C -0.0814(4) 0.2500 1.0849(3) 0.0300(7) Uani 1 2 d S . . H34 H -0.1505 0.2500 1.0105 0.036 Uiso 1 2 calc SR . . 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 Pd 0.02807(15) 0.02963(16) 0.01810(15) 0.000 0.00461(9) 0.000 P1 0.0320(3) 0.0314(3) 0.0218(3) -0.0050(2) 0.0019(2) 0.0050(2) O1 0.0515(11) 0.0499(12) 0.0236(9) -0.0056(8) 0.0080(8) 0.0168(9) C1 0.0268(17) 0.056(2) 0.0160(16) 0.000 0.0037(12) 0.000 C2 0.0316(14) 0.063(2) 0.0188(12) -0.0022(11) 0.0001(10) 0.0081(12) C3 0.0346(14) 0.091(3) 0.0231(14) -0.0060(13) 0.0041(11) 0.0161(15) C4 0.027(2) 0.114(4) 0.023(2) 0.000 0.0065(15) 0.000 C7 0.0332(13) 0.0376(14) 0.0249(12) -0.0002(10) 0.0042(9) 0.0044(11) C8 0.0337(14) 0.0458(16) 0.0390(15) 0.0003(12) -0.0038(11) 0.0030(12) C9 0.0413(15) 0.0392(15) 0.0460(16) -0.0042(12) 0.0006(12) 0.0101(12) C10 0.0338(14) 0.0354(15) 0.0521(17) -0.0156(12) -0.0018(12) 0.0010(12) C11 0.0483(19) 0.059(2) 0.066(2) -0.0185(16) -0.0212(16) 0.0100(15) C12 0.0334(15) 0.0435(17) 0.072(2) -0.0084(14) 0.0114(13) -0.0052(12) C27 0.0280(17) 0.0240(17) 0.0290(18) 0.000 0.0081(13) 0.000 C28 0.0258(16) 0.0291(17) 0.0247(17) 0.000 0.0075(12) 0.000 C29 0.0278(17) 0.0250(17) 0.0260(17) 0.000 0.0059(13) 0.000 C30 0.0266(16) 0.0332(18) 0.0256(17) 0.000 0.0062(13) 0.000 C31 0.041(2) 0.041(2) 0.0246(18) 0.000 0.0090(14) 0.000 C32 0.041(2) 0.050(2) 0.035(2) 0.000 0.0222(16) 0.000 C33 0.0284(18) 0.043(2) 0.045(2) 0.000 0.0126(16) 0.000 C34 0.0278(17) 0.0328(19) 0.0288(18) 0.000 0.0045(13) 0.000 _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 Pd C1 2.031(3) . ? Pd C27 2.066(3) . ? Pd P1 2.2549(6) 4_565 ? Pd P1 2.2549(6) . ? P1 O1 1.6622(18) . ? P1 C10 1.825(3) . ? P1 C7 1.829(2) . ? O1 C2 1.397(3) . ? C1 C2 1.389(3) . ? C1 C2 1.389(3) 4_565 ? C2 C3 1.396(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C3 1.382(4) 4_565 ? C4 H4 0.9500 . ? C7 C9 1.523(4) . ? C7 C8 1.532(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.527(4) . ? C10 C11 1.540(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C27 C28 1.329(5) . ? C27 H27 0.9500 . ? C28 C29 1.480(4) . ? C28 H28 0.9500 . ? C29 C34 1.400(5) . ? C29 C30 1.401(5) . ? C30 C31 1.386(5) . ? C30 H30 0.9500 . ? C31 C32 1.380(5) . ? C31 H31 0.9500 . ? C32 C33 1.382(5) . ? C32 H32 0.9500 . ? C33 C34 1.383(5) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd C27 179.84(12) . . ? C1 Pd P1 79.964(18) . 4_565 ? C27 Pd P1 100.030(18) . 4_565 ? C1 Pd P1 79.964(18) . . ? C27 Pd P1 100.030(18) . . ? P1 Pd P1 159.45(3) 4_565 . ? O1 P1 C10 101.99(12) . . ? O1 P1 C7 101.65(10) . . ? C10 P1 C7 107.45(13) . . ? O1 P1 Pd 105.90(7) . . ? C10 P1 Pd 120.96(9) . . ? C7 P1 Pd 116.08(8) . . ? C2 O1 P1 114.24(16) . . ? C2 C1 C2 117.6(3) . 4_565 ? C2 C1 Pd 121.18(16) . . ? C2 C1 Pd 121.18(16) 4_565 . ? C1 C2 C3 122.4(3) . . ? C1 C2 O1 118.3(2) . . ? C3 C2 O1 119.3(3) . . ? C4 C3 C2 117.3(3) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C3 123.1(4) 4_565 . ? C3 C4 H4 118.5 4_565 . ? C3 C4 H4 118.5 . . ? C9 C7 C8 111.4(2) . . ? C9 C7 P1 113.60(18) . . ? C8 C7 P1 109.10(18) . . ? C9 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? P1 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.8(3) . . ? C12 C10 P1 110.30(18) . . ? C11 C10 P1 108.7(2) . . ? C12 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? P1 C10 H10 108.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C28 C27 Pd 129.2(3) . . ? C28 C27 H27 115.4 . . ? Pd C27 H27 115.4 . . ? C27 C28 C29 128.2(3) . . ? C27 C28 H28 115.9 . . ? C29 C28 H28 115.9 . . ? C34 C29 C30 117.2(3) . . ? C34 C29 C28 122.6(3) . . ? C30 C29 C28 120.2(3) . . ? C31 C30 C29 121.6(3) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.7(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C34 120.5(3) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 121.1(3) . . ? C33 C34 H34 119.4 . . ? C29 C34 H34 119.4 . . ? 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 C1 Pd P1 O1 -3.35(11) . . . . ? C27 Pd P1 O1 176.81(11) . . . . ? P1 Pd P1 O1 -15.89(13) 4_565 . . . ? C1 Pd P1 C10 -118.36(15) . . . . ? C27 Pd P1 C10 61.80(15) . . . . ? P1 Pd P1 C10 -130.90(13) 4_565 . . . ? C1 Pd P1 C7 108.56(13) . . . . ? C27 Pd P1 C7 -71.28(14) . . . . ? P1 Pd P1 C7 96.02(12) 4_565 . . . ? C10 P1 O1 C2 133.63(18) . . . . ? C7 P1 O1 C2 -115.47(18) . . . . ? Pd P1 O1 C2 6.23(18) . . . . ? C27 Pd C1 C2 88.2(4) . . . . ? P1 Pd C1 C2 175.9(3) 4_565 . . . ? P1 Pd C1 C2 0.4(2) . . . . ? C27 Pd C1 C2 -88.2(5) . . . 4_565 ? P1 Pd C1 C2 -0.4(2) 4_565 . . 4_565 ? P1 Pd C1 C2 -175.9(3) . . . 4_565 ? C2 C1 C2 C3 -0.6(5) 4_565 . . . ? Pd C1 C2 C3 -177.1(2) . . . . ? C2 C1 C2 O1 -179.93(17) 4_565 . . . ? Pd C1 C2 O1 3.6(4) . . . . ? P1 O1 C2 C1 -6.7(3) . . . . ? P1 O1 C2 C3 173.99(19) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? O1 C2 C3 C4 179.5(3) . . . . ? C2 C3 C4 C3 0.2(6) . . . 4_565 ? O1 P1 C7 C9 -49.8(2) . . . . ? C10 P1 C7 C9 56.8(2) . . . . ? Pd P1 C7 C9 -164.20(16) . . . . ? O1 P1 C7 C8 75.12(19) . . . . ? C10 P1 C7 C8 -178.20(18) . . . . ? Pd P1 C7 C8 -39.2(2) . . . . ? O1 P1 C10 C12 161.64(19) . . . . ? C7 P1 C10 C12 55.2(2) . . . . ? Pd P1 C10 C12 -81.4(2) . . . . ? O1 P1 C10 C11 -75.5(2) . . . . ? C7 P1 C10 C11 178.1(2) . . . . ? Pd P1 C10 C11 41.5(2) . . . . ? C1 Pd C27 C28 0.0(3) . . . . ? P1 Pd C27 C28 -87.75(2) 4_565 . . . ? P1 Pd C27 C28 87.75(2) . . . . ? Pd C27 C28 C29 180.000(2) . . . . ? C27 C28 C29 C34 0.000(2) . . . . ? C27 C28 C29 C30 180.000(2) . . . . ? C34 C29 C30 C31 0.000(2) . . . . ? C28 C29 C30 C31 180.000(2) . . . . ? C29 C30 C31 C32 0.000(3) . . . . ? C30 C31 C32 C33 0.000(3) . . . . ? C31 C32 C33 C34 0.000(3) . . . . ? C32 C33 C34 C29 0.000(3) . . . . ? C30 C29 C34 C33 0.000(2) . . . . ? C28 C29 C34 C33 180.000(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 67.28 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.642 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.068 _iucr_refine_instructions_details ; TITL 4B in P2(1)/m CELL 1.54178 7.8023 14.4839 12.0669 90.000 101.659 90.000 ZERR 2.00 0.0002 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, -Z SFAC C H O P PD UNIT 52 76 4 4 2 TEMP -123.0 L.S. 5 size 0.21 0.19 0.18 acta bond $h conf mpla 4 c1 c2 c3 c4 mpla 4 c29 c30 c31 c32 FMAP 2 PLAN 5 WGHT 0.048000 0.307500 FVAR 0.15480 PD 5 0.247548 0.250000 0.758012 10.50000 0.02807 0.02963 = 0.01810 0.00000 0.00461 0.00000 P1 4 0.281224 0.096813 0.736791 11.00000 0.03198 0.03139 = 0.02176 -0.00497 0.00185 0.00500 O1 3 0.370661 0.084809 0.623737 11.00000 0.05152 0.04995 = 0.02364 -0.00563 0.00799 0.01684 C1 1 0.370008 0.250000 0.624585 10.50000 0.02677 0.05587 = 0.01603 0.00000 0.00372 0.00000 C2 1 0.417780 0.168003 0.579401 11.00000 0.03165 0.06310 = 0.01884 -0.00224 0.00014 0.00810 C3 1 0.509021 0.166097 0.491076 11.00000 0.03459 0.09085 = 0.02312 -0.00598 0.00414 0.01607 AFIX 43 H3 2 0.540423 0.109412 0.460925 11.00000 -1.20000 AFIX 0 C4 1 0.551808 0.250000 0.449281 10.50000 0.02715 0.11439 = 0.02315 0.00000 0.00647 0.00000 AFIX 43 H4 2 0.613520 0.250000 0.389000 10.50000 -1.20000 AFIX 0 C7 1 0.443354 0.040064 0.846248 11.00000 0.03317 0.03760 = 0.02495 -0.00019 0.00422 0.00436 AFIX 13 H7 2 0.389771 0.032302 0.914276 11.00000 -1.20000 AFIX 0 C8 1 0.602452 0.103487 0.879927 11.00000 0.03369 0.04578 = 0.03903 0.00027 -0.00375 0.00296 AFIX 137 H8A 2 0.690296 0.073176 0.938071 11.00000 -1.50000 H8B 2 0.566099 0.161580 0.909868 11.00000 -1.50000 H8C 2 0.652756 0.116283 0.813390 11.00000 -1.50000 AFIX 0 C9 1 0.496612 -0.055348 0.812363 11.00000 0.04129 0.03924 = 0.04596 -0.00418 0.00059 0.01009 AFIX 137 H9A 2 0.580110 -0.082722 0.875431 11.00000 -1.50000 H9B 2 0.551290 -0.049960 0.746330 11.00000 -1.50000 H9C 2 0.392717 -0.094774 0.793519 11.00000 -1.50000 AFIX 0 C10 1 0.091842 0.020413 0.702884 11.00000 0.03377 0.03541 = 0.05209 -0.01560 -0.00179 0.00104 AFIX 13 H10 2 0.128190 -0.037969 0.669855 11.00000 -1.20000 AFIX 0 C11 1 -0.049836 0.067874 0.613665 11.00000 0.04830 0.05915 = 0.06617 -0.01846 -0.02116 0.00998 AFIX 137 H11A 2 -0.146620 0.024776 0.588234 11.00000 -1.50000 H11B 2 0.000476 0.086509 0.548963 11.00000 -1.50000 H11C 2 -0.093505 0.122532 0.647032 11.00000 -1.50000 AFIX 0 C12 1 0.024821 -0.003288 0.809871 11.00000 0.03345 0.04346 = 0.07181 -0.00844 0.01136 -0.00518 AFIX 137 H12A 2 -0.086760 -0.036262 0.789246 11.00000 -1.50000 H12B 2 0.007724 0.053695 0.850069 11.00000 -1.50000 H12C 2 0.110479 -0.042509 0.858974 11.00000 -1.50000 AFIX 0 C27 1 0.123684 0.250000 0.893977 10.50000 0.02805 0.02398 = 0.02896 0.00000 0.00810 0.00000 AFIX 43 H27 2 -0.000574 0.250000 0.875166 10.50000 -1.20000 AFIX 0 C28 1 0.193123 0.250000 1.004068 10.50000 0.02585 0.02909 = 0.02472 0.00000 0.00755 0.00000 AFIX 43 H28 2 0.317338 0.250000 1.023588 10.50000 -1.20000 AFIX 0 C29 1 0.101240 0.250000 1.100064 10.50000 0.02775 0.02495 = 0.02599 0.00000 0.00592 0.00000 C30 1 0.197104 0.250000 1.211576 10.50000 0.02657 0.03315 = 0.02555 0.00000 0.00620 0.00000 AFIX 43 H30 2 0.321327 0.250000 1.224638 10.50000 -1.20000 AFIX 0 C31 1 0.115037 0.250000 1.303263 10.50000 0.04058 0.04069 = 0.02457 0.00000 0.00904 0.00000 AFIX 43 H31 2 0.182856 0.250000 1.378107 10.50000 -1.20000 AFIX 0 C32 1 -0.065354 0.250000 1.285727 10.50000 0.04069 0.04960 = 0.03534 0.00000 0.02218 0.00000 AFIX 43 H32 2 -0.122058 0.250000 1.348379 10.50000 -1.20000 AFIX 0 C33 1 -0.163051 0.250000 1.176609 10.50000 0.02842 0.04278 = 0.04539 0.00000 0.01259 0.00000 AFIX 43 H33 2 -0.287211 0.250000 1.164439 10.50000 -1.20000 AFIX 0 C34 1 -0.081418 0.250000 1.084943 10.50000 0.02778 0.03283 = 0.02877 0.00000 0.00449 0.00000 AFIX 43 H34 2 -0.150510 0.250000 1.010464 10.50000 -1.20000 HKLF 4 REM 4B in P2(1)/m REM R1 = 0.0273 for 2219 Fo > 4sig(Fo) and 0.0318 for all 2453 data REM 161 parameters refined using 0 restraints END WGHT 0.0480 0.3077 REM Highest difference peak 0.642, deepest hole -0.339, 1-sigma level 0.068 Q1 1 0.1822 0.2500 0.6869 10.50000 0.05 0.64 Q2 1 0.3225 0.2500 0.8232 10.50000 0.05 0.58 Q3 1 0.2063 0.1000 0.7772 11.00000 0.05 0.42 Q4 1 0.1582 0.2183 0.7740 11.00000 0.05 0.42 Q5 1 0.3653 0.0712 0.7864 11.00000 0.05 0.41 ; _database_code_depnum_ccdc_archive 'CCDC 965924' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5B _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H34 O2 P2 Pd' _chemical_formula_sum 'C19 H34 O2 P2 Pd' _chemical_formula_weight 462.80 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' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0315(2) _cell_length_b 10.3766(2) _cell_length_c 14.2789(3) _cell_angle_alpha 100.6670(10) _cell_angle_beta 103.3720(10) _cell_angle_gamma 101.5950(10) _cell_volume 1100.12(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6638 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 67.32 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 8.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1845 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(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 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_reflns_number 9168 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 67.46 _reflns_number_total 3781 _reflns_number_gt 3489 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.634' _computing_cell_refinement 'Bruker SAINT v7.66A' _computing_data_reduction 'Bruker SAINT v7.66A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0564P)^2^+0.1015P] 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_number_reflns 3781 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Pd Pd 0.06642(3) 0.26077(2) 0.282660(14) 0.02668(10) Uani 1 1 d . . . P1 P -0.13100(10) 0.05548(7) 0.23451(5) 0.02682(17) Uani 1 1 d . . . P2 P 0.20889(10) 0.46773(8) 0.27441(6) 0.02825(17) Uani 1 1 d . . . O1 O -0.2647(3) 0.0513(2) 0.12590(15) 0.0337(5) Uani 1 1 d . . . O2 O 0.0774(3) 0.5073(2) 0.18160(16) 0.0324(5) Uani 1 1 d . . . C1 C -0.0932(4) 0.2794(3) 0.1561(2) 0.0256(6) Uani 1 1 d . . . C2 C -0.2346(4) 0.1743(3) 0.0966(2) 0.0297(6) Uani 1 1 d . . . C3 C -0.3482(4) 0.1824(3) 0.0093(2) 0.0313(6) Uani 1 1 d . . . H3 H -0.4443 0.1080 -0.0295 0.038 Uiso 1 1 calc R . . C4 C -0.3142(4) 0.3053(3) -0.0186(2) 0.0329(7) Uani 1 1 d . . . H4 H -0.3888 0.3144 -0.0780 0.040 Uiso 1 1 calc R . . C5 C -0.1744(4) 0.4140(3) 0.0380(2) 0.0298(6) Uani 1 1 d . . . H5 H -0.1532 0.4971 0.0184 0.036 Uiso 1 1 calc R . . C6 C -0.0670(4) 0.3987(3) 0.1235(2) 0.0297(6) Uani 1 1 d . . . C7 C -0.0479(5) -0.0947(3) 0.2057(3) 0.0405(8) Uani 1 1 d . . . H7 H 0.0302 -0.1013 0.2693 0.049 Uiso 1 1 calc R . . C8 C 0.0689(7) -0.0722(5) 0.1365(4) 0.0695(13) Uani 1 1 d . . . H8A H 0.1204 -0.1495 0.1242 0.104 Uiso 1 1 calc R . . H8B H 0.1639 0.0110 0.1675 0.104 Uiso 1 1 calc R . . H8C H -0.0028 -0.0635 0.0735 0.104 Uiso 1 1 calc R . . C9 C -0.1906(6) -0.2281(4) 0.1648(3) 0.0567(11) Uani 1 1 d . . . H9A H -0.1353 -0.3028 0.1507 0.085 Uiso 1 1 calc R . . H9B H -0.2731 -0.2243 0.1036 0.085 Uiso 1 1 calc R . . H9C H -0.2551 -0.2430 0.2139 0.085 Uiso 1 1 calc R . . C10 C -0.2923(4) 0.0113(3) 0.3025(2) 0.0338(7) Uani 1 1 d . . . H10 H -0.3838 -0.0728 0.2614 0.041 Uiso 1 1 calc R . . C11 C -0.2003(5) -0.0167(4) 0.4007(2) 0.0417(8) Uani 1 1 d . . . H11A H -0.2855 -0.0328 0.4393 0.062 Uiso 1 1 calc R . . H11B H -0.1020 0.0618 0.4387 0.062 Uiso 1 1 calc R . . H11C H -0.1548 -0.0969 0.3870 0.062 Uiso 1 1 calc R . . C12 C -0.3827(5) 0.1260(4) 0.3195(3) 0.0513(9) Uani 1 1 d . . . H12A H -0.4682 0.1032 0.3567 0.077 Uiso 1 1 calc R . . H12B H -0.4444 0.1384 0.2554 0.077 Uiso 1 1 calc R . . H12C H -0.2936 0.2100 0.3574 0.077 Uiso 1 1 calc R . . C13 C 0.4120(4) 0.4821(4) 0.2354(3) 0.0384(7) Uani 1 1 d . . . H13 H 0.4387 0.5696 0.2152 0.046 Uiso 1 1 calc R . . C14 C 0.5684(4) 0.4828(4) 0.3209(3) 0.0503(9) Uani 1 1 d . . . H14A H 0.6707 0.4756 0.2958 0.075 Uiso 1 1 calc R . . H14B H 0.5358 0.4057 0.3495 0.075 Uiso 1 1 calc R . . H14C H 0.5987 0.5675 0.3721 0.075 Uiso 1 1 calc R . . C15 C 0.3823(5) 0.3647(4) 0.1450(3) 0.0512(9) Uani 1 1 d . . . H15A H 0.4887 0.3745 0.1217 0.077 Uiso 1 1 calc R . . H15B H 0.2816 0.3667 0.0917 0.077 Uiso 1 1 calc R . . H15C H 0.3577 0.2782 0.1639 0.077 Uiso 1 1 calc R . . C16 C 0.2487(4) 0.6182(3) 0.3751(3) 0.0375(7) Uani 1 1 d . . . H16 H 0.3341 0.6075 0.4346 0.045 Uiso 1 1 calc R . . C17 C 0.3286(5) 0.7507(4) 0.3529(3) 0.0506(9) Uani 1 1 d . . . H17A H 0.3360 0.8267 0.4073 0.076 Uiso 1 1 calc R . . H17B H 0.2538 0.7597 0.2909 0.076 Uiso 1 1 calc R . . H17C H 0.4474 0.7513 0.3462 0.076 Uiso 1 1 calc R . . C18 C 0.0737(5) 0.6200(4) 0.4012(3) 0.0521(10) Uani 1 1 d . . . H18A H 0.0942 0.6957 0.4585 0.078 Uiso 1 1 calc R . . H18B H 0.0282 0.5345 0.4175 0.078 Uiso 1 1 calc R . . H18C H -0.0129 0.6309 0.3444 0.078 Uiso 1 1 calc R . . C23 C 0.2320(4) 0.2414(4) 0.4161(2) 0.0381(8) Uani 1 1 d . . . H23A H 0.3498 0.3025 0.4305 0.057 Uiso 1 1 calc R . . H23B H 0.2418 0.1476 0.4085 0.057 Uiso 1 1 calc R . . H23C H 0.1807 0.2651 0.4709 0.057 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 Pd 0.02640(14) 0.03035(14) 0.02365(14) 0.01296(9) 0.00444(9) 0.00512(9) P1 0.0296(4) 0.0264(4) 0.0249(4) 0.0112(3) 0.0050(3) 0.0065(3) P2 0.0260(4) 0.0302(4) 0.0294(4) 0.0135(3) 0.0063(3) 0.0051(3) O1 0.0393(12) 0.0294(11) 0.0271(11) 0.0117(9) -0.0003(9) 0.0040(9) O2 0.0307(11) 0.0313(11) 0.0348(12) 0.0156(9) 0.0050(9) 0.0052(9) C1 0.0266(14) 0.0305(15) 0.0218(14) 0.0102(11) 0.0065(11) 0.0090(12) C2 0.0334(16) 0.0297(15) 0.0311(16) 0.0154(13) 0.0113(13) 0.0092(13) C3 0.0340(16) 0.0355(16) 0.0215(14) 0.0081(12) 0.0032(12) 0.0066(13) C4 0.0365(16) 0.0419(17) 0.0256(15) 0.0159(13) 0.0081(13) 0.0149(14) C5 0.0341(16) 0.0328(15) 0.0291(15) 0.0162(13) 0.0110(13) 0.0127(13) C6 0.0325(15) 0.0329(15) 0.0271(15) 0.0102(12) 0.0118(12) 0.0091(13) C7 0.0467(19) 0.0424(18) 0.0367(18) 0.0103(15) 0.0099(15) 0.0219(16) C8 0.081(3) 0.076(3) 0.075(3) 0.021(3) 0.044(3) 0.043(3) C9 0.074(3) 0.0328(18) 0.055(2) 0.0019(16) 0.004(2) 0.0212(19) C10 0.0302(16) 0.0371(16) 0.0345(17) 0.0164(14) 0.0077(13) 0.0040(13) C11 0.0456(19) 0.0480(19) 0.0346(18) 0.0221(15) 0.0108(15) 0.0084(16) C12 0.043(2) 0.067(2) 0.055(2) 0.022(2) 0.0203(18) 0.0266(19) C13 0.0330(16) 0.0447(18) 0.048(2) 0.0277(16) 0.0149(14) 0.0131(14) C14 0.0274(17) 0.064(2) 0.061(2) 0.022(2) 0.0086(16) 0.0128(16) C15 0.049(2) 0.074(3) 0.046(2) 0.026(2) 0.0234(18) 0.028(2) C16 0.0342(17) 0.0360(16) 0.0361(18) 0.0056(14) 0.0029(14) 0.0061(13) C17 0.044(2) 0.0350(18) 0.068(3) 0.0109(18) 0.0116(19) 0.0073(16) C18 0.048(2) 0.053(2) 0.051(2) 0.0001(18) 0.0202(18) 0.0077(17) C23 0.0314(16) 0.053(2) 0.0288(16) 0.0207(15) 0.0008(13) 0.0060(15) _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 Pd C1 2.026(3) . ? Pd C23 2.125(3) . ? Pd P2 2.2591(7) . ? Pd P1 2.2628(7) . ? P1 O1 1.657(2) . ? P1 C10 1.827(3) . ? P1 C7 1.830(3) . ? P2 O2 1.664(2) . ? P2 C13 1.829(3) . ? P2 C16 1.834(3) . ? O1 C2 1.408(4) . ? O2 C6 1.410(4) . ? C1 C2 1.384(4) . ? C1 C6 1.395(4) . ? C2 C3 1.391(4) . ? C3 C4 1.400(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C7 C9 1.524(5) . ? C7 C8 1.529(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.525(5) . ? C10 C11 1.535(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.534(5) . ? C13 C15 1.539(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.518(5) . ? C16 C18 1.538(5) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 C1 Pd C23 179.45(12) . . ? C1 Pd P2 79.47(9) . . ? C23 Pd P2 100.71(10) . . ? C1 Pd P1 79.68(9) . . ? C23 Pd P1 100.17(10) . . ? P2 Pd P1 158.87(3) . . ? O1 P1 C10 100.51(13) . . ? O1 P1 C7 102.47(14) . . ? C10 P1 C7 105.99(16) . . ? O1 P1 Pd 105.95(8) . . ? C10 P1 Pd 121.12(11) . . ? C7 P1 Pd 117.75(12) . . ? O2 P2 C13 101.05(13) . . ? O2 P2 C16 100.85(14) . . ? C13 P2 C16 106.41(16) . . ? O2 P2 Pd 106.21(8) . . ? C13 P2 Pd 117.85(11) . . ? C16 P2 Pd 121.15(12) . . ? C2 O1 P1 114.24(18) . . ? C6 O2 P2 113.77(18) . . ? C2 C1 C6 116.0(3) . . ? C2 C1 Pd 121.9(2) . . ? C6 C1 Pd 122.1(2) . . ? C1 C2 C3 124.0(3) . . ? C1 C2 O1 117.9(3) . . ? C3 C2 O1 118.0(3) . . ? C2 C3 C4 116.8(3) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 118.3(3) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C1 123.1(3) . . ? C5 C6 O2 119.3(3) . . ? C1 C6 O2 117.5(3) . . ? C9 C7 C8 111.9(3) . . ? C9 C7 P1 114.7(3) . . ? C8 C7 P1 108.9(3) . . ? C9 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? P1 C7 H7 107.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.6(3) . . ? C12 C10 P1 109.2(2) . . ? C11 C10 P1 109.9(2) . . ? C12 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? P1 C10 H10 108.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.3(3) . . ? C14 C13 P2 110.9(2) . . ? C15 C13 P2 109.1(2) . . ? C14 C13 H13 108.5 . . ? C15 C13 H13 108.5 . . ? P2 C13 H13 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 111.7(3) . . ? C17 C16 P2 114.2(3) . . ? C18 C16 P2 108.2(2) . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? P2 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Pd C23 H23A 109.5 . . ? Pd C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Pd C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 C1 Pd P1 O1 3.85(11) . . . . ? C23 Pd P1 O1 -176.68(13) . . . . ? P2 Pd P1 O1 -5.64(13) . . . . ? C1 Pd P1 C10 -109.37(15) . . . . ? C23 Pd P1 C10 70.10(16) . . . . ? P2 Pd P1 C10 -118.86(14) . . . . ? C1 Pd P1 C7 117.69(15) . . . . ? C23 Pd P1 C7 -62.84(17) . . . . ? P2 Pd P1 C7 108.20(15) . . . . ? C1 Pd P2 O2 7.69(11) . . . . ? C23 Pd P2 O2 -171.78(13) . . . . ? P1 Pd P2 O2 17.19(13) . . . . ? C1 Pd P2 C13 -104.60(15) . . . . ? C23 Pd P2 C13 75.93(17) . . . . ? P1 Pd P2 C13 -95.10(15) . . . . ? C1 Pd P2 C16 121.56(15) . . . . ? C23 Pd P2 C16 -57.91(16) . . . . ? P1 Pd P2 C16 131.06(14) . . . . ? C10 P1 O1 C2 121.4(2) . . . . ? C7 P1 O1 C2 -129.5(2) . . . . ? Pd P1 O1 C2 -5.5(2) . . . . ? C13 P2 O2 C6 113.5(2) . . . . ? C16 P2 O2 C6 -137.2(2) . . . . ? Pd P2 O2 C6 -10.0(2) . . . . ? C23 Pd C1 C2 -77(12) . . . . ? P2 Pd C1 C2 174.3(3) . . . . ? P1 Pd C1 C2 -2.2(2) . . . . ? C23 Pd C1 C6 104(12) . . . . ? P2 Pd C1 C6 -5.5(2) . . . . ? P1 Pd C1 C6 178.0(2) . . . . ? C6 C1 C2 C3 -0.5(5) . . . . ? Pd C1 C2 C3 179.8(2) . . . . ? C6 C1 C2 O1 179.1(2) . . . . ? Pd C1 C2 O1 -0.6(4) . . . . ? P1 O1 C2 C1 4.4(4) . . . . ? P1 O1 C2 C3 -176.0(2) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? O1 C2 C3 C4 -179.3(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? C4 C5 C6 C1 -0.6(5) . . . . ? C4 C5 C6 O2 179.1(3) . . . . ? C2 C1 C6 C5 0.6(4) . . . . ? Pd C1 C6 C5 -179.6(2) . . . . ? C2 C1 C6 O2 -179.1(2) . . . . ? Pd C1 C6 O2 0.6(4) . . . . ? P2 O2 C6 C5 -172.9(2) . . . . ? P2 O2 C6 C1 6.9(3) . . . . ? O1 P1 C7 C9 -58.9(3) . . . . ? C10 P1 C7 C9 46.0(3) . . . . ? Pd P1 C7 C9 -174.7(2) . . . . ? O1 P1 C7 C8 67.4(3) . . . . ? C10 P1 C7 C8 172.3(3) . . . . ? Pd P1 C7 C8 -48.4(3) . . . . ? O1 P1 C10 C12 -67.5(3) . . . . ? C7 P1 C10 C12 -173.9(2) . . . . ? Pd P1 C10 C12 48.5(3) . . . . ? O1 P1 C10 C11 169.7(2) . . . . ? C7 P1 C10 C11 63.3(3) . . . . ? Pd P1 C10 C11 -74.3(2) . . . . ? O2 P2 C13 C14 166.7(2) . . . . ? C16 P2 C13 C14 61.7(3) . . . . ? Pd P2 C13 C14 -78.2(3) . . . . ? O2 P2 C13 C15 -70.4(2) . . . . ? C16 P2 C13 C15 -175.3(2) . . . . ? Pd P2 C13 C15 44.7(3) . . . . ? O2 P2 C16 C17 -57.3(3) . . . . ? C13 P2 C16 C17 47.8(3) . . . . ? Pd P2 C16 C17 -173.9(2) . . . . ? O2 P2 C16 C18 67.7(3) . . . . ? C13 P2 C16 C18 172.8(3) . . . . ? Pd P2 C16 C18 -48.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 67.46 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.183 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.101 _iucr_refine_instructions_details ; TITL 5B in P-1 CELL 1.54178 8.0315 10.3766 14.2789 100.667 103.372 101.595 ZERR 2.00 0.0002 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H O P PD UNIT 38 68 4 4 2 TEMP -123.0 L.S. 5 acta size 0.31 0.26 0.01 rem colorless plate bond $h conf mpla 6 c1 c2 c3 c4 c5 c6 FMAP 2 PLAN 5 WGHT 0.056400 0.101500 FVAR 0.15325 PD 5 0.066417 0.260769 0.282660 11.00000 0.02640 0.03035 = 0.02365 0.01296 0.00444 0.00512 P1 4 -0.130999 0.055480 0.234512 11.00000 0.02958 0.02642 = 0.02486 0.01118 0.00499 0.00650 P2 4 0.208889 0.467734 0.274409 11.00000 0.02604 0.03024 = 0.02937 0.01351 0.00633 0.00505 O1 3 -0.264693 0.051326 0.125900 11.00000 0.03932 0.02939 = 0.02710 0.01169 -0.00030 0.00396 O2 3 0.077448 0.507317 0.181595 11.00000 0.03071 0.03126 = 0.03484 0.01558 0.00501 0.00515 C1 1 -0.093236 0.279437 0.156112 11.00000 0.02658 0.03051 = 0.02185 0.01024 0.00651 0.00897 C2 1 -0.234644 0.174297 0.096587 11.00000 0.03338 0.02969 = 0.03113 0.01544 0.01132 0.00922 C3 1 -0.348206 0.182392 0.009309 11.00000 0.03398 0.03548 = 0.02147 0.00808 0.00321 0.00660 AFIX 43 H3 2 -0.444300 0.108025 -0.029476 11.00000 -1.20000 AFIX 0 C4 1 -0.314161 0.305310 -0.018648 11.00000 0.03647 0.04186 = 0.02556 0.01585 0.00809 0.01495 AFIX 43 H4 2 -0.388751 0.314406 -0.077951 11.00000 -1.20000 AFIX 0 C5 1 -0.174438 0.414030 0.037980 11.00000 0.03408 0.03284 = 0.02912 0.01622 0.01100 0.01267 AFIX 43 H5 2 -0.153198 0.497083 0.018374 11.00000 -1.20000 AFIX 0 C6 1 -0.066951 0.398682 0.123525 11.00000 0.03254 0.03285 = 0.02713 0.01019 0.01175 0.00908 C7 1 -0.047948 -0.094702 0.205703 11.00000 0.04667 0.04235 = 0.03666 0.01029 0.00994 0.02193 AFIX 13 H7 2 0.030229 -0.101301 0.269294 11.00000 -1.20000 AFIX 0 C8 1 0.068883 -0.072156 0.136481 11.00000 0.08073 0.07625 = 0.07457 0.02096 0.04423 0.04256 AFIX 137 H8A 2 0.120369 -0.149475 0.124163 11.00000 -1.50000 H8B 2 0.163949 0.010966 0.167464 11.00000 -1.50000 H8C 2 -0.002798 -0.063510 0.073454 11.00000 -1.50000 AFIX 0 C9 1 -0.190602 -0.228112 0.164834 11.00000 0.07447 0.03279 = 0.05534 0.00190 0.00413 0.02123 AFIX 137 H9A 2 -0.135315 -0.302795 0.150685 11.00000 -1.50000 H9B 2 -0.273065 -0.224271 0.103599 11.00000 -1.50000 H9C 2 -0.255137 -0.243038 0.213943 11.00000 -1.50000 AFIX 0 C10 1 -0.292280 0.011317 0.302500 11.00000 0.03016 0.03712 = 0.03450 0.01639 0.00768 0.00405 AFIX 13 H10 2 -0.383824 -0.072845 0.261431 11.00000 -1.20000 AFIX 0 C11 1 -0.200335 -0.016683 0.400747 11.00000 0.04559 0.04800 = 0.03455 0.02209 0.01075 0.00844 AFIX 137 H11A 2 -0.285463 -0.032784 0.439289 11.00000 -1.50000 H11B 2 -0.102013 0.061772 0.438714 11.00000 -1.50000 H11C 2 -0.154820 -0.096914 0.386970 11.00000 -1.50000 AFIX 0 C12 1 -0.382719 0.125979 0.319520 11.00000 0.04319 0.06740 = 0.05517 0.02196 0.02034 0.02663 AFIX 137 H12A 2 -0.468248 0.103192 0.356744 11.00000 -1.50000 H12B 2 -0.444395 0.138420 0.255382 11.00000 -1.50000 H12C 2 -0.293649 0.210030 0.357374 11.00000 -1.50000 AFIX 0 C13 1 0.411963 0.482106 0.235431 11.00000 0.03297 0.04470 = 0.04777 0.02771 0.01488 0.01305 AFIX 13 H13 2 0.438718 0.569567 0.215244 11.00000 -1.20000 AFIX 0 C14 1 0.568405 0.482793 0.320931 11.00000 0.02738 0.06367 = 0.06127 0.02182 0.00859 0.01284 AFIX 137 H14A 2 0.670693 0.475576 0.295802 11.00000 -1.50000 H14B 2 0.535798 0.405721 0.349490 11.00000 -1.50000 H14C 2 0.598672 0.567521 0.372126 11.00000 -1.50000 AFIX 0 C15 1 0.382304 0.364720 0.144984 11.00000 0.04937 0.07399 = 0.04612 0.02644 0.02343 0.02822 AFIX 137 H15A 2 0.488736 0.374479 0.121714 11.00000 -1.50000 H15B 2 0.281600 0.366683 0.091746 11.00000 -1.50000 H15C 2 0.357683 0.278226 0.163879 11.00000 -1.50000 AFIX 0 C16 1 0.248703 0.618246 0.375143 11.00000 0.03425 0.03604 = 0.03607 0.00561 0.00293 0.00615 AFIX 13 H16 2 0.334107 0.607495 0.434592 11.00000 -1.20000 AFIX 0 C17 1 0.328556 0.750721 0.352921 11.00000 0.04436 0.03500 = 0.06842 0.01091 0.01162 0.00731 AFIX 137 H17A 2 0.336008 0.826691 0.407274 11.00000 -1.50000 H17B 2 0.253804 0.759674 0.290895 11.00000 -1.50000 H17C 2 0.447424 0.751348 0.346243 11.00000 -1.50000 AFIX 0 C18 1 0.073659 0.619982 0.401244 11.00000 0.04756 0.05300 = 0.05148 0.00014 0.02016 0.00772 AFIX 137 H18A 2 0.094229 0.695730 0.458471 11.00000 -1.50000 H18B 2 0.028165 0.534461 0.417527 11.00000 -1.50000 H18C 2 -0.012947 0.630861 0.344364 11.00000 -1.50000 AFIX 0 C23 1 0.231991 0.241406 0.416093 11.00000 0.03136 0.05254 = 0.02878 0.02065 0.00081 0.00600 AFIX 137 H23A 2 0.349788 0.302546 0.430467 11.00000 -1.50000 H23B 2 0.241825 0.147641 0.408473 11.00000 -1.50000 H23C 2 0.180715 0.265101 0.470874 11.00000 -1.50000 HKLF 4 REM 5B in P-1 REM R1 = 0.0315 for 3489 Fo > 4sig(Fo) and 0.0347 for all 3781 data REM 226 parameters refined using 0 restraints END WGHT 0.0564 0.1015 REM Highest difference peak 1.183, deepest hole -0.456, 1-sigma level 0.101 Q1 1 0.1140 0.3464 0.3299 11.00000 0.05 1.18 Q2 1 0.0142 0.1662 0.2404 11.00000 0.05 1.15 Q3 1 -0.0940 -0.0266 0.2184 11.00000 0.05 0.58 Q4 1 0.2314 0.5551 0.3246 11.00000 0.05 0.56 Q5 1 -0.0637 0.0643 0.2951 11.00000 0.05 0.55 ; #eof data_5B ================================================= #eof all data ================================================= _database_code_depnum_ccdc_archive 'CCDC 965925'