# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Pascal Le Floch' _publ_contact_author_email PASCAL.LEFLOCH@POLYTECHNIQUE.EDU _publ_section_title ; 1-Phosphabarrelene Complexes of Palladium and their use in Suzuki- Miyaura Coupling Reactions. ; loop_ _publ_author_name 'Pascal Le Floch' 'Matthias Blug' 'Clement Guibert' 'Xavier-Frederic Le Goff' 'Nicolas Mezailles' # Attachment 'Blug_chem_comm.cif' #=============================================================================== data_mb428 _database_code_depnum_ccdc_archive 'CCDC 699913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H29 P Si2' _chemical_formula_sum 'C19 H29 P Si2' _chemical_formula_weight 344.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 15.043(1) _cell_length_b 16.246(1) _cell_length_c 8.401(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2053.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 6111 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9077 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12956 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3085 _reflns_number_gt 2154 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.5825P] 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 3085 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 P1 P 0.32153(4) 0.2500 0.82690(7) 0.02100(15) Uani 1 2 d S . . Si1 Si 0.33992(3) 0.08077(3) 1.00080(5) 0.02573(14) Uani 1 1 d . . . C1 C 0.26325(10) 0.16378(9) 0.92920(18) 0.0212(3) Uani 1 1 d . . . C2 C 0.17466(11) 0.17260(9) 0.93654(18) 0.0224(3) Uani 1 1 d . . . C3 C 0.13338(14) 0.2500 0.8609(3) 0.0219(5) Uani 1 2 d S . . H3 H 0.0674 0.2500 0.8749 0.026 Uiso 1 2 calc SR . . C6 C 0.24870(14) 0.2500 0.6516(3) 0.0210(4) Uani 1 2 d S . . C7 C 0.27750(16) 0.2500 0.4951(3) 0.0259(5) Uani 1 2 d S . . H7 H 0.3394 0.2500 0.4723 0.031 Uiso 1 2 calc SR . . C8 C 0.21636(18) 0.2500 0.3714(3) 0.0331(6) Uani 1 2 d S . . H8 H 0.2362 0.2500 0.2640 0.040 Uiso 1 2 calc SR . . C9 C 0.12565(18) 0.2500 0.4053(3) 0.0313(5) Uani 1 2 d S . . H9 H 0.0838 0.2500 0.3206 0.038 Uiso 1 2 calc SR . . C10 C 0.09574(16) 0.2500 0.5628(3) 0.0261(5) Uani 1 2 d S . . H10 H 0.0339 0.2500 0.5857 0.031 Uiso 1 2 calc SR . . C11 C 0.15751(14) 0.2500 0.6852(3) 0.0210(4) Uani 1 2 d S . . C12 C 0.10888(12) 0.11391(11) 1.0099(2) 0.0341(4) Uani 1 1 d . . . H12A H 0.1408 0.0680 1.0595 0.051 Uiso 1 1 calc R . . H12B H 0.0691 0.0927 0.9271 0.051 Uiso 1 1 calc R . . H12C H 0.0739 0.1428 1.0909 0.051 Uiso 1 1 calc R . . C14 C 0.42504(13) 0.06401(11) 0.8422(2) 0.0366(4) Uani 1 1 d . . . H14A H 0.3959 0.0628 0.7379 0.055 Uiso 1 1 calc R . . H14B H 0.4554 0.0115 0.8607 0.055 Uiso 1 1 calc R . . H14C H 0.4685 0.1089 0.8448 0.055 Uiso 1 1 calc R . . C15 C 0.28597(15) -0.02002(11) 1.0456(3) 0.0472(5) Uani 1 1 d . . . H15A H 0.2493 -0.0147 1.1415 0.071 Uiso 1 1 calc R . . H15B H 0.3318 -0.0619 1.0631 0.071 Uiso 1 1 calc R . . H15C H 0.2484 -0.0364 0.9557 0.071 Uiso 1 1 calc R . . C16 C 0.39620(13) 0.11923(12) 1.1839(2) 0.0396(5) Uani 1 1 d . . . H16A H 0.4243 0.1724 1.1615 0.059 Uiso 1 1 calc R . . H16B H 0.4416 0.0796 1.2174 0.059 Uiso 1 1 calc R . . H16C H 0.3523 0.1260 1.2690 0.059 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 P1 0.0197(3) 0.0204(3) 0.0229(3) 0.000 0.0005(2) 0.000 Si1 0.0308(3) 0.0210(2) 0.0255(3) -0.00011(17) -0.0034(2) 0.00441(18) C1 0.0247(8) 0.0200(7) 0.0191(8) 0.0009(6) -0.0007(7) -0.0011(6) C2 0.0261(8) 0.0228(7) 0.0182(7) 0.0006(6) -0.0001(7) -0.0028(6) C3 0.0174(10) 0.0263(11) 0.0220(11) 0.000 0.0000(9) 0.000 C6 0.0231(11) 0.0187(10) 0.0210(11) 0.000 -0.0002(9) 0.000 C7 0.0279(12) 0.0260(11) 0.0238(12) 0.000 0.0021(10) 0.000 C8 0.0437(15) 0.0342(13) 0.0214(12) 0.000 0.0004(11) 0.000 C9 0.0367(14) 0.0347(13) 0.0225(12) 0.000 -0.0071(11) 0.000 C10 0.0257(12) 0.0267(12) 0.0259(12) 0.000 -0.0031(10) 0.000 C11 0.0250(11) 0.0174(10) 0.0206(11) 0.000 -0.0024(9) 0.000 C12 0.0302(9) 0.0354(10) 0.0368(10) 0.0091(7) 0.0021(8) -0.0070(7) C14 0.0382(10) 0.0343(9) 0.0372(11) -0.0050(8) -0.0010(9) 0.0098(8) C15 0.0595(14) 0.0252(9) 0.0570(14) 0.0086(9) -0.0001(11) 0.0025(9) C16 0.0415(11) 0.0418(11) 0.0355(11) -0.0082(8) -0.0113(9) 0.0152(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C6 1.835(2) . ? P1 C1 1.8626(15) 8_565 ? P1 C1 1.8626(15) . ? Si1 C16 1.8637(19) . ? Si1 C15 1.866(2) . ? Si1 C14 1.8679(19) . ? Si1 C1 1.8737(16) . ? C1 C2 1.342(2) . ? C2 C12 1.506(2) . ? C2 C3 1.540(2) . ? C3 C11 1.520(3) . ? C3 C2 1.540(2) 8_565 ? C3 H3 1.0000 . ? C6 C7 1.384(3) . ? C6 C11 1.400(3) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.394(4) . ? C8 H8 0.9500 . ? C9 C10 1.398(3) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 C6 P1 C1 95.12(7) . 8_565 ? C6 P1 C1 95.12(7) . . ? C1 P1 C1 97.54(10) 8_565 . ? C16 Si1 C15 108.99(10) . . ? C16 Si1 C14 109.04(9) . . ? C15 Si1 C14 108.31(10) . . ? C16 Si1 C1 107.65(8) . . ? C15 Si1 C1 115.38(9) . . ? C14 Si1 C1 107.33(8) . . ? C2 C1 P1 114.10(11) . . ? C2 C1 Si1 132.34(12) . . ? P1 C1 Si1 113.56(8) . . ? C1 C2 C12 127.14(15) . . ? C1 C2 C3 117.96(14) . . ? C12 C2 C3 114.89(15) . . ? C11 C3 C2 107.73(12) . 8_565 ? C11 C3 C2 107.73(12) . . ? C2 C3 C2 109.49(17) 8_565 . ? C11 C3 H3 110.6 . . ? C2 C3 H3 110.6 8_565 . ? C2 C3 H3 110.6 . . ? C7 C6 C11 119.9(2) . . ? C7 C6 P1 125.12(18) . . ? C11 C6 P1 115.03(16) . . ? C6 C7 C8 120.3(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 120.6(2) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 119.1(2) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C6 120.5(2) . . ? C10 C11 C3 124.1(2) . . ? C6 C11 C3 115.43(19) . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.429 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.059 #===END # compound 3 data_mb453 _database_code_depnum_ccdc_archive 'CCDC 699914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H34 Cl P Pd Si2' _chemical_formula_sum 'C22 H34 Cl P Pd Si2' _chemical_formula_weight 527.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.056(1) _cell_length_b 15.490(1) _cell_length_c 16.211(1) _cell_angle_alpha 86.602(1) _cell_angle_beta 83.472(1) _cell_angle_gamma 89.719(1) _cell_volume 2504.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 27663 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'block ' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7931 _exptl_absorpt_correction_T_max 0.9606 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22441 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11297 _reflns_number_gt 8707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+3.1896P] 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 11297 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.06147(3) 0.18506(2) 0.604916(19) 0.02855(10) Uani 1 1 d . . . Cl1 Cl -0.17475(12) 0.31953(7) 0.59567(7) 0.0393(3) Uani 1 1 d . A . P1 P 0.07226(11) 0.23309(7) 0.48740(6) 0.0254(2) Uani 1 1 d . A . Si1 Si -0.19024(13) 0.22180(8) 0.38158(8) 0.0326(3) Uani 1 1 d . A . Si2 Si 0.18800(13) 0.38790(8) 0.59192(7) 0.0318(3) Uani 1 1 d . A . C1 C -0.0141(4) 0.2561(3) 0.3941(3) 0.0300(9) Uani 1 1 d . . . C2 C 0.0689(4) 0.2949(3) 0.3313(2) 0.0294(9) Uani 1 1 d . A . C3 C 0.2160(4) 0.3071(3) 0.3442(3) 0.0303(9) Uani 1 1 d . . . H3 H 0.2667 0.3350 0.2929 0.036 Uiso 1 1 calc R A . C4 C 0.2219(4) 0.3636(3) 0.4180(3) 0.0292(9) Uani 1 1 d . A . C5 C 0.1626(4) 0.3357(3) 0.4928(2) 0.0279(8) Uani 1 1 d . . . C6 C 0.2138(4) 0.1736(3) 0.4367(2) 0.0272(8) Uani 1 1 d . . . C7 C 0.2625(5) 0.0936(3) 0.4617(3) 0.0348(10) Uani 1 1 d . A . H7 H 0.2221 0.0634 0.5108 0.042 Uiso 1 1 calc R . . C8 C 0.3708(5) 0.0578(3) 0.4146(3) 0.0406(11) Uani 1 1 d . . . H8 H 0.4047 0.0030 0.4316 0.049 Uiso 1 1 calc R A . C9 C 0.4298(5) 0.1022(3) 0.3424(3) 0.0388(11) Uani 1 1 d . A . H9 H 0.5026 0.0769 0.3097 0.047 Uiso 1 1 calc R . . C10 C 0.3832(5) 0.1828(3) 0.3181(3) 0.0346(10) Uani 1 1 d . . . H10 H 0.4247 0.2132 0.2694 0.042 Uiso 1 1 calc R A . C11 C 0.2754(4) 0.2192(3) 0.3652(2) 0.0294(9) Uani 1 1 d . A . C12 C 0.0327(5) 0.3304(3) 0.2487(3) 0.0368(10) Uani 1 1 d . . . H12A H -0.0628 0.3206 0.2456 0.055 Uiso 1 1 calc R A . H12B H 0.0856 0.3012 0.2041 0.055 Uiso 1 1 calc R . . H12C H 0.0515 0.3926 0.2425 0.055 Uiso 1 1 calc R . . C13 C 0.2947(5) 0.4475(3) 0.3970(3) 0.0383(10) Uani 1 1 d . . . H13A H 0.3911 0.4366 0.3875 0.057 Uiso 1 1 calc R A . H13B H 0.2761 0.4855 0.4432 0.057 Uiso 1 1 calc R . . H13C H 0.2644 0.4754 0.3466 0.057 Uiso 1 1 calc R . . C14 C -0.2671(5) 0.1473(3) 0.4684(3) 0.0446(12) Uani 1 1 d . . . H14A H -0.3467 0.1200 0.4516 0.067 Uiso 1 1 calc R A . H14B H -0.2929 0.1802 0.5175 0.067 Uiso 1 1 calc R . . H14C H -0.2022 0.1027 0.4818 0.067 Uiso 1 1 calc R . . C15 C -0.1783(6) 0.1548(3) 0.2879(3) 0.0472(12) Uani 1 1 d . . . H15A H -0.1244 0.1857 0.2413 0.071 Uiso 1 1 calc R A . H15B H -0.2682 0.1446 0.2728 0.071 Uiso 1 1 calc R . . H15C H -0.1359 0.0993 0.3009 0.071 Uiso 1 1 calc R . . C16 C -0.3030(5) 0.3159(3) 0.3704(4) 0.0497(13) Uani 1 1 d . . . H16A H -0.3930 0.2954 0.3636 0.074 Uiso 1 1 calc R A . H16B H -0.2688 0.3528 0.3214 0.074 Uiso 1 1 calc R . . H16C H -0.3068 0.3492 0.4201 0.074 Uiso 1 1 calc R . . C17 C 0.1536(5) 0.3095(3) 0.6844(3) 0.0370(10) Uani 1 1 d . . . H17A H 0.1950 0.3306 0.7313 0.055 Uiso 1 1 calc R A . H17B H 0.1911 0.2530 0.6707 0.055 Uiso 1 1 calc R . . H17C H 0.0567 0.3041 0.6995 0.055 Uiso 1 1 calc R . . C18 C 0.0832(5) 0.4862(3) 0.6059(3) 0.0443(12) Uani 1 1 d . . . H18A H 0.1018 0.5264 0.5569 0.066 Uiso 1 1 calc R A . H18B H 0.1042 0.5142 0.6555 0.066 Uiso 1 1 calc R . . H18C H -0.0116 0.4699 0.6125 0.066 Uiso 1 1 calc R . . C19 C 0.3706(5) 0.4175(3) 0.5872(3) 0.0467(12) Uani 1 1 d . . . H19A H 0.4245 0.3773 0.5529 0.070 Uiso 1 1 calc R A . H19B H 0.3975 0.4139 0.6435 0.070 Uiso 1 1 calc R . . H19C H 0.3845 0.4766 0.5627 0.070 Uiso 1 1 calc R . . C20A C 0.0101(5) 0.0592(3) 0.6350(3) 0.0419(11) Uani 0.597(18) 1 d P A 1 H20A H -0.0335 0.0105 0.6118 0.050 Uiso 0.597(18) 1 calc PR A 1 H20B H 0.1083 0.0527 0.6338 0.050 Uiso 0.597(18) 1 calc PR A 1 C21A C -0.0604(10) 0.0942(6) 0.7094(5) 0.041(3) Uani 0.597(18) 1 d P A 1 H21A H -0.0138 0.0963 0.7571 0.049 Uiso 0.597(18) 1 calc PR A 1 C22A C -0.1807(7) 0.1222(4) 0.7149(4) 0.0621(18) Uani 0.597(18) 1 d P A 1 H22A H -0.2087 0.1592 0.7615 0.075 Uiso 0.597(18) 1 calc PR A 1 H22B H -0.2505 0.0809 0.7040 0.075 Uiso 0.597(18) 1 calc PR A 1 C20B C 0.0101(5) 0.0592(3) 0.6350(3) 0.0419(11) Uani 0.403(18) 1 d P A 2 H20C H 0.0252 0.0201 0.5887 0.050 Uiso 0.403(18) 1 calc PR A 2 H20D H 0.0808 0.0555 0.6729 0.050 Uiso 0.403(18) 1 calc PR A 2 C21B C -0.1226(16) 0.0659(8) 0.6728(9) 0.046(5) Uani 0.403(18) 1 d P A 2 H21B H -0.1781 0.0184 0.6644 0.055 Uiso 0.403(18) 1 calc PR A 2 C22B C -0.1807(7) 0.1222(4) 0.7149(4) 0.0621(18) Uani 0.403(18) 1 d P A 2 H22C H -0.1491 0.1305 0.7695 0.075 Uiso 0.403(18) 1 calc PR A 2 H22D H -0.2792 0.1251 0.7159 0.075 Uiso 0.403(18) 1 calc PR A 2 Pd2 Pd 0.69746(3) 0.80426(2) -0.05247(2) 0.03167(10) Uani 1 1 d . . . Cl2 Cl 0.60451(13) 0.69199(8) -0.12102(7) 0.0416(3) Uani 1 1 d . B . P2 P 0.58195(11) 0.75069(7) 0.06985(7) 0.0273(2) Uani 1 1 d . B . Si3 Si 0.30205(13) 0.80168(8) -0.00977(8) 0.0355(3) Uani 1 1 d . B . Si4 Si 0.76355(13) 0.57262(8) 0.05626(7) 0.0320(3) Uani 1 1 d . B . C23 C 0.3980(4) 0.7461(3) 0.0719(3) 0.0305(9) Uani 1 1 d . . . C24 C 0.3416(4) 0.7026(3) 0.1407(3) 0.0319(9) Uani 1 1 d . B . C25 C 0.4293(4) 0.6713(3) 0.2077(3) 0.0310(9) Uani 1 1 d . . . H25 H 0.3738 0.6422 0.2565 0.037 Uiso 1 1 calc R B . C26 C 0.5302(4) 0.6078(3) 0.1665(3) 0.0310(9) Uani 1 1 d . B . C27 C 0.6173(4) 0.6377(3) 0.1025(3) 0.0295(9) Uani 1 1 d . . . C28 C 0.5842(4) 0.7959(3) 0.1718(3) 0.0307(9) Uani 1 1 d . . . C29 C 0.6510(5) 0.8693(3) 0.1895(3) 0.0355(10) Uani 1 1 d . B . H29 H 0.7048 0.9017 0.1467 0.043 Uiso 1 1 calc R . . C30 C 0.6385(5) 0.8950(3) 0.2709(3) 0.0429(11) Uani 1 1 d . . . H30 H 0.6847 0.9449 0.2839 0.051 Uiso 1 1 calc R B . C31 C 0.5586(5) 0.8480(3) 0.3331(3) 0.0417(11) Uani 1 1 d . B . H31 H 0.5507 0.8660 0.3884 0.050 Uiso 1 1 calc R . . C32 C 0.4896(5) 0.7745(3) 0.3150(3) 0.0369(10) Uani 1 1 d . . . H32 H 0.4345 0.7427 0.3576 0.044 Uiso 1 1 calc R B . C33 C 0.5030(4) 0.7486(3) 0.2338(3) 0.0316(9) Uani 1 1 d . B . C34 C 0.1959(5) 0.6767(3) 0.1614(3) 0.0399(11) Uani 1 1 d . . . H34A H 0.1477 0.6906 0.1130 0.060 Uiso 1 1 calc R B . H34B H 0.1559 0.7084 0.2086 0.060 Uiso 1 1 calc R . . H34C H 0.1898 0.6145 0.1759 0.060 Uiso 1 1 calc R . . C35 C 0.5151(5) 0.5151(3) 0.1997(3) 0.0380(10) Uani 1 1 d . . . H35A H 0.5679 0.4778 0.1617 0.057 Uiso 1 1 calc R B . H35B H 0.4206 0.4983 0.2043 0.057 Uiso 1 1 calc R . . H35C H 0.5470 0.5089 0.2546 0.057 Uiso 1 1 calc R . . C36 C 0.2448(6) 0.7238(3) -0.0817(3) 0.0468(12) Uani 1 1 d . . . H36A H 0.3224 0.7020 -0.1165 0.070 Uiso 1 1 calc R B . H36B H 0.1837 0.7530 -0.1172 0.070 Uiso 1 1 calc R . . H36C H 0.1983 0.6753 -0.0492 0.070 Uiso 1 1 calc R . . C37 C 0.4017(5) 0.8897(3) -0.0721(3) 0.0459(12) Uani 1 1 d . . . H37A H 0.4407 0.9271 -0.0345 0.069 Uiso 1 1 calc R B . H37B H 0.3431 0.9240 -0.1057 0.069 Uiso 1 1 calc R . . H37C H 0.4735 0.8641 -0.1089 0.069 Uiso 1 1 calc R . . C38 C 0.1522(5) 0.8573(3) 0.0440(4) 0.0496(13) Uani 1 1 d . . . H38A H 0.0854 0.8139 0.0671 0.074 Uiso 1 1 calc R B . H38B H 0.1132 0.8968 0.0038 0.074 Uiso 1 1 calc R . . H38C H 0.1800 0.8902 0.0889 0.074 Uiso 1 1 calc R . . C39 C 0.8444(6) 0.5126(3) 0.1424(3) 0.0468(12) Uani 1 1 d . . . H39A H 0.9281 0.4863 0.1191 0.070 Uiso 1 1 calc R B . H39B H 0.7836 0.4673 0.1690 0.070 Uiso 1 1 calc R . . H39C H 0.8634 0.5532 0.1837 0.070 Uiso 1 1 calc R . . C40 C 0.7109(6) 0.4957(3) -0.0180(3) 0.0472(13) Uani 1 1 d . . . H40A H 0.6768 0.5282 -0.0649 0.071 Uiso 1 1 calc R B . H40B H 0.6404 0.4577 0.0104 0.071 Uiso 1 1 calc R . . H40C H 0.7879 0.4608 -0.0385 0.071 Uiso 1 1 calc R . . C41 C 0.8980(5) 0.6453(3) 0.0037(3) 0.0469(12) Uani 1 1 d . . . H41A H 0.9823 0.6132 -0.0038 0.070 Uiso 1 1 calc R B . H41B H 0.9088 0.6943 0.0379 0.070 Uiso 1 1 calc R . . H41C H 0.8737 0.6667 -0.0507 0.070 Uiso 1 1 calc R . . C42A C 0.7984(5) 0.9136(3) -0.0186(3) 0.0453(12) Uani 0.624(15) 1 d P B 1 H42A H 0.7511 0.9696 -0.0230 0.054 Uiso 0.624(15) 1 calc PR B 1 H42B H 0.8452 0.9058 0.0319 0.054 Uiso 0.624(15) 1 calc PR B 1 C43A C 0.8693(9) 0.8838(5) -0.0956(5) 0.043(3) Uani 0.624(15) 1 d P B 1 H43A H 0.9620 0.8706 -0.0976 0.051 Uiso 0.624(15) 1 calc PR B 1 C44A C 0.8090(7) 0.8753(4) -0.1605(4) 0.0664(18) Uani 0.624(15) 1 d P B 1 H44A H 0.8549 0.8398 -0.2040 0.080 Uiso 0.624(15) 1 calc PR B 1 H44B H 0.7656 0.9276 -0.1831 0.080 Uiso 0.624(15) 1 calc PR B 1 C42B C 0.7984(5) 0.9136(3) -0.0186(3) 0.0453(12) Uani 0.376(15) 1 d P B 2 H42C H 0.7462 0.9516 0.0200 0.054 Uiso 0.376(15) 1 calc PR B 2 H42D H 0.8916 0.9044 -0.0060 0.054 Uiso 0.376(15) 1 calc PR B 2 C43B C 0.7792(16) 0.9264(9) -0.1060(10) 0.051(5) Uani 0.376(15) 1 d P B 2 H43B H 0.7397 0.9794 -0.1227 0.061 Uiso 0.376(15) 1 calc PR B 2 C44B C 0.8090(7) 0.8753(4) -0.1605(4) 0.0664(18) Uani 0.376(15) 1 d P B 2 H44C H 0.9052 0.8611 -0.1722 0.080 Uiso 0.376(15) 1 calc PR B 2 H44D H 0.7629 0.8832 -0.2112 0.080 Uiso 0.376(15) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03098(18) 0.03181(18) 0.02292(16) 0.00041(12) -0.00424(13) -0.00235(13) Cl1 0.0381(6) 0.0360(6) 0.0422(6) 0.0003(5) 0.0011(5) 0.0021(4) P1 0.0272(5) 0.0276(5) 0.0219(5) 0.0000(4) -0.0052(4) -0.0014(4) Si1 0.0323(6) 0.0356(6) 0.0315(6) 0.0005(5) -0.0117(5) -0.0033(5) Si2 0.0363(7) 0.0324(6) 0.0286(6) -0.0046(5) -0.0108(5) -0.0018(5) C1 0.034(2) 0.032(2) 0.025(2) -0.0030(16) -0.0071(17) -0.0012(17) C2 0.033(2) 0.031(2) 0.025(2) -0.0034(16) -0.0083(17) 0.0021(17) C3 0.030(2) 0.035(2) 0.025(2) 0.0007(17) -0.0042(17) -0.0012(17) C4 0.029(2) 0.031(2) 0.028(2) -0.0005(16) -0.0057(17) -0.0004(16) C5 0.028(2) 0.030(2) 0.027(2) -0.0026(16) -0.0062(16) -0.0012(16) C6 0.024(2) 0.032(2) 0.027(2) -0.0056(16) -0.0070(16) -0.0032(16) C7 0.039(2) 0.033(2) 0.033(2) -0.0006(18) -0.0034(19) -0.0036(18) C8 0.037(3) 0.034(2) 0.051(3) -0.001(2) -0.005(2) 0.0037(19) C9 0.032(2) 0.046(3) 0.038(2) -0.007(2) -0.001(2) 0.0059(19) C10 0.034(2) 0.039(2) 0.030(2) -0.0023(18) -0.0035(18) -0.0027(18) C11 0.033(2) 0.032(2) 0.025(2) -0.0046(16) -0.0085(17) -0.0022(17) C12 0.045(3) 0.042(3) 0.025(2) 0.0044(18) -0.0088(19) 0.000(2) C13 0.036(2) 0.037(2) 0.042(3) 0.004(2) -0.004(2) -0.0091(19) C14 0.047(3) 0.051(3) 0.038(3) 0.002(2) -0.015(2) -0.018(2) C15 0.060(3) 0.052(3) 0.034(2) -0.002(2) -0.023(2) -0.009(2) C16 0.035(3) 0.046(3) 0.071(4) 0.001(3) -0.020(3) 0.001(2) C17 0.041(3) 0.044(3) 0.027(2) -0.0020(18) -0.0088(19) -0.003(2) C18 0.054(3) 0.037(3) 0.044(3) -0.011(2) -0.014(2) 0.002(2) C19 0.047(3) 0.053(3) 0.044(3) 0.002(2) -0.020(2) -0.012(2) C20A 0.053(3) 0.034(2) 0.037(2) 0.0038(19) -0.004(2) 0.005(2) C21A 0.056(6) 0.040(5) 0.026(4) 0.016(3) -0.009(4) -0.007(4) C22A 0.080(4) 0.043(3) 0.052(3) 0.020(3) 0.029(3) 0.008(3) C20B 0.053(3) 0.034(2) 0.037(2) 0.0038(19) -0.004(2) 0.005(2) C21B 0.060(10) 0.031(7) 0.043(8) 0.014(6) 0.001(7) -0.003(6) C22B 0.080(4) 0.043(3) 0.052(3) 0.020(3) 0.029(3) 0.008(3) Pd2 0.03244(19) 0.03290(19) 0.02962(18) -0.00075(13) -0.00369(14) -0.00332(13) Cl2 0.0561(7) 0.0400(6) 0.0292(5) -0.0021(4) -0.0065(5) -0.0096(5) P2 0.0266(5) 0.0299(5) 0.0263(5) -0.0037(4) -0.0054(4) -0.0014(4) Si3 0.0321(6) 0.0352(7) 0.0407(7) 0.0009(5) -0.0124(5) -0.0002(5) Si4 0.0353(7) 0.0350(6) 0.0274(6) -0.0066(5) -0.0085(5) 0.0052(5) C23 0.027(2) 0.034(2) 0.032(2) -0.0052(17) -0.0064(17) -0.0012(17) C24 0.029(2) 0.036(2) 0.032(2) -0.0112(18) -0.0049(18) -0.0006(17) C25 0.031(2) 0.038(2) 0.024(2) -0.0042(17) -0.0031(17) -0.0053(17) C26 0.032(2) 0.037(2) 0.025(2) -0.0062(17) -0.0083(17) -0.0035(17) C27 0.033(2) 0.030(2) 0.026(2) -0.0061(16) -0.0065(17) 0.0010(17) C28 0.026(2) 0.034(2) 0.033(2) -0.0062(18) -0.0073(17) 0.0031(17) C29 0.031(2) 0.036(2) 0.041(2) -0.0083(19) -0.0095(19) 0.0007(18) C30 0.045(3) 0.040(3) 0.048(3) -0.016(2) -0.017(2) 0.003(2) C31 0.038(3) 0.050(3) 0.040(3) -0.020(2) -0.011(2) 0.007(2) C32 0.034(2) 0.047(3) 0.031(2) -0.0098(19) -0.0074(19) 0.005(2) C33 0.029(2) 0.039(2) 0.029(2) -0.0079(18) -0.0065(17) 0.0038(17) C34 0.037(3) 0.046(3) 0.037(2) -0.007(2) -0.005(2) -0.004(2) C35 0.046(3) 0.039(3) 0.030(2) -0.0019(19) -0.011(2) -0.005(2) C36 0.051(3) 0.051(3) 0.042(3) 0.006(2) -0.024(2) -0.005(2) C37 0.044(3) 0.039(3) 0.055(3) 0.009(2) -0.012(2) 0.000(2) C38 0.032(3) 0.043(3) 0.072(4) 0.004(3) -0.008(2) 0.004(2) C39 0.055(3) 0.049(3) 0.040(3) -0.008(2) -0.019(2) 0.016(2) C40 0.062(3) 0.043(3) 0.041(3) -0.014(2) -0.023(2) 0.013(2) C41 0.030(2) 0.058(3) 0.052(3) 0.004(2) -0.003(2) 0.002(2) C42A 0.045(3) 0.042(3) 0.049(3) -0.006(2) -0.002(2) -0.016(2) C43A 0.034(5) 0.042(5) 0.051(5) 0.002(4) -0.001(4) -0.016(4) C44A 0.089(5) 0.061(4) 0.045(3) 0.004(3) 0.009(3) -0.036(3) C42B 0.045(3) 0.042(3) 0.049(3) -0.006(2) -0.002(2) -0.016(2) C43B 0.054(10) 0.038(8) 0.058(10) 0.008(7) -0.001(7) -0.015(7) C44B 0.089(5) 0.061(4) 0.045(3) 0.004(3) 0.009(3) -0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C20A 2.123(5) . ? Pd1 C21A 2.139(7) . ? Pd1 C21B 2.148(12) . ? Pd1 C22A 2.210(5) . ? Pd1 P1 2.2913(10) . ? Pd1 Cl1 2.3743(11) . ? P1 C6 1.833(4) . ? P1 C1 1.845(4) . ? P1 C5 1.846(4) . ? Si1 C16 1.856(5) . ? Si1 C14 1.865(5) . ? Si1 C15 1.881(5) . ? Si1 C1 1.887(5) . ? Si2 C18 1.858(5) . ? Si2 C17 1.874(5) . ? Si2 C5 1.885(4) . ? Si2 C19 1.886(5) . ? C1 C2 1.353(6) . ? C2 C12 1.500(6) . ? C2 C3 1.532(6) . ? C3 C11 1.521(6) . ? C3 C4 1.530(6) . ? C3 H3 1.0000 . ? C4 C5 1.338(6) . ? C4 C13 1.496(6) . ? C6 C7 1.385(6) . ? C6 C11 1.403(6) . ? C7 C8 1.389(6) . ? C7 H7 0.9500 . ? C8 C9 1.395(7) . ? C8 H8 0.9500 . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.390(6) . ? C10 H10 0.9500 . ? 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 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20A C21A 1.459(10) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A C22A 1.278(11) . ? C21A H21A 0.9500 . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C21B H21B 0.9500 . ? Pd2 C42A 2.110(5) . ? Pd2 C43A 2.154(7) . ? Pd2 C43B 2.160(13) . ? Pd2 C44A 2.208(5) . ? Pd2 P2 2.2935(11) . ? Pd2 Cl2 2.3696(12) . ? P2 C28 1.835(4) . ? P2 C27 1.843(4) . ? P2 C23 1.848(4) . ? Si3 C36 1.864(5) . ? Si3 C37 1.872(5) . ? Si3 C38 1.884(5) . ? Si3 C23 1.890(5) . ? Si4 C41 1.860(5) . ? Si4 C40 1.862(5) . ? Si4 C27 1.888(4) . ? Si4 C39 1.889(5) . ? C23 C24 1.338(6) . ? C24 C34 1.516(6) . ? C24 C25 1.532(6) . ? C25 C33 1.518(6) . ? C25 C26 1.535(6) . ? C25 H25 1.0000 . ? C26 C27 1.341(6) . ? C26 C35 1.506(6) . ? C28 C29 1.385(6) . ? C28 C33 1.395(6) . ? C29 C30 1.392(6) . ? C29 H29 0.9500 . ? C30 C31 1.388(7) . ? C30 H30 0.9500 . ? C31 C32 1.399(7) . ? C31 H31 0.9500 . ? C32 C33 1.390(6) . ? C32 H32 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42A C43A 1.463(10) . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? C43A C44A 1.288(11) . ? C43A H43A 0.9500 . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C43B H43B 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 C20A Pd1 C21A 40.0(3) . . ? C20A Pd1 C21B 38.5(4) . . ? C21A Pd1 C21B 27.7(4) . . ? C20A Pd1 C22A 68.0(2) . . ? C21A Pd1 C22A 34.1(3) . . ? C21B Pd1 C22A 33.1(4) . . ? C20A Pd1 P1 105.03(13) . . ? C21A Pd1 P1 140.5(2) . . ? C21B Pd1 P1 139.7(4) . . ? C22A Pd1 P1 172.72(15) . . ? C20A Pd1 Cl1 168.08(13) . . ? C21A Pd1 Cl1 128.9(2) . . ? C21B Pd1 Cl1 130.1(4) . . ? C22A Pd1 Cl1 100.09(15) . . ? P1 Pd1 Cl1 86.89(4) . . ? C6 P1 C1 97.01(19) . . ? C6 P1 C5 96.62(18) . . ? C1 P1 C5 101.28(19) . . ? C6 P1 Pd1 125.28(14) . . ? C1 P1 Pd1 115.63(14) . . ? C5 P1 Pd1 116.58(13) . . ? C16 Si1 C14 108.4(3) . . ? C16 Si1 C15 111.7(3) . . ? C14 Si1 C15 104.2(2) . . ? C16 Si1 C1 112.0(2) . . ? C14 Si1 C1 113.7(2) . . ? C15 Si1 C1 106.6(2) . . ? C18 Si2 C17 110.4(2) . . ? C18 Si2 C5 111.7(2) . . ? C17 Si2 C5 111.1(2) . . ? C18 Si2 C19 109.8(2) . . ? C17 Si2 C19 105.7(2) . . ? C5 Si2 C19 108.0(2) . . ? C2 C1 P1 111.3(3) . . ? C2 C1 Si1 122.9(3) . . ? P1 C1 Si1 125.5(2) . . ? C1 C2 C12 127.1(4) . . ? C1 C2 C3 118.4(4) . . ? C12 C2 C3 114.5(4) . . ? C11 C3 C4 108.6(3) . . ? C11 C3 C2 108.7(4) . . ? C4 C3 C2 108.3(3) . . ? C11 C3 H3 110.4 . . ? C4 C3 H3 110.4 . . ? C2 C3 H3 110.4 . . ? C5 C4 C13 126.5(4) . . ? C5 C4 C3 119.0(4) . . ? C13 C4 C3 114.5(4) . . ? C4 C5 P1 111.4(3) . . ? C4 C5 Si2 123.3(3) . . ? P1 C5 Si2 124.8(2) . . ? C7 C6 C11 120.1(4) . . ? C7 C6 P1 127.7(3) . . ? C11 C6 P1 112.1(3) . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C6 119.9(4) . . ? C10 C11 C3 124.1(4) . . ? C6 C11 C3 116.0(4) . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21A C20A Pd1 70.5(3) . . ? C21A C20A H20A 116.6 . . ? Pd1 C20A H20A 116.6 . . ? C21A C20A H20B 116.6 . . ? Pd1 C20A H20B 116.6 . . ? H20A C20A H20B 113.6 . . ? C22A C21A C20A 124.5(9) . . ? C22A C21A Pd1 76.0(4) . . ? C20A C21A Pd1 69.4(3) . . ? C22A C21A H21A 117.8 . . ? C20A C21A H21A 117.8 . . ? Pd1 C21A H21A 129.6 . . ? C21A C22A Pd1 69.9(4) . . ? C21A C22A H22A 116.7 . . ? Pd1 C22A H22A 116.7 . . ? C21A C22A H22B 116.7 . . ? Pd1 C22A H22B 116.7 . . ? H22A C22A H22B 113.7 . . ? Pd1 C21B H21B 135.9 . . ? C42A Pd2 C43A 40.1(3) . . ? C42A Pd2 C43B 39.8(5) . . ? C43A Pd2 C43B 30.6(5) . . ? C42A Pd2 C44A 67.5(2) . . ? C43A Pd2 C44A 34.3(3) . . ? C43B Pd2 C44A 32.8(4) . . ? C42A Pd2 P2 104.12(14) . . ? C43A Pd2 P2 139.7(2) . . ? C43B Pd2 P2 138.2(4) . . ? C44A Pd2 P2 170.97(17) . . ? C42A Pd2 Cl2 167.16(14) . . ? C43A Pd2 Cl2 128.2(2) . . ? C43B Pd2 Cl2 128.1(4) . . ? C44A Pd2 Cl2 99.64(17) . . ? P2 Pd2 Cl2 88.68(4) . . ? C28 P2 C27 97.18(19) . . ? C28 P2 C23 96.69(19) . . ? C27 P2 C23 100.41(19) . . ? C28 P2 Pd2 125.66(15) . . ? C27 P2 Pd2 116.35(13) . . ? C23 P2 Pd2 115.89(14) . . ? C36 Si3 C37 109.1(2) . . ? C36 Si3 C38 109.3(3) . . ? C37 Si3 C38 105.3(2) . . ? C36 Si3 C23 111.9(2) . . ? C37 Si3 C23 112.3(2) . . ? C38 Si3 C23 108.7(2) . . ? C41 Si4 C40 110.2(3) . . ? C41 Si4 C27 110.6(2) . . ? C40 Si4 C27 111.5(2) . . ? C41 Si4 C39 104.2(3) . . ? C40 Si4 C39 110.5(2) . . ? C27 Si4 C39 109.6(2) . . ? C24 C23 P2 111.3(3) . . ? C24 C23 Si3 124.6(3) . . ? P2 C23 Si3 124.0(2) . . ? C23 C24 C34 127.5(4) . . ? C23 C24 C25 119.3(4) . . ? C34 C24 C25 113.2(4) . . ? C33 C25 C24 108.4(4) . . ? C33 C25 C26 109.7(3) . . ? C24 C25 C26 106.1(3) . . ? C33 C25 H25 110.8 . . ? C24 C25 H25 110.8 . . ? C26 C25 H25 110.8 . . ? C27 C26 C35 126.0(4) . . ? C27 C26 C25 118.5(4) . . ? C35 C26 C25 115.4(4) . . ? C26 C27 P2 111.9(3) . . ? C26 C27 Si4 123.3(3) . . ? P2 C27 Si4 124.7(2) . . ? C29 C28 C33 120.9(4) . . ? C29 C28 P2 127.3(3) . . ? C33 C28 P2 111.7(3) . . ? C28 C29 C30 119.2(4) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.6(4) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 119.0(4) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C28 120.0(4) . . ? C32 C33 C25 122.9(4) . . ? C28 C33 C25 117.1(4) . . ? C24 C34 H34A 109.5 . . ? C24 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C24 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C26 C35 H35A 109.5 . . ? C26 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C26 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si3 C36 H36A 109.5 . . ? Si3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si4 C39 H39A 109.5 . . ? Si4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43A C42A Pd2 71.6(4) . . ? C43A C42A H42A 116.4 . . ? Pd2 C42A H42A 116.4 . . ? C43A C42A H42B 116.4 . . ? Pd2 C42A H42B 116.4 . . ? H42A C42A H42B 113.4 . . ? C44A C43A C42A 121.5(8) . . ? C44A C43A Pd2 75.1(4) . . ? C42A C43A Pd2 68.3(3) . . ? C44A C43A H43A 119.3 . . ? C42A C43A H43A 119.3 . . ? Pd2 C43A H43A 129.8 . . ? C43A C44A Pd2 70.5(4) . . ? C43A C44A H44A 116.6 . . ? Pd2 C44A H44A 116.6 . . ? C43A C44A H44B 116.6 . . ? Pd2 C44A H44B 116.6 . . ? H44A C44A H44B 113.6 . . ? Pd2 C43B H43B 133.2 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.098 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.120 #===END #compound 4 data_mb462 _database_code_depnum_ccdc_archive 'CCDC 699915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H58 P2 Pd Si4' _chemical_formula_sum 'C38 H58 P2 Pd Si4' _chemical_formula_weight 795.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.310(1) _cell_length_b 18.846(1) _cell_length_c 43.610(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8473.5(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 149884 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Plate _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.9744 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44281 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.70 _reflns_number_total 10810 _reflns_number_gt 7801 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1630P)^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_number_reflns 10810 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2271 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.97886(3) -0.046189(15) -0.121103(7) 0.02931(13) Uani 1 1 d . . . P1 P 1.07464(9) 0.00605(5) -0.16230(2) 0.0282(2) Uani 1 1 d . . . P2 P 0.83210(9) -0.07048(5) -0.08382(2) 0.0279(2) Uani 1 1 d . . . Si1 Si 1.14345(11) -0.14216(6) -0.19591(3) 0.0378(3) Uani 1 1 d . . . Si2 Si 1.30037(12) 0.07198(6) -0.12166(3) 0.0369(3) Uani 1 1 d . . . Si3 Si 1.03750(10) -0.13246(6) -0.03599(3) 0.0331(3) Uani 1 1 d . . . Si4 Si 0.67972(11) -0.17091(6) -0.13063(3) 0.0337(3) Uani 1 1 d . . . C1 C 1.1294(4) -0.04281(19) -0.19705(10) 0.0343(9) Uani 1 1 d . . . C2 C 1.1606(4) 0.0005(2) -0.22063(10) 0.0408(10) Uani 1 1 d . . . C3 C 1.1598(4) 0.0810(2) -0.21442(10) 0.0405(10) Uani 1 1 d . . . H3 H 1.1911 0.1073 -0.2329 0.049 Uiso 1 1 calc R . . C4 C 1.2482(4) 0.0960(2) -0.18698(10) 0.0371(9) Uani 1 1 d . . . C5 C 1.2192(4) 0.0654(2) -0.15953(10) 0.0341(8) Uani 1 1 d . . . C6 C 0.9673(4) 0.0690(2) -0.18183(9) 0.0324(8) Uani 1 1 d . . . C7 C 0.8414(4) 0.0845(2) -0.17336(11) 0.0386(9) Uani 1 1 d . . . H7 H 0.8031 0.0616 -0.1562 0.046 Uiso 1 1 calc R . . C8 C 0.7706(5) 0.1345(2) -0.19037(11) 0.0476(11) Uani 1 1 d . . . H8 H 0.6824 0.1434 -0.1853 0.057 Uiso 1 1 calc R . . C9 C 0.8264(5) 0.1701(2) -0.21386(12) 0.0528(13) Uani 1 1 d . . . H9 H 0.7791 0.2063 -0.2241 0.063 Uiso 1 1 calc R . . C10 C 0.9521(5) 0.1543(2) -0.22318(11) 0.0466(11) Uani 1 1 d . . . H10 H 0.9898 0.1778 -0.2403 0.056 Uiso 1 1 calc R . . C11 C 1.0225(4) 0.1029(2) -0.20671(10) 0.0378(9) Uani 1 1 d . . . C12 C 1.1976(7) -0.0204(3) -0.25310(11) 0.0638(15) Uani 1 1 d . . . H12A H 1.2880 -0.0069 -0.2570 0.096 Uiso 1 1 calc R . . H12B H 1.1408 0.0040 -0.2677 0.096 Uiso 1 1 calc R . . H12C H 1.1880 -0.0718 -0.2556 0.096 Uiso 1 1 calc R . . C13 C 1.3616(5) 0.1430(2) -0.19407(11) 0.0481(11) Uani 1 1 d . . . H13A H 1.4053 0.1562 -0.1750 0.072 Uiso 1 1 calc R . . H13B H 1.3312 0.1859 -0.2045 0.072 Uiso 1 1 calc R . . H13C H 1.4225 0.1175 -0.2074 0.072 Uiso 1 1 calc R . . C14 C 1.2858(6) -0.1738(3) -0.21904(13) 0.0641(15) Uani 1 1 d . . . H14A H 1.3591 -0.1415 -0.2160 0.096 Uiso 1 1 calc R . . H14B H 1.2623 -0.1748 -0.2408 0.096 Uiso 1 1 calc R . . H14C H 1.3103 -0.2216 -0.2124 0.096 Uiso 1 1 calc R . . C15 C 1.1806(4) -0.1701(2) -0.15622(11) 0.0465(11) Uani 1 1 d . . . H15A H 1.1107 -0.1547 -0.1425 0.070 Uiso 1 1 calc R . . H15B H 1.2625 -0.1484 -0.1497 0.070 Uiso 1 1 calc R . . H15C H 1.1884 -0.2218 -0.1554 0.070 Uiso 1 1 calc R . . C16 C 0.9895(5) -0.1810(3) -0.21009(13) 0.0506(12) Uani 1 1 d . . . H16A H 0.9818 -0.2300 -0.2028 0.076 Uiso 1 1 calc R . . H16B H 0.9892 -0.1805 -0.2326 0.076 Uiso 1 1 calc R . . H16C H 0.9163 -0.1530 -0.2024 0.076 Uiso 1 1 calc R . . C17 C 1.1917(6) 0.1221(3) -0.09509(11) 0.0680(17) Uani 1 1 d . . . H17A H 1.1780 0.1702 -0.1031 0.102 Uiso 1 1 calc R . . H17B H 1.2320 0.1248 -0.0748 0.102 Uiso 1 1 calc R . . H17C H 1.1081 0.0976 -0.0935 0.102 Uiso 1 1 calc R . . C18 C 1.4629(7) 0.1153(5) -0.12285(16) 0.102(3) Uani 1 1 d . . . H18A H 1.5190 0.0898 -0.1373 0.153 Uiso 1 1 calc R . . H18B H 1.5018 0.1141 -0.1024 0.153 Uiso 1 1 calc R . . H18C H 1.4534 0.1646 -0.1295 0.153 Uiso 1 1 calc R . . C19 C 1.3292(5) -0.0190(2) -0.10647(11) 0.0475(11) Uani 1 1 d . . . H19A H 1.2465 -0.0444 -0.1050 0.071 Uiso 1 1 calc R . . H19B H 1.3689 -0.0159 -0.0861 0.071 Uiso 1 1 calc R . . H19C H 1.3875 -0.0447 -0.1203 0.071 Uiso 1 1 calc R . . C20 C 0.8651(4) -0.10816(19) -0.04486(9) 0.0303(7) Uani 1 1 d . . . C21 C 0.7591(4) -0.10937(19) -0.02704(9) 0.0333(8) Uani 1 1 d . . . C22 C 0.6306(4) -0.0816(2) -0.04027(9) 0.0347(8) Uani 1 1 d . . . H22 H 0.5590 -0.0864 -0.0249 0.042 Uiso 1 1 calc R . . C23 C 0.5993(4) -0.1245(2) -0.06980(9) 0.0337(8) Uani 1 1 d . . . C24 C 0.6845(3) -0.12403(19) -0.09252(9) 0.0297(8) Uani 1 1 d . . . C25 C 0.7498(4) 0.00918(19) -0.06972(8) 0.0298(7) Uani 1 1 d . . . C26 C 0.7817(4) 0.0786(2) -0.07706(10) 0.0371(9) Uani 1 1 d . . . H26 H 0.8497 0.0879 -0.0912 0.044 Uiso 1 1 calc R . . C27 C 0.7143(5) 0.1346(2) -0.06380(10) 0.0417(10) Uani 1 1 d . . . H27 H 0.7363 0.1821 -0.0688 0.050 Uiso 1 1 calc R . . C28 C 0.6153(5) 0.1208(2) -0.04332(11) 0.0471(11) Uani 1 1 d . . . H28 H 0.5695 0.1592 -0.0343 0.056 Uiso 1 1 calc R . . C29 C 0.5815(5) 0.0514(2) -0.03576(10) 0.0415(10) Uani 1 1 d . . . H29 H 0.5122 0.0423 -0.0220 0.050 Uiso 1 1 calc R . . C30 C 0.6511(4) -0.0045(2) -0.04877(9) 0.0338(8) Uani 1 1 d . . . C31 C 0.7495(5) -0.1326(2) 0.00597(9) 0.0420(10) Uani 1 1 d . . . H31A H 0.8340 -0.1502 0.0129 0.063 Uiso 1 1 calc R . . H31B H 0.6849 -0.1705 0.0078 0.063 Uiso 1 1 calc R . . H31C H 0.7233 -0.0922 0.0187 0.063 Uiso 1 1 calc R . . C32 C 0.4730(4) -0.1652(2) -0.06750(12) 0.0432(10) Uani 1 1 d . . . H32A H 0.4437 -0.1785 -0.0881 0.065 Uiso 1 1 calc R . . H32B H 0.4072 -0.1352 -0.0577 0.065 Uiso 1 1 calc R . . H32C H 0.4863 -0.2081 -0.0552 0.065 Uiso 1 1 calc R . . C33 C 1.1329(5) -0.0482(2) -0.03352(14) 0.0535(13) Uani 1 1 d . . . H33A H 1.1087 -0.0225 -0.0148 0.080 Uiso 1 1 calc R . . H33B H 1.1142 -0.0186 -0.0515 0.080 Uiso 1 1 calc R . . H33C H 1.2257 -0.0593 -0.0330 0.080 Uiso 1 1 calc R . . C34 C 1.0996(4) -0.1910(2) -0.06727(10) 0.0424(10) Uani 1 1 d . . . H34A H 1.1892 -0.2049 -0.0627 0.064 Uiso 1 1 calc R . . H34B H 1.0968 -0.1654 -0.0868 0.064 Uiso 1 1 calc R . . H34C H 1.0453 -0.2336 -0.0687 0.064 Uiso 1 1 calc R . . C35 C 1.0606(5) -0.1819(3) 0.00096(11) 0.0519(12) Uani 1 1 d . . . H35A H 0.9979 -0.2209 0.0021 0.078 Uiso 1 1 calc R . . H35B H 1.0471 -0.1495 0.0182 0.078 Uiso 1 1 calc R . . H35C H 1.1488 -0.2011 0.0018 0.078 Uiso 1 1 calc R . . C36 C 0.8325(4) -0.2231(2) -0.13365(11) 0.0429(10) Uani 1 1 d . . . H36A H 0.8388 -0.2440 -0.1542 0.064 Uiso 1 1 calc R . . H36B H 0.8322 -0.2609 -0.1182 0.064 Uiso 1 1 calc R . . H36C H 0.9069 -0.1918 -0.1301 0.064 Uiso 1 1 calc R . . C37 C 0.5430(5) -0.2356(3) -0.13562(15) 0.0573(14) Uani 1 1 d . . . H37A H 0.4601 -0.2105 -0.1341 0.086 Uiso 1 1 calc R . . H37B H 0.5478 -0.2720 -0.1196 0.086 Uiso 1 1 calc R . . H37C H 0.5498 -0.2583 -0.1558 0.086 Uiso 1 1 calc R . . C38 C 0.6689(5) -0.1036(3) -0.16181(10) 0.0527(12) Uani 1 1 d . . . H38A H 0.5928 -0.0734 -0.1584 0.079 Uiso 1 1 calc R . . H38B H 0.6607 -0.1277 -0.1816 0.079 Uiso 1 1 calc R . . H38C H 0.7474 -0.0743 -0.1618 0.079 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 0.02341(19) 0.0369(2) 0.0276(2) 0.00193(11) 0.00462(11) -0.00103(10) P1 0.0255(5) 0.0334(4) 0.0256(5) 0.0004(4) 0.0026(4) -0.0019(3) P2 0.0216(4) 0.0354(5) 0.0267(5) 0.0025(4) 0.0025(4) 0.0009(3) Si1 0.0340(6) 0.0374(5) 0.0418(7) -0.0045(5) 0.0086(5) 0.0000(4) Si2 0.0331(6) 0.0413(6) 0.0365(7) 0.0052(5) -0.0075(5) -0.0070(5) Si3 0.0268(5) 0.0376(5) 0.0350(6) 0.0001(5) -0.0027(4) 0.0017(4) Si4 0.0253(5) 0.0385(5) 0.0373(6) -0.0025(5) -0.0006(5) 0.0012(4) C1 0.033(2) 0.0356(18) 0.034(2) -0.0082(15) 0.0061(18) -0.0034(14) C2 0.046(2) 0.0395(19) 0.037(2) 0.0000(17) 0.006(2) -0.0071(17) C3 0.048(3) 0.044(2) 0.030(2) 0.0016(18) 0.0052(19) -0.0097(18) C4 0.039(2) 0.0345(18) 0.037(2) -0.0004(16) 0.0044(18) -0.0035(15) C5 0.0288(19) 0.0335(17) 0.040(2) 0.0007(16) 0.0028(17) -0.0038(15) C6 0.039(2) 0.0332(17) 0.0252(19) -0.0036(16) -0.0061(16) -0.0010(15) C7 0.032(2) 0.042(2) 0.042(2) -0.0030(18) -0.0043(18) 0.0019(16) C8 0.043(2) 0.047(2) 0.053(3) -0.012(2) -0.016(2) 0.0058(19) C9 0.060(3) 0.043(2) 0.056(3) -0.006(2) -0.024(3) 0.008(2) C10 0.065(3) 0.041(2) 0.034(2) 0.0070(18) -0.017(2) -0.007(2) C11 0.041(2) 0.037(2) 0.035(2) 0.0019(17) -0.0063(18) -0.0046(16) C12 0.095(5) 0.056(3) 0.040(3) -0.008(2) 0.023(3) -0.010(3) C13 0.052(3) 0.050(2) 0.043(3) 0.006(2) 0.007(2) -0.013(2) C14 0.069(4) 0.054(3) 0.070(4) -0.009(3) 0.034(3) 0.003(3) C15 0.041(2) 0.045(2) 0.053(3) -0.001(2) -0.010(2) 0.0053(18) C16 0.052(3) 0.046(2) 0.053(3) 0.001(2) -0.020(2) -0.002(2) C17 0.112(5) 0.063(3) 0.030(2) -0.007(2) -0.011(3) 0.027(3) C18 0.075(5) 0.150(7) 0.080(5) 0.056(5) -0.040(4) -0.071(5) C19 0.045(3) 0.052(2) 0.045(3) 0.012(2) -0.009(2) 0.005(2) C20 0.0304(18) 0.0345(16) 0.0261(18) 0.0048(15) -0.0004(15) 0.0021(14) C21 0.0317(19) 0.0374(18) 0.0307(19) 0.0006(16) 0.0011(16) 0.0016(15) C22 0.0274(18) 0.044(2) 0.033(2) 0.0045(17) 0.0077(16) 0.0034(15) C23 0.0255(18) 0.0384(18) 0.037(2) 0.0085(16) 0.0050(17) 0.0033(14) C24 0.0208(16) 0.0370(17) 0.031(2) 0.0028(15) 0.0025(15) 0.0008(13) C25 0.0305(18) 0.0349(17) 0.0241(17) 0.0010(14) -0.0008(16) 0.0039(14) C26 0.033(2) 0.0389(19) 0.040(2) 0.0044(17) -0.0037(18) 0.0010(16) C27 0.048(3) 0.040(2) 0.037(2) -0.0038(18) -0.008(2) 0.0080(18) C28 0.053(3) 0.046(2) 0.042(3) -0.010(2) -0.002(2) 0.017(2) C29 0.040(2) 0.055(2) 0.030(2) 0.0041(18) 0.0070(19) 0.0131(18) C30 0.0304(19) 0.0436(19) 0.0274(19) 0.0038(16) 0.0018(16) 0.0090(15) C31 0.041(2) 0.056(2) 0.030(2) 0.0098(19) 0.0055(19) 0.0047(18) C32 0.030(2) 0.048(2) 0.052(3) 0.006(2) 0.0078(19) -0.0031(16) C33 0.035(2) 0.048(2) 0.077(4) -0.008(2) 0.000(3) -0.0065(18) C34 0.031(2) 0.047(2) 0.049(3) -0.002(2) 0.0024(19) 0.0059(17) C35 0.047(3) 0.069(3) 0.040(3) 0.010(2) -0.006(2) 0.012(2) C36 0.031(2) 0.049(2) 0.048(3) -0.006(2) 0.004(2) 0.0013(17) C37 0.034(2) 0.064(3) 0.073(4) -0.020(3) -0.001(2) -0.005(2) C38 0.066(3) 0.061(3) 0.030(2) 0.010(2) -0.006(2) 0.005(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 Pd1 P2 2.2677(10) . ? Pd1 P1 2.2743(10) . ? P1 C6 1.833(4) . ? P1 C1 1.861(4) . ? P1 C5 1.867(4) . ? P2 C25 1.831(4) . ? P2 C24 1.865(4) . ? P2 C20 1.873(4) . ? Si1 C15 1.849(5) . ? Si1 C16 1.854(5) . ? Si1 C14 1.878(5) . ? Si1 C1 1.879(4) . ? Si2 C5 1.855(4) . ? Si2 C19 1.863(4) . ? Si2 C18 1.865(6) . ? Si2 C17 1.868(5) . ? Si3 C34 1.868(4) . ? Si3 C33 1.872(4) . ? Si3 C20 1.875(4) . ? Si3 C35 1.877(5) . ? Si4 C36 1.861(4) . ? Si4 C38 1.862(5) . ? Si4 C37 1.877(5) . ? Si4 C24 1.883(4) . ? C1 C2 1.352(6) . ? C2 C12 1.519(6) . ? C2 C3 1.541(6) . ? C3 C11 1.512(6) . ? C3 C4 1.531(6) . ? C3 H3 1.0000 . ? C4 C5 1.362(6) . ? C4 C13 1.499(6) . ? C6 C7 1.380(6) . ? C6 C11 1.382(6) . ? C7 C8 1.404(6) . ? C7 H7 0.9500 . ? C8 C9 1.353(7) . ? C8 H8 0.9500 . ? C9 C10 1.391(7) . ? C9 H9 0.9500 . ? C10 C11 1.408(6) . ? C10 H10 0.9500 . ? 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 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.342(5) . ? C21 C31 1.508(5) . ? C21 C22 1.537(5) . ? C22 C30 1.514(6) . ? C22 C23 1.555(6) . ? C22 H22 1.0000 . ? C23 C24 1.324(5) . ? C23 C32 1.514(5) . ? C25 C26 1.386(5) . ? C25 C30 1.391(6) . ? C26 C27 1.389(6) . ? C26 H26 0.9500 . ? C27 C28 1.381(7) . ? C27 H27 0.9500 . ? C28 C29 1.392(6) . ? C28 H28 0.9500 . ? C29 C30 1.396(5) . ? C29 H29 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 P2 Pd1 P1 160.65(4) . . ? C6 P1 C1 97.19(19) . . ? C6 P1 C5 97.15(18) . . ? C1 P1 C5 96.15(19) . . ? C6 P1 Pd1 112.65(14) . . ? C1 P1 Pd1 124.10(13) . . ? C5 P1 Pd1 123.69(14) . . ? C25 P2 C24 97.68(17) . . ? C25 P2 C20 95.20(17) . . ? C24 P2 C20 97.35(17) . . ? C25 P2 Pd1 112.61(13) . . ? C24 P2 Pd1 120.52(13) . . ? C20 P2 Pd1 127.28(13) . . ? C15 Si1 C16 112.2(2) . . ? C15 Si1 C14 104.5(2) . . ? C16 Si1 C14 111.4(3) . . ? C15 Si1 C1 108.9(2) . . ? C16 Si1 C1 108.6(2) . . ? C14 Si1 C1 111.3(2) . . ? C5 Si2 C19 109.1(2) . . ? C5 Si2 C18 114.2(2) . . ? C19 Si2 C18 105.6(3) . . ? C5 Si2 C17 108.4(2) . . ? C19 Si2 C17 109.9(2) . . ? C18 Si2 C17 109.6(4) . . ? C34 Si3 C33 111.3(2) . . ? C34 Si3 C20 108.57(19) . . ? C33 Si3 C20 107.6(2) . . ? C34 Si3 C35 106.9(2) . . ? C33 Si3 C35 107.8(3) . . ? C20 Si3 C35 114.7(2) . . ? C36 Si4 C38 111.0(2) . . ? C36 Si4 C37 106.5(2) . . ? C38 Si4 C37 108.2(3) . . ? C36 Si4 C24 106.76(19) . . ? C38 Si4 C24 109.1(2) . . ? C37 Si4 C24 115.3(2) . . ? C2 C1 P1 113.2(3) . . ? C2 C1 Si1 127.1(3) . . ? P1 C1 Si1 119.7(2) . . ? C1 C2 C12 127.8(4) . . ? C1 C2 C3 117.3(4) . . ? C12 C2 C3 114.9(4) . . ? C11 C3 C4 109.4(3) . . ? C11 C3 C2 108.2(3) . . ? C4 C3 C2 108.4(3) . . ? C11 C3 H3 110.2 . . ? C4 C3 H3 110.2 . . ? C2 C3 H3 110.2 . . ? C5 C4 C13 127.1(4) . . ? C5 C4 C3 118.6(4) . . ? C13 C4 C3 114.4(4) . . ? C4 C5 Si2 130.9(3) . . ? C4 C5 P1 111.8(3) . . ? Si2 C5 P1 117.3(2) . . ? C7 C6 C11 120.0(4) . . ? C7 C6 P1 125.5(3) . . ? C11 C6 P1 114.5(3) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.8(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 118.6(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C6 C11 C10 120.4(4) . . ? C6 C11 C3 115.7(4) . . ? C10 C11 C3 123.8(4) . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P2 112.6(3) . . ? C21 C20 Si3 130.4(3) . . ? P2 C20 Si3 116.9(2) . . ? C20 C21 C31 127.7(4) . . ? C20 C21 C22 118.6(3) . . ? C31 C21 C22 113.6(3) . . ? C30 C22 C21 107.3(3) . . ? C30 C22 C23 109.0(3) . . ? C21 C22 C23 108.2(3) . . ? C30 C22 H22 110.7 . . ? C21 C22 H22 110.7 . . ? C23 C22 H22 110.7 . . ? C24 C23 C32 128.6(4) . . ? C24 C23 C22 118.6(4) . . ? C32 C23 C22 112.7(3) . . ? C23 C24 P2 113.1(3) . . ? C23 C24 Si4 129.8(3) . . ? P2 C24 Si4 117.04(19) . . ? C26 C25 C30 120.0(4) . . ? C26 C25 P2 125.9(3) . . ? C30 C25 P2 114.0(3) . . ? C25 C26 C27 120.1(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 119.7(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.9(4) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C30 119.0(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C25 C30 C29 120.1(4) . . ? C25 C30 C22 116.2(3) . . ? C29 C30 C22 123.6(4) . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C32 H32A 109.5 . . ? C23 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C23 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si3 C34 H34A 109.5 . . ? Si3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si3 C35 H35A 109.5 . . ? Si3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si4 C36 H36A 109.5 . . ? Si4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si4 C37 H37A 109.5 . . ? Si4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si4 C38 H38A 109.5 . . ? Si4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.710 _refine_diff_density_min -1.876 _refine_diff_density_rms 0.165 #===END