# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1754 data_global _publ_requested_journal ' Journal of Chemical Society, Dalton Transactions ' _publ_section_title ; Dipalladium Complexes with Bridigng Diorganosilyl Ligands. Synthesis, Structures, and Properties of [LPd(\m-SiH(R)Ph)]2 (R = Ph, Me; L = PMe3, PEt3, PMePh2) ; _publ_author_name ; Yong-Joo Kim, Sang-Chul Lee, Jong-Il Park, Kohtaro Osakada, Jun-Chul Choi, Takakazu Yamamoto ; _publ_section_synopsis ? _publ_section_abstract ? _publ_section_comment 'xxxxx' _publ_contact_author_name ' Yong-Joo Kim ' _publ_contact_author_address ; Department of Chemistry, Kangnung National University, Kangnung 210-702, Korea ; _publ_contact_author_phone ' +82-391-640-2308 ' _publ_contact_author_fax ' +82-391-647-1183 ' _publ_contact_author_email ' yjkim@knusun.kangnung.ac.kr' data_form1 _cell_length_a 10.242(9) _cell_length_b 11.447(6) _cell_length_c 9.725(8) _cell_angle_alpha 112.13(5) _cell_angle_beta 115.65(6) _cell_angle_gamma 78.56(6) _cell_volume 951(1) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 13.96 _cell_measurement_theta_max 19.10 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' _exptl_crystal_description 'plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 815.36 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H52 P2 Pd2 Si2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 418.00 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.793 _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method ? _diffrn_reflns_number 3544 _reflns_number_total 3340 _reflns_number_gt 2835 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.07137 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02804 _diffrn_orient_matrix_UB_12 0.08868 _diffrn_orient_matrix_UB_13 0.03483 _diffrn_orient_matrix_UB_21 -0.07792 _diffrn_orient_matrix_UB_22 0.03169 _diffrn_orient_matrix_UB_23 0.04274 _diffrn_orient_matrix_UB_31 0.06997 _diffrn_orient_matrix_UB_32 -0.00641 _diffrn_orient_matrix_UB_33 0.10749 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 0 36 0.003 0.002 H 0 52 0.000 0.000 Si 0 2 0.082 0.070 P 0 2 0.102 0.094 Pd 0 2 -0.999 1.007 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.12054(5) -0.07102(4) -0.00672(5) 0.0350(1) 1.000 . Uani d ? P(1) 0.2849(2) -0.2403(1) -0.0071(2) 0.0446(4) 1.000 . Uani d ? Si(1) 0.0623(2) 0.1371(1) -0.0259(2) 0.0359(4) 1.000 . Uani d ? C(1) 0.1625(6) 0.2778(5) 0.1429(7) 0.039(1) 1.000 . Uani d ? C(2) 0.2553(8) 0.2678(6) 0.2918(8) 0.057(2) 1.000 . Uani d ? C(3) 0.3232(9) 0.3705(8) 0.4219(8) 0.072(2) 1.000 . Uani d ? C(4) 0.2981(9) 0.4884(7) 0.4052(9) 0.068(2) 1.000 . Uani d ? C(5) 0.2067(9) 0.5020(6) 0.2601(9) 0.063(2) 1.000 . Uani d ? C(6) 0.1408(7) 0.3986(5) 0.1301(8) 0.049(2) 1.000 . Uani d ? C(7) 0.0102(7) 0.1628(5) -0.2237(7) 0.044(2) 1.000 . Uani d ? C(8) 0.1053(8) 0.2133(6) -0.2538(8) 0.056(2) 1.000 . Uani d ? C(9) 0.0715(10) 0.2173(7) -0.4060(10) 0.069(3) 1.000 . Uani d ? C(10) -0.054(1) 0.1719(7) -0.5305(9) 0.077(3) 1.000 . Uani d ? C(11) -0.1505(9) 0.1240(7) -0.5045(9) 0.074(2) 1.000 . Uani d ? C(12) -0.1170(8) 0.1191(6) -0.3529(8) 0.057(2) 1.000 . Uani d ? C(13) 0.4117(9) -0.2453(7) 0.1906(9) 0.076(2) 1.000 . Uani d ? C(14) 0.491(1) -0.127(1) 0.300(1) 0.106(3) 1.000 . Uani d ? C(15) 0.3999(8) -0.2453(7) -0.1104(10) 0.067(2) 1.000 . Uani d ? C(16) 0.503(1) -0.350(2) -0.120(2) 0.164(2) 1.000 . Uani d ? C(17) 0.2172(8) -0.4007(6) -0.1051(10) 0.066(2) 1.000 . Uani d ? C(18) 0.1205(9) -0.4300(7) -0.281(1) 0.077(3) 1.000 . Uani d ? H(1) 0.2727 0.1853 0.3043 0.0678 1.000 . Uiso c ? H(2) 0.3888 0.3596 0.5248 0.0857 1.000 . Uiso c ? H(3) 0.3444 0.5610 0.4956 0.0818 1.000 . Uiso c ? H(4) 0.1876 0.5847 0.2479 0.0737 1.000 . Uiso c ? H(5) 0.0781 0.4092 0.0269 0.0600 1.000 . Uiso c ? H(6) 0.1968 0.2463 -0.1651 0.0682 1.000 . Uiso c ? H(7) 0.1394 0.2519 -0.4241 0.0852 1.000 . Uiso c ? H(8) -0.0759 0.1736 -0.6372 0.0914 1.000 . Uiso c ? H(9) -0.2430 0.0930 -0.5931 0.0886 1.000 . Uiso c ? H(10) -0.1856 0.0840 -0.3359 0.0704 1.000 . Uiso c ? H(11) 0.3597 -0.2613 0.2445 0.0921 1.000 . Uiso c ? H(12) 0.4814 -0.3140 0.1798 0.0921 1.000 . Uiso c ? H(13) 0.5572 -0.1329 0.4019 0.1226 1.000 . Uiso c ? H(14) 0.5455 -0.1090 0.2501 0.1226 1.000 . Uiso c ? H(15) 0.4244 -0.0566 0.3158 0.1226 1.000 . Uiso c ? H(16) 0.3380 -0.2482 -0.2208 0.0820 1.000 . Uiso c ? H(17) 0.4513 -0.1688 -0.0591 0.0820 1.000 . Uiso c ? H(18) 0.4560 -0.4292 -0.1736 0.1774 1.000 . Uiso c ? H(19) 0.5604 -0.3484 -0.1747 0.1774 1.000 . Uiso c ? H(20) 0.5693 -0.3498 -0.0119 0.1774 1.000 . Uiso c ? H(21) 0.2965 -0.4612 -0.0951 0.0798 1.000 . Uiso c ? H(22) 0.1622 -0.4116 -0.0516 0.0798 1.000 . Uiso c ? H(23) 0.0375 -0.3719 -0.2951 0.0919 1.000 . Uiso c ? H(24) 0.1719 -0.4210 -0.3386 0.0919 1.000 . Uiso c ? H(25) 0.0869 -0.5135 -0.3284 0.0919 1.000 . Uiso c ? H(26) 0.208(9) 0.058(8) -0.037(10) 0.12(2) 1.000 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0404(2) 0.0292(2) 0.0462(2) 0.0022(2) 0.0186(2) 0.0149(2) P(1) 0.0493(9) 0.0317(7) 0.0545(9) 0.0099(6) 0.0220(7) 0.0189(7) Si(1) 0.0439(8) 0.0226(7) 0.0462(9) -0.0007(6) 0.0183(7) 0.0154(6) C(1) 0.042(3) 0.033(3) 0.045(3) -0.005(2) 0.017(3) 0.015(2) C(2) 0.069(4) 0.049(4) 0.050(4) -0.007(3) 0.016(3) 0.019(3) C(3) 0.081(5) 0.073(5) 0.044(4) -0.012(4) 0.007(4) 0.015(4) C(4) 0.081(5) 0.052(4) 0.062(5) -0.029(4) 0.030(4) -0.008(3) C(5) 0.090(5) 0.035(3) 0.066(5) -0.019(3) 0.034(4) 0.008(3) C(6) 0.065(4) 0.030(3) 0.056(4) -0.009(3) 0.021(3) 0.016(3) C(7) 0.064(4) 0.024(3) 0.047(3) -0.001(3) 0.024(3) 0.011(2) C(8) 0.079(5) 0.043(3) 0.058(4) -0.006(3) 0.035(4) 0.018(3) C(9) 0.112(7) 0.053(4) 0.070(5) 0.001(4) 0.053(5) 0.029(4) C(10) 0.126(8) 0.056(4) 0.053(4) 0.010(5) 0.037(5) 0.026(4) C(11) 0.089(6) 0.059(4) 0.051(4) -0.001(4) 0.009(4) 0.017(4) C(12) 0.071(4) 0.042(3) 0.052(4) -0.004(3) 0.016(3) 0.017(3) C(13) 0.076(5) 0.069(5) 0.066(5) 0.024(4) 0.018(4) 0.028(4) C(14) 0.079(6) 0.112(8) 0.076(6) -0.002(5) -0.003(5) 0.015(6) C(15) 0.063(4) 0.059(4) 0.093(6) 0.014(3) 0.046(4) 0.028(4) C(16) 0.13(1) 0.19(1) 0.19(2) 0.01(1) 0.09(1) 0.06(1) C(17) 0.082(5) 0.031(3) 0.094(6) 0.007(3) 0.042(5) 0.024(3) C(18) 0.093(6) 0.050(4) 0.086(6) -0.018(4) 0.048(5) -0.004(4) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2835 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0450 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.570 _refine_ls_shift/su_max 0.228 _refine_ls_shift/su_mean ? _refine_diff_density_min -0.98 _refine_diff_density_max 1.55 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Pd(1) 2.699(2) . . yes Pd(1) P(1) 2.301(2) . . yes Pd(1) Si(1) 2.396(2) . . yes Pd(1) Si(1) 2.332(2) . . yes Pd(1) H(26) 2.04(6) . . yes P(1) C(13) 1.811(8) . . no P(1) C(15) 1.832(7) . . no P(1) C(17) 1.838(7) . . no Si(1) C(1) 1.883(6) . . no Si(1) C(7) 1.883(6) . . no Si(1) H(26) 1.60(8) . . yes C(1) C(2) 1.380(8) . . no C(1) C(6) 1.401(7) . . no C(2) C(3) 1.381(9) . . no C(2) H(1) 0.97 . . no C(3) C(4) 1.38(1) . . no C(3) H(2) 0.97 . . no C(4) C(5) 1.36(1) . . no C(4) H(3) 0.97 . . no C(5) C(6) 1.380(9) . . no C(5) H(4) 0.97 . . no C(6) H(5) 0.97 . . no C(7) C(8) 1.403(8) . . no C(7) C(12) 1.376(9) . . no C(8) C(9) 1.383(9) . . no C(8) H(6) 0.98 . . no C(9) C(10) 1.35(1) . . no C(9) H(7) 0.97 . . no C(10) C(11) 1.37(1) . . no C(10) H(8) 0.97 . . no C(11) C(12) 1.383(10) . . no C(11) H(9) 0.98 . . no C(12) H(10) 0.97 . . no C(13) C(14) 1.50(1) . . no C(13) H(11) 0.97 . . no C(13) H(12) 0.96 . . no C(14) H(13) 0.95 . . no C(14) H(14) 0.96 . . no C(14) H(15) 0.96 . . no C(15) C(16) 1.44(2) . . no C(15) H(16) 0.97 . . no C(15) H(17) 0.96 . . no C(16) H(18) 0.96 . . no C(16) H(19) 0.95 . . no C(16) H(20) 0.97 . . no C(17) C(18) 1.50(1) . . no C(17) H(21) 0.95 . . no C(17) H(22) 0.97 . . no C(18) H(23) 0.96 . . no C(18) H(24) 0.96 . . no C(18) H(25) 0.95 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd(1) Pd(1) P(1) 159.51(5) . . . yes Pd(1) Pd(1) Si(1) 54.08(4) . . . yes Pd(1) Pd(1) Si(1) 56.32(6) . . . yes P(1) Pd(1) Si(1) 146.41(6) . . . no P(1) Pd(1) Si(1) 103.19(8) . . . no Si(1) Pd(1) Si(1) 110.40(5) . . . yes Pd(1) P(1) C(13) 115.3(3) . . . no Pd(1) P(1) C(15) 112.7(2) . . . no Pd(1) P(1) C(17) 118.9(3) . . . no C(13) P(1) C(15) 104.4(4) . . . no C(13) P(1) C(17) 101.6(4) . . . no C(15) P(1) C(17) 102.1(3) . . . no Pd(1) Si(1) Pd(1) 69.60(5) . . . yes Pd(1) Si(1) C(1) 121.5(2) . . . yes Pd(1) Si(1) C(7) 120.6(2) . . . yes Pd(1) Si(1) H(26) 57.(2) . . . yes Pd(1) Si(1) C(1) 115.7(2) . . . yes Pd(1) Si(1) C(7) 116.1(2) . . . yes Pd(1) Si(1) H(26) 126.(2) . . . yes C(1) Si(1) C(7) 108.5(2) . . . yes C(1) Si(1) H(26) 93.(2) . . . no C(7) Si(1) H(26) 91.(2) . . . no Si(1) C(1) C(2) 120.6(4) . . . no Si(1) C(1) C(6) 123.1(4) . . . no C(2) C(1) C(6) 116.2(5) . . . no C(1) C(2) C(3) 122.4(6) . . . no C(1) C(2) H(1) 118.1 . . . no C(3) C(2) H(1) 119.5 . . . no C(2) C(3) C(4) 119.8(7) . . . no C(2) C(3) H(2) 120.0 . . . no C(4) C(3) H(2) 120.2 . . . no C(3) C(4) C(5) 119.5(6) . . . no C(3) C(4) H(3) 120.4 . . . no C(5) C(4) H(3) 120.0 . . . no C(4) C(5) C(6) 120.4(6) . . . no C(4) (5) H(4) 119.9 . . . no C(6) C(5) H(4) 109.7 . . . no C(1) C(6) C(5) 121.7(6) . . . no C(1) C(6) H(5) 118.7 . . . no C(5) C(6) H(5) 119.6 . . . no Si(1) C(7) C(8) 122.1(5) . . . no Si(1) C(7) C(12) 121.2(5) . . . no C(8) C(7) C(12) 116.2(6) . . . no C(7) C(8) C(9) 121.0(7) . . . no C(7) C(8) H(6) 119.1 . . . no C(9) C(8) H(6) 119.9 . . . no C(8) C(9) C(10) 120.9(7) . . . no C(8) C(9) H(7) 119.5 . . . no C(10) C(9) H(7) 119.6 . . . no C(9) C(10) C(11) 119.5(7) . . . no C(9) C(10) H(8) 120.3 . . . no C(11) C(10) H(8) 120.2 . . . no C(10) C(11) C(12) 119.8(7) . . . no C(10) C(11) H(9) 120.2 . . . no C(12) C(11) H(9) 120.0 . . . no C(7) C(12) C(11) 122.5(7) . . . no C(7) C(12) H(10) 118.3 . . . no C(11) C(12) H(10) 119.2 . . . no P(1) C(13) C(14) 114.5(6) . . . no P(1) C(13) H(11) 109.2 . . . no P(1) C(13) H(12) 109.9 . . . no C(14) C(13) H(11) 107.4 . . . no C(14) C(13) H(12) 108.5 . . . no H(11) C(13) H(12) 107.0 . . . no C(13) C(14) H(13) 112.1 . . . no C(13) C(14) H(14) 109.3 . . . no C(13) C(14) H(15) 110.3 . . . no H(13) C(14) H(14) 108.4 . . . no H(13) C(14) H(15) 108.9 . . . no H(14) C(14) H(15) 107.6 . . . no P(1) C(15) C(16) 116.2(8) . . . no P(1) C(15) H(16) 108.6 . . . no P(1) C(15) H(17) 109.4 . . . no C(16) C(15) H(16) 107.1 . . . no C(16) C(15) H(17) 108.3 . . . no H(16) C(15) H(17) 106.8 . . . no C(15) C(16) H(18) 111.1 . . . no C(15) C(16) H(19) 112.9 . . . no C(15) C(16) H(20) 110.1 . . . no H(18) C(16) H(19) 108.0 . . . no H(18) C(16) H(20) 106.9 . . . no H(19) C(16) H(20) 107.6 . . . no P(1) C(17) C(18) 113.8(5) . . . no P(1) C(17) H(21) 110.0 . . . no P(1) C(17) H(22) 109.2 . . . no C(18) C(17) H(21) 108.2 . . . no C(18) C(17) H(22) 107.6 . . . no H(21) C(17) H(22) 107.9 . . . no C(17) C(18) H(23) 110. . . . no C(17) C(18) H(24) 110.0 . . . no C(17) C(18) H(25) 111.9 . . . no H(23) C(18) H(24) 107.7 . . . no H(23) C(18) H(25) 108.3 . . . no H(24) C(18) H(25) 108.6 . . . no data_form2 _cell_length_a 8.419(4) _cell_length_b 16.222(4) _cell_length_c 10.240(4) _cell_angle_alpha 90 _cell_angle_beta 108.58(3) _cell_angle_gamma 90 _cell_volume 1325.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 13.7 _cell_measurement_theta_max 16.7 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 607.46 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H36 P2 Pd2 Si2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 616.00 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.856 _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3319 _reflns_number_total 3152 _reflns_number_gt 2114 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03509 _diffrn_orient_matrix_UB_12 0.05090 _diffrn_orient_matrix_UB_13 0.05700 _diffrn_orient_matrix_UB_21 0.11974 _diffrn_orient_matrix_UB_22 -0.01779 _diffrn_orient_matrix_UB_23 0.02551 _diffrn_orient_matrix_UB_31 0.01151 _diffrn_orient_matrix_UB_32 0.02988 _diffrn_orient_matrix_UB_33 -0.08193 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 0 40 0.003 0.002 H 0 72 0.000 0.000 Si 0 4 0.082 0.070 P 0 4 0.102 0.094 Pd 0 4 -0.999 1.007 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.37082(5) 0.45386(3) 1.01078(4) 0.03500(9) 1.000 . Uani d ? P(1) 0.2108(2) 0.39039(10) 1.1259(1) 0.0430(4) 1.000 . Uani d ? Si(1) 0.5830(2) 0.50669(9) 1.1988(1) 0.0362(4) 1.000 . Uani d ? C(1) 0.0991(9) 0.4594(5) 1.2043(7) 0.074(2) 1.000 . Uani d ? C(2) 0.0448(10) 0.3232(5) 1.0223(8) 0.084(3) 1.000 . Uani d ? C(3) 0.3137(9) 0.3221(5) 1.2696(8) 0.084(3) 1.000 . Uani d ? C(4) 0.5226(9) 0.5776(4) 1.3213(6) 0.061(2) 1.000 . Uani d ? C(5) 0.7182(6) 0.4226(4) 1.3062(5) 0.042(1) 1.000 . Uani d ? C(6) 0.7286(8) 0.3469(4) 1.2463(7) 0.060(2) 1.000 . Uani d ? C(7) 0.827(1) 0.2839(5) 1.3193(10) 0.080(3) 1.000 . Uani d ? C(8) 0.921(1) 0.2950(7) 1.453(1) 0.103(4) 1.000 . Uani d ? C(9) 0.917(1) 0.3679(8) 1.5152(9) 0.105(3) 1.000 . Uani d ? C(10) 0.8152(8) 0.4328(5) 1.4433(6) 0.066(2) 1.000 . Uani d ? H(1) 0.0380 0.4978 1.1378 0.0870 1.000 . Uiso c ? H(2) 0.0237 0.4279 1.2368 0.0870 1.000 . Uiso c ? H(3) 0.1765 0.4870 1.2789 0.0870 1.000 . Uiso c ? H(4) -0.0209 0.3519 0.9426 0.0977 1.000 . Uiso c ? H(5) -0.0239 0.3062 1.0749 0.0977 1.000 . Uiso c ? H(6) 0.0935 0.2759 0.9949 0.0977 1.000 . Uiso c ? H(7) 0.2363 0.3056 1.3147 0.0995 1.000 . Uiso c ? H(8) 0.3542 0.2743 1.2358 0.0995 1.000 . Uiso c ? H(9) 0.4055 0.3498 1.3332 0.0995 1.000 . Uiso c ? H(10) 0.4550 0.6212 1.2710 0.0736 1.000 . Uiso c ? H(11) 0.4606 0.5472 1.3685 0.0736 1.000 . Uiso c ? H(12) 0.6204 0.5995 1.3862 0.0736 1.000 . Uiso c ? H(13) 0.6662 0.3385 1.1513 0.0704 1.000 . Uiso c ? H(14) 0.8268 0.2323 1.2755 0.0924 1.000 . Uiso c ? H(15) 0.9879 0.2512 1.5015 0.1229 1.000 . Uiso c ? H(16) 0.9828 0.3751 1.6089 0.1236 1.000 . Uiso c ? H(17) 0.8136 0.4839 1.4877 0.0805 1.000 . Uiso c ? H(18) 0.2718 0.4366 0.8237 0.0648 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0349(2) 0.0410(2) 0.0300(2) -0.0033(2) 0.0115(1) 0.0022(2) P(1) 0.0409(7) 0.0513(8) 0.0399(7) -0.0040(6) 0.0171(6) 0.0053(6) Si(1) 0.0397(7) 0.0422(8) 0.0273(6) -0.0032(6) 0.0116(6) -0.0012(6) C(1) 0.068(4) 0.086(5) 0.081(5) 0.001(4) 0.046(4) 0.000(4) C(2) 0.083(5) 0.097(6) 0.078(5) -0.046(5) 0.034(4) -0.017(4) C(3) 0.072(5) 0.097(6) 0.086(5) 0.009(4) 0.031(4) 0.050(5) C(4) 0.076(4) 0.063(4) 0.051(3) 0.000(3) 0.029(3) -0.012(3) C(5) 0.038(3) 0.049(3) 0.039(3) -0.009(2) 0.012(2) 0.005(2) C(6) 0.058(4) 0.047(4) 0.072(4) 0.001(3) 0.016(3) 0.002(3) C(7) 0.074(5) 0.052(4) 0.118(7) 0.011(4) 0.037(5) 0.016(4) C(8) 0.081(6) 0.102(7) 0.126(9) 0.033(6) 0.034(6) 0.070(7) C(9) 0.089(6) 0.150(10) 0.061(5) 0.023(7) 0.002(4) 0.052(6) C(10) 0.066(4) 0.088(5) 0.037(3) 0.002(4) 0.008(3) 0.012(3) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2114 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0360 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_shift/su_max 0.0280 _refine_ls_shift/su_mean ? _refine_diff_density_min -0.6323 _refine_diff_density_max 0.6165 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Pd(1) 2.707(1) . . yes Pd(1) P(1) 2.297(2) . . yes Pd(1) Si(1) 2.333(2) . . yes Pd(1) Si(1) 2.387(1) . . yes Pd(1) H(19) 1.85 . . yes P(1) C(1) 1.806(7) . . no P(1) C(2) 1.822(7) . . no P(1) C(3) 1.825(7) . . no Si(1) C(4) 1.888(6) . . no Si(1) C(5) 1.888(6) . . no Si(1) H(18) 1.60 . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.94 . . no C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(2) H(6) 0.95 . . no C(3) H(7) 0.95 . . no C(3) H(8) 0.95 . . no C(3) H(9) 0.95 . . no C(4) H(10) 0.95 . . no C(4) H(11) 0.95 . . no C(4) H(12) 0.95 . . no C(5) C(6) 1.388(8) . . no C(5) C(10) 1.391(7) . . no C(6) C(7) 1.375(10) . . no C(6) H(13) 0.96 . . no C(7) C(8) 1.36(1) . . no C(7) H(14) 0.95 . . no C(8) C(9) 1.35(1) . . no C(8) H(15) 0.94 . . no C(9) C(10) 1.41(1) . . no C(9) H(16) 0.95 . . no C(10) H(17) 0.95 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd(1) Pd(1) P(1) 155.18(4) . . . yes Pd(1) Pd(1) Si(1) 55.95(4) . . . yes Pd(1) Pd(1) Si(1) 54.07(4) . . . yes Pd(1) Pd(1) H(19) 96.2 . . . no P(1) Pd(1) Si(1) 99.28(6) . . . no P(1) Pd(1) Si(1) 150.65(5) . . . no P(1) Pd(1) H(18) 108.6 . . . no Si(1) Pd(1) Si(1) 110.02(4) . . . yes Si(1) Pd(1) H(18) 152.1 . . . no Si(1) Pd(1) H(18) 42.2 . . . no Pd(1) P(1) C(1) 115.1(2) . . . no Pd(1) P(1) C(2) 115.8(2) . . . no Pd(1) P(1) C(3) 118.7(2) . . . no C(1) P(1) C(2) 102.6(4) . . . no C(1) P(1) C(3) 101.5(4) . . . no C(2) P(1) C(3) 100.7(4) . . . no Pd(1) Si(1) Pd(1) 69.98(4) . . . yes Pd(1) Si(1) C(4) 118.3(2) . . . yes Pd(1) Si(1) C(5) 112.1(2) . . . yes Pd(1) Si(1) H(18) 120.7 . . . yes Pd(1) Si(1) C(4) 126.2(2) . . . yes Pd(1) Si(1) C(5) 118.5(2) . . . yes Pd(1) Si(1) H(18) 50.7 . . . yes C(4) Si(1) C(5) 107.0(3) . . . yes C(4) Si(1) H(18) 97.2 . . . no C(5) Si(1) H(18) 98.8 . . . no P(1) C(1) H(1) 109.2 . . . no P(1) C(1) H(2) 108.8 . . . no P(1) C(1) H(3) 109.3 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 110.3 . . . no H(2) C(1) H(3) 109.7 . . . no P(1) C(2) H(4) 109.6 . . . no P(1) C(2) H(5) 109.7 . . . no P(1) C(2) H(6) 109.3 . . . no H(4) C(2) H(5) 109.7 . . . no H(4) C(2) H(6) 109.2 . . . no H(5) C(2) H(6) 109.3 . . . no P(1) C(3) H(7) 109.9 . . . no P(1) C(3) H(8) 109.5 . . . no P(1) C(3) H(9) 109.8 . . . no H(7) C(3) H(8) 109.1 . . . no H(7) C(3) H(9) 109.5 . . . no H(8) C(3) H(9) 109.0 . . . no Si(1) C(4) H(10) 109.5 . . . no Si(1) C(4) H(11) 109.2 . . . no Si(1) C(4) H(12) 109.6 . . . no H(10) C(4) H(11) 109.2 . . . no H(10) C(4) H(12) 109.8 . . . no H(11) C(4) H(12) 109.5 . . . no Si(1) C(5) C(6) 119.5(4) . . . no Si(1) C(5) C(10) 123.6(5) . . . no C(6) C(5) C(10) 116.8(6) . . . no C(5) C(6) C(7) 121.9(7) . . . no C(5) C(6) H(13) 118.9 . . . no C(7) C(6) H(13) 119.2 . . . no C(6) C(7) C(8) 120.4(8) . . . no C(6) C(7) H(14) 119.3 . . . no C(8) C(7) H(14) 120.3 . . . no C(7) C(8) C(9) 119.9(8) . . . no C(7) C(8) H(15) 119.3 . . . no C(9) C(8) H(15) 120.8 . . . no C(8) C(9) C(10) 120.7(8) . . . no C(8) C(9) H(16) 119.3 . . . no C(10) C(9) H(16) 120.0 . . . no C(5) C(10) C(9) 120.2(7) . . . no C(5) C(10) H(17) 119.6 . . . no C(9) C(10) H(17) 120.2 . . . no #===End of CIF