Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mitsuo Kira' 'Takeaki Iwamoto' 'Chizuko Kabuto' 'Yumiko Sekiguchi' 'Naoki Yoshida' _publ_contact_author_name 'Prof Mitsuo Kira ' _publ_contact_author_address ; Department of Chemistry Tohoku University Graduate School of Science Aoba-ku Sendai 980-8578 JAPAN ; _publ_contact_author_email 'MKIRA@SI.CHEM.TOHOKU.AC.JP ' _publ_section_title ; Ligand dependence of pai-complex character in disilene-palladium complexes ; _publ_contact_author_fax +81-22-795-6589 _publ_contact_author_phone +81-22-795-6585 data_(Cy3P)(XyNC)Pd(disilene)_complex_8 _database_code_depnum_ccdc_archive 'CCDC 282912' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H102 N P Pd Si6' _chemical_formula_weight 1035.25 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' N N 0.0061 0.0033 '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 monoclinic _symmetry_space_group_name_H-M P21/c 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 25.4468(8) _cell_length_b 20.6003(5) _cell_length_c 23.6113(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.2453(4) _cell_angle_gamma 90.00 _cell_volume 11755.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173.1500 _cell_measurement_reflns_used 28291 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 29.5736 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method dtintegrate.ref _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122930 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 26666 _reflns_number_gt 25474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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. Positional disorder was found in t-BuMe2Si group (disorder 1) on Si2 and a Me group on C60 (disorder 2). In disorder 1, all atoms in minor part were refined isotropically. In disorder 2, all heavy atoms were aniotropically refined. ; _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^)+(0.0272P)^2^+22.4926P] 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 26666 _refine_ls_number_parameters 1191 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.235 _refine_ls_shift/su_max 0.003 _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 0.141798(9) -0.723697(11) 0.395809(10) 0.02042(6) Uani 1 1 d . A . P1 P 0.21257(3) -0.66470(4) 0.36663(4) 0.02365(16) Uani 1 1 d . . . Si1 Si 0.09203(3) -0.80916(4) 0.43096(4) 0.02127(17) Uani 1 1 d . A . Si2 Si 0.10209(3) -0.82145(4) 0.33868(4) 0.02103(17) Uani 1 1 d . . . Si3 Si 0.16846(4) -0.83776(4) 0.51581(4) 0.02562(18) Uani 1 1 d . . . Si4 Si 0.01012(4) -0.78067(4) 0.45247(4) 0.02448(17) Uani 1 1 d U . . Si5 Si 0.14088(4) -0.91682(4) 0.31160(4) 0.02499(18) Uani 1 1 d . A . Si6 Si 0.04245(4) -0.76366(5) 0.25628(4) 0.0205(3) Uani 0.862(3) 1 d P A 1 N1 N 0.11062(12) -0.60816(13) 0.46584(13) 0.0305(6) Uani 1 1 d . A . C1 C 0.18948(16) -0.76033(17) 0.56027(16) 0.0374(8) Uani 1 1 d . A . H1 H 0.2231 -0.7681 0.5938 0.056 Uiso 1 1 calc R . . H2 H 0.1596 -0.7464 0.5755 0.056 Uiso 1 1 calc R . . H3 H 0.1966 -0.7264 0.5346 0.056 Uiso 1 1 calc R . . C2 C 0.22816(14) -0.86467(19) 0.49076(16) 0.0364(8) Uani 1 1 d . A . H4 H 0.2276 -0.8408 0.4547 0.055 Uiso 1 1 calc R . . H5 H 0.2250 -0.9113 0.4822 0.055 Uiso 1 1 calc R . . H6 H 0.2630 -0.8559 0.5224 0.055 Uiso 1 1 calc R . . C3 C 0.16204(15) -0.90151(17) 0.57268(15) 0.0322(7) Uani 1 1 d . A . C4 C 0.12421(19) -0.8781(2) 0.60742(18) 0.0520(11) Uani 1 1 d . . . H7 H 0.0877 -0.8676 0.5795 0.078 Uiso 1 1 calc R A . H8 H 0.1402 -0.8393 0.6304 0.078 Uiso 1 1 calc R . . H9 H 0.1204 -0.9124 0.6346 0.078 Uiso 1 1 calc R . . C5 C 0.21967(17) -0.9108(2) 0.61808(17) 0.0489(10) Uani 1 1 d . . . H10 H 0.2173 -0.9414 0.6490 0.073 Uiso 1 1 calc R A . H11 H 0.2336 -0.8690 0.6364 0.073 Uiso 1 1 calc R . . H12 H 0.2449 -0.9281 0.5978 0.073 Uiso 1 1 calc R . . C6 C 0.14318(18) -0.96706(19) 0.54399(18) 0.0465(10) Uani 1 1 d . . . H13 H 0.1423 -0.9985 0.5748 0.070 Uiso 1 1 calc R A . H14 H 0.1690 -0.9821 0.5235 0.070 Uiso 1 1 calc R . . H15 H 0.1061 -0.9629 0.5151 0.070 Uiso 1 1 calc R . . C7 C -0.03185(15) -0.72030(17) 0.39773(16) 0.0360(8) Uani 1 1 d . A . H16 H -0.0647 -0.7084 0.4087 0.054 Uiso 1 1 calc R . . H17 H -0.0433 -0.7394 0.3577 0.054 Uiso 1 1 calc R . . H18 H -0.0095 -0.6814 0.3981 0.054 Uiso 1 1 calc R . . C8 C 0.02770(16) -0.73744(19) 0.52640(16) 0.0403(9) Uani 1 1 d . A . H19 H 0.0476 -0.6972 0.5245 0.060 Uiso 1 1 calc R . . H20 H 0.0511 -0.7655 0.5578 0.060 Uiso 1 1 calc R . . H21 H -0.0064 -0.7272 0.5354 0.060 Uiso 1 1 calc R . . C9 C -0.03805(14) -0.85294(17) 0.45159(16) 0.0344(7) Uani 1 1 d U A . C10 C -0.0927(2) -0.8280(3) 0.4567(3) 0.0818(17) Uani 1 1 d U . . H22 H -0.1172 -0.8648 0.4564 0.082 Uiso 1 1 calc R A . H23 H -0.1102 -0.7993 0.4230 0.082 Uiso 1 1 calc R . . H24 H -0.0859 -0.8039 0.4941 0.082 Uiso 1 1 calc R . . C11 C -0.0506(3) -0.8888(3) 0.3939(3) 0.106(2) Uani 1 1 d U . . H25 H -0.0178 -0.9131 0.3929 0.106 Uiso 1 1 calc R A . H26 H -0.0610 -0.8579 0.3607 0.106 Uiso 1 1 calc R . . H27 H -0.0813 -0.9190 0.3901 0.106 Uiso 1 1 calc R . . C12 C -0.0148(2) -0.8982(3) 0.5024(3) 0.112(3) Uani 1 1 d U . . H28 H -0.0430 -0.9300 0.5036 0.112 Uiso 1 1 calc R A . H29 H -0.0033 -0.8736 0.5398 0.112 Uiso 1 1 calc R . . H30 H 0.0173 -0.9208 0.4972 0.112 Uiso 1 1 calc R . . C13 C 0.13504(15) -0.91374(18) 0.23030(15) 0.0365(8) Uani 1 1 d . . . H31 H 0.1523 -0.8738 0.2221 0.055 Uiso 1 1 calc R A . H32 H 0.0959 -0.9144 0.2062 0.055 Uiso 1 1 calc R . . H33 H 0.1539 -0.9514 0.2202 0.055 Uiso 1 1 calc R . . C14 C 0.21725(14) -0.92799(17) 0.35015(16) 0.0356(8) Uani 1 1 d . . . H34 H 0.2323 -0.9582 0.3271 0.053 Uiso 1 1 calc R A . H35 H 0.2231 -0.9455 0.3902 0.053 Uiso 1 1 calc R . . H36 H 0.2360 -0.8860 0.3531 0.053 Uiso 1 1 calc R . . C15 C 0.10418(15) -0.99460(17) 0.32367(16) 0.0345(8) Uani 1 1 d . . . C16 C 0.04157(16) -0.9897(2) 0.2958(2) 0.0488(10) Uani 1 1 d . A . H37 H 0.0243 -1.0301 0.3029 0.073 Uiso 1 1 calc R . . H38 H 0.0325 -0.9825 0.2527 0.073 Uiso 1 1 calc R . . H39 H 0.0277 -0.9533 0.3137 0.073 Uiso 1 1 calc R . . C17 C 0.1173(2) -1.0072(2) 0.39035(19) 0.0530(11) Uani 1 1 d . A . H40 H 0.1054 -0.9699 0.4091 0.080 Uiso 1 1 calc R . . H41 H 0.1573 -1.0135 0.4084 0.080 Uiso 1 1 calc R . . H42 H 0.0977 -1.0462 0.3964 0.080 Uiso 1 1 calc R . . C18 C 0.12500(19) -1.05247(18) 0.2957(2) 0.0505(10) Uani 1 1 d . A . H43 H 0.1090 -1.0927 0.3052 0.076 Uiso 1 1 calc R . . H44 H 0.1654 -1.0547 0.3116 0.076 Uiso 1 1 calc R . . H45 H 0.1138 -1.0469 0.2523 0.076 Uiso 1 1 calc R . . C19 C 0.0200(2) -0.6842(2) 0.28126(19) 0.0283(9) Uani 0.862(3) 1 d P A 1 H46 H 0.0478 -0.6698 0.3182 0.043 Uiso 0.862(3) 1 calc PR A 1 H47 H -0.0157 -0.6900 0.2884 0.043 Uiso 0.862(3) 1 calc PR A 1 H48 H 0.0161 -0.6513 0.2502 0.043 Uiso 0.862(3) 1 calc PR A 1 C20 C 0.08625(17) -0.7413(2) 0.20814(18) 0.0326(9) Uani 0.862(3) 1 d P A 1 H49 H 0.0653 -0.7124 0.1761 0.049 Uiso 0.862(3) 1 calc PR A 1 H50 H 0.0964 -0.7808 0.1908 0.049 Uiso 0.862(3) 1 calc PR A 1 H51 H 0.1199 -0.7193 0.2324 0.049 Uiso 0.862(3) 1 calc PR A 1 C21 C -0.02418(15) -0.80160(18) 0.20370(16) 0.0266(8) Uani 0.862(3) 1 d P A 1 C22 C -0.05785(19) -0.7481(2) 0.1626(2) 0.0437(11) Uani 0.862(3) 1 d P A 1 H52 H -0.0353 -0.7282 0.1404 0.066 Uiso 0.862(3) 1 calc PR A 1 H53 H -0.0685 -0.7150 0.1868 0.066 Uiso 0.862(3) 1 calc PR A 1 H54 H -0.0912 -0.7672 0.1346 0.066 Uiso 0.862(3) 1 calc PR A 1 C23 C -0.0120(2) -0.8549(2) 0.1648(2) 0.0378(11) Uani 0.862(3) 1 d P A 1 H55 H 0.0087 -0.8899 0.1902 0.057 Uiso 0.862(3) 1 calc PR A 1 H56 H 0.0100 -0.8370 0.1411 0.057 Uiso 0.862(3) 1 calc PR A 1 H57 H -0.0469 -0.8721 0.1381 0.057 Uiso 0.862(3) 1 calc PR A 1 C24 C -0.05913(18) -0.8308(2) 0.2388(2) 0.0357(10) Uani 0.862(3) 1 d P A 1 H58 H -0.0927 -0.8499 0.2112 0.054 Uiso 0.862(3) 1 calc PR A 1 H59 H -0.0693 -0.7969 0.2625 0.054 Uiso 0.862(3) 1 calc PR A 1 H60 H -0.0379 -0.8647 0.2655 0.054 Uiso 0.862(3) 1 calc PR A 1 C25 C 0.24415(13) -0.69544(19) 0.31039(15) 0.0340(8) Uani 1 1 d . . . H61 H 0.2216 -0.6757 0.2717 0.041 Uiso 1 1 calc R . . C26 C 0.23764(16) -0.76677(19) 0.30092(19) 0.0427(9) Uani 1 1 d . . . H62 H 0.1990 -0.7791 0.2969 0.051 Uiso 1 1 calc R . . H63 H 0.2623 -0.7894 0.3363 0.051 Uiso 1 1 calc R . . C27 C 0.25157(17) -0.7893(2) 0.2446(2) 0.0456(10) Uani 1 1 d . . . H64 H 0.2488 -0.8371 0.2410 0.055 Uiso 1 1 calc R . . H65 H 0.2250 -0.7701 0.2085 0.055 Uiso 1 1 calc R . . C28 C 0.31105(18) -0.7672(2) 0.2499(2) 0.0545(12) Uani 1 1 d . . . H66 H 0.3376 -0.7928 0.2817 0.065 Uiso 1 1 calc R . . H67 H 0.3183 -0.7767 0.2119 0.065 Uiso 1 1 calc R . . C29 C 0.32079(16) -0.6968(2) 0.26372(18) 0.0464(10) Uani 1 1 d . . . H68 H 0.2995 -0.6711 0.2286 0.056 Uiso 1 1 calc R . . H69 H 0.3605 -0.6871 0.2715 0.056 Uiso 1 1 calc R . . C30 C 0.30413(13) -0.67658(18) 0.31711(16) 0.0336(8) Uani 1 1 d . . . H70 H 0.3083 -0.6290 0.3223 0.040 Uiso 1 1 calc R . . H71 H 0.3291 -0.6974 0.3533 0.040 Uiso 1 1 calc R . . C31 C 0.27282(13) -0.64889(15) 0.43414(14) 0.0267(7) Uani 1 1 d . . . H72 H 0.3024 -0.6278 0.4209 0.032 Uiso 1 1 calc R . . C32 C 0.29606(14) -0.71283(16) 0.46517(15) 0.0314(7) Uani 1 1 d . . . H73 H 0.2669 -0.7355 0.4771 0.038 Uiso 1 1 calc R . . H74 H 0.3070 -0.7411 0.4369 0.038 Uiso 1 1 calc R . . C33 C 0.34614(16) -0.7013(2) 0.52026(17) 0.0461(10) Uani 1 1 d . . . H75 H 0.3587 -0.7433 0.5403 0.055 Uiso 1 1 calc R . . H76 H 0.3768 -0.6832 0.5077 0.055 Uiso 1 1 calc R . . C34 C 0.33297(17) -0.6551(2) 0.56408(17) 0.0477(10) Uani 1 1 d . . . H77 H 0.3057 -0.6755 0.5806 0.057 Uiso 1 1 calc R . . H78 H 0.3671 -0.6463 0.5975 0.057 Uiso 1 1 calc R . . C35 C 0.30978(16) -0.5920(2) 0.53398(17) 0.0421(9) Uani 1 1 d . . . H79 H 0.3387 -0.5691 0.5217 0.051 Uiso 1 1 calc R . . H80 H 0.2991 -0.5640 0.5626 0.051 Uiso 1 1 calc R . . C36 C 0.25935(15) -0.60374(18) 0.47922(15) 0.0351(8) Uani 1 1 d . . . H81 H 0.2459 -0.5617 0.4598 0.042 Uiso 1 1 calc R . . H82 H 0.2293 -0.6231 0.4920 0.042 Uiso 1 1 calc R . . C37 C 0.18990(14) -0.58041(16) 0.33920(16) 0.0330(7) Uani 1 1 d . . . H83 H 0.1769 -0.5598 0.3708 0.040 Uiso 1 1 calc R . . C38 C 0.23438(14) -0.53509(17) 0.33049(17) 0.0345(8) Uani 1 1 d . . . H84 H 0.2490 -0.5533 0.2996 0.041 Uiso 1 1 calc R . . H85 H 0.2654 -0.5320 0.3682 0.041 Uiso 1 1 calc R . . C39 C 0.21062(17) -0.46655(19) 0.31126(19) 0.0462(10) Uani 1 1 d . . . H86 H 0.1993 -0.4467 0.3438 0.055 Uiso 1 1 calc R . . H87 H 0.2397 -0.4389 0.3042 0.055 Uiso 1 1 calc R . . C40 C 0.16200(15) -0.46897(19) 0.25593(18) 0.0421(9) Uani 1 1 d . . . H88 H 0.1741 -0.4844 0.2223 0.051 Uiso 1 1 calc R . . H89 H 0.1465 -0.4248 0.2462 0.051 Uiso 1 1 calc R . . C41 C 0.11743(14) -0.51411(18) 0.26392(19) 0.0420(9) Uani 1 1 d . . . H90 H 0.1020 -0.4955 0.2940 0.050 Uiso 1 1 calc R . . H91 H 0.0870 -0.5175 0.2257 0.050 Uiso 1 1 calc R . . C42 C 0.14029(15) -0.58150(18) 0.28375(19) 0.0443(10) Uani 1 1 d . . . H92 H 0.1109 -0.6082 0.2914 0.053 Uiso 1 1 calc R . . H93 H 0.1508 -0.6023 0.2511 0.053 Uiso 1 1 calc R . . C43 C 0.12515(13) -0.65254(16) 0.44450(14) 0.0271(7) Uani 1 1 d . . . C44 C 0.09611(15) -0.55160(16) 0.49032(17) 0.0341(8) Uani 1 1 d . . . C45 C 0.12192(17) -0.53974(18) 0.55101(18) 0.0405(9) Uani 1 1 d . A . C46 C 0.1070(2) -0.4825(2) 0.5735(2) 0.0542(12) Uani 1 1 d . . . H94 H 0.1231 -0.4724 0.6146 0.065 Uiso 1 1 calc R A . C47 C 0.0695(2) -0.4404(2) 0.5374(2) 0.0584(13) Uani 1 1 d . A . H95 H 0.0603 -0.4016 0.5539 0.070 Uiso 1 1 calc R . . C48 C 0.04491(19) -0.45323(19) 0.4779(2) 0.0519(11) Uani 1 1 d . . . H96 H 0.0192 -0.4232 0.4537 0.062 Uiso 1 1 calc R A . C49 C 0.05754(17) -0.51014(17) 0.45254(18) 0.0398(9) Uani 1 1 d . A . C50 C 0.16367(19) -0.5859(2) 0.58874(18) 0.0514(11) Uani 1 1 d . . . H97 H 0.1787 -0.5684 0.6292 0.077 Uiso 1 1 calc R A . H98 H 0.1937 -0.5918 0.5715 0.077 Uiso 1 1 calc R . . H99 H 0.1460 -0.6278 0.5902 0.077 Uiso 1 1 calc R . . C51 C 0.03063(19) -0.5258(2) 0.38796(19) 0.0503(10) Uani 1 1 d . . . H100 H 0.0017 -0.4938 0.3702 0.076 Uiso 1 1 calc R A . H101 H 0.0141 -0.5692 0.3843 0.076 Uiso 1 1 calc R . . H102 H 0.0584 -0.5247 0.3672 0.076 Uiso 1 1 calc R . . Pd2 Pd 0.366780(9) -0.277390(10) 0.616953(9) 0.01788(6) Uani 1 1 d . . . P2 P 0.29433(3) -0.33074(4) 0.64701(3) 0.02035(15) Uani 1 1 d . . . Si7 Si 0.41169(3) -0.18881(4) 0.57945(3) 0.01944(16) Uani 1 1 d . . . Si8 Si 0.40086(3) -0.17848(4) 0.67201(3) 0.01919(16) Uani 1 1 d . . . Si9 Si 0.33394(4) -0.16511(4) 0.49394(4) 0.02356(17) Uani 1 1 d . . . Si10 Si 0.49232(3) -0.21449(4) 0.55367(4) 0.02299(17) Uani 1 1 d U G . Si11 Si 0.48178(4) -0.19976(4) 0.75600(4) 0.02583(18) Uani 1 1 d . . . Si12 Si 0.35532(4) -0.08626(4) 0.69482(4) 0.02355(17) Uani 1 1 d . . . N2 N 0.40038(11) -0.39172(12) 0.54650(11) 0.0236(5) Uani 1 1 d . . . C52 C 0.27340(14) -0.14131(17) 0.51890(16) 0.0338(7) Uani 1 1 d . . . H103 H 0.2389 -0.1507 0.4871 0.051 Uiso 1 1 calc R . . H104 H 0.2753 -0.0948 0.5280 0.051 Uiso 1 1 calc R . . H105 H 0.2744 -0.1660 0.5547 0.051 Uiso 1 1 calc R . . C53 C 0.31533(15) -0.24379(16) 0.45151(15) 0.0331(7) Uani 1 1 d . . . H106 H 0.3105 -0.2779 0.4784 0.050 Uiso 1 1 calc R . . H107 H 0.3450 -0.2562 0.4354 0.050 Uiso 1 1 calc R . . H108 H 0.2808 -0.2382 0.4187 0.050 Uiso 1 1 calc R . . C54 C 0.33661(14) -0.10117(17) 0.43500(14) 0.0311(7) Uani 1 1 d . . . C55 C 0.35218(18) -0.03369(18) 0.46100(17) 0.0443(9) Uani 1 1 d . . . H109 H 0.3897 -0.0346 0.4893 0.066 Uiso 1 1 calc R . . H110 H 0.3261 -0.0200 0.4817 0.066 Uiso 1 1 calc R . . H111 H 0.3507 -0.0031 0.4288 0.066 Uiso 1 1 calc R . . C56 C 0.3751(2) -0.1223(2) 0.3997(2) 0.0576(13) Uani 1 1 d . . . H112 H 0.3720 -0.0915 0.3673 0.086 Uiso 1 1 calc R . . H113 H 0.3645 -0.1657 0.3831 0.086 Uiso 1 1 calc R . . H114 H 0.4134 -0.1232 0.4263 0.086 Uiso 1 1 calc R . . C57 C 0.27805(17) -0.09694(19) 0.38995(18) 0.0474(10) Uani 1 1 d . . . H115 H 0.2523 -0.0808 0.4101 0.071 Uiso 1 1 calc R . . H116 H 0.2663 -0.1401 0.3734 0.071 Uiso 1 1 calc R . . H117 H 0.2783 -0.0672 0.3577 0.071 Uiso 1 1 calc R . . C58 C 0.53679(14) -0.27721(17) 0.60406(15) 0.0330(7) Uani 1 1 d . . . H118 H 0.5143 -0.3154 0.6057 0.049 Uiso 1 1 calc R . . H119 H 0.5525 -0.2591 0.6442 0.049 Uiso 1 1 calc R . . H120 H 0.5668 -0.2899 0.5886 0.049 Uiso 1 1 calc R . . C59 C 0.47109(15) -0.25724(18) 0.47912(15) 0.0350(8) Uani 1 1 d . . . H121 H 0.5041 -0.2676 0.4679 0.052 Uiso 1 1 calc R . . H122 H 0.4467 -0.2289 0.4488 0.052 Uiso 1 1 calc R . . H123 H 0.4514 -0.2974 0.4820 0.052 Uiso 1 1 calc R . . C60 C 0.53835(14) -0.14040(17) 0.55109(16) 0.0320(7) Uani 1 1 d U . . C61 C 0.48300(18) -0.1546(2) 0.82577(16) 0.0468(10) Uani 1 1 d . . . H124 H 0.5188 -0.1613 0.8564 0.070 Uiso 1 1 calc R B 1 H125 H 0.4534 -0.1710 0.8403 0.070 Uiso 1 1 calc R B 1 H126 H 0.4774 -0.1082 0.8169 0.070 Uiso 1 1 calc R B 1 C62 C 0.54679(14) -0.17041(18) 0.74288(19) 0.0414(9) Uani 1 1 d . . . H127 H 0.5436 -0.1239 0.7338 0.062 Uiso 1 1 calc R C 1 H128 H 0.5524 -0.1941 0.7092 0.062 Uiso 1 1 calc R C 1 H129 H 0.5784 -0.1779 0.7787 0.062 Uiso 1 1 calc R C 1 C63 C 0.49122(13) -0.28905(16) 0.77912(14) 0.0270(7) Uani 1 1 d . . . C64 C 0.54287(16) -0.2965(2) 0.83435(16) 0.0431(9) Uani 1 1 d . . . H130 H 0.5477 -0.3423 0.8461 0.065 Uiso 1 1 calc R D 1 H131 H 0.5381 -0.2707 0.8673 0.065 Uiso 1 1 calc R D 1 H132 H 0.5756 -0.2812 0.8248 0.065 Uiso 1 1 calc R D 1 C65 C 0.49846(14) -0.33101(16) 0.72903(14) 0.0298(7) Uani 1 1 d . . . H133 H 0.4988 -0.3769 0.7401 0.045 Uiso 1 1 calc R E 1 H134 H 0.5335 -0.3200 0.7223 0.045 Uiso 1 1 calc R E 1 H135 H 0.4677 -0.3231 0.6925 0.045 Uiso 1 1 calc R E 1 C66 C 0.44044(15) -0.31291(19) 0.79476(17) 0.0390(8) Uani 1 1 d . . . H136 H 0.4078 -0.3111 0.7592 0.059 Uiso 1 1 calc R F 1 H137 H 0.4345 -0.2852 0.8259 0.059 Uiso 1 1 calc R F 1 H138 H 0.4465 -0.3578 0.8092 0.059 Uiso 1 1 calc R F 1 C67 C 0.27824(13) -0.08317(17) 0.65717(16) 0.0328(7) Uani 1 1 d . . . H139 H 0.2629 -0.1270 0.6550 0.049 Uiso 1 1 calc R . . H140 H 0.2705 -0.0657 0.6168 0.049 Uiso 1 1 calc R . . H141 H 0.2613 -0.0552 0.6801 0.049 Uiso 1 1 calc R . . C68 C 0.36167(15) -0.08272(18) 0.77662(15) 0.0348(8) Uani 1 1 d . . . H142 H 0.3319 -0.0557 0.7820 0.052 Uiso 1 1 calc R . . H143 H 0.3975 -0.0639 0.7990 0.052 Uiso 1 1 calc R . . H144 H 0.3589 -0.1267 0.7913 0.052 Uiso 1 1 calc R . . C69 C 0.38798(14) -0.00754(15) 0.67814(15) 0.0293(7) Uani 1 1 d . . . C70 C 0.36833(17) 0.05033(17) 0.70729(18) 0.0422(9) Uani 1 1 d . . . H145 H 0.3809 0.0909 0.6940 0.063 Uiso 1 1 calc R . . H146 H 0.3837 0.0469 0.7508 0.063 Uiso 1 1 calc R . . H147 H 0.3278 0.0502 0.6957 0.063 Uiso 1 1 calc R . . C71 C 0.45103(14) -0.01169(17) 0.70262(17) 0.0366(8) Uani 1 1 d . . . H148 H 0.4639 -0.0486 0.6843 0.055 Uiso 1 1 calc R . . H149 H 0.4624 -0.0177 0.7460 0.055 Uiso 1 1 calc R . . H150 H 0.4672 0.0285 0.6933 0.055 Uiso 1 1 calc R . . C72 C 0.37143(17) 0.00318(18) 0.61078(16) 0.0406(9) Uani 1 1 d . . . H151 H 0.3896 0.0424 0.6025 0.061 Uiso 1 1 calc R . . H152 H 0.3312 0.0084 0.5947 0.061 Uiso 1 1 calc R . . H153 H 0.3829 -0.0343 0.5920 0.061 Uiso 1 1 calc R . . C73 C 0.25620(12) -0.28092(17) 0.68826(14) 0.0274(7) Uani 1 1 d . . . H154 H 0.2440 -0.2408 0.6639 0.033 Uiso 1 1 calc R . . C74 C 0.20313(14) -0.31100(19) 0.69528(16) 0.0359(8) Uani 1 1 d . . . H155 H 0.1781 -0.3241 0.6557 0.043 Uiso 1 1 calc R . . H156 H 0.2127 -0.3503 0.7206 0.043 Uiso 1 1 calc R . . C75 C 0.17367(15) -0.2622(2) 0.72375(17) 0.0450(10) Uani 1 1 d . . . H157 H 0.1615 -0.2245 0.6967 0.054 Uiso 1 1 calc R . . H158 H 0.1403 -0.2827 0.7289 0.054 Uiso 1 1 calc R . . C76 C 0.21050(15) -0.2388(2) 0.78335(16) 0.0390(8) Uani 1 1 d . . . H159 H 0.2193 -0.2755 0.8119 0.047 Uiso 1 1 calc R . . H160 H 0.1908 -0.2053 0.7991 0.047 Uiso 1 1 calc R . . C77 C 0.26352(15) -0.21051(18) 0.77796(16) 0.0350(8) Uani 1 1 d . . . H161 H 0.2882 -0.1989 0.8182 0.042 Uiso 1 1 calc R . . H162 H 0.2549 -0.1702 0.7540 0.042 Uiso 1 1 calc R . . C78 C 0.29378(13) -0.25765(17) 0.74874(14) 0.0302(7) Uani 1 1 d . . . H163 H 0.3266 -0.2358 0.7435 0.036 Uiso 1 1 calc R . . H164 H 0.3068 -0.2955 0.7752 0.036 Uiso 1 1 calc R . . C79 C 0.23693(12) -0.35550(15) 0.57944(13) 0.0233(6) Uani 1 1 d . . . H165 H 0.2082 -0.3782 0.5929 0.028 Uiso 1 1 calc R . . C80 C 0.21010(14) -0.29536(16) 0.54328(14) 0.0312(7) Uani 1 1 d . . . H166 H 0.1963 -0.2663 0.5688 0.037 Uiso 1 1 calc R . . H167 H 0.2384 -0.2714 0.5308 0.037 Uiso 1 1 calc R . . C81 C 0.16225(16) -0.3137(2) 0.48810(16) 0.0423(9) Uani 1 1 d . . . H168 H 0.1321 -0.3331 0.5007 0.051 Uiso 1 1 calc R . . H169 H 0.1476 -0.2740 0.4648 0.051 Uiso 1 1 calc R . . C82 C 0.18021(16) -0.36175(19) 0.44870(15) 0.0402(9) Uani 1 1 d . . . H170 H 0.1475 -0.3754 0.4154 0.048 Uiso 1 1 calc R . . H171 H 0.2066 -0.3404 0.4315 0.048 Uiso 1 1 calc R . . C83 C 0.20737(14) -0.42107(17) 0.48405(15) 0.0331(7) Uani 1 1 d . . . H172 H 0.2210 -0.4500 0.4582 0.040 Uiso 1 1 calc R . . H173 H 0.1796 -0.4454 0.4971 0.040 Uiso 1 1 calc R . . C84 C 0.25563(13) -0.40186(16) 0.53866(14) 0.0285(7) Uani 1 1 d . . . H174 H 0.2847 -0.3806 0.5255 0.034 Uiso 1 1 calc R . . H175 H 0.2718 -0.4414 0.5613 0.034 Uiso 1 1 calc R . . C85 C 0.31393(12) -0.40634(15) 0.69268(14) 0.0250(6) Uani 1 1 d . . . H176 H 0.3249 -0.3919 0.7352 0.030 Uiso 1 1 calc R . . C86 C 0.26829(13) -0.45776(16) 0.68591(16) 0.0309(7) Uani 1 1 d . . . H177 H 0.2355 -0.4372 0.6926 0.037 Uiso 1 1 calc R . . H178 H 0.2569 -0.4755 0.6449 0.037 Uiso 1 1 calc R . . C87 C 0.28906(15) -0.51295(17) 0.73066(17) 0.0371(8) Uani 1 1 d . . . H179 H 0.2970 -0.4957 0.7716 0.045 Uiso 1 1 calc R . . H180 H 0.2596 -0.5461 0.7244 0.045 Uiso 1 1 calc R . . C88 C 0.34025(15) -0.54428(17) 0.72465(18) 0.0384(8) Uani 1 1 d . . . H181 H 0.3312 -0.5666 0.6856 0.046 Uiso 1 1 calc R . . H182 H 0.3538 -0.5773 0.7563 0.046 Uiso 1 1 calc R . . C89 C 0.38549(14) -0.49420(17) 0.72942(17) 0.0354(8) Uani 1 1 d . . . H183 H 0.4175 -0.5156 0.7219 0.042 Uiso 1 1 calc R . . H184 H 0.3981 -0.4762 0.7704 0.042 Uiso 1 1 calc R . . C90 C 0.36498(13) -0.43880(15) 0.68473(15) 0.0281(7) Uani 1 1 d . . . H185 H 0.3948 -0.4062 0.6904 0.034 Uiso 1 1 calc R . . H186 H 0.3559 -0.4561 0.6437 0.034 Uiso 1 1 calc R . . C91 C 0.38521(12) -0.34803(15) 0.56812(13) 0.0221(6) Uani 1 1 d . . . C92 C 0.41315(13) -0.44916(14) 0.52181(14) 0.0230(6) Uani 1 1 d . . . C93 C 0.45226(13) -0.49122(15) 0.55864(15) 0.0275(7) Uani 1 1 d . . . C94 C 0.46276(15) -0.54881(16) 0.53338(17) 0.0350(8) Uani 1 1 d . . . H187 H 0.4886 -0.5790 0.5572 0.042 Uiso 1 1 calc R . . C95 C 0.43600(16) -0.56258(17) 0.47412(18) 0.0385(9) Uani 1 1 d . . . H188 H 0.4437 -0.6022 0.4576 0.046 Uiso 1 1 calc R . . C96 C 0.39837(15) -0.51979(17) 0.43853(16) 0.0333(8) Uani 1 1 d . . . H189 H 0.3807 -0.5300 0.3978 0.040 Uiso 1 1 calc R . . C97 C 0.38596(13) -0.46176(15) 0.46158(14) 0.0265(7) Uani 1 1 d . . . C98 C 0.48211(16) -0.47399(18) 0.62279(15) 0.0366(8) Uani 1 1 d . . . H190 H 0.4931 -0.4282 0.6254 0.055 Uiso 1 1 calc R . . H191 H 0.5151 -0.5012 0.6378 0.055 Uiso 1 1 calc R . . H192 H 0.4575 -0.4813 0.6468 0.055 Uiso 1 1 calc R . . C99 C 0.34523(15) -0.41442(18) 0.42399(15) 0.0367(8) Uani 1 1 d . . . H193 H 0.3313 -0.4306 0.3830 0.055 Uiso 1 1 calc R . . H194 H 0.3634 -0.3724 0.4244 0.055 Uiso 1 1 calc R . . H195 H 0.3143 -0.4092 0.4400 0.055 Uiso 1 1 calc R . . C100 C 0.5132(4) -0.0997(5) 0.4956(5) 0.067(3) Uani 0.519(6) 1 d PU G 2 H196 H 0.4801 -0.0777 0.4986 0.100 Uiso 0.519(6) 1 calc PR G 2 H197 H 0.5031 -0.1279 0.4604 0.100 Uiso 0.519(6) 1 calc PR G 2 H198 H 0.5402 -0.0674 0.4920 0.100 Uiso 0.519(6) 1 calc PR G 2 C101 C 0.5969(4) -0.1493(5) 0.5955(5) 0.061(2) Uani 0.481(6) 1 d PU G 1 H199 H 0.6213 -0.1151 0.5892 0.091 Uiso 0.481(6) 1 calc PR G 1 H200 H 0.6114 -0.1919 0.5893 0.091 Uiso 0.481(6) 1 calc PR G 1 H201 H 0.5952 -0.1465 0.6364 0.091 Uiso 0.481(6) 1 calc PR G 1 C102 C 0.5159(4) -0.0785(4) 0.5688(6) 0.063(3) Uani 0.481(6) 1 d PU G 1 H202 H 0.5103 -0.0845 0.6077 0.094 Uiso 0.481(6) 1 calc PR G 1 H203 H 0.4805 -0.0678 0.5389 0.094 Uiso 0.481(6) 1 calc PR G 1 H204 H 0.5423 -0.0432 0.5713 0.094 Uiso 0.481(6) 1 calc PR G 1 C103 C 0.5466(5) -0.1334(5) 0.4901(4) 0.059(2) Uani 0.481(6) 1 d PU G 1 H205 H 0.5717 -0.0970 0.4910 0.088 Uiso 0.481(6) 1 calc PR G 1 H206 H 0.5109 -0.1251 0.4598 0.088 Uiso 0.481(6) 1 calc PR G 1 H207 H 0.5626 -0.1735 0.4803 0.088 Uiso 0.481(6) 1 calc PR G 1 C104 C 0.5937(3) -0.1651(5) 0.5465(5) 0.060(2) Uani 0.519(6) 1 d PU G 2 H208 H 0.6182 -0.1282 0.5475 0.090 Uiso 0.519(6) 1 calc PR G 2 H209 H 0.5873 -0.1889 0.5090 0.090 Uiso 0.519(6) 1 calc PR G 2 H210 H 0.6109 -0.1942 0.5801 0.090 Uiso 0.519(6) 1 calc PR G 2 C105 C 0.5508(5) -0.1001(5) 0.6066(5) 0.068(2) Uani 0.519(6) 1 d PU G 2 H211 H 0.5792 -0.0680 0.6069 0.102 Uiso 0.519(6) 1 calc PR G 2 H212 H 0.5642 -0.1283 0.6417 0.102 Uiso 0.519(6) 1 calc PR G 2 H213 H 0.5171 -0.0779 0.6076 0.102 Uiso 0.519(6) 1 calc PR G 2 Si13 Si 0.0177(3) -0.8043(3) 0.2489(3) 0.030(2) Uiso 0.138(3) 1 d P A 2 C106 C 0.0090(11) -0.7145(13) 0.2244(12) 0.035(6) Uiso 0.138(3) 1 d P A 2 C107 C 0.0626(13) -0.6916(16) 0.2108(14) 0.052(8) Uiso 0.138(3) 1 d P A 2 H214 H 0.0658 -0.7147 0.1757 0.077 Uiso 0.138(3) 1 calc PR A 2 H215 H 0.0951 -0.7009 0.2452 0.077 Uiso 0.138(3) 1 calc PR A 2 H216 H 0.0604 -0.6448 0.2029 0.077 Uiso 0.138(3) 1 calc PR A 2 C108 C -0.0405(12) -0.7068(16) 0.1674(13) 0.044(7) Uiso 0.138(3) 1 d P A 2 H217 H -0.0746 -0.7186 0.1758 0.066 Uiso 0.138(3) 1 calc PR A 2 H218 H -0.0355 -0.7354 0.1363 0.066 Uiso 0.138(3) 1 calc PR A 2 H219 H -0.0428 -0.6617 0.1539 0.066 Uiso 0.138(3) 1 calc PR A 2 C109 C 0.0131(15) -0.8527(19) 0.1785(17) 0.050(9) Uiso 0.138(3) 1 d P A 2 H220 H -0.0211 -0.8413 0.1470 0.075 Uiso 0.138(3) 1 calc PR A 2 H221 H 0.0131 -0.8992 0.1871 0.075 Uiso 0.138(3) 1 calc PR A 2 H222 H 0.0450 -0.8423 0.1653 0.075 Uiso 0.138(3) 1 calc PR A 2 C110 C 0.0011(13) -0.6710(16) 0.2738(14) 0.030(8) Uiso 0.138(3) 1 d P A 2 H223 H -0.0022 -0.6257 0.2606 0.045 Uiso 0.138(3) 1 calc PR A 2 H224 H 0.0331 -0.6756 0.3098 0.045 Uiso 0.138(3) 1 calc PR A 2 H225 H -0.0326 -0.6839 0.2826 0.045 Uiso 0.138(3) 1 calc PR A 2 C111 C -0.0509(15) -0.8303(18) 0.2640(15) 0.039(9) Uiso 0.138(3) 1 d P A 2 H226 H -0.0826 -0.8211 0.2287 0.058 Uiso 0.138(3) 1 calc PR A 2 H227 H -0.0548 -0.8058 0.2981 0.058 Uiso 0.138(3) 1 calc PR A 2 H228 H -0.0497 -0.8768 0.2729 0.058 Uiso 0.138(3) 1 calc PR A 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 0.02351(11) 0.01879(12) 0.02132(11) 0.00001(8) 0.01042(9) 0.00161(9) P1 0.0219(4) 0.0259(4) 0.0246(4) 0.0026(3) 0.0093(3) 0.0007(3) Si1 0.0229(4) 0.0221(4) 0.0207(4) 0.0024(3) 0.0094(3) 0.0027(3) Si2 0.0221(4) 0.0209(4) 0.0209(4) -0.0006(3) 0.0079(3) 0.0027(3) Si3 0.0283(4) 0.0253(4) 0.0225(4) 0.0014(3) 0.0067(3) 0.0025(3) Si4 0.0257(4) 0.0259(4) 0.0251(4) -0.0007(3) 0.0127(3) 0.0030(3) Si5 0.0266(4) 0.0221(4) 0.0274(4) -0.0042(3) 0.0101(3) 0.0030(3) Si6 0.0208(5) 0.0220(5) 0.0168(5) -0.0007(3) 0.0032(4) -0.0007(4) N1 0.0370(15) 0.0257(15) 0.0352(15) -0.0032(12) 0.0208(13) -0.0021(12) C1 0.045(2) 0.0328(19) 0.0305(18) -0.0026(14) 0.0063(16) 0.0000(16) C2 0.0303(17) 0.041(2) 0.0380(19) 0.0020(16) 0.0115(15) 0.0049(15) C3 0.0389(19) 0.0301(18) 0.0266(17) 0.0061(13) 0.0089(14) 0.0047(14) C4 0.065(3) 0.058(3) 0.039(2) 0.0145(19) 0.025(2) 0.015(2) C5 0.052(2) 0.050(2) 0.035(2) 0.0163(18) 0.0007(18) 0.0073(19) C6 0.062(3) 0.033(2) 0.043(2) 0.0058(17) 0.0147(19) -0.0109(18) C7 0.0375(18) 0.0304(19) 0.040(2) 0.0019(15) 0.0121(16) 0.0061(15) C8 0.046(2) 0.047(2) 0.0322(19) -0.0065(16) 0.0182(16) 0.0006(17) C9 0.0306(17) 0.0341(19) 0.0429(19) 0.0022(14) 0.0179(15) -0.0012(14) C10 0.047(3) 0.079(4) 0.136(5) -0.002(3) 0.054(3) -0.005(2) C11 0.132(6) 0.102(5) 0.115(4) -0.066(4) 0.083(4) -0.084(4) C12 0.064(3) 0.091(4) 0.149(5) 0.079(4) -0.014(4) -0.033(3) C13 0.0396(19) 0.040(2) 0.0324(18) -0.0054(15) 0.0149(15) 0.0023(16) C14 0.0324(18) 0.0319(19) 0.040(2) -0.0063(15) 0.0083(15) 0.0074(14) C15 0.0364(18) 0.0252(17) 0.043(2) -0.0028(14) 0.0136(16) 0.0001(14) C16 0.039(2) 0.038(2) 0.071(3) -0.001(2) 0.019(2) -0.0085(17) C17 0.075(3) 0.040(2) 0.049(2) 0.0108(19) 0.026(2) -0.004(2) C18 0.060(3) 0.0229(19) 0.070(3) -0.0089(18) 0.023(2) 0.0020(18) C19 0.026(2) 0.028(2) 0.027(2) -0.0013(16) 0.0027(18) 0.0032(19) C20 0.036(2) 0.035(2) 0.0270(19) 0.0019(16) 0.0093(16) -0.0040(17) C21 0.0250(18) 0.0267(19) 0.0224(18) -0.0033(14) -0.0006(14) 0.0000(14) C22 0.040(2) 0.038(2) 0.036(2) -0.0015(19) -0.0136(19) 0.001(2) C23 0.033(2) 0.044(3) 0.031(2) -0.0154(19) 0.003(2) -0.004(2) C24 0.026(2) 0.043(3) 0.037(3) -0.006(2) 0.007(2) -0.0025(18) C25 0.0237(16) 0.049(2) 0.0305(17) -0.0065(15) 0.0103(14) -0.0009(15) C26 0.041(2) 0.039(2) 0.056(2) -0.0064(18) 0.0274(19) -0.0053(16) C27 0.051(2) 0.038(2) 0.063(3) -0.0093(18) 0.038(2) 0.0011(17) C28 0.053(2) 0.050(3) 0.082(3) 0.003(2) 0.051(2) 0.009(2) C29 0.0327(19) 0.064(3) 0.049(2) 0.004(2) 0.0224(18) -0.0003(18) C30 0.0243(16) 0.039(2) 0.043(2) 0.0062(15) 0.0177(15) 0.0035(14) C31 0.0271(15) 0.0264(16) 0.0276(16) 0.0003(13) 0.0098(13) -0.0030(13) C32 0.0329(17) 0.0284(17) 0.0297(17) 0.0025(13) 0.0053(14) 0.0000(14) C33 0.041(2) 0.050(2) 0.039(2) 0.0046(18) -0.0003(17) 0.0051(18) C34 0.045(2) 0.061(3) 0.0309(19) -0.0014(18) 0.0027(17) -0.009(2) C35 0.046(2) 0.047(2) 0.035(2) -0.0123(17) 0.0141(17) -0.0138(18) C36 0.0398(19) 0.0320(19) 0.0332(18) -0.0017(14) 0.0109(15) 0.0017(15) C37 0.0293(17) 0.0281(18) 0.0394(19) 0.0085(14) 0.0076(14) -0.0015(14) C38 0.0269(16) 0.0307(18) 0.043(2) 0.0094(15) 0.0066(15) -0.0056(14) C39 0.048(2) 0.032(2) 0.054(2) 0.0119(18) 0.0095(19) -0.0046(17) C40 0.038(2) 0.034(2) 0.053(2) 0.0116(17) 0.0119(18) 0.0066(16) C41 0.0263(17) 0.038(2) 0.057(2) 0.0131(18) 0.0070(16) 0.0046(15) C42 0.0300(18) 0.033(2) 0.061(3) 0.0091(18) 0.0017(17) -0.0034(15) C43 0.0327(16) 0.0250(16) 0.0269(16) 0.0012(13) 0.0144(13) -0.0007(13) C44 0.044(2) 0.0215(16) 0.050(2) -0.0071(15) 0.0336(17) -0.0061(14) C45 0.054(2) 0.035(2) 0.046(2) -0.0121(16) 0.0357(19) -0.0128(17) C46 0.080(3) 0.039(2) 0.063(3) -0.024(2) 0.051(3) -0.020(2) C47 0.084(3) 0.029(2) 0.090(4) -0.018(2) 0.068(3) -0.011(2) C48 0.067(3) 0.0253(19) 0.084(3) 0.001(2) 0.053(3) 0.0030(18) C49 0.055(2) 0.0243(18) 0.057(2) -0.0006(16) 0.041(2) -0.0020(16) C50 0.066(3) 0.054(3) 0.038(2) -0.0130(19) 0.022(2) -0.008(2) C51 0.065(3) 0.038(2) 0.056(3) 0.0096(19) 0.030(2) 0.009(2) Pd2 0.02148(11) 0.01522(11) 0.01791(11) -0.00072(8) 0.00755(8) 0.00083(8) P2 0.0210(3) 0.0198(4) 0.0212(4) 0.0008(3) 0.0079(3) 0.0010(3) Si7 0.0217(4) 0.0190(4) 0.0191(4) 0.0015(3) 0.0084(3) 0.0018(3) Si8 0.0215(4) 0.0169(4) 0.0194(4) -0.0019(3) 0.0068(3) 0.0017(3) Si9 0.0271(4) 0.0222(4) 0.0202(4) 0.0013(3) 0.0058(3) 0.0027(3) Si10 0.0251(4) 0.0235(4) 0.0236(4) 0.0002(3) 0.0122(3) 0.0023(3) Si11 0.0260(4) 0.0254(4) 0.0226(4) -0.0045(3) 0.0027(3) 0.0015(3) Si12 0.0258(4) 0.0206(4) 0.0252(4) -0.0049(3) 0.0092(3) 0.0024(3) N2 0.0289(13) 0.0209(13) 0.0227(13) -0.0005(10) 0.0107(11) 0.0008(10) C52 0.0329(17) 0.0330(19) 0.0364(19) 0.0006(15) 0.0122(15) 0.0029(14) C53 0.043(2) 0.0247(17) 0.0265(17) -0.0013(13) 0.0045(14) 0.0011(14) C54 0.0385(18) 0.0314(18) 0.0233(16) 0.0071(13) 0.0094(14) 0.0068(14) C55 0.063(3) 0.032(2) 0.036(2) 0.0060(16) 0.0134(18) -0.0091(18) C56 0.073(3) 0.065(3) 0.048(2) 0.029(2) 0.038(2) 0.027(2) C57 0.054(2) 0.036(2) 0.040(2) 0.0128(17) -0.0032(18) 0.0054(18) C58 0.0345(17) 0.0296(18) 0.0355(18) 0.0021(14) 0.0121(15) 0.0061(14) C59 0.0400(19) 0.038(2) 0.0306(18) -0.0036(15) 0.0164(15) 0.0010(15) C60 0.0312(16) 0.0299(17) 0.0399(18) 0.0016(14) 0.0185(14) -0.0026(13) C61 0.061(3) 0.042(2) 0.0294(19) -0.0105(16) 0.0026(18) 0.0159(19) C62 0.0295(18) 0.034(2) 0.060(3) -0.0008(17) 0.0129(17) -0.0056(15) C63 0.0276(15) 0.0297(17) 0.0211(15) 0.0022(12) 0.0040(12) 0.0024(13) C64 0.044(2) 0.044(2) 0.0308(19) 0.0024(16) -0.0026(16) 0.0115(17) C65 0.0378(18) 0.0233(16) 0.0277(16) -0.0002(13) 0.0093(14) 0.0020(13) C66 0.043(2) 0.041(2) 0.037(2) 0.0058(16) 0.0183(17) -0.0005(16) C67 0.0295(17) 0.0322(18) 0.0357(18) -0.0048(14) 0.0089(14) 0.0061(14) C68 0.0370(18) 0.040(2) 0.0299(18) -0.0071(15) 0.0145(15) 0.0022(15) C69 0.0348(17) 0.0190(15) 0.0341(18) -0.0060(13) 0.0109(14) -0.0017(13) C70 0.048(2) 0.0242(18) 0.054(2) -0.0096(16) 0.0153(19) 0.0009(16) C71 0.0361(18) 0.0278(18) 0.046(2) -0.0050(15) 0.0137(16) -0.0072(14) C72 0.053(2) 0.0293(19) 0.040(2) 0.0030(15) 0.0147(18) -0.0043(16) C73 0.0243(15) 0.0356(18) 0.0226(15) -0.0022(13) 0.0078(12) 0.0030(13) C74 0.0258(16) 0.046(2) 0.0390(19) -0.0094(16) 0.0146(15) -0.0006(15) C75 0.0276(17) 0.067(3) 0.043(2) -0.0114(19) 0.0145(16) 0.0057(17) C76 0.0376(19) 0.049(2) 0.0354(19) -0.0053(16) 0.0190(16) 0.0099(16) C77 0.0403(19) 0.0358(19) 0.0319(18) -0.0069(15) 0.0156(15) 0.0030(15) C78 0.0265(16) 0.0374(19) 0.0281(17) -0.0039(14) 0.0103(13) 0.0000(14) C79 0.0248(14) 0.0240(15) 0.0220(15) -0.0010(12) 0.0085(12) -0.0015(12) C80 0.0353(18) 0.0287(17) 0.0263(16) -0.0016(13) 0.0050(14) 0.0045(14) C81 0.041(2) 0.044(2) 0.0313(19) -0.0022(16) -0.0032(16) 0.0091(17) C82 0.043(2) 0.046(2) 0.0242(17) -0.0054(15) -0.0002(15) 0.0016(17) C83 0.0347(18) 0.0332(19) 0.0320(18) -0.0072(14) 0.0114(15) -0.0045(14) C84 0.0311(16) 0.0268(17) 0.0277(16) -0.0057(13) 0.0091(13) 0.0004(13) C85 0.0263(15) 0.0219(15) 0.0269(16) 0.0034(12) 0.0085(12) -0.0014(12) C86 0.0256(16) 0.0283(17) 0.0408(19) 0.0084(14) 0.0132(14) 0.0002(13) C87 0.041(2) 0.0287(18) 0.046(2) 0.0096(15) 0.0205(17) -0.0030(15) C88 0.043(2) 0.0226(17) 0.051(2) 0.0122(15) 0.0161(17) 0.0035(15) C89 0.0286(17) 0.0299(18) 0.047(2) 0.0129(15) 0.0117(15) 0.0056(14) C90 0.0257(15) 0.0247(16) 0.0344(17) 0.0055(13) 0.0100(13) 0.0009(12) C91 0.0253(14) 0.0219(15) 0.0201(14) -0.0001(11) 0.0085(12) -0.0002(12) C92 0.0303(15) 0.0157(14) 0.0283(16) -0.0044(11) 0.0166(13) -0.0028(12) C93 0.0322(16) 0.0224(16) 0.0331(17) 0.0013(13) 0.0179(14) 0.0020(13) C94 0.045(2) 0.0211(16) 0.047(2) 0.0038(14) 0.0267(17) 0.0056(14) C95 0.054(2) 0.0202(17) 0.053(2) -0.0122(15) 0.0339(19) -0.0062(15) C96 0.0408(19) 0.0312(18) 0.0347(18) -0.0137(14) 0.0217(15) -0.0120(15) C97 0.0315(16) 0.0246(16) 0.0284(16) -0.0057(12) 0.0167(13) -0.0065(13) C98 0.046(2) 0.0348(19) 0.0319(18) 0.0045(15) 0.0154(16) 0.0132(16) C99 0.042(2) 0.041(2) 0.0256(17) -0.0061(15) 0.0082(15) -0.0003(16) C100 0.061(5) 0.051(5) 0.077(5) 0.030(4) 0.004(4) -0.019(4) C101 0.040(3) 0.048(4) 0.088(6) 0.009(4) 0.010(4) -0.020(3) C102 0.057(5) 0.030(3) 0.118(8) -0.016(5) 0.053(5) -0.016(3) C103 0.066(5) 0.061(5) 0.059(4) 0.010(4) 0.034(4) -0.024(4) C104 0.041(3) 0.052(4) 0.098(6) 0.003(4) 0.037(4) -0.006(3) C105 0.075(5) 0.058(5) 0.085(5) -0.028(4) 0.045(4) -0.038(4) _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 C43 1.989(3) . ? Pd1 P1 2.4437(8) . ? Pd1 Si2 2.4581(9) . ? Pd1 Si1 2.4597(8) . ? P1 C31 1.862(3) . ? P1 C25 1.865(3) . ? P1 C37 1.880(3) . ? Si1 Si2 2.2861(11) . ? Si1 Si4 2.3685(11) . ? Si1 Si3 2.3882(12) . ? Si2 Si5 2.3745(12) . ? Si2 Si6 2.3784(12) . ? Si2 Si13 2.525(7) . ? Si3 C2 1.878(3) . ? Si3 C1 1.892(4) . ? Si3 C3 1.921(3) . ? Si4 C7 1.869(4) . ? Si4 C8 1.884(4) . ? Si4 C9 1.925(4) . ? Si5 C13 1.879(3) . ? Si5 C14 1.884(3) . ? Si5 C15 1.920(4) . ? Si6 C20 1.881(4) . ? Si6 C19 1.889(5) . ? Si6 C21 1.926(4) . ? N1 C43 1.159(4) . ? N1 C44 1.400(4) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H6 0.9800 . ? C3 C6 1.520(5) . ? C3 C4 1.525(5) . ? C3 C5 1.534(5) . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? C5 H10 0.9800 . ? C5 H11 0.9800 . ? C5 H12 0.9800 . ? C6 H13 0.9800 . ? C6 H14 0.9800 . ? C6 H15 0.9800 . ? C7 H16 0.9800 . ? C7 H17 0.9800 . ? C7 H18 0.9800 . ? C8 H19 0.9800 . ? C8 H20 0.9800 . ? C8 H21 0.9800 . ? C9 C12 1.487(6) . ? C9 C11 1.494(6) . ? C9 C10 1.522(5) . ? C10 H22 0.9800 . ? C10 H23 0.9800 . ? C10 H24 0.9800 . ? C11 H25 0.9800 . ? C11 H26 0.9800 . ? C11 H27 0.9800 . ? C12 H28 0.9800 . ? C12 H29 0.9800 . ? C12 H30 0.9800 . ? C13 H31 0.9800 . ? C13 H32 0.9800 . ? C13 H33 0.9800 . ? C14 H34 0.9800 . ? C14 H35 0.9800 . ? C14 H36 0.9800 . ? C15 C16 1.525(5) . ? C15 C17 1.526(5) . ? C15 C18 1.536(5) . ? C16 H37 0.9800 . ? C16 H38 0.9800 . ? C16 H39 0.9800 . ? C17 H40 0.9800 . ? C17 H41 0.9800 . ? C17 H42 0.9800 . ? C18 H43 0.9800 . ? C18 H44 0.9800 . ? C18 H45 0.9800 . ? C19 H46 0.9800 . ? C19 H47 0.9800 . ? C19 H48 0.9800 . ? C20 H49 0.9800 . ? C20 H50 0.9800 . ? C20 H51 0.9800 . ? C21 C24 1.518(6) . ? C21 C23 1.525(6) . ? C21 C22 1.539(5) . ? C22 H52 0.9800 . ? C22 H53 0.9800 . ? C22 H54 0.9800 . ? C23 H55 0.9800 . ? C23 H56 0.9800 . ? C23 H57 0.9800 . ? C24 H58 0.9800 . ? C24 H59 0.9800 . ? C24 H60 0.9800 . ? C25 C26 1.488(5) . ? C25 C30 1.534(4) . ? C25 H61 1.0000 . ? C26 C27 1.551(5) . ? C26 H62 0.9900 . ? C26 H63 0.9900 . ? C27 C28 1.547(5) . ? C27 H64 0.9900 . ? C27 H65 0.9900 . ? C28 C29 1.489(6) . ? C28 H66 0.9900 . ? C28 H67 0.9900 . ? C29 C30 1.509(5) . ? C29 H68 0.9900 . ? C29 H69 0.9900 . ? C30 H70 0.9900 . ? C30 H71 0.9900 . ? C31 C36 1.531(5) . ? C31 C32 1.533(4) . ? C31 H72 1.0000 . ? C32 C33 1.528(5) . ? C32 H73 0.9900 . ? C32 H74 0.9900 . ? C33 C34 1.519(6) . ? C33 H75 0.9900 . ? C33 H76 0.9900 . ? C34 C35 1.510(6) . ? C34 H77 0.9900 . ? C34 H78 0.9900 . ? C35 C36 1.529(5) . ? C35 H79 0.9900 . ? C35 H80 0.9900 . ? C36 H81 0.9900 . ? C36 H82 0.9900 . ? C37 C42 1.508(5) . ? C37 C38 1.530(4) . ? C37 H83 1.0000 . ? C38 C39 1.547(5) . ? C38 H84 0.9900 . ? C38 H85 0.9900 . ? C39 C40 1.493(5) . ? C39 H86 0.9900 . ? C39 H87 0.9900 . ? C40 C41 1.523(5) . ? C40 H88 0.9900 . ? C40 H89 0.9900 . ? C41 C42 1.521(5) . ? C41 H90 0.9900 . ? C41 H91 0.9900 . ? C42 H92 0.9900 . ? C42 H93 0.9900 . ? C44 C49 1.393(5) . ? C44 C45 1.398(5) . ? C45 C46 1.394(5) . ? C45 C50 1.495(6) . ? C46 C47 1.373(7) . ? C46 H94 0.9500 . ? C47 C48 1.373(7) . ? C47 H95 0.9500 . ? C48 C49 1.398(5) . ? C48 H96 0.9500 . ? C49 C51 1.498(6) . ? C50 H97 0.9800 . ? C50 H98 0.9800 . ? C50 H99 0.9800 . ? C51 H100 0.9800 . ? C51 H101 0.9800 . ? C51 H102 0.9800 . ? Pd2 C91 2.001(3) . ? Pd2 Si8 2.4264(8) . ? Pd2 P2 2.4352(8) . ? Pd2 Si7 2.4603(8) . ? P2 C79 1.865(3) . ? P2 C85 1.871(3) . ? P2 C73 1.880(3) . ? Si7 Si8 2.2967(11) . ? Si7 Si10 2.3754(11) . ? Si7 Si9 2.3933(11) . ? Si8 Si12 2.3734(11) . ? Si8 Si11 2.4099(11) . ? Si9 C52 1.879(3) . ? Si9 C53 1.886(3) . ? Si9 C54 1.933(3) . ? Si10 C58 1.877(3) . ? Si10 C59 1.889(3) . ? Si10 C60 1.936(3) . ? Si11 C62 1.876(4) . ? Si11 C61 1.883(4) . ? Si11 C63 1.912(3) . ? Si12 C67 1.884(3) . ? Si12 C68 1.888(3) . ? Si12 C69 1.919(3) . ? N2 C91 1.159(4) . ? N2 C92 1.402(4) . ? C52 H103 0.9800 . ? C52 H104 0.9800 . ? C52 H105 0.9800 . ? C53 H106 0.9800 . ? C53 H107 0.9800 . ? C53 H108 0.9800 . ? C54 C55 1.521(5) . ? C54 C56 1.534(5) . ? C54 C57 1.538(5) . ? C55 H109 0.9800 . ? C55 H110 0.9800 . ? C55 H111 0.9800 . ? C56 H112 0.9800 . ? C56 H113 0.9800 . ? C56 H114 0.9800 . ? C57 H115 0.9800 . ? C57 H116 0.9800 . ? C57 H117 0.9800 . ? C58 H118 0.9800 . ? C58 H119 0.9800 . ? C58 H120 0.9800 . ? C59 H121 0.9800 . ? C59 H122 0.9800 . ? C59 H123 0.9800 . ? C60 C105 1.499(10) . ? C60 C102 1.508(10) . ? C60 C100 1.517(9) . ? C60 C103 1.526(9) . ? C60 C104 1.533(9) . ? C60 C101 1.541(10) . ? C61 H124 0.9800 . ? C61 H125 0.9800 . ? C61 H126 0.9800 . ? C62 H127 0.9800 . ? C62 H128 0.9800 . ? C62 H129 0.9800 . ? C63 C65 1.522(4) . ? C63 C66 1.532(5) . ? C63 C64 1.542(4) . ? C64 H130 0.9800 . ? C64 H131 0.9800 . ? C64 H132 0.9800 . ? C65 H133 0.9800 . ? C65 H134 0.9800 . ? C65 H135 0.9800 . ? C66 H136 0.9800 . ? C66 H137 0.9800 . ? C66 H138 0.9800 . ? C67 H139 0.9800 . ? C67 H140 0.9800 . ? C67 H141 0.9800 . ? C68 H142 0.9800 . ? C68 H143 0.9800 . ? C68 H144 0.9800 . ? C69 C71 1.528(5) . ? C69 C72 1.528(5) . ? C69 C70 1.536(5) . ? C70 H145 0.9800 . ? C70 H146 0.9800 . ? C70 H147 0.9800 . ? C71 H148 0.9800 . ? C71 H149 0.9800 . ? C71 H150 0.9800 . ? C72 H151 0.9800 . ? C72 H152 0.9800 . ? C72 H153 0.9800 . ? C73 C78 1.526(4) . ? C73 C74 1.541(4) . ? C73 H154 1.0000 . ? C74 C75 1.530(5) . ? C74 H155 0.9900 . ? C74 H156 0.9900 . ? C75 C76 1.505(5) . ? C75 H157 0.9900 . ? C75 H158 0.9900 . ? C76 C77 1.511(5) . ? C76 H159 0.9900 . ? C76 H160 0.9900 . ? C77 C78 1.531(4) . ? C77 H161 0.9900 . ? C77 H162 0.9900 . ? C78 H163 0.9900 . ? C78 H164 0.9900 . ? C79 C84 1.534(4) . ? C79 C80 1.538(4) . ? C79 H165 1.0000 . ? C80 C81 1.526(5) . ? C80 H166 0.9900 . ? C80 H167 0.9900 . ? C81 C82 1.523(5) . ? C81 H168 0.9900 . ? C81 H169 0.9900 . ? C82 C83 1.519(5) . ? C82 H170 0.9900 . ? C82 H171 0.9900 . ? C83 C84 1.528(4) . ? C83 H172 0.9900 . ? C83 H173 0.9900 . ? C84 H174 0.9900 . ? C84 H175 0.9900 . ? C85 C90 1.524(4) . ? C85 C86 1.543(4) . ? C85 H176 1.0000 . ? C86 C87 1.529(5) . ? C86 H177 0.9900 . ? C86 H178 0.9900 . ? C87 C88 1.500(5) . ? C87 H179 0.9900 . ? C87 H180 0.9900 . ? C88 C89 1.524(5) . ? C88 H181 0.9900 . ? C88 H182 0.9900 . ? C89 C90 1.531(4) . ? C89 H183 0.9900 . ? C89 H184 0.9900 . ? C90 H185 0.9900 . ? C90 H186 0.9900 . ? C92 C97 1.397(4) . ? C92 C93 1.398(4) . ? C93 C94 1.391(4) . ? C93 C98 1.509(5) . ? C94 C95 1.380(5) . ? C94 H187 0.9500 . ? C95 C96 1.377(5) . ? C95 H188 0.9500 . ? C96 C97 1.390(4) . ? C96 H189 0.9500 . ? C97 C99 1.496(5) . ? C98 H190 0.9800 . ? C98 H191 0.9800 . ? C98 H192 0.9800 . ? C99 H193 0.9800 . ? C99 H194 0.9800 . ? C99 H195 0.9800 . ? C100 H196 0.9800 . ? C100 H197 0.9800 . ? C100 H198 0.9800 . ? C101 H199 0.9800 . ? C101 H200 0.9800 . ? C101 H201 0.9800 . ? C102 H202 0.9800 . ? C102 H203 0.9800 . ? C102 H204 0.9800 . ? C103 H205 0.9800 . ? C103 H206 0.9800 . ? C103 H207 0.9800 . ? C104 H208 0.9800 . ? C104 H209 0.9800 . ? C104 H210 0.9800 . ? C105 H211 0.9800 . ? C105 H212 0.9800 . ? C105 H213 0.9800 . ? Si13 C109 1.91(4) . ? Si13 C106 1.93(3) . ? Si13 C111 1.96(4) . ? C106 C110 1.53(4) . ? C106 C108 1.54(4) . ? C106 C107 1.57(4) . ? C107 H214 0.9800 . ? C107 H215 0.9800 . ? C107 H216 0.9800 . ? C108 H217 0.9800 . ? C108 H218 0.9800 . ? C108 H219 0.9800 . ? C109 H220 0.9800 . ? C109 H221 0.9800 . ? C109 H222 0.9800 . ? C110 H223 0.9800 . ? C110 H224 0.9800 . ? C110 H225 0.9800 . ? C111 H226 0.9800 . ? C111 H227 0.9800 . ? C111 H228 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 C43 Pd1 P1 96.06(9) . . ? C43 Pd1 Si2 142.72(9) . . ? P1 Pd1 Si2 117.73(3) . . ? C43 Pd1 Si1 96.15(9) . . ? P1 Pd1 Si1 162.52(3) . . ? Si2 Pd1 Si1 55.40(3) . . ? C31 P1 C25 104.24(15) . . ? C31 P1 C37 102.42(15) . . ? C25 P1 C37 102.85(17) . . ? C31 P1 Pd1 109.12(10) . . ? C25 P1 Pd1 123.49(12) . . ? C37 P1 Pd1 112.51(11) . . ? Si2 Si1 Si4 126.91(5) . . ? Si2 Si1 Si3 117.87(4) . . ? Si4 Si1 Si3 114.92(4) . . ? Si2 Si1 Pd1 62.26(3) . . ? Si4 Si1 Pd1 118.40(4) . . ? Si3 Si1 Pd1 95.14(4) . . ? Si1 Si2 Si5 121.89(5) . . ? Si1 Si2 Si6 119.41(5) . . ? Si5 Si2 Si6 113.98(5) . . ? Si1 Si2 Pd1 62.33(3) . . ? Si5 Si2 Pd1 133.75(4) . . ? Si6 Si2 Pd1 94.95(4) . . ? Si1 Si2 Si13 117.68(16) . . ? Si5 Si2 Si13 101.86(16) . . ? Pd1 Si2 Si13 116.21(17) . . ? C2 Si3 C1 107.91(17) . . ? C2 Si3 C3 105.81(16) . . ? C1 Si3 C3 105.04(16) . . ? C2 Si3 Si1 109.58(12) . . ? C1 Si3 Si1 105.78(12) . . ? C3 Si3 Si1 121.99(11) . . ? C7 Si4 C8 104.16(17) . . ? C7 Si4 C9 106.44(16) . . ? C8 Si4 C9 109.95(17) . . ? C7 Si4 Si1 111.55(12) . . ? C8 Si4 Si1 110.26(13) . . ? C9 Si4 Si1 113.97(11) . . ? C13 Si5 C14 103.73(16) . . ? C13 Si5 C15 107.05(16) . . ? C14 Si5 C15 107.60(16) . . ? C13 Si5 Si2 109.91(12) . . ? C14 Si5 Si2 115.07(11) . . ? C15 Si5 Si2 112.83(11) . . ? C20 Si6 C19 105.8(2) . . ? C20 Si6 C21 106.16(17) . . ? C19 Si6 C21 105.15(18) . . ? C20 Si6 Si2 105.65(13) . . ? C19 Si6 Si2 110.89(14) . . ? C21 Si6 Si2 122.12(12) . . ? C43 N1 C44 175.5(3) . . ? Si3 C1 H1 109.5 . . ? Si3 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? Si3 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? Si3 C2 H4 109.5 . . ? Si3 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? Si3 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? C6 C3 C4 110.9(3) . . ? C6 C3 C5 107.4(3) . . ? C4 C3 C5 106.9(3) . . ? C6 C3 Si3 112.3(2) . . ? C4 C3 Si3 111.5(2) . . ? C5 C3 Si3 107.6(3) . . ? C3 C4 H7 109.5 . . ? C3 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C3 C4 H9 109.5 . . ? H7 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C3 C5 H10 109.5 . . ? C3 C5 H11 109.5 . . ? H10 C5 H11 109.5 . . ? C3 C5 H12 109.5 . . ? H10 C5 H12 109.5 . . ? H11 C5 H12 109.5 . . ? C3 C6 H13 109.5 . . ? C3 C6 H14 109.5 . . ? H13 C6 H14 109.5 . . ? C3 C6 H15 109.5 . . ? H13 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? Si4 C7 H16 109.5 . . ? Si4 C7 H17 109.5 . . ? H16 C7 H17 109.5 . . ? Si4 C7 H18 109.5 . . ? H16 C7 H18 109.5 . . ? H17 C7 H18 109.5 . . ? Si4 C8 H19 109.5 . . ? Si4 C8 H20 109.5 . . ? H19 C8 H20 109.5 . . ? Si4 C8 H21 109.5 . . ? H19 C8 H21 109.5 . . ? H20 C8 H21 109.5 . . ? C12 C9 C11 110.0(5) . . ? C12 C9 C10 106.9(4) . . ? C11 C9 C10 107.4(4) . . ? C12 C9 Si4 112.6(3) . . ? C11 C9 Si4 110.3(3) . . ? C10 C9 Si4 109.4(3) . . ? C9 C10 H22 109.5 . . ? C9 C10 H23 109.5 . . ? H22 C10 H23 109.5 . . ? C9 C10 H24 109.5 . . ? H22 C10 H24 109.5 . . ? H23 C10 H24 109.5 . . ? C9 C11 H25 109.5 . . ? C9 C11 H26 109.5 . . ? H25 C11 H26 109.5 . . ? C9 C11 H27 109.5 . . ? H25 C11 H27 109.5 . . ? H26 C11 H27 109.5 . . ? C9 C12 H28 109.5 . . ? C9 C12 H29 109.5 . . ? H28 C12 H29 109.5 . . ? C9 C12 H30 109.5 . . ? H28 C12 H30 109.5 . . ? H29 C12 H30 109.5 . . ? Si5 C13 H31 109.5 . . ? Si5 C13 H32 109.5 . . ? H31 C13 H32 109.5 . . ? Si5 C13 H33 109.5 . . ? H31 C13 H33 109.5 . . ? H32 C13 H33 109.5 . . ? Si5 C14 H34 109.5 . . ? Si5 C14 H35 109.5 . . ? H34 C14 H35 109.5 . . ? Si5 C14 H36 109.5 . . ? H34 C14 H36 109.5 . . ? H35 C14 H36 109.5 . . ? C16 C15 C17 108.6(3) . . ? C16 C15 C18 108.7(3) . . ? C17 C15 C18 108.6(3) . . ? C16 C15 Si5 111.8(3) . . ? C17 C15 Si5 109.6(3) . . ? C18 C15 Si5 109.5(3) . . ? C15 C16 H37 109.5 . . ? C15 C16 H38 109.5 . . ? H37 C16 H38 109.5 . . ? C15 C16 H39 109.5 . . ? H37 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? C15 C17 H40 109.5 . . ? C15 C17 H41 109.5 . . ? H40 C17 H41 109.5 . . ? C15 C17 H42 109.5 . . ? H40 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? C15 C18 H43 109.5 . . ? C15 C18 H44 109.5 . . ? H43 C18 H44 109.5 . . ? C15 C18 H45 109.5 . . ? H43 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? C24 C21 C23 108.0(4) . . ? C24 C21 C22 108.8(4) . . ? C23 C21 C22 108.3(3) . . ? C24 C21 Si6 110.9(3) . . ? C23 C21 Si6 112.1(3) . . ? C22 C21 Si6 108.7(3) . . ? C26 C25 C30 109.0(3) . . ? C26 C25 P1 112.9(3) . . ? C30 C25 P1 118.5(2) . . ? C26 C25 H61 105.0 . . ? C30 C25 H61 105.0 . . ? P1 C25 H61 105.0 . . ? C25 C26 C27 112.3(3) . . ? C25 C26 H62 109.1 . . ? C27 C26 H62 109.1 . . ? C25 C26 H63 109.1 . . ? C27 C26 H63 109.1 . . ? H62 C26 H63 107.9 . . ? C28 C27 C26 108.8(3) . . ? C28 C27 H64 109.9 . . ? C26 C27 H64 109.9 . . ? C28 C27 H65 109.9 . . ? C26 C27 H65 109.9 . . ? H64 C27 H65 108.3 . . ? C29 C28 C27 113.3(3) . . ? C29 C28 H66 108.9 . . ? C27 C28 H66 108.9 . . ? C29 C28 H67 108.9 . . ? C27 C28 H67 108.9 . . ? H66 C28 H67 107.7 . . ? C28 C29 C30 112.4(3) . . ? C28 C29 H68 109.1 . . ? C30 C29 H68 109.1 . . ? C28 C29 H69 109.1 . . ? C30 C29 H69 109.1 . . ? H68 C29 H69 107.9 . . ? C29 C30 C25 112.0(3) . . ? C29 C30 H70 109.2 . . ? C25 C30 H70 109.2 . . ? C29 C30 H71 109.2 . . ? C25 C30 H71 109.2 . . ? H70 C30 H71 107.9 . . ? C36 C31 C32 109.1(3) . . ? C36 C31 P1 113.4(2) . . ? C32 C31 P1 110.5(2) . . ? C36 C31 H72 107.9 . . ? C32 C31 H72 107.9 . . ? P1 C31 H72 107.9 . . ? C33 C32 C31 111.6(3) . . ? C33 C32 H73 109.3 . . ? C31 C32 H73 109.3 . . ? C33 C32 H74 109.3 . . ? C31 C32 H74 109.3 . . ? H73 C32 H74 108.0 . . ? C34 C33 C32 112.0(3) . . ? C34 C33 H75 109.2 . . ? C32 C33 H75 109.2 . . ? C34 C33 H76 109.2 . . ? C32 C33 H76 109.2 . . ? H75 C33 H76 107.9 . . ? C35 C34 C33 110.9(3) . . ? C35 C34 H77 109.5 . . ? C33 C34 H77 109.5 . . ? C35 C34 H78 109.5 . . ? C33 C34 H78 109.5 . . ? H77 C34 H78 108.1 . . ? C34 C35 C36 111.3(3) . . ? C34 C35 H79 109.4 . . ? C36 C35 H79 109.4 . . ? C34 C35 H80 109.4 . . ? C36 C35 H80 109.4 . . ? H79 C35 H80 108.0 . . ? C35 C36 C31 111.9(3) . . ? C35 C36 H81 109.2 . . ? C31 C36 H81 109.2 . . ? C35 C36 H82 109.2 . . ? C31 C36 H82 109.2 . . ? H81 C36 H82 107.9 . . ? C42 C37 C38 110.2(3) . . ? C42 C37 P1 111.6(2) . . ? C38 C37 P1 116.7(2) . . ? C42 C37 H83 105.8 . . ? C38 C37 H83 105.8 . . ? P1 C37 H83 105.8 . . ? C37 C38 C39 111.0(3) . . ? C37 C38 H84 109.4 . . ? C39 C38 H84 109.4 . . ? C37 C38 H85 109.4 . . ? C39 C38 H85 109.4 . . ? H84 C38 H85 108.0 . . ? C40 C39 C38 111.5(3) . . ? C40 C39 H86 109.3 . . ? C38 C39 H86 109.3 . . ? C40 C39 H87 109.3 . . ? C38 C39 H87 109.3 . . ? H86 C39 H87 108.0 . . ? C39 C40 C41 110.9(3) . . ? C39 C40 H88 109.5 . . ? C41 C40 H88 109.5 . . ? C39 C40 H89 109.5 . . ? C41 C40 H89 109.5 . . ? H88 C40 H89 108.0 . . ? C42 C41 C40 111.5(3) . . ? C42 C41 H90 109.3 . . ? C40 C41 H90 109.3 . . ? C42 C41 H91 109.3 . . ? C40 C41 H91 109.3 . . ? H90 C41 H91 108.0 . . ? C37 C42 C41 112.9(3) . . ? C37 C42 H92 109.0 . . ? C41 C42 H92 109.0 . . ? C37 C42 H93 109.0 . . ? C41 C42 H93 109.0 . . ? H92 C42 H93 107.8 . . ? N1 C43 Pd1 170.9(3) . . ? C49 C44 C45 124.0(3) . . ? C49 C44 N1 118.0(3) . . ? C45 C44 N1 117.9(3) . . ? C46 C45 C44 116.2(4) . . ? C46 C45 C50 122.6(4) . . ? C44 C45 C50 121.2(3) . . ? C47 C46 C45 121.1(4) . . ? C47 C46 H94 119.4 . . ? C45 C46 H94 119.4 . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H95 119.3 . . ? C48 C47 H95 119.3 . . ? C47 C48 C49 120.5(4) . . ? C47 C48 H96 119.8 . . ? C49 C48 H96 119.8 . . ? C44 C49 C48 116.8(4) . . ? C44 C49 C51 121.7(3) . . ? C48 C49 C51 121.5(4) . . ? C45 C50 H97 109.5 . . ? C45 C50 H98 109.5 . . ? H97 C50 H98 109.5 . . ? C45 C50 H99 109.5 . . ? H97 C50 H99 109.5 . . ? H98 C50 H99 109.5 . . ? C49 C51 H100 109.5 . . ? C49 C51 H101 109.5 . . ? H100 C51 H101 109.5 . . ? C49 C51 H102 109.5 . . ? H100 C51 H102 109.5 . . ? H101 C51 H102 109.5 . . ? C91 Pd2 Si8 144.13(9) . . ? C91 Pd2 P2 100.09(9) . . ? Si8 Pd2 P2 113.52(3) . . ? C91 Pd2 Si7 96.48(9) . . ? Si8 Pd2 Si7 56.06(3) . . ? P2 Pd2 Si7 156.77(3) . . ? C79 P2 C85 105.15(14) . . ? C79 P2 C73 101.51(13) . . ? C85 P2 C73 104.10(15) . . ? C79 P2 Pd2 109.61(10) . . ? C85 P2 Pd2 117.01(10) . . ? C73 P2 Pd2 117.73(11) . . ? Si8 Si7 Si10 129.43(4) . . ? Si8 Si7 Si9 118.04(4) . . ? Si10 Si7 Si9 112.42(4) . . ? Si8 Si7 Pd2 61.22(3) . . ? Si10 Si7 Pd2 117.58(4) . . ? Si9 Si7 Pd2 95.77(4) . . ? Si7 Si8 Si12 120.18(4) . . ? Si7 Si8 Si11 116.11(4) . . ? Si12 Si8 Si11 108.12(4) . . ? Si7 Si8 Pd2 62.72(3) . . ? Si12 Si8 Pd2 132.51(4) . . ? Si11 Si8 Pd2 110.99(4) . . ? C52 Si9 C53 107.25(16) . . ? C52 Si9 C54 105.37(15) . . ? C53 Si9 C54 105.23(15) . . ? C52 Si9 Si7 109.34(12) . . ? C53 Si9 Si7 106.06(11) . . ? C54 Si9 Si7 122.71(11) . . ? C58 Si10 C59 102.09(16) . . ? C58 Si10 C60 108.18(16) . . ? C59 Si10 C60 109.72(16) . . ? C58 Si10 Si7 112.87(11) . . ? C59 Si10 Si7 108.94(12) . . ? C60 Si10 Si7 114.34(11) . . ? C62 Si11 C61 102.2(2) . . ? C62 Si11 C63 108.58(16) . . ? C61 Si11 C63 105.00(16) . . ? C62 Si11 Si8 112.08(13) . . ? C61 Si11 Si8 113.95(13) . . ? C63 Si11 Si8 114.10(10) . . ? C67 Si12 C68 102.97(16) . . ? C67 Si12 C69 109.17(16) . . ? C68 Si12 C69 105.87(16) . . ? C67 Si12 Si8 115.48(11) . . ? C68 Si12 Si8 111.81(12) . . ? C69 Si12 Si8 110.88(11) . . ? C91 N2 C92 172.5(3) . . ? Si9 C52 H103 109.5 . . ? Si9 C52 H104 109.5 . . ? H103 C52 H104 109.5 . . ? Si9 C52 H105 109.5 . . ? H103 C52 H105 109.5 . . ? H104 C52 H105 109.5 . . ? Si9 C53 H106 109.5 . . ? Si9 C53 H107 109.5 . . ? H106 C53 H107 109.5 . . ? Si9 C53 H108 109.5 . . ? H106 C53 H108 109.5 . . ? H107 C53 H108 109.5 . . ? C55 C54 C56 110.4(3) . . ? C55 C54 C57 107.5(3) . . ? C56 C54 C57 106.6(3) . . ? C55 C54 Si9 113.3(2) . . ? C56 C54 Si9 111.7(2) . . ? C57 C54 Si9 107.0(2) . . ? C54 C55 H109 109.5 . . ? C54 C55 H110 109.5 . . ? H109 C55 H110 109.5 . . ? C54 C55 H111 109.5 . . ? H109 C55 H111 109.5 . . ? H110 C55 H111 109.5 . . ? C54 C56 H112 109.5 . . ? C54 C56 H113 109.5 . . ? H112 C56 H113 109.5 . . ? C54 C56 H114 109.5 . . ? H112 C56 H114 109.5 . . ? H113 C56 H114 109.5 . . ? C54 C57 H115 109.5 . . ? C54 C57 H116 109.5 . . ? H115 C57 H116 109.5 . . ? C54 C57 H117 109.5 . . ? H115 C57 H117 109.5 . . ? H116 C57 H117 109.5 . . ? Si10 C58 H118 109.5 . . ? Si10 C58 H119 109.5 . . ? H118 C58 H119 109.5 . . ? Si10 C58 H120 109.5 . . ? H118 C58 H120 109.5 . . ? H119 C58 H120 109.5 . . ? Si10 C59 H121 109.5 . . ? Si10 C59 H122 109.5 . . ? H121 C59 H122 109.5 . . ? Si10 C59 H123 109.5 . . ? H121 C59 H123 109.5 . . ? H122 C59 H123 109.5 . . ? C105 C60 C100 111.5(7) . . ? C102 C60 C103 110.9(7) . . ? C105 C60 C104 107.3(6) . . ? C100 C60 C104 105.7(6) . . ? C102 C60 C101 106.3(7) . . ? C103 C60 C101 105.3(6) . . ? C105 C60 Si10 111.9(4) . . ? C102 C60 Si10 111.8(4) . . ? C100 C60 Si10 111.5(4) . . ? C103 C60 Si10 111.6(4) . . ? C104 C60 Si10 108.6(4) . . ? C101 C60 Si10 110.5(4) . . ? Si11 C61 H124 109.5 . . ? Si11 C61 H125 109.5 . . ? Si11 C61 H126 109.5 . . ? Si11 C62 H127 109.5 . . ? Si11 C62 H128 109.5 . . ? Si11 C62 H129 109.5 . . ? C65 C63 C66 108.8(3) . . ? C65 C63 C64 108.8(3) . . ? C66 C63 C64 108.9(3) . . ? C65 C63 Si11 111.1(2) . . ? C66 C63 Si11 109.7(2) . . ? C64 C63 Si11 109.5(2) . . ? C63 C64 H130 109.5 . . ? C63 C64 H131 109.5 . . ? C63 C64 H132 109.5 . . ? C63 C65 H133 109.5 . . ? C63 C65 H134 109.5 . . ? C63 C65 H135 109.5 . . ? C63 C66 H136 109.5 . . ? C63 C66 H137 109.5 . . ? C63 C66 H138 109.5 . . ? Si12 C67 H139 109.5 . . ? Si12 C67 H140 109.5 . . ? H139 C67 H140 109.5 . . ? Si12 C67 H141 109.5 . . ? H139 C67 H141 109.5 . . ? H140 C67 H141 109.5 . . ? Si12 C68 H142 109.5 . . ? Si12 C68 H143 109.5 . . ? H142 C68 H143 109.5 . . ? Si12 C68 H144 109.5 . . ? H142 C68 H144 109.5 . . ? H143 C68 H144 109.5 . . ? C71 C69 C72 108.4(3) . . ? C71 C69 C70 108.9(3) . . ? C72 C69 C70 109.4(3) . . ? C71 C69 Si12 110.2(2) . . ? C72 C69 Si12 109.9(2) . . ? C70 C69 Si12 110.0(2) . . ? C69 C70 H145 109.5 . . ? C69 C70 H146 109.5 . . ? H145 C70 H146 109.5 . . ? C69 C70 H147 109.5 . . ? H145 C70 H147 109.5 . . ? H146 C70 H147 109.5 . . ? C69 C71 H148 109.5 . . ? C69 C71 H149 109.5 . . ? H148 C71 H149 109.5 . . ? C69 C71 H150 109.5 . . ? H148 C71 H150 109.5 . . ? H149 C71 H150 109.5 . . ? C69 C72 H151 109.5 . . ? C69 C72 H152 109.5 . . ? H151 C72 H152 109.5 . . ? C69 C72 H153 109.5 . . ? H151 C72 H153 109.5 . . ? H152 C72 H153 109.5 . . ? C78 C73 C74 109.8(3) . . ? C78 C73 P2 112.5(2) . . ? C74 C73 P2 116.6(2) . . ? C78 C73 H154 105.7 . . ? C74 C73 H154 105.7 . . ? P2 C73 H154 105.7 . . ? C75 C74 C73 110.4(3) . . ? C75 C74 H155 109.6 . . ? C73 C74 H155 109.6 . . ? C75 C74 H156 109.6 . . ? C73 C74 H156 109.6 . . ? H155 C74 H156 108.1 . . ? C76 C75 C74 112.0(3) . . ? C76 C75 H157 109.2 . . ? C74 C75 H157 109.2 . . ? C76 C75 H158 109.2 . . ? C74 C75 H158 109.2 . . ? H157 C75 H158 107.9 . . ? C75 C76 C77 110.8(3) . . ? C75 C76 H159 109.5 . . ? C77 C76 H159 109.5 . . ? C75 C76 H160 109.5 . . ? C77 C76 H160 109.5 . . ? H159 C76 H160 108.1 . . ? C76 C77 C78 112.4(3) . . ? C76 C77 H161 109.1 . . ? C78 C77 H161 109.1 . . ? C76 C77 H162 109.1 . . ? C78 C77 H162 109.1 . . ? H161 C77 H162 107.8 . . ? C73 C78 C77 111.4(3) . . ? C73 C78 H163 109.4 . . ? C77 C78 H163 109.4 . . ? C73 C78 H164 109.4 . . ? C77 C78 H164 109.4 . . ? H163 C78 H164 108.0 . . ? C84 C79 C80 108.9(3) . . ? C84 C79 P2 113.2(2) . . ? C80 C79 P2 110.3(2) . . ? C84 C79 H165 108.1 . . ? C80 C79 H165 108.1 . . ? P2 C79 H165 108.1 . . ? C81 C80 C79 111.8(3) . . ? C81 C80 H166 109.3 . . ? C79 C80 H166 109.3 . . ? C81 C80 H167 109.3 . . ? C79 C80 H167 109.3 . . ? H166 C80 H167 107.9 . . ? C82 C81 C80 111.7(3) . . ? C82 C81 H168 109.3 . . ? C80 C81 H168 109.3 . . ? C82 C81 H169 109.3 . . ? C80 C81 H169 109.3 . . ? H168 C81 H169 107.9 . . ? C83 C82 C81 111.0(3) . . ? C83 C82 H170 109.4 . . ? C81 C82 H170 109.4 . . ? C83 C82 H171 109.4 . . ? C81 C82 H171 109.4 . . ? H170 C82 H171 108.0 . . ? C82 C83 C84 111.3(3) . . ? C82 C83 H172 109.4 . . ? C84 C83 H172 109.4 . . ? C82 C83 H173 109.4 . . ? C84 C83 H173 109.4 . . ? H172 C83 H173 108.0 . . ? C83 C84 C79 111.4(3) . . ? C83 C84 H174 109.3 . . ? C79 C84 H174 109.3 . . ? C83 C84 H175 109.3 . . ? C79 C84 H175 109.3 . . ? H174 C84 H175 108.0 . . ? C90 C85 C86 109.2(3) . . ? C90 C85 P2 112.2(2) . . ? C86 C85 P2 117.1(2) . . ? C90 C85 H176 105.8 . . ? C86 C85 H176 105.8 . . ? P2 C85 H176 105.8 . . ? C87 C86 C85 110.7(3) . . ? C87 C86 H177 109.5 . . ? C85 C86 H177 109.5 . . ? C87 C86 H178 109.5 . . ? C85 C86 H178 109.5 . . ? H177 C86 H178 108.1 . . ? C88 C87 C86 112.2(3) . . ? C88 C87 H179 109.2 . . ? C86 C87 H179 109.2 . . ? C88 C87 H180 109.2 . . ? C86 C87 H180 109.2 . . ? H179 C87 H180 107.9 . . ? C87 C88 C89 111.1(3) . . ? C87 C88 H181 109.4 . . ? C89 C88 H181 109.4 . . ? C87 C88 H182 109.4 . . ? C89 C88 H182 109.4 . . ? H181 C88 H182 108.0 . . ? C88 C89 C90 111.5(3) . . ? C88 C89 H183 109.3 . . ? C90 C89 H183 109.3 . . ? C88 C89 H184 109.3 . . ? C90 C89 H184 109.3 . . ? H183 C89 H184 108.0 . . ? C85 C90 C89 111.2(3) . . ? C85 C90 H185 109.4 . . ? C89 C90 H185 109.4 . . ? C85 C90 H186 109.4 . . ? C89 C90 H186 109.4 . . ? H185 C90 H186 108.0 . . ? N2 C91 Pd2 171.5(3) . . ? C97 C92 C93 123.2(3) . . ? C97 C92 N2 118.3(3) . . ? C93 C92 N2 118.5(3) . . ? C94 C93 C92 117.2(3) . . ? C94 C93 C98 121.8(3) . . ? C92 C93 C98 121.0(3) . . ? C95 C94 C93 120.7(3) . . ? C95 C94 H187 119.7 . . ? C93 C94 H187 119.7 . . ? C96 C95 C94 121.0(3) . . ? C96 C95 H188 119.5 . . ? C94 C95 H188 119.5 . . ? C95 C96 C97 120.7(3) . . ? C95 C96 H189 119.6 . . ? C97 C96 H189 119.6 . . ? C96 C97 C92 117.2(3) . . ? C96 C97 C99 121.9(3) . . ? C92 C97 C99 120.9(3) . . ? C93 C98 H190 109.5 . . ? C93 C98 H191 109.5 . . ? H190 C98 H191 109.5 . . ? C93 C98 H192 109.5 . . ? H190 C98 H192 109.5 . . ? H191 C98 H192 109.5 . . ? C97 C99 H193 109.5 . . ? C97 C99 H194 109.5 . . ? H193 C99 H194 109.5 . . ? C97 C99 H195 109.5 . . ? H193 C99 H195 109.5 . . ? H194 C99 H195 109.5 . . ? C60 C100 H196 109.5 . . ? C60 C100 H197 109.5 . . ? H196 C100 H197 109.5 . . ? C60 C100 H198 109.5 . . ? H196 C100 H198 109.5 . . ? H197 C100 H198 109.5 . . ? C60 C101 H199 109.5 . . ? C60 C101 H200 109.5 . . ? C60 C101 H201 109.5 . . ? C60 C102 H202 109.5 . . ? C60 C102 H203 109.5 . . ? C60 C102 H204 109.5 . . ? C60 C103 H205 109.5 . . ? C60 C103 H206 109.5 . . ? C60 C103 H207 109.5 . . ? C60 C104 H208 109.5 . . ? C60 C104 H209 109.5 . . ? H208 C104 H209 109.5 . . ? C60 C104 H210 109.5 . . ? H208 C104 H210 109.5 . . ? H209 C104 H210 109.5 . . ? C60 C105 H211 109.5 . . ? C60 C105 H212 109.5 . . ? H211 C105 H212 109.5 . . ? C60 C105 H213 109.5 . . ? H211 C105 H213 109.5 . . ? H212 C105 H213 109.5 . . ? C109 Si13 C106 105.6(15) . . ? C109 Si13 C111 101.6(16) . . ? C106 Si13 C111 106.9(14) . . ? C109 Si13 Si2 117.5(12) . . ? C106 Si13 Si2 111.9(8) . . ? C111 Si13 Si2 112.4(10) . . ? C110 C106 C108 110(2) . . ? C110 C106 C107 108(2) . . ? C108 C106 C107 108(2) . . ? C110 C106 Si13 111.2(19) . . ? C108 C106 Si13 110.3(19) . . ? C107 C106 Si13 108.9(19) . . ? C106 C107 H214 109.5 . . ? C106 C107 H215 109.5 . . ? H214 C107 H215 109.5 . . ? C106 C107 H216 109.5 . . ? H214 C107 H216 109.5 . . ? H215 C107 H216 109.5 . . ? C106 C108 H217 109.5 . . ? C106 C108 H218 109.5 . . ? H217 C108 H218 109.5 . . ? C106 C108 H219 109.5 . . ? H217 C108 H219 109.5 . . ? H218 C108 H219 109.5 . . ? Si13 C109 H220 109.5 . . ? Si13 C109 H221 109.5 . . ? H220 C109 H221 109.5 . . ? Si13 C109 H222 109.5 . . ? H220 C109 H222 109.5 . . ? H221 C109 H222 109.5 . . ? C106 C110 H223 109.5 . . ? C106 C110 H224 109.5 . . ? H223 C110 H224 109.5 . . ? C106 C110 H225 109.5 . . ? H223 C110 H225 109.5 . . ? H224 C110 H225 109.5 . . ? Si13 C111 H226 109.5 . . ? Si13 C111 H227 109.5 . . ? H226 C111 H227 109.5 . . ? Si13 C111 H228 109.5 . . ? H226 C111 H228 109.5 . . ? H227 C111 H228 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.584 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.073 #===END data_(XylNC)2Ph(disilene)_complex_9 _database_code_depnum_ccdc_archive 'CCDC 282913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H78 N2 Pd Si6' _chemical_formula_weight 886.00 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' N N 0.0061 0.0033 '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 12.988(4) _cell_length_b 13.561(4) _cell_length_c 16.667(5) _cell_angle_alpha 97.695(2) _cell_angle_beta 104.615(2) _cell_angle_gamma 114.174(3) _cell_volume 2496.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 5388 _cell_measurement_theta_min 3.0267 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Organge _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9312 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method dtintegrate.ref _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18243 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10160 _reflns_number_gt 8578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0243P)^2^+3.8429P] 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 10160 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 0.53787(2) 0.81535(2) 0.771601(17) 0.02288(8) Uani 1 1 d . . . Si1 Si 0.33610(9) 0.72940(8) 0.66668(6) 0.0214(2) Uani 1 1 d . . . Si2 Si 0.36901(9) 0.65100(8) 0.77774(6) 0.0221(2) Uani 1 1 d . . . C1 C 0.6397(3) 0.9115(3) 0.7115(2) 0.0291(8) Uani 1 1 d . . . N1 N 0.7114(3) 0.9588(3) 0.6824(2) 0.0306(7) Uani 1 1 d . . . C2 C 0.6669(3) 0.8700(3) 0.8888(2) 0.0284(8) Uani 1 1 d . . . N2 N 0.7470(3) 0.9161(3) 0.95313(19) 0.0282(7) Uani 1 1 d . . . Si3 Si 0.34065(9) 0.67145(8) 0.52767(6) 0.0248(2) Uani 1 1 d . . . C3 C 0.1935(3) 0.5560(3) 0.4425(2) 0.0319(9) Uani 1 1 d . . . C4 C 0.2136(4) 0.5411(4) 0.3561(3) 0.0475(11) Uani 1 1 d . . . H1 H 0.2780 0.5219 0.3615 0.071 Uiso 1 1 calc R . . H2 H 0.2338 0.6098 0.3393 0.071 Uiso 1 1 calc R . . H3 H 0.1416 0.4822 0.3132 0.071 Uiso 1 1 calc R . . C5 C 0.0920(4) 0.5874(4) 0.4331(3) 0.0419(10) Uani 1 1 d . . . H4 H 0.0201 0.5288 0.3899 0.063 Uiso 1 1 calc R . . H5 H 0.1132 0.6562 0.4165 0.063 Uiso 1 1 calc R . . H6 H 0.0786 0.5969 0.4871 0.063 Uiso 1 1 calc R . . C6 C 0.1573(4) 0.4450(3) 0.4673(3) 0.0456(11) Uani 1 1 d . . . H7 H 0.1491 0.4552 0.5231 0.068 Uiso 1 1 calc R . . H8 H 0.2179 0.4214 0.4688 0.068 Uiso 1 1 calc R . . H9 H 0.0822 0.3890 0.4256 0.068 Uiso 1 1 calc R . . C7 C 0.4596(3) 0.6253(3) 0.5311(3) 0.0338(9) Uani 1 1 d . . . H10 H 0.4782 0.6280 0.4789 0.051 Uiso 1 1 calc R . . H11 H 0.4308 0.5500 0.5366 0.051 Uiso 1 1 calc R . . H12 H 0.5306 0.6745 0.5794 0.051 Uiso 1 1 calc R . . C8 C 0.3917(4) 0.8001(3) 0.4867(3) 0.0361(9) Uani 1 1 d . . . H13 H 0.4647 0.8590 0.5287 0.054 Uiso 1 1 calc R . . H14 H 0.3309 0.8244 0.4765 0.054 Uiso 1 1 calc R . . H15 H 0.4056 0.7826 0.4339 0.054 Uiso 1 1 calc R . . Si4 Si 0.25328(9) 0.85736(8) 0.67209(6) 0.0259(2) Uani 1 1 d . . . C9 C 0.3696(4) 1.0133(3) 0.7163(3) 0.0327(9) Uani 1 1 d . . . C10 C 0.4459(4) 1.0469(3) 0.6593(3) 0.0408(10) Uani 1 1 d . . . H16 H 0.3951 1.0335 0.6019 0.061 Uiso 1 1 calc R . . H17 H 0.4883 1.0033 0.6585 0.061 Uiso 1 1 calc R . . H18 H 0.5024 1.1252 0.6816 0.061 Uiso 1 1 calc R . . C11 C 0.3029(4) 1.0846(3) 0.7168(3) 0.0508(12) Uani 1 1 d . . . H19 H 0.3602 1.1627 0.7384 0.076 Uiso 1 1 calc R . . H20 H 0.2549 1.0649 0.7530 0.076 Uiso 1 1 calc R . . H21 H 0.2521 1.0708 0.6592 0.076 Uiso 1 1 calc R . . C12 C 0.4515(4) 1.0385(3) 0.8082(3) 0.0427(10) Uani 1 1 d . . . H22 H 0.4904 0.9916 0.8096 0.064 Uiso 1 1 calc R . . H23 H 0.4046 1.0239 0.8455 0.064 Uiso 1 1 calc R . . H24 H 0.5109 1.1159 0.8273 0.064 Uiso 1 1 calc R . . C13 C 0.1489(4) 0.8257(4) 0.7354(3) 0.0400(10) Uani 1 1 d . . . H25 H 0.1028 0.8657 0.7248 0.060 Uiso 1 1 calc R . . H26 H 0.1945 0.8486 0.7957 0.060 Uiso 1 1 calc R . . H27 H 0.0958 0.7466 0.7183 0.060 Uiso 1 1 calc R . . C14 C 0.1556(4) 0.8436(4) 0.5623(3) 0.0397(10) Uani 1 1 d . . . H28 H 0.0879 0.7702 0.5407 0.059 Uiso 1 1 calc R . . H29 H 0.2010 0.8542 0.5239 0.059 Uiso 1 1 calc R . . H30 H 0.1281 0.8992 0.5661 0.059 Uiso 1 1 calc R . . Si5 Si 0.40614(9) 0.49223(8) 0.76007(7) 0.0254(2) Uani 1 1 d . . . C15 C 0.5726(3) 0.5276(3) 0.7909(2) 0.0267(8) Uani 1 1 d . . . C16 C 0.5836(4) 0.4190(3) 0.7739(3) 0.0349(9) Uani 1 1 d . . . H31 H 0.6668 0.4368 0.7896 0.052 Uiso 1 1 calc R . . H32 H 0.5436 0.3799 0.7138 0.052 Uiso 1 1 calc R . . H33 H 0.5471 0.3723 0.8075 0.052 Uiso 1 1 calc R . . C17 C 0.6376(3) 0.5885(3) 0.8862(2) 0.0322(9) Uani 1 1 d . . . H34 H 0.7193 0.6016 0.9019 0.048 Uiso 1 1 calc R . . H35 H 0.5985 0.5434 0.9196 0.048 Uiso 1 1 calc R . . H36 H 0.6358 0.6590 0.8973 0.048 Uiso 1 1 calc R . . C18 C 0.6335(4) 0.6017(3) 0.7381(3) 0.0347(9) Uani 1 1 d . . . H37 H 0.6236 0.6683 0.7458 0.052 Uiso 1 1 calc R . . H38 H 0.5976 0.5612 0.6783 0.052 Uiso 1 1 calc R . . H39 H 0.7175 0.6221 0.7573 0.052 Uiso 1 1 calc R . . C19 C 0.3274(4) 0.3975(3) 0.6471(3) 0.0394(10) Uani 1 1 d . . . H40 H 0.3315 0.3283 0.6460 0.059 Uiso 1 1 calc R . . H41 H 0.3657 0.4336 0.6094 0.059 Uiso 1 1 calc R . . H42 H 0.2449 0.3825 0.6283 0.059 Uiso 1 1 calc R . . C20 C 0.3422(4) 0.3970(3) 0.8269(3) 0.0357(9) Uani 1 1 d . . . H43 H 0.2569 0.3699 0.8090 0.054 Uiso 1 1 calc R . . H44 H 0.3778 0.4381 0.8865 0.054 Uiso 1 1 calc R . . H45 H 0.3593 0.3347 0.8190 0.054 Uiso 1 1 calc R . . Si6 Si 0.33652(9) 0.68922(8) 0.90953(6) 0.0256(2) Uani 1 1 d . . . C21 C 0.1828(3) 0.5989(3) 0.9177(3) 0.0331(9) Uani 1 1 d . . . C22 C 0.0887(4) 0.6268(5) 0.8665(3) 0.0564(13) Uani 1 1 d . . . H46 H 0.0808 0.6101 0.8068 0.085 Uiso 1 1 calc R . . H47 H 0.1126 0.7051 0.8874 0.085 Uiso 1 1 calc R . . H48 H 0.0131 0.5829 0.8729 0.085 Uiso 1 1 calc R . . C23 C 0.1409(4) 0.4732(4) 0.8854(3) 0.0542(13) Uani 1 1 d . . . H49 H 0.1990 0.4542 0.9180 0.081 Uiso 1 1 calc R . . H50 H 0.1322 0.4549 0.8257 0.081 Uiso 1 1 calc R . . H51 H 0.0651 0.4317 0.8924 0.081 Uiso 1 1 calc R . . C24 C 0.1917(4) 0.6232(4) 1.0124(3) 0.0492(12) Uani 1 1 d . . . H52 H 0.1128 0.5883 1.0162 0.074 Uiso 1 1 calc R . . H53 H 0.2276 0.7028 1.0366 0.074 Uiso 1 1 calc R . . H54 H 0.2402 0.5939 1.0436 0.074 Uiso 1 1 calc R . . C25 C 0.4530(4) 0.6732(3) 0.9929(2) 0.0349(9) Uani 1 1 d . . . H55 H 0.5297 0.7116 0.9864 0.052 Uiso 1 1 calc R . . H56 H 0.4314 0.5951 0.9854 0.052 Uiso 1 1 calc R . . H57 H 0.4571 0.7049 1.0494 0.052 Uiso 1 1 calc R . . C26 C 0.3723(4) 0.8403(3) 0.9456(3) 0.0366(9) Uani 1 1 d . . . H58 H 0.3716 0.8567 1.0033 0.055 Uiso 1 1 calc R . . H59 H 0.3133 0.8539 0.9078 0.055 Uiso 1 1 calc R . . H60 H 0.4502 0.8875 0.9441 0.055 Uiso 1 1 calc R . . C27 C 0.8135(3) 1.0199(3) 0.6614(2) 0.0298(8) Uani 1 1 d . . . C28 C 0.8692(3) 1.1370(3) 0.6894(2) 0.0342(9) Uani 1 1 d . . . C29 C 0.9757(4) 1.1941(4) 0.6736(3) 0.0430(11) Uani 1 1 d . . . H61 H 1.0155 1.2721 0.6910 0.052 Uiso 1 1 calc R . . C30 C 1.0232(4) 1.1377(4) 0.6328(3) 0.0464(11) Uani 1 1 d . . . H62 H 1.0958 1.1776 0.6247 0.056 Uiso 1 1 calc R . . C31 C 0.9642(4) 1.0229(4) 0.6038(3) 0.0429(10) Uani 1 1 d . . . H63 H 0.9959 0.9861 0.5744 0.051 Uiso 1 1 calc R . . C32 C 0.8578(4) 0.9604(4) 0.6175(3) 0.0363(9) Uani 1 1 d . . . C33 C 0.8159(4) 1.1977(4) 0.7335(3) 0.0454(11) Uani 1 1 d . . . H64 H 0.7405 1.1843 0.6940 0.068 Uiso 1 1 calc R . . H65 H 0.8697 1.2768 0.7520 0.068 Uiso 1 1 calc R . . H66 H 0.8036 1.1710 0.7825 0.068 Uiso 1 1 calc R . . C34 C 0.7950(4) 0.8353(4) 0.5872(3) 0.0517(12) Uani 1 1 d . . . H67 H 0.7184 0.8107 0.5439 0.078 Uiso 1 1 calc R . . H68 H 0.7834 0.8048 0.6348 0.078 Uiso 1 1 calc R . . H69 H 0.8426 0.8099 0.5633 0.078 Uiso 1 1 calc R . . C35 C 0.8522(3) 0.9873(3) 1.0226(2) 0.0269(8) Uani 1 1 d . . . C36 C 0.9208(3) 1.0941(3) 1.0171(2) 0.0304(8) Uani 1 1 d . . . C37 C 1.0261(4) 1.1631(3) 1.0858(3) 0.0382(10) Uani 1 1 d . . . H70 H 1.0741 1.2354 1.0844 0.046 Uiso 1 1 calc R . . C38 C 1.0606(4) 1.1260(4) 1.1558(3) 0.0422(10) Uani 1 1 d . . . H71 H 1.1315 1.1735 1.2011 0.051 Uiso 1 1 calc R . . C39 C 0.9909(3) 1.0192(4) 1.1591(2) 0.0364(9) Uani 1 1 d . . . H72 H 1.0150 0.9952 1.2069 0.044 Uiso 1 1 calc R . . C40 C 0.8850(3) 0.9465(3) 1.0921(2) 0.0306(8) Uani 1 1 d . . . C41 C 0.8821(4) 1.1327(3) 0.9400(3) 0.0403(10) Uani 1 1 d . . . H73 H 0.8768 1.0850 0.8894 0.060 Uiso 1 1 calc R . . H74 H 0.9398 1.2086 0.9475 0.060 Uiso 1 1 calc R . . H75 H 0.8051 1.1293 0.9336 0.060 Uiso 1 1 calc R . . C42 C 0.8111(4) 0.8286(4) 1.0941(3) 0.0474(11) Uani 1 1 d . . . H76 H 0.8469 0.8170 1.1475 0.071 Uiso 1 1 calc R . . H77 H 0.8078 0.7768 1.0470 0.071 Uiso 1 1 calc R . . H78 H 0.7313 0.8167 1.0890 0.071 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 0.02207(15) 0.02077(14) 0.02333(14) 0.00651(11) 0.00722(11) 0.00773(12) Si1 0.0231(5) 0.0207(5) 0.0207(5) 0.0053(4) 0.0075(4) 0.0105(4) Si2 0.0234(5) 0.0199(5) 0.0234(5) 0.0070(4) 0.0093(4) 0.0093(4) C1 0.030(2) 0.028(2) 0.0246(19) 0.0067(16) 0.0069(16) 0.0111(17) N1 0.0262(17) 0.0355(18) 0.0312(17) 0.0164(15) 0.0119(14) 0.0118(15) C2 0.029(2) 0.0264(19) 0.034(2) 0.0126(16) 0.0155(18) 0.0122(17) N2 0.0235(17) 0.0283(16) 0.0267(17) 0.0062(13) 0.0041(14) 0.0093(14) Si3 0.0258(5) 0.0257(5) 0.0216(5) 0.0046(4) 0.0086(4) 0.0111(4) C3 0.030(2) 0.034(2) 0.0267(19) 0.0010(16) 0.0063(16) 0.0136(18) C4 0.054(3) 0.058(3) 0.025(2) -0.003(2) 0.011(2) 0.027(2) C5 0.032(2) 0.046(3) 0.039(2) 0.003(2) 0.0054(19) 0.017(2) C6 0.033(2) 0.030(2) 0.055(3) -0.001(2) 0.004(2) 0.0071(19) C7 0.032(2) 0.037(2) 0.035(2) 0.0109(18) 0.0132(18) 0.0168(19) C8 0.041(2) 0.037(2) 0.032(2) 0.0145(18) 0.0153(18) 0.017(2) Si4 0.0278(6) 0.0252(5) 0.0261(5) 0.0059(4) 0.0078(4) 0.0148(5) C9 0.038(2) 0.027(2) 0.040(2) 0.0076(17) 0.0164(18) 0.0194(18) C10 0.042(3) 0.029(2) 0.051(3) 0.0136(19) 0.017(2) 0.013(2) C11 0.049(3) 0.029(2) 0.077(3) 0.007(2) 0.019(3) 0.024(2) C12 0.048(3) 0.029(2) 0.036(2) -0.0013(18) 0.003(2) 0.013(2) C13 0.037(2) 0.041(2) 0.042(2) 0.008(2) 0.015(2) 0.019(2) C14 0.047(3) 0.043(2) 0.035(2) 0.0083(19) 0.0081(19) 0.030(2) Si5 0.0270(5) 0.0188(5) 0.0303(5) 0.0082(4) 0.0119(4) 0.0090(4) C15 0.031(2) 0.0246(18) 0.0297(19) 0.0092(15) 0.0129(16) 0.0154(17) C16 0.039(2) 0.027(2) 0.047(2) 0.0131(18) 0.019(2) 0.0188(19) C17 0.030(2) 0.031(2) 0.038(2) 0.0113(17) 0.0132(18) 0.0148(18) C18 0.034(2) 0.031(2) 0.044(2) 0.0112(18) 0.0180(19) 0.0162(18) C19 0.044(3) 0.028(2) 0.042(2) 0.0080(18) 0.015(2) 0.013(2) C20 0.042(2) 0.028(2) 0.046(2) 0.0173(18) 0.023(2) 0.0167(19) Si6 0.0270(5) 0.0256(5) 0.0232(5) 0.0073(4) 0.0103(4) 0.0099(4) C21 0.029(2) 0.039(2) 0.034(2) 0.0110(18) 0.0162(17) 0.0136(18) C22 0.036(3) 0.072(4) 0.065(3) 0.030(3) 0.022(2) 0.023(3) C23 0.046(3) 0.040(3) 0.073(3) 0.009(2) 0.036(3) 0.009(2) C24 0.052(3) 0.054(3) 0.052(3) 0.017(2) 0.033(2) 0.024(2) C25 0.036(2) 0.040(2) 0.029(2) 0.0114(18) 0.0125(18) 0.0165(19) C26 0.041(2) 0.032(2) 0.032(2) 0.0051(17) 0.0119(18) 0.0139(19) C27 0.0223(19) 0.035(2) 0.0273(19) 0.0163(17) 0.0049(15) 0.0092(17) C28 0.028(2) 0.038(2) 0.029(2) 0.0160(18) 0.0013(16) 0.0104(18) C29 0.028(2) 0.038(2) 0.044(3) 0.022(2) -0.0004(19) 0.0019(19) C30 0.026(2) 0.058(3) 0.053(3) 0.028(2) 0.015(2) 0.013(2) C31 0.032(2) 0.058(3) 0.042(2) 0.020(2) 0.016(2) 0.020(2) C32 0.033(2) 0.041(2) 0.032(2) 0.0130(18) 0.0115(18) 0.0126(19) C33 0.049(3) 0.037(2) 0.046(3) 0.013(2) 0.007(2) 0.021(2) C34 0.051(3) 0.044(3) 0.058(3) 0.007(2) 0.027(2) 0.017(2) C35 0.0232(19) 0.0291(19) 0.0263(19) 0.0033(15) 0.0076(15) 0.0118(16) C36 0.030(2) 0.027(2) 0.038(2) 0.0078(17) 0.0136(17) 0.0160(17) C37 0.028(2) 0.027(2) 0.049(3) 0.0043(19) 0.0132(19) 0.0052(18) C38 0.024(2) 0.040(2) 0.041(2) -0.007(2) 0.0014(18) 0.0068(19) C39 0.029(2) 0.047(2) 0.025(2) 0.0008(18) 0.0003(16) 0.017(2) C40 0.027(2) 0.032(2) 0.028(2) 0.0065(16) 0.0077(16) 0.0112(17) C41 0.045(3) 0.032(2) 0.048(3) 0.0176(19) 0.018(2) 0.018(2) C42 0.050(3) 0.044(3) 0.034(2) 0.015(2) 0.005(2) 0.013(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 C1 2.014(4) . ? Pd1 C2 2.029(4) . ? Pd1 Si1 2.4340(11) . ? Pd1 Si2 2.4411(11) . ? Si1 Si2 2.2891(14) . ? Si1 Si3 2.3681(15) . ? Si1 Si4 2.3900(14) . ? Si2 Si6 2.3694(15) . ? Si2 Si5 2.3891(15) . ? C1 N1 1.157(5) . ? N1 C27 1.408(5) . ? C2 N2 1.161(5) . ? N2 C35 1.400(5) . ? Si3 C7 1.881(4) . ? Si3 C8 1.885(4) . ? Si3 C3 1.925(4) . ? C3 C5 1.522(5) . ? C3 C4 1.529(5) . ? C3 C6 1.531(6) . ? C4 H1 0.9600 . ? C4 H2 0.9600 . ? C4 H3 0.9600 . ? C5 H4 0.9600 . ? C5 H5 0.9600 . ? C5 H6 0.9600 . ? C6 H7 0.9600 . ? C6 H8 0.9600 . ? C6 H9 0.9600 . ? C7 H10 0.9600 . ? C7 H11 0.9600 . ? C7 H12 0.9600 . ? C8 H13 0.9600 . ? C8 H14 0.9600 . ? C8 H15 0.9600 . ? Si4 C13 1.872(4) . ? Si4 C14 1.881(4) . ? Si4 C9 1.924(4) . ? C9 C10 1.521(5) . ? C9 C12 1.528(5) . ? C9 C11 1.541(5) . ? C10 H16 0.9600 . ? C10 H17 0.9600 . ? C10 H18 0.9600 . ? C11 H19 0.9600 . ? C11 H20 0.9600 . ? C11 H21 0.9600 . ? C12 H22 0.9600 . ? C12 H23 0.9600 . ? C12 H24 0.9600 . ? C13 H25 0.9600 . ? C13 H26 0.9600 . ? C13 H27 0.9600 . ? C14 H28 0.9600 . ? C14 H29 0.9600 . ? C14 H30 0.9600 . ? Si5 C19 1.883(4) . ? Si5 C20 1.890(4) . ? Si5 C15 1.922(4) . ? C15 C17 1.524(5) . ? C15 C18 1.531(5) . ? C15 C16 1.533(5) . ? C16 H31 0.9600 . ? C16 H32 0.9600 . ? C16 H33 0.9600 . ? C17 H34 0.9600 . ? C17 H35 0.9600 . ? C17 H36 0.9600 . ? C18 H37 0.9600 . ? C18 H38 0.9600 . ? C18 H39 0.9600 . ? C19 H40 0.9600 . ? C19 H41 0.9600 . ? C19 H42 0.9600 . ? C20 H43 0.9600 . ? C20 H44 0.9600 . ? C20 H45 0.9600 . ? Si6 C26 1.877(4) . ? Si6 C25 1.886(4) . ? Si6 C21 1.919(4) . ? C21 C22 1.519(6) . ? C21 C23 1.528(6) . ? C21 C24 1.534(6) . ? C22 H46 0.9600 . ? C22 H47 0.9600 . ? C22 H48 0.9600 . ? C23 H49 0.9600 . ? C23 H50 0.9600 . ? C23 H51 0.9600 . ? C24 H52 0.9600 . ? C24 H53 0.9600 . ? C24 H54 0.9600 . ? C25 H55 0.9600 . ? C25 H56 0.9600 . ? C25 H57 0.9600 . ? C26 H58 0.9600 . ? C26 H59 0.9600 . ? C26 H60 0.9600 . ? C27 C32 1.397(6) . ? C27 C28 1.397(5) . ? C28 C29 1.395(6) . ? C28 C33 1.502(6) . ? C29 C30 1.374(6) . ? C29 H61 0.9300 . ? C30 C31 1.370(6) . ? C30 H62 0.9300 . ? C31 C32 1.389(6) . ? C31 H63 0.9300 . ? C32 C34 1.492(6) . ? C33 H64 0.9600 . ? C33 H65 0.9600 . ? C33 H66 0.9600 . ? C34 H67 0.9600 . ? C34 H68 0.9600 . ? C34 H69 0.9600 . ? C35 C36 1.386(5) . ? C35 C40 1.394(5) . ? C36 C37 1.390(5) . ? C36 C41 1.500(5) . ? C37 C38 1.376(6) . ? C37 H70 0.9300 . ? C38 C39 1.377(6) . ? C38 H71 0.9300 . ? C39 C40 1.390(5) . ? C39 H72 0.9300 . ? C40 C42 1.500(6) . ? C41 H73 0.9600 . ? C41 H74 0.9600 . ? C41 H75 0.9600 . ? C42 H76 0.9600 . ? C42 H77 0.9600 . ? C42 H78 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C2 97.59(15) . . ? C1 Pd1 Si1 103.36(11) . . ? C2 Pd1 Si1 157.63(11) . . ? C1 Pd1 Si2 154.45(11) . . ? C2 Pd1 Si2 105.48(11) . . ? Si1 Pd1 Si2 56.01(4) . . ? Si2 Si1 Si3 125.88(5) . . ? Si2 Si1 Si4 121.20(5) . . ? Si3 Si1 Si4 111.86(5) . . ? Si2 Si1 Pd1 62.15(4) . . ? Si3 Si1 Pd1 109.73(5) . . ? Si4 Si1 Pd1 110.04(5) . . ? Si1 Si2 Si6 126.22(6) . . ? Si1 Si2 Si5 121.23(5) . . ? Si6 Si2 Si5 111.62(5) . . ? Si1 Si2 Pd1 61.84(4) . . ? Si6 Si2 Pd1 109.71(5) . . ? Si5 Si2 Pd1 109.88(5) . . ? N1 C1 Pd1 167.9(3) . . ? C1 N1 C27 169.8(4) . . ? N2 C2 Pd1 170.1(3) . . ? C2 N2 C35 169.1(4) . . ? C7 Si3 C8 103.93(18) . . ? C7 Si3 C3 107.36(18) . . ? C8 Si3 C3 108.34(18) . . ? C7 Si3 Si1 112.14(13) . . ? C8 Si3 Si1 106.79(13) . . ? C3 Si3 Si1 117.40(13) . . ? C5 C3 C4 108.8(3) . . ? C5 C3 C6 108.8(3) . . ? C4 C3 C6 109.2(3) . . ? C5 C3 Si3 111.3(3) . . ? C4 C3 Si3 108.4(3) . . ? C6 C3 Si3 110.2(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? Si3 C7 H10 109.5 . . ? Si3 C7 H11 109.5 . . ? H10 C7 H11 109.5 . . ? Si3 C7 H12 109.5 . . ? H10 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si3 C8 H13 109.5 . . ? Si3 C8 H14 109.5 . . ? H13 C8 H14 109.5 . . ? Si3 C8 H15 109.5 . . ? H13 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? C13 Si4 C14 103.6(2) . . ? C13 Si4 C9 108.53(18) . . ? C14 Si4 C9 105.68(19) . . ? C13 Si4 Si1 111.79(14) . . ? C14 Si4 Si1 111.58(13) . . ? C9 Si4 Si1 114.91(12) . . ? C10 C9 C12 109.1(3) . . ? C10 C9 C11 108.4(3) . . ? C12 C9 C11 108.4(3) . . ? C10 C9 Si4 110.5(3) . . ? C12 C9 Si4 111.5(3) . . ? C11 C9 Si4 108.8(3) . . ? C9 C10 H16 109.5 . . ? C9 C10 H17 109.5 . . ? H16 C10 H17 109.5 . . ? C9 C10 H18 109.5 . . ? H16 C10 H18 109.5 . . ? H17 C10 H18 109.5 . . ? C9 C11 H19 109.5 . . ? C9 C11 H20 109.5 . . ? H19 C11 H20 109.5 . . ? C9 C11 H21 109.5 . . ? H19 C11 H21 109.5 . . ? H20 C11 H21 109.5 . . ? C9 C12 H22 109.5 . . ? C9 C12 H23 109.5 . . ? H22 C12 H23 109.5 . . ? C9 C12 H24 109.5 . . ? H22 C12 H24 109.5 . . ? H23 C12 H24 109.5 . . ? Si4 C13 H25 109.5 . . ? Si4 C13 H26 109.5 . . ? H25 C13 H26 109.5 . . ? Si4 C13 H27 109.5 . . ? H25 C13 H27 109.5 . . ? H26 C13 H27 109.5 . . ? Si4 C14 H28 109.5 . . ? Si4 C14 H29 109.5 . . ? H28 C14 H29 109.5 . . ? Si4 C14 H30 109.5 . . ? H28 C14 H30 109.5 . . ? H29 C14 H30 109.5 . . ? C19 Si5 C20 103.12(19) . . ? C19 Si5 C15 107.47(18) . . ? C20 Si5 C15 106.32(17) . . ? C19 Si5 Si2 112.73(14) . . ? C20 Si5 Si2 111.40(13) . . ? C15 Si5 Si2 114.94(12) . . ? C17 C15 C18 109.0(3) . . ? C17 C15 C16 108.5(3) . . ? C18 C15 C16 108.6(3) . . ? C17 C15 Si5 110.0(2) . . ? C18 C15 Si5 111.1(3) . . ? C16 C15 Si5 109.6(3) . . ? C15 C16 H31 109.5 . . ? C15 C16 H32 109.5 . . ? H31 C16 H32 109.5 . . ? C15 C16 H33 109.5 . . ? H31 C16 H33 109.5 . . ? H32 C16 H33 109.5 . . ? C15 C17 H34 109.5 . . ? C15 C17 H35 109.5 . . ? H34 C17 H35 109.5 . . ? C15 C17 H36 109.5 . . ? H34 C17 H36 109.5 . . ? H35 C17 H36 109.5 . . ? C15 C18 H37 109.5 . . ? C15 C18 H38 109.5 . . ? H37 C18 H38 109.5 . . ? C15 C18 H39 109.5 . . ? H37 C18 H39 109.5 . . ? H38 C18 H39 109.5 . . ? Si5 C19 H40 109.5 . . ? Si5 C19 H41 109.5 . . ? H40 C19 H41 109.5 . . ? Si5 C19 H42 109.5 . . ? H40 C19 H42 109.5 . . ? H41 C19 H42 109.5 . . ? Si5 C20 H43 109.5 . . ? Si5 C20 H44 109.5 . . ? H43 C20 H44 109.5 . . ? Si5 C20 H45 109.5 . . ? H43 C20 H45 109.5 . . ? H44 C20 H45 109.5 . . ? C26 Si6 C25 104.57(19) . . ? C26 Si6 C21 107.77(18) . . ? C25 Si6 C21 107.76(18) . . ? C26 Si6 Si2 111.13(13) . . ? C25 Si6 Si2 105.86(13) . . ? C21 Si6 Si2 118.78(13) . . ? C22 C21 C23 108.6(4) . . ? C22 C21 C24 108.7(4) . . ? C23 C21 C24 107.5(4) . . ? C22 C21 Si6 110.5(3) . . ? C23 C21 Si6 112.6(3) . . ? C24 C21 Si6 108.8(3) . . ? C21 C22 H46 109.5 . . ? C21 C22 H47 109.5 . . ? H46 C22 H47 109.5 . . ? C21 C22 H48 109.5 . . ? H46 C22 H48 109.5 . . ? H47 C22 H48 109.5 . . ? C21 C23 H49 109.5 . . ? C21 C23 H50 109.5 . . ? H49 C23 H50 109.5 . . ? C21 C23 H51 109.5 . . ? H49 C23 H51 109.5 . . ? H50 C23 H51 109.5 . . ? C21 C24 H52 109.5 . . ? C21 C24 H53 109.5 . . ? H52 C24 H53 109.5 . . ? C21 C24 H54 109.5 . . ? H52 C24 H54 109.5 . . ? H53 C24 H54 109.5 . . ? Si6 C25 H55 109.5 . . ? Si6 C25 H56 109.5 . . ? H55 C25 H56 109.5 . . ? Si6 C25 H57 109.5 . . ? H55 C25 H57 109.5 . . ? H56 C25 H57 109.5 . . ? Si6 C26 H58 109.5 . . ? Si6 C26 H59 109.5 . . ? H58 C26 H59 109.5 . . ? Si6 C26 H60 109.5 . . ? H58 C26 H60 109.5 . . ? H59 C26 H60 109.5 . . ? C32 C27 C28 123.3(4) . . ? C32 C27 N1 118.3(3) . . ? C28 C27 N1 118.3(4) . . ? C29 C28 C27 116.5(4) . . ? C29 C28 C33 121.9(4) . . ? C27 C28 C33 121.5(4) . . ? C30 C29 C28 121.4(4) . . ? C30 C29 H61 119.3 . . ? C28 C29 H61 119.3 . . ? C31 C30 C29 120.3(4) . . ? C31 C30 H62 119.8 . . ? C29 C30 H62 119.8 . . ? C30 C31 C32 121.4(4) . . ? C30 C31 H63 119.3 . . ? C32 C31 H63 119.3 . . ? C31 C32 C27 117.0(4) . . ? C31 C32 C34 121.2(4) . . ? C27 C32 C34 121.8(4) . . ? C28 C33 H64 109.5 . . ? C28 C33 H65 109.5 . . ? H64 C33 H65 109.5 . . ? C28 C33 H66 109.5 . . ? H64 C33 H66 109.5 . . ? H65 C33 H66 109.5 . . ? C32 C34 H67 109.5 . . ? C32 C34 H68 109.5 . . ? H67 C34 H68 109.5 . . ? C32 C34 H69 109.5 . . ? H67 C34 H69 109.5 . . ? H68 C34 H69 109.5 . . ? C36 C35 C40 123.3(3) . . ? C36 C35 N2 117.8(3) . . ? C40 C35 N2 118.9(3) . . ? C35 C36 C37 117.2(4) . . ? C35 C36 C41 121.0(4) . . ? C37 C36 C41 121.8(4) . . ? C38 C37 C36 121.1(4) . . ? C38 C37 H70 119.4 . . ? C36 C37 H70 119.4 . . ? C37 C38 C39 120.3(4) . . ? C37 C38 H71 119.8 . . ? C39 C38 H71 119.8 . . ? C38 C39 C40 121.0(4) . . ? C38 C39 H72 119.5 . . ? C40 C39 H72 119.5 . . ? C39 C40 C35 117.1(4) . . ? C39 C40 C42 121.1(4) . . ? C35 C40 C42 121.8(3) . . ? C36 C41 H73 109.5 . . ? C36 C41 H74 109.5 . . ? H73 C41 H74 109.5 . . ? C36 C41 H75 109.5 . . ? H73 C41 H75 109.5 . . ? H74 C41 H75 109.5 . . ? C40 C42 H76 109.5 . . ? C40 C42 H77 109.5 . . ? H76 C42 H77 109.5 . . ? C40 C42 H78 109.5 . . ? H76 C42 H78 109.5 . . ? H77 C42 H78 109.5 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.817 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.091 #===END data_(PhMe2P)2Ph(disilene)_complex_13 _database_code_depnum_ccdc_archive 'CCDC 282914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H82 P2 Pd Si6' _chemical_formula_weight 899.94 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.326(3) _cell_length_b 11.988(3) _cell_length_c 19.426(5) _cell_angle_alpha 93.507(3) _cell_angle_beta 94.393(3) _cell_angle_gamma 100.588(4) _cell_volume 2577.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173.1500 _cell_measurement_reflns_used 6916 _cell_measurement_theta_min 3.0539 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9439 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.1500 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method dtintegrate.ref _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19373 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10555 _reflns_number_gt 8754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0148P)^2^+3.1594P] 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 10555 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.81298(2) 0.44787(2) 0.230650(12) 0.01895(7) Uani 1 1 d . . . P1 P 0.90231(8) 0.47317(8) 0.12563(4) 0.0258(2) Uani 1 1 d . . . P2 P 0.88547(8) 0.62690(7) 0.29105(5) 0.0245(2) Uani 1 1 d . . . Si1 Si 0.73222(8) 0.31756(8) 0.31625(4) 0.01912(19) Uani 1 1 d . . . Si2 Si 0.66217(8) 0.27592(7) 0.20182(4) 0.01911(19) Uani 1 1 d . . . Si3 Si 0.60809(9) 0.34727(9) 0.40634(5) 0.0263(2) Uani 1 1 d . . . Si4 Si 0.92353(8) 0.27933(8) 0.35988(5) 0.0235(2) Uani 1 1 d . . . Si5 Si 0.68579(9) 0.10278(8) 0.14358(5) 0.0276(2) Uani 1 1 d . . . Si6 Si 0.48137(8) 0.33268(8) 0.15523(5) 0.0253(2) Uani 1 1 d . . . C1 C 0.5130(3) 0.4572(3) 0.38999(19) 0.0392(10) Uani 1 1 d . . . H1 H 0.4719 0.4705 0.4303 0.059 Uiso 1 1 calc R . . H2 H 0.4549 0.4306 0.3512 0.059 Uiso 1 1 calc R . . H3 H 0.5636 0.5269 0.3802 0.059 Uiso 1 1 calc R . . C2 C 0.7046(3) 0.3995(3) 0.48966(17) 0.0363(9) Uani 1 1 d . . . H4 H 0.7566 0.4703 0.4836 0.054 Uiso 1 1 calc R . . H5 H 0.7525 0.3442 0.5019 0.054 Uiso 1 1 calc R . . H6 H 0.6538 0.4104 0.5259 0.054 Uiso 1 1 calc R . . C3 C 0.4976(3) 0.2121(3) 0.42313(19) 0.0366(9) Uani 1 1 d . . . C4 C 0.5628(4) 0.1142(4) 0.4376(2) 0.0563(13) Uani 1 1 d . . . H7 H 0.5046 0.0461 0.4412 0.084 Uiso 1 1 calc R . . H8 H 0.6134 0.1325 0.4803 0.084 Uiso 1 1 calc R . . H9 H 0.6115 0.1023 0.4005 0.084 Uiso 1 1 calc R . . C5 C 0.4278(4) 0.2350(4) 0.4860(2) 0.0598(13) Uani 1 1 d . . . H10 H 0.3833 0.2942 0.4770 0.090 Uiso 1 1 calc R . . H11 H 0.4836 0.2581 0.5262 0.090 Uiso 1 1 calc R . . H12 H 0.3729 0.1668 0.4939 0.090 Uiso 1 1 calc R . . C6 C 0.4066(4) 0.1748(4) 0.3603(2) 0.0510(12) Uani 1 1 d . . . H13 H 0.4485 0.1604 0.3205 0.076 Uiso 1 1 calc R . . H14 H 0.3616 0.2338 0.3519 0.076 Uiso 1 1 calc R . . H15 H 0.3525 0.1066 0.3690 0.076 Uiso 1 1 calc R . . C7 C 0.9944(3) 0.4071(3) 0.42041(17) 0.0314(8) Uani 1 1 d . . . H16 H 1.0761 0.4021 0.4347 0.047 Uiso 1 1 calc R . . H17 H 0.9496 0.4091 0.4603 0.047 Uiso 1 1 calc R . . H18 H 0.9935 0.4752 0.3970 0.047 Uiso 1 1 calc R . . C8 C 1.0239(3) 0.2767(3) 0.28720(18) 0.0340(9) Uani 1 1 d . . . H19 H 0.9985 0.3210 0.2513 0.051 Uiso 1 1 calc R . . H20 H 1.0187 0.1996 0.2688 0.051 Uiso 1 1 calc R . . H21 H 1.1058 0.3082 0.3044 0.051 Uiso 1 1 calc R . . C9 C 0.9427(3) 0.1509(3) 0.41143(18) 0.0322(9) Uani 1 1 d . . . C10 C 0.8774(4) 0.0375(3) 0.3737(2) 0.0462(11) Uani 1 1 d . . . H22 H 0.8913 -0.0241 0.4007 0.069 Uiso 1 1 calc R . . H23 H 0.9075 0.0284 0.3293 0.069 Uiso 1 1 calc R . . H24 H 0.7924 0.0372 0.3676 0.069 Uiso 1 1 calc R . . C11 C 0.8969(4) 0.1622(3) 0.48356(19) 0.0458(11) Uani 1 1 d . . . H25 H 0.9058 0.0963 0.5077 0.069 Uiso 1 1 calc R . . H26 H 0.8133 0.1682 0.4787 0.069 Uiso 1 1 calc R . . H27 H 0.9429 0.2291 0.5093 0.069 Uiso 1 1 calc R . . C12 C 1.0783(4) 0.1484(4) 0.4210(2) 0.0548(12) Uani 1 1 d . . . H28 H 1.1212 0.2201 0.4426 0.082 Uiso 1 1 calc R . . H29 H 1.1073 0.1350 0.3767 0.082 Uiso 1 1 calc R . . H30 H 1.0911 0.0886 0.4498 0.082 Uiso 1 1 calc R . . C13 C 0.6623(4) 0.0951(3) 0.04587(18) 0.0430(10) Uani 1 1 d . . . H31 H 0.7046 0.1639 0.0295 0.064 Uiso 1 1 calc R . . H32 H 0.5778 0.0860 0.0318 0.064 Uiso 1 1 calc R . . H33 H 0.6926 0.0313 0.0267 0.064 Uiso 1 1 calc R . . C14 C 0.8417(4) 0.0737(4) 0.1624(2) 0.0480(11) Uani 1 1 d . . . H34 H 0.8471 0.0017 0.1396 0.072 Uiso 1 1 calc R . . H35 H 0.8585 0.0717 0.2115 0.072 Uiso 1 1 calc R . . H36 H 0.8992 0.1328 0.1458 0.072 Uiso 1 1 calc R . . C15 C 0.5748(3) -0.0233(3) 0.17185(18) 0.0324(9) Uani 1 1 d . . . C16 C 0.6052(4) -0.0414(3) 0.24796(19) 0.0460(11) Uani 1 1 d . . . H37 H 0.6029 0.0268 0.2761 0.069 Uiso 1 1 calc R . . H38 H 0.6845 -0.0592 0.2538 0.069 Uiso 1 1 calc R . . H39 H 0.5474 -0.1031 0.2618 0.069 Uiso 1 1 calc R . . C17 C 0.5828(4) -0.1324(3) 0.1280(2) 0.0519(12) Uani 1 1 d . . . H40 H 0.6648 -0.1435 0.1309 0.078 Uiso 1 1 calc R . . H41 H 0.5561 -0.1254 0.0806 0.078 Uiso 1 1 calc R . . H42 H 0.5324 -0.1963 0.1450 0.078 Uiso 1 1 calc R . . C18 C 0.4449(4) -0.0040(3) 0.1629(2) 0.0497(11) Uani 1 1 d . . . H43 H 0.3916 -0.0684 0.1774 0.075 Uiso 1 1 calc R . . H44 H 0.4235 0.0051 0.1150 0.075 Uiso 1 1 calc R . . H45 H 0.4380 0.0633 0.1905 0.075 Uiso 1 1 calc R . . C19 C 0.3404(3) 0.2836(3) 0.1990(2) 0.0433(10) Uani 1 1 d . . . H46 H 0.2720 0.2993 0.1716 0.065 Uiso 1 1 calc R . . H47 H 0.3469 0.3232 0.2440 0.065 Uiso 1 1 calc R . . H48 H 0.3304 0.2032 0.2037 0.065 Uiso 1 1 calc R . . C20 C 0.4467(4) 0.2695(3) 0.06291(19) 0.0418(10) Uani 1 1 d . . . H49 H 0.4252 0.1882 0.0625 0.063 Uiso 1 1 calc R . . H50 H 0.5166 0.2895 0.0379 0.063 Uiso 1 1 calc R . . H51 H 0.3809 0.2988 0.0413 0.063 Uiso 1 1 calc R . . C21 C 0.4930(3) 0.4939(3) 0.15111(17) 0.0254(8) Uani 1 1 d . . . C22 C 0.3728(3) 0.5201(4) 0.1207(2) 0.0447(10) Uani 1 1 d . . . H52 H 0.3109 0.4951 0.1505 0.067 Uiso 1 1 calc R . . H53 H 0.3516 0.4809 0.0756 0.067 Uiso 1 1 calc R . . H54 H 0.3807 0.6005 0.1170 0.067 Uiso 1 1 calc R . . C23 C 0.5912(3) 0.5419(3) 0.10517(18) 0.0320(8) Uani 1 1 d . . . H55 H 0.5918 0.6215 0.1013 0.048 Uiso 1 1 calc R . . H56 H 0.5751 0.5022 0.0600 0.048 Uiso 1 1 calc R . . H57 H 0.6683 0.5321 0.1254 0.048 Uiso 1 1 calc R . . C24 C 0.5220(3) 0.5556(3) 0.22350(18) 0.0364(9) Uani 1 1 d . . . H58 H 0.5274 0.6359 0.2202 0.055 Uiso 1 1 calc R . . H59 H 0.5976 0.5415 0.2435 0.055 Uiso 1 1 calc R . . H60 H 0.4594 0.5281 0.2522 0.055 Uiso 1 1 calc R . . C25 C 0.8342(3) 0.6587(3) 0.37615(18) 0.0382(9) Uani 1 1 d . . . H61 H 0.8614 0.6095 0.4086 0.057 Uiso 1 1 calc R . . H62 H 0.7477 0.6467 0.3725 0.057 Uiso 1 1 calc R . . H63 H 0.8667 0.7366 0.3919 0.057 Uiso 1 1 calc R . . C26 C 0.8349(3) 0.7396(3) 0.24418(19) 0.0371(9) Uani 1 1 d . . . H64 H 0.8563 0.8103 0.2721 0.056 Uiso 1 1 calc R . . H65 H 0.7489 0.7212 0.2341 0.056 Uiso 1 1 calc R . . H66 H 0.8727 0.7464 0.2017 0.056 Uiso 1 1 calc R . . C27 C 1.0485(3) 0.6788(3) 0.30709(17) 0.0285(8) Uani 1 1 d . . . C28 C 1.0986(4) 0.7923(4) 0.3232(2) 0.0546(12) Uani 1 1 d . . . H67 H 1.0487 0.8456 0.3263 0.066 Uiso 1 1 calc R . . C29 C 1.2222(5) 0.8276(5) 0.3347(3) 0.0786(17) Uani 1 1 d . . . H68 H 1.2546 0.9044 0.3453 0.094 Uiso 1 1 calc R . . C30 C 1.2968(4) 0.7509(6) 0.3308(3) 0.0739(18) Uani 1 1 d . . . H69 H 1.3798 0.7752 0.3386 0.089 Uiso 1 1 calc R . . C31 C 1.2493(4) 0.6380(5) 0.3153(2) 0.0563(13) Uani 1 1 d . . . H70 H 1.3001 0.5855 0.3128 0.068 Uiso 1 1 calc R . . C32 C 1.1254(3) 0.6018(4) 0.30336(18) 0.0378(9) Uani 1 1 d . . . H71 H 1.0937 0.5249 0.2927 0.045 Uiso 1 1 calc R . . C33 C 1.0413(3) 0.4162(4) 0.1270(2) 0.0426(10) Uani 1 1 d . . . H72 H 1.0800 0.4336 0.0856 0.064 Uiso 1 1 calc R . . H73 H 1.0226 0.3352 0.1293 0.064 Uiso 1 1 calc R . . H74 H 1.0943 0.4500 0.1667 0.064 Uiso 1 1 calc R . . C34 C 0.8259(3) 0.3993(3) 0.04502(17) 0.0371(9) Uani 1 1 d . . . H75 H 0.7499 0.4225 0.0359 0.056 Uiso 1 1 calc R . . H76 H 0.8126 0.3186 0.0491 0.056 Uiso 1 1 calc R . . H77 H 0.8751 0.4179 0.0077 0.056 Uiso 1 1 calc R . . C35 C 0.9534(3) 0.6169(3) 0.09927(17) 0.0305(8) Uani 1 1 d . . . C36 C 0.8794(4) 0.6683(3) 0.05542(19) 0.0390(10) Uani 1 1 d . . . H78 H 0.8046 0.6272 0.0372 0.047 Uiso 1 1 calc R . . C37 C 0.9152(5) 0.7784(4) 0.0387(2) 0.0557(12) Uani 1 1 d . . . H79 H 0.8647 0.8110 0.0092 0.067 Uiso 1 1 calc R . . C38 C 1.0253(5) 0.8407(4) 0.0653(3) 0.0630(14) Uani 1 1 d . . . H80 H 1.0493 0.9152 0.0539 0.076 Uiso 1 1 calc R . . C39 C 1.0996(4) 0.7924(4) 0.1086(2) 0.0581(13) Uani 1 1 d . . . H81 H 1.1741 0.8344 0.1265 0.070 Uiso 1 1 calc R . . C40 C 1.0642(4) 0.6816(4) 0.12574(19) 0.0429(10) Uani 1 1 d . . . H82 H 1.1152 0.6500 0.1554 0.051 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 0.01873(13) 0.01853(13) 0.01888(14) 0.00045(10) 0.00083(10) 0.00233(10) P1 0.0237(5) 0.0312(5) 0.0226(5) 0.0034(4) 0.0054(4) 0.0039(4) P2 0.0252(5) 0.0202(5) 0.0267(5) -0.0023(4) -0.0002(4) 0.0027(4) Si1 0.0210(5) 0.0194(5) 0.0168(5) 0.0006(3) 0.0009(4) 0.0040(4) Si2 0.0196(5) 0.0182(5) 0.0183(5) -0.0009(4) -0.0017(4) 0.0028(4) Si3 0.0276(5) 0.0305(5) 0.0208(5) 0.0010(4) 0.0043(4) 0.0048(4) Si4 0.0251(5) 0.0235(5) 0.0217(5) 0.0000(4) -0.0031(4) 0.0069(4) Si5 0.0341(6) 0.0219(5) 0.0250(5) -0.0057(4) -0.0040(4) 0.0056(4) Si6 0.0197(5) 0.0271(5) 0.0276(5) 0.0032(4) -0.0047(4) 0.0034(4) C1 0.039(2) 0.046(3) 0.037(2) 0.0016(18) 0.0117(18) 0.0163(19) C2 0.035(2) 0.049(3) 0.024(2) -0.0018(17) 0.0054(17) 0.0066(19) C3 0.033(2) 0.044(2) 0.031(2) 0.0068(17) 0.0065(17) -0.0009(18) C4 0.060(3) 0.051(3) 0.059(3) 0.030(2) 0.012(2) 0.000(2) C5 0.049(3) 0.079(4) 0.048(3) 0.011(2) 0.024(2) -0.004(3) C6 0.043(3) 0.050(3) 0.053(3) 0.007(2) 0.007(2) -0.014(2) C7 0.034(2) 0.033(2) 0.0255(19) -0.0005(15) -0.0060(16) 0.0061(17) C8 0.030(2) 0.036(2) 0.037(2) -0.0008(17) -0.0004(17) 0.0107(17) C9 0.038(2) 0.028(2) 0.031(2) 0.0057(16) -0.0061(17) 0.0102(17) C10 0.064(3) 0.032(2) 0.043(2) 0.0060(18) -0.008(2) 0.015(2) C11 0.058(3) 0.042(3) 0.037(2) 0.0159(19) -0.006(2) 0.009(2) C12 0.049(3) 0.053(3) 0.068(3) 0.019(2) -0.011(2) 0.026(2) C13 0.058(3) 0.034(2) 0.032(2) -0.0091(17) 0.002(2) -0.001(2) C14 0.044(3) 0.042(3) 0.058(3) -0.016(2) -0.004(2) 0.018(2) C15 0.040(2) 0.0214(19) 0.032(2) 0.0001(15) -0.0080(17) 0.0026(16) C16 0.063(3) 0.032(2) 0.039(2) 0.0061(18) -0.002(2) 0.001(2) C17 0.080(3) 0.020(2) 0.050(3) -0.0099(18) -0.010(2) 0.006(2) C18 0.045(3) 0.033(2) 0.064(3) 0.012(2) -0.002(2) -0.008(2) C19 0.027(2) 0.041(2) 0.062(3) 0.016(2) 0.0034(19) 0.0019(18) C20 0.046(2) 0.035(2) 0.041(2) -0.0019(18) -0.0184(19) 0.0081(19) C21 0.0223(18) 0.0275(19) 0.0278(19) 0.0027(15) -0.0016(15) 0.0096(15) C22 0.029(2) 0.046(3) 0.061(3) 0.007(2) -0.005(2) 0.0150(19) C23 0.035(2) 0.028(2) 0.035(2) 0.0060(16) 0.0008(17) 0.0103(16) C24 0.036(2) 0.036(2) 0.040(2) 0.0015(17) 0.0025(18) 0.0142(18) C25 0.041(2) 0.034(2) 0.039(2) -0.0078(17) 0.0105(18) 0.0057(18) C26 0.041(2) 0.028(2) 0.041(2) -0.0008(17) -0.0058(18) 0.0062(17) C27 0.0281(19) 0.030(2) 0.0249(19) 0.0010(15) 0.0042(15) -0.0022(16) C28 0.046(3) 0.036(3) 0.073(3) -0.006(2) -0.006(2) -0.007(2) C29 0.054(3) 0.060(4) 0.101(4) -0.001(3) -0.010(3) -0.032(3) C30 0.033(3) 0.116(5) 0.062(3) 0.018(3) 0.002(2) -0.017(3) C31 0.031(2) 0.091(4) 0.050(3) 0.011(3) 0.006(2) 0.017(3) C32 0.032(2) 0.048(3) 0.031(2) 0.0033(18) 0.0032(17) 0.0021(19) C33 0.035(2) 0.062(3) 0.038(2) 0.012(2) 0.0148(18) 0.021(2) C34 0.043(2) 0.040(2) 0.025(2) -0.0028(17) 0.0072(17) 0.0012(19) C35 0.033(2) 0.035(2) 0.0213(19) 0.0028(15) 0.0100(16) -0.0033(17) C36 0.041(2) 0.040(2) 0.034(2) 0.0074(18) 0.0040(18) -0.0025(19) C37 0.071(3) 0.043(3) 0.055(3) 0.020(2) 0.015(3) 0.006(2) C38 0.083(4) 0.032(3) 0.070(3) 0.011(2) 0.023(3) -0.007(3) C39 0.053(3) 0.057(3) 0.052(3) -0.001(2) 0.010(2) -0.021(2) C40 0.039(2) 0.050(3) 0.032(2) 0.0016(19) 0.0047(18) -0.009(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 2.3566(10) . ? Pd1 P1 2.3574(10) . ? Pd1 Si2 2.4287(10) . ? Pd1 Si1 2.4632(10) . ? P1 C34 1.824(3) . ? P1 C33 1.826(4) . ? P1 C35 1.831(4) . ? P2 C26 1.827(4) . ? P2 C27 1.833(4) . ? P2 C25 1.835(4) . ? Si1 Si2 2.2952(13) . ? Si1 Si3 2.3772(13) . ? Si1 Si4 2.3990(14) . ? Si2 Si5 2.3713(14) . ? Si2 Si6 2.4040(13) . ? Si3 C1 1.876(4) . ? Si3 C2 1.887(3) . ? Si3 C3 1.918(4) . ? Si4 C8 1.882(4) . ? Si4 C7 1.886(3) . ? Si4 C9 1.923(4) . ? Si5 C14 1.875(4) . ? Si5 C13 1.891(4) . ? Si5 C15 1.917(4) . ? Si6 C19 1.882(4) . ? Si6 C20 1.887(4) . ? Si6 C21 1.920(4) . ? C1 H1 0.9600 . ? C1 H2 0.9600 . ? C1 H3 0.9600 . ? C2 H4 0.9600 . ? C2 H5 0.9600 . ? C2 H6 0.9600 . ? C3 C6 1.524(5) . ? C3 C4 1.526(6) . ? C3 C5 1.542(5) . ? C4 H7 0.9600 . ? C4 H8 0.9600 . ? C4 H9 0.9600 . ? C5 H10 0.9600 . ? C5 H11 0.9600 . ? C5 H12 0.9600 . ? C6 H13 0.9600 . ? C6 H14 0.9600 . ? C6 H15 0.9600 . ? C7 H16 0.9600 . ? C7 H17 0.9600 . ? C7 H18 0.9600 . ? C8 H19 0.9600 . ? C8 H20 0.9600 . ? C8 H21 0.9600 . ? C9 C10 1.536(5) . ? C9 C11 1.538(5) . ? C9 C12 1.539(5) . ? C10 H22 0.9600 . ? C10 H23 0.9600 . ? C10 H24 0.9600 . ? C11 H25 0.9600 . ? C11 H26 0.9600 . ? C11 H27 0.9600 . ? C12 H28 0.9600 . ? C12 H29 0.9600 . ? C12 H30 0.9600 . ? C13 H31 0.9600 . ? C13 H32 0.9600 . ? C13 H33 0.9600 . ? C14 H34 0.9600 . ? C14 H35 0.9600 . ? C14 H36 0.9600 . ? C15 C18 1.530(5) . ? C15 C16 1.530(5) . ? C15 C17 1.537(5) . ? C16 H37 0.9600 . ? C16 H38 0.9600 . ? C16 H39 0.9600 . ? C17 H40 0.9600 . ? C17 H41 0.9600 . ? C17 H42 0.9600 . ? C18 H43 0.9600 . ? C18 H44 0.9600 . ? C18 H45 0.9600 . ? C19 H46 0.9600 . ? C19 H47 0.9600 . ? C19 H48 0.9600 . ? C20 H49 0.9600 . ? C20 H50 0.9600 . ? C20 H51 0.9600 . ? C21 C23 1.531(5) . ? C21 C24 1.532(5) . ? C21 C22 1.535(5) . ? C22 H52 0.9600 . ? C22 H53 0.9600 . ? C22 H54 0.9600 . ? C23 H55 0.9600 . ? C23 H56 0.9600 . ? C23 H57 0.9600 . ? C24 H58 0.9600 . ? C24 H59 0.9600 . ? C24 H60 0.9600 . ? C25 H61 0.9600 . ? C25 H62 0.9600 . ? C25 H63 0.9600 . ? C26 H64 0.9600 . ? C26 H65 0.9600 . ? C26 H66 0.9600 . ? C27 C28 1.381(5) . ? C27 C32 1.383(5) . ? C28 C29 1.382(6) . ? C28 H67 0.9300 . ? C29 C30 1.361(7) . ? C29 H68 0.9300 . ? C30 C31 1.367(7) . ? C30 H69 0.9300 . ? C31 C32 1.388(5) . ? C31 H70 0.9300 . ? C32 H71 0.9300 . ? C33 H72 0.9600 . ? C33 H73 0.9600 . ? C33 H74 0.9600 . ? C34 H75 0.9600 . ? C34 H76 0.9600 . ? C34 H77 0.9600 . ? C35 C40 1.391(5) . ? C35 C36 1.397(5) . ? C36 C37 1.375(5) . ? C36 H78 0.9300 . ? C37 C38 1.375(6) . ? C37 H79 0.9300 . ? C38 C39 1.371(7) . ? C38 H80 0.9300 . ? C39 C40 1.384(6) . ? C39 H81 0.9300 . ? C40 H82 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pd1 P1 101.14(4) . . ? P2 Pd1 Si2 152.76(3) . . ? P1 Pd1 Si2 102.13(3) . . ? P2 Pd1 Si1 106.87(4) . . ? P1 Pd1 Si1 148.44(3) . . ? Si2 Pd1 Si1 55.96(3) . . ? C34 P1 C33 99.05(18) . . ? C34 P1 C35 101.83(17) . . ? C33 P1 C35 101.52(18) . . ? C34 P1 Pd1 120.28(13) . . ? C33 P1 Pd1 110.81(13) . . ? C35 P1 Pd1 119.95(11) . . ? C26 P2 C27 102.83(17) . . ? C26 P2 C25 99.55(18) . . ? C27 P2 C25 101.54(16) . . ? C26 P2 Pd1 110.58(12) . . ? C27 P2 Pd1 119.45(12) . . ? C25 P2 Pd1 119.92(13) . . ? Si2 Si1 Si3 124.12(5) . . ? Si2 Si1 Si4 121.28(5) . . ? Si3 Si1 Si4 112.20(5) . . ? Si2 Si1 Pd1 61.26(3) . . ? Si3 Si1 Pd1 129.55(5) . . ? Si4 Si1 Pd1 95.82(4) . . ? Si1 Si2 Si5 119.99(5) . . ? Si1 Si2 Si6 121.34(5) . . ? Si5 Si2 Si6 110.30(5) . . ? Si1 Si2 Pd1 62.78(3) . . ? Si5 Si2 Pd1 128.11(5) . . ? Si6 Si2 Pd1 107.37(4) . . ? C1 Si3 C2 105.83(18) . . ? C1 Si3 C3 105.65(18) . . ? C2 Si3 C3 107.84(17) . . ? C1 Si3 Si1 114.02(12) . . ? C2 Si3 Si1 109.99(12) . . ? C3 Si3 Si1 113.05(13) . . ? C8 Si4 C7 106.24(17) . . ? C8 Si4 C9 105.88(17) . . ? C7 Si4 C9 104.45(16) . . ? C8 Si4 Si1 109.57(12) . . ? C7 Si4 Si1 105.35(12) . . ? C9 Si4 Si1 124.06(12) . . ? C14 Si5 C13 104.60(19) . . ? C14 Si5 C15 107.42(18) . . ? C13 Si5 C15 106.13(17) . . ? C14 Si5 Si2 111.65(13) . . ? C13 Si5 Si2 115.64(13) . . ? C15 Si5 Si2 110.86(12) . . ? C19 Si6 C20 105.28(19) . . ? C19 Si6 C21 105.34(17) . . ? C20 Si6 C21 105.86(16) . . ? C19 Si6 Si2 116.71(13) . . ? C20 Si6 Si2 107.97(13) . . ? C21 Si6 Si2 114.79(11) . . ? Si3 C1 H1 109.5 . . ? Si3 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? Si3 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? Si3 C2 H4 109.5 . . ? Si3 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? Si3 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? C6 C3 C4 108.3(4) . . ? C6 C3 C5 108.2(3) . . ? C4 C3 C5 108.3(3) . . ? C6 C3 Si3 110.1(3) . . ? C4 C3 Si3 111.6(3) . . ? C5 C3 Si3 110.3(3) . . ? C3 C4 H7 109.5 . . ? C3 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C3 C4 H9 109.5 . . ? H7 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C3 C5 H10 109.5 . . ? C3 C5 H11 109.5 . . ? H10 C5 H11 109.5 . . ? C3 C5 H12 109.5 . . ? H10 C5 H12 109.5 . . ? H11 C5 H12 109.5 . . ? C3 C6 H13 109.5 . . ? C3 C6 H14 109.5 . . ? H13 C6 H14 109.5 . . ? C3 C6 H15 109.5 . . ? H13 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? Si4 C7 H16 109.5 . . ? Si4 C7 H17 109.5 . . ? H16 C7 H17 109.5 . . ? Si4 C7 H18 109.5 . . ? H16 C7 H18 109.5 . . ? H17 C7 H18 109.5 . . ? Si4 C8 H19 109.5 . . ? Si4 C8 H20 109.5 . . ? H19 C8 H20 109.5 . . ? Si4 C8 H21 109.5 . . ? H19 C8 H21 109.5 . . ? H20 C8 H21 109.5 . . ? C10 C9 C11 108.9(3) . . ? C10 C9 C12 108.3(3) . . ? C11 C9 C12 108.2(3) . . ? C10 C9 Si4 112.4(2) . . ? C11 C9 Si4 111.2(3) . . ? C12 C9 Si4 107.7(3) . . ? C9 C10 H22 109.5 . . ? C9 C10 H23 109.5 . . ? H22 C10 H23 109.5 . . ? C9 C10 H24 109.5 . . ? H22 C10 H24 109.5 . . ? H23 C10 H24 109.5 . . ? C9 C11 H25 109.5 . . ? C9 C11 H26 109.5 . . ? H25 C11 H26 109.5 . . ? C9 C11 H27 109.5 . . ? H25 C11 H27 109.5 . . ? H26 C11 H27 109.5 . . ? C9 C12 H28 109.5 . . ? C9 C12 H29 109.5 . . ? H28 C12 H29 109.5 . . ? C9 C12 H30 109.5 . . ? H28 C12 H30 109.5 . . ? H29 C12 H30 109.5 . . ? Si5 C13 H31 109.5 . . ? Si5 C13 H32 109.5 . . ? H31 C13 H32 109.5 . . ? Si5 C13 H33 109.5 . . ? H31 C13 H33 109.5 . . ? H32 C13 H33 109.5 . . ? Si5 C14 H34 109.5 . . ? Si5 C14 H35 109.5 . . ? H34 C14 H35 109.5 . . ? Si5 C14 H36 109.5 . . ? H34 C14 H36 109.5 . . ? H35 C14 H36 109.5 . . ? C18 C15 C16 108.5(3) . . ? C18 C15 C17 108.3(3) . . ? C16 C15 C17 108.3(3) . . ? C18 C15 Si5 111.4(3) . . ? C16 C15 Si5 110.4(2) . . ? C17 C15 Si5 109.8(3) . . ? C15 C16 H37 109.5 . . ? C15 C16 H38 109.5 . . ? H37 C16 H38 109.5 . . ? C15 C16 H39 109.5 . . ? H37 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? C15 C17 H40 109.5 . . ? C15 C17 H41 109.5 . . ? H40 C17 H41 109.5 . . ? C15 C17 H42 109.5 . . ? H40 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? C15 C18 H43 109.5 . . ? C15 C18 H44 109.5 . . ? H43 C18 H44 109.5 . . ? C15 C18 H45 109.5 . . ? H43 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? Si6 C19 H46 109.5 . . ? Si6 C19 H47 109.5 . . ? H46 C19 H47 109.5 . . ? Si6 C19 H48 109.5 . . ? H46 C19 H48 109.5 . . ? H47 C19 H48 109.5 . . ? Si6 C20 H49 109.5 . . ? Si6 C20 H50 109.5 . . ? H49 C20 H50 109.5 . . ? Si6 C20 H51 109.5 . . ? H49 C20 H51 109.5 . . ? H50 C20 H51 109.5 . . ? C23 C21 C24 108.8(3) . . ? C23 C21 C22 108.1(3) . . ? C24 C21 C22 107.8(3) . . ? C23 C21 Si6 110.8(2) . . ? C24 C21 Si6 110.9(2) . . ? C22 C21 Si6 110.2(2) . . ? C21 C22 H52 109.5 . . ? C21 C22 H53 109.5 . . ? H52 C22 H53 109.5 . . ? C21 C22 H54 109.5 . . ? H52 C22 H54 109.5 . . ? H53 C22 H54 109.5 . . ? C21 C23 H55 109.5 . . ? C21 C23 H56 109.5 . . ? H55 C23 H56 109.5 . . ? C21 C23 H57 109.5 . . ? H55 C23 H57 109.5 . . ? H56 C23 H57 109.5 . . ? C21 C24 H58 109.5 . . ? C21 C24 H59 109.5 . . ? H58 C24 H59 109.5 . . ? C21 C24 H60 109.5 . . ? H58 C24 H60 109.5 . . ? H59 C24 H60 109.5 . . ? P2 C25 H61 109.5 . . ? P2 C25 H62 109.5 . . ? H61 C25 H62 109.5 . . ? P2 C25 H63 109.5 . . ? H61 C25 H63 109.5 . . ? H62 C25 H63 109.5 . . ? P2 C26 H64 109.5 . . ? P2 C26 H65 109.5 . . ? H64 C26 H65 109.5 . . ? P2 C26 H66 109.5 . . ? H64 C26 H66 109.5 . . ? H65 C26 H66 109.5 . . ? C28 C27 C32 118.1(4) . . ? C28 C27 P2 122.7(3) . . ? C32 C27 P2 119.1(3) . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H67 119.6 . . ? C29 C28 H67 119.6 . . ? C30 C29 C28 120.5(5) . . ? C30 C29 H68 119.7 . . ? C28 C29 H68 119.7 . . ? C29 C30 C31 119.8(5) . . ? C29 C30 H69 120.1 . . ? C31 C30 H69 120.1 . . ? C30 C31 C32 120.1(5) . . ? C30 C31 H70 120.0 . . ? C32 C31 H70 120.0 . . ? C27 C32 C31 120.7(4) . . ? C27 C32 H71 119.7 . . ? C31 C32 H71 119.7 . . ? P1 C33 H72 109.5 . . ? P1 C33 H73 109.5 . . ? H72 C33 H73 109.5 . . ? P1 C33 H74 109.5 . . ? H72 C33 H74 109.5 . . ? H73 C33 H74 109.5 . . ? P1 C34 H75 109.5 . . ? P1 C34 H76 109.5 . . ? H75 C34 H76 109.5 . . ? P1 C34 H77 109.5 . . ? H75 C34 H77 109.5 . . ? H76 C34 H77 109.5 . . ? C40 C35 C36 117.6(4) . . ? C40 C35 P1 121.1(3) . . ? C36 C35 P1 121.2(3) . . ? C37 C36 C35 121.2(4) . . ? C37 C36 H78 119.4 . . ? C35 C36 H78 119.4 . . ? C36 C37 C38 120.3(4) . . ? C36 C37 H79 119.9 . . ? C38 C37 H79 119.9 . . ? C39 C38 C37 119.7(4) . . ? C39 C38 H80 120.1 . . ? C37 C38 H80 120.1 . . ? C38 C39 C40 120.4(4) . . ? C38 C39 H81 119.8 . . ? C40 C39 H81 119.8 . . ? C39 C40 C35 120.9(4) . . ? C39 C40 H82 119.6 . . ? C35 C40 H82 119.6 . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.655 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.088 #===END