# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Watanabe, Chieko' 'Inagawa, Y.' 'Iwamoto, Takeaki' 'Kira, Mitsuo' _publ_contact_author_name 'Takeaki Iwamoto' _publ_contact_author_address ; 6-3 Aramakiazaaoba Aoba-ku Sendai Miyagi Japan 980-8578 ; _publ_contact_author_email iwamoto@m.tains.tohoku.ac.jp data_(silylene)(Me3P)2Ni_cw20 _database_code_depnum_ccdc_archive 'CCDC 775908' #TrackingRef '- silylenecomplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H58 Ni P2 Si5' _chemical_formula_weight 583.78 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' Si Si 0.0817 0.0704 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.476(3) _cell_length_b 32.504(9) _cell_length_c 11.672(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.327(3) _cell_angle_gamma 90.00 _cell_volume 3325.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 7916 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.40 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8453 _exptl_absorpt_correction_T_max 0.8453 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36966 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7603 _reflns_number_gt 5865 _reflns_threshold_expression >2sigma _computing_data_collection 'APEX2 ' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0418P)^2^+0.8623P] 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 7603 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Si1 Si 0.73984(7) 0.136739(17) 0.55279(5) 0.01567(13) Uani 1 1 d . . . C1 C 0.6189(2) 0.11324(6) 0.39381(19) 0.0167(4) Uani 1 1 d . . . C2 C 0.6115(3) 0.14764(6) 0.2973(2) 0.0202(5) Uani 1 1 d . . . H1 H 0.6999 0.1450 0.2724 0.024 Uiso 1 1 calc R . . H2 H 0.5172 0.1444 0.2224 0.024 Uiso 1 1 calc R . . C3 C 0.6132(3) 0.19035(6) 0.3550(2) 0.0196(5) Uani 1 1 d . . . H3 H 0.5110 0.1965 0.3551 0.024 Uiso 1 1 calc R . . H4 H 0.6375 0.2116 0.3044 0.024 Uiso 1 1 calc R . . C4 C 0.7344(2) 0.19189(6) 0.4907(2) 0.0179(4) Uani 1 1 d . . . Ni1 Ni 0.84261(3) 0.110962(8) 0.73379(2) 0.01714(8) Uani 1 1 d . . . P1 P 1.06471(7) 0.082261(18) 0.81638(5) 0.02090(13) Uani 1 1 d . . . P2 P 0.74225(7) 0.106656(18) 0.87199(5) 0.02095(13) Uani 1 1 d . . . C5 C 1.1727(3) 0.06712(8) 0.7224(2) 0.0331(6) Uani 1 1 d . . . H5 H 1.1920 0.0914 0.6808 0.050 Uiso 1 1 calc R . . H6 H 1.1138 0.0469 0.6603 0.050 Uiso 1 1 calc R . . H7 H 1.2700 0.0549 0.7758 0.050 Uiso 1 1 calc R . . C6 C 1.2096(3) 0.11269(8) 0.9353(2) 0.0313(6) Uani 1 1 d . . . H8 H 1.3048 0.0969 0.9690 0.047 Uiso 1 1 calc R . . H9 H 1.1742 0.1192 1.0019 0.047 Uiso 1 1 calc R . . H10 H 1.2276 0.1383 0.8986 0.047 Uiso 1 1 calc R . . C7 C 1.0756(3) 0.03377(7) 0.8992(2) 0.0311(6) Uani 1 1 d . . . H11 H 1.0099 0.0133 0.8422 0.047 Uiso 1 1 calc R . . H12 H 1.0416 0.0382 0.9677 0.047 Uiso 1 1 calc R . . H13 H 1.1813 0.0239 0.9320 0.047 Uiso 1 1 calc R . . C8 C 0.6584(3) 0.05614(7) 0.8762(2) 0.0285(5) Uani 1 1 d . . . H14 H 0.6183 0.0558 0.9423 0.043 Uiso 1 1 calc R . . H15 H 0.7367 0.0348 0.8922 0.043 Uiso 1 1 calc R . . H16 H 0.5752 0.0508 0.7965 0.043 Uiso 1 1 calc R . . C9 C 0.8662(3) 0.11353(8) 1.0348(2) 0.0325(6) Uani 1 1 d . . . H17 H 0.9114 0.1411 1.0467 0.049 Uiso 1 1 calc R . . H18 H 0.9474 0.0928 1.0583 0.049 Uiso 1 1 calc R . . H19 H 0.8061 0.1104 1.0865 0.049 Uiso 1 1 calc R . . C10 C 0.5854(3) 0.14025(8) 0.8672(2) 0.0319(6) Uani 1 1 d . . . H20 H 0.4972 0.1355 0.7901 0.048 Uiso 1 1 calc R . . H21 H 0.6175 0.1690 0.8709 0.048 Uiso 1 1 calc R . . H22 H 0.5573 0.1342 0.9381 0.048 Uiso 1 1 calc R . . Si2 Si 0.73165(8) 0.067647(18) 0.37456(6) 0.02039(14) Uani 1 1 d . . . C11 C 0.9309(3) 0.08239(7) 0.3937(2) 0.0268(5) Uani 1 1 d . . . H23 H 0.9776 0.0986 0.4696 0.040 Uiso 1 1 calc R . . H24 H 0.9277 0.0988 0.3223 0.040 Uiso 1 1 calc R . . H25 H 0.9913 0.0575 0.3991 0.040 Uiso 1 1 calc R . . C12 C 0.7451(3) 0.02670(7) 0.4912(2) 0.0286(6) Uani 1 1 d . . . H26 H 0.8146 0.0050 0.4866 0.043 Uiso 1 1 calc R . . H27 H 0.6438 0.0149 0.4735 0.043 Uiso 1 1 calc R . . H28 H 0.7840 0.0387 0.5744 0.043 Uiso 1 1 calc R . . C13 C 0.6486(3) 0.04573(8) 0.2131(2) 0.0301(6) Uani 1 1 d . . . H29 H 0.5987 0.0677 0.1542 0.045 Uiso 1 1 calc R . . H30 H 0.5736 0.0245 0.2092 0.045 Uiso 1 1 calc R . . H31 H 0.7304 0.0336 0.1921 0.045 Uiso 1 1 calc R . . Si3 Si 0.42174(7) 0.096762(19) 0.38254(6) 0.01988(14) Uani 1 1 d . . . C14 C 0.3373(3) 0.05235(8) 0.2747(2) 0.0299(6) Uani 1 1 d . . . H32 H 0.3997 0.0277 0.3061 0.045 Uiso 1 1 calc R . . H33 H 0.3348 0.0590 0.1921 0.045 Uiso 1 1 calc R . . H34 H 0.2332 0.0472 0.2699 0.045 Uiso 1 1 calc R . . C15 C 0.4185(3) 0.08049(7) 0.5349(2) 0.0275(5) Uani 1 1 d . . . H35 H 0.4447 0.1040 0.5918 0.041 Uiso 1 1 calc R . . H36 H 0.4928 0.0584 0.5697 0.041 Uiso 1 1 calc R . . H37 H 0.3163 0.0706 0.5232 0.041 Uiso 1 1 calc R . . C16 C 0.2770(3) 0.13860(8) 0.3177(2) 0.0313(6) Uani 1 1 d . . . H38 H 0.1756 0.1282 0.3070 0.047 Uiso 1 1 calc R . . H39 H 0.2769 0.1474 0.2374 0.047 Uiso 1 1 calc R . . H40 H 0.3028 0.1620 0.3749 0.047 Uiso 1 1 calc R . . Si4 Si 0.92741(8) 0.21010(2) 0.49539(7) 0.02653(16) Uani 1 1 d . . . C17 C 0.9549(3) 0.19710(8) 0.3488(3) 0.0399(7) Uani 1 1 d . . . H41 H 0.8689 0.2079 0.2778 0.060 Uiso 1 1 calc R . . H42 H 0.9600 0.1672 0.3414 0.060 Uiso 1 1 calc R . . H43 H 1.0500 0.2095 0.3507 0.060 Uiso 1 1 calc R . . C18 C 1.0897(3) 0.18868(9) 0.6297(3) 0.0465(8) Uani 1 1 d . . . H44 H 1.1854 0.2010 0.6326 0.070 Uiso 1 1 calc R . . H45 H 1.0939 0.1588 0.6205 0.070 Uiso 1 1 calc R . . H46 H 1.0751 0.1950 0.7065 0.070 Uiso 1 1 calc R . . C19 C 0.9525(3) 0.26741(8) 0.5043(3) 0.0382(7) Uani 1 1 d . . . H47 H 0.9516 0.2773 0.5833 0.057 Uiso 1 1 calc R . . H48 H 0.8690 0.2803 0.4358 0.057 Uiso 1 1 calc R . . H49 H 1.0501 0.2745 0.4985 0.057 Uiso 1 1 calc R . . Si5 Si 0.66557(7) 0.225056(19) 0.59255(6) 0.02207(15) Uani 1 1 d . . . C20 C 0.4757(3) 0.20733(8) 0.5885(2) 0.0293(6) Uani 1 1 d . . . H50 H 0.4774 0.1774 0.5993 0.044 Uiso 1 1 calc R . . H51 H 0.3961 0.2147 0.5087 0.044 Uiso 1 1 calc R . . H52 H 0.4542 0.2206 0.6555 0.044 Uiso 1 1 calc R . . C21 C 0.8055(3) 0.22398(8) 0.7560(2) 0.0305(6) Uani 1 1 d . . . H53 H 0.7639 0.2391 0.8087 0.046 Uiso 1 1 calc R . . H54 H 0.9011 0.2369 0.7608 0.046 Uiso 1 1 calc R . . H55 H 0.8251 0.1954 0.7844 0.046 Uiso 1 1 calc R . . C22 C 0.6312(3) 0.28055(7) 0.5445(2) 0.0356(6) Uani 1 1 d . . . H56 H 0.5554 0.2922 0.5736 0.053 Uiso 1 1 calc R . . H57 H 0.5934 0.2825 0.4540 0.053 Uiso 1 1 calc R . . H58 H 0.7270 0.2959 0.5808 0.053 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 Si1 0.0164(3) 0.0138(3) 0.0179(3) 0.0014(2) 0.0077(2) 0.0004(2) C1 0.0211(11) 0.0137(10) 0.0172(10) 0.0012(8) 0.0096(9) 0.0005(8) C2 0.0230(12) 0.0189(11) 0.0186(11) 0.0019(9) 0.0079(9) 0.0008(9) C3 0.0218(12) 0.0159(10) 0.0210(11) 0.0041(9) 0.0081(9) 0.0022(9) C4 0.0160(11) 0.0153(10) 0.0209(11) 0.0025(9) 0.0054(9) -0.0004(8) Ni1 0.01938(16) 0.01674(14) 0.01695(14) 0.00243(11) 0.00876(12) 0.00156(11) P1 0.0228(3) 0.0210(3) 0.0199(3) 0.0040(2) 0.0092(2) 0.0046(2) P2 0.0254(3) 0.0211(3) 0.0195(3) -0.0012(2) 0.0121(2) -0.0021(2) C5 0.0307(14) 0.0412(15) 0.0311(14) 0.0084(12) 0.0160(12) 0.0126(12) C6 0.0241(13) 0.0350(14) 0.0311(13) -0.0001(11) 0.0064(11) 0.0005(11) C7 0.0356(15) 0.0239(13) 0.0326(14) 0.0095(11) 0.0115(12) 0.0058(11) C8 0.0351(15) 0.0265(13) 0.0260(12) -0.0005(10) 0.0141(11) -0.0069(11) C9 0.0380(15) 0.0396(15) 0.0228(12) -0.0043(11) 0.0148(11) -0.0103(12) C10 0.0343(15) 0.0343(14) 0.0362(14) -0.0008(11) 0.0238(12) 0.0049(11) Si2 0.0275(4) 0.0158(3) 0.0212(3) 0.0012(2) 0.0130(3) 0.0027(3) C11 0.0263(13) 0.0299(13) 0.0278(13) 0.0043(10) 0.0143(11) 0.0084(10) C12 0.0408(15) 0.0178(12) 0.0312(13) 0.0036(10) 0.0180(12) 0.0039(10) C13 0.0430(16) 0.0236(13) 0.0288(13) -0.0047(10) 0.0195(12) -0.0010(11) Si3 0.0204(3) 0.0184(3) 0.0209(3) -0.0023(2) 0.0079(3) -0.0030(2) C14 0.0332(14) 0.0262(13) 0.0287(13) -0.0047(10) 0.0100(11) -0.0079(11) C15 0.0302(14) 0.0288(13) 0.0276(13) -0.0050(10) 0.0156(11) -0.0109(10) C16 0.0194(13) 0.0273(13) 0.0418(15) -0.0022(11) 0.0056(11) -0.0006(10) Si4 0.0217(4) 0.0221(3) 0.0352(4) 0.0091(3) 0.0101(3) -0.0033(3) C17 0.0388(17) 0.0341(15) 0.0596(19) 0.0055(13) 0.0333(15) -0.0028(12) C18 0.0196(14) 0.0498(18) 0.061(2) 0.0272(15) 0.0057(13) -0.0033(12) C19 0.0395(17) 0.0293(14) 0.0436(16) 0.0062(12) 0.0132(13) -0.0142(12) Si5 0.0237(3) 0.0152(3) 0.0237(3) -0.0025(2) 0.0049(3) -0.0001(2) C20 0.0281(14) 0.0280(13) 0.0320(14) -0.0052(11) 0.0118(11) 0.0030(10) C21 0.0328(14) 0.0256(13) 0.0281(13) -0.0043(10) 0.0060(11) -0.0046(11) C22 0.0432(16) 0.0165(12) 0.0385(15) -0.0035(11) 0.0058(13) 0.0022(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C4 1.927(2) . ? Si1 C1 1.930(2) . ? Si1 Ni1 2.1331(8) . ? C1 C2 1.570(3) . ? C1 Si2 1.890(2) . ? C1 Si3 1.899(2) . ? C2 C3 1.540(3) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.565(3) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 Si5 1.895(2) . ? C4 Si4 1.903(2) . ? Ni1 P1 2.1650(8) . ? Ni1 P2 2.1661(8) . ? P1 C6 1.828(2) . ? P1 C5 1.829(3) . ? P1 C7 1.831(2) . ? P2 C10 1.828(2) . ? P2 C9 1.828(2) . ? P2 C8 1.833(2) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? C8 H14 0.9800 . ? C8 H15 0.9800 . ? C8 H16 0.9800 . ? C9 H17 0.9800 . ? C9 H18 0.9800 . ? C9 H19 0.9800 . ? C10 H20 0.9800 . ? C10 H21 0.9800 . ? C10 H22 0.9800 . ? Si2 C12 1.873(2) . ? Si2 C11 1.877(3) . ? Si2 C13 1.884(2) . ? C11 H23 0.9800 . ? C11 H24 0.9800 . ? C11 H25 0.9800 . ? C12 H26 0.9800 . ? C12 H27 0.9800 . ? C12 H28 0.9800 . ? C13 H29 0.9800 . ? C13 H30 0.9800 . ? C13 H31 0.9800 . ? Si3 C15 1.867(2) . ? Si3 C16 1.875(2) . ? Si3 C14 1.882(2) . ? C14 H32 0.9800 . ? C14 H33 0.9800 . ? C14 H34 0.9800 . ? C15 H35 0.9800 . ? C15 H36 0.9800 . ? C15 H37 0.9800 . ? C16 H38 0.9800 . ? C16 H39 0.9800 . ? C16 H40 0.9800 . ? Si4 C18 1.864(3) . ? Si4 C17 1.873(3) . ? Si4 C19 1.876(3) . ? C17 H41 0.9800 . ? C17 H42 0.9800 . ? C17 H43 0.9800 . ? C18 H44 0.9800 . ? C18 H45 0.9800 . ? C18 H46 0.9800 . ? C19 H47 0.9800 . ? C19 H48 0.9800 . ? C19 H49 0.9800 . ? Si5 C21 1.865(2) . ? Si5 C20 1.873(3) . ? Si5 C22 1.880(2) . ? C20 H50 0.9800 . ? C20 H51 0.9800 . ? C20 H52 0.9800 . ? C21 H53 0.9800 . ? C21 H54 0.9800 . ? C21 H55 0.9800 . ? C22 H56 0.9800 . ? C22 H57 0.9800 . ? C22 H58 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 C4 Si1 C1 94.88(9) . . ? C4 Si1 Ni1 132.45(7) . . ? C1 Si1 Ni1 132.67(7) . . ? C2 C1 Si2 110.27(14) . . ? C2 C1 Si3 112.12(15) . . ? Si2 C1 Si3 110.88(11) . . ? C2 C1 Si1 104.85(14) . . ? Si2 C1 Si1 105.59(10) . . ? Si3 C1 Si1 112.79(11) . . ? C3 C2 C1 109.79(17) . . ? C3 C2 H1 109.7 . . ? C1 C2 H1 109.7 . . ? C3 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? H1 C2 H2 108.2 . . ? C2 C3 C4 110.67(17) . . ? C2 C3 H3 109.5 . . ? C4 C3 H3 109.5 . . ? C2 C3 H4 109.5 . . ? C4 C3 H4 109.5 . . ? H3 C3 H4 108.1 . . ? C3 C4 Si5 111.01(15) . . ? C3 C4 Si4 111.51(15) . . ? Si5 C4 Si4 111.15(11) . . ? C3 C4 Si1 104.82(14) . . ? Si5 C4 Si1 105.04(11) . . ? Si4 C4 Si1 112.97(11) . . ? Si1 Ni1 P1 127.67(3) . . ? Si1 Ni1 P2 126.76(3) . . ? P1 Ni1 P2 105.55(3) . . ? C6 P1 C5 99.83(13) . . ? C6 P1 C7 100.92(12) . . ? C5 P1 C7 98.78(12) . . ? C6 P1 Ni1 115.32(9) . . ? C5 P1 Ni1 121.30(9) . . ? C7 P1 Ni1 117.16(9) . . ? C10 P2 C9 98.77(13) . . ? C10 P2 C8 100.36(12) . . ? C9 P2 C8 101.26(11) . . ? C10 P2 Ni1 121.38(9) . . ? C9 P2 Ni1 118.39(9) . . ? C8 P2 Ni1 113.31(8) . . ? P1 C5 H5 109.5 . . ? P1 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? P1 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? P1 C6 H8 109.5 . . ? P1 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? P1 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? P1 C7 H11 109.5 . . ? P1 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? P1 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? P2 C8 H14 109.5 . . ? P2 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? P2 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? P2 C9 H17 109.5 . . ? P2 C9 H18 109.5 . . ? H17 C9 H18 109.5 . . ? P2 C9 H19 109.5 . . ? H17 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? P2 C10 H20 109.5 . . ? P2 C10 H21 109.5 . . ? H20 C10 H21 109.5 . . ? P2 C10 H22 109.5 . . ? H20 C10 H22 109.5 . . ? H21 C10 H22 109.5 . . ? C12 Si2 C11 107.89(11) . . ? C12 Si2 C13 110.20(11) . . ? C11 Si2 C13 103.55(11) . . ? C12 Si2 C1 110.88(10) . . ? C11 Si2 C1 111.98(10) . . ? C13 Si2 C1 112.04(11) . . ? Si2 C11 H23 109.5 . . ? Si2 C11 H24 109.5 . . ? H23 C11 H24 109.5 . . ? Si2 C11 H25 109.5 . . ? H23 C11 H25 109.5 . . ? H24 C11 H25 109.5 . . ? Si2 C12 H26 109.5 . . ? Si2 C12 H27 109.5 . . ? H26 C12 H27 109.5 . . ? Si2 C12 H28 109.5 . . ? H26 C12 H28 109.5 . . ? H27 C12 H28 109.5 . . ? Si2 C13 H29 109.5 . . ? Si2 C13 H30 109.5 . . ? H29 C13 H30 109.5 . . ? Si2 C13 H31 109.5 . . ? H29 C13 H31 109.5 . . ? H30 C13 H31 109.5 . . ? C15 Si3 C16 108.41(12) . . ? C15 Si3 C14 105.24(11) . . ? C16 Si3 C14 103.08(12) . . ? C15 Si3 C1 112.68(10) . . ? C16 Si3 C1 111.90(11) . . ? C14 Si3 C1 114.83(11) . . ? Si3 C14 H32 109.5 . . ? Si3 C14 H33 109.5 . . ? H32 C14 H33 109.5 . . ? Si3 C14 H34 109.5 . . ? H32 C14 H34 109.5 . . ? H33 C14 H34 109.5 . . ? Si3 C15 H35 109.5 . . ? Si3 C15 H36 109.5 . . ? H35 C15 H36 109.5 . . ? Si3 C15 H37 109.5 . . ? H35 C15 H37 109.5 . . ? H36 C15 H37 109.5 . . ? Si3 C16 H38 109.5 . . ? Si3 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? Si3 C16 H40 109.5 . . ? H38 C16 H40 109.5 . . ? H39 C16 H40 109.5 . . ? C18 Si4 C17 109.09(14) . . ? C18 Si4 C19 106.11(13) . . ? C17 Si4 C19 102.47(13) . . ? C18 Si4 C4 112.64(11) . . ? C17 Si4 C4 111.64(11) . . ? C19 Si4 C4 114.25(11) . . ? Si4 C17 H41 109.5 . . ? Si4 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? Si4 C17 H43 109.5 . . ? H41 C17 H43 109.5 . . ? H42 C17 H43 109.5 . . ? Si4 C18 H44 109.5 . . ? Si4 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? Si4 C18 H46 109.5 . . ? H44 C18 H46 109.5 . . ? H45 C18 H46 109.5 . . ? Si4 C19 H47 109.5 . . ? Si4 C19 H48 109.5 . . ? H47 C19 H48 109.5 . . ? Si4 C19 H49 109.5 . . ? H47 C19 H49 109.5 . . ? H48 C19 H49 109.5 . . ? C21 Si5 C20 108.84(12) . . ? C21 Si5 C22 107.37(11) . . ? C20 Si5 C22 103.41(12) . . ? C21 Si5 C4 110.54(11) . . ? C20 Si5 C4 111.44(10) . . ? C22 Si5 C4 114.85(12) . . ? Si5 C20 H50 109.5 . . ? Si5 C20 H51 109.5 . . ? H50 C20 H51 109.5 . . ? Si5 C20 H52 109.5 . . ? H50 C20 H52 109.5 . . ? H51 C20 H52 109.5 . . ? Si5 C21 H53 109.5 . . ? Si5 C21 H54 109.5 . . ? H53 C21 H54 109.5 . . ? Si5 C21 H55 109.5 . . ? H53 C21 H55 109.5 . . ? H54 C21 H55 109.5 . . ? Si5 C22 H56 109.5 . . ? Si5 C22 H57 109.5 . . ? H56 C22 H57 109.5 . . ? Si5 C22 H58 109.5 . . ? H56 C22 H58 109.5 . . ? H57 C22 H58 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 C1 C2 12.01(15) . . . . ? Ni1 Si1 C1 C2 -168.25(10) . . . . ? C4 Si1 C1 Si2 128.51(11) . . . . ? Ni1 Si1 C1 Si2 -51.76(14) . . . . ? C4 Si1 C1 Si3 -110.26(11) . . . . ? Ni1 Si1 C1 Si3 69.48(13) . . . . ? Si2 C1 C2 C3 -145.67(15) . . . . ? Si3 C1 C2 C3 90.25(18) . . . . ? Si1 C1 C2 C3 -32.5(2) . . . . ? C1 C2 C3 C4 43.5(2) . . . . ? C2 C3 C4 Si5 -144.54(15) . . . . ? C2 C3 C4 Si4 90.93(19) . . . . ? C2 C3 C4 Si1 -31.6(2) . . . . ? C1 Si1 C4 C3 10.47(15) . . . . ? Ni1 Si1 C4 C3 -169.27(10) . . . . ? C1 Si1 C4 Si5 127.54(11) . . . . ? Ni1 Si1 C4 Si5 -52.20(14) . . . . ? C1 Si1 C4 Si4 -111.14(12) . . . . ? Ni1 Si1 C4 Si4 69.12(14) . . . . ? C4 Si1 Ni1 P1 -93.79(10) . . . . ? C1 Si1 Ni1 P1 86.57(10) . . . . ? C4 Si1 Ni1 P2 88.04(10) . . . . ? C1 Si1 Ni1 P2 -91.61(10) . . . . ? Si1 Ni1 P1 C6 106.78(10) . . . . ? P2 Ni1 P1 C6 -74.73(10) . . . . ? Si1 Ni1 P1 C5 -13.81(12) . . . . ? P2 Ni1 P1 C5 164.68(11) . . . . ? Si1 Ni1 P1 C7 -134.65(10) . . . . ? P2 Ni1 P1 C7 43.83(10) . . . . ? Si1 Ni1 P2 C10 -21.49(11) . . . . ? P1 Ni1 P2 C10 160.01(11) . . . . ? Si1 Ni1 P2 C9 -143.67(10) . . . . ? P1 Ni1 P2 C9 37.82(10) . . . . ? Si1 Ni1 P2 C8 98.00(10) . . . . ? P1 Ni1 P2 C8 -80.51(10) . . . . ? C2 C1 Si2 C12 178.83(15) . . . . ? Si3 C1 Si2 C12 -56.38(14) . . . . ? Si1 C1 Si2 C12 66.08(13) . . . . ? C2 C1 Si2 C11 58.26(17) . . . . ? Si3 C1 Si2 C11 -176.95(11) . . . . ? Si1 C1 Si2 C11 -54.49(13) . . . . ? C2 C1 Si2 C13 -57.59(18) . . . . ? Si3 C1 Si2 C13 67.20(14) . . . . ? Si1 C1 Si2 C13 -170.34(11) . . . . ? C2 C1 Si3 C15 -148.37(15) . . . . ? Si2 C1 Si3 C15 87.89(13) . . . . ? Si1 C1 Si3 C15 -30.28(15) . . . . ? C2 C1 Si3 C16 -25.90(18) . . . . ? Si2 C1 Si3 C16 -149.64(12) . . . . ? Si1 C1 Si3 C16 92.19(13) . . . . ? C2 C1 Si3 C14 91.15(17) . . . . ? Si2 C1 Si3 C14 -32.58(15) . . . . ? Si1 C1 Si3 C14 -150.76(11) . . . . ? C3 C4 Si4 C18 -151.11(17) . . . . ? Si5 C4 Si4 C18 84.43(16) . . . . ? Si1 C4 Si4 C18 -33.36(18) . . . . ? C3 C4 Si4 C17 -27.96(18) . . . . ? Si5 C4 Si4 C17 -152.42(12) . . . . ? Si1 C4 Si4 C17 89.79(14) . . . . ? C3 C4 Si4 C19 87.72(17) . . . . ? Si5 C4 Si4 C19 -36.73(16) . . . . ? Si1 C4 Si4 C19 -154.53(12) . . . . ? C3 C4 Si5 C21 176.47(15) . . . . ? Si4 C4 Si5 C21 -58.79(14) . . . . ? Si1 C4 Si5 C21 63.71(13) . . . . ? C3 C4 Si5 C20 55.30(17) . . . . ? Si4 C4 Si5 C20 -179.96(11) . . . . ? Si1 C4 Si5 C20 -57.47(13) . . . . ? C3 C4 Si5 C22 -61.87(18) . . . . ? Si4 C4 Si5 C22 62.87(15) . . . . ? Si1 C4 Si5 C22 -174.63(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.792 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.076 #===END data_(silylene)(Me3P)2Pd_cw07 _database_code_depnum_ccdc_archive 'CCDC 775909' #TrackingRef '- silylenecomplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H58 P2 Pd Si5' _chemical_formula_weight 631.47 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' Si Si 0.0817 0.0704 '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' _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 9.596(3) _cell_length_b 11.341(3) _cell_length_c 16.777(5) _cell_angle_alpha 78.740(8) _cell_angle_beta 82.334(9) _cell_angle_gamma 78.477(8) _cell_volume 1746.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 5505 _cell_measurement_theta_min 3.1052 _cell_measurement_theta_max 27.8764 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25206 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7987 _reflns_number_gt 6729 _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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7987 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.28282(5) 0.33964(4) 0.76203(3) 0.01754(10) Uani 1 1 d . . . C1 C 0.35890(19) 0.21778(15) 0.69453(10) 0.0201(3) Uani 1 1 d . . . C2 C 0.3145(2) 0.09645(15) 0.74451(10) 0.0243(4) Uani 1 1 d . . . H1 H 0.2188 0.0902 0.7317 0.029 Uiso 1 1 calc R . . H2 H 0.3835 0.0253 0.7289 0.029 Uiso 1 1 calc R . . C3 C 0.3116(2) 0.09513(15) 0.83676(10) 0.0231(4) Uani 1 1 d . . . H3 H 0.4104 0.0746 0.8527 0.028 Uiso 1 1 calc R . . H4 H 0.2581 0.0319 0.8679 0.028 Uiso 1 1 calc R . . C4 C 0.23821(18) 0.22405(15) 0.85760(10) 0.0194(3) Uani 1 1 d . . . Pd1 Pd 0.257091(14) 0.543690(11) 0.740403(8) 0.02076(5) Uani 1 1 d . . . P1 P 0.06011(6) 0.68733(5) 0.69714(3) 0.03212(12) Uani 1 1 d . . . P2 P 0.41451(5) 0.65878(4) 0.76717(3) 0.02741(11) Uani 1 1 d . . . Si2 Si 0.26264(6) 0.26662(5) 0.59818(3) 0.02640(12) Uani 1 1 d . . . C5 C 0.0633(2) 0.3032(2) 0.62218(13) 0.0413(5) Uani 1 1 d . . . H5 H 0.0265 0.2274 0.6436 0.062 Uiso 1 1 calc R . . H6 H 0.0191 0.3445 0.5723 0.062 Uiso 1 1 calc R . . H7 H 0.0405 0.3569 0.6632 0.062 Uiso 1 1 calc R . . C6 C 0.2897(3) 0.1378(2) 0.53860(13) 0.0439(6) Uani 1 1 d . . . H8 H 0.2120 0.1511 0.5036 0.066 Uiso 1 1 calc R . . H9 H 0.2897 0.0602 0.5765 0.066 Uiso 1 1 calc R . . H10 H 0.3813 0.1350 0.5047 0.066 Uiso 1 1 calc R . . C7 C 0.3189(3) 0.40678(19) 0.53295(12) 0.0396(5) Uani 1 1 d . . . H11 H 0.2652 0.4309 0.4848 0.059 Uiso 1 1 calc R . . H12 H 0.4214 0.3892 0.5154 0.059 Uiso 1 1 calc R . . H13 H 0.2996 0.4735 0.5645 0.059 Uiso 1 1 calc R . . Si3 Si 0.56073(6) 0.19999(5) 0.66804(3) 0.02834(12) Uani 1 1 d . . . C8 C 0.6262(3) 0.1506(3) 0.56715(16) 0.0650(8) Uani 1 1 d . . . H14 H 0.7304 0.1434 0.5581 0.097 Uiso 1 1 calc R . . H15 H 0.5823 0.2113 0.5234 0.097 Uiso 1 1 calc R . . H16 H 0.6002 0.0713 0.5673 0.097 Uiso 1 1 calc R . . C9 C 0.6309(2) 0.3440(2) 0.66571(16) 0.0464(6) Uani 1 1 d . . . H17 H 0.5795 0.4110 0.6283 0.070 Uiso 1 1 calc R . . H18 H 0.7331 0.3317 0.6469 0.070 Uiso 1 1 calc R . . H19 H 0.6167 0.3645 0.7207 0.070 Uiso 1 1 calc R . . C10 C 0.6582(2) 0.0732(2) 0.74182(15) 0.0434(5) Uani 1 1 d . . . H20 H 0.7608 0.0610 0.7240 0.065 Uiso 1 1 calc R . . H21 H 0.6225 -0.0025 0.7434 0.065 Uiso 1 1 calc R . . H22 H 0.6422 0.0950 0.7964 0.065 Uiso 1 1 calc R . . Si4 Si 0.32479(6) 0.25863(5) 0.94380(3) 0.02517(11) Uani 1 1 d . . . C11 C 0.5189(2) 0.2669(2) 0.91363(13) 0.0364(5) Uani 1 1 d . . . H23 H 0.5559 0.2996 0.9549 0.055 Uiso 1 1 calc R . . H24 H 0.5291 0.3205 0.8606 0.055 Uiso 1 1 calc R . . H25 H 0.5729 0.1848 0.9097 0.055 Uiso 1 1 calc R . . C12 C 0.3293(2) 0.1327(2) 1.03566(12) 0.0408(5) Uani 1 1 d . . . H26 H 0.2379 0.1436 1.0696 0.061 Uiso 1 1 calc R . . H27 H 0.4067 0.1355 1.0675 0.061 Uiso 1 1 calc R . . H28 H 0.3457 0.0535 1.0176 0.061 Uiso 1 1 calc R . . C13 C 0.2340(2) 0.40832(19) 0.97419(13) 0.0398(5) Uani 1 1 d . . . H29 H 0.2299 0.4727 0.9257 0.060 Uiso 1 1 calc R . . H30 H 0.2880 0.4286 1.0138 0.060 Uiso 1 1 calc R . . H31 H 0.1368 0.4018 0.9989 0.060 Uiso 1 1 calc R . . Si5 Si 0.03754(6) 0.23162(5) 0.88510(3) 0.02726(12) Uani 1 1 d . . . C14 C -0.0351(2) 0.1271(2) 0.83349(14) 0.0460(6) Uani 1 1 d . . . H32 H -0.0341 0.1594 0.7748 0.069 Uiso 1 1 calc R . . H33 H -0.1334 0.1219 0.8567 0.069 Uiso 1 1 calc R . . H34 H 0.0243 0.0455 0.8420 0.069 Uiso 1 1 calc R . . C15 C -0.0683(2) 0.3894(2) 0.85919(15) 0.0457(6) Uani 1 1 d . . . H35 H -0.0261 0.4471 0.8808 0.069 Uiso 1 1 calc R . . H36 H -0.1672 0.3907 0.8834 0.069 Uiso 1 1 calc R . . H37 H -0.0669 0.4130 0.7997 0.069 Uiso 1 1 calc R . . C16 C -0.0141(2) 0.1789(2) 0.99662(13) 0.0449(6) Uani 1 1 d . . . H38 H -0.1163 0.1751 1.0052 0.067 Uiso 1 1 calc R . . H39 H 0.0057 0.2366 1.0284 0.067 Uiso 1 1 calc R . . H40 H 0.0413 0.0977 1.0144 0.067 Uiso 1 1 calc R . . C17 C -0.0668(3) 0.6435(3) 0.64088(17) 0.0596(7) Uani 1 1 d . . . H41 H -0.1456 0.7122 0.6296 0.089 Uiso 1 1 calc R . . H42 H -0.1046 0.5732 0.6737 0.089 Uiso 1 1 calc R . . H43 H -0.0181 0.6216 0.5892 0.089 Uiso 1 1 calc R . . C18 C 0.0851(3) 0.8347(2) 0.63484(18) 0.0699(9) Uani 1 1 d . . . H44 H 0.1392 0.8755 0.6633 0.105 Uiso 1 1 calc R . . H45 H -0.0084 0.8861 0.6257 0.105 Uiso 1 1 calc R . . H46 H 0.1378 0.8215 0.5822 0.105 Uiso 1 1 calc R . . C19 C -0.0617(2) 0.7413(2) 0.78095(15) 0.0483(6) Uani 1 1 d . . . H47 H -0.1433 0.7994 0.7589 0.072 Uiso 1 1 calc R . . H48 H -0.0115 0.7818 0.8119 0.072 Uiso 1 1 calc R . . H49 H -0.0957 0.6718 0.8171 0.072 Uiso 1 1 calc R . . C20 C 0.5753(3) 0.5880(2) 0.81806(18) 0.0532(7) Uani 1 1 d . . . H50 H 0.6257 0.6517 0.8252 0.080 Uiso 1 1 calc R . . H51 H 0.6379 0.5331 0.7847 0.080 Uiso 1 1 calc R . . H52 H 0.5483 0.5414 0.8716 0.080 Uiso 1 1 calc R . . C21 C 0.3370(3) 0.7696(2) 0.83373(15) 0.0441(6) Uani 1 1 d . . . H53 H 0.2568 0.8264 0.8091 0.066 Uiso 1 1 calc R . . H54 H 0.4097 0.8153 0.8408 0.066 Uiso 1 1 calc R . . H55 H 0.3027 0.7267 0.8870 0.066 Uiso 1 1 calc R . . C22 C 0.4922(3) 0.7556(2) 0.67892(15) 0.0467(6) Uani 1 1 d . . . H56 H 0.5492 0.7043 0.6413 0.070 Uiso 1 1 calc R . . H57 H 0.5535 0.8024 0.6974 0.070 Uiso 1 1 calc R . . H58 H 0.4155 0.8121 0.6508 0.070 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 Si1 0.0205(2) 0.0159(2) 0.0163(2) -0.00341(17) -0.00212(18) -0.00244(18) C1 0.0258(9) 0.0178(8) 0.0169(8) -0.0062(6) 0.0021(7) -0.0038(7) C2 0.0335(10) 0.0168(9) 0.0226(9) -0.0056(7) -0.0006(8) -0.0039(7) C3 0.0315(10) 0.0168(8) 0.0187(9) -0.0018(7) 0.0009(7) -0.0024(7) C4 0.0244(9) 0.0166(8) 0.0162(8) -0.0040(6) 0.0000(7) -0.0014(7) Pd1 0.02220(8) 0.01542(7) 0.02383(8) -0.00351(5) -0.00279(5) -0.00094(5) P1 0.0301(3) 0.0271(3) 0.0327(3) 0.0011(2) -0.0043(2) 0.0047(2) P2 0.0293(3) 0.0194(2) 0.0351(3) -0.0079(2) -0.0032(2) -0.00496(19) Si2 0.0355(3) 0.0265(3) 0.0177(2) -0.0041(2) -0.0028(2) -0.0063(2) C5 0.0389(12) 0.0546(14) 0.0324(11) -0.0060(10) -0.0105(9) -0.0096(10) C6 0.0649(16) 0.0422(13) 0.0286(11) -0.0131(10) -0.0070(11) -0.0108(11) C7 0.0533(14) 0.0363(12) 0.0258(10) 0.0029(9) -0.0023(9) -0.0090(10) Si3 0.0266(3) 0.0292(3) 0.0272(3) -0.0094(2) 0.0044(2) -0.0006(2) C8 0.0510(16) 0.095(2) 0.0455(15) -0.0364(15) 0.0075(12) 0.0119(15) C9 0.0336(12) 0.0391(13) 0.0635(16) -0.0070(11) 0.0113(11) -0.0120(10) C10 0.0301(12) 0.0412(13) 0.0544(15) -0.0068(11) -0.0075(10) 0.0046(10) Si4 0.0317(3) 0.0247(3) 0.0187(2) -0.0053(2) -0.0052(2) -0.0009(2) C11 0.0348(11) 0.0389(12) 0.0378(12) -0.0050(9) -0.0124(9) -0.0074(9) C12 0.0476(13) 0.0443(13) 0.0246(10) 0.0024(9) -0.0069(9) -0.0006(10) C13 0.0519(14) 0.0372(12) 0.0326(11) -0.0172(9) -0.0078(10) 0.0003(10) Si5 0.0245(3) 0.0324(3) 0.0229(3) -0.0026(2) 0.0028(2) -0.0059(2) C14 0.0398(13) 0.0676(16) 0.0369(12) -0.0068(11) 0.0007(10) -0.0295(12) C15 0.0284(11) 0.0487(14) 0.0481(14) 0.0003(11) 0.0042(10) 0.0073(10) C16 0.0451(13) 0.0590(15) 0.0291(11) -0.0051(10) 0.0112(10) -0.0182(11) C17 0.0559(16) 0.0657(18) 0.0554(16) -0.0103(13) -0.0284(13) 0.0088(13) C18 0.0560(17) 0.0504(16) 0.077(2) 0.0280(15) 0.0057(15) 0.0056(13) C19 0.0413(13) 0.0450(14) 0.0521(15) -0.0105(11) 0.0033(11) 0.0046(11) C20 0.0478(15) 0.0397(13) 0.0796(19) -0.0130(13) -0.0262(13) -0.0094(11) C21 0.0544(14) 0.0370(12) 0.0465(13) -0.0199(10) 0.0038(11) -0.0149(11) C22 0.0473(14) 0.0493(14) 0.0461(14) -0.0111(11) 0.0092(11) -0.0214(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C4 1.9216(17) . ? Si1 C1 1.9268(17) . ? Si1 Pd1 2.2395(8) . ? C1 C2 1.570(2) . ? C1 Si2 1.9019(18) . ? C1 Si3 1.9075(19) . ? C2 C3 1.541(2) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.574(2) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 Si4 1.8994(18) . ? C4 Si5 1.9080(19) . ? Pd1 P2 2.3205(7) . ? Pd1 P1 2.3297(7) . ? P1 C19 1.825(2) . ? P1 C17 1.831(3) . ? P1 C18 1.832(2) . ? P2 C21 1.826(2) . ? P2 C20 1.828(2) . ? P2 C22 1.831(2) . ? Si2 C7 1.877(2) . ? Si2 C5 1.880(2) . ? Si2 C6 1.885(2) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? Si3 C8 1.876(2) . ? Si3 C9 1.879(2) . ? Si3 C10 1.885(2) . ? C8 H14 0.9800 . ? C8 H15 0.9800 . ? C8 H16 0.9800 . ? C9 H17 0.9800 . ? C9 H18 0.9800 . ? C9 H19 0.9800 . ? C10 H20 0.9800 . ? C10 H21 0.9800 . ? C10 H22 0.9800 . ? Si4 C13 1.879(2) . ? Si4 C11 1.880(2) . ? Si4 C12 1.884(2) . ? C11 H23 0.9800 . ? C11 H24 0.9800 . ? C11 H25 0.9800 . ? C12 H26 0.9800 . ? C12 H27 0.9800 . ? C12 H28 0.9800 . ? C13 H29 0.9800 . ? C13 H30 0.9800 . ? C13 H31 0.9800 . ? Si5 C15 1.874(2) . ? Si5 C14 1.880(2) . ? Si5 C16 1.881(2) . ? C14 H32 0.9800 . ? C14 H33 0.9800 . ? C14 H34 0.9800 . ? C15 H35 0.9800 . ? C15 H36 0.9800 . ? C15 H37 0.9800 . ? C16 H38 0.9800 . ? C16 H39 0.9800 . ? C16 H40 0.9800 . ? C17 H41 0.9800 . ? C17 H42 0.9800 . ? C17 H43 0.9800 . ? C18 H44 0.9800 . ? C18 H45 0.9800 . ? C18 H46 0.9800 . ? C19 H47 0.9800 . ? C19 H48 0.9800 . ? C19 H49 0.9800 . ? C20 H50 0.9800 . ? C20 H51 0.9800 . ? C20 H52 0.9800 . ? C21 H53 0.9800 . ? C21 H54 0.9800 . ? C21 H55 0.9800 . ? C22 H56 0.9800 . ? C22 H57 0.9800 . ? C22 H58 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 C4 Si1 C1 94.83(8) . . ? C4 Si1 Pd1 131.60(5) . . ? C1 Si1 Pd1 133.56(6) . . ? C2 C1 Si2 109.63(12) . . ? C2 C1 Si3 111.69(12) . . ? Si2 C1 Si3 110.63(8) . . ? C2 C1 Si1 104.98(11) . . ? Si2 C1 Si1 106.20(9) . . ? Si3 C1 Si1 113.42(9) . . ? C3 C2 C1 110.05(14) . . ? C3 C2 H1 109.7 . . ? C1 C2 H1 109.7 . . ? C3 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? H1 C2 H2 108.2 . . ? C2 C3 C4 109.92(14) . . ? C2 C3 H3 109.7 . . ? C4 C3 H3 109.7 . . ? C2 C3 H4 109.7 . . ? C4 C3 H4 109.7 . . ? H3 C3 H4 108.2 . . ? C3 C4 Si4 110.02(12) . . ? C3 C4 Si5 110.93(12) . . ? Si4 C4 Si5 110.96(8) . . ? C3 C4 Si1 105.28(11) . . ? Si4 C4 Si1 106.64(9) . . ? Si5 C4 Si1 112.77(9) . . ? Si1 Pd1 P2 127.19(2) . . ? Si1 Pd1 P1 128.07(2) . . ? P2 Pd1 P1 104.55(3) . . ? C19 P1 C17 99.84(13) . . ? C19 P1 C18 99.38(13) . . ? C17 P1 C18 100.89(14) . . ? C19 P1 Pd1 113.49(8) . . ? C17 P1 Pd1 119.42(9) . . ? C18 P1 Pd1 120.20(9) . . ? C21 P2 C20 98.90(12) . . ? C21 P2 C22 101.56(11) . . ? C20 P2 C22 99.99(12) . . ? C21 P2 Pd1 114.82(8) . . ? C20 P2 Pd1 121.85(8) . . ? C22 P2 Pd1 116.36(8) . . ? C7 Si2 C5 107.01(11) . . ? C7 Si2 C6 111.08(10) . . ? C5 Si2 C6 103.91(11) . . ? C7 Si2 C1 111.62(9) . . ? C5 Si2 C1 111.88(9) . . ? C6 Si2 C1 111.02(9) . . ? Si2 C5 H5 109.5 . . ? Si2 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? Si2 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? Si2 C6 H8 109.5 . . ? Si2 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? Si2 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? Si2 C7 H11 109.5 . . ? Si2 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si2 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? C8 Si3 C9 106.26(13) . . ? C8 Si3 C10 102.31(12) . . ? C9 Si3 C10 108.83(12) . . ? C8 Si3 C1 114.46(11) . . ? C9 Si3 C1 113.11(9) . . ? C10 Si3 C1 111.17(9) . . ? Si3 C8 H14 109.5 . . ? Si3 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? Si3 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? Si3 C9 H17 109.5 . . ? Si3 C9 H18 109.5 . . ? H17 C9 H18 109.5 . . ? Si3 C9 H19 109.5 . . ? H17 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? Si3 C10 H20 109.5 . . ? Si3 C10 H21 109.5 . . ? H20 C10 H21 109.5 . . ? Si3 C10 H22 109.5 . . ? H20 C10 H22 109.5 . . ? H21 C10 H22 109.5 . . ? C13 Si4 C11 107.81(10) . . ? C13 Si4 C12 110.17(10) . . ? C11 Si4 C12 103.28(10) . . ? C13 Si4 C4 111.36(9) . . ? C11 Si4 C4 111.43(9) . . ? C12 Si4 C4 112.42(9) . . ? Si4 C11 H23 109.5 . . ? Si4 C11 H24 109.5 . . ? H23 C11 H24 109.5 . . ? Si4 C11 H25 109.5 . . ? H23 C11 H25 109.5 . . ? H24 C11 H25 109.5 . . ? Si4 C12 H26 109.5 . . ? Si4 C12 H27 109.5 . . ? H26 C12 H27 109.5 . . ? Si4 C12 H28 109.5 . . ? H26 C12 H28 109.5 . . ? H27 C12 H28 109.5 . . ? Si4 C13 H29 109.5 . . ? Si4 C13 H30 109.5 . . ? H29 C13 H30 109.5 . . ? Si4 C13 H31 109.5 . . ? H29 C13 H31 109.5 . . ? H30 C13 H31 109.5 . . ? C15 Si5 C14 108.02(12) . . ? C15 Si5 C16 105.73(11) . . ? C14 Si5 C16 103.31(11) . . ? C15 Si5 C4 113.16(9) . . ? C14 Si5 C4 112.01(9) . . ? C16 Si5 C4 113.90(9) . . ? Si5 C14 H32 109.5 . . ? Si5 C14 H33 109.5 . . ? H32 C14 H33 109.5 . . ? Si5 C14 H34 109.5 . . ? H32 C14 H34 109.5 . . ? H33 C14 H34 109.5 . . ? Si5 C15 H35 109.5 . . ? Si5 C15 H36 109.5 . . ? H35 C15 H36 109.5 . . ? Si5 C15 H37 109.5 . . ? H35 C15 H37 109.5 . . ? H36 C15 H37 109.5 . . ? Si5 C16 H38 109.5 . . ? Si5 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? Si5 C16 H40 109.5 . . ? H38 C16 H40 109.5 . . ? H39 C16 H40 109.5 . . ? P1 C17 H41 109.5 . . ? P1 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? P1 C17 H43 109.5 . . ? H41 C17 H43 109.5 . . ? H42 C17 H43 109.5 . . ? P1 C18 H44 109.5 . . ? P1 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? P1 C18 H46 109.5 . . ? H44 C18 H46 109.5 . . ? H45 C18 H46 109.5 . . ? P1 C19 H47 109.5 . . ? P1 C19 H48 109.5 . . ? H47 C19 H48 109.5 . . ? P1 C19 H49 109.5 . . ? H47 C19 H49 109.5 . . ? H48 C19 H49 109.5 . . ? P2 C20 H50 109.5 . . ? P2 C20 H51 109.5 . . ? H50 C20 H51 109.5 . . ? P2 C20 H52 109.5 . . ? H50 C20 H52 109.5 . . ? H51 C20 H52 109.5 . . ? P2 C21 H53 109.5 . . ? P2 C21 H54 109.5 . . ? H53 C21 H54 109.5 . . ? P2 C21 H55 109.5 . . ? H53 C21 H55 109.5 . . ? H54 C21 H55 109.5 . . ? P2 C22 H56 109.5 . . ? P2 C22 H57 109.5 . . ? H56 C22 H57 109.5 . . ? P2 C22 H58 109.5 . . ? H56 C22 H58 109.5 . . ? H57 C22 H58 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 C1 C2 12.05(12) . . . . ? Pd1 Si1 C1 C2 -168.97(8) . . . . ? C4 Si1 C1 Si2 128.15(9) . . . . ? Pd1 Si1 C1 Si2 -52.87(11) . . . . ? C4 Si1 C1 Si3 -110.15(9) . . . . ? Pd1 Si1 C1 Si3 68.83(11) . . . . ? Si2 C1 C2 C3 -146.36(13) . . . . ? Si3 C1 C2 C3 90.65(15) . . . . ? Si1 C1 C2 C3 -32.66(17) . . . . ? C1 C2 C3 C4 43.2(2) . . . . ? C2 C3 C4 Si4 -145.97(13) . . . . ? C2 C3 C4 Si5 90.87(15) . . . . ? C2 C3 C4 Si1 -31.41(17) . . . . ? C1 Si1 C4 C3 10.45(12) . . . . ? Pd1 Si1 C4 C3 -168.57(8) . . . . ? C1 Si1 C4 Si4 127.33(9) . . . . ? Pd1 Si1 C4 Si4 -51.68(11) . . . . ? C1 Si1 C4 Si5 -110.64(9) . . . . ? Pd1 Si1 C4 Si5 70.35(11) . . . . ? C4 Si1 Pd1 P2 84.91(8) . . . . ? C1 Si1 Pd1 P2 -93.73(8) . . . . ? C4 Si1 Pd1 P1 -89.31(8) . . . . ? C1 Si1 Pd1 P1 92.05(8) . . . . ? Si1 Pd1 P1 C19 94.33(9) . . . . ? P2 Pd1 P1 C19 -80.91(9) . . . . ? Si1 Pd1 P1 C17 -22.98(12) . . . . ? P2 Pd1 P1 C17 161.78(11) . . . . ? Si1 Pd1 P1 C18 -148.37(13) . . . . ? P2 Pd1 P1 C18 36.39(13) . . . . ? Si1 Pd1 P2 C21 -124.12(9) . . . . ? P1 Pd1 P2 C21 51.17(9) . . . . ? Si1 Pd1 P2 C20 -4.91(12) . . . . ? P1 Pd1 P2 C20 170.39(11) . . . . ? Si1 Pd1 P2 C22 117.48(9) . . . . ? P1 Pd1 P2 C22 -67.22(9) . . . . ? C2 C1 Si2 C7 -176.94(12) . . . . ? Si3 C1 Si2 C7 -53.33(12) . . . . ? Si1 C1 Si2 C7 70.15(11) . . . . ? C2 C1 Si2 C5 63.18(14) . . . . ? Si3 C1 Si2 C5 -173.21(10) . . . . ? Si1 C1 Si2 C5 -49.74(12) . . . . ? C2 C1 Si2 C6 -52.41(14) . . . . ? Si3 C1 Si2 C6 71.20(12) . . . . ? Si1 C1 Si2 C6 -165.33(10) . . . . ? C2 C1 Si3 C8 91.40(16) . . . . ? Si2 C1 Si3 C8 -31.02(15) . . . . ? Si1 C1 Si3 C8 -150.22(13) . . . . ? C2 C1 Si3 C9 -146.70(14) . . . . ? Si2 C1 Si3 C9 90.88(12) . . . . ? Si1 C1 Si3 C9 -28.32(14) . . . . ? C2 C1 Si3 C10 -23.90(15) . . . . ? Si2 C1 Si3 C10 -146.32(10) . . . . ? Si1 C1 Si3 C10 94.48(12) . . . . ? C3 C4 Si4 C13 -177.09(12) . . . . ? Si5 C4 Si4 C13 -53.95(12) . . . . ? Si1 C4 Si4 C13 69.22(11) . . . . ? C3 C4 Si4 C11 62.49(14) . . . . ? Si5 C4 Si4 C11 -174.36(9) . . . . ? Si1 C4 Si4 C11 -51.20(11) . . . . ? C3 C4 Si4 C12 -52.91(14) . . . . ? Si5 C4 Si4 C12 70.24(11) . . . . ? Si1 C4 Si4 C12 -166.59(9) . . . . ? C3 C4 Si5 C15 -150.67(13) . . . . ? Si4 C4 Si5 C15 86.71(12) . . . . ? Si1 C4 Si5 C15 -32.86(13) . . . . ? C3 C4 Si5 C14 -28.27(15) . . . . ? Si4 C4 Si5 C14 -150.89(10) . . . . ? Si1 C4 Si5 C14 89.54(12) . . . . ? C3 C4 Si5 C16 88.52(14) . . . . ? Si4 C4 Si5 C16 -34.10(13) . . . . ? Si1 C4 Si5 C16 -153.67(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.556 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.064 #===END data_(silylene)(Me3P)2Pt_cw17 _database_code_depnum_ccdc_archive 'CCDC 775910' #TrackingRef '- silylenecomplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H58 P2 Pt Si5' _chemical_formula_weight 720.16 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' Si Si 0.0817 0.0704 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.506(2) _cell_length_b 32.484(7) _cell_length_c 11.773(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.417(2) _cell_angle_gamma 90.00 _cell_volume 3360.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 6706 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.43 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.459 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1750 _exptl_absorpt_correction_T_max 0.6641 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36859 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7634 _reflns_number_gt 7094 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0000P)^2^+9.6747P] 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 7634 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.336 _refine_ls_restrained_S_all 1.336 _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 Si1 Si 0.27203(11) 0.13769(3) 0.45916(9) 0.0122(2) Uani 1 1 d . . . C1 C 0.3913(4) 0.11381(12) 0.6140(3) 0.0150(7) Uani 1 1 d . . . C2 C 0.3971(5) 0.14797(11) 0.7099(4) 0.0173(8) Uani 1 1 d . . . H1 H 0.3084 0.1450 0.7338 0.021 Uiso 1 1 calc R . . H2 H 0.4907 0.1447 0.7846 0.021 Uiso 1 1 calc R . . C3 C 0.3954(4) 0.19078(11) 0.6544(3) 0.0161(8) Uani 1 1 d . . . H3 H 0.4977 0.1972 0.6553 0.019 Uiso 1 1 calc R . . H4 H 0.3702 0.2117 0.7048 0.019 Uiso 1 1 calc R . . C4 C 0.2754(4) 0.19266(11) 0.5191(4) 0.0155(8) Uani 1 1 d . . . Pt1 Pt 0.165057(16) 0.110682(4) 0.273311(13) 0.01293(4) Uani 1 1 d . . . P1 P -0.06694(12) 0.08035(3) 0.18476(9) 0.0168(2) Uani 1 1 d . . . P2 P 0.26674(12) 0.10565(3) 0.12765(9) 0.0172(2) Uani 1 1 d . . . Si2 Si 0.28081(13) 0.06742(3) 0.63225(10) 0.0165(2) Uani 1 1 d . . . C5 C 0.0798(5) 0.08114(14) 0.6100(4) 0.0241(9) Uani 1 1 d . . . H5 H 0.0334 0.0971 0.5342 0.036 Uiso 1 1 calc R . . H6 H 0.0802 0.0975 0.6800 0.036 Uiso 1 1 calc R . . H7 H 0.0210 0.0559 0.6042 0.036 Uiso 1 1 calc R . . C6 C 0.3633(5) 0.04645(13) 0.7938(4) 0.0240(9) Uani 1 1 d . . . H8 H 0.2833 0.0324 0.8124 0.036 Uiso 1 1 calc R . . H9 H 0.4048 0.0691 0.8518 0.036 Uiso 1 1 calc R . . H10 H 0.4447 0.0269 0.8010 0.036 Uiso 1 1 calc R . . C7 C 0.2728(5) 0.02626(13) 0.5188(4) 0.0262(10) Uani 1 1 d . . . H11 H 0.2061 0.0040 0.5242 0.039 Uiso 1 1 calc R . . H12 H 0.3753 0.0154 0.5372 0.039 Uiso 1 1 calc R . . H13 H 0.2327 0.0378 0.4357 0.039 Uiso 1 1 calc R . . Si3 Si 0.58935(12) 0.09790(3) 0.62582(10) 0.0164(2) Uani 1 1 d . . . C8 C 0.6735(5) 0.05277(13) 0.7300(4) 0.0268(9) Uani 1 1 d . . . H14 H 0.7771 0.0477 0.7343 0.040 Uiso 1 1 calc R . . H15 H 0.6108 0.0283 0.6975 0.040 Uiso 1 1 calc R . . H16 H 0.6765 0.0588 0.8124 0.040 Uiso 1 1 calc R . . C9 C 0.5949(5) 0.08316(13) 0.4741(4) 0.0240(9) Uani 1 1 d . . . H17 H 0.6944 0.0712 0.4868 0.036 Uiso 1 1 calc R . . H18 H 0.5784 0.1077 0.4221 0.036 Uiso 1 1 calc R . . H19 H 0.5149 0.0629 0.4340 0.036 Uiso 1 1 calc R . . C10 C 0.7319(5) 0.13970(13) 0.6939(4) 0.0269(10) Uani 1 1 d . . . H20 H 0.7282 0.1484 0.7724 0.040 Uiso 1 1 calc R . . H21 H 0.7083 0.1632 0.6375 0.040 Uiso 1 1 calc R . . H22 H 0.8340 0.1294 0.7076 0.040 Uiso 1 1 calc R . . Si4 Si 0.08232(13) 0.21056(4) 0.51248(12) 0.0237(3) Uani 1 1 d . . . C11 C 0.0535(6) 0.19715(16) 0.6563(5) 0.0401(13) Uani 1 1 d . . . H23 H -0.0414 0.2095 0.6542 0.060 Uiso 1 1 calc R . . H24 H 0.1390 0.2077 0.7275 0.060 Uiso 1 1 calc R . . H25 H 0.0480 0.1672 0.6628 0.060 Uiso 1 1 calc R . . C12 C 0.0569(6) 0.26794(14) 0.5041(5) 0.0338(11) Uani 1 1 d . . . H26 H 0.0619 0.2781 0.4274 0.051 Uiso 1 1 calc R . . H27 H 0.1378 0.2807 0.5742 0.051 Uiso 1 1 calc R . . H28 H -0.0423 0.2749 0.5065 0.051 Uiso 1 1 calc R . . C13 C -0.0792(5) 0.18930(18) 0.3778(5) 0.0447(14) Uani 1 1 d . . . H29 H -0.0874 0.1596 0.3887 0.067 Uiso 1 1 calc R . . H30 H -0.0608 0.1943 0.3025 0.067 Uiso 1 1 calc R . . H31 H -0.1741 0.2028 0.3715 0.067 Uiso 1 1 calc R . . Si5 Si 0.34693(13) 0.22645(3) 0.42100(10) 0.0184(2) Uani 1 1 d . . . C14 C 0.5343(5) 0.20794(14) 0.4221(4) 0.0257(9) Uani 1 1 d . . . H32 H 0.5307 0.1780 0.4110 0.039 Uiso 1 1 calc R . . H33 H 0.6153 0.2150 0.5008 0.039 Uiso 1 1 calc R . . H34 H 0.5546 0.2211 0.3550 0.039 Uiso 1 1 calc R . . C15 C 0.2088(5) 0.22700(13) 0.2590(4) 0.0263(9) Uani 1 1 d . . . H35 H 0.2513 0.2427 0.2086 0.039 Uiso 1 1 calc R . . H36 H 0.1136 0.2399 0.2548 0.039 Uiso 1 1 calc R . . H37 H 0.1884 0.1987 0.2282 0.039 Uiso 1 1 calc R . . C16 C 0.3844(5) 0.28143(13) 0.4744(4) 0.0304(10) Uani 1 1 d . . . H38 H 0.4574 0.2937 0.4438 0.046 Uiso 1 1 calc R . . H39 H 0.4265 0.2822 0.5645 0.046 Uiso 1 1 calc R . . H40 H 0.2890 0.2970 0.4429 0.046 Uiso 1 1 calc R . . C17 C -0.2119(5) 0.11082(15) 0.0673(4) 0.0288(10) Uani 1 1 d . . . H41 H -0.3081 0.0955 0.0366 0.043 Uiso 1 1 calc R . . H42 H -0.1791 0.1163 -0.0007 0.043 Uiso 1 1 calc R . . H43 H -0.2263 0.1370 0.1030 0.043 Uiso 1 1 calc R . . C18 C -0.0757(5) 0.03194(13) 0.1037(4) 0.0281(10) Uani 1 1 d . . . H44 H -0.0087 0.0117 0.1604 0.042 Uiso 1 1 calc R . . H45 H -0.0426 0.0365 0.0354 0.042 Uiso 1 1 calc R . . H46 H -0.1805 0.0216 0.0716 0.042 Uiso 1 1 calc R . . C19 C -0.1702(5) 0.06542(15) 0.2807(4) 0.0293(10) Uani 1 1 d . . . H47 H -0.2667 0.0524 0.2296 0.044 Uiso 1 1 calc R . . H48 H -0.1906 0.0899 0.3206 0.044 Uiso 1 1 calc R . . H49 H -0.1088 0.0459 0.3435 0.044 Uiso 1 1 calc R . . C20 C 0.3561(5) 0.05603(13) 0.1269(4) 0.0241(9) Uani 1 1 d . . . H50 H 0.3962 0.0558 0.0615 0.036 Uiso 1 1 calc R . . H51 H 0.2806 0.0341 0.1122 0.036 Uiso 1 1 calc R . . H52 H 0.4395 0.0516 0.2064 0.036 Uiso 1 1 calc R . . C21 C 0.1405(5) 0.11139(16) -0.0337(4) 0.0307(10) Uani 1 1 d . . . H53 H 0.0927 0.1386 -0.0465 0.046 Uiso 1 1 calc R . . H54 H 0.0616 0.0901 -0.0555 0.046 Uiso 1 1 calc R . . H55 H 0.1996 0.1085 -0.0857 0.046 Uiso 1 1 calc R . . C22 C 0.4172(6) 0.14101(15) 0.1334(5) 0.0325(11) Uani 1 1 d . . . H56 H 0.4460 0.1360 0.0630 0.049 Uiso 1 1 calc R . . H57 H 0.5059 0.1367 0.2098 0.049 Uiso 1 1 calc R . . H58 H 0.3811 0.1694 0.1304 0.049 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 Si1 0.0120(5) 0.0128(5) 0.0123(5) -0.0009(4) 0.0052(4) -0.0006(4) C1 0.0173(18) 0.0154(18) 0.0135(18) -0.0020(15) 0.0073(14) -0.0002(15) C2 0.019(2) 0.0171(19) 0.0146(19) -0.0023(15) 0.0054(16) -0.0004(15) C3 0.0172(19) 0.0150(18) 0.0147(19) -0.0038(14) 0.0044(15) -0.0018(14) C4 0.0144(18) 0.0132(18) 0.018(2) -0.0011(14) 0.0057(15) 0.0018(14) Pt1 0.01296(7) 0.01416(7) 0.01244(7) -0.00189(6) 0.00572(5) -0.00118(6) P1 0.0169(5) 0.0184(5) 0.0150(5) -0.0041(4) 0.0062(4) -0.0043(4) P2 0.0202(5) 0.0191(5) 0.0151(5) 0.0013(4) 0.0099(4) 0.0022(4) Si2 0.0224(6) 0.0137(5) 0.0165(5) -0.0011(4) 0.0109(4) -0.0030(4) C5 0.024(2) 0.032(2) 0.021(2) -0.0031(18) 0.0130(18) -0.0050(18) C6 0.034(2) 0.018(2) 0.022(2) 0.0009(16) 0.0138(19) -0.0030(17) C7 0.038(3) 0.016(2) 0.026(2) -0.0037(17) 0.014(2) -0.0050(18) Si3 0.0148(5) 0.0175(5) 0.0167(5) 0.0024(4) 0.0058(4) 0.0033(4) C8 0.028(2) 0.026(2) 0.025(2) 0.0067(18) 0.0094(19) 0.0072(18) C9 0.025(2) 0.025(2) 0.026(2) 0.0051(17) 0.0142(18) 0.0121(17) C10 0.015(2) 0.027(2) 0.033(3) 0.0026(19) 0.0024(18) -0.0006(17) Si4 0.0173(6) 0.0217(6) 0.0314(7) -0.0088(5) 0.0086(5) 0.0034(4) C11 0.036(3) 0.037(3) 0.062(4) -0.002(2) 0.035(3) 0.007(2) C12 0.033(3) 0.028(2) 0.039(3) -0.005(2) 0.011(2) 0.015(2) C13 0.015(2) 0.052(3) 0.061(4) -0.025(3) 0.007(2) 0.004(2) Si5 0.0180(5) 0.0137(5) 0.0188(6) 0.0023(4) 0.0018(4) 0.0000(4) C14 0.022(2) 0.029(2) 0.026(2) 0.0068(18) 0.0096(18) -0.0019(18) C15 0.026(2) 0.022(2) 0.028(2) 0.0022(17) 0.0067(19) 0.0040(17) C16 0.035(3) 0.015(2) 0.031(3) 0.0023(18) 0.002(2) -0.0028(18) C17 0.017(2) 0.034(2) 0.030(2) -0.001(2) 0.0025(18) -0.0002(19) C18 0.032(2) 0.024(2) 0.029(2) -0.0098(18) 0.012(2) -0.0064(19) C19 0.024(2) 0.041(3) 0.026(2) -0.007(2) 0.0131(19) -0.014(2) C20 0.029(2) 0.026(2) 0.021(2) 0.0010(17) 0.0130(18) 0.0087(18) C21 0.032(2) 0.044(3) 0.018(2) 0.007(2) 0.0102(18) 0.012(2) C22 0.036(3) 0.038(3) 0.034(3) -0.002(2) 0.026(2) -0.008(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 Si1 C1 1.907(4) . ? Si1 C4 1.916(4) . ? Si1 Pt1 2.2123(11) . ? C1 C2 1.569(5) . ? C1 Si2 1.895(4) . ? C1 Si3 1.906(4) . ? C2 C3 1.534(5) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.568(5) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 Si5 1.897(4) . ? C4 Si4 1.898(4) . ? Pt1 P2 2.2729(10) . ? Pt1 P1 2.2733(11) . ? P1 C19 1.822(4) . ? P1 C18 1.825(4) . ? P1 C17 1.827(4) . ? P2 C22 1.816(5) . ? P2 C20 1.824(4) . ? P2 C21 1.829(4) . ? Si2 C7 1.870(4) . ? Si2 C5 1.881(4) . ? Si2 C6 1.886(4) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? Si3 C9 1.869(4) . ? Si3 C10 1.870(4) . ? Si3 C8 1.883(4) . ? C8 H14 0.9800 . ? C8 H15 0.9800 . ? C8 H16 0.9800 . ? C9 H17 0.9800 . ? C9 H18 0.9800 . ? C9 H19 0.9800 . ? C10 H20 0.9800 . ? C10 H21 0.9800 . ? C10 H22 0.9800 . ? Si4 C11 1.867(5) . ? Si4 C13 1.868(5) . ? Si4 C12 1.877(5) . ? C11 H23 0.9800 . ? C11 H24 0.9800 . ? C11 H25 0.9800 . ? C12 H26 0.9800 . ? C12 H27 0.9800 . ? C12 H28 0.9800 . ? C13 H29 0.9800 . ? C13 H30 0.9800 . ? C13 H31 0.9800 . ? Si5 C15 1.858(4) . ? Si5 C14 1.875(4) . ? Si5 C16 1.882(4) . ? C14 H32 0.9800 . ? C14 H33 0.9800 . ? C14 H34 0.9800 . ? C15 H35 0.9800 . ? C15 H36 0.9800 . ? C15 H37 0.9800 . ? C16 H38 0.9800 . ? C16 H39 0.9800 . ? C16 H40 0.9800 . ? C17 H41 0.9800 . ? C17 H42 0.9800 . ? C17 H43 0.9800 . ? C18 H44 0.9800 . ? C18 H45 0.9800 . ? C18 H46 0.9800 . ? C19 H47 0.9800 . ? C19 H48 0.9800 . ? C19 H49 0.9800 . ? C20 H50 0.9800 . ? C20 H51 0.9800 . ? C20 H52 0.9800 . ? C21 H53 0.9800 . ? C21 H54 0.9800 . ? C21 H55 0.9800 . ? C22 H56 0.9800 . ? C22 H57 0.9800 . ? C22 H58 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C4 96.13(17) . . ? C1 Si1 Pt1 131.76(12) . . ? C4 Si1 Pt1 132.11(13) . . ? C2 C1 Si2 110.5(2) . . ? C2 C1 Si3 112.1(3) . . ? Si2 C1 Si3 110.53(19) . . ? C2 C1 Si1 104.2(2) . . ? Si2 C1 Si1 106.18(19) . . ? Si3 C1 Si1 112.98(19) . . ? C3 C2 C1 110.1(3) . . ? C3 C2 H1 109.6 . . ? C1 C2 H1 109.6 . . ? C3 C2 H2 109.6 . . ? C1 C2 H2 109.6 . . ? H1 C2 H2 108.2 . . ? C2 C3 C4 110.7(3) . . ? C2 C3 H3 109.5 . . ? C4 C3 H3 109.5 . . ? C2 C3 H4 109.5 . . ? C4 C3 H4 109.5 . . ? H3 C3 H4 108.1 . . ? C3 C4 Si5 110.5(3) . . ? C3 C4 Si4 111.8(3) . . ? Si5 C4 Si4 111.30(19) . . ? C3 C4 Si1 104.0(2) . . ? Si5 C4 Si1 105.95(19) . . ? Si4 C4 Si1 112.98(19) . . ? Si1 Pt1 P2 127.40(4) . . ? Si1 Pt1 P1 128.69(4) . . ? P2 Pt1 P1 103.89(4) . . ? C19 P1 C18 99.6(2) . . ? C19 P1 C17 100.6(2) . . ? C18 P1 C17 101.5(2) . . ? C19 P1 Pt1 119.25(15) . . ? C18 P1 Pt1 117.14(16) . . ? C17 P1 Pt1 115.60(15) . . ? C22 P2 C20 101.4(2) . . ? C22 P2 C21 99.8(2) . . ? C20 P2 C21 101.9(2) . . ? C22 P2 Pt1 118.84(16) . . ? C20 P2 Pt1 113.60(14) . . ? C21 P2 Pt1 118.51(15) . . ? C7 Si2 C5 107.9(2) . . ? C7 Si2 C6 110.5(2) . . ? C5 Si2 C6 103.6(2) . . ? C7 Si2 C1 111.18(18) . . ? C5 Si2 C1 111.91(18) . . ? C6 Si2 C1 111.47(18) . . ? Si2 C5 H5 109.5 . . ? Si2 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? Si2 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? Si2 C6 H8 109.5 . . ? Si2 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? Si2 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? Si2 C7 H11 109.5 . . ? Si2 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si2 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? C9 Si3 C10 108.4(2) . . ? C9 Si3 C8 105.3(2) . . ? C10 Si3 C8 103.2(2) . . ? C9 Si3 C1 112.78(18) . . ? C10 Si3 C1 111.63(19) . . ? C8 Si3 C1 114.90(19) . . ? Si3 C8 H14 109.5 . . ? Si3 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? Si3 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? Si3 C9 H17 109.5 . . ? Si3 C9 H18 109.5 . . ? H17 C9 H18 109.5 . . ? Si3 C9 H19 109.5 . . ? H17 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? Si3 C10 H20 109.5 . . ? Si3 C10 H21 109.5 . . ? H20 C10 H21 109.5 . . ? Si3 C10 H22 109.5 . . ? H20 C10 H22 109.5 . . ? H21 C10 H22 109.5 . . ? C11 Si4 C13 109.1(3) . . ? C11 Si4 C12 102.6(2) . . ? C13 Si4 C12 105.9(2) . . ? C11 Si4 C4 111.4(2) . . ? C13 Si4 C4 113.0(2) . . ? C12 Si4 C4 114.2(2) . . ? Si4 C11 H23 109.5 . . ? Si4 C11 H24 109.5 . . ? H23 C11 H24 109.5 . . ? Si4 C11 H25 109.5 . . ? H23 C11 H25 109.5 . . ? H24 C11 H25 109.5 . . ? Si4 C12 H26 109.5 . . ? Si4 C12 H27 109.5 . . ? H26 C12 H27 109.5 . . ? Si4 C12 H28 109.5 . . ? H26 C12 H28 109.5 . . ? H27 C12 H28 109.5 . . ? Si4 C13 H29 109.5 . . ? Si4 C13 H30 109.5 . . ? H29 C13 H30 109.5 . . ? Si4 C13 H31 109.5 . . ? H29 C13 H31 109.5 . . ? H30 C13 H31 109.5 . . ? C15 Si5 C14 107.9(2) . . ? C15 Si5 C16 107.7(2) . . ? C14 Si5 C16 104.1(2) . . ? C15 Si5 C4 110.67(19) . . ? C14 Si5 C4 111.73(18) . . ? C16 Si5 C4 114.3(2) . . ? Si5 C14 H32 109.5 . . ? Si5 C14 H33 109.5 . . ? H32 C14 H33 109.5 . . ? Si5 C14 H34 109.5 . . ? H32 C14 H34 109.5 . . ? H33 C14 H34 109.5 . . ? Si5 C15 H35 109.5 . . ? Si5 C15 H36 109.5 . . ? H35 C15 H36 109.5 . . ? Si5 C15 H37 109.5 . . ? H35 C15 H37 109.5 . . ? H36 C15 H37 109.5 . . ? Si5 C16 H38 109.5 . . ? Si5 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? Si5 C16 H40 109.5 . . ? H38 C16 H40 109.5 . . ? H39 C16 H40 109.5 . . ? P1 C17 H41 109.5 . . ? P1 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? P1 C17 H43 109.5 . . ? H41 C17 H43 109.5 . . ? H42 C17 H43 109.5 . . ? P1 C18 H44 109.5 . . ? P1 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? P1 C18 H46 109.5 . . ? H44 C18 H46 109.5 . . ? H45 C18 H46 109.5 . . ? P1 C19 H47 109.5 . . ? P1 C19 H48 109.5 . . ? H47 C19 H48 109.5 . . ? P1 C19 H49 109.5 . . ? H47 C19 H49 109.5 . . ? H48 C19 H49 109.5 . . ? P2 C20 H50 109.5 . . ? P2 C20 H51 109.5 . . ? H50 C20 H51 109.5 . . ? P2 C20 H52 109.5 . . ? H50 C20 H52 109.5 . . ? H51 C20 H52 109.5 . . ? P2 C21 H53 109.5 . . ? P2 C21 H54 109.5 . . ? H53 C21 H54 109.5 . . ? P2 C21 H55 109.5 . . ? H53 C21 H55 109.5 . . ? H54 C21 H55 109.5 . . ? P2 C22 H56 109.5 . . ? P2 C22 H57 109.5 . . ? H56 C22 H57 109.5 . . ? P2 C22 H58 109.5 . . ? H56 C22 H58 109.5 . . ? H57 C22 H58 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 C1 C2 12.4(3) . . . . ? Pt1 Si1 C1 C2 -167.33(18) . . . . ? C4 Si1 C1 Si2 129.08(18) . . . . ? Pt1 Si1 C1 Si2 -50.6(2) . . . . ? C4 Si1 C1 Si3 -109.6(2) . . . . ? Pt1 Si1 C1 Si3 70.7(2) . . . . ? Si2 C1 C2 C3 -146.4(3) . . . . ? Si3 C1 C2 C3 89.8(3) . . . . ? Si1 C1 C2 C3 -32.7(3) . . . . ? C1 C2 C3 C4 43.5(4) . . . . ? C2 C3 C4 Si5 -144.3(3) . . . . ? C2 C3 C4 Si4 91.1(3) . . . . ? C2 C3 C4 Si1 -31.0(4) . . . . ? C1 Si1 C4 C3 9.9(3) . . . . ? Pt1 Si1 C4 C3 -170.40(17) . . . . ? C1 Si1 C4 Si5 126.43(19) . . . . ? Pt1 Si1 C4 Si5 -53.9(2) . . . . ? C1 Si1 C4 Si4 -111.5(2) . . . . ? Pt1 Si1 C4 Si4 68.2(2) . . . . ? C1 Si1 Pt1 P2 -91.84(16) . . . . ? C4 Si1 Pt1 P2 88.57(17) . . . . ? C1 Si1 Pt1 P1 86.55(17) . . . . ? C4 Si1 Pt1 P1 -93.04(17) . . . . ? Si1 Pt1 P1 C19 -14.2(2) . . . . ? P2 Pt1 P1 C19 164.44(19) . . . . ? Si1 Pt1 P1 C18 -134.40(18) . . . . ? P2 Pt1 P1 C18 44.28(18) . . . . ? Si1 Pt1 P1 C17 105.94(18) . . . . ? P2 Pt1 P1 C17 -75.37(18) . . . . ? Si1 Pt1 P2 C22 -23.3(2) . . . . ? P1 Pt1 P2 C22 158.0(2) . . . . ? Si1 Pt1 P2 C20 95.77(17) . . . . ? P1 Pt1 P2 C20 -82.94(17) . . . . ? Si1 Pt1 P2 C21 -144.61(19) . . . . ? P1 Pt1 P2 C21 36.7(2) . . . . ? C2 C1 Si2 C7 -179.9(3) . . . . ? Si3 C1 Si2 C7 -55.2(3) . . . . ? Si1 C1 Si2 C7 67.7(2) . . . . ? C2 C1 Si2 C5 59.4(3) . . . . ? Si3 C1 Si2 C5 -175.92(19) . . . . ? Si1 C1 Si2 C5 -53.0(2) . . . . ? C2 C1 Si2 C6 -56.2(3) . . . . ? Si3 C1 Si2 C6 68.5(2) . . . . ? Si1 C1 Si2 C6 -168.60(18) . . . . ? C2 C1 Si3 C9 -147.1(3) . . . . ? Si2 C1 Si3 C9 89.2(2) . . . . ? Si1 C1 Si3 C9 -29.7(3) . . . . ? C2 C1 Si3 C10 -24.7(3) . . . . ? Si2 C1 Si3 C10 -148.5(2) . . . . ? Si1 C1 Si3 C10 92.7(2) . . . . ? C2 C1 Si3 C8 92.3(3) . . . . ? Si2 C1 Si3 C8 -31.5(3) . . . . ? Si1 C1 Si3 C8 -150.3(2) . . . . ? C3 C4 Si4 C11 -27.8(3) . . . . ? Si5 C4 Si4 C11 -151.9(2) . . . . ? Si1 C4 Si4 C11 89.1(3) . . . . ? C3 C4 Si4 C13 -150.9(3) . . . . ? Si5 C4 Si4 C13 85.0(3) . . . . ? Si1 C4 Si4 C13 -34.1(3) . . . . ? C3 C4 Si4 C12 87.9(3) . . . . ? Si5 C4 Si4 C12 -36.2(3) . . . . ? Si1 C4 Si4 C12 -155.2(2) . . . . ? C3 C4 Si5 C15 177.6(3) . . . . ? Si4 C4 Si5 C15 -57.6(3) . . . . ? Si1 C4 Si5 C15 65.6(2) . . . . ? C3 C4 Si5 C14 57.3(3) . . . . ? Si4 C4 Si5 C14 -177.9(2) . . . . ? Si1 C4 Si5 C14 -54.7(2) . . . . ? C3 C4 Si5 C16 -60.6(3) . . . . ? Si4 C4 Si5 C16 64.2(3) . . . . ? Si1 C4 Si5 C16 -172.64(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.430 _refine_diff_density_min -3.381 _refine_diff_density_rms 0.120 #===END data_(silylene)(toluene)Ni_cw19 _database_code_depnum_ccdc_archive 'CCDC 775911' #TrackingRef '- silylenecomplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H48 Ni Si5' _chemical_formula_weight 523.77 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 9.386(3) _cell_length_b 10.766(4) _cell_length_c 16.176(6) _cell_angle_alpha 73.590(4) _cell_angle_beta 74.064(4) _cell_angle_gamma 70.214(4) _cell_volume 1446.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 5015 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.40 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7180 _exptl_absorpt_correction_T_max 0.9165 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16070 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6437 _reflns_number_gt 5112 _reflns_threshold_expression >2sigma _computing_data_collection 'APEX2 ' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0925P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6437 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Si1 Si 0.40948(9) 0.21145(8) 0.23323(5) 0.01417(18) Uani 1 1 d . . . C1 C 0.5663(3) 0.0473(3) 0.26008(18) 0.0150(6) Uani 1 1 d . . . C2 C 0.5906(3) 0.0455(3) 0.35267(18) 0.0169(6) Uani 1 1 d . . . H1 H 0.6318 -0.0488 0.3832 0.020 Uiso 1 1 calc R . . H2 H 0.6664 0.0950 0.3454 0.020 Uiso 1 1 calc R . . C3 C 0.4362(3) 0.1119(3) 0.40783(18) 0.0172(6) Uani 1 1 d . . . H3 H 0.4557 0.1363 0.4575 0.021 Uiso 1 1 calc R . . H4 H 0.3738 0.0471 0.4324 0.021 Uiso 1 1 calc R . . C4 C 0.3442(3) 0.2420(3) 0.35001(18) 0.0147(6) Uani 1 1 d . . . Ni1 Ni 0.32353(4) 0.31282(4) 0.11824(2) 0.01564(13) Uani 1 1 d . . . C5 C 0.1702(3) 0.5028(3) 0.06227(19) 0.0195(6) Uani 1 1 d . . . C6 C 0.3179(4) 0.4817(3) 0.00753(19) 0.0209(6) Uani 1 1 d . . . H5 H 0.3687 0.5503 -0.0093 0.025 Uiso 1 1 calc R . . C7 C 0.3916(4) 0.3602(3) -0.02270(19) 0.0222(7) Uani 1 1 d . . . H6 H 0.4909 0.3480 -0.0600 0.027 Uiso 1 1 calc R . . C8 C 0.3185(4) 0.2575(3) 0.0023(2) 0.0236(7) Uani 1 1 d . . . H7 H 0.3671 0.1761 -0.0186 0.028 Uiso 1 1 calc R . . C9 C 0.1727(4) 0.2760(3) 0.0586(2) 0.0239(7) Uani 1 1 d . . . H8 H 0.1238 0.2057 0.0773 0.029 Uiso 1 1 calc R . . C10 C 0.0988(4) 0.3980(3) 0.0875(2) 0.0218(6) Uani 1 1 d . . . H9 H -0.0007 0.4101 0.1245 0.026 Uiso 1 1 calc R . . C11 C 0.0920(4) 0.6340(3) 0.0923(2) 0.0250(7) Uani 1 1 d . . . H10 H 0.1703 0.6733 0.0951 0.038 Uiso 1 1 calc R . . H11 H 0.0267 0.6177 0.1507 0.038 Uiso 1 1 calc R . . H12 H 0.0280 0.6967 0.0507 0.038 Uiso 1 1 calc R . . Si2 Si 0.51405(10) -0.10909(8) 0.26085(5) 0.01738(19) Uani 1 1 d . . . C12 C 0.6862(4) -0.2561(3) 0.2380(2) 0.0269(7) Uani 1 1 d . . . H13 H 0.6513 -0.3322 0.2380 0.040 Uiso 1 1 calc R . . H14 H 0.7476 -0.2826 0.2836 0.040 Uiso 1 1 calc R . . H15 H 0.7496 -0.2303 0.1804 0.040 Uiso 1 1 calc R . . C13 C 0.4099(4) -0.1794(3) 0.3724(2) 0.0259(7) Uani 1 1 d . . . H16 H 0.3120 -0.1125 0.3889 0.039 Uiso 1 1 calc R . . H17 H 0.4742 -0.2006 0.4158 0.039 Uiso 1 1 calc R . . H18 H 0.3892 -0.2618 0.3704 0.039 Uiso 1 1 calc R . . C14 C 0.3915(4) -0.0746(3) 0.1784(2) 0.0225(6) Uani 1 1 d . . . H19 H 0.4373 -0.0264 0.1218 0.034 Uiso 1 1 calc R . . H20 H 0.2873 -0.0191 0.1989 0.034 Uiso 1 1 calc R . . H21 H 0.3857 -0.1602 0.1715 0.034 Uiso 1 1 calc R . . Si3 Si 0.75004(9) 0.06296(8) 0.17633(5) 0.01735(19) Uani 1 1 d . . . C15 C 0.9287(4) -0.0618(3) 0.2126(2) 0.0268(7) Uani 1 1 d . . . H22 H 1.0204 -0.0412 0.1718 0.040 Uiso 1 1 calc R . . H23 H 0.9293 -0.1533 0.2131 0.040 Uiso 1 1 calc R . . H24 H 0.9295 -0.0562 0.2719 0.040 Uiso 1 1 calc R . . C16 C 0.7457(4) 0.0464(3) 0.0648(2) 0.0243(7) Uani 1 1 d . . . H25 H 0.8417 0.0569 0.0241 0.036 Uiso 1 1 calc R . . H26 H 0.6576 0.1164 0.0433 0.036 Uiso 1 1 calc R . . H27 H 0.7355 -0.0429 0.0688 0.036 Uiso 1 1 calc R . . C17 C 0.7797(4) 0.2325(3) 0.1631(2) 0.0215(6) Uani 1 1 d . . . H28 H 0.8216 0.2316 0.2126 0.032 Uiso 1 1 calc R . . H29 H 0.6806 0.3025 0.1620 0.032 Uiso 1 1 calc R . . H30 H 0.8523 0.2515 0.1080 0.032 Uiso 1 1 calc R . . Si4 Si 0.12823(9) 0.25981(8) 0.38418(5) 0.01805(19) Uani 1 1 d . . . C18 C 0.0672(4) 0.1439(3) 0.3418(2) 0.0278(7) Uani 1 1 d . . . H31 H -0.0434 0.1539 0.3645 0.042 Uiso 1 1 calc R . . H32 H 0.1260 0.0503 0.3615 0.042 Uiso 1 1 calc R . . H33 H 0.0871 0.1672 0.2774 0.042 Uiso 1 1 calc R . . C19 C 0.0696(4) 0.2137(3) 0.5067(2) 0.0262(7) Uani 1 1 d . . . H34 H 0.0954 0.2724 0.5334 0.039 Uiso 1 1 calc R . . H35 H 0.1246 0.1194 0.5278 0.039 Uiso 1 1 calc R . . H36 H -0.0420 0.2253 0.5229 0.039 Uiso 1 1 calc R . . C20 C 0.0095(4) 0.4327(3) 0.3404(2) 0.0251(7) Uani 1 1 d . . . H37 H -0.1002 0.4363 0.3579 0.038 Uiso 1 1 calc R . . H38 H 0.0386 0.4536 0.2761 0.038 Uiso 1 1 calc R . . H39 H 0.0278 0.4989 0.3643 0.038 Uiso 1 1 calc R . . Si5 Si 0.38483(10) 0.39740(8) 0.36113(5) 0.01766(19) Uani 1 1 d . . . C21 C 0.5915(4) 0.3650(3) 0.3676(2) 0.0247(7) Uani 1 1 d . . . H40 H 0.6050 0.4457 0.3776 0.037 Uiso 1 1 calc R . . H41 H 0.6591 0.3436 0.3123 0.037 Uiso 1 1 calc R . . H42 H 0.6184 0.2889 0.4163 0.037 Uiso 1 1 calc R . . C22 C 0.3414(4) 0.5437(3) 0.2668(2) 0.0261(7) Uani 1 1 d . . . H43 H 0.2334 0.5647 0.2622 0.039 Uiso 1 1 calc R . . H44 H 0.4094 0.5202 0.2121 0.039 Uiso 1 1 calc R . . H45 H 0.3587 0.6226 0.2768 0.039 Uiso 1 1 calc R . . C23 C 0.2725(4) 0.4523(3) 0.4664(2) 0.0259(7) Uani 1 1 d . . . H46 H 0.2969 0.5321 0.4698 0.039 Uiso 1 1 calc R . . H47 H 0.3002 0.3790 0.5164 0.039 Uiso 1 1 calc R . . H48 H 0.1617 0.4745 0.4679 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0165(4) 0.0087(4) 0.0192(4) -0.0040(3) -0.0055(3) -0.0035(3) C1 0.0163(14) 0.0099(13) 0.0197(14) -0.0051(10) -0.0041(11) -0.0027(11) C2 0.0186(15) 0.0115(14) 0.0219(14) -0.0027(11) -0.0087(12) -0.0031(11) C3 0.0207(15) 0.0120(14) 0.0202(14) -0.0032(11) -0.0067(11) -0.0041(12) C4 0.0164(14) 0.0100(13) 0.0183(13) -0.0038(10) -0.0031(11) -0.0042(11) Ni1 0.0179(2) 0.0108(2) 0.0201(2) -0.00348(14) -0.00651(15) -0.00403(15) C5 0.0190(15) 0.0157(15) 0.0249(15) -0.0014(12) -0.0123(12) -0.0024(12) C6 0.0234(16) 0.0158(15) 0.0240(15) 0.0005(12) -0.0098(12) -0.0059(13) C7 0.0207(16) 0.0244(17) 0.0201(15) -0.0054(12) -0.0059(12) -0.0025(13) C8 0.0318(18) 0.0177(16) 0.0252(16) -0.0084(12) -0.0117(13) -0.0038(13) C9 0.0270(18) 0.0216(16) 0.0304(16) -0.0040(13) -0.0138(13) -0.0107(14) C10 0.0174(15) 0.0229(17) 0.0260(16) -0.0027(12) -0.0099(12) -0.0043(13) C11 0.0274(18) 0.0190(16) 0.0279(16) -0.0053(13) -0.0107(13) -0.0012(13) Si2 0.0195(4) 0.0089(4) 0.0250(4) -0.0046(3) -0.0051(3) -0.0042(3) C12 0.0263(18) 0.0131(15) 0.0409(19) -0.0090(13) -0.0081(14) -0.0011(13) C13 0.0301(18) 0.0175(16) 0.0322(17) -0.0031(13) -0.0064(14) -0.0108(14) C14 0.0258(17) 0.0139(15) 0.0307(16) -0.0075(12) -0.0065(13) -0.0064(13) Si3 0.0159(4) 0.0145(4) 0.0230(4) -0.0067(3) -0.0035(3) -0.0040(3) C15 0.0207(17) 0.0201(17) 0.0396(19) -0.0110(14) -0.0082(14) -0.0001(13) C16 0.0224(17) 0.0247(17) 0.0272(16) -0.0106(13) -0.0021(13) -0.0064(13) C17 0.0215(16) 0.0188(16) 0.0253(15) -0.0041(12) -0.0020(12) -0.0097(13) Si4 0.0168(4) 0.0133(4) 0.0234(4) -0.0041(3) -0.0039(3) -0.0033(3) C18 0.0220(17) 0.0246(18) 0.0417(19) -0.0110(15) -0.0068(14) -0.0090(14) C19 0.0254(18) 0.0247(18) 0.0247(16) -0.0028(13) -0.0010(13) -0.0072(14) C20 0.0212(16) 0.0199(17) 0.0297(17) -0.0038(13) -0.0058(13) -0.0005(13) Si5 0.0232(4) 0.0112(4) 0.0216(4) -0.0056(3) -0.0056(3) -0.0059(3) C21 0.0230(17) 0.0244(17) 0.0332(17) -0.0125(14) -0.0049(13) -0.0102(14) C22 0.040(2) 0.0133(16) 0.0309(17) -0.0039(12) -0.0117(15) -0.0125(14) C23 0.0337(19) 0.0203(17) 0.0275(16) -0.0112(13) -0.0063(14) -0.0073(14) _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 Si1 C4 1.906(3) . ? Si1 C1 1.906(3) . ? Si1 Ni1 2.0936(10) . ? C1 C2 1.570(4) . ? C1 Si2 1.902(3) . ? C1 Si3 1.904(3) . ? C2 C3 1.535(4) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.570(4) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 Si5 1.902(3) . ? C4 Si4 1.906(3) . ? Ni1 C9 2.107(3) . ? Ni1 C10 2.132(3) . ? Ni1 C8 2.138(3) . ? Ni1 C7 2.152(3) . ? Ni1 C6 2.159(3) . ? Ni1 C5 2.180(3) . ? C5 C6 1.409(4) . ? C5 C10 1.410(4) . ? C5 C11 1.504(4) . ? C6 C7 1.411(4) . ? C6 H5 0.9500 . ? C7 C8 1.402(4) . ? C7 H6 0.9500 . ? C8 C9 1.406(4) . ? C8 H7 0.9500 . ? C9 C10 1.406(5) . ? C9 H8 0.9500 . ? C10 H9 0.9500 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C11 H12 0.9800 . ? Si2 C14 1.874(3) . ? Si2 C12 1.877(3) . ? Si2 C13 1.883(3) . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C12 H15 0.9800 . ? C13 H16 0.9800 . ? C13 H17 0.9800 . ? C13 H18 0.9800 . ? C14 H19 0.9800 . ? C14 H20 0.9800 . ? C14 H21 0.9800 . ? Si3 C16 1.875(3) . ? Si3 C15 1.879(3) . ? Si3 C17 1.883(3) . ? C15 H22 0.9800 . ? C15 H23 0.9800 . ? C15 H24 0.9800 . ? C16 H25 0.9800 . ? C16 H26 0.9800 . ? C16 H27 0.9800 . ? C17 H28 0.9800 . ? C17 H29 0.9800 . ? C17 H30 0.9800 . ? Si4 C20 1.869(3) . ? Si4 C19 1.872(3) . ? Si4 C18 1.880(3) . ? C18 H31 0.9800 . ? C18 H32 0.9800 . ? C18 H33 0.9800 . ? C19 H34 0.9800 . ? C19 H35 0.9800 . ? C19 H36 0.9800 . ? C20 H37 0.9800 . ? C20 H38 0.9800 . ? C20 H39 0.9800 . ? Si5 C23 1.876(3) . ? Si5 C22 1.877(3) . ? Si5 C21 1.879(3) . ? C21 H40 0.9800 . ? C21 H41 0.9800 . ? C21 H42 0.9800 . ? C22 H43 0.9800 . ? C22 H44 0.9800 . ? C22 H45 0.9800 . ? C23 H46 0.9800 . ? C23 H47 0.9800 . ? C23 H48 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 C4 Si1 C1 95.44(12) . . ? C4 Si1 Ni1 132.07(10) . . ? C1 Si1 Ni1 132.24(9) . . ? C2 C1 Si2 111.62(19) . . ? C2 C1 Si3 108.22(18) . . ? Si2 C1 Si3 111.45(14) . . ? C2 C1 Si1 104.64(18) . . ? Si2 C1 Si1 113.52(14) . . ? Si3 C1 Si1 106.98(14) . . ? C3 C2 C1 109.8(2) . . ? C3 C2 H1 109.7 . . ? C1 C2 H1 109.7 . . ? C3 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? H1 C2 H2 108.2 . . ? C2 C3 C4 110.6(2) . . ? C2 C3 H3 109.5 . . ? C4 C3 H3 109.5 . . ? C2 C3 H4 109.5 . . ? C4 C3 H4 109.5 . . ? H3 C3 H4 108.1 . . ? C3 C4 Si5 110.11(18) . . ? C3 C4 Si1 105.38(18) . . ? Si5 C4 Si1 113.22(14) . . ? C3 C4 Si4 110.37(19) . . ? Si5 C4 Si4 110.13(14) . . ? Si1 C4 Si4 107.51(13) . . ? Si1 Ni1 C9 131.73(9) . . ? Si1 Ni1 C10 134.89(9) . . ? C9 Ni1 C10 38.74(12) . . ? Si1 Ni1 C8 135.55(9) . . ? C9 Ni1 C8 38.68(12) . . ? C10 Ni1 C8 69.64(12) . . ? Si1 Ni1 C7 142.75(9) . . ? C9 Ni1 C7 69.41(12) . . ? C10 Ni1 C7 81.75(12) . . ? C8 Ni1 C7 38.15(12) . . ? Si1 Ni1 C6 146.24(8) . . ? C9 Ni1 C6 82.01(12) . . ? C10 Ni1 C6 68.59(12) . . ? C8 Ni1 C6 69.08(12) . . ? C7 Ni1 C6 38.22(12) . . ? Si1 Ni1 C5 141.45(8) . . ? C9 Ni1 C5 69.74(12) . . ? C10 Ni1 C5 38.17(11) . . ? C8 Ni1 C5 82.28(12) . . ? C7 Ni1 C5 69.08(12) . . ? C6 Ni1 C5 37.89(11) . . ? C6 C5 C10 118.1(3) . . ? C6 C5 C11 120.4(3) . . ? C10 C5 C11 121.5(3) . . ? C6 C5 Ni1 70.26(16) . . ? C10 C5 Ni1 69.09(17) . . ? C11 C5 Ni1 132.6(2) . . ? C5 C6 C7 121.1(3) . . ? C5 C6 Ni1 71.85(17) . . ? C7 C6 Ni1 70.61(18) . . ? C5 C6 H5 119.4 . . ? C7 C6 H5 119.4 . . ? Ni1 C6 H5 130.9 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 Ni1 70.41(17) . . ? C6 C7 Ni1 71.17(17) . . ? C8 C7 H6 120.0 . . ? C6 C7 H6 120.0 . . ? Ni1 C7 H6 131.2 . . ? C7 C8 C9 119.4(3) . . ? C7 C8 Ni1 71.44(17) . . ? C9 C8 Ni1 69.44(17) . . ? C7 C8 H7 120.3 . . ? C9 C8 H7 120.3 . . ? Ni1 C8 H7 131.6 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 Ni1 71.61(17) . . ? C8 C9 Ni1 71.88(17) . . ? C10 C9 H8 119.9 . . ? C8 C9 H8 119.9 . . ? Ni1 C9 H8 129.0 . . ? C9 C10 C5 121.0(3) . . ? C9 C10 Ni1 69.65(17) . . ? C5 C10 Ni1 72.75(17) . . ? C9 C10 H9 119.5 . . ? C5 C10 H9 119.5 . . ? Ni1 C10 H9 130.9 . . ? C5 C11 H10 109.5 . . ? C5 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? C5 C11 H12 109.5 . . ? H10 C11 H12 109.5 . . ? H11 C11 H12 109.5 . . ? C14 Si2 C12 107.38(15) . . ? C14 Si2 C13 108.61(15) . . ? C12 Si2 C13 102.53(15) . . ? C14 Si2 C1 111.86(13) . . ? C12 Si2 C1 113.71(14) . . ? C13 Si2 C1 112.21(13) . . ? Si2 C12 H13 109.5 . . ? Si2 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? Si2 C12 H15 109.5 . . ? H13 C12 H15 109.5 . . ? H14 C12 H15 109.5 . . ? Si2 C13 H16 109.5 . . ? Si2 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? Si2 C13 H18 109.5 . . ? H16 C13 H18 109.5 . . ? H17 C13 H18 109.5 . . ? Si2 C14 H19 109.5 . . ? Si2 C14 H20 109.5 . . ? H19 C14 H20 109.5 . . ? Si2 C14 H21 109.5 . . ? H19 C14 H21 109.5 . . ? H20 C14 H21 109.5 . . ? C16 Si3 C15 109.09(15) . . ? C16 Si3 C17 107.29(14) . . ? C15 Si3 C17 104.26(15) . . ? C16 Si3 C1 112.74(13) . . ? C15 Si3 C1 112.67(14) . . ? C17 Si3 C1 110.33(13) . . ? Si3 C15 H22 109.5 . . ? Si3 C15 H23 109.5 . . ? H22 C15 H23 109.5 . . ? Si3 C15 H24 109.5 . . ? H22 C15 H24 109.5 . . ? H23 C15 H24 109.5 . . ? Si3 C16 H25 109.5 . . ? Si3 C16 H26 109.5 . . ? H25 C16 H26 109.5 . . ? Si3 C16 H27 109.5 . . ? H25 C16 H27 109.5 . . ? H26 C16 H27 109.5 . . ? Si3 C17 H28 109.5 . . ? Si3 C17 H29 109.5 . . ? H28 C17 H29 109.5 . . ? Si3 C17 H30 109.5 . . ? H28 C17 H30 109.5 . . ? H29 C17 H30 109.5 . . ? C20 Si4 C19 110.58(15) . . ? C20 Si4 C18 104.48(15) . . ? C19 Si4 C18 104.89(16) . . ? C20 Si4 C4 112.32(14) . . ? C19 Si4 C4 110.74(14) . . ? C18 Si4 C4 113.43(14) . . ? Si4 C18 H31 109.5 . . ? Si4 C18 H32 109.5 . . ? H31 C18 H32 109.5 . . ? Si4 C18 H33 109.5 . . ? H31 C18 H33 109.5 . . ? H32 C18 H33 109.5 . . ? Si4 C19 H34 109.5 . . ? Si4 C19 H35 109.5 . . ? H34 C19 H35 109.5 . . ? Si4 C19 H36 109.5 . . ? H34 C19 H36 109.5 . . ? H35 C19 H36 109.5 . . ? Si4 C20 H37 109.5 . . ? Si4 C20 H38 109.5 . . ? H37 C20 H38 109.5 . . ? Si4 C20 H39 109.5 . . ? H37 C20 H39 109.5 . . ? H38 C20 H39 109.5 . . ? C23 Si5 C22 108.66(15) . . ? C23 Si5 C21 103.70(14) . . ? C22 Si5 C21 107.24(15) . . ? C23 Si5 C4 111.93(14) . . ? C22 Si5 C4 112.33(13) . . ? C21 Si5 C4 112.51(14) . . ? Si5 C21 H40 109.5 . . ? Si5 C21 H41 109.5 . . ? H40 C21 H41 109.5 . . ? Si5 C21 H42 109.5 . . ? H40 C21 H42 109.5 . . ? H41 C21 H42 109.5 . . ? Si5 C22 H43 109.5 . . ? Si5 C22 H44 109.5 . . ? H43 C22 H44 109.5 . . ? Si5 C22 H45 109.5 . . ? H43 C22 H45 109.5 . . ? H44 C22 H45 109.5 . . ? Si5 C23 H46 109.5 . . ? Si5 C23 H47 109.5 . . ? H46 C23 H47 109.5 . . ? Si5 C23 H48 109.5 . . ? H46 C23 H48 109.5 . . ? H47 C23 H48 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 C1 C2 -15.23(19) . . . . ? Ni1 Si1 C1 C2 170.18(13) . . . . ? C4 Si1 C1 Si2 106.72(15) . . . . ? Ni1 Si1 C1 Si2 -67.87(18) . . . . ? C4 Si1 C1 Si3 -129.92(14) . . . . ? Ni1 Si1 C1 Si3 55.49(17) . . . . ? Si2 C1 C2 C3 -89.1(2) . . . . ? Si3 C1 C2 C3 147.95(19) . . . . ? Si1 C1 C2 C3 34.1(3) . . . . ? C1 C2 C3 C4 -41.8(3) . . . . ? C2 C3 C4 Si5 -94.5(2) . . . . ? C2 C3 C4 Si1 27.9(3) . . . . ? C2 C3 C4 Si4 143.68(19) . . . . ? C1 Si1 C4 C3 -6.5(2) . . . . ? Ni1 Si1 C4 C3 168.09(13) . . . . ? C1 Si1 C4 Si5 113.88(16) . . . . ? Ni1 Si1 C4 Si5 -71.51(18) . . . . ? C1 Si1 C4 Si4 -124.25(14) . . . . ? Ni1 Si1 C4 Si4 50.36(18) . . . . ? C4 Si1 Ni1 C9 -96.26(18) . . . . ? C1 Si1 Ni1 C9 76.48(18) . . . . ? C4 Si1 Ni1 C10 -42.19(18) . . . . ? C1 Si1 Ni1 C10 130.54(17) . . . . ? C4 Si1 Ni1 C8 -150.49(18) . . . . ? C1 Si1 Ni1 C8 22.24(19) . . . . ? C4 Si1 Ni1 C7 150.49(18) . . . . ? C1 Si1 Ni1 C7 -36.8(2) . . . . ? C4 Si1 Ni1 C6 82.1(2) . . . . ? C1 Si1 Ni1 C6 -105.2(2) . . . . ? C4 Si1 Ni1 C5 15.76(19) . . . . ? C1 Si1 Ni1 C5 -171.50(17) . . . . ? Si1 Ni1 C5 C6 124.03(17) . . . . ? C9 Ni1 C5 C6 -103.5(2) . . . . ? C10 Ni1 C5 C6 -132.3(3) . . . . ? C8 Ni1 C5 C6 -65.64(19) . . . . ? C7 Ni1 C5 C6 -28.56(17) . . . . ? Si1 Ni1 C5 C10 -103.65(19) . . . . ? C9 Ni1 C5 C10 28.84(19) . . . . ? C8 Ni1 C5 C10 66.68(19) . . . . ? C7 Ni1 C5 C10 103.8(2) . . . . ? C6 Ni1 C5 C10 132.3(3) . . . . ? Si1 Ni1 C5 C11 10.4(4) . . . . ? C9 Ni1 C5 C11 142.9(3) . . . . ? C10 Ni1 C5 C11 114.1(4) . . . . ? C8 Ni1 C5 C11 -179.2(3) . . . . ? C7 Ni1 C5 C11 -142.2(3) . . . . ? C6 Ni1 C5 C11 -113.6(4) . . . . ? C10 C5 C6 C7 1.1(4) . . . . ? C11 C5 C6 C7 -178.7(3) . . . . ? Ni1 C5 C6 C7 52.7(2) . . . . ? C10 C5 C6 Ni1 -51.6(2) . . . . ? C11 C5 C6 Ni1 128.6(3) . . . . ? Si1 Ni1 C6 C5 -111.65(19) . . . . ? C9 Ni1 C6 C5 67.11(19) . . . . ? C10 Ni1 C6 C5 29.39(18) . . . . ? C8 Ni1 C6 C5 104.9(2) . . . . ? C7 Ni1 C6 C5 133.8(3) . . . . ? Si1 Ni1 C6 C7 114.55(19) . . . . ? C9 Ni1 C6 C7 -66.69(19) . . . . ? C10 Ni1 C6 C7 -104.4(2) . . . . ? C8 Ni1 C6 C7 -28.90(18) . . . . ? C5 Ni1 C6 C7 -133.8(3) . . . . ? C5 C6 C7 C8 -0.6(4) . . . . ? Ni1 C6 C7 C8 52.7(2) . . . . ? C5 C6 C7 Ni1 -53.3(2) . . . . ? Si1 Ni1 C7 C8 103.6(2) . . . . ? C9 Ni1 C7 C8 -29.33(18) . . . . ? C10 Ni1 C7 C8 -67.38(19) . . . . ? C6 Ni1 C7 C8 -133.0(3) . . . . ? C5 Ni1 C7 C8 -104.7(2) . . . . ? Si1 Ni1 C7 C6 -123.37(17) . . . . ? C9 Ni1 C7 C6 103.7(2) . . . . ? C10 Ni1 C7 C6 65.67(19) . . . . ? C8 Ni1 C7 C6 133.0(3) . . . . ? C5 Ni1 C7 C6 28.33(17) . . . . ? C6 C7 C8 C9 -1.0(4) . . . . ? Ni1 C7 C8 C9 52.1(2) . . . . ? C6 C7 C8 Ni1 -53.0(2) . . . . ? Si1 Ni1 C8 C7 -122.86(17) . . . . ? C9 Ni1 C8 C7 132.8(3) . . . . ? C10 Ni1 C8 C7 103.0(2) . . . . ? C6 Ni1 C8 C7 28.95(18) . . . . ? C5 Ni1 C8 C7 65.74(19) . . . . ? Si1 Ni1 C8 C9 104.34(19) . . . . ? C10 Ni1 C8 C9 -29.81(19) . . . . ? C7 Ni1 C8 C9 -132.8(3) . . . . ? C6 Ni1 C8 C9 -103.9(2) . . . . ? C5 Ni1 C8 C9 -67.06(19) . . . . ? C7 C8 C9 C10 1.9(4) . . . . ? Ni1 C8 C9 C10 54.9(2) . . . . ? C7 C8 C9 Ni1 -53.0(2) . . . . ? Si1 Ni1 C9 C10 113.54(18) . . . . ? C8 Ni1 C9 C10 -131.9(3) . . . . ? C7 Ni1 C9 C10 -102.9(2) . . . . ? C6 Ni1 C9 C10 -65.54(19) . . . . ? C5 Ni1 C9 C10 -28.45(18) . . . . ? Si1 Ni1 C9 C8 -114.60(17) . . . . ? C10 Ni1 C9 C8 131.9(3) . . . . ? C7 Ni1 C9 C8 28.96(18) . . . . ? C6 Ni1 C9 C8 66.32(19) . . . . ? C5 Ni1 C9 C8 103.4(2) . . . . ? C8 C9 C10 C5 -1.3(4) . . . . ? Ni1 C9 C10 C5 53.7(3) . . . . ? C8 C9 C10 Ni1 -55.0(2) . . . . ? C6 C5 C10 C9 -0.2(4) . . . . ? C11 C5 C10 C9 179.7(3) . . . . ? Ni1 C5 C10 C9 -52.3(2) . . . . ? C6 C5 C10 Ni1 52.1(2) . . . . ? C11 C5 C10 Ni1 -128.0(3) . . . . ? Si1 Ni1 C10 C9 -105.06(19) . . . . ? C8 Ni1 C10 C9 29.77(19) . . . . ? C7 Ni1 C10 C9 67.2(2) . . . . ? C6 Ni1 C10 C9 104.5(2) . . . . ? C5 Ni1 C10 C9 133.7(3) . . . . ? Si1 Ni1 C10 C5 121.26(16) . . . . ? C9 Ni1 C10 C5 -133.7(3) . . . . ? C8 Ni1 C10 C5 -103.9(2) . . . . ? C7 Ni1 C10 C5 -66.45(19) . . . . ? C6 Ni1 C10 C5 -29.19(18) . . . . ? C2 C1 Si2 C14 150.94(19) . . . . ? Si3 C1 Si2 C14 -87.92(17) . . . . ? Si1 C1 Si2 C14 33.0(2) . . . . ? C2 C1 Si2 C12 -87.2(2) . . . . ? Si3 C1 Si2 C12 33.9(2) . . . . ? Si1 C1 Si2 C12 154.82(15) . . . . ? C2 C1 Si2 C13 28.6(2) . . . . ? Si3 C1 Si2 C13 149.73(15) . . . . ? Si1 C1 Si2 C13 -89.39(18) . . . . ? C2 C1 Si3 C16 173.41(19) . . . . ? Si2 C1 Si3 C16 50.30(19) . . . . ? Si1 C1 Si3 C16 -74.33(17) . . . . ? C2 C1 Si3 C15 49.4(2) . . . . ? Si2 C1 Si3 C15 -73.71(18) . . . . ? Si1 C1 Si3 C15 161.66(14) . . . . ? C2 C1 Si3 C17 -66.7(2) . . . . ? Si2 C1 Si3 C17 170.23(14) . . . . ? Si1 C1 Si3 C17 45.59(17) . . . . ? C3 C4 Si4 C20 164.54(19) . . . . ? Si5 C4 Si4 C20 42.76(18) . . . . ? Si1 C4 Si4 C20 -81.02(17) . . . . ? C3 C4 Si4 C19 40.4(2) . . . . ? Si5 C4 Si4 C19 -81.42(17) . . . . ? Si1 C4 Si4 C19 154.80(15) . . . . ? C3 C4 Si4 C18 -77.3(2) . . . . ? Si5 C4 Si4 C18 160.96(15) . . . . ? Si1 C4 Si4 C18 37.18(19) . . . . ? C3 C4 Si5 C23 -78.3(2) . . . . ? Si1 C4 Si5 C23 164.03(15) . . . . ? Si4 C4 Si5 C23 43.63(18) . . . . ? C3 C4 Si5 C22 159.1(2) . . . . ? Si1 C4 Si5 C22 41.5(2) . . . . ? Si4 C4 Si5 C22 -78.93(18) . . . . ? C3 C4 Si5 C21 38.0(2) . . . . ? Si1 C4 Si5 C21 -79.67(18) . . . . ? Si4 C4 Si5 C21 159.94(15) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.775 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.129 #===END