# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1571 data_apr599 _audit_creation_date 2000-01-14T16:29:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[N{C(SiMe3)2(SiMe2py)}(PPh3)]' ; _chemical_formula_sum 'C32 H43 N Ni P Si3' _chemical_formula_weight 615.62 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 16.476(2) _cell_length_b 9.142(3) _cell_length_c 21.687(5) _cell_angle_alpha 90 _cell_angle_beta 91.22(2) _cell_angle_gamma 90 _cell_volume 3265.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.775 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5932 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5732 _reflns_number_gt 3974 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0445P)^2^+0.7126P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5732 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.102 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.447 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ni Ni 0.98951(3) 0.81420(6) 0.25041(2) 0.02024(14) Uani 1 1 d . . . P P 0.99309(6) 0.86719(11) 0.34936(4) 0.0194(2) Uani 1 1 d . . . Si1 Si 0.94983(7) 0.66964(13) 0.13507(5) 0.0234(3) Uani 1 1 d . . . Si2 Si 1.13079(7) 0.65599(13) 0.17329(5) 0.0252(3) Uani 1 1 d . . . Si3 Si 1.05161(7) 0.95345(13) 0.13375(5) 0.0250(3) Uani 1 1 d . . . N N 0.87274(19) 0.8332(4) 0.22329(15) 0.0270(8) Uani 1 1 d . . . C1 C 1.0371(2) 0.7686(4) 0.16726(16) 0.0196(9) Uani 1 1 d . . . C2 C 0.9336(3) 0.6701(5) 0.04884(18) 0.0393(12) Uani 1 1 d . . . H2A H 0.8847 0.6137 0.0381 0.059 Uiso 1 1 calc R . . H2B H 0.9807 0.6259 0.0292 0.059 Uiso 1 1 calc R . . H2C H 0.9269 0.7711 0.0343 0.059 Uiso 1 1 calc R . . C3 C 0.9399(3) 0.4727(5) 0.1583(2) 0.0380(11) Uani 1 1 d . . . H3A H 0.8912 0.4307 0.1386 0.057 Uiso 1 1 calc R . . H3B H 0.9356 0.4662 0.2032 0.057 Uiso 1 1 calc R . . H3C H 0.9878 0.4183 0.1452 0.057 Uiso 1 1 calc R . . C4 C 0.8572(2) 0.7616(5) 0.16894(18) 0.0251(9) Uani 1 1 d . . . C5 C 0.7792(3) 0.7636(5) 0.1437(2) 0.0344(11) Uani 1 1 d . . . H5 H 0.7681 0.7117 0.1065 0.041 Uiso 1 1 calc R . . C6 C 0.7180(3) 0.8385(6) 0.1710(2) 0.0440(13) Uani 1 1 d . . . H6 H 0.6648 0.8385 0.1531 0.053 Uiso 1 1 calc R . . C7 C 0.7341(3) 0.9144(6) 0.2250(2) 0.0423(13) Uani 1 1 d . . . H7 H 0.6929 0.969 0.2447 0.051 Uiso 1 1 calc R . . C8 C 0.8122(3) 0.9080(5) 0.2493(2) 0.0362(11) Uani 1 1 d . . . H8 H 0.8237 0.9594 0.2865 0.043 Uiso 1 1 calc R . . C9 C 1.1252(3) 0.5143(5) 0.2353(2) 0.0385(11) Uani 1 1 d . . . H9A H 1.1758 0.4578 0.2368 0.058 Uiso 1 1 calc R . . H9B H 1.0794 0.4487 0.2265 0.058 Uiso 1 1 calc R . . H9C H 1.1176 0.5624 0.2752 0.058 Uiso 1 1 calc R . . C10 C 1.2245(3) 0.7639(6) 0.1925(2) 0.0425(12) Uani 1 1 d . . . H10A H 1.2714 0.6979 0.1949 0.064 Uiso 1 1 calc R . . H10B H 1.2181 0.813 0.2323 0.064 Uiso 1 1 calc R . . H10C H 1.2331 0.8372 0.1603 0.064 Uiso 1 1 calc R . . C11 C 1.1537(3) 0.5552(5) 0.0999(2) 0.0420(12) Uani 1 1 d . . . H11A H 1.2035 0.498 0.1058 0.063 Uiso 1 1 calc R . . H11B H 1.1609 0.6258 0.0665 0.063 Uiso 1 1 calc R . . H11C H 1.1085 0.4895 0.0893 0.063 Uiso 1 1 calc R . . C12 C 1.1105(3) 1.0831(5) 0.1853(2) 0.0388(12) Uani 1 1 d . . . H12A H 1.1155 1.178 0.1647 0.058 Uiso 1 1 calc R . . H12B H 1.1647 1.043 0.1939 0.058 Uiso 1 1 calc R . . H12C H 1.0819 1.0958 0.2241 0.058 Uiso 1 1 calc R . . C13 C 0.9534(3) 1.0520(5) 0.1164(2) 0.0379(11) Uani 1 1 d . . . H13A H 0.965 1.1483 0.0988 0.057 Uiso 1 1 calc R . . H13B H 0.9233 1.0641 0.1546 0.057 Uiso 1 1 calc R . . H13C H 0.9207 0.9949 0.0868 0.057 Uiso 1 1 calc R . . C14 C 1.1071(3) 0.9481(5) 0.05852(19) 0.0361(11) Uani 1 1 d . . . H14A H 1.1131 1.0478 0.0427 0.054 Uiso 1 1 calc R . . H14B H 1.0762 0.8891 0.0285 0.054 Uiso 1 1 calc R . . H14C H 1.1609 0.9045 0.0653 0.054 Uiso 1 1 calc R . . C15 C 0.8972(2) 0.8456(4) 0.38986(16) 0.0212(9) Uani 1 1 d . . . C16 C 0.8528(3) 0.7192(5) 0.37917(19) 0.0301(10) Uani 1 1 d . . . H16 H 0.8743 0.6453 0.3534 0.036 Uiso 1 1 calc R . . C17 C 0.7782(3) 0.6983(6) 0.4051(2) 0.0377(11) Uani 1 1 d . . . H17 H 0.7487 0.6107 0.3973 0.045 Uiso 1 1 calc R . . C18 C 0.7465(2) 0.8054(5) 0.44260(19) 0.0354(11) Uani 1 1 d . . . H18 H 0.6946 0.7923 0.4601 0.042 Uiso 1 1 calc R . . C19 C 0.7901(3) 0.9312(5) 0.45457(19) 0.0325(11) Uani 1 1 d . . . H19 H 0.7689 1.0041 0.481 0.039 Uiso 1 1 calc R . . C20 C 0.8652(2) 0.9513(5) 0.42791(17) 0.0242(9) Uani 1 1 d . . . H20 H 0.8949 1.0386 0.4359 0.029 Uiso 1 1 calc R . . C21 C 1.0655(2) 0.7697(4) 0.39923(17) 0.0203(9) Uani 1 1 d . . . C22 C 1.0466(3) 0.7169(5) 0.45730(17) 0.0271(10) Uani 1 1 d . . . H22 H 0.9931 0.7286 0.4721 0.033 Uiso 1 1 calc R . . C23 C 1.1051(3) 0.6472(5) 0.49405(19) 0.0352(11) Uani 1 1 d . . . H23 H 1.0911 0.6099 0.5333 0.042 Uiso 1 1 calc R . . C24 C 1.1832(3) 0.6321(5) 0.4736(2) 0.0370(11) Uani 1 1 d . . . H24 H 1.2232 0.5853 0.4989 0.044 Uiso 1 1 calc R . . C25 C 1.2032(3) 0.6852(5) 0.4163(2) 0.0343(10) Uani 1 1 d . . . H25 H 1.2571 0.6754 0.4023 0.041 Uiso 1 1 calc R . . C26 C 1.1447(2) 0.7529(5) 0.37921(19) 0.0276(10) Uani 1 1 d . . . H26 H 1.1589 0.7883 0.3397 0.033 Uiso 1 1 calc R . . C27 C 1.0207(2) 1.0578(4) 0.36423(17) 0.0208(9) Uani 1 1 d . . . C28 C 0.9858(2) 1.1651(5) 0.32681(19) 0.0285(10) Uani 1 1 d . . . H28 H 0.9483 1.138 0.2949 0.034 Uiso 1 1 calc R . . C29 C 1.0050(3) 1.3111(5) 0.3357(2) 0.0320(10) Uani 1 1 d . . . H29 H 0.9796 1.3836 0.3105 0.038 Uiso 1 1 calc R . . C30 C 1.0604(3) 1.3519(5) 0.3804(2) 0.0320(10) Uani 1 1 d . . . H30 H 1.0742 1.4521 0.3859 0.038 Uiso 1 1 calc R . . C31 C 1.0961(3) 1.2464(5) 0.41754(19) 0.0297(10) Uani 1 1 d . . . H31 H 1.1347 1.2739 0.4485 0.036 Uiso 1 1 calc R . . C32 C 1.0759(2) 1.1013(5) 0.40987(18) 0.0254(9) Uani 1 1 d . . . H32 H 1.1001 1.0298 0.4362 0.031 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 Ni 0.0196(3) 0.0238(3) 0.0173(2) -0.0034(2) -0.00031(19) 0.0006(2) P 0.0213(5) 0.0201(6) 0.0170(5) -0.0030(4) 0.0004(4) 0.0004(4) Si1 0.0260(6) 0.0219(6) 0.0222(6) -0.0036(5) -0.0043(5) -0.0011(5) Si2 0.0226(6) 0.0292(7) 0.0237(6) 0.0004(5) 0.0013(5) 0.0026(5) Si3 0.0327(6) 0.0186(6) 0.0236(6) -0.0011(5) 0.0005(5) -0.0015(5) N 0.0215(17) 0.036(2) 0.0237(17) 0.0010(16) 0.0019(14) 0.0018(16) C1 0.0200(19) 0.024(2) 0.0153(19) -0.0023(16) 0.0005(15) -0.0042(17) C2 0.046(3) 0.046(3) 0.026(2) -0.011(2) -0.011(2) -0.005(2) C3 0.037(3) 0.027(3) 0.050(3) -0.003(2) -0.007(2) -0.007(2) C4 0.026(2) 0.023(2) 0.026(2) 0.0014(18) -0.0044(17) -0.0060(18) C5 0.029(2) 0.032(3) 0.041(3) -0.003(2) -0.010(2) -0.005(2) C6 0.019(2) 0.056(4) 0.056(3) 0.009(3) -0.009(2) 0.003(2) C7 0.023(2) 0.059(4) 0.044(3) 0.006(3) 0.007(2) 0.011(2) C8 0.032(2) 0.050(3) 0.027(2) 0.000(2) 0.0035(19) 0.012(2) C9 0.040(3) 0.036(3) 0.039(3) 0.010(2) -0.007(2) 0.007(2) C10 0.024(2) 0.051(3) 0.052(3) 0.004(3) 0.003(2) 0.001(2) C11 0.045(3) 0.040(3) 0.042(3) -0.005(2) 0.013(2) 0.013(2) C12 0.047(3) 0.031(3) 0.039(3) -0.009(2) 0.010(2) -0.014(2) C13 0.051(3) 0.022(3) 0.040(3) 0.003(2) -0.004(2) 0.009(2) C14 0.050(3) 0.028(3) 0.030(2) 0.003(2) 0.005(2) -0.008(2) C15 0.021(2) 0.026(2) 0.0163(19) 0.0011(17) -0.0018(15) 0.0008(17) C16 0.034(2) 0.027(3) 0.030(2) -0.0038(19) 0.0060(19) -0.002(2) C17 0.033(2) 0.043(3) 0.037(3) 0.001(2) -0.001(2) -0.012(2) C18 0.022(2) 0.052(3) 0.032(2) 0.010(2) 0.0078(18) -0.002(2) C19 0.031(2) 0.043(3) 0.024(2) 0.007(2) 0.0026(19) 0.013(2) C20 0.026(2) 0.028(2) 0.019(2) 0.0031(18) -0.0010(17) 0.0017(19) C21 0.026(2) 0.015(2) 0.020(2) -0.0069(16) 0.0000(16) -0.0027(17) C22 0.033(2) 0.028(3) 0.021(2) -0.0032(18) 0.0038(18) 0.0027(19) C23 0.045(3) 0.037(3) 0.024(2) 0.002(2) 0.000(2) 0.007(2) C24 0.039(3) 0.036(3) 0.035(3) 0.004(2) -0.008(2) 0.011(2) C25 0.025(2) 0.036(3) 0.043(3) -0.003(2) 0.0033(19) 0.006(2) C26 0.025(2) 0.027(2) 0.030(2) 0.0006(19) -0.0002(18) -0.0009(19) C27 0.022(2) 0.022(2) 0.019(2) 0.0008(17) 0.0064(16) -0.0011(17) C28 0.027(2) 0.030(3) 0.028(2) 0.0012(19) -0.0020(17) 0.002(2) C29 0.031(2) 0.026(2) 0.039(3) 0.009(2) 0.0025(19) 0.002(2) C30 0.034(2) 0.024(3) 0.039(3) 0.000(2) 0.010(2) -0.005(2) C31 0.036(2) 0.024(2) 0.029(2) -0.0049(19) -0.0015(19) -0.005(2) C32 0.028(2) 0.022(2) 0.026(2) 0.0008(18) -0.0026(18) -0.0010(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ni N 2.007(3) . ? Ni C1 2.025(4) . ? Ni P 2.1996(12) . ? P C21 1.825(4) . ? P C27 1.827(4) . ? P C15 1.835(4) . ? Si1 C1 1.826(4) . ? Si1 C3 1.878(5) . ? Si1 C2 1.883(4) . ? Si1 C4 1.903(4) . ? Si2 C1 1.857(4) . ? Si2 C9 1.871(4) . ? Si2 C10 1.872(5) . ? Si2 C11 1.884(4) . ? Si3 C1 1.857(4) . ? Si3 C13 1.883(4) . ? Si3 C12 1.885(4) . ? Si3 C14 1.888(4) . ? N C8 1.344(5) . ? N C4 1.367(5) . ? C4 C5 1.386(5) . ? C5 C6 1.366(6) . ? C6 C7 1.381(7) . ? C7 C8 1.381(6) . ? C15 C20 1.382(5) . ? C15 C16 1.384(6) . ? C16 C17 1.377(6) . ? C17 C18 1.382(6) . ? C18 C19 1.378(6) . ? C19 C20 1.389(6) . ? C21 C22 1.390(5) . ? C21 C26 1.393(5) . ? C22 C23 1.392(6) . ? C23 C24 1.377(6) . ? C24 C25 1.380(6) . ? C25 C26 1.388(6) . ? C27 C32 1.388(5) . ? C27 C28 1.390(5) . ? C28 C29 1.385(6) . ? C29 C30 1.370(6) . ? C30 C31 1.380(6) . ? C31 C32 1.377(6) . ? 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 N Ni C1 98.28(14) . . ? N Ni P 105.81(10) . . ? C1 Ni P 155.67(11) . . ? C21 P C27 101.78(17) . . ? C21 P C15 102.85(17) . . ? C27 P C15 103.40(17) . . ? C21 P Ni 118.30(13) . . ? C27 P Ni 112.55(12) . . ? C15 P Ni 115.97(13) . . ? C1 Si1 C3 116.42(19) . . ? C1 Si1 C2 118.20(19) . . ? C3 Si1 C2 104.9(2) . . ? C1 Si1 C4 105.36(18) . . ? C3 Si1 C4 104.2(2) . . ? C2 Si1 C4 106.5(2) . . ? C1 Si2 C9 112.40(19) . . ? C1 Si2 C10 113.8(2) . . ? C9 Si2 C10 104.9(2) . . ? C1 Si2 C11 113.12(19) . . ? C9 Si2 C11 106.4(2) . . ? C10 Si2 C11 105.4(2) . . ? C1 Si3 C13 113.4(2) . . ? C1 Si3 C12 114.14(19) . . ? C13 Si3 C12 104.3(2) . . ? C1 Si3 C14 112.52(19) . . ? C13 Si3 C14 105.7(2) . . ? C12 Si3 C14 106.1(2) . . ? C8 N C4 118.6(4) . . ? C8 N Ni 129.6(3) . . ? C4 N Ni 111.8(3) . . ? Si1 C1 Si3 114.1(2) . . ? Si1 C1 Si2 113.5(2) . . ? Si3 C1 Si2 114.8(2) . . ? Si1 C1 Ni 97.20(17) . . ? Si3 C1 Ni 102.52(18) . . ? Si2 C1 Ni 112.85(18) . . ? N C4 C5 119.3(4) . . ? N C4 Si1 114.0(3) . . ? C5 C4 Si1 126.7(3) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C7 119.3(4) . . ? C6 C7 C8 117.5(4) . . ? N C8 C7 123.8(4) . . ? C20 C15 C16 118.5(4) . . ? C20 C15 P 123.6(3) . . ? C16 C15 P 117.8(3) . . ? C17 C16 C15 121.3(4) . . ? C16 C17 C18 119.6(4) . . ? C19 C18 C17 120.0(4) . . ? C18 C19 C20 119.8(4) . . ? C15 C20 C19 120.7(4) . . ? C22 C21 C26 118.3(4) . . ? C22 C21 P 123.4(3) . . ? C26 C21 P 118.3(3) . . ? C21 C22 C23 120.8(4) . . ? C24 C23 C22 120.1(4) . . ? C23 C24 C25 119.8(4) . . ? C24 C25 C26 120.2(4) . . ? C25 C26 C21 120.8(4) . . ? C32 C27 C28 118.1(4) . . ? C32 C27 P 123.8(3) . . ? C28 C27 P 118.1(3) . . ? C29 C28 C27 120.6(4) . . ? C30 C29 C28 120.6(4) . . ? C29 C30 C31 119.5(4) . . ? C32 C31 C30 120.3(4) . . ? C31 C32 C27 121.0(4) . . ? #===END data_oct199 _audit_creation_date 1999-10-04T16:20:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Ni{C(SiMe3)(SiMe2O)(SiMe2C5H4N)}}2]' _chemical_formula_moiety 'C26 H50 N2 Ni2 O2 Si6' _chemical_formula_structural 'C26 H50 N2 Ni2 O2 Si6' _chemical_formula_sum 'C26 H50 N2 Ni2 O2 Si6' _chemical_formula_weight 708.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8600(8) _cell_length_b 10.1220(10) _cell_length_c 10.6164(11) _cell_angle_alpha 91.437(6) _cell_angle_beta 111.283(7) _cell_angle_gamma 92.595(5) _cell_volume 885.36(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15870 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.875 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 8262 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 25.17 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.97 _reflns_number_total 3091 _reflns_number_gt 2618 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^+6.3900P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3091 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.079 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.817 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.115 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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' 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 Ni Ni 0.08357(9) -0.10083(8) -0.03699(8) 0.0206(2) Uani 1 1 d . . . Si1 Si 0.2634(2) -0.17998(17) -0.20696(17) 0.0220(4) Uani 1 1 d . . . Si2 Si -0.0689(2) -0.01724(18) -0.27478(17) 0.0240(4) Uani 1 1 d . . . Si3 Si -0.0705(2) -0.32566(18) -0.24724(19) 0.0273(4) Uani 1 1 d . . . O O -0.0788(5) 0.0160(5) -0.1250(4) 0.0298(11) Uani 1 1 d . . . N N 0.2566(6) -0.2095(5) 0.0436(5) 0.0215(11) Uani 1 1 d . . . C1 C 0.0504(7) -0.1655(6) -0.2233(6) 0.0210(13) Uani 1 1 d . . . C2 C 0.3908(8) -0.0233(7) -0.1943(7) 0.0329(16) Uani 1 1 d . . . H2C H 0.3422 0.0268 -0.2757 0.049 Uiso 1 1 calc R . . H2B H 0.5005 -0.0452 -0.1861 0.049 Uiso 1 1 calc R . . H2A H 0.3963 0.0304 -0.1144 0.049 Uiso 1 1 calc R . . C3 C 0.2997(8) -0.2930(7) -0.3350(7) 0.0313(16) Uani 1 1 d . . . H3C H 0.2579 -0.3831 -0.3292 0.047 Uiso 1 1 calc R . . H3B H 0.4164 -0.2931 -0.3166 0.047 Uiso 1 1 calc R . . H3A H 0.2437 -0.2619 -0.426 0.047 Uiso 1 1 calc R . . C4 C 0.3471(7) -0.2468(6) -0.0310(6) 0.0221(13) Uani 1 1 d . . . C5 C 0.4837(7) -0.3209(6) 0.0290(7) 0.0286(15) Uani 1 1 d . . . H5 H 0.5466 -0.347 -0.0221 0.034 Uiso 1 1 calc R . . C6 C 0.5262(8) -0.3553(7) 0.1601(7) 0.0334(16) Uani 1 1 d . . . H6 H 0.6196 -0.4039 0.2009 0.04 Uiso 1 1 calc R . . C7 C 0.4326(8) -0.3190(7) 0.2335(7) 0.0310(15) Uani 1 1 d . . . H7 H 0.4592 -0.3436 0.3245 0.037 Uiso 1 1 calc R . . C8 C 0.3003(8) -0.2466(6) 0.1719(6) 0.0276(14) Uani 1 1 d . . . H8 H 0.2363 -0.2215 0.2226 0.033 Uiso 1 1 calc R . . C9 C 0.0291(9) 0.1254(7) -0.3274(8) 0.0407(18) Uani 1 1 d . . . H9C H 0.1284 0.1564 -0.2524 0.061 Uiso 1 1 calc R . . H9B H -0.0455 0.1971 -0.3522 0.061 Uiso 1 1 calc R . . H9A H 0.0563 0.0981 -0.4054 0.061 Uiso 1 1 calc R . . C10 C -0.2786(9) -0.0412(8) -0.4058(7) 0.0394(18) Uani 1 1 d . . . H10C H -0.2729 -0.0795 -0.4895 0.059 Uiso 1 1 calc R . . H10B H -0.3278 0.0445 -0.4235 0.059 Uiso 1 1 calc R . . H10A H -0.3447 -0.1011 -0.3728 0.059 Uiso 1 1 calc R . . C11 C -0.2277(9) -0.3162(8) -0.1671(8) 0.0415(19) Uani 1 1 d . . . H11C H -0.1739 -0.2952 -0.0699 0.062 Uiso 1 1 calc R . . H11B H -0.2896 -0.4015 -0.1812 0.062 Uiso 1 1 calc R . . H11A H -0.3013 -0.2468 -0.2085 0.062 Uiso 1 1 calc R . . C12 C -0.1765(10) -0.3767(8) -0.4319(8) 0.050(2) Uani 1 1 d . . . H12C H -0.2502 -0.3088 -0.4773 0.074 Uiso 1 1 calc R . . H12B H -0.2387 -0.4612 -0.4401 0.074 Uiso 1 1 calc R . . H12A H -0.0958 -0.3867 -0.4741 0.074 Uiso 1 1 calc R . . C13 C 0.0497(10) -0.4695(7) -0.1688(9) 0.0432(19) Uani 1 1 d . . . H13C H 0.1326 -0.4828 -0.2082 0.065 Uiso 1 1 calc R . . H13B H -0.0228 -0.5494 -0.1862 0.065 Uiso 1 1 calc R . . H13A H 0.1024 -0.4516 -0.071 0.065 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 Ni 0.0200(4) 0.0248(5) 0.0163(4) -0.0010(3) 0.0054(3) 0.0064(3) Si1 0.0198(9) 0.0255(9) 0.0209(9) -0.0041(7) 0.0080(7) 0.0003(7) Si2 0.0248(9) 0.0301(10) 0.0169(9) -0.0002(7) 0.0070(7) 0.0067(8) Si3 0.0216(9) 0.0263(10) 0.0329(10) -0.0041(8) 0.0091(8) -0.0010(7) O 0.035(3) 0.039(3) 0.016(2) -0.0001(19) 0.008(2) 0.019(2) N 0.019(3) 0.024(3) 0.022(3) 0.000(2) 0.008(2) 0.003(2) C1 0.017(3) 0.024(3) 0.020(3) -0.004(2) 0.004(2) 0.001(2) C2 0.028(4) 0.035(4) 0.032(4) 0.003(3) 0.007(3) -0.005(3) C3 0.020(3) 0.038(4) 0.031(4) -0.009(3) 0.006(3) 0.000(3) C4 0.016(3) 0.019(3) 0.027(3) -0.006(3) 0.003(3) -0.003(2) C5 0.020(3) 0.030(4) 0.037(4) -0.005(3) 0.012(3) 0.005(3) C6 0.026(4) 0.027(4) 0.045(4) 0.007(3) 0.009(3) 0.008(3) C7 0.031(4) 0.028(4) 0.030(4) 0.008(3) 0.007(3) 0.004(3) C8 0.028(4) 0.030(4) 0.027(4) 0.001(3) 0.013(3) 0.005(3) C9 0.045(5) 0.038(4) 0.043(4) 0.009(3) 0.019(4) 0.012(4) C10 0.040(4) 0.050(5) 0.022(4) -0.001(3) 0.003(3) 0.015(4) C11 0.029(4) 0.037(4) 0.062(5) 0.003(4) 0.022(4) -0.001(3) C12 0.049(5) 0.046(5) 0.042(5) -0.008(4) 0.004(4) -0.005(4) C13 0.044(5) 0.029(4) 0.061(5) 0.002(4) 0.024(4) 0.003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ni N 1.881(5) . ? Ni O 1.891(4) . ? Ni O 1.918(4) 2 ? Ni C1 1.980(6) . ? Ni Si2 2.5784(18) . ? Ni Ni 2.8308(15) 2 ? Si1 C1 1.844(6) . ? Si1 C2 1.878(7) . ? Si1 C3 1.880(7) . ? Si1 C4 1.898(6) . ? Si2 O 1.651(4) . ? Si2 C9 1.851(8) . ? Si2 C1 1.853(6) . ? Si2 C10 1.874(7) . ? Si3 C1 1.861(6) . ? Si3 C13 1.873(8) . ? Si3 C11 1.881(7) . ? Si3 C12 1.887(8) . ? O Ni 1.918(4) 2 ? N C8 1.342(8) . ? N C4 1.374(8) . ? C4 C5 1.406(9) . ? C5 C6 1.362(10) . ? C6 C7 1.383(10) . ? C7 C8 1.372(9) . ? 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 N Ni O 175.0(2) . . ? N Ni O 98.2(2) . 2 ? O Ni O 84.00(18) . 2 ? N Ni C1 93.7(2) . . ? O Ni C1 84.2(2) . . ? O Ni C1 168.1(2) 2 . ? N Ni Si2 137.04(16) . . ? O Ni Si2 39.74(13) . . ? O Ni Si2 122.85(14) 2 . ? C1 Ni Si2 45.67(18) . . ? N Ni Ni 139.64(15) . 2 ? O Ni Ni 42.36(12) . 2 ? O Ni Ni 41.63(13) 2 2 ? C1 Ni Ni 126.52(18) . 2 ? Si2 Ni Ni 81.60(5) . 2 ? C1 Si1 C2 118.0(3) . . ? C1 Si1 C3 116.6(3) . . ? C2 Si1 C3 106.4(3) . . ? C1 Si1 C4 99.4(3) . . ? C2 Si1 C4 104.2(3) . . ? C3 Si1 C4 111.4(3) . . ? O Si2 C9 110.2(3) . . ? O Si2 C1 95.4(2) . . ? C9 Si2 C1 117.1(3) . . ? O Si2 C10 109.9(3) . . ? C9 Si2 C10 105.8(4) . . ? C1 Si2 C10 117.8(3) . . ? O Si2 Ni 47.08(15) . . ? C9 Si2 Ni 116.6(3) . . ? C1 Si2 Ni 49.86(18) . . ? C10 Si2 Ni 136.4(3) . . ? C1 Si3 C13 114.8(3) . . ? C1 Si3 C11 111.1(3) . . ? C13 Si3 C11 104.6(4) . . ? C1 Si3 C12 112.0(3) . . ? C13 Si3 C12 105.4(4) . . ? C11 Si3 C12 108.4(4) . . ? Si2 O Ni 93.2(2) . . ? Si2 O Ni 165.2(3) . 2 ? Ni O Ni 96.00(18) . 2 ? C8 N C4 118.7(5) . . ? C8 N Ni 123.2(4) . . ? C4 N Ni 118.0(4) . . ? Si1 C1 Si2 126.0(3) . . ? Si1 C1 Si3 115.0(3) . . ? Si2 C1 Si3 115.6(3) . . ? Si1 C1 Ni 99.8(3) . . ? Si2 C1 Ni 84.5(2) . . ? Si3 C1 Ni 104.9(3) . . ? N C4 C5 119.4(6) . . ? N C4 Si1 110.6(4) . . ? C5 C4 Si1 129.9(5) . . ? C6 C5 C4 120.4(6) . . ? C5 C6 C7 119.6(6) . . ? C8 C7 C6 118.5(6) . . ? N C8 C7 123.3(6) . . ? #===END  data_jul1399 _audit_creation_date 1999-07-28T15:21:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C100 H116 Cl2 N2 P4 Pd2 Si6' _chemical_formula_structural 'C100 H116 CL2 N2 P4 PD2 SI6' _chemical_formula_sum 'C28 H56 Cl2 N2 Pd2 Si6' _chemical_formula_weight 872.99 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.465(5) _cell_length_b 23.390(12) _cell_length_c 25.032(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7884(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 8.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_factor_muR 0.015 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 2 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7053 _exptl_absorpt_correction_T_max 0.9754 _exptl_absorpt_correction_T_ave 0.7807 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.45622E-1 _diffrn_orient_matrix_ub_12 0.29072E-1 _diffrn_orient_matrix_ub_13 -0.16062E-1 _diffrn_orient_matrix_ub_21 0.24193E-1 _diffrn_orient_matrix_ub_22 0.29147E-1 _diffrn_orient_matrix_ub_23 0.02621 _diffrn_orient_matrix_ub_31 0.53384E-1 _diffrn_orient_matrix_ub_32 0.11624E-1 _diffrn_orient_matrix_ub_33 -0.25523E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_standards_decay_corr_max 2.742 _diffrn_standards_decay_corr_min 0.921 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 8 5 4 5 3 _diffrn_reflns_number 13619 _diffrn_reflns_av_R_equivalents 0.1279 _diffrn_reflns_av_sigmaI/netI 0.1508 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6907 _reflns_number_gt 3750 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The structure has molecules apparently disordered 0.80:0.20 over two overlapping orientations, but only the Pd atom sites of the lower occupancy set were included in the refinement. 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^)+(0.1108P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6907 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1539 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2264 _refine_ls_wR_factor_gt 0.1875 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.369 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.186 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.84230(7) 0.15893(4) 0.45488(3) 0.0159(2) Uani 0.804(10) 1 d P A 1 Pd2 Pd 0.83795(7) 0.08937(4) 0.56230(3) 0.0155(2) Uani 0.804(10) 1 d P A 1 Cl1 Cl 0.9056(3) 0.17923(12) 0.54553(12) 0.0249(7) Uani 0.804(10) 1 d P A 1 Cl2 Cl 0.9049(2) 0.06851(12) 0.47290(12) 0.0230(7) Uani 0.804(10) 1 d P A 1 Si1 Si 0.6631(3) 0.18563(15) 0.38434(14) 0.0244(8) Uani 0.804(10) 1 d P A 1 Si2 Si 0.8661(3) 0.15581(15) 0.32999(13) 0.0210(8) Uani 0.804(10) 1 d P A 1 Si3 Si 0.7299(3) 0.05932(16) 0.37946(15) 0.0244(8) Uani 0.804(10) 1 d P A 1 Si4 Si 0.6613(3) 0.06202(14) 0.63627(13) 0.0207(7) Uani 0.804(10) 1 d P A 1 Si5 Si 0.8679(3) 0.09119(14) 0.68583(13) 0.0187(7) Uani 0.804(10) 1 d P A 1 Si6 Si 0.7275(3) 0.18822(15) 0.64013(14) 0.0233(8) Uani 0.804(10) 1 d P A 1 N1 N 0.8008(8) 0.2410(4) 0.4429(4) 0.021(2) Uani 0.804(10) 1 d P A 1 N2 N 0.7935(7) 0.0072(4) 0.5722(3) 0.013(2) Uani 0.804(10) 1 d P A 1 C1 C 0.7734(10) 0.1355(5) 0.3826(4) 0.019(3) Uani 0.804(10) 1 d P A 1 C2 C 0.6051(11) 0.2032(7) 0.3174(6) 0.040(4) Uani 0.804(10) 1 d P A 1 H2A H 0.5748 0.1686 0.3024 0.06 Uiso 0.804(10) 1 calc PR A 1 H2B H 0.6564 0.2174 0.2931 0.06 Uiso 0.804(10) 1 calc PR A 1 H2C H 0.554 0.2326 0.3222 0.06 Uiso 0.804(10) 1 calc PR A 1 C3 C 0.5614(11) 0.1657(7) 0.4312(6) 0.044(4) Uani 0.804(10) 1 d P A 1 H3A H 0.5286 0.1309 0.4184 0.066 Uiso 0.804(10) 1 calc PR A 1 H3B H 0.5129 0.1969 0.4331 0.066 Uiso 0.804(10) 1 calc PR A 1 H3C H 0.5892 0.1588 0.4668 0.066 Uiso 0.804(10) 1 calc PR A 1 C4 C 0.7196(9) 0.2517(5) 0.4125(5) 0.020(3) Uani 0.804(10) 1 d P A 1 C5 C 0.6903(13) 0.3094(6) 0.4053(6) 0.043(4) Uani 0.804(10) 1 d P A 1 H5 H 0.6312 0.3176 0.3861 0.051 Uiso 0.804(10) 1 calc PR A 1 C6 C 0.7452(12) 0.3530(6) 0.4255(7) 0.039(4) Uani 0.804(10) 1 d P A 1 H6 H 0.726 0.3916 0.4196 0.047 Uiso 0.804(10) 1 calc PR A 1 C7 C 0.8293(11) 0.3404(5) 0.4546(5) 0.033(3) Uani 0.804(10) 1 d P A 1 H7 H 0.8694 0.3703 0.4684 0.039 Uiso 0.804(10) 1 calc PR A 1 C8 C 0.8547(11) 0.2843(5) 0.4634(5) 0.030(3) Uani 0.804(10) 1 d P A 1 H8 H 0.9116 0.2758 0.4845 0.036 Uiso 0.804(10) 1 calc PR A 1 C9 C 0.8780(11) 0.2341(6) 0.3185(5) 0.032(3) Uani 0.804(10) 1 d P A 1 H9A H 0.8129 0.2501 0.3094 0.048 Uiso 0.804(10) 1 calc PR A 1 H9B H 0.9244 0.241 0.2891 0.048 Uiso 0.804(10) 1 calc PR A 1 H9C H 0.903 0.2525 0.351 0.048 Uiso 0.804(10) 1 calc PR A 1 C10 C 0.9927(10) 0.1302(6) 0.3466(6) 0.036(4) Uani 0.804(10) 1 d P A 1 H10A H 0.991 0.0889 0.353 0.055 Uiso 0.804(10) 1 calc PR A 1 H10B H 1.0164 0.1498 0.3789 0.055 Uiso 0.804(10) 1 calc PR A 1 H10C H 1.0377 0.1385 0.3169 0.055 Uiso 0.804(10) 1 calc PR A 1 C11 C 0.8318(13) 0.1261(6) 0.2630(5) 0.040(4) Uani 0.804(10) 1 d P A 1 H11A H 0.765 0.139 0.2533 0.06 Uiso 0.804(10) 1 calc PR A 1 H11B H 0.833 0.0842 0.2645 0.06 Uiso 0.804(10) 1 calc PR A 1 H11C H 0.8795 0.1394 0.2362 0.06 Uiso 0.804(10) 1 calc PR A 1 C12 C 0.6282(12) 0.0532(7) 0.3283(6) 0.044(4) Uani 0.804(10) 1 d P A 1 H12A H 0.5752 0.0804 0.3368 0.066 Uiso 0.804(10) 1 calc PR A 1 H12B H 0.6013 0.0143 0.3287 0.066 Uiso 0.804(10) 1 calc PR A 1 H12C H 0.6551 0.0617 0.2928 0.066 Uiso 0.804(10) 1 calc PR A 1 C13 C 0.8250(11) 0.0060(5) 0.3594(5) 0.031(3) Uani 0.804(10) 1 d P A 1 H13A H 0.8802 0.0068 0.3849 0.047 Uiso 0.804(10) 1 calc PR A 1 H13B H 0.8497 0.0153 0.3236 0.047 Uiso 0.804(10) 1 calc PR A 1 H13C H 0.7952 -0.0322 0.3591 0.047 Uiso 0.804(10) 1 calc PR A 1 C14 C 0.6702(11) 0.0342(6) 0.4442(5) 0.034(4) Uani 0.804(10) 1 d P A 1 H14A H 0.6197 0.0618 0.4555 0.051 Uiso 0.804(10) 1 calc PR A 1 H14B H 0.7212 0.031 0.472 0.051 Uiso 0.804(10) 1 calc PR A 1 H14C H 0.6391 -0.0032 0.4386 0.051 Uiso 0.804(10) 1 calc PR A 1 C15 C 0.7694(9) 0.1118(5) 0.6365(5) 0.016(3) Uani 0.804(10) 1 d P A 1 C16 C 0.5529(10) 0.0836(6) 0.5919(6) 0.034(3) Uani 0.804(10) 1 d P A 1 H16A H 0.5002 0.0548 0.5946 0.052 Uiso 0.804(10) 1 calc PR A 1 H16B H 0.5755 0.0863 0.5548 0.052 Uiso 0.804(10) 1 calc PR A 1 H16C H 0.5273 0.1208 0.6035 0.052 Uiso 0.804(10) 1 calc PR A 1 C17 C 0.6128(11) 0.0414(6) 0.7030(5) 0.031(3) Uani 0.804(10) 1 d P A 1 H17A H 0.5563 0.0154 0.6986 0.047 Uiso 0.804(10) 1 calc PR A 1 H17B H 0.5912 0.0757 0.7222 0.047 Uiso 0.804(10) 1 calc PR A 1 H17C H 0.6652 0.0222 0.7233 0.047 Uiso 0.804(10) 1 calc PR A 1 C18 C 0.7113(9) -0.0033(5) 0.6029(5) 0.025(3) Uani 0.804(10) 1 d P A 1 C19 C 0.6835(12) -0.0605(5) 0.6111(5) 0.032(4) Uani 0.804(10) 1 d P A 1 H19 H 0.6299 -0.0689 0.6345 0.038 Uiso 0.804(10) 1 calc PR A 1 C20 C 0.7313(12) -0.1040(6) 0.5866(6) 0.037(4) Uani 0.804(10) 1 d P A 1 H20 H 0.7087 -0.1422 0.5906 0.045 Uiso 0.804(10) 1 calc PR A 1 C21 C 0.8111(12) -0.0923(6) 0.5566(6) 0.037(4) Uani 0.804(10) 1 d P A 1 H21 H 0.8469 -0.1223 0.5398 0.045 Uiso 0.804(10) 1 calc PR A 1 C22 C 0.8413(11) -0.0356(5) 0.5503(4) 0.022(3) Uani 0.804(10) 1 d P A 1 H22 H 0.8985 -0.0278 0.5293 0.026 Uiso 0.804(10) 1 calc PR A 1 C23 C 0.8913(11) 0.0129(5) 0.6893(5) 0.027(3) Uani 0.804(10) 1 d P A 1 H23A H 0.9435 0.0052 0.7157 0.04 Uiso 0.804(10) 1 calc PR A 1 H23B H 0.9127 -0.001 0.6542 0.04 Uiso 0.804(10) 1 calc PR A 1 H23C H 0.8302 -0.0068 0.6999 0.04 Uiso 0.804(10) 1 calc PR A 1 C24 C 0.8330(12) 0.1143(6) 0.7562(5) 0.035(3) Uani 0.804(10) 1 d P A 1 H24A H 0.8206 0.1556 0.7567 0.052 Uiso 0.804(10) 1 calc PR A 1 H24B H 0.8874 0.1051 0.7807 0.052 Uiso 0.804(10) 1 calc PR A 1 H24C H 0.7728 0.094 0.7674 0.052 Uiso 0.804(10) 1 calc PR A 1 C25 C 0.9904(10) 0.1243(6) 0.6691(5) 0.028(3) Uani 0.804(10) 1 d P A 1 H25A H 0.9828 0.1659 0.6669 0.043 Uiso 0.804(10) 1 calc PR A 1 H25B H 1.0138 0.1095 0.6347 0.043 Uiso 0.804(10) 1 calc PR A 1 H25C H 1.0387 0.1149 0.697 0.043 Uiso 0.804(10) 1 calc PR A 1 C26 C 0.6678(11) 0.2156(6) 0.5788(5) 0.035(3) Uani 0.804(10) 1 d P A 1 H26A H 0.6172 0.1883 0.5667 0.053 Uiso 0.804(10) 1 calc PR A 1 H26B H 0.718 0.2204 0.5508 0.053 Uiso 0.804(10) 1 calc PR A 1 H26C H 0.6364 0.2525 0.5863 0.053 Uiso 0.804(10) 1 calc PR A 1 C27 C 0.8222(11) 0.2411(5) 0.6613(6) 0.035(4) Uani 0.804(10) 1 d P A 1 H27A H 0.8548 0.2277 0.694 0.053 Uiso 0.804(10) 1 calc PR A 1 H27B H 0.79 0.2779 0.6682 0.053 Uiso 0.804(10) 1 calc PR A 1 H27C H 0.8718 0.2456 0.633 0.053 Uiso 0.804(10) 1 calc PR A 1 C28 C 0.6289(11) 0.1928(6) 0.6944(6) 0.038(4) Uani 0.804(10) 1 d P A 1 H28A H 0.575 0.166 0.6863 0.057 Uiso 0.804(10) 1 calc PR A 1 H28B H 0.6024 0.2318 0.6959 0.057 Uiso 0.804(10) 1 calc PR A 1 H28C H 0.6585 0.1829 0.729 0.057 Uiso 0.804(10) 1 calc PR A 1 PD1A Si 0.6604(19) 0.1557(9) 0.4392(9) 0.060(8) Uiso 0.196(10) 1 d P A 2 PD2A Si 0.656(2) 0.0918(11) 0.5469(11) 0.077(9) Uiso 0.196(10) 1 d P 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 0.0136(5) 0.0186(4) 0.0155(5) 0.0000(3) -0.0005(4) 0.0005(4) Pd2 0.0119(5) 0.0203(5) 0.0142(5) 0.0006(3) -0.0004(4) -0.0001(4) Cl1 0.0286(18) 0.0261(15) 0.0199(16) 0.0027(12) -0.0070(14) -0.0091(13) Cl2 0.0231(17) 0.0260(15) 0.0200(16) 0.0034(12) 0.0032(13) 0.0088(13) Si1 0.0127(17) 0.0338(19) 0.0265(19) -0.0033(14) -0.0029(16) 0.0030(16) Si2 0.0193(19) 0.0262(18) 0.0176(18) 0.0009(14) 0.0016(14) 0.0006(15) Si3 0.028(2) 0.0222(19) 0.023(2) -0.0044(15) -0.0001(16) -0.0055(16) Si4 0.0137(17) 0.0285(17) 0.0200(18) -0.0014(14) 0.0007(15) -0.0010(16) Si5 0.0145(18) 0.0236(17) 0.0180(17) 0.0013(14) -0.0038(13) -0.0049(14) Si6 0.030(2) 0.0204(18) 0.0196(19) -0.0037(14) -0.0061(16) 0.0052(16) N1 0.031(6) 0.016(5) 0.015(5) -0.008(4) 0.006(5) 0.002(4) N2 0.009(5) 0.025(5) 0.004(5) -0.007(4) -0.003(4) 0.000(4) C1 0.014(6) 0.034(7) 0.007(6) 0.005(5) 0.006(5) 0.001(6) C2 0.020(8) 0.068(10) 0.033(8) -0.007(7) -0.022(7) 0.006(7) C3 0.022(8) 0.050(9) 0.060(11) -0.015(8) 0.018(8) 0.003(7) C4 0.015(7) 0.022(6) 0.023(7) 0.005(5) -0.001(5) 0.008(5) C5 0.049(11) 0.036(8) 0.044(10) 0.001(7) -0.016(8) 0.021(7) C6 0.047(11) 0.013(7) 0.058(11) -0.001(6) -0.017(8) 0.016(6) C7 0.042(9) 0.019(6) 0.037(8) -0.008(6) 0.001(7) -0.010(7) C8 0.041(9) 0.029(7) 0.020(7) -0.002(5) -0.001(6) -0.010(7) C9 0.029(8) 0.044(8) 0.024(8) 0.002(6) -0.008(6) -0.006(7) C10 0.009(7) 0.052(9) 0.049(9) 0.006(7) 0.015(6) 0.006(6) C11 0.043(10) 0.046(9) 0.030(8) -0.011(6) 0.005(8) -0.004(8) C12 0.041(10) 0.051(10) 0.041(9) -0.014(7) -0.007(7) -0.027(8) C13 0.035(9) 0.024(7) 0.035(8) -0.006(6) -0.003(7) 0.007(6) C14 0.029(8) 0.048(8) 0.024(7) 0.012(6) -0.004(6) -0.031(7) C15 0.002(5) 0.022(6) 0.025(7) -0.001(5) -0.005(5) -0.003(5) C16 0.022(8) 0.042(8) 0.040(9) -0.008(7) -0.003(7) 0.000(6) C17 0.022(8) 0.040(8) 0.033(8) 0.002(6) 0.007(6) -0.014(6) C18 0.015(7) 0.026(7) 0.032(8) -0.010(6) -0.007(6) -0.003(6) C19 0.049(10) 0.021(7) 0.026(8) 0.001(5) 0.003(7) -0.022(6) C20 0.053(10) 0.019(7) 0.040(9) -0.004(6) -0.011(8) -0.008(7) C21 0.044(10) 0.035(8) 0.032(8) -0.003(6) -0.010(7) 0.023(7) C22 0.031(7) 0.021(6) 0.014(6) -0.004(5) -0.010(6) -0.009(6) C23 0.039(9) 0.027(7) 0.015(7) 0.001(5) -0.001(6) 0.005(6) C24 0.038(9) 0.039(8) 0.028(8) 0.003(6) -0.012(7) -0.004(7) C25 0.023(8) 0.048(8) 0.014(7) 0.008(6) -0.013(6) 0.006(6) C26 0.033(9) 0.040(8) 0.033(8) 0.003(6) -0.003(7) 0.021(7) C27 0.049(10) 0.018(6) 0.038(9) -0.009(6) 0.009(7) -0.009(6) C28 0.038(9) 0.046(9) 0.031(8) -0.008(7) 0.001(7) 0.014(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 2.022(10) . ? Pd1 C1 2.106(12) . ? Pd1 Cl2 2.321(3) . ? Pd1 Cl1 2.470(3) . ? Pd1 Pd2 3.1433(15) . ? Pd2 N2 2.029(9) . ? Pd2 C15 2.140(12) . ? Pd2 Cl1 2.329(3) . ? Pd2 Cl2 2.461(3) . ? Si1 C4 1.862(13) . ? Si1 C3 1.862(15) . ? Si1 C2 1.893(13) . ? Si1 C1 1.892(13) . ? Si2 C10 1.854(14) . ? Si2 C9 1.861(13) . ? Si2 C11 1.873(14) . ? Si2 C1 1.876(12) . ? Si3 C13 1.857(13) . ? Si3 C1 1.878(13) . ? Si3 C12 1.880(15) . ? Si3 C14 1.903(12) . ? Si4 C17 1.857(13) . ? Si4 C15 1.864(12) . ? Si4 C18 1.867(13) . ? Si4 C16 1.901(14) . ? Si5 C23 1.861(12) . ? Si5 C25 1.869(14) . ? Si5 C15 1.874(12) . ? Si5 C24 1.901(14) . ? Si6 C26 1.848(13) . ? Si6 C27 1.853(14) . ? Si6 C15 1.877(12) . ? Si6 C28 1.904(15) . ? N1 C8 1.348(16) . ? N1 C4 1.356(16) . ? N2 C22 1.311(15) . ? N2 C18 1.369(16) . ? C4 C5 1.416(17) . ? C5 C6 1.36(2) . ? C6 C7 1.38(2) . ? C7 C8 1.375(18) . ? C18 C19 1.404(17) . ? C19 C20 1.35(2) . ? C20 C21 1.34(2) . ? C21 C22 1.395(18) . ? 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 N1 Pd1 C1 89.9(4) . . ? N1 Pd1 Cl2 174.0(3) . . ? C1 Pd1 Cl2 95.2(3) . . ? N1 Pd1 Cl1 92.8(3) . . ? C1 Pd1 Cl1 172.5(3) . . ? Cl2 Pd1 Cl1 82.61(11) . . ? N1 Pd1 Pd2 127.8(3) . . ? C1 Pd1 Pd2 126.3(3) . . ? Cl2 Pd1 Pd2 50.87(8) . . ? Cl1 Pd1 Pd2 47.16(7) . . ? N2 Pd2 C15 89.9(4) . . ? N2 Pd2 Cl1 173.1(3) . . ? C15 Pd2 Cl1 96.0(3) . . ? N2 Pd2 Cl2 91.8(3) . . ? C15 Pd2 Cl2 174.9(3) . . ? Cl1 Pd2 Cl2 82.63(11) . . ? N2 Pd2 Pd1 126.9(2) . . ? C15 Pd2 Pd1 128.6(3) . . ? Cl1 Pd2 Pd1 51.05(8) . . ? Cl2 Pd2 Pd1 47.00(7) . . ? Pd2 Cl1 Pd1 81.78(10) . . ? Pd1 Cl2 Pd2 82.13(10) . . ? C4 Si1 C3 105.6(6) . . ? C4 Si1 C2 108.9(6) . . ? C3 Si1 C2 108.0(7) . . ? C4 Si1 C1 101.7(6) . . ? C3 Si1 C1 115.9(6) . . ? C2 Si1 C1 115.9(6) . . ? C10 Si2 C9 105.8(7) . . ? C10 Si2 C11 107.9(7) . . ? C9 Si2 C11 104.4(6) . . ? C10 Si2 C1 111.9(6) . . ? C9 Si2 C1 114.5(6) . . ? C11 Si2 C1 111.7(7) . . ? C13 Si3 C1 115.7(6) . . ? C13 Si3 C12 105.4(7) . . ? C1 Si3 C12 109.1(6) . . ? C13 Si3 C14 108.3(7) . . ? C1 Si3 C14 112.9(6) . . ? C12 Si3 C14 104.4(7) . . ? C17 Si4 C15 115.7(6) . . ? C17 Si4 C18 108.4(6) . . ? C15 Si4 C18 103.4(6) . . ? C17 Si4 C16 108.9(7) . . ? C15 Si4 C16 115.9(6) . . ? C18 Si4 C16 103.5(6) . . ? C23 Si5 C25 105.6(6) . . ? C23 Si5 C15 113.8(6) . . ? C25 Si5 C15 111.8(5) . . ? C23 Si5 C24 106.2(6) . . ? C25 Si5 C24 107.9(6) . . ? C15 Si5 C24 111.2(6) . . ? C26 Si6 C27 107.8(7) . . ? C26 Si6 C15 114.9(6) . . ? C27 Si6 C15 116.3(6) . . ? C26 Si6 C28 105.7(7) . . ? C27 Si6 C28 103.8(6) . . ? C15 Si6 C28 107.3(6) . . ? C8 N1 C4 120.7(11) . . ? C8 N1 Pd1 120.5(9) . . ? C4 N1 Pd1 118.8(8) . . ? C22 N2 C18 119.7(11) . . ? C22 N2 Pd2 121.8(8) . . ? C18 N2 Pd2 118.6(8) . . ? Si2 C1 Si3 114.7(6) . . ? Si2 C1 Si1 112.5(6) . . ? Si3 C1 Si1 110.1(7) . . ? Si2 C1 Pd1 104.1(6) . . ? Si3 C1 Pd1 114.8(6) . . ? Si1 C1 Pd1 99.5(5) . . ? N1 C4 C5 118.1(12) . . ? N1 C4 Si1 112.9(8) . . ? C5 C4 Si1 129.0(10) . . ? C6 C5 C4 121.2(14) . . ? C5 C6 C7 118.9(12) . . ? C8 C7 C6 119.6(13) . . ? N1 C8 C7 121.4(13) . . ? Si4 C15 Si5 113.3(6) . . ? Si4 C15 Si6 111.1(6) . . ? Si5 C15 Si6 115.2(6) . . ? Si4 C15 Pd2 100.4(5) . . ? Si5 C15 Pd2 101.7(5) . . ? Si6 C15 Pd2 113.8(6) . . ? N2 C18 C19 117.9(12) . . ? N2 C18 Si4 113.3(9) . . ? C19 C18 Si4 128.2(11) . . ? C20 C19 C18 121.6(14) . . ? C21 C20 C19 118.9(13) . . ? C20 C21 C22 119.5(13) . . ? N2 C22 C21 122.3(13) . . ? #===END