data_compound_3a # 1. SUBMISSION DETAILS _publ_contact_author ;Wagler, J\"org Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; _publ_contact_author_phone '03731 39-3556 ' _publ_contact_author_fax '03731 39-4058 ' _publ_requested_journal 'Inorg.Chem.' _publ_section_title ; Reactions of Hydridochlorosilanes with 2,2'-Bipyridine and 1,10-Phenanthroline - Complexation vs. Dismutation and Metal-Catalyst-free Hydrosilyation ; _publ_section_abstract ; Surprisingly stable are adducts of H2SiCl2, HSiCl3 and RSiCl3 with N,N'-chelating ligands in the solid state. Their dismutation was observed only in polar solvents at elevated temperatures. For RHSiCl2 only hydrosilyation and dismutation were observed. ; loop_ _publ_author_name _publ_author_address 'Fester, Gerrit ' ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; 'Eckstein, Jana ' ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; 'Wagler, J\"org ' ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; 'Brendler, Erica ' ; Institut f\"ur Analytische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; 'Kroke, Edwin ' ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrachlorosilane 1,10-phenanthroline complex, acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H8 Cl4 N2 Si), C2 H3 N' _chemical_formula_sum 'C26 H19 Cl8 N5 Si2' _chemical_formula_weight 741.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4952(10) _cell_length_b 12.3284(18) _cell_length_c 16.551(2) _cell_angle_alpha 89.334(5) _cell_angle_beta 87.725(4) _cell_angle_gamma 78.770(4) _cell_volume 1498.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5636 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 29.44 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7929 _exptl_absorpt_correction_T_max 0.9343 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29374 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8686 _reflns_number_gt 6484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _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^)+(0.0463P)^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 8686 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 Cl1 Cl 0.33937(8) 0.10633(4) 0.22389(3) 0.02743(13) Uani 1 1 d . . . Cl2 Cl 0.09613(8) 0.34417(4) 0.24478(3) 0.02520(13) Uani 1 1 d . . . Cl3 Cl 0.51386(7) 0.31902(5) 0.20719(3) 0.02509(12) Uani 1 1 d . . . Cl4 Cl 0.07380(7) 0.20274(4) 0.08896(3) 0.02134(11) Uani 1 1 d . . . Si1 Si 0.28739(8) 0.25805(5) 0.15652(3) 0.01818(13) Uani 1 1 d . . . N1 N 0.2546(2) 0.38808(14) 0.08404(10) 0.0152(3) Uani 1 1 d . . . N2 N 0.4604(2) 0.19473(15) 0.06868(10) 0.0184(4) Uani 1 1 d . . . C1 C 0.1565(3) 0.48947(17) 0.09750(12) 0.0178(4) Uani 1 1 d . . . H1 H 0.0935 0.5054 0.1482 0.021 Uiso 1 1 calc R . . C2 C 0.1443(3) 0.57264(18) 0.03871(13) 0.0197(4) Uani 1 1 d . . . H2 H 0.0751 0.6443 0.0503 0.024 Uiso 1 1 calc R . . C3 C 0.2310(3) 0.55174(19) -0.03528(13) 0.0212(4) Uani 1 1 d . . . H3 H 0.2188 0.6074 -0.0760 0.025 Uiso 1 1 calc R . . C4 C 0.3389(3) 0.44627(18) -0.05038(12) 0.0182(4) Uani 1 1 d . . . C5 C 0.4442(3) 0.4147(2) -0.12329(13) 0.0248(5) Uani 1 1 d . . . H5 H 0.4359 0.4651 -0.1674 0.030 Uiso 1 1 calc R . . C6 C 0.5552(3) 0.3145(2) -0.13069(13) 0.0260(5) Uani 1 1 d . . . H6 H 0.6258 0.2969 -0.1794 0.031 Uiso 1 1 calc R . . C7 C 0.5686(3) 0.23469(19) -0.06695(13) 0.0219(5) Uani 1 1 d . . . C8 C 0.6850(3) 0.1307(2) -0.06763(15) 0.0281(5) Uani 1 1 d . . . H8 H 0.7601 0.1067 -0.1141 0.034 Uiso 1 1 calc R . . C9 C 0.6892(3) 0.0645(2) -0.00122(15) 0.0277(5) Uani 1 1 d . . . H9 H 0.7703 -0.0051 -0.0011 0.033 Uiso 1 1 calc R . . C10 C 0.5760(3) 0.09726(18) 0.06689(14) 0.0245(5) Uani 1 1 d . . . H10 H 0.5814 0.0496 0.1126 0.029 Uiso 1 1 calc R . . C11 C 0.4595(3) 0.26267(18) 0.00360(12) 0.0178(4) Uani 1 1 d . . . C12 C 0.3462(2) 0.36815(17) 0.01179(11) 0.0158(4) Uani 1 1 d . . . Cl5 Cl 0.12702(7) 0.17227(5) 0.84333(3) 0.02467(12) Uani 1 1 d . . . Cl6 Cl 0.13029(7) 0.37886(4) 0.73160(3) 0.02381(12) Uani 1 1 d . . . Cl7 Cl 0.44594(6) 0.16972(4) 0.71540(3) 0.02017(11) Uani 1 1 d . . . Cl8 Cl -0.13798(6) 0.22090(5) 0.69767(3) 0.02300(12) Uani 1 1 d . . . Si2 Si 0.15177(7) 0.20429(5) 0.71459(3) 0.01709(12) Uani 1 1 d . . . N3 N 0.1821(2) 0.21841(14) 0.59564(10) 0.0177(4) Uani 1 1 d . . . N4 N 0.1676(2) 0.04799(14) 0.68671(10) 0.0172(4) Uani 1 1 d . . . C13 C 0.1807(3) 0.30943(19) 0.55165(13) 0.0233(5) Uani 1 1 d . . . H13 H 0.1574 0.3794 0.5775 0.028 Uiso 1 1 calc R . . C14 C 0.2130(3) 0.3039(2) 0.46764(14) 0.0296(5) Uani 1 1 d . . . H14 H 0.2119 0.3700 0.4375 0.036 Uiso 1 1 calc R . . C15 C 0.2460(3) 0.2045(2) 0.42859(13) 0.0272(5) Uani 1 1 d . . . H15 H 0.2694 0.2010 0.3717 0.033 Uiso 1 1 calc R . . C16 C 0.2449(3) 0.10769(19) 0.47365(13) 0.0220(5) Uani 1 1 d . . . C17 C 0.2699(3) -0.0009(2) 0.44037(13) 0.0263(5) Uani 1 1 d . . . H17 H 0.2949 -0.0109 0.3839 0.032 Uiso 1 1 calc R . . C18 C 0.2587(3) -0.0895(2) 0.48752(14) 0.0280(5) Uani 1 1 d . . . H18 H 0.2751 -0.1606 0.4635 0.034 Uiso 1 1 calc R . . C19 C 0.2225(3) -0.07890(18) 0.57328(14) 0.0222(5) Uani 1 1 d . . . C20 C 0.1977(3) -0.16503(19) 0.62594(15) 0.0256(5) Uani 1 1 d . . . H20 H 0.2093 -0.2383 0.6063 0.031 Uiso 1 1 calc R . . C21 C 0.1567(3) -0.14229(19) 0.70588(15) 0.0263(5) Uani 1 1 d . . . H21 H 0.1372 -0.1998 0.7419 0.032 Uiso 1 1 calc R . . C22 C 0.1433(3) -0.03517(19) 0.73494(13) 0.0231(5) Uani 1 1 d . . . H22 H 0.1160 -0.0213 0.7909 0.028 Uiso 1 1 calc R . . C23 C 0.2033(3) 0.02650(18) 0.60648(12) 0.0179(4) Uani 1 1 d . . . C24 C 0.2122(3) 0.11958(18) 0.55698(13) 0.0177(4) Uani 1 1 d . . . N5 N 0.7266(4) 0.3992(2) 0.50248(15) 0.0479(6) Uani 1 1 d . . . C25 C 0.6565(4) 0.4249(2) 0.56459(16) 0.0339(6) Uani 1 1 d . . . C26 C 0.5669(4) 0.4606(2) 0.64167(15) 0.0371(6) Uani 1 1 d . . . H26A H 0.4665 0.5231 0.6331 0.056 Uiso 1 1 calc R . . H26B H 0.6546 0.4835 0.6770 0.056 Uiso 1 1 calc R . . H26C H 0.5191 0.3994 0.6670 0.056 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 Cl1 0.0412(3) 0.0166(3) 0.0213(3) 0.0017(2) 0.0024(2) 0.0014(2) Cl2 0.0352(3) 0.0178(3) 0.0202(2) -0.0015(2) 0.0110(2) -0.0015(2) Cl3 0.0297(3) 0.0222(3) 0.0226(3) -0.0035(2) -0.0076(2) -0.0016(2) Cl4 0.0196(2) 0.0179(3) 0.0261(3) -0.0025(2) 0.0036(2) -0.00356(19) Si1 0.0228(3) 0.0147(3) 0.0157(3) -0.0018(2) 0.0025(2) -0.0007(2) N1 0.0138(7) 0.0169(9) 0.0147(8) -0.0033(7) 0.0005(6) -0.0025(6) N2 0.0167(8) 0.0193(9) 0.0188(8) -0.0054(7) 0.0001(7) -0.0026(7) C1 0.0147(9) 0.0200(11) 0.0188(10) -0.0031(8) -0.0003(8) -0.0037(8) C2 0.0167(9) 0.0170(10) 0.0261(11) 0.0010(9) -0.0049(8) -0.0045(8) C3 0.0202(10) 0.0261(12) 0.0200(10) 0.0061(9) -0.0069(8) -0.0104(9) C4 0.0170(9) 0.0248(11) 0.0153(9) -0.0009(8) -0.0032(8) -0.0098(8) C5 0.0251(11) 0.0400(14) 0.0147(10) 0.0005(9) -0.0011(8) -0.0194(10) C6 0.0231(11) 0.0417(15) 0.0166(10) -0.0121(10) 0.0054(8) -0.0151(10) C7 0.0166(10) 0.0300(12) 0.0212(10) -0.0127(9) 0.0034(8) -0.0098(9) C8 0.0185(10) 0.0328(13) 0.0350(13) -0.0209(11) 0.0087(9) -0.0104(9) C9 0.0170(10) 0.0229(12) 0.0420(14) -0.0147(11) 0.0035(10) -0.0013(9) C10 0.0206(10) 0.0186(11) 0.0333(12) -0.0081(9) -0.0013(9) -0.0010(8) C11 0.0145(9) 0.0221(11) 0.0177(10) -0.0066(8) 0.0003(7) -0.0054(8) C12 0.0126(9) 0.0220(11) 0.0133(9) -0.0045(8) 0.0001(7) -0.0045(8) Cl5 0.0241(3) 0.0331(3) 0.0165(2) -0.0036(2) 0.0023(2) -0.0053(2) Cl6 0.0244(3) 0.0202(3) 0.0255(3) -0.0086(2) 0.0020(2) -0.0010(2) Cl7 0.0126(2) 0.0227(3) 0.0251(3) -0.0077(2) 0.00077(18) -0.00303(18) Cl8 0.0125(2) 0.0317(3) 0.0240(3) -0.0051(2) 0.00170(19) -0.0025(2) Si2 0.0131(3) 0.0206(3) 0.0174(3) -0.0052(2) 0.0023(2) -0.0031(2) N3 0.0147(8) 0.0194(9) 0.0193(8) -0.0033(7) 0.0027(7) -0.0043(7) N4 0.0134(8) 0.0205(9) 0.0183(8) -0.0009(7) 0.0005(6) -0.0047(7) C13 0.0232(11) 0.0203(11) 0.0262(11) -0.0026(9) 0.0001(9) -0.0040(9) C14 0.0367(13) 0.0292(13) 0.0235(11) 0.0027(10) 0.0043(10) -0.0090(11) C15 0.0280(12) 0.0354(14) 0.0174(10) -0.0012(10) 0.0013(9) -0.0047(10) C16 0.0189(10) 0.0257(12) 0.0202(10) -0.0051(9) -0.0025(8) -0.0006(9) C17 0.0295(12) 0.0280(13) 0.0184(10) -0.0088(9) -0.0014(9) 0.0025(10) C18 0.0289(12) 0.0242(12) 0.0286(12) -0.0128(10) -0.0041(10) 0.0017(9) C19 0.0175(10) 0.0205(11) 0.0278(11) -0.0051(9) -0.0037(9) -0.0010(8) C20 0.0232(11) 0.0173(11) 0.0360(13) -0.0012(10) -0.0090(10) -0.0018(9) C21 0.0223(11) 0.0227(12) 0.0347(13) 0.0067(10) -0.0038(9) -0.0061(9) C22 0.0187(10) 0.0279(12) 0.0230(11) 0.0038(9) 0.0003(8) -0.0054(9) C23 0.0118(9) 0.0219(11) 0.0201(10) -0.0036(8) -0.0009(7) -0.0034(8) C24 0.0129(9) 0.0203(11) 0.0198(10) -0.0043(8) 0.0021(7) -0.0030(8) N5 0.0572(16) 0.0401(15) 0.0395(13) -0.0041(11) -0.0004(12) 0.0071(12) C25 0.0403(14) 0.0228(13) 0.0373(14) -0.0002(11) -0.0037(12) -0.0022(11) C26 0.0440(15) 0.0308(14) 0.0324(13) -0.0025(11) 0.0051(12) 0.0014(12) _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 Cl1 Si1 2.1438(8) . ? Cl2 Si1 2.1431(8) . ? Cl3 Si1 2.1850(8) . ? Cl4 Si1 2.2053(8) . ? Si1 N2 1.9714(18) . ? Si1 N1 1.9734(17) . ? N1 C1 1.337(3) . ? N1 C12 1.356(2) . ? N2 C10 1.338(3) . ? N2 C11 1.356(3) . ? C1 C2 1.398(3) . ? C1 H1 0.9500 . ? C2 C3 1.367(3) . ? C2 H2 0.9500 . ? C3 C4 1.410(3) . ? C3 H3 0.9500 . ? C4 C12 1.396(3) . ? C4 C5 1.430(3) . ? C5 C6 1.352(3) . ? C5 H5 0.9500 . ? C6 C7 1.427(3) . ? C6 H6 0.9500 . ? C7 C8 1.403(3) . ? C7 C11 1.405(3) . ? C8 C9 1.359(3) . ? C8 H8 0.9500 . ? C9 C10 1.398(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.413(3) . ? Cl5 Si2 2.1697(8) . ? Cl6 Si2 2.1476(9) . ? Cl7 Si2 2.1632(7) . ? Cl8 Si2 2.1704(8) . ? Si2 N4 1.9666(19) . ? Si2 N3 1.9825(18) . ? N3 C13 1.329(3) . ? N3 C24 1.358(3) . ? N4 C22 1.328(3) . ? N4 C23 1.363(3) . ? C13 C14 1.402(3) . ? C13 H13 0.9500 . ? C14 C15 1.367(3) . ? C14 H14 0.9500 . ? C15 C16 1.401(3) . ? C15 H15 0.9500 . ? C16 C24 1.395(3) . ? C16 C17 1.429(3) . ? C17 C18 1.349(3) . ? C17 H17 0.9500 . ? C18 C19 1.437(3) . ? C18 H18 0.9500 . ? C19 C23 1.396(3) . ? C19 C20 1.401(3) . ? C20 C21 1.366(3) . ? C20 H20 0.9500 . ? C21 C22 1.395(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.413(3) . ? N5 C25 1.155(3) . ? C25 C26 1.450(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 N2 Si1 N1 81.84(7) . . ? N2 Si1 Cl2 173.56(6) . . ? N1 Si1 Cl2 91.76(5) . . ? N2 Si1 Cl1 91.78(6) . . ? N1 Si1 Cl1 173.47(6) . . ? Cl2 Si1 Cl1 94.64(3) . . ? N2 Si1 Cl3 86.66(6) . . ? N1 Si1 Cl3 87.46(6) . . ? Cl2 Si1 Cl3 92.39(3) . . ? Cl1 Si1 Cl3 93.57(3) . . ? N2 Si1 Cl4 87.23(6) . . ? N1 Si1 Cl4 86.70(5) . . ? Cl2 Si1 Cl4 93.12(3) . . ? Cl1 Si1 Cl4 91.65(3) . . ? Cl3 Si1 Cl4 172.08(3) . . ? C1 N1 C12 118.07(17) . . ? C1 N1 Si1 128.63(14) . . ? C12 N1 Si1 113.30(13) . . ? C10 N2 C11 118.28(19) . . ? C10 N2 Si1 128.42(15) . . ? C11 N2 Si1 113.28(13) . . ? N1 C1 C2 121.60(19) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 119.02(19) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C12 C4 C3 116.98(19) . . ? C12 C4 C5 118.0(2) . . ? C3 C4 C5 125.01(19) . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.4(2) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C11 116.6(2) . . ? C8 C7 C6 125.6(2) . . ? C11 C7 C6 117.8(2) . . ? C9 C8 C7 119.4(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 121.0(2) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? N2 C10 C9 121.0(2) . . ? N2 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? N2 C11 C7 123.63(19) . . ? N2 C11 C12 115.67(18) . . ? C7 C11 C12 120.63(19) . . ? N1 C12 C4 123.76(19) . . ? N1 C12 C11 115.50(17) . . ? C4 C12 C11 120.68(18) . . ? N4 Si2 N3 81.91(7) . . ? N4 Si2 Cl6 173.88(6) . . ? N3 Si2 Cl6 92.15(6) . . ? N4 Si2 Cl7 87.29(5) . . ? N3 Si2 Cl7 86.06(5) . . ? Cl6 Si2 Cl7 93.79(3) . . ? N4 Si2 Cl5 92.91(6) . . ? N3 Si2 Cl5 174.63(6) . . ? Cl6 Si2 Cl5 93.06(3) . . ? Cl7 Si2 Cl5 92.33(3) . . ? N4 Si2 Cl8 85.42(5) . . ? N3 Si2 Cl8 87.47(5) . . ? Cl6 Si2 Cl8 92.88(3) . . ? Cl7 Si2 Cl8 170.87(4) . . ? Cl5 Si2 Cl8 93.53(3) . . ? C13 N3 C24 118.31(18) . . ? C13 N3 Si2 128.58(16) . . ? C24 N3 Si2 113.09(13) . . ? C22 N4 C23 118.00(19) . . ? C22 N4 Si2 128.48(15) . . ? C23 N4 Si2 113.49(14) . . ? N3 C13 C14 121.1(2) . . ? N3 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.0(2) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C24 C16 C15 117.0(2) . . ? C24 C16 C17 118.1(2) . . ? C15 C16 C17 124.9(2) . . ? C18 C17 C16 121.3(2) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 121.5(2) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C23 C19 C20 117.2(2) . . ? C23 C19 C18 117.5(2) . . ? C20 C19 C18 125.3(2) . . ? C21 C20 C19 119.1(2) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? N4 C22 C21 121.9(2) . . ? N4 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? N4 C23 C19 123.34(19) . . ? N4 C23 C24 115.56(19) . . ? C19 C23 C24 121.04(19) . . ? N3 C24 C16 123.78(19) . . ? N3 C24 C23 115.63(18) . . ? C16 C24 C23 120.6(2) . . ? N5 C25 C26 178.2(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 N2 Si1 N1 C1 -174.29(18) . . . . ? Cl2 Si1 N1 C1 5.02(17) . . . . ? Cl3 Si1 N1 C1 -87.30(17) . . . . ? Cl4 Si1 N1 C1 98.04(17) . . . . ? N2 Si1 N1 C12 5.65(14) . . . . ? Cl2 Si1 N1 C12 -175.05(13) . . . . ? Cl3 Si1 N1 C12 92.64(13) . . . . ? Cl4 Si1 N1 C12 -82.02(13) . . . . ? N1 Si1 N2 C10 173.33(19) . . . . ? Cl1 Si1 N2 C10 -8.04(19) . . . . ? Cl3 Si1 N2 C10 85.43(18) . . . . ? Cl4 Si1 N2 C10 -99.61(18) . . . . ? N1 Si1 N2 C11 -5.28(14) . . . . ? Cl1 Si1 N2 C11 173.34(14) . . . . ? Cl3 Si1 N2 C11 -93.19(14) . . . . ? Cl4 Si1 N2 C11 81.78(14) . . . . ? C12 N1 C1 C2 1.4(3) . . . . ? Si1 N1 C1 C2 -178.70(14) . . . . ? N1 C1 C2 C3 1.0(3) . . . . ? C1 C2 C3 C4 -2.5(3) . . . . ? C2 C3 C4 C12 1.6(3) . . . . ? C2 C3 C4 C5 -176.75(19) . . . . ? C12 C4 C5 C6 -3.5(3) . . . . ? C3 C4 C5 C6 174.8(2) . . . . ? C4 C5 C6 C7 1.7(3) . . . . ? C5 C6 C7 C8 -177.3(2) . . . . ? C5 C6 C7 C11 1.3(3) . . . . ? C11 C7 C8 C9 -1.2(3) . . . . ? C6 C7 C8 C9 177.3(2) . . . . ? C7 C8 C9 C10 1.7(3) . . . . ? C11 N2 C10 C9 -2.0(3) . . . . ? Si1 N2 C10 C9 179.45(16) . . . . ? C8 C9 C10 N2 0.0(3) . . . . ? C10 N2 C11 C7 2.5(3) . . . . ? Si1 N2 C11 C7 -178.77(16) . . . . ? C10 N2 C11 C12 -174.70(18) . . . . ? Si1 N2 C11 C12 4.1(2) . . . . ? C8 C7 C11 N2 -0.8(3) . . . . ? C6 C7 C11 N2 -179.49(19) . . . . ? C8 C7 C11 C12 176.19(19) . . . . ? C6 C7 C11 C12 -2.5(3) . . . . ? C1 N1 C12 C4 -2.3(3) . . . . ? Si1 N1 C12 C4 177.75(16) . . . . ? C1 N1 C12 C11 174.86(18) . . . . ? Si1 N1 C12 C11 -5.1(2) . . . . ? C3 C4 C12 N1 0.8(3) . . . . ? C5 C4 C12 N1 179.28(18) . . . . ? C3 C4 C12 C11 -176.20(18) . . . . ? C5 C4 C12 C11 2.3(3) . . . . ? N2 C11 C12 N1 0.7(3) . . . . ? C7 C11 C12 N1 -176.57(18) . . . . ? N2 C11 C12 C4 177.94(18) . . . . ? C7 C11 C12 C4 0.7(3) . . . . ? N4 Si2 N3 C13 176.74(18) . . . . ? Cl6 Si2 N3 C13 -1.78(18) . . . . ? Cl7 Si2 N3 C13 -95.44(17) . . . . ? Cl8 Si2 N3 C13 91.01(17) . . . . ? N4 Si2 N3 C24 -4.94(13) . . . . ? Cl6 Si2 N3 C24 176.54(13) . . . . ? Cl7 Si2 N3 C24 82.88(13) . . . . ? Cl8 Si2 N3 C24 -90.67(13) . . . . ? N3 Si2 N4 C22 -173.40(18) . . . . ? Cl7 Si2 N4 C22 100.20(17) . . . . ? Cl5 Si2 N4 C22 8.01(17) . . . . ? Cl8 Si2 N4 C22 -85.31(17) . . . . ? N3 Si2 N4 C23 4.57(13) . . . . ? Cl7 Si2 N4 C23 -81.82(13) . . . . ? Cl5 Si2 N4 C23 -174.02(13) . . . . ? Cl8 Si2 N4 C23 92.66(13) . . . . ? C24 N3 C13 C14 -1.3(3) . . . . ? Si2 N3 C13 C14 176.97(16) . . . . ? N3 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C24 -1.0(3) . . . . ? C14 C15 C16 C17 177.4(2) . . . . ? C24 C16 C17 C18 1.4(3) . . . . ? C15 C16 C17 C18 -176.9(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C23 -1.4(3) . . . . ? C17 C18 C19 C20 175.9(2) . . . . ? C23 C19 C20 C21 0.0(3) . . . . ? C18 C19 C20 C21 -177.3(2) . . . . ? C19 C20 C21 C22 -1.3(3) . . . . ? C23 N4 C22 C21 1.2(3) . . . . ? Si2 N4 C22 C21 179.09(15) . . . . ? C20 C21 C22 N4 0.7(3) . . . . ? C22 N4 C23 C19 -2.6(3) . . . . ? Si2 N4 C23 C19 179.21(15) . . . . ? C22 N4 C23 C24 174.72(17) . . . . ? Si2 N4 C23 C24 -3.5(2) . . . . ? C20 C19 C23 N4 2.0(3) . . . . ? C18 C19 C23 N4 179.54(18) . . . . ? C20 C19 C23 C24 -175.17(19) . . . . ? C18 C19 C23 C24 2.4(3) . . . . ? C13 N3 C24 C16 1.1(3) . . . . ? Si2 N3 C24 C16 -177.40(16) . . . . ? C13 N3 C24 C23 -177.01(18) . . . . ? Si2 N3 C24 C23 4.5(2) . . . . ? C15 C16 C24 N3 0.0(3) . . . . ? C17 C16 C24 N3 -178.43(18) . . . . ? C15 C16 C24 C23 178.05(19) . . . . ? C17 C16 C24 C23 -0.4(3) . . . . ? N4 C23 C24 N3 -0.7(3) . . . . ? C19 C23 C24 N3 176.68(17) . . . . ? N4 C23 C24 C16 -178.88(18) . . . . ? C19 C23 C24 C16 -1.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.527 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.087 #===END data_compound_2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; trichlorosilane 2,2'-bipyridine complex ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H9 Cl3 N2 Si' _chemical_formula_sum 'C10 H9 Cl3 N2 Si' _chemical_formula_weight 291.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4724(6) _cell_length_b 7.6648(3) _cell_length_c 12.9933(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.940(2) _cell_angle_gamma 90.00 _cell_volume 1235.47(10) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3504 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 32.02 _exptl_crystal_description piece _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7897 _exptl_absorpt_correction_T_max 0.8678 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15199 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 32.00 _reflns_number_total 4277 _reflns_number_gt 3433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _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^)+(0.0420P)^2^+1.8867P] 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_extinction_coef ? _refine_ls_number_reflns 4277 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Cl1 Cl 0.24646(4) 0.36411(7) 0.11154(4) 0.01532(11) Uani 1 1 d . . . Cl2 Cl 0.19732(4) -0.19754(7) 0.03864(4) 0.01930(12) Uani 1 1 d . . . Cl3 Cl 0.33393(4) 0.10591(8) -0.04988(4) 0.02015(13) Uani 1 1 d . . . Si1 Si 0.21891(5) 0.08727(8) 0.06430(5) 0.01287(12) Uani 1 1 d . . . H1A H 0.122(2) 0.140(4) -0.033(2) 0.015 Uiso 1 1 d . . . N1 N 0.12568(14) 0.0702(2) 0.17414(14) 0.0131(3) Uani 1 1 d . . . N2 N 0.32722(14) 0.0244(2) 0.17926(14) 0.0130(3) Uani 1 1 d . . . C1 C 0.01908(17) 0.0945(3) 0.15774(19) 0.0174(4) Uani 1 1 d . . . H1 H -0.0132 0.1165 0.0895 0.021 Uiso 1 1 calc R . . C2 C -0.04492(18) 0.0880(3) 0.2382(2) 0.0210(5) Uani 1 1 d . . . H2 H -0.1209 0.1011 0.2253 0.025 Uiso 1 1 calc R . . C3 C 0.00307(19) 0.0621(3) 0.3381(2) 0.0220(5) Uani 1 1 d . . . H3 H -0.0395 0.0616 0.3946 0.026 Uiso 1 1 calc R . . C4 C 0.11430(18) 0.0369(3) 0.35514(18) 0.0183(4) Uani 1 1 d . . . H4 H 0.1488 0.0188 0.4230 0.022 Uiso 1 1 calc R . . C5 C 0.17286(17) 0.0391(3) 0.27054(17) 0.0136(4) Uani 1 1 d . . . C6 C 0.28901(16) 0.0070(3) 0.27292(16) 0.0143(4) Uani 1 1 d . . . C7 C 0.35545(18) -0.0406(3) 0.36060(18) 0.0186(4) Uani 1 1 d . . . H7 H 0.3273 -0.0517 0.4255 0.022 Uiso 1 1 calc R . . C8 C 0.46336(19) -0.0718(3) 0.35205(18) 0.0214(5) Uani 1 1 d . . . H8 H 0.5104 -0.1055 0.4109 0.026 Uiso 1 1 calc R . . C9 C 0.50220(19) -0.0529(4) 0.25599(19) 0.0218(5) Uani 1 1 d . . . H9 H 0.5763 -0.0723 0.2488 0.026 Uiso 1 1 calc R . . C10 C 0.43194(17) -0.0057(3) 0.17114(17) 0.0172(4) Uani 1 1 d . . . H10 H 0.4585 0.0056 0.1055 0.021 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 Cl1 0.0149(2) 0.0131(2) 0.0174(2) 0.00005(18) -0.00049(17) -0.00096(17) Cl2 0.0216(2) 0.0135(2) 0.0222(3) -0.00282(19) -0.00014(19) 0.00000(18) Cl3 0.0196(2) 0.0266(3) 0.0152(2) 0.0028(2) 0.00586(18) 0.0034(2) Si1 0.0126(2) 0.0133(3) 0.0125(3) 0.0005(2) 0.00048(19) 0.0004(2) N1 0.0112(7) 0.0140(8) 0.0140(8) 0.0012(6) 0.0004(6) 0.0008(6) N2 0.0113(7) 0.0153(9) 0.0126(8) 0.0000(6) 0.0024(6) 0.0016(6) C1 0.0126(9) 0.0171(10) 0.0222(10) 0.0021(8) 0.0002(8) 0.0003(7) C2 0.0131(9) 0.0218(12) 0.0287(12) 0.0035(9) 0.0046(8) 0.0017(8) C3 0.0187(10) 0.0229(12) 0.0259(12) 0.0009(10) 0.0093(9) 0.0016(9) C4 0.0179(10) 0.0200(11) 0.0174(10) 0.0011(8) 0.0048(8) 0.0017(8) C5 0.0137(8) 0.0119(9) 0.0151(9) 0.0008(7) 0.0012(7) 0.0014(7) C6 0.0134(8) 0.0149(10) 0.0144(9) -0.0003(7) 0.0000(7) 0.0015(7) C7 0.0167(9) 0.0239(12) 0.0148(9) 0.0019(8) 0.0006(8) 0.0028(8) C8 0.0186(10) 0.0283(13) 0.0166(10) 0.0025(9) -0.0015(8) 0.0078(9) C9 0.0140(9) 0.0304(13) 0.0209(10) 0.0017(9) 0.0014(8) 0.0045(9) C10 0.0126(9) 0.0221(11) 0.0173(10) 0.0007(8) 0.0040(7) 0.0042(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Si1 2.2256(8) . ? Cl2 Si1 2.2206(8) . ? Cl3 Si1 2.1724(8) . ? Si1 N1 1.9364(19) . ? Si1 N2 1.9674(18) . ? Si1 H1A 1.70(3) . ? N1 C1 1.338(3) . ? N1 C5 1.349(3) . ? N2 C10 1.341(3) . ? N2 C6 1.359(3) . ? C1 C2 1.381(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C5 C6 1.467(3) . ? C6 C7 1.386(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 C9 1.392(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N2 80.87(8) . . ? N1 Si1 Cl3 175.62(6) . . ? N2 Si1 Cl3 94.85(6) . . ? N1 Si1 Cl2 88.36(6) . . ? N2 Si1 Cl2 86.34(6) . . ? Cl3 Si1 Cl2 92.32(3) . . ? N1 Si1 Cl1 87.05(6) . . ? N2 Si1 Cl1 87.14(6) . . ? Cl3 Si1 Cl1 91.81(3) . . ? Cl2 Si1 Cl1 172.55(4) . . ? N1 Si1 H1A 97.5(9) . . ? N2 Si1 H1A 178.3(9) . . ? Cl3 Si1 H1A 86.8(9) . . ? Cl2 Si1 H1A 93.3(9) . . ? Cl1 Si1 H1A 93.1(9) . . ? C1 N1 C5 120.22(19) . . ? C1 N1 Si1 122.42(15) . . ? C5 N1 Si1 117.31(14) . . ? C10 N2 C6 119.23(18) . . ? C10 N2 Si1 125.46(15) . . ? C6 N2 Si1 115.29(14) . . ? N1 C1 C2 121.2(2) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C1 C2 C3 119.1(2) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.1(2) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 121.7(2) . . ? N1 C5 C6 112.60(19) . . ? C4 C5 C6 125.7(2) . . ? N2 C6 C7 121.78(19) . . ? N2 C6 C5 113.69(18) . . ? C7 C6 C5 124.5(2) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 119.1(2) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 119.4(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N2 C10 C9 121.6(2) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? 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 N2 Si1 N1 C1 -178.26(19) . . . . ? Cl2 Si1 N1 C1 -91.70(18) . . . . ? Cl1 Si1 N1 C1 94.17(18) . . . . ? N2 Si1 N1 C5 4.32(16) . . . . ? Cl2 Si1 N1 C5 90.87(16) . . . . ? Cl1 Si1 N1 C5 -83.25(16) . . . . ? N1 Si1 N2 C10 176.1(2) . . . . ? Cl3 Si1 N2 C10 -4.8(2) . . . . ? Cl2 Si1 N2 C10 87.19(19) . . . . ? Cl1 Si1 N2 C10 -96.41(19) . . . . ? N1 Si1 N2 C6 -2.16(16) . . . . ? Cl3 Si1 N2 C6 176.89(15) . . . . ? Cl2 Si1 N2 C6 -91.09(16) . . . . ? Cl1 Si1 N2 C6 85.31(16) . . . . ? C5 N1 C1 C2 -0.2(3) . . . . ? Si1 N1 C1 C2 -177.51(18) . . . . ? N1 C1 C2 C3 2.3(4) . . . . ? C1 C2 C3 C4 -2.3(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C1 N1 C5 C4 -2.1(3) . . . . ? Si1 N1 C5 C4 175.35(18) . . . . ? C1 N1 C5 C6 177.1(2) . . . . ? Si1 N1 C5 C6 -5.5(2) . . . . ? C3 C4 C5 N1 2.1(3) . . . . ? C3 C4 C5 C6 -177.0(2) . . . . ? C10 N2 C6 C7 0.2(3) . . . . ? Si1 N2 C6 C7 178.56(18) . . . . ? C10 N2 C6 C5 -178.5(2) . . . . ? Si1 N2 C6 C5 -0.1(2) . . . . ? N1 C5 C6 N2 3.5(3) . . . . ? C4 C5 C6 N2 -177.3(2) . . . . ? N1 C5 C6 C7 -175.1(2) . . . . ? C4 C5 C6 C7 4.0(4) . . . . ? N2 C6 C7 C8 -0.2(4) . . . . ? C5 C6 C7 C8 178.3(2) . . . . ? C6 C7 C8 C9 0.5(4) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C6 N2 C10 C9 -0.4(4) . . . . ? Si1 N2 C10 C9 -178.65(19) . . . . ? C8 C9 C10 N2 0.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.805 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.099 #===END data_compound_2c _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichlorosilane 2,2'-bipyridine complex ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cl2 N2 Si' _chemical_formula_sum 'C10 H10 Cl2 N2 Si' _chemical_formula_weight 257.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4591(5) _cell_length_b 7.6165(5) _cell_length_c 11.4825(8) _cell_angle_alpha 77.309(4) _cell_angle_beta 78.019(4) _cell_angle_gamma 63.007(4) _cell_volume 562.70(7) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 1055 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 23.05 _exptl_crystal_description piece _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5749 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2451 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; The crystal structure was refined as a twin (with 2.74 percent contributions of a twin population). Twin law: (0 1 0)(1 0 0)(0 0 1). 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^)+(0.0698P)^2^+0.5803P] 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_extinction_coef ? _refine_ls_number_reflns 2451 _refine_ls_number_parameters 143 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cl1 Cl 0.1969(2) -0.0459(2) 0.19405(12) 0.0355(4) Uani 1 1 d . . . Cl2 Cl 0.5670(2) 0.1982(2) 0.31686(12) 0.0381(4) Uani 1 1 d . . . Si1 Si 0.3945(2) 0.0624(2) 0.25736(13) 0.0298(4) Uani 1 1 d D . . H1A H 0.420(8) -0.091(7) 0.365(4) 0.036 Uiso 1 1 d D . . H1B H 0.567(7) -0.041(7) 0.170(4) 0.036 Uiso 1 1 d D . . N1 N 0.3058(6) 0.2926(6) 0.1311(4) 0.0249(10) Uani 1 1 d . . . N2 N 0.1450(6) 0.2464(6) 0.3420(4) 0.0256(10) Uani 1 1 d . . . C1 C 0.4092(8) 0.2905(8) 0.0204(4) 0.0271(12) Uani 1 1 d . . . H1 H 0.5256 0.1729 0.0018 0.033 Uiso 1 1 calc R . . C2 C 0.3499(8) 0.4554(8) -0.0670(5) 0.0297(12) Uani 1 1 d . . . H2 H 0.4221 0.4504 -0.1457 0.036 Uiso 1 1 calc R . . C3 C 0.1834(8) 0.6285(8) -0.0382(5) 0.0338(13) Uani 1 1 d . . . H3 H 0.1426 0.7448 -0.0964 0.041 Uiso 1 1 calc R . . C4 C 0.0773(8) 0.6302(7) 0.0760(5) 0.0294(12) Uani 1 1 d . . . H4 H -0.0362 0.7479 0.0975 0.035 Uiso 1 1 calc R . . C5 C 0.1391(8) 0.4573(7) 0.1589(5) 0.0254(11) Uani 1 1 d . . . C6 C 0.0399(7) 0.4273(7) 0.2808(5) 0.0252(11) Uani 1 1 d . . . C7 C -0.1450(8) 0.5603(8) 0.3308(5) 0.0338(13) Uani 1 1 d . . . H7 H -0.2170 0.6869 0.2867 0.041 Uiso 1 1 calc R . . C8 C -0.2233(8) 0.5068(9) 0.4452(5) 0.0394(15) Uani 1 1 d . . . H8 H -0.3510 0.5955 0.4803 0.047 Uiso 1 1 calc R . . C9 C -0.1151(8) 0.3238(8) 0.5084(5) 0.0336(13) Uani 1 1 d . . . H9 H -0.1675 0.2855 0.5875 0.040 Uiso 1 1 calc R . . C10 C 0.0714(8) 0.1957(8) 0.4554(5) 0.0301(12) Uani 1 1 d . . . H10 H 0.1480 0.0710 0.4996 0.036 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 Cl1 0.0431(8) 0.0282(7) 0.0303(8) -0.0047(6) -0.0008(6) -0.0125(6) Cl2 0.0327(8) 0.0522(9) 0.0253(7) -0.0011(6) -0.0039(6) -0.0164(7) Si1 0.0301(8) 0.0243(8) 0.0205(8) 0.0013(6) 0.0008(6) -0.0029(6) N1 0.029(2) 0.026(2) 0.017(2) 0.0007(17) -0.0047(17) -0.0101(19) N2 0.027(2) 0.029(2) 0.016(2) -0.0018(18) 0.0007(17) -0.0087(19) C1 0.032(3) 0.028(3) 0.020(3) -0.002(2) 0.000(2) -0.014(2) C2 0.036(3) 0.040(3) 0.019(3) -0.001(2) -0.002(2) -0.024(3) C3 0.042(3) 0.035(3) 0.027(3) 0.013(2) -0.014(2) -0.022(3) C4 0.030(3) 0.022(3) 0.031(3) 0.003(2) -0.006(2) -0.009(2) C5 0.028(3) 0.022(3) 0.026(3) -0.002(2) -0.006(2) -0.010(2) C6 0.025(3) 0.020(3) 0.028(3) -0.002(2) -0.005(2) -0.007(2) C7 0.034(3) 0.031(3) 0.027(3) -0.001(2) -0.005(2) -0.007(3) C8 0.028(3) 0.042(4) 0.045(4) -0.018(3) 0.005(3) -0.010(3) C9 0.036(3) 0.040(3) 0.023(3) -0.008(2) 0.010(2) -0.018(3) C10 0.037(3) 0.029(3) 0.022(3) 0.002(2) 0.000(2) -0.016(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 Cl1 Si1 2.279(2) . ? Cl2 Si1 2.253(2) . ? Si1 N1 1.960(4) . ? Si1 N2 1.962(4) . ? Si1 H1A 1.48(4) . ? Si1 H1B 1.47(4) . ? N1 C1 1.342(6) . ? N1 C5 1.348(6) . ? N2 C10 1.350(6) . ? N2 C6 1.352(6) . ? C1 C2 1.380(7) . ? C1 H1 0.9500 . ? C2 C3 1.388(8) . ? C2 H2 0.9500 . ? C3 C4 1.383(7) . ? C3 H3 0.9500 . ? C4 C5 1.391(7) . ? C4 H4 0.9500 . ? C5 C6 1.464(7) . ? C6 C7 1.384(7) . ? C7 C8 1.376(8) . ? C7 H7 0.9500 . ? C8 C9 1.378(8) . ? C8 H8 0.9500 . ? C9 C10 1.391(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N2 79.02(17) . . ? N1 Si1 Cl2 88.21(14) . . ? N2 Si1 Cl2 88.84(15) . . ? N1 Si1 Cl1 87.66(14) . . ? N2 Si1 Cl1 87.14(14) . . ? Cl2 Si1 Cl1 174.71(9) . . ? N1 Si1 H1A 168(2) . . ? N2 Si1 H1A 90(2) . . ? Cl2 Si1 H1A 94(2) . . ? Cl1 Si1 H1A 89(2) . . ? N1 Si1 H1B 88(2) . . ? N2 Si1 H1B 167(2) . . ? Cl2 Si1 H1B 92.4(19) . . ? Cl1 Si1 H1B 91(2) . . ? H1A Si1 H1B 103(3) . . ? C1 N1 C5 120.2(4) . . ? C1 N1 Si1 121.6(4) . . ? C5 N1 Si1 118.1(3) . . ? C10 N2 C6 119.6(4) . . ? C10 N2 Si1 122.6(4) . . ? C6 N2 Si1 117.8(3) . . ? N1 C1 C2 121.4(5) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 119.1(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.3(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 120.8(5) . . ? N1 C5 C6 112.3(4) . . ? C4 C5 C6 126.9(5) . . ? N2 C6 C7 121.4(5) . . ? N2 C6 C5 112.6(4) . . ? C7 C6 C5 125.9(5) . . ? C8 C7 C6 119.2(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.6(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 119.4(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 120.8(5) . . ? N2 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? 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 N2 Si1 N1 C1 -178.3(4) . . . . ? Cl2 Si1 N1 C1 92.5(4) . . . . ? Cl1 Si1 N1 C1 -90.8(4) . . . . ? N2 Si1 N1 C5 3.2(4) . . . . ? Cl2 Si1 N1 C5 -85.9(4) . . . . ? Cl1 Si1 N1 C5 90.8(4) . . . . ? N1 Si1 N2 C10 176.6(4) . . . . ? Cl2 Si1 N2 C10 -95.0(4) . . . . ? Cl1 Si1 N2 C10 88.4(4) . . . . ? N1 Si1 N2 C6 -0.4(4) . . . . ? Cl2 Si1 N2 C6 88.0(4) . . . . ? Cl1 Si1 N2 C6 -88.5(4) . . . . ? C5 N1 C1 C2 0.6(8) . . . . ? Si1 N1 C1 C2 -177.8(4) . . . . ? N1 C1 C2 C3 1.9(8) . . . . ? C1 C2 C3 C4 -1.8(8) . . . . ? C2 C3 C4 C5 -0.7(8) . . . . ? C1 N1 C5 C4 -3.2(8) . . . . ? Si1 N1 C5 C4 175.2(4) . . . . ? C1 N1 C5 C6 176.3(5) . . . . ? Si1 N1 C5 C6 -5.2(6) . . . . ? C3 C4 C5 N1 3.3(8) . . . . ? C3 C4 C5 C6 -176.3(5) . . . . ? C10 N2 C6 C7 -1.8(8) . . . . ? Si1 N2 C6 C7 175.2(4) . . . . ? C10 N2 C6 C5 -179.3(5) . . . . ? Si1 N2 C6 C5 -2.2(6) . . . . ? N1 C5 C6 N2 4.6(6) . . . . ? C4 C5 C6 N2 -175.8(5) . . . . ? N1 C5 C6 C7 -172.7(5) . . . . ? C4 C5 C6 C7 6.9(9) . . . . ? N2 C6 C7 C8 0.0(8) . . . . ? C5 C6 C7 C8 177.0(5) . . . . ? C6 C7 C8 C9 1.0(9) . . . . ? C7 C8 C9 C10 -0.2(9) . . . . ? C6 N2 C10 C9 2.7(8) . . . . ? Si1 N2 C10 C9 -174.2(4) . . . . ? C8 C9 C10 N2 -1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.494 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.092 #===END data_compound_6f _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-dihydro-1,10-phenanthrolin-1-yl-methyldichlorosilane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H12 Cl2 N2 Si' _chemical_formula_sum 'C13 H12 Cl2 N2 Si' _chemical_formula_weight 295.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall -P2ac2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 18.4023(3) _cell_length_b 6.93200(10) _cell_length_c 9.9505(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1269.33(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6136 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 30.07 _exptl_crystal_description piece _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8817 _exptl_absorpt_correction_T_max 0.9436 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14770 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1990 _reflns_number_gt 1720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; The molecule is situated on a crystallographically imposed mirror plane. Hence, the equatorially Si-bound CH3 group and Cl atom are disordered by symmetry in 0.5 : 0.5 ratio. In the same way atoms C1 and C2, which are located out of this plane, are disordered equally over two sites. 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^)+(0.0512P)^2^+0.5596P] 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 1990 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Cl1 Cl 0.17248(3) 0.2500 0.49133(5) 0.02967(15) Uani 1 2 d S A . Cl2 Cl 0.20084(19) -0.0011(4) 0.7393(3) 0.0237(3) Uani 0.50 1 d P A 1 C13 C 0.2003(8) 0.019(2) 0.7314(16) 0.0237(3) Uani 0.50 1 d P A 2 H13A H 0.1772 -0.0851 0.6804 0.036 Uiso 0.50 1 calc PR A 2 H13B H 0.2014 -0.0151 0.8269 0.036 Uiso 0.50 1 calc PR A 2 H13C H 0.2500 0.0381 0.6988 0.036 Uiso 0.50 1 calc PR A 2 Si1 Si 0.14658(3) 0.2500 0.70829(5) 0.01766(14) Uani 1 2 d S . . N1 N 0.05119(9) 0.2281(19) 0.68583(18) 0.0143(18) Uani 0.50 1 d P . . N2 N 0.12001(7) 0.2500 0.90364(14) 0.0150(3) Uani 1 2 d S A . C1 C 0.01132(14) 0.2012(5) 0.5648(3) 0.0304(9) Uani 0.50 1 d P . . H1 H 0.0374 0.1835 0.4834 0.036 Uiso 0.50 1 calc PR A . C2 C -0.06140(15) 0.1995(5) 0.5606(3) 0.0358(11) Uani 0.50 1 d P A . H2 H -0.0838 0.1637 0.4783 0.043 Uiso 0.50 1 calc PR . . C3 C -0.10991(10) 0.2500 0.6761(2) 0.0284(4) Uani 1 2 d S . . H3A H -0.1500 0.1551 0.6823 0.034 Uiso 0.50 1 calc PR A . H3B H -0.1315 0.3791 0.6613 0.034 Uiso 0.50 1 calc PR . . C4 C -0.06721(9) 0.2500 0.80509(19) 0.0192(3) Uani 1 2 d S A . C5 C -0.10132(10) 0.2500 0.9330(2) 0.0228(4) Uani 1 2 d S . . H5 H -0.1529 0.2500 0.9364 0.027 Uiso 1 2 calc SR A . C6 C -0.06367(10) 0.2500 1.0515(2) 0.0233(4) Uani 1 2 d S A . H6 H -0.0889 0.2500 1.1348 0.028 Uiso 1 2 calc SR . . C7 C 0.01379(9) 0.2500 1.04883(18) 0.0178(3) Uani 1 2 d S . . C8 C 0.06060(11) 0.2500 1.16072(18) 0.0225(4) Uani 1 2 d S A . H8 H 0.0412 0.2500 1.2492 0.027 Uiso 1 2 calc SR . . C9 C 0.13468(11) 0.2500 1.14145(18) 0.0226(4) Uani 1 2 d S . . H9 H 0.1665 0.2500 1.2166 0.027 Uiso 1 2 calc SR A . C10 C 0.16290(10) 0.2500 1.01110(18) 0.0202(4) Uani 1 2 d S A . H10 H 0.2141 0.2500 0.9990 0.024 Uiso 1 2 calc SR . . C11 C 0.04701(9) 0.2500 0.92195(17) 0.0142(3) Uani 1 2 d S A . C12 C 0.00776(9) 0.2500 0.80111(17) 0.0157(3) Uani 1 2 d S . . 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 Cl1 0.0265(3) 0.0471(3) 0.0154(2) 0.000 0.00623(16) 0.000 Cl2 0.0205(3) 0.0211(8) 0.0296(6) -0.0008(5) 0.0063(3) 0.0030(4) C13 0.0205(3) 0.0211(8) 0.0296(6) -0.0008(5) 0.0063(3) 0.0030(4) Si1 0.0109(2) 0.0275(3) 0.0145(2) 0.000 0.00215(15) 0.000 N1 0.0128(7) 0.016(5) 0.0145(7) 0.0004(10) -0.0008(5) -0.0033(11) N2 0.0109(6) 0.0189(7) 0.0150(6) 0.000 0.0004(5) 0.000 C1 0.0226(11) 0.048(3) 0.0201(10) -0.0009(11) -0.0050(8) -0.0054(11) C2 0.0231(12) 0.056(3) 0.0281(12) 0.0023(13) -0.0114(10) -0.0073(12) C3 0.0149(8) 0.0325(11) 0.0378(11) 0.000 -0.0070(8) 0.000 C4 0.0128(7) 0.0162(8) 0.0287(9) 0.000 0.0001(6) 0.000 C5 0.0123(7) 0.0188(9) 0.0374(10) 0.000 0.0067(7) 0.000 C6 0.0197(8) 0.0208(9) 0.0293(9) 0.000 0.0123(7) 0.000 C7 0.0184(8) 0.0153(8) 0.0198(8) 0.000 0.0061(6) 0.000 C8 0.0294(9) 0.0238(10) 0.0144(7) 0.000 0.0048(7) 0.000 C9 0.0253(9) 0.0277(10) 0.0148(8) 0.000 -0.0035(7) 0.000 C10 0.0152(7) 0.0276(10) 0.0177(8) 0.000 -0.0024(6) 0.000 C11 0.0117(7) 0.0131(8) 0.0178(7) 0.000 0.0025(5) 0.000 C12 0.0118(7) 0.0157(8) 0.0196(8) 0.000 0.0006(6) 0.000 _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 Cl1 Si1 2.2108(6) . ? Cl2 Si1 2.030(3) . ? C13 Si1 1.895(14) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Si1 N1 1.776(2) . ? Si1 C13 1.895(14) 7_565 ? Si1 N2 2.0044(15) . ? N1 C12 1.406(3) . ? N1 C1 1.422(3) . ? N2 C10 1.329(2) . ? N2 C11 1.356(2) . ? C1 C2 1.339(4) . ? C1 H1 0.9500 . ? C2 C3 1.497(4) . ? C2 H2 0.9500 . ? C3 C4 1.505(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C12 1.380(2) . ? C4 C5 1.419(3) . ? C5 C6 1.368(3) . ? C5 H5 0.9500 . ? C6 C7 1.426(2) . ? C6 H6 0.9500 . ? C7 C11 1.403(2) . ? C7 C8 1.408(3) . ? C8 C9 1.377(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.403(2) . ? 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 Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 Si1 C13 117.3(7) . . ? N1 Si1 N2 83.16(7) . . ? C13 Si1 N2 90.6(5) . . ? C13 Si1 Cl2 116.7(4) . 7_565 ? N1 Si1 Cl2 115.6(4) . . ? N2 Si1 Cl2 88.42(10) . . ? N1 Si1 Cl1 95.18(6) . . ? C13 Si1 Cl1 90.3(5) . . ? N2 Si1 Cl1 178.33(5) . . ? Cl2 Si1 Cl1 92.44(10) . . ? C12 N1 C1 114.30(17) . . ? C12 N1 Si1 116.7(2) . . ? C1 N1 Si1 128.87(16) . . ? C10 N2 C11 118.71(15) . . ? C10 N2 Si1 129.46(12) . . ? C11 N2 Si1 111.84(11) . . ? C2 C1 N1 122.9(3) . . ? C2 C1 H1 118.6 . . ? N1 C1 H1 118.6 . . ? C1 C2 C3 124.8(2) . . ? C1 C2 H2 117.6 . . ? C3 C2 H2 117.6 . . ? C2 C3 C4 110.08(17) . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? C12 C4 C5 117.90(17) . . ? C12 C4 C3 119.84(17) . . ? C5 C4 C3 122.26(16) . . ? C6 C5 C4 123.32(16) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C7 119.35(17) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C11 C7 C8 116.43(15) . . ? C11 C7 C6 116.92(17) . . ? C8 C7 C6 126.65(17) . . ? C9 C8 C7 119.72(16) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.83(17) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 121.75(17) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N2 C11 C12 113.28(14) . . ? N2 C11 C7 123.56(15) . . ? C12 C11 C7 123.16(15) . . ? C4 C12 C11 119.36(16) . . ? C4 C12 N1 126.27(17) . . ? C11 C12 N1 113.98(15) . . ? 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 C13 Si1 N1 C12 95.9(10) . . . . ? N2 Si1 N1 C12 8.9(8) . . . . ? Cl2 Si1 N1 C12 93.8(8) . . . . ? Cl1 Si1 N1 C12 -171.0(8) . . . . ? C13 Si1 N1 C1 -87.7(11) . . . . ? N2 Si1 N1 C1 -174.8(11) . . . . ? Cl2 Si1 N1 C1 -89.9(10) . . . . ? Cl1 Si1 N1 C1 5.3(11) . . . . ? N1 Si1 N2 C10 175.1(4) . . . . ? C13 Si1 N2 C10 57.6(5) . . . . ? Cl2 Si1 N2 C10 59.05(10) . . . . ? N1 Si1 N2 C11 -4.9(4) . . . . ? C13 Si1 N2 C11 -122.4(5) . . . . ? Cl2 Si1 N2 C11 -120.95(10) . . . . ? N1 N1 C1 C2 -85.7(5) 7_565 . . . ? C12 N1 C1 C2 0.9(12) . . . . ? C1 N1 C1 C2 -85.7(5) 7_565 . . . ? Si1 N1 C1 C2 -175.5(7) . . . . ? N1 C1 C2 C3 8.2(8) . . . . ? C1 C2 C3 C4 -15.3(4) . . . . ? C2 C3 C4 C12 14.42(14) . . . . ? C2 C3 C4 C5 -165.58(14) . . . . ? C12 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C6 180.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C11 0.0 . . . . ? C5 C6 C7 C8 180.0 . . . . ? C11 C7 C8 C9 0.0 . . . . ? C6 C7 C8 C9 180.0 . . . . ? C7 C8 C9 C10 0.0 . . . . ? C11 N2 C10 C9 0.0 . . . . ? Si1 N2 C10 C9 180.0 . . . . ? C8 C9 C10 N2 0.0 . . . . ? C10 N2 C11 C12 180.0 . . . . ? Si1 N2 C11 C12 0.0 . . . . ? C10 N2 C11 C7 0.0 . . . . ? Si1 N2 C11 C7 180.0 . . . . ? C8 C7 C11 N2 0.0 . . . . ? C6 C7 C11 N2 180.0 . . . . ? C8 C7 C11 C12 180.0 . . . . ? C6 C7 C11 C12 0.0 . . . . ? C5 C4 C12 C11 0.0 . . . . ? C3 C4 C12 C11 180.0 . . . . ? C5 C4 C12 N1 172.3(7) . . . . ? C3 C4 C12 N1 -7.7(7) . . . . ? N2 C11 C12 C4 180.0 . . . . ? C7 C11 C12 C4 0.0 . . . . ? N2 C11 C12 N1 6.8(6) . . . . ? C7 C11 C12 N1 -173.2(6) . . . . ? C1 N1 C12 C4 -1.0(12) . . . . ? Si1 N1 C12 C4 175.9(3) . . . . ? C1 N1 C12 C11 171.7(6) . . . . ? Si1 N1 C12 C11 -11.4(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.642 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.062 #===END data_compound_3f _audit_creation_method SHELXL-97 _chemical_name_systematic ; methyltrichlorosilane 1,10-phenanthroline complex, THF solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H11 Cl3 N2 Si, C4 H8 O' _chemical_formula_sum 'C17 H19 Cl3 N2 O Si' _chemical_formula_weight 401.78 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.253(2) _cell_length_b 10.967(2) _cell_length_c 15.886(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.316(8) _cell_angle_gamma 90.00 _cell_volume 1786.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4791 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 23.27 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8459 _exptl_absorpt_correction_T_max 0.9613 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17344 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 23.50 _reflns_number_total 2643 _reflns_number_gt 2103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; The crystal structure was refined as a twin (with ratio 58:42 of the twin populations). Twin law: (1 0 0)(0 -1 0)(0 0 -1). The Si-bound methyl group and the trans-N-situated Si-bound chlorine atom are disordered over their two sites (s.o.f. 0.54; 0.46 and vice versa). 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^)+(0.0141P)^2^+7.1278P] 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 2643 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Cl1 Cl 0.4137(2) 0.14914(16) 0.20841(12) 0.0448(5) Uani 1 1 d . A . Cl2 Cl 0.0953(2) -0.12112(15) 0.23200(12) 0.0429(5) Uani 1 1 d . A . Cl3 Cl 0.1689(10) 0.1349(9) 0.3230(5) 0.0385(14) Uani 0.456(7) 1 d PD A 1 C13A C 0.181(4) 0.119(3) 0.308(2) 0.0385(14) Uani 0.544(7) 1 d PD A 2 H13D H 0.1839 0.2027 0.2859 0.058 Uiso 0.544(7) 1 calc PR A 2 H13E H 0.2281 0.1162 0.3620 0.058 Uiso 0.544(7) 1 calc PR A 2 H13F H 0.0896 0.0957 0.3172 0.058 Uiso 0.544(7) 1 calc PR A 2 C13 C 0.346(4) -0.078(4) 0.310(2) 0.0486(14) Uani 0.456(7) 1 d PD A 1 H13A H 0.4366 -0.0887 0.2918 0.073 Uiso 0.456(7) 1 calc PR A 1 H13B H 0.3047 -0.1584 0.3155 0.073 Uiso 0.456(7) 1 calc PR A 1 H13C H 0.3457 -0.0373 0.3652 0.073 Uiso 0.456(7) 1 calc PR A 1 Cl3A Cl 0.3649(8) -0.0811(7) 0.3286(3) 0.0486(14) Uani 0.544(7) 1 d PD A 2 Si1 Si 0.2565(2) 0.01428(16) 0.23314(10) 0.0323(5) Uani 1 1 d D . . N1 N 0.1597(6) 0.0891(5) 0.1348(3) 0.0268(14) Uani 1 1 d . A . N2 N 0.3360(6) -0.0793(5) 0.1387(3) 0.0241(13) Uani 1 1 d . A . C1 C 0.0643(8) 0.1716(6) 0.1344(4) 0.0348(19) Uani 1 1 d . . . H1 H 0.0338 0.2011 0.1870 0.042 Uiso 1 1 calc R A . C2 C 0.0064(7) 0.2173(6) 0.0609(5) 0.0354(18) Uani 1 1 d . A . H2 H -0.0625 0.2750 0.0646 0.042 Uiso 1 1 calc R . . C3 C 0.0484(7) 0.1796(6) -0.0159(4) 0.0334(18) Uani 1 1 d . . . H3 H 0.0125 0.2127 -0.0662 0.040 Uiso 1 1 calc R A . C4 C 0.1469(7) 0.0897(6) -0.0187(4) 0.0280(17) Uani 1 1 d . A . C5 C 0.1981(8) 0.0407(7) -0.0945(4) 0.0344(19) Uani 1 1 d . . . H5 H 0.1668 0.0694 -0.1473 0.041 Uiso 1 1 calc R A . C6 C 0.2908(8) -0.0461(6) -0.0916(5) 0.036(2) Uani 1 1 d . A . H6 H 0.3235 -0.0774 -0.1431 0.043 Uiso 1 1 calc R . . C7 C 0.3425(7) -0.0934(6) -0.0137(4) 0.0285(17) Uani 1 1 d . . . C8 C 0.4380(7) -0.1851(6) -0.0053(5) 0.0378(19) Uani 1 1 d . A . H8 H 0.4741 -0.2226 -0.0538 0.045 Uiso 1 1 calc R . . C9 C 0.4784(7) -0.2194(7) 0.0738(5) 0.0378(19) Uani 1 1 d . . . H9 H 0.5433 -0.2807 0.0798 0.045 Uiso 1 1 calc R A . C10 C 0.4258(8) -0.1658(6) 0.1450(4) 0.0357(19) Uani 1 1 d . A . H10 H 0.4545 -0.1915 0.1991 0.043 Uiso 1 1 calc R . . C11 C 0.2930(6) -0.0454(6) 0.0609(4) 0.0251(17) Uani 1 1 d . A . C12 C 0.1969(7) 0.0480(5) 0.0570(4) 0.0223(16) Uani 1 1 d . . . O1 O 0.1777(7) 0.6226(6) 0.0888(4) 0.079(2) Uani 1 1 d . . . C14 C 0.1980(11) 0.5284(9) 0.0319(6) 0.078(3) Uani 1 1 d . . . H14A H 0.2337 0.5607 -0.0214 0.094 Uiso 1 1 calc R . . H14B H 0.1149 0.4860 0.0194 0.094 Uiso 1 1 calc R . . C15 C 0.2937(9) 0.4416(9) 0.0722(6) 0.063(3) Uani 1 1 d . . . H15A H 0.3848 0.4638 0.0587 0.076 Uiso 1 1 calc R . . H15B H 0.2773 0.3564 0.0544 0.076 Uiso 1 1 calc R . . C16 C 0.2647(12) 0.4597(9) 0.1671(5) 0.083(3) Uani 1 1 d . . . H16A H 0.2048 0.3960 0.1881 0.099 Uiso 1 1 calc R . . H16B H 0.3461 0.4579 0.2009 0.099 Uiso 1 1 calc R . . C17 C 0.2058(11) 0.5760(8) 0.1702(6) 0.073(3) Uani 1 1 d . . . H17A H 0.2647 0.6332 0.2000 0.088 Uiso 1 1 calc R . . H17B H 0.1238 0.5705 0.2027 0.088 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 Cl1 0.0481(12) 0.0419(11) 0.0443(11) -0.0115(9) 0.0021(10) -0.0102(10) Cl2 0.0526(12) 0.0321(9) 0.0440(10) 0.0099(9) 0.0092(10) -0.0041(9) Cl3 0.056(3) 0.041(3) 0.019(4) -0.012(2) 0.007(2) 0.017(2) C13A 0.056(3) 0.041(3) 0.019(4) -0.012(2) 0.007(2) 0.017(2) C13 0.058(4) 0.069(2) 0.019(3) 0.004(2) -0.010(2) 0.028(2) Cl3A 0.058(4) 0.069(2) 0.019(3) 0.004(2) -0.010(2) 0.028(2) Si1 0.0442(11) 0.0311(10) 0.0214(9) -0.0003(9) -0.0016(12) -0.0019(9) N1 0.038(4) 0.016(3) 0.026(3) -0.001(2) 0.006(3) 0.002(3) N2 0.025(3) 0.023(3) 0.024(3) 0.004(2) -0.003(3) 0.000(3) C1 0.044(5) 0.027(4) 0.034(4) 0.000(3) 0.014(4) 0.003(4) C2 0.034(4) 0.026(4) 0.046(5) 0.007(4) 0.007(4) 0.009(3) C3 0.045(5) 0.024(4) 0.031(4) 0.009(3) -0.002(4) 0.001(3) C4 0.036(5) 0.024(4) 0.024(4) 0.005(3) 0.000(3) -0.004(3) C5 0.046(5) 0.036(4) 0.022(4) 0.000(3) 0.003(4) 0.003(4) C6 0.048(6) 0.033(4) 0.027(4) -0.004(3) 0.010(4) -0.006(4) C7 0.035(5) 0.030(4) 0.021(4) -0.003(3) 0.002(4) -0.002(3) C8 0.046(5) 0.031(4) 0.037(4) -0.006(3) 0.006(4) 0.005(4) C9 0.035(4) 0.030(4) 0.048(5) 0.004(4) 0.006(4) 0.007(3) C10 0.049(5) 0.031(4) 0.027(4) 0.005(3) -0.003(4) 0.007(4) C11 0.029(4) 0.023(4) 0.023(4) 0.001(3) 0.002(3) -0.010(3) C12 0.032(4) 0.012(3) 0.023(4) 0.001(3) 0.005(3) -0.004(3) O1 0.103(5) 0.073(4) 0.060(4) 0.011(4) -0.001(4) 0.028(4) C14 0.111(9) 0.080(7) 0.044(6) 0.006(5) 0.004(6) 0.031(7) C15 0.057(6) 0.063(6) 0.069(6) -0.020(5) 0.011(5) 0.009(5) C16 0.135(10) 0.077(7) 0.037(5) 0.001(5) 0.003(6) 0.029(7) C17 0.114(9) 0.050(6) 0.056(6) 0.013(5) 0.022(6) 0.010(6) _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 Cl1 Si1 2.224(3) . ? Cl2 Si1 2.222(3) . ? Cl3 Si1 2.146(4) . ? C13A Si1 1.837(19) . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C13 Si1 1.837(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Cl3A Si1 2.147(4) . ? Si1 N2 1.996(6) . ? Si1 N1 2.021(6) . ? N1 C1 1.333(9) . ? N1 C12 1.372(8) . ? N2 C10 1.325(8) . ? N2 C11 1.362(8) . ? C1 C2 1.400(10) . ? C1 H1 0.9500 . ? C2 C3 1.361(10) . ? C2 H2 0.9500 . ? C3 C4 1.412(9) . ? C3 H3 0.9500 . ? C4 C12 1.383(9) . ? C4 C5 1.420(10) . ? C5 C6 1.346(8) . ? C5 H5 0.9500 . ? C6 C7 1.441(10) . ? C6 H6 0.9500 . ? C7 C11 1.395(9) . ? C7 C8 1.409(10) . ? C8 C9 1.374(10) . ? C8 H8 0.9500 . ? C9 C10 1.386(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.422(8) . ? O1 C14 1.390(10) . ? O1 C17 1.419(11) . ? C14 C15 1.507(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.552(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.412(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 Si1 C13A H13D 109.5 . . ? Si1 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? Si1 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? C13A Si1 C13 97.2(18) . . ? C13A Si1 N2 171.2(14) . . ? C13 Si1 N2 90.7(14) . . ? C13A Si1 N1 92.3(13) . . ? C13 Si1 N1 169.6(14) . . ? N2 Si1 N1 80.12(19) . . ? C13 Si1 Cl3 96.1(14) . . ? N2 Si1 Cl3 172.3(3) . . ? N1 Si1 Cl3 93.3(3) . . ? C13A Si1 Cl3A 93.8(13) . . ? N2 Si1 Cl3A 93.9(3) . . ? N1 Si1 Cl3A 173.8(3) . . ? Cl3 Si1 Cl3A 92.7(3) . . ? C13A Si1 Cl2 96.2(13) . . ? C13 Si1 Cl2 90.4(15) . . ? N2 Si1 Cl2 87.53(18) . . ? N1 Si1 Cl2 84.43(19) . . ? Cl3 Si1 Cl2 95.9(3) . . ? Cl3A Si1 Cl2 93.6(3) . . ? C13A Si1 Cl1 90.4(13) . . ? C13 Si1 Cl1 97.2(16) . . ? N2 Si1 Cl1 84.84(18) . . ? N1 Si1 Cl1 86.94(18) . . ? Cl3 Si1 Cl1 90.8(3) . . ? Cl3A Si1 Cl1 94.3(3) . . ? Cl2 Si1 Cl1 169.34(11) . . ? C1 N1 C12 115.3(6) . . ? C1 N1 Si1 129.6(5) . . ? C12 N1 Si1 115.1(4) . . ? C10 N2 C11 119.0(6) . . ? C10 N2 Si1 126.7(4) . . ? C11 N2 Si1 114.2(4) . . ? N1 C1 C2 123.7(6) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 120.3(6) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 118.1(7) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C12 C4 C3 117.7(6) . . ? C12 C4 C5 118.3(6) . . ? C3 C4 C5 124.0(7) . . ? C6 C5 C4 120.2(7) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 122.7(7) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C11 C7 C8 116.5(6) . . ? C11 C7 C6 117.3(6) . . ? C8 C7 C6 126.2(6) . . ? C9 C8 C7 119.2(7) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.9(7) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? N2 C10 C9 121.0(6) . . ? N2 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? N2 C11 C7 123.4(6) . . ? N2 C11 C12 117.2(6) . . ? C7 C11 C12 119.4(6) . . ? N1 C12 C4 124.8(6) . . ? N1 C12 C11 113.2(6) . . ? C4 C12 C11 122.0(6) . . ? C14 O1 C17 107.1(6) . . ? O1 C14 C15 107.0(7) . . ? O1 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? O1 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C14 C15 C16 101.8(7) . . ? C14 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? C14 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.3 . . ? C17 C16 C15 103.5(8) . . ? C17 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? C17 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? C16 C17 O1 112.2(8) . . ? C16 C17 H17A 109.2 . . ? O1 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? O1 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? 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 C13A Si1 N1 C1 -8.3(14) . . . . ? C13 Si1 N1 C1 148(9) . . . . ? N2 Si1 N1 C1 176.2(6) . . . . ? Cl3 Si1 N1 C1 -7.9(7) . . . . ? Cl2 Si1 N1 C1 87.7(6) . . . . ? Cl1 Si1 N1 C1 -98.5(6) . . . . ? C13A Si1 N1 C12 172.4(14) . . . . ? C13 Si1 N1 C12 -31(9) . . . . ? N2 Si1 N1 C12 -3.1(5) . . . . ? Cl3 Si1 N1 C12 172.8(5) . . . . ? Cl2 Si1 N1 C12 -91.6(4) . . . . ? Cl1 Si1 N1 C12 82.2(4) . . . . ? C13 Si1 N2 C10 -4.3(16) . . . . ? N1 Si1 N2 C10 -179.4(6) . . . . ? Cl3A Si1 N2 C10 -1.2(6) . . . . ? Cl2 Si1 N2 C10 -94.6(6) . . . . ? Cl1 Si1 N2 C10 92.8(6) . . . . ? C13 Si1 N2 C11 177.6(16) . . . . ? N1 Si1 N2 C11 2.5(5) . . . . ? Cl3A Si1 N2 C11 -179.3(5) . . . . ? Cl2 Si1 N2 C11 87.2(4) . . . . ? Cl1 Si1 N2 C11 -85.3(4) . . . . ? C12 N1 C1 C2 -1.6(10) . . . . ? Si1 N1 C1 C2 179.1(5) . . . . ? N1 C1 C2 C3 -1.2(11) . . . . ? C1 C2 C3 C4 2.8(10) . . . . ? C2 C3 C4 C12 -1.7(10) . . . . ? C2 C3 C4 C5 178.9(7) . . . . ? C12 C4 C5 C6 1.5(10) . . . . ? C3 C4 C5 C6 -179.1(6) . . . . ? C4 C5 C6 C7 0.0(10) . . . . ? C5 C6 C7 C11 -0.2(10) . . . . ? C5 C6 C7 C8 179.1(7) . . . . ? C11 C7 C8 C9 -1.4(10) . . . . ? C6 C7 C8 C9 179.3(7) . . . . ? C7 C8 C9 C10 0.5(11) . . . . ? C11 N2 C10 C9 1.7(10) . . . . ? Si1 N2 C10 C9 -176.4(5) . . . . ? C8 C9 C10 N2 -0.6(11) . . . . ? C10 N2 C11 C7 -2.8(9) . . . . ? Si1 N2 C11 C7 175.5(5) . . . . ? C10 N2 C11 C12 -179.8(6) . . . . ? Si1 N2 C11 C12 -1.5(7) . . . . ? C8 C7 C11 N2 2.6(10) . . . . ? C6 C7 C11 N2 -178.0(6) . . . . ? C8 C7 C11 C12 179.6(6) . . . . ? C6 C7 C11 C12 -1.0(9) . . . . ? C1 N1 C12 C4 2.9(9) . . . . ? Si1 N1 C12 C4 -177.7(5) . . . . ? C1 N1 C12 C11 -176.2(5) . . . . ? Si1 N1 C12 C11 3.2(6) . . . . ? C3 C4 C12 N1 -1.3(10) . . . . ? C5 C4 C12 N1 178.1(7) . . . . ? C3 C4 C12 C11 177.7(6) . . . . ? C5 C4 C12 C11 -2.8(9) . . . . ? N2 C11 C12 N1 -1.1(7) . . . . ? C7 C11 C12 N1 -178.3(6) . . . . ? N2 C11 C12 C4 179.8(6) . . . . ? C7 C11 C12 C4 2.6(8) . . . . ? C17 O1 C14 C15 -24.8(12) . . . . ? O1 C14 C15 C16 29.1(11) . . . . ? C14 C15 C16 C17 -22.2(11) . . . . ? C15 C16 C17 O1 8.8(12) . . . . ? C14 O1 C17 C16 9.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.334 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.080 #===END data_compound_3g _audit_creation_method SHELXL-97 _chemical_name_systematic ; phenyltrichlorosilane 1,10-phenanthroline complex ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H13 Cl3 N2 Si' _chemical_formula_sum 'C18 H13 Cl3 N2 Si' _chemical_formula_weight 391.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 8.8765(4) _cell_length_b 13.2802(5) _cell_length_c 14.3927(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.071(2) _cell_angle_gamma 90.00 _cell_volume 1645.73(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5086 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.82 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8109 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17380 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3582 _reflns_number_gt 2891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _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^)+(0.0431P)^2^+0.7283P] 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 3582 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Cl1 Cl 0.34977(5) 0.15514(4) 0.13465(3) 0.01837(12) Uani 1 1 d . . . Cl2 Cl 0.58325(5) 0.33747(3) 0.19558(4) 0.01889(12) Uani 1 1 d . . . Cl3 Cl 0.71757(5) 0.22328(3) 0.39464(3) 0.01696(12) Uani 1 1 d . . . Si1 Si 0.55422(6) 0.18912(4) 0.25516(4) 0.01388(13) Uani 1 1 d . . . N1 N 0.50168(17) 0.06329(12) 0.31746(11) 0.0147(3) Uani 1 1 d . . . N2 N 0.39123(18) 0.24391(12) 0.31849(11) 0.0149(3) Uani 1 1 d . . . C1 C 0.5703(2) -0.02616(14) 0.32066(14) 0.0171(4) Uani 1 1 d . . . H1 H 0.6570 -0.0333 0.2933 0.020 Uiso 1 1 calc R . . C2 C 0.5185(2) -0.11027(15) 0.36324(14) 0.0204(4) Uani 1 1 d . . . H2 H 0.5699 -0.1732 0.3643 0.025 Uiso 1 1 calc R . . C3 C 0.3929(2) -0.10172(15) 0.40360(14) 0.0208(4) Uani 1 1 d . . . H3 H 0.3547 -0.1589 0.4303 0.025 Uiso 1 1 calc R . . C4 C 0.3219(2) -0.00656(15) 0.40457(14) 0.0181(4) Uani 1 1 d . . . C5 C 0.1976(2) 0.01530(16) 0.44959(15) 0.0227(5) Uani 1 1 d . . . H5 H 0.1527 -0.0379 0.4779 0.027 Uiso 1 1 calc R . . C6 C 0.1433(2) 0.11038(16) 0.45242(15) 0.0226(5) Uani 1 1 d . . . H6 H 0.0619 0.1225 0.4834 0.027 Uiso 1 1 calc R . . C7 C 0.2056(2) 0.19286(16) 0.40992(14) 0.0198(4) Uani 1 1 d . . . C8 C 0.1587(2) 0.29431(16) 0.41180(15) 0.0220(4) Uani 1 1 d . . . H8 H 0.0801 0.3126 0.4431 0.026 Uiso 1 1 calc R . . C9 C 0.2284(2) 0.36615(16) 0.36774(15) 0.0221(4) Uani 1 1 d . . . H9 H 0.1983 0.4347 0.3689 0.027 Uiso 1 1 calc R . . C10 C 0.3439(2) 0.33890(15) 0.32087(15) 0.0191(4) Uani 1 1 d . . . H10 H 0.3896 0.3896 0.2900 0.023 Uiso 1 1 calc R . . C11 C 0.3237(2) 0.17262(14) 0.36264(14) 0.0157(4) Uani 1 1 d . . . C12 C 0.3822(2) 0.07304(14) 0.36105(13) 0.0147(4) Uani 1 1 d . . . C13 C 0.7026(2) 0.12490(14) 0.19771(14) 0.0159(4) Uani 1 1 d . . . C14 C 0.6666(2) 0.04829(15) 0.12896(15) 0.0210(4) Uani 1 1 d . . . H14 H 0.5633 0.0233 0.1111 0.025 Uiso 1 1 calc R . . C15 C 0.7772(3) 0.00756(16) 0.08598(15) 0.0252(5) Uani 1 1 d . . . H15 H 0.7498 -0.0457 0.0409 0.030 Uiso 1 1 calc R . . C16 C 0.9280(3) 0.04503(17) 0.10922(16) 0.0268(5) Uani 1 1 d . . . H16 H 1.0032 0.0191 0.0785 0.032 Uiso 1 1 calc R . . C17 C 0.9680(2) 0.11993(17) 0.17693(16) 0.0252(5) Uani 1 1 d . . . H17 H 1.0711 0.1454 0.1933 0.030 Uiso 1 1 calc R . . C18 C 0.8575(2) 0.15832(15) 0.22142(15) 0.0202(4) Uani 1 1 d . . . H18 H 0.8876 0.2086 0.2693 0.024 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 Cl1 0.0176(2) 0.0179(2) 0.0183(2) -0.00086(19) 0.00193(19) -0.00091(18) Cl2 0.0223(2) 0.0135(2) 0.0222(3) 0.00280(19) 0.0080(2) -0.00143(18) Cl3 0.0165(2) 0.0175(2) 0.0168(2) -0.00124(18) 0.00394(18) -0.00221(18) Si1 0.0145(3) 0.0118(3) 0.0162(3) 0.0004(2) 0.0054(2) -0.0005(2) N1 0.0145(8) 0.0144(8) 0.0150(8) -0.0001(7) 0.0032(7) -0.0013(6) N2 0.0137(8) 0.0138(8) 0.0170(8) -0.0012(7) 0.0032(6) -0.0001(6) C1 0.0187(9) 0.0161(10) 0.0161(10) 0.0005(8) 0.0037(8) 0.0014(8) C2 0.0267(11) 0.0149(10) 0.0188(11) -0.0011(8) 0.0036(9) -0.0005(8) C3 0.0272(11) 0.0161(10) 0.0180(10) 0.0010(8) 0.0032(9) -0.0073(9) C4 0.0190(9) 0.0197(10) 0.0145(10) -0.0003(8) 0.0019(8) -0.0052(8) C5 0.0204(10) 0.0289(12) 0.0198(11) 0.0018(9) 0.0067(9) -0.0101(9) C6 0.0160(10) 0.0328(12) 0.0201(11) -0.0020(9) 0.0068(8) -0.0050(9) C7 0.0152(9) 0.0268(11) 0.0176(10) -0.0032(9) 0.0040(8) -0.0009(8) C8 0.0164(10) 0.0276(11) 0.0217(11) -0.0058(9) 0.0041(8) 0.0033(9) C9 0.0203(10) 0.0197(10) 0.0256(11) -0.0048(9) 0.0040(9) 0.0045(8) C10 0.0198(10) 0.0156(10) 0.0208(11) -0.0012(8) 0.0030(8) 0.0007(8) C11 0.0146(9) 0.0176(10) 0.0138(10) -0.0005(8) 0.0015(8) -0.0014(7) C12 0.0137(9) 0.0175(10) 0.0126(9) -0.0003(8) 0.0024(7) -0.0023(7) C13 0.0174(9) 0.0146(9) 0.0165(10) 0.0036(8) 0.0057(8) 0.0005(8) C14 0.0263(11) 0.0163(10) 0.0210(11) 0.0023(8) 0.0069(9) 0.0007(8) C15 0.0393(13) 0.0197(11) 0.0172(11) 0.0012(9) 0.0084(9) 0.0079(9) C16 0.0294(11) 0.0308(12) 0.0230(11) 0.0069(10) 0.0119(10) 0.0132(10) C17 0.0196(10) 0.0312(12) 0.0268(12) 0.0039(10) 0.0094(9) 0.0048(9) C18 0.0190(10) 0.0211(10) 0.0211(11) 0.0006(9) 0.0057(8) 0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Si1 2.2304(7) . ? Cl2 Si1 2.1887(7) . ? Cl3 Si1 2.2188(7) . ? Si1 C13 1.9170(19) . ? Si1 N1 2.0044(16) . ? Si1 N2 2.0236(16) . ? N1 C1 1.331(2) . ? N1 C12 1.363(2) . ? N2 C10 1.332(2) . ? N2 C11 1.358(2) . ? C1 C2 1.404(3) . ? C1 H1 0.9500 . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C3 C4 1.413(3) . ? C3 H3 0.9500 . ? C4 C12 1.399(3) . ? C4 C5 1.439(3) . ? C5 C6 1.356(3) . ? C5 H5 0.9500 . ? C6 C7 1.430(3) . ? C6 H6 0.9500 . ? C7 C11 1.407(3) . ? C7 C8 1.412(3) . ? C8 C9 1.373(3) . ? C8 H8 0.9500 . ? C9 C10 1.405(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.423(3) . ? C13 C14 1.401(3) . ? C13 C18 1.405(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.391(3) . ? C15 H15 0.9500 . ? C16 C17 1.377(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Si1 N1 94.64(7) . . ? C13 Si1 N2 174.66(8) . . ? N1 Si1 N2 80.13(6) . . ? C13 Si1 Cl2 94.18(6) . . ? N1 Si1 Cl2 171.15(5) . . ? N2 Si1 Cl2 91.03(5) . . ? C13 Si1 Cl3 96.60(6) . . ? N1 Si1 Cl3 86.42(5) . . ? N2 Si1 Cl3 84.29(5) . . ? Cl2 Si1 Cl3 93.28(3) . . ? C13 Si1 Cl1 95.10(6) . . ? N1 Si1 Cl1 86.87(5) . . ? N2 Si1 Cl1 83.53(5) . . ? Cl2 Si1 Cl1 91.63(3) . . ? Cl3 Si1 Cl1 166.94(3) . . ? C1 N1 C12 118.02(16) . . ? C1 N1 Si1 127.25(13) . . ? C12 N1 Si1 114.73(12) . . ? C10 N2 C11 118.05(16) . . ? C10 N2 Si1 128.04(13) . . ? C11 N2 Si1 113.92(12) . . ? N1 C1 C2 121.95(18) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.12(18) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 118.99(18) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C12 C4 C3 116.83(18) . . ? C12 C4 C5 117.88(18) . . ? C3 C4 C5 125.25(18) . . ? C6 C5 C4 121.25(18) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.53(18) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C11 C7 C8 116.69(18) . . ? C11 C7 C6 118.15(19) . . ? C8 C7 C6 125.15(18) . . ? C9 C8 C7 119.07(18) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 120.40(19) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N2 C10 C9 121.83(19) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N2 C11 C7 123.95(18) . . ? N2 C11 C12 115.84(16) . . ? C7 C11 C12 120.19(17) . . ? N1 C12 C4 123.98(18) . . ? N1 C12 C11 115.05(16) . . ? C4 C12 C11 120.94(17) . . ? C14 C13 C18 116.25(18) . . ? C14 C13 Si1 124.42(15) . . ? C18 C13 Si1 119.26(15) . . ? C15 C14 C13 122.18(19) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 119.71(19) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 122.0(2) . . ? C17 C18 H18 119.0 . . ? C13 C18 H18 119.0 . . ? 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 C13 Si1 N1 C1 6.63(17) . . . . ? N2 Si1 N1 C1 -174.52(17) . . . . ? Cl3 Si1 N1 C1 -89.71(16) . . . . ? Cl1 Si1 N1 C1 101.50(16) . . . . ? C13 Si1 N1 C12 -173.62(13) . . . . ? N2 Si1 N1 C12 5.23(13) . . . . ? Cl3 Si1 N1 C12 90.05(12) . . . . ? Cl1 Si1 N1 C12 -78.74(12) . . . . ? N1 Si1 N2 C10 176.26(18) . . . . ? Cl2 Si1 N2 C10 -4.28(17) . . . . ? Cl3 Si1 N2 C10 88.92(16) . . . . ? Cl1 Si1 N2 C10 -95.80(17) . . . . ? N1 Si1 N2 C11 -4.25(13) . . . . ? Cl2 Si1 N2 C11 175.21(13) . . . . ? Cl3 Si1 N2 C11 -91.60(13) . . . . ? Cl1 Si1 N2 C11 83.69(13) . . . . ? C12 N1 C1 C2 3.0(3) . . . . ? Si1 N1 C1 C2 -177.24(14) . . . . ? N1 C1 C2 C3 -0.1(3) . . . . ? C1 C2 C3 C4 -2.5(3) . . . . ? C2 C3 C4 C12 2.0(3) . . . . ? C2 C3 C4 C5 -175.58(19) . . . . ? C12 C4 C5 C6 -1.9(3) . . . . ? C3 C4 C5 C6 175.6(2) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C5 C6 C7 C11 1.4(3) . . . . ? C5 C6 C7 C8 -178.3(2) . . . . ? C11 C7 C8 C9 0.5(3) . . . . ? C6 C7 C8 C9 -179.8(2) . . . . ? C7 C8 C9 C10 0.4(3) . . . . ? C11 N2 C10 C9 0.3(3) . . . . ? Si1 N2 C10 C9 179.82(15) . . . . ? C8 C9 C10 N2 -0.9(3) . . . . ? C10 N2 C11 C7 0.7(3) . . . . ? Si1 N2 C11 C7 -178.88(15) . . . . ? C10 N2 C11 C12 -177.79(17) . . . . ? Si1 N2 C11 C12 2.7(2) . . . . ? C8 C7 C11 N2 -1.1(3) . . . . ? C6 C7 C11 N2 179.22(18) . . . . ? C8 C7 C11 C12 177.31(18) . . . . ? C6 C7 C11 C12 -2.4(3) . . . . ? C1 N1 C12 C4 -3.5(3) . . . . ? Si1 N1 C12 C4 176.70(15) . . . . ? C1 N1 C12 C11 174.42(17) . . . . ? Si1 N1 C12 C11 -5.4(2) . . . . ? C3 C4 C12 N1 1.0(3) . . . . ? C5 C4 C12 N1 178.76(17) . . . . ? C3 C4 C12 C11 -176.82(18) . . . . ? C5 C4 C12 C11 0.9(3) . . . . ? N2 C11 C12 N1 1.7(3) . . . . ? C7 C11 C12 N1 -176.78(17) . . . . ? N2 C11 C12 C4 179.75(17) . . . . ? C7 C11 C12 C4 1.2(3) . . . . ? N1 Si1 C13 C14 63.02(17) . . . . ? Cl2 Si1 C13 C14 -116.27(16) . . . . ? Cl3 Si1 C13 C14 149.94(16) . . . . ? Cl1 Si1 C13 C14 -24.25(17) . . . . ? N1 Si1 C13 C18 -120.05(16) . . . . ? Cl2 Si1 C13 C18 60.67(16) . . . . ? Cl3 Si1 C13 C18 -33.12(16) . . . . ? Cl1 Si1 C13 C18 152.69(15) . . . . ? C18 C13 C14 C15 -0.3(3) . . . . ? Si1 C13 C14 C15 176.75(16) . . . . ? C13 C14 C15 C16 -1.8(3) . . . . ? C14 C15 C16 C17 2.1(3) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? C16 C17 C18 C13 -1.7(3) . . . . ? C14 C13 C18 C17 2.0(3) . . . . ? Si1 C13 C18 C17 -175.15(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.473 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.066